Minimizing Fire Risk at CPI Facilities Volume 2

Minimizing Fire Risk at CPI Facilities
Focus on Plant Hazards
volume two
Table of Contents
How to Handle Hydrogen In Process Plants ......................................................................................... 4
Process-unit layout, piping, instrumentation/control and materials of construction are but a few of the technical
issues requiring special attention during the design or retrofitting of process plants that use hydrogen as a
raw material
A Checklist for Safer Chemical Batch Reactions .................................................................................. 10

A good understanding of the reaction chemistry is needed for a safe process design
Designing Safer Process Plants ............................................................................................................. 12

Several often-overlooked strategies to increase inherent safety are discussed here
Preventing Self-Heating and Ignition in Drying Operations ................................................................ 17

Incident investigation reveals that the most common root cause is lack of understanding
Facts at Your Fingertips: Gas Hazard Definitions and Data .................................................................. 20

Facts at Your Fingertips: Static Electricity Discharge and Fire Prevention ......................................... 21
Designing for A Safe Process ................................................................................................................ 22
Incorporating safety considerations throughout process design lowers the risk of a hazardous event
Clearing the Air About Respiratory Protection ..................................................................................... 26

Learn the basics about selection and regulatory compliance for these potentially life-saving devices
Eye-and-Face Personal Protective Equipment ..................................................................................... 32

Protecting the eyes and face in the workplace is imperative to preventing the estimated 1020% of work-related
eye injuries that result in temporary or permanent vision loss
Managing Compliant MSDSs and Labels ............................................................................................. 36

Compliant MSDS programs depend on inventory management, regulatory knowledge and consistent authoring
Design Safer Solids Processing Plants ................................................................................................. 39

This approach defines a systematic framework and points toward relevant sources in the public domain
Finding the Right Gloves To Fit the Application ................................................................................... 45

There is a wide range of gloves available for hand protection on the job. Matching gloves to their chemicalresistance properties is one criterion for selection
Dust Control in the Chemical Processing Industries ........................................................................... 49

The prevention of dust hazards in the CPI is integral to process-safety management widereaching mitigation
schemes must be implemented
Avoiding Static Sparks In Hazardous Atmospheres ............................................................................ 53

Relatively simple steps can be taken to mitigate risks associated with static electricity in process plants
Piping Design for Hazardous Fluid Service .......................................................................................... 57

Extra considerations and precautions are needed beyond the requirements of codes and standards
Chemical Protective Clothing ................................................................................................................ 64

ISO 16602 offers a much-needed, common global language for expressing protective clothing performance
Managing Material Safety Data Sheets in the Workplace ................................................................... 67

While regulatory agencies outline requirements for communicating chemical hazards, the format of compliance is up to the employer. Software tools can be helpful aids in meeting these requirements
Dust Explosions: Prevention & Protection ............................................................................................ 70

Understand what causes these disasters and then put these practical measures in place
Prevent Explosions During Transfer Of Powders Into Flammable Solvents ...................................... 75

Explanations of the development and characteristics of explosive atmospheres and the potential for an explosion to occur are given, along with the advantages and disadvantages of preventative practices
Preventing Dust Explosions ................................................................................................................... 83

Risk management programs are critical for safe handling and processing of combustible dust as well as for
OSHA regulatory compliance
Compressed Gases: Managing Cylinders Safely ................................................................................. 86

Follow these recommendations to ensure the safe handling, storage and use of gas cylinders
Reduce Hazards in Process Vacuum Systems ...................................................................................... 93

Reduce explosion risks, and chemical and physical hazards, to ensure safer operation of vacuum pumps and
related systems
Tolerable Risk .......................................................................................................................................... 100

While determined risk is generally well understood, tolerable risk can be the missing link to complete
risk assessments
Vacuum Systems: Recommendations For Safe Operation ................................................................. 106

Follow this guidance to ensure that steam ejector systems, mechanical vacuum pumps and integrated vacuum
systems are designed, operated and maintained to ensure process safety
Feature Report
Part 1
How to Handle Hydrogen

In Process Plants
Richard C.Hachoose
CH2M HILL
Lockwood Greene
ydrogen is widely employed

for hydrogenation and other
purposes in chemicals manufacture, petroleum refining
and other chemical process
industries (Hydrogen: The Real Action
Is Today, CE, February, pp. 28ff), and
it holds promise as a fuel. However,
this gas is highly explosive, prone
to leakage and permeation, and difficult to detect, so special care must
be taken during process engineering
design of equipment and systems
that handle or contain hydrogen. This
knowledge and attention to detail is
all the more important inasmuch as
the reactions involving hydrogen tend
to be exothermic and in many cases
are conducted under high pressures
and temperatures.
Hydrogenation and other hydrogenhandling processes involve a considerable amount of process equipment, instrumentation and piping components,
such as reactors, catalyst feed vessels,
spent catalyst filters, pumps, valves,
pressure relief devices, pressure regulators and check valves. Many such
systems, particularly those for hydrogenation of organic chemicals, are located inside a building. Such facilities
must be designed with four levels of
safeguards, namely:
A high degree of automation, with
remote operations, interlocks and
alarms to monitor process and environment conditions
Certified relief devices for process
equipment and piping. The relief
devices vent discharges must be directed to safe locations
Adequate, dependable space ventilation to prevent accumulation of
hydrogen gas pockets for systems
located inside buildings
Damage-limiting building construction to protect personnel and property.
54
Process-unit layout, piping, instrumentation/control

and materials of construction are but a few of the
technical issues requiring special attention during
the design or retrofitting of process plants that use
hydrogen as a raw material
Hydrogens hazards
When gas is released or escapes from

containers, it presents detonation, deflagration and fire hazards. The wide
flammability range, high burning rate,
low ignition energy and non-luminous
flame of hydrogen accentuate the combustion hazards.
The flammability range for hydrogen in dry air at atmospheric pressure
and ambient temperature is about 4 to
75%. With so wide a range, virtually
any release of hydrogen has a great
potential of igniting. The minimum
energy required for ignition of hydrogen in air at atmospheric pressure is
about 1.6 X 108 Btu, which is considerably less than the value for other
fuels, such as methane (2.7 X 107
Btu at 14.7 psia). As a consequence
of low ignition energy, even a small
heat-producing source, such as friction
and static charge, may result in ignition when hydrogen gas is released at
high pressure. In fact, hydrogen is frequently thought of as self-igniting. All
ignition sources in the hydrogenation
system must be eliminated or safely
isolated.
The outcome of hydrogen combustion due to a release in air is cannot be
predicted. Some of the many possible
hazardous outcomes of hydrogen combustion are as follows:
Fire: In this case, a release of hydrogen gas in air ignites and burns like
fuel at a burner. The size and type of
flame will depend on the hydrogen re-
CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006
lease rate. In any case, the flame radiates very little heat, and is visually
imperceptible under artificial light or
daylight. Therefore, reliable methods
of fire detection must be provided in
facilities that handle hydrogen.
Deflagration consists of a flame that
propagates through a combustion
zone at a velocity less than the speed
of sound in the unreacted medium.
The flammability range is the same
as that for fire. The presence of confining surfaces such as piping, ducting or vessels can elevate the pressure and accelerate the flame speed.
If the flame speed exceeds the speed
of sound, the deflagration process can
transition into a detonation.
Detonations, propagating at a rate
greater than the speed of sound
within the unreacted media, generate
high pressures. Detonation requires a
richer hydrogen-oxidizer mixture and
a more-energetic source of ignition to
occur than does a deflagration. Very
high pressures can be generated in
a detonation when a pressure wave
is reflected from wall to wall inside
a building. Detonation is associated
with shock waves and an accompanying blast wave that can severely injure
personnel and damage property.
BLEVEs (boiling-liquid expanding-vapor explosions): Theoretically,
cryogenic containers with liquid hydrogen present are subject to BLEVE.
Under rapid heating (for example, due
to engulfment by fire), a vessel contain-
HYDROGENATION
IN CHEMICALS
MANUFACTURE
Hydrogenation of complex molecules is a
key reaction for organic synthesis of many
products. Examples of hydrogenation reactions that are commonly encountered in the
chemical industry include:
Saturation of unsaturated aromatics, olefins, fatty acids and esters
Reduction of nitro and nitroso compounds
to amines
Reduction of ketones, aldehydes, esters
and carboxylic acids to alcohols
The reaction typically involves an unsaturated organic compound with at least one
pair of carbon atom connected by double or triple bonds. In the reaction, hydrogen
breaks the bonds between the carbon atoms, resulting in a hydrogen atom attaching to
each carbon atom. The reactions are liquid-phase, heterogeneous and exothermic and
frequently occur at high pressures and temperatures in the presence of a catalyst. The
flow diagram shows a typical hydrogenation system.
ing pressurized liquid hydrogen may

fail suddenly, producing this explosive
effect. On the other hand, a cylinder
containing compressed hydrogen gas
is not subject to BLEVE if it fails.
Deflagrations and detonations alike
are perceived as explosions. The resulting shock waves and hot product gases
impinging upon the surroundings outside of the combustible region can also
be referred to as blast waves. There is
no combustion in a blast wave, but it
physically displaces the surrounding
gases and it propels shrapnel.
Most hydrogenation and hydrotreating reactions are performed at high
pressures (pressures as high as 100
atm or more are not unheard of) and
over wide temperature ranges; for instance, for some types of reactions, 20
to 350F. These conditions generate
high stress in equipment and piping
systems, so that achieving leak-tight
design is not a trivial matter especially in light of hydrogen having the
lowest molecular weight of an industrial gas. Aside from being prone to
leak easily through seals, the gas readily permeates through various materials that are impervious to other gases.
Materials selection
Key considerations that must be taken

into account when selecting materials
of construction for hydrogenation and
other hydrogen-handling system include the following:
Design temperature and pressure
Hydrogen embrittlement
Permeability and porosity
Compatibility between dissimilar
metals
In the design of low- and high-pressure
hydrogen systems alike, stainless steel
(Types 304, 316) is the most commonly
used material for equipment, tubing,
piping, fittings, and components. Other
construction materials that are satisfactory in hydrogen service include Monel,
Hastelloys, aluminum alloys, suitable
grades of carbon steel, glass-lined carbon steel and copper alloys. However,
the final selection should be based on
full awareness of all the raw materials,
catalysts and other substances that are
used in the process. Some process compounds can significantly affect materials suitability even when present only
in trace amounts.
Ordinary carbon steel, iron, low-alloy
steels, chromium, molybdenum, niobium, zinc, nickel, etc are not acceptable for use at cryogenic temperatures.
Cast iron is not acceptable for hydrogen service due to its porosity. Nickel
should not be used because it is subject
to severe hydrogen embrittlement.
Elastomers and plastics such as
polytetrafluoroethylene are in many
installations used for gasketing, Orings, packing, seats and other sealing
elements. Ideally, their usage in hydrogen service should be limited, because they can fail in the event of fire.
In a hydrogen environment, most
welds are susceptible to hydrogen em-
brittlement. Therefore, post-weld annealing is recommended to restore the

microstructure.
Outside is best
Some important factors in determining the location for a hydrogen facility

include the following:
Climate condition (warm or cold)
Process condition of the hydrogen
reaction system (pressure, temperature, other properties)
Quantity of hydrogen involved
Type of adjacent property
Nature and presence of other fuels or
oxidizers in the facility or vicinity
Protection afforded by shielding,
barricading, or other means.
From a safety standpoint, the ideal location of a hydrogenation or other hydrogen-handling facility is outdoors.
This allows any hydrogen leak to
quickly disperse into the atmosphere,
thus minimizing the potential for a
deflagration or detonation. A separate,
dedicated building, away from the rest
of other buildings is the next best option for location of a hydrogenation
system.
In cases where a reactor must be located indoors, the building should be
designed to prevent leakage and migration of hydrogen vapors into other
parts of the building, as discussed
below. The reactor should be installed
on an outer building wall on the top
floor; or at a building corner, where
there are at least two walls for venting. A missile containment courtyard
with limited access should be provided
in front of the hydrogenation building,
facing pressure relief panels.
The minimum distance requirements
between properties constitutes a critical parameter that must be evaluated early during
the design phase. There are several useful
55
TABLE 1. PIPING SYSTEMS FOR HYDROGEN
Feature Report
Piping materials and designs should be in compliance with ANSI/ASME B31.1,

ANSI/ASME B31.3, NFPA 55 and, if relevant, other industry standards and codes
Critical piping systems should be protected from accidental damage. Install
barriers to shield critical process piping, such as hydrogen supply lines
sources of information that relate hydrogen

quantity to separation distance. Two such
sources are the U.S. National Fire Protection Assn.s NFPA 59 (Table 5.4.1.2 Non-refrigerated Container Installation Minimum
Distances) and Data Sheet FM 1-44 of FM
Global (Johnston, R.I.).
As a matter of good engineering practice, the separation distance should be
checked by energy release calculations
involving the rupture of an overpressurized vessel. The energy release
is converted to equivalent pounds of
TNT, a quantity which is related to
shock and gas pressure waves. From
the calculation, one can determine the
resultant blast wave pressure at any
distance from the source of explosion.
Damage-limiting construction
All buildings used in hydrogen services must be designed to limit personnel injury and facility damage in the
event of fire or explosion. The building
should be constructed in accordance
with the International Building Code,
the NFPA (e.g. 55, 68), the Code of
Federal Regulations 29CFR1910.103
(in the U.S.), as well as with any other
codes and insurance regulations that
have jurisdiction in the location. Damage-limiting construction for the building requires pressure resistant walls
to contain explosion and pressure-relieving panels to vent an explosion.
Both NFPA 68 and FM Globals
datasheet FM 1-44 provide useful
methods for sizing deflagration vent
panels. Under the FM 1-44 guidelines,
for example, the facility must meet the
following design criteria:
The ratio of the enclosure surface
area (As) to vent area (Av) should
equal less than 7.25.
A minimum of 1 ft2 of vent area is
required for every 15 ft3 of room volume. (Note, however, that this requirement results in large facilities,
which are costly in todays economy.
It is therefore recommended to consult with all stakeholders early in
the design, to establish the appropriate codes, guides and standards
for use in the design. This point
is particularly important because
other codes, such as NFPA 68, do
not require this ratio criterion.)
The pressure-resistant walls must
be designed to a minimum pressure
56
All hydrogen lines should be labeled as HYDROGEN, with flow-direction arrows

Hydrogen gas lines should not be buried. If underground installation cannot be
avoided, the piping should be installed in an open trench with removable grating
Avoid locating hydrogen lines beneath power transmission lines
All piping lines in a hydrogen system should be electrically bonded per the
NFPA 70 electrical code to prevent static charge accumulation in the system
All piping and tubing joints should be made by welding or brazing. Flanges
should only be used where absolutely necessary
Assure adequate structural flexibility to limit forces and moments between fixed
systems. Expansion joints and loops are acceptable in hydrogen service
Design piping-support members to account for all concurrently acting loads
transmitted into such members
If polytetrafluoroethylene gaskets are used, install them in such a way that they
are constrained on all sides (to prevent cold flow and subsequent leakage)
Design reactor piping with double block and bleed arrangements to separate
equipment and piping systems rated at high and at low pressures
of 100 and a maximum of 216 lb/ft2.

As good engineering practice, the
pressure-resistant-wall rating should
also be confirmed by calculations of
the shock and gas pressure waves
generated by the energy release of an
overpressurized reactor (equivalent
pounds of TNT).
Some features of a safely designed
building in which hydrogen is stored
or used are as follows:
Hinged doors swing outward in an
explosion
There are no pockets or space where
hydrogen gas could accumulate
Window panes (if installed) are shatterproof or plastic in frame
Floors, walls and ceilings are designed and installed to limit the
generation and accumulation of
static electricity
Floors, walls and ceilings are designed for at least 2 h of fire resistance
Walls or partitions are continuous
from floor to ceiling, and securely
anchored
The building is constructed of noncombustible materials, on a substantial frame
Restrained deflagration vent panels
are present
There is adequate ventilation, and
any heating in rooms is limited to
steam, hot water, or other indirect
means
Deflagration venting is provided in
exterior walls or the roof
There are no national codes, standards
or guides that cover design-limiting
construction for detonation occurrence.
Since detonation takes microseconds to
occur, per NFPA 68, it cannot be successfully vented. Also, there are currently no known pressure relief devices
that can react to a detonation speed.
Piping and supply lines
The attributes of a piping system suitable for handling hydrogen are summarized in Table 1. Although some
of those attributes, such as the ones
relating to structural matters, are
shared by other piping systems, the
adherence to then is especially important with hydrogen.
The piping to convey hydrogen gas
from cylinders entails special considerations. If the cylinders cannot be
stored outside, then a well ventilated
storage shed is required. The temperature in the shed must be kept below
50C. Hydrogen cylinders must be
segregated from cylinders, tanks, silos
or other containers that store oxidant
gases or other oxidants.
Hydrogen cylinders supplying the
process must be connected through
approved gas manifold. The following
components and attributes are typical
in such a hydrogen supply line:
The gas manifold usually consists
of pressure regulators, pressure
gauges, relief valve(s), vent connections, and provision for automatic switchover between online
and standby cylinders. An alarm
for alerting operator to a switchover
must be provided. A supply of inert
gas, usually nitrogen, must be provided for purging the hydrogen lines
before and after use. Hydrogen detection sensors with alarms are also
required in the area
TABLE 2. INSTRUMENTATION AND CONTROL
FOR HYDROGEN-HANDLING SYSTEMS
All instrumentation and wiring designed to meet the electrical hazardous area
classification of Class I, Division (I or II), Group B
Instruments designed with appropriate range, accuracy, reliability and response
time. The appropriate response times of the complete loop, from input device to
final control element, should be consistent with the fast process kinetics of most
reactions involving hydrogen
Critical safety instruments provided with redundancy
Computer control system provided with data acquisition capability, backup
power, and fail-safe action on the loss of electrical power or instrument air
Remote location for the control system provided. Design the process plant to operate without personnel in the reactor vicinity when a hydrogenation process is taking
place. However, controls should also be provided to permit local operation
TABLE 3. INTERLOCKS OFTEN USED WITH REACTORS
Upset Process Condition
Interlock Action
1. On high temperature in
the reactor
Shut off the hydrogen supply and open vent line

(block and bleed design).
Shut off the reactor heating system.
Turn on the reactor cooling system.
2. On high pressure in the

reactor

Vent off the hydrogen to atmosphere.
3. On low speed of reactor

agitator

4. On hydrogen detection
in reactor room

Start the room emergency exhaust fan.
Shut off all rotating equipment motors in room.
5. On flame out of the flare

unit

An excess flow valve is required to

shut down the hydrogen supply in
the event of downstream line rupture or similar failures
Automated block and bleed valves
should be provided to isolate the
cylinders from the reactor or other
process equipment. A bleed line having a flame arrestor must be vented
outside at a safe location
Cylinders must be adequately
earthed, and piping line bonded.
Check valves must be installed in appropriate locations to prevent backflow of process contents into the line
Control and monitoring
Minimum instrumentation and control practices for hydrogen plants are

summarized in Table 2. Note the importance of adopting a fail-safe design
philosophy. Critical process-safety
interlocks, soft- and/or hard-wired,
should be actuated by redundant in-
strument sensors. Examples of critical safety instruments installed with

redundancy are those for hydrogenation-reactor process temperature and
pressure, and hydrogen detection in
confined spaces. Some of the common
interlocks associated with hydrogenation reactors are found in Table 3.
Hydrogen detection: Because hydrogen gas is colorless and odorless,
means for its detection must be provided in all areas where leakage or
hazardous accumulations may occur.
For hydrogen-detection sensors installed in confined spaces, current
standard practice at hydrogenation
plants calls for alarm setpoint at 1%
concentration by volume in the ambient air (which is 25% of the lower
flammability limit, as given earlier).
Furthermore, operators should not
enter any confined space in which the
ambient hydrogen concentration is
greater than 0.25%.
Indoor process units that employ hydrogen should be supplied with fixed
and portable hydrogen sensors. Portable sensors are used by personnel
when entering an area where a leak
may have occurred. It is suggested
that the fixed detectors be located in
the following areas:
Reactor room, where hydrogen leakage, accumulation or spill is possible
Storage area, where hydrogen connections are routinely made and
separated
Building-air intake ducts, if hydrogen could be carried into the building
Building-air exhaust ducts if hydrogen could be released inside the
building
The appropriate response to a detection of the presence of hydrogen in
ambient air varies with the likely
degree of risk. Examples of common
responses include isolation of the hydrogen supply source, shutdown of
the hydrogen-handling and process
system, provision for issuing a visual
and audible warning, and/or increased
ventilation of the enclosed space. In
addition, remote television monitoring
should be considered for systems not
visible from the control room.
Fire detection: Because a hydrogen
flame in air is usually almost invisible
and because the emissivity of a hydrogen flame is low, the flame is hard to
see or feel. So, aside from the detection
of the gas itself, the design of a hydrogen-using facility must provide detection of a hydrogen flame in all areas
where leaks or hazardous accumulations omay occur. Infrared (IR) and
ultraviolet (UV) are two technologies
commonly used.
Process venting
In any hydrogen-using facility, provision must be made for safe disposal of

unused hydrogen. The most-common
methods employ burn-off flares or
roof-venting.
For large quantities of unused hydrogen (the definition of large varying
by industry), a flare system is generally the choice. The hydrogen-containing exhaust process gas is piped to a
remote area, where it is burned with
air in a multiple burner arrangement.
57
Feature Report
Flare systems are equipped with pilot
ignition and a warning systems in case
of flameout The exhaust-gas header to
the flares is usually kept under slight
negative pressure, so extra care must
be taken to ensure that the vent systems is leaktight to avoid air intrusion
and possible detonation.
Although flare-system design technology is mature, flares continue to
pose hazards of flame stability, flame
blowoff, and flame blowout. To minimize the malfunction of flare systems,
it is important to keep the stack discharge velocity between 10 to 20% of
the sonic velocity in hydrogen at the
temperature prevailing in the exhaust
line. Velocities above the recommended
range may cause the flame to blow off
or blow out.
For roof venting, the main variables
to consider are such site-specific conditions as the prevailing-wind direction and speed, proximity to adjacent
buildings, vent stack height, and local
discharge limitations or other environmental restrictions.
In a roof-vent system for a process
plant in which hydrogen is used, it
is better to vent each major piece of
equipment (such as each of several
hydrogenation reactors) separately
instead of using an interconnected
collection header. The separate-vents
approach avoids the possibility of any
high-pressure, high-throughput discharges overpressurizing the low-pressure parts of the system. If, however,
collection headers cannot be avoided,
be sure to size the header to handle
the flows from all discharges with only
minimal back pressure developing at
the lowest-pressure equipment.
The roof-vent lines should be designed with inert-gas (usually nitrogen) purging and steam snuffing at the
end of each line. The purging takes air
out of the system before introduction
of hydrogen, and removes hydrogen at
the end of the process. The design activity must include a review of all piping and equipment system to ensure
that they can be adequately purged
and leak tested prior to admission of
hydrogen. The vent piping must be
designed with care to prevent steam
condensate from flowing back into the
process equipment. During plant operation, both nitrogen and steam flow
58
should be commenced upon the introduction of hydrogen gas in the process

equipment.
Avoidance of flammable atmospheres is a key aspect of preventing
combustion hazards. If the exhaust
vent stream happens to be solventladen, the stream should be passed
through the condenser, scrubber or absorber prior to discharge to the atmosphere. For additional safety, a certified flame arrester should be installed
in the vent line. Be aware, however,
that flame arresters certified for use
with hydrogen are still not common;
the equipment suppliers are still in
the process of development and certification.
The venting system must be designed to handle both normal and
emergency venting requirements.
Normal venting usually involves, for
example, exhaust gas streams from
process reactions, distillation, and
equipment and piping-systems purges,
which are handled in the venting systems as just discussed. For emergency
venting, the plant must install safety
valve or rupture disks, as appropriate,
on vessels, lines, and component systems for emergency venting to prevent
damage by overpressure. Each safety
device must, of course, be sized for the
complete system that it protects.
Although there are a few exceptions, most hydrogenation reactions
are not usually subject to runaway.
In cases where a potential for runaway does exist, the emergency vent
system should be sized by a rigorous methodology such as that developed by AIChEs Design Institute for
Emergency Relief Systems (DIERS).
As a rule, rupture disks are used for
runaway conditions because their
response time is faster than that of
safety valves. In many cases, a rupture disk is installed in series with a
safety relief valve, to protect that valve
from corrosive chemicals or sticky
solids such as catalyst particles. As
a minimum, if there is no indication
of a runaway-reaction potential, the
relief devices should be sized for fire
exposure conditions and set to relieve
at the maximum allowable working
pressure (MAWP) of the vessel.
The vent line from emergency devices should be routed to a catch tank.
This tank should be sized for at least

one and half times the volume of the
largest process vessel at the facility,
to provide liquid containment and
phase separation. Both horizontal
and vertical catch tanks are common
in practice. The tanks and vent headers are usually purged with nitrogen
to reduce oxygen concentration to
below 5% by volume. All nozzles, attachments, supports, and internals
for the catch tank should be designed
for shock loadings resulting from thermal effects and slugs of liquid during
emergency relief.
Room ventilation
In light of hydrogens wide flammability range and low ignition energy, hydrogen leaks or spills in a non-ventilated, confined space can readily form
an ignitable gas mixture. Accordingly,
all such spaces should be provided
with room ventilation, in addition to
the aforementioned hydrogen-concentration monitoring. Confined spaces
for hydrogenation systems are usually
designed for 15 to 20 air changes per
hour during normal conditions, and 30
to 40 when high hydrogen concentration has been detected. To accommodate the necessary ramped-up volumetric flowrate for emergencies, the
ventilation exhaust fan should be a
variable-speed or two-speed unit. Exhaust fans must be fabricated of nonsparking materials, and their motors
rated for the same electrical classification as that of the other motors in
the room.
Rooms in which hydrogenations or
other hydrogen-using operations take
place must be kept at a negative pressure with respect to outside areas to
prevent outward hydrogen flow. The
room pressure should be monitored,
with provision for an alarm to sound.
Electrical requirements
Most fires in hydrogenation facilities

are caused by electrical faults, so careful consideration needs to be given to
the design of electrical equipment or
wiring in such a facility. Electrical
systems should be designed to comply
with the Electrical Area Hazardous
Classification. Per the NFPA 70 Code,
an area where flammable hydrogen
mixture is normally present is clas-
sified as Class I, Division 1, Group

B, whereas an area where hydrogen
is contained and only present under
abnormal conditions is classified as
Class I, Division 2, Group B. All potential sources of ignition should be
prohibited in such areas.
Electrical installations in Class I,
Division 1, should meet the following
requirements:
Certified for use in hydrogen environment
Intrinsically safe per NFPA 70 and
Underwriters Laboratories Specification UL 913
Non-certified electrical equipment
to be located in purged enclosures.
In this case, the enclosure should
be maintained under positive pressure and purged with an inert gas
such as nitrogen. This is a meaningful requirement at present, because
there are no commercially available
motors that are suitable for use in
Class 1 Division 1 Group B environment; therefore, purged enclosures
are employed routinely in this application
All piping joints electrically bonded
All portable equipment electrically
grounded prior to use
For Class I, Division 2, Group B environments, explosionproof motors
are not available. Standard totally
enclosed, fan cooled (TEFC) motors
can be used, provided that there are
no arcing devices in the motor. Motors
suitable for this area classification
should include an approved thermal
switch, which limits the external surface temperature of the motor housing
for the Group B rating. Installations
for explosionproof equipment should
meet NFPA 70 and 496 guidelines as
a minimum.
Fire protection
A fire protection system is required for

all hydrogenation facilities. At a minimum, the design of the system should
include all the following features:
Automatic process shutdown system
on fire detection
Water sprinkler system
Water deluge system
Dry-chemical extinguishing system
Dry-chemical extinguishers, carbondioxide extinguishers, nitrogen and
steam are all acceptable for use to
extinguish small fires. As precaution

to prevent major explosion hazards, it
is recommended that a hydrogen fire
should not be extinguished until the
hydrogen source has been isolated, to
prevent ignition of a large combustible
cloud of the gas.
Hydrogenation equipment should
be protected by water-deluge sprinkler systems designed for coverage of
at least 0.35 gallons per minute per
square foot. The fire-water supply
system must be designed with enough
capacity that when a hydrogen fire
is detected, water can be applied on
equipment in the nearby surroundings as well. The facility should be
provided with a spill protection and
drainage sized for the largest possible
single spill to prevent the spread of
fire to other areas.
Safety sum-up
A hydrogenation or other hydrogenusing facility is designed safely if it

minimizes the severity of the consequences of a mishap. The people and
facilities are separated from the potential effects of fire, deflagration, or
detonation originating from failure
of hydrogen-handling equipment. All
the confined spaces are adequately
ventilated to prevent accumulation
of flammable mixtures and all unused hydrogen gas from the process is
safely disposed of by flare system or
vented above other facilities. The instrumentation and control system is a
fail-safe design with features such as
redundant sensors for critical safety
instruments, remote monitoring of
critical information, remote operation
with process safety interlocks.

Edited by Nicholas P. Chopey
Author
Richard C Hachoose is a
Senior Principal Technologist
in the Somerset, NJ, office of
CH2M HILL Lockwood Greene
(Phone: (732) 868-2282; e-mail:
rhachoose@lg.com). He has
over 24 years of process engineering design experience in
the pharmaceutical, chemical
and metallurgical processing
industries. He is also an adjunct professor at Stevens Institute of Technology, where he teaches a course
on Chemical Technology Processes in API Manufacturing. He is a registered Chartered Engineer
in the U.K. He holds a B.Sc. (Hons) in chemical
engineering from the University of Manchester
Institute of Science and Technology (UMIST),
Manchester, England.
Circle 40 on p. 93 or go to
adlinks.che.com/5828-40
59
Solids
Environmental
Processing
Manager
A Checklist for
Safer Chemical
Batch Reactions
A good understanding of the reaction
chemistry is needed for a safe process design
Richard Kwasny , Chilworth Technology Inc.
t is a fact that safety-related incidents do occur in the chemical

process industries (CPI). These
incidents have, in part, led to increased attention to reactive-chemical
issues by industry, government and
other stakeholders. We know that good
safety-management systems take the
reactivity of chemicals as well as the
energetics of both desired and adverse
reactions into consideration.
This article provides a safety checklist that can be used as a guide for the
design of a new process. Alternatively,
it can be used to identify information
gaps when existing processes undergo
periodic review.
Runaway reactions
It is known that in many cases, thermal runaway reactions occur due to

the following factors:
1. Lack of understanding of the process chemistry and energy for the
desired reaction
2. Inadequate heat transfer capacity
at the plant level
3. Insufficient control and inadequate
plant-safety back-up systems, including emergency venting
4. Ineffective plant operational procedures and inadequate training
The reader is encouraged to add
plant-specific items to this list, as
needed. A hazard analysis can then
be used to identify appropriate controls and safeguards to reduce risk. It
is important to note that as a process
undergoes changes, the safety information also needs to be updated. The final
process-safety package should be at
such a level that it can be used for technology-transfer purposes at the R&D
or commercial-production stage by out-
sourcing contractors and by in-house

personnel. When developing safety
documentation, it is important to keep
in mind that it must comply with company policies and procedures as well as
country and local regulations.
Process safety checklist
The following items should be considered in relation to process safety.

Preliminary hazard assessment:
Determine the thermal stability of
all reaction components within the
minimum and maximum process
temperatures attainable under a
worst-case scenario
Identify unwanted interaction between reagents and solvents
Identify potential reaction contaminants that may have an inhibitory
or catalytic effect on the desired
reaction
Quantification of desired reactions:
Determine the heat of reaction and offgas rates for the desired and quench
reactions, including the heat resulting
from accumulation of reagents or slow
forming intermediates
Determine the maximum adiabatic
temperature for the reaction, and
determine the basis of safety relative to the estimated boiling point of
the reaction mixture
Understand the relative rates of all
chemical reactions
Quantification of adverse reactions:
Assess the thermal stability of the
reaction mixture over a wide temperature range
When optimizing the robustness of
the process, consider other reaction
variables, such as pH, concentration, conversion rate, off-gas rate,
stability of starting and product sub-
strates in solution and as a slurry

Consider the potential and impact of
unwanted vapor-phase reactions
Develop a chemical-interaction matrix for materials present in the
reaction mixture, classify the reactivity, and communicate this information to operational personnel
Plant considerations:
Conduct a basic energy balance to
consider the heats during various
additions, heat generated during the
chemical reaction, and the heat removal capability of the plant reactor
system. Remember to include reactor agitation as a source of energy
(~2250 Btu/h/hp)
Consider the impact of possible deviations from the intended reactant
charges and operating conditions
Identify all heat sources connected
to a reaction vessel and assume
the maximum possible worst-case
scenario
Determine the effect of the lowest
possible temperature to which the
reactor heat-transfer fluid could cool
the reaction mixture
Consider the impact of temperature
gradients and other issues, such as
increased viscosity, freezing at reactor walls, fouling, and so on, in
plant-scale equipment
General chemistry and engineering design concepts:
Design reactions that occur fairly
rapidly
If possible, avoid batch reactions
in which all the potential chemical
energy is present at the onset of the
reaction
Use semi-batch processes for exothermic reactions in which the batch
temperature and any off-gassing can
Chemical Engineering www.che.com April 2008
61
Environmental Manager
be maintained through controlled
addition of the reagent
For highly exothermic reactions,
avoid using temperature control
of the reaction mixture as the only
means for limiting the reaction rate
When scaling up a reaction, account
for the impact of vessel size on heat
generation and heat removal: The
volume of the reaction mixture increases by the cube of the vessel
radius but the heat-transfer area increases by the square of the radius
A comprehensive hazard evaluation should be conducted using appropriate estimation and experimental
techniques to identify potential reac-
tion hazards in materials, as well as

the desired and adverse reactions. We
use estimation techniques, differential
scanning calorimetry (DSC), Carius
Tube, and reaction calorimetry as
needed. Identify any adverse or thermal runaway reactions and, if needed,
characterize them using adiabatic
calorimetry, such as ARC (accelerating rate calorimetry) or an Adiabatic
Dewar Calorimeter. If required, the
vent size can be determined using
Design Institute for Emergency Relief
Systems (DIERS, an AIChE industry
alliance) methodology with data generated using an adiabatic dewar or
Vent Sizing Package (VSP; a special-
ized adiabatic calorimeter that uses

temperature, pressure, and rate data
to allow for sizing emergency vents).
The references given below were used
to develop this article and are an excellent source of information.
n
Edited by Dorothy Lozowski
Author
Richard Kwasny is the associate director of the Process Safety Laboratory at
Chilworth Technology Inc.
(250 Plainsboro Road, Building 7, Plainsboro, N.J. 08536;
Email: rkwasny@chilworth.
com; Phone: 6097994449),
where he has responsibility
for the quality, safety and
productivity of the thermal
hazard laboratory. His expertise encompasses all areas of chemical reaction
hazards and flammability of dusts, vapors and
gases. Kwasny completed his Ph.D. at London
South Bank University. His research developed,
in part, an assessment strategy to allow for the
safe scale up of reduction reactions. Before his
current position, Kwasny headed the Process
Safety & Hazard Identification group for Schering-Ploughs Chemical and Physical Services
Dept. Previously, he managed the Dow Chemical
Reactive Chemicals testing function for Canada.
Kwasny is a member of the ASTM Committee
E27 on hazard potential of chemicals.
References
3. Barton, J. and Rogers, R., Chemical Reaction

Hazards, 2nd ed., Gulf Publishing, 1997.
1. Hendershot, Dennis C., A Checklist for In4. Brethericks Handbook of Reactive Chemical
herently Safer Chemical Reaction Process
Hazards, 6th ed., Butterworth Heinemann,
Design and Operation, Center for Chemical
1999.
Process Safety International Conference and
Workshop on Risk and Reliability, 2002.
5. Guidelines for Chemical Reaction Hazard
Evaluation and Application to Process De2. Kwasny, Richard S., Hazard Assessment
sign, Center for Chemical Process Safety of
Strategies for Reduction Reactions, SouthChem_Eng1-1_177x123_M_April08
07.12.2007
11:33
the AIChE,
1995.Uhr Seite 1
bank University, London, 1999.
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62
8
7
Feature Report
Engineering
Practice
Designing
5
4
3
Safer
2
1
Process Plants
Several often-overlooked strategies
to increase inherent safety are discussed here
Victor H. Edwards, P.E., Aker Solutions
any individuals and organizations have made important contributions to the creation of inherently safer (IS)
products, processes and process plants
[13]. A brief survey of successful case
histories shows that most reported
applications relied on only a few of
the core IS principles. This paper emphasizes the opportunities presented
by three particular and often-overlooked possibilities for inherently
safer processes.
The methods proposed here ensure
integration of IS methods beginning
with process conception and continuing through process plant engineering
design. Particular emphasis is given
to matching the IS principles with the
state of the project. For example, substitution is best applied during product and process research, while limitation of effects is most effective during
plot plan layout and equipment arrangement.
The chemical process industries
(CPI) face the challenge of working
with processes and products that
present many hazards, such as
the following:
The manufacture of fuels uses and
produces products that burn with
significant energy release
Certain basic chemicals, such as
mineral acids and halogens are toxic
and/or corrosive
Many manufacturing processes either release or require significant
44
energy transfer to achieve chemical

transformation
Some manufacturing processes produce benign products but require
hazardous chemical intermediates
in their manufacture
For these reasons, rigorous process
and product safety practices must be
used throughout the lifecycle of process plants and must be applied to
their associated raw materials and
products. In recent years, this has
led to major efforts in green chemistry and engineering to develop products, manufacturing processes, and
plants that are safer for both people
and the environment.
Before green chemistry and engineering achieved prominence, there
were pioneering insights in the design of safer process plants. Early approaches to safer processes often employed additional instrumentation and
procedures. These measures were often
helpful and necessary, but instrumentation and operators can fail, especially
when faced with complexity.
Trevor Kletz [1] recognized that
What you dont have cant leak, when
he first proposed the concept of the
inherently safer chemical processes
in 1977. His approach placed an emphasis on the inherent nature of the
process. Since then, important related
concepts such as product design for
safety and safer products, process and
plant lifecycles have also advanced.
Creation of IS processes has been the
1. Process design
2. Basic controls, process alarms and
operator supervision
3. Critical alarms, operator supervision
and manual intervention
4. Automatic action safety-instrumented
systems (SIS) or ESD
5. Physical protection (relief devices)
6. Physical protection (dikes)
7. Plant emergency response
8. Community emergency response
FIGURE 1. Shown here are some

typical layers of protection that can be
employed in a modern process plant [4].
At the core is an inherently safe process
design. Moving outward from the core,
the proposed options move through the
spectrum from inherent to passive to
active to procedural or administrative
controls, which are considered to be
progressively less reliable
objectives of a number of creative individuals and organizations since Kletzs

path finding proposal, with many notable successes.
Complete coverage of the entire product/process/plant lifecycle is needed to
assure optimum health, safety and environmental performance of a chemical enterprise.
This article focuses on how to ensure maximum incorporation of IS
processes into the creation of a process plant by beginning at the product
and process research stages and concluding with the detailed design. No
effort is made to address the application of inherently safer principles beyond plant design, although these are
also important.
Layers of protection
The classical onion diagram (Figure

1) illustrates the safety layers that
technical professionals throughout
Often-overlooked IS concepts
FIGURE 2. The Flixborough tragedy ushered in a new era in process safety [6]
the CPI use to prevent process plant

incidents. This diagram helps to explain the following four basic process
risk-management strategies: Inherent, passive, active, and procedural or
administrative
Inherent safety is at the core of the
onion the process design. A process
that cannot have a major fire, explosion or toxic release is inherently safer
than one that could if one or more layers of protection were to fail.
Passive safety layers represent the
addition of such safety features as a
dike or a blast wall. Because passive
layers of protection require no active
intervention by a human or by a machine, they are deemed more reliable
than active layers of protection or
procedural layers of protection. Nonetheless, the ability to make an explosion impossible when possible is
clearly better than trying to mitigate
the effects of a potential explosion by
adding a blast wall.
Active layers of protection represent such features as the basic process
control system, a safety-instrumented
system, and mechanical interlocks.
Procedural or administrative
safety layers are generally considered
to be the least reliable and include operating procedures and operator intervention. Depending on the site-specific
hazard, procedural or administrative
controls may be entirely appropriate.
In general, the preferred ranking
of methods to control process risks is
shown below:
Inherent > passive > active > procedural or administrative
Basic concepts
Inherently safer process concepts are

summarized below [1]:
Substitution
Minimization or intensification
Moderation or attenuation
Simplification
Limitation of (hazardous) effects
Avoiding knock-on effects
Making incorrect assembly impossible
Make status clear
Tolerance of error
Ease of control
Administrative controls or procedures
In 2007, the Center for Chemical
Process Safety (CCPS) of the American Institute of Chemical Engineers
(AIChE) concluded that these eleven
basic concepts could be reduced to the
following four principles [2]:
Minimize
Substitute
Moderate
Moderate and simplify
This more concise set of principles
makes IS practices simpler to understand and easier to apply. The excellent new CCPS book (2009) goes on to
distinguish between first-order and
second-order IS:
First-order IS efforts change the
chemistry of a process
Second-order IS efforts change the
process variables
As can be seen by a survey of the process safety literature, most published
work has applied one or more of the
first four concepts of the eleven cited
by Kletz and Amyotte [1] For this
reason, this article emphasizes three
other promising concepts.
Three underutilized IS concepts are

presented here and illustrated with
examples:
1. Hybridization or transformation. One relatively new IS concept is
based on the recent innovative work
by Chen [5] who reports an inherently
safer process for the partial oxidation
of cyclohexane. Partial oxidation processes often involve hazardous conditions, as illustrated by the Flixborough,
England, tragedy in 1974 which
killed 28 people, destroyed a plant, led
to new process safety regulations, and
inspired Trevor Kletz to propose his
inherently safer design concept. The
Flixborough plant carried out liquidphase oxidation of large inventories of
hot cyclohexane in large pressurized
vessels. When containment was lost, a
large flammable vapor cloud formed,
ignited, and exploded with devastating
effect (Figure 2, from Mannan [6]).
The traditional cyclohexane-oxidation process to produce a mixture of cyclohexanone and cyclohexanol (K/A oil
or ketone/alcohol oil) was operated at
low conversion rates (typically 35%)
to avoid formation of unwanted byproducts. The K/A oil was subsequently converted into adipic acid and caprolactam
for the production of nylon.
Oxidation of cyclohexane with air
instead of oxygen is common practice
to reduce risks of transition from a
partial oxidation reaction to an uncontrolled deflagration in bubbles
or in the vapor space in the reactor.
Low
conversions
and
reaction
rates led to large inventories of liquid
cyclohexane.
During systematic research on the
flammability and deflagration hazards of cyclohexane, air and oxygen
mixtures, Chen [5] discovered that the
addition of a small amount of water
which is inert and does not participate in the reaction helped to
inert the otherwise flammable vapors.
Cyclohexane and water are known to
form minimum-boiling azeotropes.
The increase in the vapor pressure of
the cyclohexane/water liquid results
from the increased vapor pressure of
the water. The water vapor inerts the
vapor mixture by lowering the upper
flammable limit of the vapor [5].
Chens work suggests that it will be
45
Engineering Practice
46
Btu/h
safe and practical to use pure oxygen

for cyclohexane oxidation. Benefits include both IS operation and improved
productivity. They also suggest that
this approach could be extended to
safer processes for partial oxidation of
other liquid hydrocarbons using pure
oxygen.
Chens approach is a first-order IS
process innovation because it changes
the chemistry of the gas phase in a
gas-liquid reaction and prevents the
unwanted side reaction of combustion
from occurring in the gas phase.
Although reference [5] did not claim
to have demonstrated a new IS concept, Chens work is different from the
classical definition of the Substitute
principle because the same reactants,
chemical reactions, and products are
involved. If the name Substitute were
broadened to names such as Change
in Chemistry or Hybridize, then it
could be lumped in with the many successful applications that are possible
when using the Substitute concept.
Chens innovation permits rapid cyclohexane oxidation at lower temperatures and pressures, and could thus
be said to be an example of the inherently safer principle Moderate. However, Chens approach enables more
moderate conditions by narrowing the
flammability limits through the addition of a new component, water. It is
thus an example of supplementation
or hybridization.
Although not proposed by Chen [5]
himself, his work suggests that there
may be many other opportunities
for transformation or hybridization
of other potentially hazardous reactions to make them inherently safer.
Although water would be high on anyones list as a potentially transforming additive, it probably will not help
many potentially hazardous reactions.
However, there are many other chemicals that may be inert to the reaction
and thus also be capable of inerting the
vapor phase involved in an otherwise
reactive liquid-vapor reaction. For instance, there are many examples of
azeotropic mixtures in the literature
and there are many compounds that
could prove inert to oxidation reactions (such as, certain halocarbons).
Applications are not limited to
partial oxidation with air or oxygen;
Qout
3
D
Qout
Qheat generated
Heat removed
Qout
other oxidations include

1
2
chlorination and bromination reactions, for exC
ample. And there may be
A
other examples of vaporliquid reactions, such as
Reactor temperature
hydrogenation reactions,
where addition of a new FIGURE 3. Heat-generation (Q
heat generated) and heatchemical could improve removal (QOut) rates as a function of reactor temperature
the safety of the process. for three different heat-removal designs [9]. Heat genAddition of an ad- eration is equal to heat removal at points A, C, D, E, and
so steady state operation is possible. However, the
ditional compound to a B,
reactor is not stable at point D without the addition of
reaction mixture to min- controls or a modification of the design
imize hazardous reactions may add complexity to the puri- in the process variables and is a form
fication process, but it may be justified of Moderate, a second-order inherently
safer design.
by the increased safety.
CCPS [2] also cites the work of
Chens [5] paper on cyclohexane
oxidation illustrates transformation Luyben and Hendershot [8] that highor hybridization, in which the basic lights how minimization or intensifichemistry is maintained, but the ad- cation in a reaction system that is indition of another chemical component tended to improve process safety may
transforms a potentially hazardous re- lead to less robust processes with the
opposite effect.
action process into a much safer one.
I propose here that Stabilize or En2. Create a robust process to stabilize or ensure dynamic stability. sure Dynamic Stability be added to
Not all process designs are inherently the list of IS concepts to be sure that
stable, and if the process design is to be it is not overlooked in the quest for insafe, the process engineer must ensure herently safer processes.
Application of some of the other IS
dynamic stability as well as ensuring
that the steady-state mass and energy principles can adversely affect the dybalances are achieved. A number of namic stability of a process. For examprocesses exist that have narrow safe- ple, reduced liquid inventories (Minioperating limits but have been made mize) in a distillation train make the
stable by the addition of control sys- process inherently safer from one pertems. Dynamic stability and control spective because the smaller process
of chemical processes has been exten- inventory decreases the consequences
of loss of containment. However, the
sively studied [7].
Designing the process to be more smaller inventory also shortens the
inherently stable to process upsets response time of the distillation syswith and without control systems is tem to process upsets, increasing the
clearly inherently safer, although this risk that the basic control system will
principle is not addressed in most dis- not be able to restore the distillation
cussions of IS. The IS principle Ease of system to the desired operating condiControl has usually been interpreted tions and avoid a potentially unsafe
to mean a process with a control sys- operating condition and/or an untem that the operator can understand scheduled process shutdown [2].
Chemical reactors carrying out
clearly and manage effectively.
CCPS briefly mentions the advan- exothermic chemical reactions are
tages of designing processes that are perhaps the best known examples of
processes that can be dynamically
inherently more stable or robust [2]:
It is inherently safer to develop unstable. Harriott [9] provides the ilprocesses with wide operating limits lustration of an irreversible first-order
that are less sensitive to variations in chemical reaction being conducted in
the operating parameters...Sometimes a continuous-flow, stirred-tank reactor
this type of process is referred to as a (CSTR). Figure 3 shows the heat-generation rate by the chemical reaction
forgiving or robust process.
Designing a robust process increases as a function of reactor temperature.
inherent safety by imposing a change Heat-generation rates are low at low
Tools for Inherently Safer Process Plant Design

P rocess hazards reviews
Chemical interaction matrices
Dow Fire and Explosion Index and
Chemical Exposure Index
Fire, explosion and toxic-release
consequence modeling and risk
assessments
Layer of protection analysis
Spacing tables for units and for
process equipment
temperatures, but as temperature

increases, the reaction rate increases
rapidly because of the exponential
dependence of the reaction rate coefficient on temperature. At higher
reactor temperatures, the shrinking
concentration of reactant (due to conversion to product) reduces the reaction rate and partially overcomes the
still-increasing reaction-rate coefficient. The heat-generation rate eventually reaches a constant maximum
value when the reaction has reached
complete conversion.
Figure 3 also shows three different
straight lines for the heat-removal
rate from the reactor for three different reactor-cooling-system designs. To
achieve a steady-state energy balance,
the rate of heat generation (Qheat generated) by the chemical reaction must
equal the rate of heat removal (Qout)
by the reactor cooling system. That
energy balance occurs when the heat
generation curve intersects the heat
removal curve (where Qheat generated
= Qout). In Figure 3, the three different heat-removal-rate lines intersect
the reactor heat generation rate curve
at five points. At four of these points
(A, B, C, E), the steady-state energy
balance solution is stable. At each of
these points, if there is an increase in
temperature, the rate of heat removal
increases more rapidly than the rate
of heat generation by the reaction and
the reactor temperature tends to return to the desired operating point.
Similarly, if the temperature drops
slightly at one of these four operating
conditions, the rate of heat removal
decreases more than the rate of heat
generation by the reactor and the temperature trends back up to the desired
operating condition.
In contrast, point D in Figure 3 is an
inherently unstable operating condition even though the steady state rate
of heat generation by the reactor equals
the rate of heat removal by the reactor
cooling system. At point D, an increase
in reactor temperature increases the
rate of heat generation by the reactor
Dynamic process simulation

Inherent safety analysis
P eriodic design reviews during
product and process research,
development and design
R
eviews of plant siting, plot plan,
equipment arrangement and 3-D
computer models
more than it increases the rate of heat

removal by the reactor cooling system,
so the reactor temperature increases
more instead of cooling back to the desired operating point.
This further increase in reactor temperature then leads to an even larger
rate of heat generation rate by the
reactor and additional heating of the
reactor. Without any effective control
actions, the reactor temperature will
tend to increase to point E in Figure 3
before it stabilizes.
Similarly, in Figure 3 a decrease in
reactor temperature at point D could
eventually lead to the reactor temperature and conversion dropping back to
point C.
Clearly, of the three reactor coolingsystem designs represented by the
three straight lines in Figure 3, the
reactor cooling system represented by
line CDE is the least desirable from
a dynamic-stability perspective. Addition of an effective control system
might be able to provide dynamic stability but at the cost of installation
and maintenance of the control system and at the cost of residual risk if
the control system fails.
Another example of potential
sources of process instability results
from efforts to improve energy efficiencies in distillation trains through
heat integration. In these cases, the
feed to a column may be preheated
by the bottoms product of a second
downstream column. This may increase the risk of process upsets due
to increased interactions between the
two columns.
While avoidance of add-on controls
has always been a goal of inherently
safer design, achievement of that goal
has seldom mentioned the concepts
of Ensure dynamic stability or Stabilize as tools of the process engineer. It
should be considered when considering other means to assure inherently
safer processes during process design.
The process engineer should work
closely with the control systems engineer to address the dynamic stability
O
ccupied building evaluation
and design
Area electrical classification
Safety integrity level assessments
and safety instrumented systems
Human factors reviews
Ergonomics reviews
Safety case development
The design process itself
of both the uncontrolled process and

the controlled process to ensure a robust process.
3. Limit hazardous effects during
conceptual and detailed engineering. David Clark published a seminal
paper [10] on the limitation of effects
when siting and designing process
plants. He reminds us that there is a
strong, non-linear decrease of fire, explosion, and toxic effects with separation distance. Comparatively small decreases in separation distance have a
major effect, while larger increases in
separation offer diminishing returns.
Methods, such as the Dow Fire and
Explosion Index [11] and the Dow
Chemical Exposure Index [12, 13], provide quantitative screening estimates
of the hazards from various parts of a
chemical process. Other indices have
been developed and evaluated to perform a similar objective to the Dow indices [1, 2, 14]. These screening tools
can identify those parts of a process
where increased separation distances
are needed to limit potential escalation of an incident.
In one typical plant design, a 10%
increase in separation distances for
all units increases total plant investment cost by only 3%. Similarly, doubling the separation distance for a
hazardous unit representing 10% of
the investment cost of the plant would
cost only 3% more. Because of the nonlinear effect of separation distance,
doubling the separation distance for a
hazardous unit could reduce explosion
overpressures on the adjacent units
by a factor of four or more.
The strong decrease in hazardous
effects with modest increases in separation distances will often more than
justify increased capital cost.
Spacing also offers important benefits in crane and other maintenance
access, ergonomic advantages and
decreased risk of incident escalation.
Future plant expansions or process
improvements are also facilitated, although expansions that decrease spacing may increase hazardous effects.
47
Applying different IS principles
As discussed, the different IS principles are best applied at different

stages of the process plant timeline.
Although IS checklists are often used
at the screening process hazards analysis (PHA) level, much more is needed
throughout the development and design of a process plant.
For example, Substitute is best
done during the product and process
research phases before significant
investments of time and resources in
a particular product and process are
made. Hybridize or Transform is best
done during process research and development, as is Moderate.
Minimize, Simplify, and Error tolerance have the best result when applied during the process development,
conceptual design and detail design
phases. Stabilize or Ensure Dynamic
Stability is also best done during design development.
Limitation of effects, which is closely
related to passive protection, has its
greatest impact during development
of the plot plan and equipment arrangement.
IS processes and plants
As mentioned previously, the CCPS [2]

defines two levels of inherent safety:
First-order inherent safety results
References
1. Kletz, Trevor A., and Amyotte, Paul, Process
Plants a Handbook of Inherently Safer Design, 2nd Ed., Taylor and Francis, Philadelphia, PA, 2010.
2. Center for Chemical Process Safety (CCPS),
Inherently Safer Chemical Processes A
Life Cycle Approach, 2nd Ed., AIChE, New
York, NY, 2009.
3. Hendershot, Dennis C., An overview of inherently safer design, Process Safety Progress,
Vol. 25, No. 2, 98107, June 2006.
4. Dowell, III, Arthur M., Layer of protection
analysis and inherently safer processes, Process Safety Progress, Vol. 18, No. 4, 214220,
Winter 1999.
5. Chen, Jenq-Renn, An inherently safer process
of cyclohexane oxidation using pure oxygen
An example of how better process safety leads
to better productivity, Process Safety Progress,
Vol. 23, No. 1, 7281, March 2004.
6. Mannan, Sam, Ed., Lees Loss Prevention in
the Process Industries, 3rd Ed., Elsevier Butterworth Heinemann, Oxford, U.K., 2005.
7. Edgar, Thomas F., and others, Process Control,
Section 8 in Perrys Chemical Engineers Handbook, 8th Edition, Don W. Green, Editor-in-Chief,
McGraw-Hill Book, New York, NY, 2008.
8. Luyben, W.L., and Hendershot, D.C., Dynamic disadvantages of intensification in
inherently safer process design, Industrial
Engineering Chemistry Research, Vol. 43, No.
2 (2004) cited in CCPS, 2009.
9. Harriott, Peter, Process Control, McGrawHill, New York, NY, 1964.
48
from changes in the chemistry of a

process that reduces the hazards
of the chemicals used or produced.
Substitute or Hybridize efforts lead
to first-order inherent safety
Second-order inherent safety results
from changes in the process variables. Examples include Minimize,
Simplify and Stabilize the operations.
It is also helpful to distinguish between IS processes and IS plants.
Even when hazards cannot be
eliminated from the chemistry of
the process, the plant using the potentially hazardous process can be
made inherently safer through judicious design.
Note also that even with IS process
chemistry, it is essential to employ
IS principles during the process and
plant design to ensure an IS plant.
Tools for IS plant design
There are a number of tools available

to aid in designing process plants that
are inherently safer (Box, p. 18). Although inherently safer reviews are a
valuable tool for identifying opportunities for improvement, it is important
to keep the principles of inherently
safer in mind throughout the design
process.
n
Edited by Suzanne Shelley
10. Clark, David G., Applying the limitation of effects inherently safer processing strategy when
siting and designing facilities, Process Safety
Progress, Vol. 27, No. 2, 121130, June 2008.
11. Dows Fire and Explosion Index Hazard Classification Guide, 7th Ed., American Institute
of Chemical Engineers, New York, NY, 1994.
12. Dows Chemical Exposure Index Guide,
American Institute of Chemical Engineers,
New York, NY, 1994.
13. Suardin, Jaffee, Mannan, M. Sam, and ElHalwagi, Mahmoud, The integration of Dows
Fire and Explosion Index (F&EI) into process
design and optimization to achieve inherently
safer design, Journal of Loss Prevention in the
Process Industries, Vol. 20, pp. 7990, 2007.
14. Khan, Faisal I., and Amyotte, Paul R., How
to make inherent safety practice a reality,
Canadian Journal of Chemical Engineering,
Vol. 81, No. 2, 216, February 2003.
Additional suggested reading

1. Edwards, David, Editorial Special Topic
Issue Inherent safety Are we too safe for
inherent safety?, Process Safety and Environmental Protection Transactions of the
Institution of Chemical Engineers Part B,
Vol. 81, No. B6, 399400, November 2003.
2. Englund, Stanley M., Inherently safer plants:
Practical applications, Process Safety Progress, Vol. 14, No. 1, 6370, January 1995.
3. French, Raymond W., Williams, Donald D., and
Wixom, Everett D., Inherent safety, health, and
environmental (SHE) reviews, Process Safety
Progress, Vol. 15, No. 1, 4851, Spring 1996.
Acknowledgments
I gratefully acknowledge the process safety insights from my colleagues at Aker Solutions and
at the leading operating companies whose facilities we have helped to design, from Professors
Sam Mannan, Trevor Kletz, Ron Darby, Harry
West and the Mary Kay OConnor Process Safety
Center at Texas A & M University, and from
many others in the community of process safety
professionals. The financial support of Aker Solutions is also appreciated.
Author
Victor H. Edwards, P.E.,
is director of process safety
for Aker Solutions Americas Inc., (3010 Briarpark
Drive, Houston, TX 77042;
Phone:
713-270-2817;
Fax: 713-270-3195; mail:
vic.edwards@akersolutions.
com). In his 28 years with
Aker, Edwards experience
includes process engineering,
safety management and process, biochemical and environmental technologies. He has received numerous accolades in the
areas of safety and environmental engineering,
including five DuPont awards, and has contributed extensively to the engineering literature.
His earlier experience includes assistant professor of chemical engineering at Cornell University, an assignment at the National Science
Foundation, pharmaceutical research at Merck,
alternate energy research at United Energy
Resources, visiting professor at Rice University
and process engineering at Fluor Corp. Edwards
earned his B.A.Ch.E from Rice University and
his Ph.D. in chemical engineering from the University of California at Berkeley. A registered
professional engineer in Texas, he is an AIChE
Fellow, and a member of ACS, AAAS, NFPA,
NSPE, and the N.Y. Academy of Sciences.
Note: This article is based on a paper presented
at the Mary Kay OConnor International Symposium, Texas A & M University, October 27-28,
2009.
4. Gupta, J.R., and Edwards, D.W., Inherently
safer design Present and future, Process
Safety and Environmental Protection Transactions of the Institution of Chemical Engineers
Part B, Vol. 80, 115125, May 2002.
5. Gupta, J.R., Hendershot, D.C., and Mannan,
M.S., The real cost of process safety A clear
case for inherent safety, Process Safety and
Environmental Protection Transactions of
the Institution of Chemical Engineers Part
B, Vol. 81, No. B6, 406413, November 2003.
6. Hendershot, Dennis C., et al., Implementing inherently safer design in an existing plant, Process
Safety Progress, Vol. 25, No. 1, 5257, March 2006.
7. Kletz, Trevor A., Inherently safer design: The
growth of an idea, Process Safety Progress,
Vol. 15, No. 1, 58, Spring 1996.
8. Lutz, William K., Take chemistry and physics into consideration in all phases of chemical plant design, Process Safety Progress, Vol.
14, No. 3, 153160, July 1995.
9. Lutz, William K., Advancing inherent safety
into methodology, Process Safety Progress,
Vol. 16, No. 2, 8688, Summer 1997.
10. Maxwell, Gary R. Edwards, Victor H., Robertson, Mark, and Shah, Kamal, Assuring process
safety in the transfer of hydrogen cyanide manufacturing technology, Journal of Hazardous
Materials, Vol. 142, pp. 677684, June 2007.
11. Overton, Tim and King, George M., Inherently safer technology: An evolutionary approach, Process Safety Progress, Vol. 25, No.
2, 116119, June 2006.
12. Study, Karen, A real-llife example of choosing an
inherently safer process option, Process Safety
Progress, Vol. 25, No. 4, 274279, December 2006.
Solids Processing
Preventing Self-Heating and

Ignition in Drying Operations
Incident investigation reveals that the
most common root cause is lack of understanding
Pieter Zeeuwen and Vahid Ebadat
Chilworth Global
any solid materials can

exhibit self-heating, which
if unchecked can
progress to a fire or even
explosion. And even if the situation
does not get that far, it is likely to affect the output of the process, in terms
of product quality degradation, for example. Recognizing that your product
in powder or granular form can selfheat is the first step in controlling the
risks associated with self-heating.
Whenever self-heating incidents are
investigated, we find that a common
root cause is a lack of understanding of self-heating phenomena. This
article provides an introduction to
self-heating phenomena and suggests
measures to control this type of ignition source.
What is self-heating?
Not all particulate solids that are classified as combustible dust (in other
words, pose a dust explosion hazard)
will self-heat at normal processing
temperatures, and conversely, some of
the materials that do self-heat react
too slowly to pose a dust explosion
hazard. Some materials can self-heat
at ambient temperatures, especially
in large-scale storage, but for most
materials the hazards arise when they
are heated.
Self-heating can arise by one of two
different mechanisms: by exothermic
(heat releasing) chemical reactions
and by exothermic decomposition.
The chemical reactions are often the
same as what occurs during a fire or
explosion: an oxidation reaction with
the oxygen in the air. At the start of
the self-heating process, the reaction
is very slow, like steel that oxidizes
Figure 2. Product in the test cell

(right) is discolored significantly after
the test compared to the original sample (left), even though the self-heating
has not led to smoldering or burning of
the material
Figure 1. After completion of a test,
in which self-heating of the product took
place, the product was completely burnt.
The charred and partly molten remains no
longer fit inside the sample holder
with atmospheric oxygen to form rust.

Decomposition happens in a material
that is unstable, and the material will
fall apart while releasing heat. A significant difference between the two
mechanisms is that decomposition
does not require additional reactants
and is therefore largely independent
of the environment, while an oxidation
reaction only happens if certain conditions are present, making it more difficult to predict its occurrence without
detailed experimental studies.
What happens in self-heating?
Step 1. Rate of heat generation exceeds rate of heat loss. If a material

undergoes an exothermic chemical
reaction (or multiple reactions) or decomposes exothermically, the temperature of the material will rise due to the
heat released from the exothermic reaction or decomposition. In the meantime, some of the heat is lost to the
environment. If the rate of heat loss
exceeds the rate of heat generation,
the temperature of the material will
be the same as the ambient temperature, otherwise, it will increase. Due
to the poor thermal conductivities of
many solids, a large portion of the re-
Figure 3. In this typical test cell for

bulk conditions (50-mm dia., 80-mm
height), air can diffuse into the sample
through the open top of the cell and
through the bottom of the cell, which is
closed with a sintered glass disc. The
sample temperature is measured continuously at various locations along the
height of the cell
action heat is retained in the powder.

Step 2. Resulting temperature
rise further increases chemical
reaction rate exponentially. The
temperature rise of the material due
to the exothermic reaction will further
increase the chemical reaction rate,
which in turn will cause the temperature to increase further. The increase
of material temperature also results
in an increase in the rate of heat loss.
However, the rate of heat loss increases
linearly with temperature, while the
chemical reaction rate, and thus the
Chemical Engineering www.che.com august 2011
45
Solids Processing
Figure 5. Basket test sample holders, for testing at different scales, allow extrapolation to large-scale storage conditions. The baskets typically have sides of 25, 50 and 100 mm
Figure 4. (Top left) In the test for aerated conditions, air

flows through the sample from top to bottom, which are both
closed by sintered glass discs. The cylindrical section has a 50
mm dia. and a height of 80 mm. (Bottom) For "air over layer"
testing, warm air flows over the powder layer in the sample
tray. (Top right) The wire basket for basket testing is illustrated
more clearly in Figure 5
heat generation rate, increases exponentially with temperature. Consequently, the heat generation rate will
exceed the rate of heat loss and the
temperature of the material will rise
higher. This process is referred to as
self-heating. Self-heating begins at a
temperature at which the rate of heat
generation is greater than the rate of
heat loss and this temperature is called
the exothermic onset temperature.
Subsequent effects
Potential smoldering. Self-heating

of solid materials usually results in
smoldering, which can set the material on fire or cause dust explosions,
particularly when the smoldering
material is disturbed and exposed to
air (Figure 1). Many plants that experience self-heating incidents have
a history of near misses where some
self-heating occurs but does not progress to full-blown ignition. In such
cases there may be black spots in an
otherwise light-colored product, or a
lump of charred product may be found,
a so-called smoldering nest. It is important to recognize such occurrences
as indications of a potentially serious
problem, rather than to learn to live
with it.
Potential release of flammable
46
Figure 6. This basket test sample holder is prepared for

testing inside a laboratory oven
gases. Self-heating reactions may

also produce flammable gases, which
may lead to gas explosions in process
vessels or compromise product quality
(Figure 2).
Testing self-heating behavior
The exothermic onset temperature

is influenced not only by the chemical and physical properties, such as
chemical reaction kinetics and heat
of reaction, but also by other factors,
including the following:
Dimension and geometry of the solid
bulk
Ambient airflow
Availability of oxygen in the bulk
Additives and contaminants
Usually, the material has to be exposed
to an elevated temperature for a period
of time before it self-heats. This time is
referred to as the induction time, which
is dependent on temperature; and usually the higher the temperature, the
shorter the induction time will be.
Because of the influencing factors
mentioned, a single test is usually unable to predict self-heating behavior
for all different drying and storage
conditions. Instead, separate tests
have been developed to simulate the
conditions where the powder is in bulk
form (Figure 3), layer form (with air
flowing over the powder; Figure 4)

and aerated form (Figure 4), where
air is passing through the bulk of the
product, increasing the oxygen availability for the reaction and also helping to remove heat from the reacting
material. For large-scale storage situations tests are carried out at different scales so that the effect of the size
of the bulk material can be assessed
(Figure 5). All tests are carried out in
temperature-controlled ovens (Figure
6) that allow screening tests (with the
temperature ramped up at a defined
rate) and isothermal testing (with
a constant temperature controlled
within narrow margins). Because of
the potential for violent reactions during the self-heating process, all testing
equipment needs to be fitted with explosion protection.
Learning from a real incident
In one incident, the powder in a fluidized bed dryer caught fire when the
powder conveyer in the dryer was
turned off in order to fix clogging in
an upstream wet-product conveyer.
During this period, the hot air supply
was continued.
A screening test was conducted to
determine whether this powder could
self-heat under the conditions that ex-
450
Temperature, C
400
Oven
75% height
50% height
25% height
12.5% height
350
300
250
200
150
100
50
0
100
200
300
400
Time, min
500
600
700
Figure 7. In this screening test, the oven temperature was

increased from 20 to 400C at a rate of 0.5C/min. The exothermic
onset temperature was identified to be 166C, which was lower
than the hot air temperature of the dryer, indicating that selfheating was the most probable ignition source for this incident
isted in the dryer before the incident.

An typical powder sample was placed
in a temperature-programmed oven
and the temperature of the oven was
increased from 20 to 400C at a rate
of 0.5C/min (Figure 7). The exothermic onset temperature was identified
to be 166C, which was lower than the
hot air temperature of the dryer. The
result indicated that self-heating was
the most probable ignition source for
this incident.
This test provides a useful tool for a
quick identification of the self-ignition
hazard of materials and should be conducted for materials whose thermal
stability characteristics are not known.
However, to be of any practical value,
the test results obtained in a laboratory-scale apparatus have to be scaled
up to plant-size process. In order to
establish the relationship between
the exothermic onset temperature and
powder layer thickness with the aid of
thermal explosion theory, the sample of
the powder that was being dried in the
same incident batch was tested at three
different layer thicknesses. In each
trial, the powder sample was exposed
to a constant temperature to test if
self-heating would actually take place.
The highest temperature at which selfheating did not occur and the lowest
temperature at which self-heating did
occur were determined. The average
value of these two temperatures was
taken as the exothermic onset temperature for each powder layer.
The exothermic onset temperatures were used to determine the
unknown constants of the following
equation, which expresses the relationship between the exothermic
onset temperature and the thickness
of the powder layer:
Dependence of self-heating onset

on the thickness of powder layer
Onset temperature of self-heating, C
Self-heating test with a constant rate

of temperature rise, 0.5C/min
180
170
160
150
140
130
120
10
12
Thickness of powder layer, in
Figure 8. Using Equation (1), the exothermic onset temperatures of layers of the powder at different thicknesses were
calculated and the results plotted here. As the thickness of the
powder layer was increased from 1 to 12 in., the exothermic
onset temperature decreased by 48C
(1)

Where
Ta = Exothermic onset temperature for a powder layer, K
r
= One half of the powder layer
thickness, m
c = Frank-Kamenetskii-parameter, dimensionless
M, N = Constants determined by properties of the powder material
Using Equation (1), the exothermic
onset temperatures of layers of the
powder at different thicknesses were
calculated and the results are plotted (Figure 8). As the thickness of the
powder layer was increased from 1 to
12 in., the exothermic onset temperature decreased by 48C.
The powder layer in the dryer before
the incident was on the order of 48
in. This suggests that the exothermic
onset temperature for the powder layer
was well below the hot air temperature.
Ignition would occur if the heating time
exceeded the induction time.
Concluding remarks
The self-heating hazard of solid materials to be dried should be determined.

Depending on the drying process, the
solid materials can be tested in different shape, heating environment, with
or without an airflow through the material and an airflow at the surface of
the material. The exothermic onset
temperatures can be used to determine safe drying temperatures using
sufficient safety margins. However, the
relationship between the exothermic
onset temperature and the dimension
of solid bulk is often needed in order to
design a safe drying process. This rela-
tionship can be established from selfheating experiments based on thermal

explosion theories, as demonstrated by
the example introduced above.
Edited by Rebekkah Marshall
Suggested reading
J.A. Abbott (technical ed.), Prevention of Fire &

Explosions in Dryers, 2nd ed., The Institution of
Chemical Engineers, Rugby U.K. 1990.
Authors
Vahid Ebadat is the CEO
of Chilworth North America
(Chilworth Global, Princeton, NJ; Phone: 609-7994449; Email: safety-usa@
chilworthglobal.com; Website:
www.chilworth.com). He holds
a B.S. in electrical engineering
and a Ph.D. from Southampton University. He has worked
extensively as a process and
operational hazards consultant for the chemical, pharmaceutical and food
industries. Ebadat is a regular speaker at training courses on gas and vapor flammability, dust
explosions, and controlling electrostatic hazards.
He is a member of NFPA 77 Technical Committee on Static Electricity; NFPA 654 Standard for
the Prevention of Fire and Dust Explosions from
the Manufacturing, Processing, and Handling of
Combustible Particular Solids; and ASTM E27
Committee on Hazard Potential of Chemicals.
Ebadats research has culminated in the publication of numerous technical articles and papers.
Pieter Zeeuwen, is a senior
process safety specialist at
Chilworth Global. He holds
a M.Sc. in applied physics
from Eindhoven University
of Technology and has more
than 30 years experience
in the gas and dust explosion fields, including materials testing, small and large
scale explosion research, and
consultancy for industry and
government agencies in a number of countries.
His areas of expertise include gas and dust explosion hazard assessment, gas and dust explosion
prevention and protection, electrostatic hazard
assessment, hazardous area classification, and
gas cloud explosions as well as incident investigations. Over the years, Zeeuwen has served on
many working groups including various standards
committees, both nationally and internationally, for instance, most recently CEN (European
Standards Committee) working groups on explosion protection methods and on test methods. He
regularly lectures on various aspects of explosion
safety and acts as seminar chairman and course
director. Zeeuwen has published numerous articles in scientific journals and presented many
papers at international conferences.
47
Gas Hazard
Definitions and Data
Department Editor: Scott Jenkins
he detection of gases in plant environments

has a critical and wide-ranging role in the
chemical process industries (CPI). Among
the major applications of gas detection are
limiting personnel exposure to hazardous
chemicals, preventing explosive atmospheres,
protecting the environment and identifying
leaks in process equipment. Table 1 summarizes the main reasons for gas monitoring.
All CPI workers should be conversant with
gas-detection terms to promote safety, health
and environmental quality. The following is a
collection of terms and data involving hazardous gases (Table 2).
PEL (permissible exposure limit). Set by OSHA
to limit workers exposure to an airborne
substance, PELs are based on an eight-hour
time-weighted average. PELs are enforceable
legal limits.
TLV (threshold limit value). Established by
the American Conference of Governmental
Industrial Hygienists, TLVs are based on known
toxicity of chemicals in humans or animals, and
are recommendations, rather than legal limits.
IDLH (immediately dangerous to life and
health). Defined in the U.S. by the National
Institute for Industrial Safety and Health (Part of
the Centers for Disease Control and Prevention) as a level of exposure that is likely to
cause death or immediate or delayed permanent adverse health effects
LC50 (median lethal concentration). A measure
of the toxicity of a surrounding medium that
will kill half of a sample population of test
animals in a specified period through exposure
via inhalation.
Oxygen deficiency
Normal ambient air contains 20.8 vol.% oxygen. When oxygen concentration dips below
19.5 vol.% of the total atmosphere, the area
is considered oxygen deficient. Oxygen deficiency may result from O2 being displaced by
other gases, such as carbon dioxide, and can
also be caused by rust, corrosion, fermentation
or other forms of oxidation that consume oxygen. Table 3 outlines the physiological effects
of oxygen deficiency by concentration.
If oxygen concentrations in the air rise
above 20.8%, the atmosphere is said to be
oxygen-enriched. Higher oxygen levels can
increase the likelihood and severity of a flash
fire or explosion, because the oxygen-enriched
atmosphere tends to be less stable than air.
Combustible atmospheres
Vapor and gas. Although these two terms

are sometimes used interchangeably, they
are not identical. Vapor refers to a substance
that, though present in the gaseous phase,
generally exists as a liquid or solid at ambient
temperatures. Gas refers to a substance that
generally exists as a gas at room temperature.
Vapor pressure and boiling point. Vapor pressure can be defined as the pressure exerted
by a vapor in thermodynamic equilibrium with
its condensed or solid form. Vapor pressure is
directly related to temperature, and along with
boiling point, determines how much of a chemical is likely to become airborne. Substances
with low vapor pressures generally present less
of a hazard because there are fewer molecules
of the substance to ignite, but they may require
higher-sensitivity instrumentation to detect.
Vapor density. Vapor density is the weight ratio
of a volume of vapor compared to an equal volume of air. Most flammable vapors are heavier
than air, so they may settle in low areas.
Explosive limits. To produce a flame, a sufficient amount of gas or vapor must exist. But
too much gas can displace the oxygen in an
table 1. summary OF The Main reasons for gas monitoring.

Type of monitoring
Purpose
Hazard
Possible source of hazard
Personal protection Worker safety
Toxic gases
Leaks, fugitive emissions,
industrial process defects
Explosive
Worker safety
Explosions
Presence of combustible
gases and vapors due to
and facility
safety
leaks or process defects
Environmental
Environmental
Environmental degAcid gas emissions
safety
radation
Industrial process
Process control Process malfunction Process errors
Source: MSA
table 2. exposure data for selected hazardous gases

Chemical and formula
Properties
OSHA PEL IDLH
LC50 (ppm)
(ppm)
(ppm)
Ammonia (NH3)
Corrosive, flammable
50
300
4,000
Boron trifluoride (BF3)
Toxic
1
25
806
Bromine (Br2)
Highly toxic, corrosive,
0.1
3
113
oxidizer
Carbon monoxide (CO) flammable
50
1,200
3,760
Carbon dioxide (CO2)
5,000
40,000 Not available
Chlorine (Cl2)
Toxic, corrosive, oxidizer
1
10
293
Chlorine dioxide (ClO2) Toxic, oxidizer
0.1
5
250
Ethylene oxide (C2H4O)
Flammable
1
800
4,350
Hydrogen chloride (HCl) corrosive
5
50
2,810
Hydrogen sulfide (H2S)
Toxic, flammable
20
100
712
Methyl isocyanate
Highly toxic, flammable
0.02
3
22
(CH3NCO)
Nitrogen dioxide (NO2)
Highly toxic, oxidizer
5
20
115
Phosphine (PH3)
Highly toxic, pyrophoric
0.3
50
20
Sulfur dioxide (SO2)
Corrosive
5
100
2,520
table 3. physiological effects of oxygen deficiency by degree
Concentration of O2
in atmosphere, vol. %
Physiological effect
19.5 to 16
No visible effect
16 to 12
Increased breathing rate; accelerated heartbeat; Impaired

attention, thinking and coordination
14 to 10
Faulty judgment and poor muscular coordination; Muscular

exertion, causing rapid fatigue; Intermittent respiration
10 to 6
Nausea and vomiting; Inability to perform vigorous movement or

loss of the ability to move; Unconsciousness, followed by death
Below 6
Difficulty breathing; convulsive movements; death in minutes
Source: MSA
table 4. Explosion concentration Ranges for selected gases

Gas type
LEL
UEL
Methane
5.0 vol. %
15 vol. %
Hydrogen
4.0 vol. %
75 vol. %
Propane
2.1 vol. %
9.5 vol. %
Acetylene
2.5 vol. %
100 vol. %
Source: MSA
area, making it unable to support combustion.

Therefore, there is a window of concentrations
for flammable gas concentrations where combustion can occur. The lower explosive limit
(LEL) indicates the lowest quantity of gas required for combustion, while the upper explosive limit (UEL) indicates the maximum quantity
of gas (Table 4). Gas LELs and UELs can be
found in NFPA 325. LELs are typically 1.4 to
5 vol.%. As temperature increases, less energy
is required to ignite a fire and the percent gas
by volume required to reach the LEL decreases,
increasing the hazard. An environment with
enriched oxygen levels raises the UEL of a gas,
and the rate of flame propagation. Mixtures of
multiple gases add complexity, so their exact
LEL must be determined by testing.
References
1. U.S. Dept. of Labor, Occupational Safety
& Health Administration (OSHA), 29 CFR
1910.1000 Table Z-1.
2. U.S. Centers for Disease Control and Prevention. National Institute for Occupational Safety
and Health (NIOSH). NIOSH Pocket Guide to
Chemical Hazards. www.cdc.gov/niosh/npg.
Accessed March 2013.
3. Mine Safety Appliances Co., Gas Detection
Handbook 5th ed. MSA Instrument Div.,
August 2007.
4. National Fire Protection Association. NFPA 325:
Guide to Fire Hazard Properties of Flammable
Liquids, Gases and Volatile Solids, 1994.
Static Electricity
Discharge and Fire
Prevention
Department Editor: Scott Jenkins
hen flammable or combustible atmospheres are present,

uncontrolled discharges of static
electricity are potentially dangerous or
even catastrophic. A significant portion
of industrial explosions and fires are
attributable to static electricity each year.
In theory, controlling static electricity by
grounding potential sources is simple, but
in practice, doing so effectively requires
thorough knowledge of processes and
operations, sound engineering controls,
properly specified safety equipment and
properly trained operational staff. This
column provides information on potential
sources of static electrical discharge.
Static risk
Static electricity discharges are possible almost continuously in the chemical process industries (CPI), because
static electricity is generated whenever
surfaces come into contact and then
separate. In most cases, the charging
currents generated over time in industrial processes are small typically no
greater than 1 104 Amps. However,
in hazardous areas, even small charges
can be a problem when the allowed to
accumulate on objects that are not at
ground (earth) potential. If no ground is
present, voltages in excess of 30 kV can
develop. Depending on the capacitance
of the object, this may result in significant levels of energy being available
for discharge. If the energy equals or
exceeds the minimum ignition energy
(MIE) of the surrounding flammable atmosphere, the potential for an explosion
and fire exist. Many commonly used
solvents and other flammable chemicals
have MIEs that are relatively low on
the order of 1 mJ or less (Table 1).
Isolated conductors
Isolated conductors are electrically

conductive objects that are either inherently or accidentally insulated from earth.
During day-to-day operations at industrial facilities, isolated conductors are
probably the most likely source of static
ignition incidents.
The insulation effectively keeps any
static electricity buildup from safely
discharging, thereby resulting in accumulation of charge on the object. If
the isolated conductor then comes into
proximity with another object at a lower
potential, energy could be released in
the form of an incendive spark.
Isolated conductors may arise from
metal flanges, fittings or valves in pipework systems; portable drums, containers
or vessels; tanker trucks, railcars and
intermediate bulk containers (IBCs); and
even people.
Many modern industrial paints,
coatings, gaskets, seals and other
non-conductive materials are sufficiently

insulating, so as to to possibly prevent
the proper dissipation of static charge.
Static discharge sources
Static discharges come in several forms,

the most important for CPI interests being
spark and brush discharges. A spark
is a discharge from a charged isolated
conductor to another conductor at lower
potential. A brush discharge occurs from
an electrostatically charged insulator to a
grounded conductor.
Typical possible sources of static electrical discharges include the following:
Spark discharges from any conductive,
but not earthed (grounded), bag, bin,
drum, container and so on, from which
a powder is transferred into a reactor
Brush discharges from any non-conductive bag, bin, drum, container, and so
on, from which a powder is transferred
into a reactor
but not earthed, auxiliary device used
in the transfer procedure, including, but
not limited to, shovels, funnels, chutes
and pipes
Spark discharges from the operator, if
he or she is not adequately earthed
Brush discharges from any non-conductive auxiliary devices, such as shovels,
funnels, chutes and pipes
Brush discharge from the dust cloud
formed within a reactor during powder
transfer
but not earthed, fixtures and fittings
within a reactor
Brush discharges from the charged solvent, suspension or emulsion preloaded
in a reactor
Brush discharges from the powder
heap formed on top of the liquid phase
within a reactor
Cone discharges from the powder heap
formed on top of the liquid phase
Liquids flowing through pipelines or
filling into drums and tanks
Persons walking across an insulating
floor
Static discharge prevention
Where recommendations tend to

converge is in the recommendation to always use conductive or static dissipative
materials, and to ensure effective bonding and grounding. For information on
grounding best practices and examples
of preventing static electrical discharge,
consult National Fire Protection Association (NFPA; Quincy, Mass.; www.nfpa.
org) standards 77 and 30.
In this context, the term conductive
would apply to metal materials, such
as stainless or carbon steel, aluminum
and others; and static-dissipative may
indicate rubber or plastics that have
Table 1. Typical MIE values

Material
(gas/vapor or
powder/dust)
Minimum
Ignition Energy
(MIE), mJ
Carbon disulfide
Methanol
Xylene
Toluene
Propane
0.009
0.14
0.20
0.24
0.25
Ethyl acetate
Zirconium
Epoxy resin
Aluminum
Sugar
Wheat flour
0.46
5.00
9.00
10.00
30.00
50.00
Note 1: Minimum ignition energy (MIE) is defined

as the minimum energy that can ignite a mixture
of a specified flammable material with air or oxygen, measured by a standard procedure.
Note 2: MIE values are provided for guidance
only specific MIE data for any material
should be verified.
Source: NFPA, IChemE
been formulated with some added semiconductive additives. Bonding means

linking these objects together by means
of a suitably strong conductor (wire), and
grounding refers to a true ground/
earth connection that is applied to one
or more of the bonded objects.
When one or both of these techniques
is applied, and while a low resistance
connection between the objects and
ground is maintained, operators are
able to prevent dangerous levels of static
charge from accumulating. In the case
of fixed installations such as pipe work,
storage tanks and so forth, grounding is
relatively simple to implement.
However, these preventive measures
are more difficult to implement with
portable objects, such as drums, IBCs
and tankers. In these instances, purposedesigned temporary grounding and
bonding devices must be used, with
strict procedures to ensure that they are
always in place prior to starting the
process. For instance, specific types of
clamps and devices for grounding and
bonding portable or mobile plant equipment, drums and containers are recommended in NFPA 77, and such grounding clamps and devices generally should
employ sharp contact points. These
contact points should be made of a wearresistant material, have positive spring
pressure, and be universally adaptable to
a wide range of plant objects.
References
1. Tyers, G., Avoiding Static Sparks in Hazardous Atmospheres, Chem. Eng., June 2009, pp. 4449.
2. Glor, M., Preventing Explosions During the Transfer of Solids into Flammable Solvents, Chem.
Eng., October 2007, pp. 8895.
Editors note. This edition of Facts at your Fingertips was adapted from information in the two articles referenced above.
Feature
Cover
Story
Report
Part 1
Designing for
A Safe Process
Phil Leckner
CH2M Hill Lockwood Greene
ccidents do happen. While not

everything can be predicted,
addressing safety concerns
throughout the design of a process can help to prevent accidents
from occurring. Designing with safety
in mind can also help to minimize potentially serious consequences that
would result if an accident did occur.
On April 12, 2004, toxic allyl alcohol
and allyl chloride were released from
a reactor at a facility in Dalton, Ga.
The consequences included injuries
and chemical contamination to people
and property in the surrounding area.
According to their report [1], the U.S.
Chemical Safety and Hazard Investigation Board (CSB) concluded that
better process design, engineering,
and hazard analysis would likely have
prevented the 2004 runaway chemical reaction and toxic vapor cloud release...
On March 23, 2005, an explosion at
a refinery in Texas City, Tex. killed 15
workers and injured 180 others when
flammable liquid and vapor overfilled
a blowdown drum during the startup
of the refinerys isomerization unit [1].
All of the fatalities and many of the
injuries occurred in and around trailers that had been positioned near the
isomerization unit to support maintenance activities on adjacent refinery
units. The CSB report on this incident
[1] recommended that new guidelines
be developed for the placement of
these and similar temporary structures around hazardous areas.
Having a procedure in place to promote safe process design can help
ensure that safety concerns are considered at appropriate phases in the
design. The methodology presented
here, as outlined in Table 1, may help
prevent accidents such as those in
30
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Dalton, Ga. and Texas City, Tex. This

methodology applies to process designs throughout the chemical process
industries (CPI), which include not
just chemical production, but also, for
example, wastewater-treatment facilities, pharmaceutical and food-andbeverage plants. While following these
guidelines will cost time and money,
the practice can be a very inexpensive
way to help prevent the much more
costly consequences of not providing
the safest design possible.
Basic Engineering
Process flow diagrams
As a process engineer, there are two

types of flow diagrams that interest
me: the block flow diagram (BFD) and
the process flow diagram (PFD).
The BFD (Figure 1) presents an
overall picture of the process, showing only major process steps. These
steps are shown as black boxes with
simple descriptions. Equipment can
be depicted singly or grouped together
as a system.
The PFD (Figure 2), meanwhile,
depicts major and minor equipment
with specific symbols that are typi-
cally used in the CPI. Equipment is

usually identified and shown with an
alphanumeric designation. The PFD
includes major and some minor process streams as well as utility streams,
such as steam, condensate and cooling
media. This diagram can also be used
to show process safety requirements,
such as proposed locations for relief
valves. Often, a heat-and-material
balance and major control loops are
included.
The PFD should be used as the basis
for generating the more detailed piping-and-instrument diagram (P&ID).
Prior to P&ID preparation, the PFD is
reviewed by the design team and issued for design (IFD), with a revision
number of zero.
At a minimum, the basic design
package should include the BFD and
the PFD. However, I believe that another document, which takes the PFD
to a new level, better promotes a safe
process design. This document, which
I call the process definition drawing
(PDD), is not ordinarily a part of the
basic design package, but is a great
tool for the process design engineer.
The PDD includes operating-and-
Chemical Engineering www.che.com December 2006
30-33 Ce 12-06.indd 30
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1
design conditions for each equipment

item, each control-valve station and
all relief devices. The benefit of this
document is that the process engineer
can quickly recognize inconsistent or
conflicting operating-and-design conditions. It helps the engineer think
about the process in terms of how
it will operate and what needs to be
done to make it safe.
Detailed engineering work is also
aided by the PDD, since much of the
information included on this document will be used in the generation of
process-equipment, instrumentation
and safety-device duty specifications.
The PDD is a living document and
will change as the process design progresses. As such, it is often sketched
using rudimentary drawing software
rather than CAD, thereby making it
simple to construct and maintain.
Preliminary safety review
After the PFDs are created and approved for design, a preliminary safety
review (PSR) is undertaken.
The PSR is the gathering of documentation with an emphasis on process safety. Included are items such as
the project scope definition, the process design basis, the process description and a material safety data sheet
(MSDS) for each substance used. An
extensive list of documentation that
may be included in the PSR can be
found in Ref. [2].
The MSDS is an important docu-
ment that provides a wealth of information including the proper handling of a substance, special storage
requirements (such as keep out of the
sun) and required personal-protection
equipment (PPE), such as breathing
apparatuses.
The MSDS also provides basic physical-property and toxicity data, exposure limits and flammability ranges.
It may describe what to do in case of
spills. The manufacturer or supplier
of the raw materials and various websites on the Internet are sources for
MSDSs. If the facility is producing a
finished product, then the plant owner
will have to develop an MSDS for
that product and make the document
available to potential users. Table 2
lists information typically found in an
MSDS.
Once the documentation is gathered, the PSR is assembled into a
formal report and issued to all pertinent members of the design team for
comment. The report is given to project management for distribution as a
revision 0 issue. Note that the PSR
is a living document and is subject to
change as the design progresses. The
PSR document is issued as soon as
feasibly possible because it will form
the foundation for the balance of the
safety review of the project.
Design safety review
Once the PSR is issued, the process

can be reviewed for major safety con-
Figure 2. Process flow diagrams give more detail than

BFDs, and include at least
major process streams and
equipment items. Symbols that
are typical for the CPI are used
cerns in the design safety review.

Using the most up-to-date version
of the PSR, all features associated
with safety, environmental and layout
issues are reviewed, including the following:
Defining the hazardous location
classification (HLC), or the electrical area classification as it is sometimes called The HLC is used to
determine electrical-design criteria,
such as equipment that may require
explosion-proof motors. The HLC
boundaries should be shown on appropriate documents such as the
PFD or equipment-layout drawings
(if available). One source of definitions for HLCs can be obtained from
Ref. [3].
Locating major pressure-relief devices, such as relief valves and rupture disks, explosion panels and
flame arrestors These devices
should be indicated on the PFD
and, in more detail on the PDD. The
destination of the vent from these
particular safety devices needs to
be considered. The applicability and
use of alternate safety systems, such
as safety-instrumented systems
(SIS) is also evaluated at this time.
(For more, see Part 2 of this report,
p.34)
Evaluating the layout with respect
to minimizing hazards As noted
earlier in the Texas City, Tex. accident, personnel placement is a
very important consideration. For
30-33 Ce 12-06.indd 31
31
11/22/06 4:36:16 Pm
Cover Story
equipment placement, the American
Petroleum Institute (API; www.api.
org) recommends that all equipment
with a ground area of 2,500 to 5,000
ft2 should be considered part of the
same fire-relief scenario [4]. Determine if larger-sized equipment can
be moved outside the common fire
zone to reduce overall relieving capacity. Also be cognizant of where
chemicals are stored in proximity to
each other. You may not want acids
stored near bases, for example.
Locating flares in safe areas, taking
into account their radiation effects
at ground level.
Evaluating the need for and placement of, fire and gas detectors (for
more, see p.18).
With the major pressure-relief devices located and the operating and
design conditions fully defined, it is
appropriate to evaluate modifications
that might make the system safer.
For example, determine if there are
safety advantages to changing storage requirements from concentrated
solutions to more dilute solutions, or
vise-versa. Evaluate the advantages
and disadvantages of breaking unit
operations into smaller, more discrete
pieces to make process equipment,
such as heat exchangers and reactors,
smaller.
Preliminary hazard analysis. Finally, some type of preliminary hazard
analysis (PrHA) should be undertaken
before moving into the detailed process engineering phase of the project.
During a PrHA, team members visualize ways in which a process design
can malfunction or be operated incorrectly. The PrHA can take one of many
forms, such as a pre-HAZOP, a what
if, failure mode-and-effects analysis
(FMEA) or FMEA check list. The various types of hazard analyses that are
acceptable to the U.S. Occupational
Safety and Health Administration
(OSHA) are outlined in Refs. [2] and
[5]. The PrHA is performed on the detailed PFD that is issued for design.
The documents collected during the
PSR and the PDD provide reference
materials. Note that a preliminary or
IFD issue of the P&ID may have been
developed by this time and if so, would
be part of the PrHA.
At the conclusion of the design safety
32
review, all documents and results are

collated and issued. This compilation
is included as part of the front-end design package and the design proceeds
to the next phase of the project, the
detailed process engineering.
Detailed Engineering
Piping and instrument diagram
At the start of the detailed processengineering phase of design, all outstanding issues and especially those
brought up during the design safety
review are examined and addressed.
The P&IDs, PFDs and the PDDs are
updated as required. The P&IDs are
then reviewed in a formal setting as
a team, which should include the process, mechanical, and piping and instrumentation engineers.
The review will expose any last minute safety and design issues that must
be addressed before the more detailed,
and required, process hazard analysis
(PHA) is undertaken. Changes are
documented by again updating the
P&IDs and PFDs. I suggest that these
documents be issued with a separate
revision number established exclusively for the PHA.
The process hazard analysis
The PHA evaluates the design in

terms of both safety and operability.
The analysis should be performed on
the process, as well as instrumentation and control systems, such as the
digital control system (DCS).
PHAs are mandatory for all plants
that fall within the scope of OSHA 29
CFR 1910.119 [5]. This scope applies
to plants that meet the following two
criteria:
1. Those whose processes involve one
or more of certain chemicals (listed
in appendix A of the regulation), and
in quantities at or above the threshold given
2. Those whose processes involve flammable liquid or gas onsite in one location in a quantity of 10,000 lb or
more with the exception of:
a. Hydrocarbon fuels used solely for
workplace consumption as a fuel
b. Flammable liquids stored in atmospheric tanks and kept below
their normal boiling point without the aid of chillers or refrigeration
Table 1.
A methodology to promote
a safe process design
I. Basic process engineering
Create the process flow diagram
Perform a formal review of the process flow diagram
Conduct a preliminary safety review
Perform a design safety review
II. Detailed process engineering

Create the piping and instrumentation diagram
Conduct a formal P&ID review
Perform the process hazard analysis on the process
Perform the process hazard analysis on the control system
III. Implement a management of

change procedure
Facilities that do not fall within 29 CFR

1910.119 would still benefit greatly
from the PHA if not for the safety aspects of the process, then for process
operability. I cant stress this enough:
not being required to do a PHA by law
should not exclude you from doing one
to ensure that your process is indeed
safe in design and operation.
The team make-up. The PHA team
should include a facilitator and a scribe
(who serves the function of recording secretary), the design firms area
process engineer, the plant process
engineer and representatives from
the plants safety-and-environmental
and operations-and-maintenance departments. If vendor packages are involved, a vendor representative is also
advised as a team member. An extensive list of possible participants can be
found in Ref. [2]. The PHA team makeup and the extent of their efforts will
vary based on the nature and complexity of the process design.
The facilitator should be chosen
with the following criteria in mind:
The person should be knowledgeable
in the type of PHA to be performed
The person should not be intimately
involved in the process design (thats
what the process engineers are for)
The person does not necessarily need
to be very knowledgeable about the
particular process to be reviewed
The facilitators function is to guide
30-33 Ce 12-06.indd 32
11/22/06 4:37:10 Pm
Table 2. INFORMATION typically found in an msds

Item
Remarks
Chemical name and any

common names
The common name will be the same name on

the label
Date of preparation or revision The date the MSDS was prepared or revised
List of contacts that can provide more information
Physical characteristics
Includes smell, color, appearance, flash point

and vapor pressure
Physical hazards
For example, if the substance is subject to violent reactions such as explosions or fires
Health hazards
Describes if and how a substance can cause

harm to human health and also provides
symptoms of exposure
Route of entry information
Describes how the substance can enter the

body, for example by ingestion or inhalation
Exposure limits
The maximum amount of exposure a person

should have to the substance
Carcinogenic status
Whether the substance causes cancer
Safe handling and use
Explains precautions and protective measures

needed when using and handling, including
spill control
Control measures
Suggested engineering controls, work practices

and personal protective equipment
Emergency and first aid procedures
How to deal with releases and exposure
the team, keep the PHA on track and

motivate participation. The facilitator
is not the person who brings up all of
the issues. A facilitator who is too involved with the process is analogous
to someone proofreading his or her
own material things are going to be
missed that would otherwise not.
Preparation. Having the right documentation available is key to a smooth
PHA. The team should at a minimum
have all the documents from the PSR
and the DSR, as well as the P&IDs
and PFDs, plot plans, equipment layouts, hazardous classification drawings, operating-and-maintenance procedures, batch sheets (if applicable), a
summary of relief-device calculations
and specifications for equipment, instrumentation and piping.
A PHA can be very time consuming and expensive to implement. Poor
documentation and the failure to perform a comprehensive P&ID review
prior to the PHA can contribute significantly to the cost. More time spent
on the earlier steps mentioned in this

methodology can reduce the cost and
duration of the PHA.
Documenting the PHA. One common problem is that many PHAs almost become P&ID reviews and fix it
sessions. Any problems identified with
the P&ID that need fixing should be
recorded for further action and not
discussed in detail during this analysis. Note that once the P&ID fix is
implemented, the change needs to be
re-evaluated.
After the PHA is completed, a report is issued documenting what was
checked and any actions that need to
be addressed, such as additional relief
devices, changing instrumentation
and adding information to what will
eventually become standard operating
procedures. These action items are to
be addressed in a timely manner and
the plant design should be revised as
required. Once all issues are addressed
and design changes implemented, the
design becomes fixed in terms of
References
1. The U.S. Chemical Safety and Hazard Investigation Board website (www.csb.gov)
2. The Center for Chemical Process Safety,
Guidelines for Hazard Evaluation Procedures with Worked Examples, 2nd ed.,
AIChE, 1992.
3. National Fire Protection Association, NFPA
70, National Electric Code, Chapter 5,
2005.
4. American Petroleum Institute, Recommended
Practice 521, Guide for Pressure-Relieving

and Depressuring Systems, 4th ed., March,
1997.
5. The Occupational Safety and Health Administration, Process Safety Management
of Highly Hazardous Chemicals, in 29 CFR
1910.119, OSHA, Washington, D.C., 1992.
6. The Center for Chemical Process Safety,
Plant Guidelines for Technical Management of Chemical Process Safety (Revised
Edition), AIChE, 1992, 1995.
safety. The design documents should

be issued as process safety management approved.
More specifics on PHAs can be found
in Refs. [2] and [5] and in an abundant
number of books and government publications (OSHA), that the reader is
encouraged to research and review.
Management of change
As in all designs, things change even

after the PHA is completed. These
changes must be captured as they
can affect the safety of the design and
create new problems. Management
of change (MOC) procedures capture
these changes and should be strictly
followed.
A MOC procedure is simply a written way of documenting and informing people about changes made to the
design after the PHA. The MOC may
even outline when a change necessitates a new PHA. For example, if a
valve is added to a line that was not
there when the original PHA was performed, a PHA must be performed on
this area of the design to ensure that
no additional safety hazards were
introduced, or if they were, are addressed accordingly.
There is no single way to design
and implement a MOC procedure. It
is up to the discretion of the project
team as to how it should be done. The
MOC complexity will depend on the
complexity of the process. The key is
to ensure that the MOC procedure is
easy to follow and that it allows easy
documentation of all required activities and includes a system for approvals by the appropriate project team
members [6].
n

Author
Phil Leckner is a senior
process engineer with CH2MHILL
Lockwood
Greene
(Phone: 732-868-2277; Email:
Philip.leckner@ch2m.com).
Phil has over 30 years experience in process design and
project engineering, and commissioning and startup for the
chemical, petrochemical, foodand-beverage and bio-pharmaceutical industries. Over the
past 10 years, he has been deeply involved with
process-safety issues with emphasis on reliefsystem design. He has been involved in a number
of PHAs, including serving as HAZOP and What
if? facilitator. Phil received his B.S.Ch.E. from
Lowell Technological Institute, which is now part
of the University of Massachusetts.
30-33 Ce 12-06.indd 33
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Cover Story
Figure 1. When
engineering controls
are not enough to
reduce or eliminate
airborne hazards,
respirators are
needed for protection
Clearing the
Air About
Respiratory
Protection
Learn the basics about selection
and regulatory compliance for these
potentially life-saving devices
Dennis Capizzi
MSA Safety
irborne respiratory hazards are a

very real threat in the chemical
process industries (CPI). Existing in a variety of forms including gases, vapors, dusts, mists, fumes,
smoke, sprays and fog, such hazards can
cause illnesses including cancer and
lung impairment, or even death. Examples of respiratory hazards include
combustion byproducts; toxic fumes or
dust created by metal melting; ozone
and nitrogen oxides from processes
involving an electric discharge in air;
and dust particles released by grinding
(notably dry grinding such as blasting) and crushing applications, and the
transport, sieving, mixing or screening
of any dry material.
The specific hazardous gases present in a workplace will, of course,
vary according to the processes of the
facility, but commonly include chlorine, chlorine dioxide, ammonia, nitrogen dioxide, nitric oxide and volatile organic compounds (VOCs). Some
hazardous gases, such as carbon
monoxide, act rapidly and can cause
unconsciousness or death within minutes, while other toxic gases can take
28
years to produce noticeable harm.

Where toxic substances are present in the workplace and engineering
controls (such as enclosing or confining the contaminant-producing operation, exhausting the contaminant, or
substituting with less toxic materials)
are inadequate to reduce or eliminate
them, it is time to turn to respirators
(Figure 1).
What is a respirator?
A respirator is a protective device that

covers the nose and mouth or the entire face or head to guard the wearer
against hazardous atmospheres. Respirators may be either tight-fitting or
loose-fitting. There are two types of
tight-fitting respirators: half masks
cover the wearers mouth and nose,
while full facepieces cover from the
hairline to below the chin (Figure
2). Loose-fitting respirators include
hoods and helmets that cover the
head completely.
The OSHA standard
The appropriate use of respiratory protection is not only important for worker
health and safety in the U.S., it is
the law. The U.S. Occupational Health
and Safety Administration (OSHA) is
the main federal agency charged with

the enforcement of safety and health
legislation in the U.S. Much of this legislation is written in the form of standards. OSHA standards are rules designed to provide a work environment
free from known dangers or hazards.
They require the use of certain safe
practices and equipment, and assign
employers the responsibility of monitoring hazards and keeping records of
workplace injuries and illnesses. Compliance with OSHAs standards is mandatory and is stringently enforced.
In 2011, Respiratory Protection,
General Industry (29 CFR 1910.134)
was OSHAs fourth most frequently
cited standard violation. Standard 29
CFR 1910.134 covers the respiratory
protection division of the personal
protective-equipment category. Essentially, it details the requirements for
compliance in workplaces where respiratory hazards are a potential threat
(Figure 3). The aforementioned statistic reveals that too many workers are
not employing appropriate protection
from respiratory hazards on the job.
According to OSHA, an estimated 5
million workers are required to wear
respirators in 1.3 million workplaces
throughout the U.S.
protection in the workplace, including

the following:
Respiratory protection program requirements
Standard operating procedures for
programs
Respirator selection, limitation and
use
Training
Fit testing
Maintenance, inspection, storage
and disposal
Breathing air and oxygen-deficient
atmospheres
Recordkeeping
Establishing a program
FIgure 2. This is an example of a
full-facepiece respirator that covers the
wearers face from the hairline to below
the chin
The role of ANSI
In addition to OSHA, another driving force in the regulatory arena is

the American National Standards Institute (ANSI). As a voice of the U.S.
standards and conformity assessment
system, ANSIs mission is to enhance
both the global competitiveness of
U.S. business and quality of life by
promoting and facilitating voluntary
consensus standards and conformity
assessment systems, and safeguarding their integrity, in an effort to protect workers.
ANSI thus provides a neutral
forum for the development of policies
on standards issues and serves as a
watchdog for standards development
and conformity assessment programs
and processes [2]. ANSI/AIHA Z88.2
Standard Practices for Respiratory
Protection is a voluntary consensus
standard drafted by the ANSI Z88
Committee on Respiratory Protection
[3]. This standard is significant, as it
addresses the issue of assigned protection factors (APFs). APFs are the main
factor used by many employers when
they select respirators for worker protection from airborne hazards. The
ANSI standard recommends protective factors that are very similar to
those of OSHA, except for a more conservative APF for filtering facepieces
(disposable respirators). The standard
also addresses other key issues regarding the proper use of respiratory
The fundamental goal of any respiratory protection program is to control

occupational diseases and injuries
caused by breathing air contaminated
with harmful dusts, fogs, fumes, mists,
gases, smoke, sprays and vapors. The
defense against these contaminants is
simple: keep them out of the workers
breathing air.
Engineering and administrative
controls, which have the potential to
completely eliminate the hazard, must
always be implemented first. These
include actions such as enclosing or
confining the contaminant-producing
operation, exhausting the contaminant, or substituting the contaminant with a less-toxic material. Work
practices such as limiting employee
exposure should also be considered.
If these controls do not eliminate the
hazards, then employers must provide
appropriate respiratory protection for
every employee who might be exposed
to them.
Whenever OSHA standards or employers require respirator use, there
must be a complete respiratory protection program in place. Employers must
have written operating procedures to
ensure that employees use the respirators safely and properly. Users must
be familiar with these procedures as
well as the types of respirators available and their limitations.
A qualified program administrator. First of all, a qualified program
administrator must be responsible for
the program. This person must know
enough about respirators to supervise
the program properly. Larger plants
or companies with industrial-hygiene,
in-house medical, safety-engineering

or fire-prevention departments should
administer the program in liaison with
the program administrator. In smaller
plants that do not have specialists, an
upper-level superintendent, foreman
or qualified person must serve as the
program administrator.
Employee training. Any respirator program should stress thorough
training of all respirator users. Employees must be aware that a respirator does not eliminate the hazard.
If the respirator fails, the user will be
overexposed to dangerous substances.
To reduce the possibility of failure, the
respirator must fit properly and be
maintained in a clean and serviceable
condition. Employers and employees
must understand the respirators purpose and limitations. Users must not
alter or remove the respirator even
for a short time, regardless of its potential discomfort.
Regular evaluation. Employers
must evaluate the effectiveness of
their companys respirator program
regularly and modify the written operating procedure as necessary to
reflect the evaluation results. Workplace conditions that affect respiratory hazards and respirator use may
change over time. This would include
new work processes or techniques,
the use of new or different materials
or chemicals, changes in the amount
of a respiratory hazard present in the
workplace and changes in the types
of respirators being used. The written
program must therefore be updated as
necessary to reflect and address these
changes. Employees should always notify their employer if a change in the
workplace occurs that conflicts with,
or may not be covered by, the existing respirator training or established
workplace policies or procedures.
Choosing the correct respirator
Selecting the right equipment is a

three-step process:
1. Define the hazard and determine its
extent.
2. Evaluate user factors that affect respirator performance and reliability.
3. Select an appropriate respirator that
is certified by the National Institute
for Occupational Safety and Health
(NIOSH) [1]. Note that equipment
29
Written respirator program

sec (c)
Cover Story
Hazard assessment
sec (d)
must always be used in accordance

with the specifications accompanying the NIOSH certification.
When selecting respirators, employers must consider the chemical and
physical properties of the contaminant, as well as the toxicity and concentration of the hazardous material
and the amount of oxygen present.
Other selection factors are the nature
and extent of the hazard, employee
work rate, the size of the area to be
covered, worker mobility, work requirements and conditions, and the
limitations and characteristics of the
available respirators.
Air-purifying respirators use filters
or sorbents to remove harmful substances from the air. They range from
simple disposable masks to sophisticated devices. They do not supply
oxygen and must not be used in oxygen-deficient atmospheres or in other
atmospheres that are immediately
dangerous to life or health (IDLH).
Atmosphere-supplying respirators
are designed to provide breathable air
from a clean air source other than the
surrounding contaminated work atmosphere. They include self-contained
breathing apparatus (SCBA) units
(Figure 4a) and supplied-air respirators (SARs; Figure 4b).
The time needed to perform a given
task, including the time necessary to
enter and leave a contaminated area,
is an important factor in determining the type of respiratory protection
needed. For example, SCBAs, gas
masks, or air-purifying chemical-cartridge respirators provide respiratory
protection for relatively short periods.
On the other hand, an atmospheresupplying respirator that supplies
breathable air from an air compressor
through an air line can provide protection for extended periods.
If the total concentration of airborne
particulate matter is low, particulatefilter air-purifying respirators can
provide protection for long periods
without the need to replace the filter.
Where there are higher concentrations of contaminants, however, an
atmosphere-supplying respirator such
as the positive-pressure SAR offers
better protection for a longer time.
Since they use an independent air
source, SARs eliminate the need for
30
Voluntary respirator use

sec (c)(2)
Filtering facepiece
sec (c)(2)(ii)
Traditional facepiece
sec (c)(2)(i)
concern about filter breakthrough

times, change schedules, or the use of
end-of-service-life indicators (ESLIs)
for airborne toxic materials factors
that must be considered when using
air-purifying respirators.
Respirators must not impair the
workers ability to see, hear, communicate or move as necessary to perform the job safely. For example, atmosphere-supplying respirators may
restrict movement and present other
potential hazards. SARs, with their
trailing hoses, can limit the area
the wearer can cover and may present a hazard if the hose comes into
contact with machinery. Similarly, a
SCBA that includes a back-mounted,
compressed-air cylinder is both large
and heavy. This may restrict climbing and movement in tight places,
and the added weight of the air cylinder presents an additional burden
to the wearer.
Another factor to consider when
using respirators is the air-supply
rate. The wearers work rate determines the volume of air breathed per
minute. The volume of air supplied to
meet breathing requirements is very
significant when using atmospheresupplying respirators, such as selfcontained and air-line respirators that
use cylinders, because this volume determines their operating lives.
Peak airflow rate is also important
in the use of a constant-flow SAR.
The air-supply rate should always be
greater than the maximum amount
of air being inhaled in order to maintain positive pressure in the respiratory enclosure.
The increased breathing resistance of air-purifying respirators
under conditions of heavy work may
cause the user breathing difficulty,
especially in hot, humid conditions.
To avoid placing additional stress on
the wearer, use the lightest respirator possible that presents the least
Select type of protection

sec (d)
Medical evaluation
sec (e)
Fit testing
sec (f)
Training
sec (k)
Respirator use
sec (g)
Cleaning and maintenance
sec (h)
Program evaluation
sec (l)
Record keeping
sec (m)
Figure 3. This simplified illustration

shows the requirements that employers
must follow to comply with the 29 CFR
Part 1910.134 Standard
breathing resistance.
SCBAs and some chemical canister respirators provide a warning of
remaining service time. This may be
a pressure gage or timer with an audible alarm for SCBAs or a color ESLI
on the cartridge or canister. The user
should understand the operation and
limitations of each type of warning
device. For the many gas masks and
chemical-cartridge respirators without ESLI devices, the employer must
establish and enforce a cartridge or
canister change schedule. Employees
should begin each work shift with new
canisters and cartridges.
Ensuring proper fit
Different types of respirators, and

even different brands of the same type
of respirator, have different fit characteristics. No one respirator will fit
everyone. Some employees may be unable to get an adequate fit with certain
respirator models of a particular type
of respirator. This is why employers
must provide a sufficient number of
respirator models and sizes to ensure
ADDITIONAL RESOURCES
dditional information on protecting yourself from airborne

hazards can be obtained from the U.S. Occupational Safety
and Health Administration (OSHA), the National Institute for
Occupational Safety (NIOSH), and the American National Standards Institute (ANSI). Safety product manufacturers websites can
also be a helpful resource. Here are a few useful website links:
www.osha.gov/law-regs.html For OSHAs standards
www.cdc.gov/niosh The home page for the and Healths
National Personal Protective Technology Laboratory, which contains a variety of information and links related to respiratory
protection and other personal protective equipment
www.ansi.org The home page for ANSI
www.osha.gov/dte/library/materials_library.html OSHA
Directorate of Training and Educations Training and Reference Materials Library. Provides outreach training materials
(such as slide presentations) for OSHAs respiratory protection
standard, as well as links to additional resources about respiratory protection
webapps.msanet.com/ResponseGuide/ Website from authors company that contains two interactive tools: Chemical
Database & Respirator Selection and Cartridge Service Life Calculator, as well as a complimentary download entitled Managing a Respiratory Protection Program, a guide to simplifying
compliance with 29 CFR Part 1910.134
w ww.osha.gov/dts/shib/respiratory_protection_bulletin
_2011.html OSHA bulletin, General Respiratory Protection
Guidance for Employers and Workers (2011), which provides
basic information to employers and workers who may find
themselves using respiratory protection for the first time. It also
provides information on what respirators are, how they work,
that every employee can select an acceptable respirator that fits properly.
Corrective eyeglasses worn by
employees can also present a problem when fitting respirators. Special
mountings are available to hold corrective lenses inside full facepieces.
A qualified individual must fit the
facepiece and lenses to provide good
vision, comfort and proper sealing.
Tight-fitting respirators cannot provide proper protection without a tight
seal between the facepiece and the
wearers face. Consequently, beards
and other facial hair, the absence of
normally worn dentures, facial deformities, jewelry or head gear that projects under the facepiece seal can also
seriously affect the fit of a facepiece.
To ensure proper respiratory protection, check the facepiece each time you
wear the respirator. You can do this by
performing either a positive-pressure
or negative-pressure user-seal check.
Detailed instructions for performing
these checks are in Appendix B-1 of
OSHA 29 CFR 1910.134.
Qualitative versus quantitative
fit testing. Fit testing is required for
tight-fitting facepiece respirators. You
can test the effectiveness of the fit of
the facepiece two ways: qualitatively
and quantitatively.
Qualitative fit testing involves the
and what is needed for a respirator to provide protection

www.osha.gov/SLTC/etools/respiratory/index.html OSHAs
eTool, Respiratory Protection (1998), which provides employers with instruction on the proper selection of respiratory protection and the development of change schedules for gas/
vapor cartridges
www.osha.gov/Publications/OSHA3079/osha3079.html
OSHA guidebook, Respiratory Protection, publication no.
3079, (2002). This booklet clarifies key provisions of the respirator protection standard, which was revised in January 1998.
It also provides specific guidance on respirator selection, fit testing, hazard evaluation and medical evaluation
w w w. o s h a . g o v / P u b l i c a t i o n s / 3 2 8 0 - 1 0 N - 0 5 - e n g l i s h
-06-27-2007.html OSHA quick card, Respirators Quick
Card, publication no. 3280 (2005), which provides employees with a brief description of the different types of respirators available
w ww.cdc.gov/niosh/npptl/topics/respirators/disp_part/
RespSource.html NIOSH Web page, NIOSH Respirator
Trusted-Source Information Page, which provides information
to understand the types of respirators, how to identify approved
models and outlets for purchase, a listing of all NIOSH-approved
and U.S. Food and Drug Admin. (FDA) -cleared surgical N95
respirators, a listing of recently revoked respirator approvals
and relevant user notices. It also contains information on how
to implement the use of respirators in the workplace and use
them appropriately, including commonly asked questions and
answers (fact sheets), respirator myths, the science of respirator
function and performance, and respiratory protective devices
not approved by NIOSH
introduction of a harmless, but strong,

smell or irritating substance into the
breathing zone around the respirator
being worn. If no odor or irritation is
detected by the wearer, then this indicates a proper fit.
Quantitative fit testing offers more
accurate, detailed information on respirator fit. While the wearer performs
exercises that could induce facepiece
leakage, a fit-testing instrument numerically measures the amount of
leakage into the respirator. This testing can be done either by generating
a test aerosol as a test atmosphere,
using ambient aerosol as a test agent,
or using controlled negative pressure
to measure any leakage. Detailed instructions for performing both qualitative and quantitative fit testing are
contained in Appendix A of OSHA 29
CFR 1910.134.
Proper inspection and care
It is important to inspect all respirators for wear and tear before and
after each use, giving special attention to rubber or plastic parts that
can deteriorate or lose pliability. All
parts including the facepiece, headband, valves, connecting tube, fittings
and cartridges, canisters or filters
must be in good condition. A respirator inspection must include check-
ing the tightness of the connections.

SCBAs should be inspected at least
monthly, and air and oxygen cylinders
should be fully charged according to
the manufacturers instructions. This
inspection should include a check of
regulator and warning devices to ensure proper functioning. Employers
must keep a record of inspection dates
and results.
Chemical cartridges and gas mask
canisters should be replaced as necessary to provide complete protection,
following the manufacturers recommendations. Additionally, mechanical
filters should be replaced as necessary
to avoid high breathing resistance.
Only an experienced person is permitted to make repairs, using parts
specifically designed for the respirator. This person must consult the manufacturers instructions for any repair,
and no attempt should be made to repair or replace components or make
adjustments or repairs beyond the
manufacturers recommendations.
Employers must ensure that respirators are cleaned and disinfected
as often as necessary to keep them
sanitary. In addition, the employer
must have emergency-use respirators
cleaned and disinfected immediately
after each use.
Respirators should be washed in
31
Cover Story
a detergent solution and then disinfected by immersing them in a sanitizing solution. Cleaner-sanitizers
that effectively clean the respirator
and contain a bactericidal agent are
commercially available. Strong cleaning and sanitizing agents and many
solvents can damage rubber or plastic
respirator parts. Use these materials
with caution or after consultation with
the respirator manufacturer.
Store respirators in a manner that
provides protection against dust, sunlight, heat, extreme cold, excessive
moisture and damaging chemicals.
When packed or stored, each respirator should be positioned to retain its
natural configuration. Facepieces and
exhalation valves should rest in a normal position to prevent the rubber or
plastic from deforming.
Manufacturers tools
There are three especially valuable

tools that can assist in the development, administration and maintenance of a workplace respiratory protection program:
Respirator selection guide
Cartridge life expectancy calculator
Manufacturer training programs
Many respirator manufacturers
websites contain these tools. OSHAs
website contains a respirator selection guide.
Respirator selection guide. A respirator selection guide is designed
to help users identify the proper
respirator solution to meet their individual needs. Choices include everything from SCBAs to half- and
quarter-type facemasks. In addition
to selecting the proper respirator, a
respirator selection guide also helps
users choose the correct filtering
element if their exposure situation
allows for the use of an air-purifying respirator. The following steps
should be taken to use a respirator
selection guide.
Step 1: Assess your environmental
conditions to determine the hazard(s).
To determine an atmospheres oxygen
content or concentration level of gaseous contaminants, proper air sampling must be conducted. The results
of this sampling will determine what
level of protection is required. Generally, respirator and cartridge selection
32
FigureS 4a and 4b. Supplied-air respirators are designed to provide breathable air
from a clean air source other than the surrounding work atmosphere. They include selfcontained breathing apparatus units (left) and air-line respirators (right)
is based on three factors:

1. The results of the atmospheric monitoring or sampling program
2. The accepted American Conference
of Industrial Hygienists (ACGIH),
OSHA or NIOSH exposure limits for
the substance(s) present
3. The maximum use concentration of
a substance for which a respirator
can be used
An additional part of the hazard assessment process is determining
whether the contaminant has adequate warning properties. This affects respirator selection because
chemical cartridge respirators and
gas masks should only be for routine
use against gases and vapors with
adequate warning properties, unless
the cartridge is equipped with an
end-of-service life indicator.
Step 2: Check chemical exposure
limits. After finding out what hazards
exist, compare the chemical concentration at your facility (determined by air
sampling) with the chemicals exposure limits. Note that most respirator
selection guides use the lowest exposure limit published by ACGIH, OSHA
or NIOSH as a baseline to determine
the need for respiratory protection.
One exception to this rule is when an
OSHA substance-specific standard
exists with applicable respirator use
limitations for protection against the

chemical of interest. In this case, the
OSHA requirement is specified.
Step 3: Select a respirator and cartridge. Now it is time to select a respirator and cartridge. During this
process it is important to note that
recommendations in a respirator selection guide are typically based on
appropriate levels of respiratory protection. If you choose, a higher level of
protection can be used by selecting a
respirator with a higher maximumuse concentration or, if applicable, a
higher cartridge-filter efficiency. This
is advisable if the atmosphere in the
work area is prone to changes, since
the contaminant concentration has
the potential to become higher.
Cartridge life-expectancy calculator. Lets assume that you determined that the respirator of choice
should be a full-facepiece with a
multi-gas cartridge. It is now time to
use the cartridge life-expectancy calculator. This tool is interactive and
is designed to provide guidance as to
how long a specific cartridge should
be used before it needs to be replaced.
The determination is called time of
breakthrough and refers to the point
at which a hazardous chemical will
begin to break through the cartridge
or filter without being absorbed or
collected by the protective barrier.

OSHA requires that respirator cartridges be replaced at pre-determined
intervals based on worksite-specific
usage conditions [4].
A cartridge life-expectancy calculator is very easy to use. Simply answer a minimal number of questions
by entering key environmental and
usage factors. The calculator then
provides a suggested maximum service time for the cartridge(s) being
used in that specific environment.
Although cartridge calculators may
vary somewhat, they all require the
same basic input:
Chemical hazard and concentration
Temperature
Relative humidity
Atmospheric pressure or altitude
Type of respirator and cartridge
Type of work and average breathing
rate (light, moderate or heavy)
Breakthrough concentration preference
Safety factor
When using a cartridge life-expectancy
calculator you must remember that
this tool provides a guideline for your
final decision on cartridge replacement. Several other factors should
also be considered, such as changes
in conditions during the work shift,
changing climate conditions (seasonal
changes), condition of the cartridge
or respirator, cartridge storage con-
ditions, accuracy in determining the

ambient conditions and user training
experience. Ultimately, the appropriate change-out schedule must be developed by a qualified professional.
Manufacturer training programs.
The third tool is the training programs that are available from respirator manufacturers. In addition
to onsite training, some respirator

manufacturers offer online programs
through their websites. As part of an
effective training program, the user
may be required to pass a test about
the respirator, including how to wear
and maintain it. An employee training
program is required by OSHA.
References
1. A list of NIOSH-approved respirators can be
found at http://www.cdc.gov/niosh/npptl/topics/respirators/cel/
2. About ANSI Overview, http://ansi.org/about_
a n s i / o v e r v i e w / o v e r v i e w. a s p x ? m e n u i d
=1 (accessed September 18, 2012)
3. The ANSI/AIHA Z88.2 Standard Practices
for Respiratory Protection is available on
the ANSI website, www.ansi.org
4. Federal Register, p. 1272, col.1 OSHA
1910.134(d)(3)(iii)
Get more out of your coal.

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Author
Dennis Capizzi is the product line manager for air purifying respirators at MSA
Safety
(1100
Cranberry
Woods Dr., Cranberry Twp.,
PA, 16066; Phone: 724-7768600; Email: dennis.capizzi@
MSAsafety.com), where he
has worked since 2007. He
serves as head of the North
American Air-Purifying Respirator Steering Team, and
has a seat on the International Safety Equipment Assn.s Committee for Respiratory Protective Escape Devices.
ThyssenKrupp Uhde
www.uhde.eu
33
Solids
Environmental
Processing
Manager
Eye-and-Face Personal
Protective
Equipment
Gateway Safety
Protecting the eyes and face in the workplace

is imperative to preventing the estimated
1020% of work-related eye injuries
that result in temporary or permanent vision loss
Victor J. DAmato
Atrium Environmental Health and Safety Services
ye injuries of all types occur

at a rate of more than 2,000
per day in the U.S., and half
of those occur in the workplace. In 2006, the U.S. Bureau of
Labor Statistics (BLS) reported over
52,000 workplace injuries to the eyes
and face, and approximately 70% of
those were eye injuries [1]. The need
to protect the face and eyes in the
workplace is clear.
Implementing an eye-and-face
protection program is important for
several reasons. One is compliance.
Between October 2006 and September 2007, more than 450 citations resulted in more than $215,000 in fines
and penalties to manufacturers for
failure to comply with the U.S. Occupational Safety & Health Administration (OSHA) standard for eye and face
protection [2].
Another reason is the cost of eye
and face injuries. The financial cost
of these injuries is enormous and can
range from $300 to $3,000 per case.
More than $300 million per year is lost
in production time, medical expenses,
and workers compensation according
to OSHA. The return on investment
for implementing an eye-and-face
safety program is huge as its cost is
48
relatively inexpensive compared to

the potential expense of an injury. But,
no dollar figure can adequately reflect
the personal toll these accidents take
on injured workers. Prevent Blindness America estimates that 1020%
of work-related eye injuries result in
temporary or permanent vision loss.
This article outlines the basics of
eye-and-face protection programs for
plant operations, including key compliance requirements and practical
information for personal protective
equipment (PPE) selection.
The causes of injuries
Most impacts to the face come from

flying objects, usually particulate
matter. When a particle hits the face it
might cause a cut or scratch, and the
skin will repair itself over time given
proper medical attention. If the particle hits the eye, it causes direct damage, and it is far more difficult for the
eye to repair itself.
BLS reports that of the nearly 36,000
injuries to workers eyes in 2006, nearly
70% resulted from contact with objects
like flying particles, falling objects or
sparks striking the eye. Contact with
chemicals was responsible for the remaining 30% of eye injuries.
Chemical Engineering www.che.com February 2009
FIGURE 1.
Safety glasses help
shield eyes from impact hazards
OSHA compliance
OSHA defines minimum requirements for workplace PPE in Subpart I

of the Occupational Safety and Health
Standards for general industry employers (29 CFR 1910), which include
the chemical process industries (CPI).
The general requirements of this standard include that employers select
PPE for their employees based on the
hazards present in the workplace, and
that employers train employees on the
proper use and limitations of the PPE
selected for use. In November 2007,
OSHA updated the standard to specifically require employers to pay for
the PPE required under the standard,
with some limited exceptions [3].
The OSHA Eye and Face Protection
Standard (29 CFR 1910.133) was established specifically to protect employees
from eye and face hazards in the workplace. To comply with this standard,
employers must ensure the following:
1. Employees who may be exposed to
eye or face hazards from flying particles, molten metal, liquid chemicals,
acids, caustic gases, vapors or potentially injurious light radiation use
appropriate eye or face protection.
2. Employees who may be exposed to
a hazard from flying objects use
eye protection that provides side
protection.
3. Employees who require prescription lenses while engaged in operations that involve eye hazards wear eye protection that
incorporates the prescription in
table 1. Hazard Assessment
Gateway Safety
Hazard type
Examples of hazard
Common related tasks
Impact
Flying objects, such as

large chips, fragments,
particles, sand and dirt
Chipping, grinding, machining, masonry

work, wood working, sawing, drilling, chiseling, powered fastening, riveting and sanding
Heat
Anything emitting extreme heat
Furnace operations, pouring, casting, hot

dipping and welding
Splash, fumes, vapors

and irritating mists
Acid and chemical handling, degreasing,

plating and working with blood
Dust
Harmful dust
Woodworking, buffing and generally dusty

conditions
Optical
radiation
Radiant energy, glare

and intense light
Welding, torch-cutting, brazing, soldering and

laser work
Chemicals
FIGURE 2. Face
shields protect the
entire face, but do not
protect the eyes from
impact hazards when
worn alone. Safety glasses
or goggles should also be worn
its design, or that they wear eye

protection that can be worn over
the prescription lenses without
disturbing the proper position of
the prescription lenses or the protective lenses.
4. Eye-and-face personal protective
equipment is distinctly marked so
that the manufacturer is clearly
identified.
5. Employees who may be exposed
to injurious light radiation during
work process, such as welding, thermal cutting, brazing, torch soldering, and using lasers, use eye protection equipped with filter lenses that
have a shade number appropriate
for the work being performed.
implementation
Implementing a practical, effective

PPE program includes the following
straightforward steps, which are described in more detail below.
1. Assess the workplace for hazards.
2. Select PPE based on these hazards.
3. Train workers on proper PPE use.
4. Determine how prompt emergency
care will be provided in the event of
an accident.
Hazard assessment
OSHA provides guidance on conducting hazard assessments, which are

summarized as follows [4].
1. The first step in the hazard assessment for eye and face protection is
to walk through your facility and
identify the potential hazards that
can injure the eyes or face. Hazards
should be assessed by occupation or
trade, work area and work activity.
Source: U.S. Dept. of Labor, Occupational Safety & Health Administration (OSHA), Eye and
Face Protection eTool, http://www.osha.gov/SLTC/etools/eyeandface/ppe/selection.html
2. Identify the sources of the hazards. Talk to employees as they

know best about their trades,
work areas and processes.
Consider all possible hazards,
even those that seem minor or
unlikely. Some examples of eye and
face hazards and typical sources are
summarized in Table 1.
3. Organize the data collected. Develop a table or spreadsheet listing
the occupations, work areas, and
processes you identify, the hazards
identified in each category, and the
sources of the hazards.
4. Analyze your data, considering the
probability and severity of each
hazard. Keep in mind that multiple hazards and sources may be
present. This will help in deciding
which PPE is appropriate.
5. Certify your assessment. OSHA requires that every employer verify its
assessment, identifying the areas
assessed, who performed the assessment, and the dates it was performed.
6. Review and update your assessment
on a routine basis, or if changes in the
workplace or processes are planned.
PPE selection
The American National Standards

Institute (ANSI) standard for eye and
face protection (Z87.1) sets forth criteria related to the description, general requirements, testing, marking,
selection, care and use of eye and face
PPE in the workplace. The 2003 edition specifies requirements for safety
glasses, safety goggles, face shields
and full-face and hooded respirators.
This ANSI standard is revised and
updated routinely to reflect current
technologies and the current state of
practice. While most PPE manufacturers have adopted the 2003 edition
of the standard in new products, eye
and face PPE currently being used
may have been manufactured to

meet earlier editions of ANSI Z87.1.
OSHA requires that eye and face
PPE purchased after July 1994 be
manufactured to meet the 1989 edition of ANSI Z87.1.
Eye and face PPE that meets the criteria specified in ANSI Z87.1 must be
marked with a manufacturers unique
marking and the Z87 marking. Special purpose lenses and shaded lenses
must also be marked indicating the
purpose and shade. Eye and face PPE
must be selected based on the hazards
identified in the hazard assessment.
Some examples of the types of protection available for hazards are summarized in the next sections.
Ultimately, the eye and face protection must be comfortable to wear
and not interfere with the employees
work. Poor-fitting PPE will not afford
the necessary protection, may be uncomfortable to wear, and may not get
used. Since eye-and-face protection
devices can come in different sizes,
care should be taken to ensure that
the right size is selected.
Impact hazards. Safety spectacles
(Figure 1) are intended to shield the
wearers eyes from impact hazards,
such as flying fragments, objects,
large chips, and particles. Workers
are required to use eye safety spectacles with side shields when there is
a hazard from flying objects. Non sideshield spectacles are not acceptable
eye protection for impact hazards. The
selection of safety glasses is almost infinite as a host of manufacturers have
stepped up to meet employee demand.
Safety goggles are also intended to
shield the wearers eyes from impact
hazards. Goggles fit the face immediately surrounding the eyes and form
a protective seal around the eyes. This
prevents objects from entering under
or around the goggles.
49
Face shields (Figure 2) are intended
to protect the entire face or portions of
it, but they do not protect employees
eyes from impact hazards when worn
alone. Face shields should be used in
combination with safety spectacles or
goggles for additional protection. Faceshield windows are made of varying
types of transparent materials and
in varying thicknesses, both of which
should be considered when selecting
face shields for specific tasks. Window
and headgear devices are available in
various combinations to be compatible
with other PPE, such as hardhats.
Welding shields (Figure 3) provide
eye and face protection from flying
particulate matter during welding,
thermal cutting and other hot-work
activities. These shields are typically
equipped with shaded lenses that provide protection from optical radiation.
Heat hazards. Working with heat
requires goggles or safety spectacles
with special-purpose lenses and side
shields. However, many heat-hazard
exposures require the use of a face
shield in addition to safety spectacles
or goggles. When selecting PPE, consider the source and intensity of the
heat and the type of splashes that may
occur in the workplace.
Chemical hazards. Safety goggles
(Figure 4) protect the eyes, eye sockets, and the facial area immediately
surrounding the eyes from a variety of chemical hazards. The protective seal formed around the eyes is
especially important when working with or around liquids that may
splash, spray or mist. Several kinds
of cover-type goggles are available:
direct vented, indirectly vented or
non-vented. Its important to select
the right type. Vented goggles, for
example, may be less effective in protecting the eyes from splashes and
respiratory aerosols than non-vented
or indirectly vented goggles.
Face shields are intended to protect
the entire face from a variety of chemical hazards, particularly when pouring chemicals or where splashes may
occur. Face shields are considered secondary protection and must be used in
addition to safety goggles to provide
adequate protection.
Dust hazards. Working in a dusty environment can cause eye injuries and
50
presents additional hazards

to contact lens wearers. Safety
goggles should be worn when
dust is present. Safety goggles
are the only effective type of eye
protection from nuisance dust.
Optical radiation hazards.
Welding, thermal cutting, brazing, laser work and similar
operations create intense concentrations of heat, ultraviolet,
infrared, and reflected-light radiation. Some of these activities
can produce optical radiation
intensities greater than those
experienced when looking directly at the sun. Unprotected
exposure may result in eye injuries including retinal burns,
cataracts, and permanent blindness. Many lasers produce invisible ultraviolet, and other forms
FIGURE 3. Welding shields are typically equipped
of non-ionizing radiation.
with shaded lenses to protect from optical radiation
The OSHA standard (29 CFR
1010.133) includes a table that lists Institute for Occupational Safety
the minimum shade requirements and Health (NIOSH) issued a Curfor eye protection during industrial rent Intelligence Bulletin (CIB) on
processes that generate optical radia- the use of contact lenses in chemical
tion. The selection of eye protection for environments. In this CIB, NIOSH
lasers should depend on the lasers in recommends that workers be permituse and the operating conditions, and ted to wear contact lenses when hanshould be consistent with the laser dling hazardous chemicals provided
that certain safety guidelines are folmanufacturers specifications.
PPE and prescription lenses. If lowed and that contact lenses are not
employees wear reading glasses with banned by regulation or contraindibasic magnification, ANSI-approved cated by medical or industrial hygiene
safety glasses and goggles with read- recommendations. OSHA recommends
ing magnifiers in the lenses are an op- against contact-lens use when worktion. Its also possible to buy prescrip- ing with certain chemicals, including
tion safety glasses and goggles that acrylonitrile, methylene chloride, 1,2
ethylene
are compliant with the ANSI stan- dibromo-3-chloropropane,
dard. ANSI-compliant goggles and oxide and methylene dianiline.
The NIOSH recommendations are
safety glasses are also available to fit
over prescription glasses; but, they specifically intended for work with chemcan be uncomfortable and less likely ical hazards, and do not address hazards
from heat, radiation, or high-dust or
to be worn.
Wearing contact lenses under some high-particulate environments [5].
circumstances provides workers with Usable life of PPE. All PPE has a
a greater choice of eye and face pro- usable lifespan. Most manufacturers
tection and better visual acuity. How- recommend how frequently eye-andever, the risk of injury to the eye from face protection equipment should be
chemical exposure is unknown for con- replaced. If the PPE becomes damtact lens wearers compared with non- aged or distorted, it must be replaced
wearers working with chemicals. It is to work properly. As far as the usable
important to note that contact lenses life of a product, a good rule of thumb
are not eye protective devices, and is if your safety glasses are more than
wearing them does not reduce the re- five years old, they may not be compliquirement for eye and face protection. ant with the latest ANSI standards, so
In June 2005, the U.S. National you should get a new pair.
Summary of NIOSH Recommended Safety Guidelines

for Contact Lens Use in Chemical Environments
1. Conduct an eye-injury hazard
evaluation* in the workplace
that includes an assessment of
the following:
Chemical exposures
Contact lens use
Appropriate eye and face
protection for contact lens
wearers
2. Provide suitable eye and face
* NIOSH recommends that eye injury
hazard evaluations be conducted by
competent, qualified persons such as
certified industrial hygienists, certified
safety professionals, or toxicologists.
Information from the hazard evaluation
should be provided to the examining occupational health nurse or occupational
medicine physician.
contact lenses as soon as pracabout any defined areas where

protection for all workers extical. Do not delay irrigation
contact lenses are restricted.
posed to eye injury hazards,
while waiting for contact lens
6. Identify to supervisors all conregardless of contact lens
removal.
tact lens wearers working in
wear.
9. Instruct workers who wear conchemical environments to en3. Establish a written policy
tact lenses to remove the lenses
sure that the proper hazard asdocumenting general safety reat the first signs of eye redness
sessment is completed and the
quirements for wearing contact
or irritation.
proper eye protection and first
lenses, including the eye and
10. Evaluate restrictions on
aid equipment are available.
face protection required and
7. Train medical and first aid per- contact lens wear on a caseany contact lens wear restricby-case basis, taking into
sonnel in the removal of contact
tions by work location or task.
account the visual requirelenses and have the appropri4. Comply with current OSHA
ments of individual workers
ate equipment available.
regulations on contact lens
wearing contact lenses as
8. In the event of a chemical
wear and eye and face
recommended by a qualified
exposure, begin eye irrigaprotection.
ophthalmologist or optometrist.
tion immediately and remove
5. Notify workers and visitors
Source: Contact Lens Use in a Chemical Environment, Current Intelligence Bulletin 59, NIOSH Publication No. 2005-139: June 2005
FIGURE 4. Safety goggles form a

protective seal around the eyes
Gateway Safety
Employee training
BLS reports that workers injured

while not wearing protective eyewear
often say they believed it was not required by the situation. Even though
the vast majority of employers furnish
eye protection to employees at no cost,
about 40% of workers report they receive no information on where and
what kind of eyewear should be used.
OSHA requires that all employees
who use PPE for protection against
workplace hazards be trained in when
and how to use their PPE. This training must include the following:
1. A summary of the occupations, work
areas or tasks where eye and face
protection is necessary.
2. What types of eye and face protection are necessary for each occupation, work area or task.
3. How the eye and face protection is
put on, taken off, adjusted and worn
to be effective.
4. The limitations of the eye and face
protection used.
5. The manufacturers recommendations on the proper care, maintenance, useful life and disposal of eye
and face protection devices.
Training must be conducted prior to an employees assignment

to the work area or
task where the hazards may be present, and
at the time when the eye and
face protection is issued. There
is no annual requirement for retraining; the onus of ensuring that
employees understand when and how
to use their eye and face protection
is on the employer. OSHA does state
that when employees are found wearing PPE improperly or not at all, they
need to be retrained.
Emergency care
OSHA mandates that if a hazard exists, a means for flushing the eye must
be provided. The eye-and-face protection program should include considerations for emergency eyewash stations
that provide a full 15-min flush. There
is an ANSI standard (Z358) for eyewash stations. In the field, eyewash
bottles can be on hand for interim assistance until an eyewash station can
be reached. There are also portable
eyewash stations available that can
dispense water for 15 minutes.
Resources
OSHA has an excellent Eye and

Face Protection eTool on its website
(http://www.osha.gov/SLTC/etools/
eyeandface/ppe/selection.html) that
can assist with hazard assessments,
provides information about selecting
PPE and summarizes specific OSHA
requirements. The OSHA guidelines

in Ref. 4 also include a useful PPE selection guide.
The American Industrial Hygiene
Association website (www.aiha.org) offers more information on occupational
health and safety topics including a
list of industrial hygiene consultants
who specialize in safety issues.

References
1. Bureau of Labor Statistics, Case and Demographic Characteristics for Work-related
Injuries and Illnesses Involving Days Away
From Work (2006), http://stats.bls.gov/iif/oshcdnew.htm
2. Occupational Safety & Health Administration Inspection Data, http://www.osha.gov/
pls/imis/industryprofile.html
3. Occupational Safety & Health Administration, Employer Payment for Personal
Protective Equipment; Final Rule FR
72:64341-64430, Table XV-2 l, Vol. 72, No.
220, Nov. 15, 2007.
4. Occupational Safety & Health Administration, Compliance Guidelines for Hazard
Assessment and Personal Protective Equipment Selection, 29 CFR 1910, Subpart I, Appendix B .
5. Contact Lens Use in a Chemical Environment, Current Intelligence Bulletin 59,
NIOSH Publication No. 2005-139, June 2005.
Author
Victor DAmato is the director for Atrium Environmental,
Health and Safety Services,
LLC (11495 Sunset Hills Road
Suite 210, Reston, VA 20190;
Phone: 7036899482; Email:
vdamato@atriumehs.com). He
has been providing environmental, safety and industrial
hygiene support to manufacturing, research and development, utilities, telecommunications, aerospace, shipyard, facilities management
and defense industries for more than 20 years.
He has a B.S. in Environmental Health from Old
Dominion University, and a M.S. in Engineering
Management from The George Washington University. He is an American Board of Industrial
Hygiene Certified Industrial Hygienist (CIH) and
a Board of Certified Safety Professionals Certified Safety Professional (CSP). He is a member
of the American Industrial Hygiene Association
(AIHA) and has served as president of the AIHA
Potomac Section.
51
Solids
Environmental
Processing
Manager
Managing Compliant
MSDSs and Labels
Compliant MSDS programs
depend on inventory management,
regulatory knowledge and consistent authoring
Jytte Syska and Tamie Webber
3E Company
hemical regulatory compliance is growing in complexity

as product sourcing and formulations proliferate and organizations expand into new markets
on a global scale. Staying current with
the requirements of international regulatory initiatives such as the Globally Harmonized System of Classification and Labeling of Chemicals (GHS)
and the Registration, Evaluation and
Authorization of Chemicals (REACH)
adds to the challenge (CE, March 15,
2008, p. 3847, and CE, June 15, 2008,
p. 2630).
A key compliance requirement of
these initiatives is the proper management of Material Safety Data
Sheets (MSDSs) and labels. Both GHS
and REACH significantly impact the
corporate strategy for MSDS management, as the regulations require
affected companies to update these
documents to maintain compliance.
Comprehensive inventory management, thorough regulatory reporting
and consistent MSDS and label authoring are three critical components
of a REACH- and GHS-compliant
MSDS management program.
MSDS management
Accurate chemical inventory management is the cornerstone of any MSDS

management program. Regulatory
compliance mandates that companies
obtain and maintain MSDSs for the
raw materials, as well as for the full
composition of mixtures. For REACH
compliance, this requirement helps
companies establish the category into
which individual substances fall: man-
ufactured within the European

Union (E.U.), imported into the
E.U., or purchased from a supplier
within the E.U. For REACH,
companies also must identify
each substances tonnage and
current classification.
Comprehensive regulatory reporting is also crucial to achieving
GHS compliance. In addition to
consistently tracking regulations, companies must track
modifications made to ingredients, products, and quantities and inventories.
While authoring accurate and
compliant MSDSs has always
been a mission-critical obligation, the advent of REACH
and GHS brings new challenges to this already highly
demanding task. For highervolume hazardous substances,
REACH requires companies to
attach an exposure scenario
to the MSDS. The exposure
scenario describes how the
chemical can be used in a safe
manner, with minimal risk, for the
intended use. The exposure scenario can cover either each
individual substance in the
chemical product or describe
the mixture as a whole.
The first registration deadline under REACH passed on
December 1, 2010. Import or
manufacture of high-volume
chemical substances and of
CMR- (carcinogenic, mutagenic and toxic-to-reproduction) classified substances is no
Figure 1.
The advent of GHS and R
EACH regulations brings new
challenges to the already demanding and mission-critical task of
authoring compliant MSDSs
longer possible unless the importer or manufacturer has registered under REACH. Many
of the substances that were
registered for the December 1, 2010 deadline have
exposure scenarios. The
registrant must attach the appropriate exposure scenarios to
their MSDSs, and the company
using these substances must
then include the information from the exposure scenarios when they prepare
and supply the MSDSs to their
customers. The European Chemical Agency (ECHA) has recommended a four-section exposure-scenario format, but
many different formats are
being used. Work is ongoing
to harmonize the information in
the exposure scenarios and to
establish a common XML format for data exchange.
As a step toward improved
compliance, companies should
obtain the necessary overview of
the current regulations and detailed
understanding of how they relate
to their chemicals and their
supply chain. Manufacturers,
users and distributors should
be aware not only of their own
obligations but also of those to
downstream customers and to employees. In addition, corporate
product-stewardship
staff
must understand when these
regulations are implemented
by country in order to know
how to properly plan.
Chemical Engineering www.che.com february 2011
43
GHS
GHS is the United Nations (UN) system for harmonization of classification and labeling of chemicals. GHS
has already been officially adopted by
certain countries in regions around
the globe. Countries can choose to
implement GHS in its entirety or
implement only certain parts of the
regulation, otherwise known as the
building block approach.
The true complexity of the standard is realized when reviewing its
implementation status in a sample of
countries around the world. For representative comparison purposes, we
have provided a brief overview of the
status of GHS in the following areas:
the U.S., Japan and the E.U.
The U.S. On September 30, 2009, the
U.S. Occupational Safety and Health
Admin. (OSHA; Washington, D.C.;
www.osha.gov) released its proposal
to modify the current Hazard Communication Standard (HCS) to conform
with the GHS.
The proposed OSHA revisions include both philosophical and tactical
changes to hazard communications,
which have far-reaching implications
for MSDSs and the authoring, publishing, distribution and management
of labels. The proposal also includes
revised criteria for the classification
of hazardous chemicals, as well as
changes to definitions and terms used
in the standards, and new training
requirements for employees. When
the final rule is promulgated, companies will
face many challenges,
including re-evaluating how their substances and mixtures
are classified, re-issuing MSDSs and labels,
Figure 2.
Service providers
can help companies
stay ahead of the
regulatory compliance curve
44
and training staff as appropriate.

After having accepted public comments until the end of 2009, OSHA
has estimated that a minimum of 18
months will pass from the notice of
proposed rulemaking before the final
rule is promulgated. Companies will
have three years from promulgation
to come into compliance with the final
rule and two years to implement training requirements on the final regulation. Once the rule is final, companies
can begin implementation. However,
in accordance with a letter of interpretation from OSHA on October 6, 2009,
companies can begin following the
E.U. GHS-label format for their OSHA
labels as long as the labels also comply
with the current HCS.
In addition, 26 U.S. states and territories have their own OSHA-approved
plans. The 26 are: Alaska, Arizona,
California, Connecticut, Hawaii, Indiana, Iowa, Kentucky, Maryland,
Michigan, Minnesota, Nevada, New
Jersey, New York, New Mexico, North
Carolina, Oregon, Puerto Rico, South
Carolina, Tennessee, Utah, Vermont,
Virginia, Virgin Islands, Washington,
Wyoming. They will have six months
from promulgation to adopt comparable provisions of the final standard.
In the meantime, each individual
state plan will remain in effect until it
adopts the required revisions.
Provided the legal process proceeds as planned, companies would
be allowed to issue MSDSs and labels
for the U.S. market according to the
changed rule, based on GHS classification, no earlier than July 2011, and
all existing MSDSs and labels would
have to be updated in accordance with
the new requirements no later than
July 2014. In comparison, MSDSs for
the European market had to be in
line with the E.U. GHS implementation no later than December 2010 for
pure substances and by June 2015 for
chemical mixtures.
The label requirements will involve
changes in the printing process and
most likely will require many companies to invest in new label printers.
Labels on products that are shipped
outside the U.S. must have the chemical hazard pictograms with a red
frame, signal words and the required
hazard and precautionary statements.
It is still being determined whether or

not empty frames will be accepted on
the label and whether or not labels for
products sold and used exclusively in
the U.S. can have the frame printed
in black.
Japan. In Japan, the Industrial Safety
& Health Law (ISHL; December 2006)
currently details requirements for
MSDSs and labels. The ISHL provides
a list of substances that are subject to
MSDS and label requirements, and
also provides a classification results
list, which details the classification
of about 1,500 regulated chemicals.
The Japanese Industrial Standard
(JIS), which specifies the standards
used for industrial activities in Japan,
also has requirements for labels (JIS
Z 7251:2006) and MSDSs (JIS Z
7250:2005). Recently JIS Z 7252:2009
was published for the standard of GHS
classifications for health and environmental hazards.
E.U. The European Union is currently
in a transitional period with regard to
GHS. The European Parliament finalized and issued the Regulation (EC No.
1272/2008 on classification, labeling and
packaging of substances and mixtures
the CLP Regulation) in late 2008. An
amendment bringing the CLP in line
with the third revision of the GHS was
drafted in 2010.
The CLP Regulation provides the
following transitional periods for classifying and labeling hazardous substances and mixtures:
Substances must be classified, labeled and packaged according to CLP
from December 1, 2010 forward
Mixtures can be classified, labeled
and packaged according to the Preparations Directive until June 1, 2015
Supplemental labeling information,
in line with the old labeling systems
requirements, is still applicable
under the CLP
The transitional periods for re-labeling and re-packaging of substances
and mixtures placed in the supply
chain before December 1, 2010 are
postponed until December 1, 2012 and
June 1, 2017 respectively.
REACH
The E.U.s REACH regulation went

into effect on June 1, 2007 sometimes simplifying, but also complicat-
ing, the compliance work for companies manufacturing in, importing into
or exporting from European countries.
As a result of the new legislation, all
companies manufacturing, importing,
distributing or using chemical substances (on their own, in mixtures or
in articles) in Europe, are required to
closely examine their chemical inventory for substances within the scope of
the regulation to ensure compliance.
Key components of REACH mandate the following:
Registration of manufactured/imported chemical substances
Increased information and communication throughout the entire supply chain
Evaluation of some registered substances
Authorization for use of substances
of very high concern
Restriction of the use of certain substances for specific applications
The scope of REACH is vast, and
there are several issues that could
impact a companys ability to meet
its obligations under REACH, including changes to the content of MSDSs.
Under REACH, additional information
from manufacturers is required and
the information must be aligned with
that associated with the registration of
the substance. When an exposure scenario has been required as part of the
REACH registration of a substance,
every safety data sheet for a product
containing this substance must have
the exposure scenario attached.
Choosing the right tools
As many companies realize, establishing GHS and REACH compliance is

difficult. However, there are service
providers who can help companies stay
ahead of the curve with solutions for
identifying and managing the increasingly complex and changing global
chemical-regulatory obligations associated with GHS and REACH. These
vendors can help address the new
requirements and associated chemical regulatory information needed for
compliance management as they arise.
For example, there are several commercially available content tools that
can be used to feed chemical regulatory data into corporate EH&S (environmental, health and safety) and
MSDS authoring systems. These integrated data tools provide efficient

change management and regular updates as regulations change and new
ones are released. These tools can
help ensure correct, consistent GHS
classification and labeling according
to the U.N. purple book and also take
into consideration the national deviations and other national regulations.
Document templates for producing
MSDS, labels and other hazard communication documents and multilingual phrase libraries can complete the
content suite for efficient production
of accurate documents.
Companies also may choose to employ
outsourced services for their GHS classification of substances and mixtures as
a separate service or as part of outsourcing MSDS and label authoring.
In-house MSDS authoring staff may
want to adopt an authoring platform
that will help generate hazard communication documents to meet GHSrelated, international-regulatory compliance and business requirements.
Such a platform should provide full
support of hazard communication,
classification and labeling requirements to generate globally compliant
MSDS and label documents as well as
business- or user-definable documents,
such as technical data sheets, product
data sheets, hazard summaries and
product stewardship summaries. The
system should use algorithms to accommodate the requirements outlined
in the GHS. This consists of the classification of substances and mixtures
according to their health, environmental and physical hazards and hazardous communication requirements for
labeling and MSDS.
For inbound vendor MSDS management, users will want to search,
print, view and Email vendor and
raw material safety data sheets in a
company-specific database via a Webbrowser interface. As GHS require-
References
1. The U.S. Chemical Safety and Hazard Investigation Board (CSB), webpage, (www.csb.gov).
2. Center for Chemical Process Safety. Guidelines for Hazard Evaluation Procedures
With Worked Examples (2nd Ed.), AIChE,
1992.
3. American Equipment, Inc., Process Safety
Management Guidelines for Compliance,
OSHA document 3133, 1994 Appendix., copyright 1999 2005; www.exforklifts.com.
ments increase the burden of vendor

MSDS management, a robust MSDS
management system can help reduce
the time and resources necessary for
effective compliance management.
Compliance help is available
Creating, analyzing and managing

globally compliant MSDSs, product
label content and hazardous materials
transportation documents that reflect
both GHS and REACH requirements
can be extremely challenging. Strong
processes, applications, systems and
service providers are needed to support the various aspects of compliance
management. Companies that are impacted by GHS or REACH, or both, can
seek assistance from providers who
are well versed in data and other content and information as they relate to
global EHS regulations and who thoroughly understand the global regulatory environment. These providers will
be able to assist in implementing GHS
and REACH compliance activities into
the organization, and can help facilitate compliance with these increasingly complex and changing global,
chemical regulatory obligations.
Edited by Scott Jenkins
Authors
Jytte Syska is managing director of 3E Company Europe
ApS (Lyngbyvej 20, 3, DK
2100, Copenhagen, Denmark.
Phone: +1-760-602-8700; Email: jsyska@3ecompany.com)
and president of Ariel operations. Syska has more than 20
years of experience as an environmental, Health and Safety
(EHS) regulatory expert.
Prior to her present duties,
she spent several years as 3Es vice president of
international operations. Syska has also held the
position of director of occupational health and
toxicology for the prestigious Danish Toxicology
Center (DTC). Syska holds an M.S. degree in
civil engineering from the Technical University
of Denmark. She is fluent in Danish and English,
and reads and understands German, French,
Norwegian and Swedish.
Tamie Webber is director of
product management at 3E
Company and is responsible
for product management initiatives, product planning
and strategies and product
development for 3Es product
line, including MSDS distribution and management,
emergency response, regulatory reporting, training and
waste services. She joined 3E
after several years of marketing and product
management experience in the chemical distribution and high-tech industries. She has worked
for Great Western Chemical and Intel Corp. She
holds a B.S. degree in finance and marketing
from the University of Oregon.
45
Feature
Cover
Story
Report
Design Safer Solids

Processing Plants
This approach defines a
systematic framework
and points toward
relevant sources in the
public domain
Identify
raw materials
& intermediates
START
Background
Through dedicated efforts of the larger

process safety community, a tremendous body of useful technical information has been compiled in various
handbooks and publications [112].
These guidelines are based on current
state of knowledge and vast industrial
34
Assess
hazard
potential
Measure
relevant
properties
Preliminary
process
configuration
Define operating
conditions /
window
Investigate alternate
unit operations, configuration
and raw materials
Shrikant Dhodapkar
Konanur Manjunath
Pradeep Jain
The Dow Chemical Company
hemicals, plastics, pharmaceutical, food, agricultural chemicals,
coal and bio-chemical industries
have a wide array of processes
where the raw materials, intermediates and products are in particulate
form. Hazards associated with particulate solids are unique, and in most
cases depend on the particle size. The
purpose of this paper is to present a
systematic framework for designing
particulate processes with appropriate pointers towards relevant sources
in the public domain. We hope to raise
safety awareness among chemical engineers dealing with particulate solids.
It is not possible to design and operate a process safely and reliably unless
the equipment suppliers, design team
and plant personnel are aware of the
potential hazards. Hazard awareness
should include material properties, process design and operational issues. The
readers are strongly encouraged to read
relevant references cited in this article.
Review
MSDS, tech
datasheets
Key Issues
No
Safety factors & design codes

Corrosion and erosion allowances
Specifications - flexibility vs. clarity
Environmental impact
Energy efficiency
Testing and inspection
OSHA standards
EPA regulations
Management of change
Employee training & documentation
Preventive maintenance vs.
predictive maintenance
Assess
severity of
process hazards
LO
PA
Process
risk
acceptable?
Identify measures
to reduce
hazard severity
Yes
Design
Installation
Operation &
maintenance
Key Issues
Proper
installation
of process
Testing and
inspection
Guidelines
for on-site
fabrication
Figure 1. Overall systematic approach for safer design
experience in handling and processing

particulate materials.
A flowchart has been developed to
guide the reader through the process
(Figure 1). Each step is discussed in
the supporting text. The overall design
process is an iterative process. Hazards
due to the material and due to the process must be considered independently
and then jointly to assess the risk.
What makes solids or particulate
processes challenging is the lack of generic databases of material properties.
Most of the properties have to be measured in the laboratory. Determination
of suitable tests and understanding the
limitation of the test result is critical.
Assess hazard potential
The hazards associated with particulate process can be broadly categorized per the following:
Material (particulate) related

Mechanical rotating equipment,
pinch points
Thermal potential of burns
Environmental noise, dustiness,
pollution or waste streams
During handling, manufacturing,
storage and transport of particulate
solids, four generic chemical hazards
related to material properties can be
identified:
Combustibility or flammability
Reactivity
Toxicity
Instability
An in-depth discussion of these hazards can be found in the National Fire
Protection Associations NFPA 704,
NFPA 654 and various publications
from the Center for Chemical Process
Safety (CCPS). Many important concepts and issues are addressed here.
Chemical Engineering www.che.com January 2007
34-39 CHE 1-07.indd 34
12/26/06 5:22:55 PM
Fuel
Others
26%
Ignition
Dispersion
Confinement
Dust collector
26%
Mixers/
blenders 4%
Grinders /
pulverizers
13%
Oxygen
Dryers
9%
Figure 2. These conditions must be

present for an explosion to occur
Conveying
systems
10%
Table 1. Measured Properties of Combustible Dust

Property
Definition
ASTM Test
Method
Application
KSt
Dust deflagration index
ASTM E
1226
Measures the relative explosion

severity compared to other dusts
Pmax
Maximum explosion
overpressure generated
in the test chamber
ASTM E
1226
Used to design enclosures and

predict the severity of the consequence
(dp/dt)max
Maximum rate of pressure rise
ASTM E
1226
Predicts the violence of an explosion. Used to calculate KSt
MIE
Minimum ignition energy
ASTM E
2019
Predicts the ease and likelihood

of ignition of a dispersed dust
cloud
MEC
Minimum explosible
concentration
ASTM E
1515
Measures the minimum amount

of dust, dispersed in air, required
to spread an explosion. Analogous to LFL for gas air mixture
LOC
Limiting oxygen concentration
ASTM standard under

development
Determines the least amount of

oxygen required for explosion
propagation through the dust
cloud
ECT
Electrostatic charging
tendency
No ASTM
standard
Predicts the likelihood of the material to develop and discharge

sufficient static electricity to ignite
a dispersed dust cloud
A two-step approach to assessment of particulate hazards is recommended. A preliminary assessment is

based on NFPA 704 rating, UN guidelines and material safety data sheets
(MSDSs). The final assessment must
include laboratory data and larger
scale testing.
Combustibility or flammability.
Information on combustibility is often
lacking in MSDSs. Even when the
data are reported, failure to report
test method and material-specific information (such as, moisture, particle
size distribution) makes the data unusable. Some guidance can be found in
Flammability Rating as described in
NFPA 704.
Handbooks written by Eckhoff [2],
Barknecht [4] and Babrauskas [5]
are excellent sources for ignition and
combustibility of wide variety of materials.
According to NFPA 654, combustible
dust is a combustible particulate solid
that presents a fire and deflagration
hazard when suspended in air or some
other oxidizing medium over a range
of concentration, regardless of particle size or shape. Dusts traditionally
have been defined as materials 420
microns or smaller (capable of passing

through a U.S. No. 40 standard sieve).
The exceptions are fibers with high
aspect ratio and agglomerates of fine
particles formed by electrostatic attraction.
Combustible particulate solids, on
the other hand, include fines, chips,
chunks, flakes, fibers and mixtures of
these. Upon handling, these can attrit
and generate combustible dust.
A deflagration is propagation of a
combustion zone at a velocity that is
less than the speed of sound in the unreacted medium, whereas explosion is
bursting or rupture of an enclosure or
a container due to the development of
internal pressure from a deflagration.
For a dust explosion to occur, the following requirements must be met:
Fuel The dust must be combustible
Oxygen and dispersion Dust must
be dispersed in air or an oxidant at
or exceeding minimum explosible
concentration (MEC)
Process confinement
Ignition source with sufficient energy (such as an electric spark, electrostatic discharge, flame, hot surface or glowing embers)
Silos /bunkers
12%
Figure 3. Equipment involved in dust

explosions in the U.S. (1975-2001), U.K.
(1979-1988) and Germany (1965-1985) [1]
These requirements are pictorially

represented by the dust explosion
pentagon (Figure 2). Two additional
requirements (dispersion and confinement) have been added to the wellestablished fire triangle. In the absence of these, fire or deflagration can
still occur.
Historical data (Figure 3) show that
the probability of dust explosion can
be varied, depending on the unit operation. While explosions in dust collectors are the most common, other
process units should also be designed
with particulate safety in mind. To determine potential of deflagration of a
combustible dust, one must use actual
test data. Depending on the process
and operating conditions, some or all
of the following tests may be used:
1. Particle size distribution
2. Moisture content (as received)
3. Electrical volume resistivity
4. Charge relaxation time
5. Chargeability
6. Minimum ignition energy (MIE)
7. Minimum explosible concentration
(MEC)
8. Limiting oxidant concentration
(LOC) to prevent ignition
9. Maximum explosion pressure at
optimum concentration
10. Maximum rate of pressure rise at
optimum concentration
11. KSt (normalized rate of pressure
rise)
12. Dust cloud ignition temperature
13. Layer ignition temperature
These properties should be measured
according to ASTM standards (see Table
1). In addition, a number of consensus
and other government standards have
been prepared and universally practiced in the industry (Table 2).
Reactivity. Preliminary evaluation of
reactivity hazards can be done from
MSDSs and chemical incompatibility
charts provided by NOAA/EPA Chemical Reactivity Worksheet. There are
specific NFPA guidelines for various
materials. Brethericks Handbook [8]
34-39 CHE 1-07.indd 35
35
12/26/06 5:23:22 PM
Table 2. Relevant NFPA Standards For Combustible Dusts
Cover Story
and CCPS Guidelines [1, 9] on reactivity hazard evaluation are excellent
resources. Other resources are listed
in Table 3.
Toxicity. Inhalation of fine particles
(typically 0.2 to 7 m [1]) poses respiratory hazard since the particles can
get lodged in the lungs. Other potential hazards include ingestion, dermal
contact and eye contact. It is also important to evaluate the carcinogenicity and allergenic properties of particulate solids. Relevant parameters are
summarized in Table 4.
Instability. Instability refers to materials susceptibility to release energy
either through decomposition or polymerization. NFPA 704 provides classification 0 to 4 in increasing order of
instability hazard. Many U.S.-based
companies include this information in
the MSDSs. Methods for measuring instability are described in Table 5.
Measure relevant properties
Particulate hazards are related to particle size, size distribution, dispersion,

moisture content and chemical nature. All the generic hazards stated
earlier (combustibility, reactivity,
instability and toxicity) increase
with decreasing particle size.
Unlike liquids, where general conclusions can be drawn from published
data, for particulate solids one must
generate material specific data. The
following parameters are important in
this context:
Particle size and size distribution
Shape
Specific surface area
Bulk Density
Fluidization characteristics
Dispersibility
Abrasiveness
Friability and hardness
Moisture content
Electrical volume resistivity
Common methods for measurement
of these parameters are shown in
Table 6.
Define the operating window
One must consider not only steady state

conditions but also include startup,
shutdown and transgression scenarios
in defining the operating window. Perform sensitivity analysis on control
variables to estimate the variability
36
Standard
NFPA 61
NFPA 68
NFPA 69
NFPA 654
NFPA 70
NFPA 499
NFPA 655
NFPA 664
Title
Standard for the Prevention of Fires
and Dust Explosions in Agricultural
and Food Processing Facilities
Coverage or Purpose
Applies to facilities that receive, dry,
handle, process, blend, use, mill, package,
store, or ship bulk dry agricultural material;
their products or dusts; or facilities that
handle or manufacture starch, or facilities
that handle and process oil seed
Guidelines for Deflagration Venting Provides technical guidance on designing,
sizing, installing, and maintaining deflagration vents
Standard on Explosion Prevention Addresses the design of explosion prevenSystems
tion, protection, and mitigation systems
Applies to the manufacturing,
It covers all combustible dusts, except those
processing, blending, conveying,
specifically addressed in other NFPA stanrepackaging, and handling of
dards, and is one of the most cited docucombustible particulate solids and ments for control measures for combustible
their dusts
dust hazards (OSHA, 2005; CCPS, 2005)
The National Electric Code 2005 Addresses electrical equipment and wiring
requirements for special situations, including those in which an explosive atmosphere may exist. Defines combustible-dust
classified locations
Recommended Practice for the
Provides guidance for classifying dust proClassification of Combustible
cessing locations for electrical equipment
Dusts and Hazardous (Classified) installation
Locations for Electrical Installations in Chemical Process Areas
Standard for the Prevention of Sul- Discusses facilities that handle, grind, profur Fires and Explosions
cess, pulverize, or crush elemental sulfur
Standard for the Prevention of Fires Discusses facilities that process or manuand Explosions in Wood Processing facture wood and wood products, or that
and Woodworking Facilities
create wood dust and particles
Table 3. Resources for Chemical Reactivity and Compatibility

EPA/NOAA Reactivity
Worksheet Reactivity
Groupings
The EPA/NOAA Reactivity Worksheet defines 47 chemical groupings for reactivity hazard considerations. Representative groupings and combinations of groupings are shown in Table 2-10 of
Ref [1]
Coast Guard Chemical This chart has 22 primary reactive groupings, and another 14
Compatibility Chart
groups that may potentially react with some of the primary
groups. An X in a particular cell of the chart indicates that the
corresponding combination of groupings should be avoided because of reactivity problems
Chemical-Specific Com- These are matrices that provide summary descriptions or hazard
patibility Charts
ratings for pairs of specific chemicals, as opposed to chemical
groupings. The hazards of the individual materials are indicated
in the cells along the diagonal, while the hazards of binary combinations are indicated in the cells below the diagonal
in operating conditions. Consider situations corresponding to emergency

shut-down and loss of utilities (electric
power, steam, water and nitrogen).
Assess severity
of process hazards
A detail analysis and how-to guide

can be found in the CCPS publication
Guidelines for Hazard Evaluation
Procedures Second Edition [9]. A
brief snapshot of various available approaches is listed below.
Safety review: This is intended to
identify plant conditions or operating
procedures that could lead to significant property damage, injury or environmental impact. This is also known
as Process Safety Review, Design Review or Loss Prevention Review.
Checklists: Provide a written list of
items or procedural steps written by a
group of experienced experts drawing
upon information from various codes
and standards. The level of detail can
vary depending on the process under
investigation. This is an excellent tool

to get inexperienced team members
familiarized with the process.
Relative ranking: It is a strategy for
comparing and ranking the attributes
of various process options to determine whether they warrant further
investigation.
Preliminary hazard evaluation:
It focuses on the hazardous materials
and major process areas in the plant.
It covers raw materials, intermediates
and final products, plant equipment,
operating conditions, operational procedures and facility layout.
What-if analysis: It is a brainstorming (hence relatively unstructured)
approach where a group of experience
subject matter experts generate list of
questions and discuss about possible
undesired and unintended vents.
What-if/checklist analysis: This approach combines the systematic approach of checklists with rather unstructured approach of brainstorming.
Hazard and operability analysis
34-39 CHE 1-07.indd 36
12/26/06 5:23:49 PM
Table 4. Summary of Toxicity Parameters [1]

Property
Threshold Limit Value
(TLV)
Permissible Exposure
Limit (PEL)
Governing body
American Conference of
Government Industrial Hygienists (ACGIH)
OSHA
Immediately Dangerous to Life and Health

(IDLH)
Short Term Exposure
Limit (STEL)
American Conference of
Government Industrial Hygienists (ACGIH)
Amount
Maximum exposure concentration
recommended
Maximum permissible exposure limit
for systemic workplace 8-hour timeweighted average exposures
Concentration that poses a threat of
either death, adverse health effects,
or inability to escape danger without
respiratory protective equipment.
Limiting exposure concentration for
exposure durations up to 15 minutes,
Table 5. Methods to Measure Instability
of Particulate Materials
Parameter
Differential
Mackey test
Standard
ASTM
Self-accelerating
decomposition
temperature
Relative selfignition temperature
Coal dust adiabatic heating
Procedure
Open-top double chamber for test sample and
inert sample with a 10 g
of sample for up to 72 hrs
BAM SADT
0.5 liter Dewar in oven
with 400 ml of sample
size for 168 hrs
VDI 2263
Grewer oven with preheated air flow with 8 ml
sample for uptp 5.5 hrs
Bureau Mines AdiaOven with preheated air
batic Heating Oven (RI flow with 100 g
8473)
Application
In the case of
particulate materials prone to
self-heating and
possible spontaneous ignition, in unit
operations such as
drying at elevated
temperature, heating, and deposition
of solids on heated
surfaces.
Table 6. Summary of Relevant Standards for

Material Property
Particle size and size distribution
Bulk Density, Fluidity and Dispersity
Moisture Content
Hardness and Friability
Electrical Resistivity
Combustibility
Standardized Measurement Methods

Sampling & Size Analysis (NIST SP-960); Sieving
(ASTM D-1921-96); Electrozone method (ASTM
F577);
Carr Indices (ASTM D6393)
See Iinoya et al. [11]
Hardness (ASTM E140), Fracture toughness
(ASTM E1820), Vickers Hardness (ASTM E384)
IEC 61241-2-2
See Table 1
(HAZOP): This technique identifies

and evaluates safety hazards and potential operability problems in a process plant.
Failure mode and effects analysis
(FMEA): This approach tabulates the
failure modes of equipment and their
effects on a system or process.
Fault tree analysis (FT): It is a deductive technique which focuses on
one particular event or failure and
provides a method for determining
the causes.
Event tree analysis (ET): This analysis considers the responses of safety
systems and operators to the event
and determines the potential outcome
using a graphical approach.
Cause-consequence analysis (CCA):
It is a blend of fault tree analysis and
event tree analysis.
Human reliability analysis (HRA):
It is a systematic evaluation of factors
that influence the performance of operators, maintenance staff and other
plant personnel.
The applicability of these approaches
at various stages of a project has been
summarized in Figure 4. To prepare

for process hazard analysis, the following information should be gathered:
Material-specific hazard data (such
as flammability, reactivity, toxicity
and instability)
Process and instrumentation diagrams and index flowsheets of the
process
Instrumentation: Purpose (diagnostics, safety or process control) and
list of critical instruments
Control logic, including interlock logic
and safety shutdown sequences
Equipment specifications and maintenance history (if preexisting)
Applicable codes, material of construction, chemical compatibility
and corrosion tolerances for each
equipment
Electrical area classification and requirements
Steady state operating conditions
and their range for each of the unit
operations
Effect of deviation of control variables on the system response, along
with the response strategy This is
procedural and computer driven

Hazard analysis of each unit operation and interconnect unit operations where applicable
Methodology to handle equipment
failure or loss of utilities (steam, nitrogen, water and electric power)
Industrial hygiene and occupational
safety requirements
Analysis of environmental impact of
the process
Refer to the detailed check list presented in CCPS publication [Table 7-1;
1] for process hazard analysis for solids processes. It should be noted that
each company has its own guidelines
and exhaustive list of questions to
evaluate process hazards.
General tips
Take a system-wide approach. Processes have interconnected unit operations. Sudden change in process
conditions can have a dominoes effect in an interconnected system.
It is important to perform sensitivity
analysis on the basic assumptions of
process parameters to ensure that
conclusions are still valid for the entire range.
Identify measures
to reduce hazard severity
Process safety system measures or design solutions can be grouped into the
following three categories:
1. Inherently safer processes / passive
2. Active
3. Procedural
Inherently safer processes refer to selection of alternate process conditions
or materials that are less hazardous. A
common example would be the use of
water as a solvent in paint formulation
as compared to an organic solvent. For
particulate processes, particles with
larger particle size can be produced
through agglomeration. However, the
feasibility of this approach depends on
the chemistry of the process and final
application of the product.
Other ideas include minimizing
hazardous material in the process,
designing the process with less severe
conditions (temperature and pressure)
and simplifying process configuration.
Passive systems rely on reducing the
frequency and consequences of an incident through process or equipment
design, and without the use of any ac-
34-39 CHE 1-07.indd 37
37
12/26/06 5:24:16 PM
CC
A
ET
Sa
fe
t
Ch y re
ec vi
e
Re klis w
t
la
tiv
PH e
ra
A
nk
W
in
ha
g
t
W -if
ha
t
HA -if c
ZO he
FM P ckl
is
EA
t
FT
Cyclone
Solvent
recycle
Reactants
A
B
Research and development

Conceptual design
Pilot plant operation
Solid-liquid
separation
Detailed engineering
Dust
collector
Silo
Construction / start-up
Reactor
Routine operation
Expansion or modification
Dryer
Additives
Incident investigation
Decommissioning
Mixer
Rarely used or
inappropriate
Commonly
used
Figure 4. Applicability of Hazard Evaluation Techniques [9]
tive device. For instance, a vessel can

be designed to contain the maximum
pressure during a deflagration. These
approaches are most robust amongst
all approaches because they do not require intervention.
Active safety systems are designed
to monitor a hazard and react to prevent an incident or minimize its consequences. They are also known as Engineering Controls. Safety valves rupture
disks, sprinkler systems, safety interlocks, automatic shutdown, process
control system and check valves are
common examples of active systems.
Since their effectiveness depends on
reliable operation, these systems are
often installed with redundancy and
accompanied with a preventive or routine maintenance program.
Procedural safety measures (administrative controls) refer to a set of
instructions that require action from
personnel to avoid an incident or minimize its consequences. The human factor inherent in this approach makes
it least reliable. Standard operating
procedures (SOP), safety rules, preventive maintenance, emergency response and management of change
are typical examples.
A simple hypothetical process example is shown in Figure 5 with a summary of appropriate process safety measures listed in Table 7. To determine the
process safety measures, one must first
identify all the failure scenarios for
each unit operation. All the safety measures associated with each unit operation should then be listed. Consider the
consequences of each failure scenario
on connected unit operations, and check
if it leads to additional failures.
For example, dust explosion in a
dryer can damage the downstream
38
Figure 5.
Pneumatic
Example of solids
conveying
processing plant with
some typical unit operations
dust collector. Prioritize the measures

by first selecting the most common
passive measures, followed by the active measures and then the procedural
measures. One must keep track of
process economics while adding
each layer of protection.
Analyze and assess process risk
For any unit operation involving solids

or a combination of solids with vapors
and liquids, an analysis of risk using
tools such as layer of protection analysis (LOPA) is recommended. A team of
people must be in place to carry out
LOPA, representing the facility, process safety and the unit operation.
In order to identify the potential for
risk, the team must understand the
process and be familiar with the operating conditions so that a potential
scenario can be identified. There may
be several such potential scenarios for
a given unit operation and the team
must focus on each of these scenarios
and provide independent, auditable
and measurable layers of protection
[12]. The independent layer is required
for a particular scenario and does not
depend on other scenarios. Its effectiveness must be focused on stopping
the scenario, and in order to do so a
measurement layer must be in place.
LOPA is very effective in analyzing
the situation and designing a safer
plant. In order to conduct LOPA, following information is essential:
Data on the four generic chemical
hazards (reactivity, flammability,
toxicity and instability
Knowledge of various unit operations
Knowledge of plant problems
Knowledge to fix and troubleshoot
problems
FIBC
Engineering to minimize risk
Various engineering approaches are

possible to minimize risk in a process:
Process equipment design (use passive measures)
Select alternate unit operations
Optimize process configuration or
sequence
Use different chemistry or route
Select less severe process conditions
Use raw materials and intermediate
which are less hazardous
Process design
It is recommended that the following

issues be included while evaluating
design options:
Noise generation (especially for air
movers)
Energy efficiency (especially for
dryers)
Capital intensity (capital investment / production rate)
Process layout (minimize material
transfer distances and use gravity
whenever possible)
Waste stream management
Environmental impact of the process
While writing equipment specification, one must pay close attention
to the code requirements in country
where the process will be installed.
Instrumentation: Identify critical
instruments and provide redundancy
or have an on-line spare. Include sufficient instrumentation to aid process
diagnostics.
Any process design change must undergo full review to understand unintended consequences.
Installation
Make sure that delivered equipment

is inspected and tested.
Provide detailed guidelines for on-
34-39 CHE 1-07.indd 38
12/26/06 5:24:56 PM
Table 7. Summary of Typical Process Safety Measures

for The Hypothetical Process (Figure 5)
Preventive Measure for Process Safety /
Inherently Safe /
Active
Passive
Reactor
Design reactor to con- Vent the deflatain pressure; Congration; Inerting
sider non-flammable or purging
solvent and reactants
Solid-Liquid Mechanical spark Select design with no Relief valve; Fire
Separator in rotating equip- moving parts; Design suppression sysment with flamto contain the prestem; Inerting or
mable solvent
sure; Non-flammable purging
solvent
Filter plugging
Design to contain
Relief valve
resulting in overpressure; Select
pressure
proper filter media
Dryer
Combustible
Design dryer to mini- Inerting or purgdust buildup
mize build up; Reduce ing; Venting defin dryer
residence time; Con- lagration; Autotain overpressure; Per- matic isolation
manent bonding and
grounding
Unit
Operation
Potential Failure
Scenario /
Process Hazard
Explosive concentration in headspace
Design Solutions
Procedural
Ground and
bond all conductors and personnel
Preventive maintenance; Monitor
vibrations
Frequent cleaning cycle
Periodic inspection and cleaning; Emergency

response procedures; Manual
activation of fire
fighting
Dust ColCombustible fines Design to contain def- Venting deflagra- Frequent backlector
built-up and unlagration;
tion or supprespulsing; Ground
grounded cages
Design to minimize
sion; Automatic
check during
and bags
dust buildup
isolation
installation
Mixer
Combustible dust Design mixer to
Inerting or purg- Operate mixer at
concentration in
contain deflagration ing; Venting
low speed
mixer headspace Consider coating
deflagration or
combustible dust with suppression; Auinert material
tomatic isolation
Cyclone
Discharge outlet
Provide a secondary Level sensor in
plugged, resulting filter

cyclone
in emission
Pneumatic Pipe joints (com- Use flanges instead
System shutdown Regular inspecConveying pression coupling)
with pressure
tion and mainSystem
failure resulting in
surge
tenance of couspillage
plings
Silo
Vent plugged re
Provide pressure- Inspection and
Storage
sulting in overpresvacuum relief
maintenance
sure or vacuum
of vent keep
clean
FIBC
Ungrounded
Use Type D FIBC
site fabrication (such as welding), construction and testing.
Maintenance
There are two types of routine maintenance: preventive and predictive.

The preventive maintenance schedule
draws upon recommendations from
the manufacturer, repair history, design life and mean time between failure data. This type of maintenance
can be planned and conducted safely
in controlled conditions. Predictive
maintenance relies on real-time data
in put to anticipate the need for maintenance before a failure can occur.
Summary
In this paper, we have proposed a logical approach towards designing safer

solids processing plants. Particulate
materials behave differently from liquids and gases, and it is essential to
appreciate these differences. Acquiring relevant and reliable characterization data, evaluating process hazards systematically, selecting effective
Use self testing grounding

clamps
Make sure that

the FIBC is
grounded and
bonded (Type C)
safety measures (design solutions)

and leveraging extensive information
available in the public domain [112]
are essential for designing safer solids
processing plants.
Acknowledgements
The authors would like to thank Tim

Overton (chief process safety engineer,
The Dow Chemical Company, Freeport, Texas) for his valuable comments
and suggestions.
References
1. Center for Chemical Process Safety, Guidelines for Safe Handling of Powders and Bulk
Solids, AIChE, 2005.
2. Eckhoff, R., Dust Explosion in Process Industries, Butterworth-Heinneman, 1997.
3. National Fire Protection Association, Bulletins 654 and 59.
4. Bartknecht, W., Dust Explosions: Course,
Prevention, Protection, Springer-Verlag,
New York, 1989.
5. Babrauskas, V., Ignition Handbook, Fire
Science Publishers, Society of Fire Protection
Engineers (NFPA), Quincy, MA, 2003.
6. Standard for Prevention of Fire and Dust
Explosion from the Manufacturing Processing and Handling of Combustible Particulate
Solids, NFPA 654, 2005.
Authors
Shrikant V. Dhodapkar is a
technical leader in the Process
Fundamentals Group at The
Dow Chemical Co. (B-4810, Dow
Chemical, Freeport, TX 77541;
Phone: 979-238-7940; Fax: 979238-7463; E-mail: sdhodapkar
@dow.com). He received his
B.Tech. in Chemical Engineering from I.I.T-Delhi (India) and
his M.S.Ch.E. and Ph.D. from
the University of Pittsburgh.
During the past 18 years, he has published numerous papers in particle technology and contributed
chapters to several handbooks. He has extensive
industrial experience in powder characterization,
fluidization, pneumatic conveying, silo design, gassolid separation, mixing, coating and the design of
solids processing plants. He is a member of AIChE
and chair of the Particle Technology Forum.
Manjunath Konanur is a
core technology discipline
leader for solids processing
at The Dow Chemical Co.
(APB/1624, Dow Chemical,
Freeport, Tx 77541. Phone:
979-238-1501; Fax: 979-2380688; E-mail: KManjunath@
dow.com. Previous to joining
Dow, he worked in Norway,
with
CMR/POSTEC
and
Norsk Hydro as a principal
scientist and group leader for solids processing.
He received B.E.(Hons.) from the University of
Mysore (India) in mechanical engineering and
Ph.D. in solids processing from the University
of Newcastle, Australia. He has about 20 years
of experience in solids processing focusing on
various aspects of characterization, storage,
conveying, drying including dust explosion and
electrostatics for integrated designs and has contributed more than 30 publications.
Pradeep Jain is a Sr. Scientist in the Performance Plastics & Chemicals process R&D
at The Dow Chemical Co. (B4810, Dow Chemical, Freeport, TX 77541; Phone:979238-2782; Fax:979-238-2347;
Email: pjain@dow.com). He
received his B.Tech. In Chemical Engineering with honors
from the Institute of Technology, Banaras Hindu University (India) and his M.S.ChE from the University
of New Mexico. Over the past 20 years, he has
led the process development for the properiatery
olefins polymerization technologies, including
INSITE* and INFUSE*. He has extensive industrial experience in reaction kinetics, reactor
design and heat transfer and has designed the
processes that helped launch several new products, including AFFINITY*, ENGAGE*, ELITE*,
VERSIFY* and more recently INFUSE*. He has
been awarded several patents for these breakthrough product and process technologies. He is
a member of AIChE.
7. Standard System for Identification of the
Hazards of Materials for Emergency Response, NFPA 704, 2007.
8. Bretherick, L., Handbook of Reactive Chemical Hazards, (4th Edition), Butterworths,
London, 1990.
9. Center for Chemical Process Safety, Guidelines for Hazard Evaluation Procedures With Worked Examples (2nd Edition), Center
for Chemical Process Safety/AIChE, 1992.
10. Sax, I. and Lewis, R., Hazardous Chemicals
Desk Reference, Van Nostrand Reinhold,
New York, 1987.
11. Iinoya, K, Masuda, H. and Watanabe, K.,
Powder and Bulk Solids Handling Processes, Marcel-Dekker, New York, 1988.
12. Center for Chemical Process Safety, Layer
of Protection Analysis Simplified Process
Risk Assessment, Center for Chemical Process Safety/AIChE, 2001.
34-39 CHE 1-07.indd 39
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12/26/06 5:25:23 PM
Solids
Environmental
Processing
Manager
Finding the Right Gloves

To Fit the Application
There is a wide range of gloves available for hand protection
on the job. Matching gloves to their chemical-resistance
properties is one criterion for selection
Nelson Schlatter
Ansell
orkers in the chemical process industries (CPI) would

certainly benefit from the
perfect glove that would
be thick enough for thermal insulation, thin enough to promote dexterity
and tough enough to protect workers
from cuts and abrasion. The glove
would also protect against all known
chemicals and be offered at a minimal
price. This perfect glove, however, does
not exist. Processors and handlers,
therefore, must provide workers with
the most suitable, available gloves for
the application, considering individual
circumstances and how the gloves will
be used. Considerations to help choose
proper gloves for a given application,
with particular focus on chemical resistance, are presented here.
Factors to Consider
A person who selects gloves needs to

know much more than just the name
of the chemical to be handled. If an
employee, for example, is working
with nitric acid, then PVC (polyvinyl chloride) and neoprene are the
preferred glove materials. Several
questions, however, must still be answered. Is the worker cleaning up
spills? If so, the person will require
highly chemical-resistant gloves with
good storage stability because the
gloves may be kept in a spill-control
cabinet for several years until they
are urgently needed.
Is the person handling sealed bottles, which will require minimal protection unless the bottle breaks? Could
a spill be caused by breaking a bottle?
If so, the worker will need protection
from cuts as well as nitric acid. What
52
FIGURE 1.
Nitrile gloves
are low cost and have
excellent physical
properties, providing
protection against
oils and grease,
xylene, perchloroethylene and
aliphatic
solutions
is the probable length of exposure?

The longer workers are exposed to a
certain chemical, the greater the level
of protection required.
The chemical concentration must
also be considered. Is the compound
present only as a trace impurity? Is
the employee working with a pure
chemical or a dilute solution? If the
chemical is diluted, what solvent was
used for dilution?
Companies sometimes over-specify
gloves, which can lead to unecessary
expense. Once for example, a request
from a chemical company indicated
the need for gloves that would resist
high concentrations of toluene. When
questioned about the application, it
was revealed that workers would be
exposed to groundwater with a toluene
concentration of less than 100 parts
Chemical Engineering www.che.com July 2008
per million. While this is indeed a high

concentration for toluene in groundwater, in this case, gloves that protect
against water would be more appropriate and cost-effective than gloves that
protect against pure toluene.
Glove types
Gloves are generally categorized according to the materials used and

whether they are supported or unsupported (see definitions below). The
following glove types are available in
a range of lengths, thicknesses and
finishes, while some styles are offered
with special modifications.
Unsupported vs. supported
Unsupported gloves are made of

materials such as natural or synthetic latex, nitrile and neoprene and
Chemical-Resistance Information for Various Glove Materials

Chemical
Laminate
Nitrile
Neoprene
Polyvinyl
Chloride
PVC
NR
E
P
NR
E
P
Natural
Latex
Butyl
Viton
E
E
E
F
E
NR
Polyvinyl
Alcohol
PVA
P
NR
E
G
F
G
Acetone
Ammonium hydroxide
Butyl glycol ether
Ethyl acetate
Ethylene glycol
Gasoline (hi-test)
Hydrochloric acid,
concentrated
Hydrofluoric acid, 48%
Methanol
Methylene chloride
N-Methyl-2-Pyrrolidone
Mineral spirits, rule 66
Perchloroethylene
Sulfuric acid, concentrated
Xylene
>480
E
>480
>480
>480
E
NR
>480
E
NR
E
E
E
E
E
G
E
NR
>480
>480
>480
E
>480
F
P
>480
>480
NR
>480
>480
>480
>480
NR
>480
>480
>480
>480
E
>480
>480
>480
>480
>480
E
E
NR
NR
E
E
NR
G
>480
E
NR
NR
E
NR
F
NR
NR
NR
G
NR
E
E
NR
E
G
G
NR
NR
F
NR
G
NR
E
E
NR
E
NR
NR
NR
NR
>480
>480
G
>480
60
P
>480
P
180
F
E
NR
>480
E
>480
E
NR=not recommended; P=poor; F=fair; G=good; E=excellent; >480

indicates breakthrough times that are greater than 480 minutes (8
h) and correlates well with extremely good degradation resistance
achieve their glove shape by dipping

hand forms directly into the glove
compound without a supporting liner
or fabric. This type of glove generally
provides the dexterity and tactile
sensitivity required for many chemical applications.
Unsupported gloves offer a broad
spectrum of chemical resistance,
based on the material used. Nitrile
gloves, for instance, are excellent for
many chemical processing, oil refining, food processing and petrochemical applications. Gloves made with a
neoprene and natural-rubber-latex
blend provide the protection workers
need in food processing facilities and
certain chemical- and pesticide-manufacturing plants.
Supported gloves are made by dipping a hand form wearing a knitted- or woven-cloth liner into a glove
compound such as nitrile. The liner
supports the compound and adds
strength to the glove. Some supported
styles have continuous coatings to ensure protection from chemicals. Cotton
and polyester may be used in various
combinations as a yarn for woven or
knitted products, coated with various compounds including natural
latex, neoprene and PVC to protect
against petrochemicals, oils, acids, alcohols and solvents.
Supported gloves with non-continuous coatings are better suited
for applications that require comfort
and grip. Many supported gloves also
offer cut, snag, puncture and abrasion resistance.
Fabric gloves
Permeation is also color coded: red indicates breakthrough times of only a

few minutes; yellow indicates breakthrough times of up to two hours; and
blue indicates longer breakthrough times
This category includes general purpose gloves made with polyester,

nylon and cotton; cut-resistant gloves
constructed with Kevlar, Dyneema
and steel; stretch gloves made with
small percentages of natural latex and
Lycra yarns added to other fibers; and
special purpose gloves with materials, such as thermal foam or vibration
foam. Special purpose gloves include
extra clean gloves and sterile gloves.
General purpose gloves. Nylon,
polyester and cotton gloves are comfortable and protect against snags,
punctures, cuts and abrasion. They do
not, however, protect against chemicals and liquids, which is why chemically resistant gloves may need to be
worn as liners in some applications.
Nylon is an alternative fabric that
may be used in cleanrooms, automotive paint rooms and inspection stations where there is concern about
lint contamination.
Cut resistant gloves. Gloves made
with Kevlar typically provide the best
cut protection based on price, and
gloves made with Spectra or Dyneema
ultra-high-molecular-weight polyethylene typically offer the best cut protection based on weight. Steel assures
the best cut protection based on bulk.
None of these materials, however,
will protect the hands from liquids.
Liquid-protective cut-resistant gloves
need to be coated with a compound,
such as nitrile.
Stretch gloves. Most of todays fabric
gloves are made from knitted fabric
rather than woven fabric, because knits

have a natural tendency to stretch and
fit closely. Natural rubber latex is used
to make the least expensive additive
elastic yarn for making tighter-fitting
gloves and cuffs. Workers, who need a
tighter fit and know or suspect they
have a latex allergy, should consider
switching to gloves made with a synthetic alternative, such as spandex.
Special purpose gloves
Specialty gloves include those made

with thermal foam for protection from
heat or cold, vibration-absorbing foam
for workers handling power tools and
other vibrating machinery, or products
with radiation-absorbing additives
such as lead or bismuth. This category also includes extra-clean gloves
for electronics cleanrooms and sterile
gloves for pharmaceutical facilities.
Chemical Barriers
Descriptions of glove materials that

may be used with various chemicals
follow, with advantages and disadvantages listed. In addition, the Table above
summarizes some chemical-resistance
information. Gloves are listed below in
order, by degree of specialized use.
Natural rubber (latex)
Natural-rubber latex gloves (Figure 2)

are generally unsupported and available in many styles, including cleanroom and sterile styles. These gloves
provide excellent protection from bases,
alcohols, and dilute water solutions of
many chemicals, with fair protection
53
against aldehydes and ketones.
Advantages: Low in cost, good physical properties, good cut protection in
heavy duty styles1, excellent dexterity
Disadvantages: Poor protection
against oils, greases and organic compounds; risk of protein allergies. Some
manufacturers use shortcuts that result in a poor quality product
Polyvinyl chloride (PVC)
Gloves made with PVC are generally

available in heavy supported or lightweight disposable styles, and protect
against strong acids, strong bases,
salt solutions and some heavy organic
chemicals. Many PVC or vinyl gloves
offer good abrasion and cut resistance,
although some styles may be susceptible to cuts.
Advantages: Low in cost, fair physical properties, minimal risk of allergic reactions
Disadvantages: Organic solvents can
wash plasticizers out, leaving holes
in the glove polymer on the molecular
level that may allow rapid chemical
permeation; gloves from some manufacturers are poor quality
Nitrile (Buna, NBR)
Nitrile gloves (Figure 1) are generally available as disposable, mediumweight unsupported, or lightweight
supported styles. They protect against
oils and greases (including animal
fats), xylene, perchloroethylene and
aliphatic solvents. They also protect
against most agricultural pesticide
formulations, chemicals and biological components used in weapons, and
other chemicals.
Advantages: Low in cost, excellent
physical properties, good dexterity; excellent resistance to snags, punctures,
abrasions and cuts
Disadvantages: Poor protection
against many ketones, some aromatic chemicals, and medium-polar
compounds
Neoprene
Neoprene is available in disposable,

1. Products that provide cut resistance and cut
protection do not completely prevent or eliminate the potential for cuts or punctures, and
are not intended or tested to provide protection
against powered blades or other sharp or rotating equipment. Users are encouraged to always
use caution and care when handling sharp materials.
54
medium-weight unsupported,
medium-weight supported and
heavy supported styles. Neoprene protects against a broad
range of oils, oxidizing acids
(nitric and sulfuric), polar aromatics (phenol and aniline),
glycol ethers, oils, greases and
many other chemicals. Other
types of gloves may, however,
offer better protection against
some of these chemicals.
Advantages: Medium cost,
FIGURE 2. Natural-rubber latex gloves are availmedium physical properties, able in many styles and provide excellent protecmedium but broad-ranging tion from bases, alcohols and dilute water solutions of many chemicals
chemical resistance
Disadvantages: Less resistant to snags, punctures, abrasions and Disadvantages: Poor resistance to
cuts than nitrile or natural rubber
certain solvents, including ketones,
esters and amines; poor physical properties, extremely expensive
Butyl rubber
Butyl rubber is used only in mediumweight unsupported gloves (Figure 3). Sealed-film (laminate) gloves
Advantages: Dexterity and out- Laminate is one of the most chemistanding resistance to moderately cally resistant materials available
polar organic compounds, such as and protects against almost anyaniline and phenol, glycol ethers, thing, including most chemicals and
ketones and aldehydes
biological compounds used in weapDisadvantages: Poor protection ons. Gloves made with this material
against non-polar solvents, including are excellent for hazmat applications.
hydrocarbons, chloro- and fluoro-car- Laminate gloves are often used as
bons; expensive
liners, which takes advantage of their
thinness and is often the best way to
address their disadvantages.
Polyvinyl alcohol (PVA)
PVA is used for medium-weight sup- Advantages: Moderate cost; thin;
ported gloves that provide a high level outstanding resistance to almost all
of resistance to many organic chemi- organic compounds
cals, such as aliphatics, aromatics, Disadvantages: No grip finish, poor
chlorinated solvents, fluorocarbons physical properties (very low resisand most ketones (except acetone), es- tance to physical damage), not as
form-fitting as dipped gloves
ters and ethers.
Advantages: Very rugged and highly
chemical-resistant; good physical Chemical
properties with resistance to snags, Resistance Tests
punctures, abrasions and cuts
Chemical-resistant gloves are typiDisadvantages: Will quickly break cally tested for degradation, permedown when exposed to water and ation-breakthrough times, and final
light alcohols, less flexible than many permeation rates.
other types of chemically resistant
Degradation is a deleterious change
gloves, expensive
in the physical properties of a glove
due to the effects of a chemical. It is
commonly evaluated by measuring
Viton
This compound is used primarily in weight or dimension changes upon
medium-weight unsupported gloves to exposure. Currently, no widely used
protect against aromatics, chlorinated standard degradation test exists for
gloves, although several groups have
solvents, aliphatics and alcohols.
Advantages: Good dexterity, out- tried to converge on one. The problem
standing resistance to many organic is that during actual use, only the outside of a glove is exposed to chemicals,
compounds
wearers hands to higher temperatures than those used in testing,

which will make chemicals permeate more rapidly. Gloves will be
flexed and squeezed rather than
held in place in a test cell, which
will also make chemicals permeate more rapidly.
Gloves, however, are typically
FIGURE 3. Unsupported butyl
worn
to protect against possible
gloves offer dexterity and outsplashes not continuous liquid
standing resistance to moderately polar organic compounds
contact. Chemicals, therefore, will
permeate through more slowly
and it is difficult to test the outside of during actual use than in a standard
a multi-layer glove without having the permeation test. Breakthrough times
results distorted by the properties of and permeation rates from F 739,
therefore, should not be considered as
the inner layers.
Permeation is the process by which absolute constants. The data is usea chemical moves into and through ful only to compare gloves and obtain
a chemically resistant glove film by a general indication of how well they
adsorption on the outside, diffusion can be expected to perform.
through, and then desorption on the
inside. Measurements commonly tabu- ASTM F 739-07
lated include breakthrough time (how This is the newest version of ASTM
long after exposure the permeation F 739 and uses 27C as the standard
valve was opened) and permeation temperature since gloves are generrate (how wide it was opened).
ally warmer than room temperature
Both degradation and permeation during use. Much older data and Euresult from a chemical being absorbed ropean data were obtained at room
and diffused into the film. The amount temperature (21C). Europeans deof chemical absorbed and the rate of cided that a consistent established
transport, however, are independent method is more important than a
variables, which means that neither somewhat more realistic method,
property can be predicted based on which is why they continue to use
the test results for the other property. 21C as the test temperature. When
A simple degradation test, therefore, selecting gloves, it is important to
cannot be used to extrapolate the re- compare test data that were obtained
sults expected from a more complex at the same temperature.
and time-consuming permeation test.
ASTM F 739
This is the permeation test most commonly used and represents the original permeation standard, although a
substantial amount of data has been
accumulated since it was first issued.
European-standards writers adopted
ASTM F 739 with minor modifications as EN 388. During testing, permeation test cells are filled once and
remain filled. The results typically
provide the time delay until the chemical breaks through, and the flowrate
through the material, which increases
to a final constant value.
Method F 739 does not realistically
simulate most end uses for chemically
resistant gloves. During actual use,
gloves are likely to be warmed by the
ASTM F 1383
This test can be used to simulate intermittent contact applications, although

the test focuses on permeation only.
During F 1383 tests, permeation test
cells are filled and emptied repeatedly on a schedule developed to match
the intended end use. Air or nitrogen
is blown through the chemical compartment during the entire empty
cycle, with evaporation away from and
diffusion into the sample occurring
simultaneously. The ASTM F1383 Intermittent-Contact Permeation Test,
therefore, may provide a more realistic permeation measurement of realworld breakthrough times.
Breakthrough ratings indicate how
long a glove may be safely worn after a
splash occurs. Final permeation rates
show how much of a chemical permeates the glove barrier during continuous exposure. While lower ratings are
better, there is still no allowable skin
contact threshold limit value (TLV) for
any chemical. Most people who select
gloves tend to pay more attention to
the breakthrough time.
ConclusionS
Since the perfect glove does not exist

to protect workers in every chemical
application, gloves should be selected
that provide the appropriate level of
protection for the specific chemical
handled. Questions should be considered regarding the chemical concentration and length of exposure,
dexterity, tactile sensitivity and cut
protection required.
Many glove manufacturers offer
hand protection products that protect workers from a variety of chemicals. In general, natural rubber latex
is the least expensive alternative for
tight-fitting gloves that resist bases,
acids, alcohols and the diluted aqueous solutions of most chemicals.
Unsupported gloves offer a broad
spectrum of chemical resistance,
depending on the material used.
Supported styles are often used for
general purpose, chemical- or cutresistant requirements.

Notes
1. Kevlar is a registered trademark of Dupont.
Dyneema is a registered trademark of Royal
DSM, N.V. Lycra is a registered trademark of
Invista.
2. Neither this article nor any other statement
made herein by or on behalf of Ansell should
be construed as a warranty of merchantability or that any Ansell product is fit for
a particular purpose. Ansell assumes no responsibility for the suitability or adequacy of
an end users selection of gloves or clothing
for a specific indication. Upon request, Ansell
will provide a sample of material to aid you
in making your own selection to meet your
own individual safety requirements.
Author
Nelson Schlatter is a technical applications
chemist for Ansell Occupational Healthcare
(1300 Walnut St., Coshocton, OH 43812; Phone:
740-623-3591; Email: nschlatter@ansell.com;
Fax: 740-623-3556). He has worked with Ansell
for 30 years on the chemical interaction and processing of textiles, rubber and solvents. He presently answers technical inquiries and provides
recommendations regarding the proper use of
Ansell gloves and clothing. Schlatter holds a B.S.
degree from the University of Delaware. He is
an active member of ASTM Committee F-23 on
Protective Clothing and belongs to International
Safety Equipment Organization Committees on
hand protection and clothing.
55
Solids
Environmental
Processing
Manager
Dust Control in the

Chemical Processing
Industries
Figure 1.
The lack of proper
dust-control techniques can result in
catastrophic fires
and explosions in
many types of
facilities
Walter S. Kessler
Chilworth Technology, Inc.
ust in the chemical processing industries (CPI) is

present in numerous operations, including powder
processing; the transport of materials on belt or rotary-screw conveyors; grinding materials in giant
shredders and pulverizers; machining, sawing, grinding or sanding operations; dumping bags of materials
into reactors; handling coating materials; as well as the processing of
pharmaceuticals and foods. An integral industry-safety issue arises
when we consider the handling
and suppression of the dust and
particulate matter associated with
these processes, namely preventing the formation of combustible
clouds that can create a fire hazard
or even trigger an explosion. Such
a catastrophic dust explosion in a
manufacturing facility is depicted
in Figure 1. Additionally, protect-
ing workers from the dangers of

potentially dusty environments,
including contact irritations and inhalation exposure, is an important
factor in determining the methods and extent to which the particulate matter or dust needs to be
suppressed or eliminated.
Regulations
Dust hazards are so problematic

to employees that the U.S. Occupational Safety and Health Administration (OSHA; Washington D.C.;
www.osha.gov) has implemented
rules for personal protective equipment (PPE) specifically dust
masks and respirators, under standard 29CFR 1910.134 to protect
workers [1]. This standard states:
In the control of those occupational
diseases caused by breathing air
contaminated with harmful dusts,
fogs, fumes, mists, gases, smokes,
The prevention of dust

hazards in the CPI is
integral to process-safety
management widereaching mitigation
schemes must be
implemented
sprays or vapors, the primary objective shall be to prevent atmospheric
contamination. This shall be accomplished as far as feasible by accepted
engineering control measures (for
example, enclosure or confinement
of the operation, general and local
ventilation, and substitution of less
toxic materials). When effective engineering controls are not feasible,
or while they are being instituted,
appropriate respirators shall be
used pursuant to this section. It
goes on to state: A respirator shall
be provided to each employee when
such equipment is necessary to protect the health of such employee.
The employer shall provide the respirators, which are applicable and
suitable for the purpose intended.
The employer shall be responsible
for the establishment and maintenance of a respiratory protection
program. The program shall cover
each employee required by this section to use a respirator.
Additionally, the National Fire
Protection Association
(NFPA;
Quincy, Mass.; www.nfpa.org) has
stepped in and set consensus standards, based upon good engineering
practices, to control and prevent
combustible-dust related hazards.
NFPA 654 (Standard for the Prevention of Fire and Dust Explosions
from the Manufacturing, Processing and Handling of Combustible
Particulate Solids) applies to all
phases of the manufacture, processing, blending, pneumatic conveying,
repackaging and handling of combustible particulate solids or hybrid
mixtures, regardless of concentration or particle size, where the materials present a fire or explosion
hazard [2]. In addition to this standard, the NFPA has also set stan-
59
dards for specific industries and
processes, such as: NFPA 61 (Standard for the Prevention of Fires and
Dust Explosions in Agricultural and
Food Products Facilities), NFPA 484
(Standard for Combustible Metals) and NFPA 664 (Standard for
the Prevention of Fires and Explosions in Wood Processing and Working Facilities). These standards
hold, as a top priority, the action
of minimizing and controlling dust
and particulate matter in processing industries from both a fire- and
explosion-hazard safety standpoint.
In addition to the human-health
impact, combustible airborne dust
and particulates in the right environment where confinement, dispersion, concentration, oxidants and
ignition are present or potentially
present can create explosions.
Combustible dust, according to both
OSHA (CPL 03-00-008) and NFPA
654, is defined as a particulate solid
that presents a fire or deflagration
hazard when suspended in air or
some other oxidizing medium over a
range of concentrations, regardless
of particle size or shape. The most
common industrial sources of combustible dust include: food (such as
candy, sugar, spice, starch, flour and
feed), grain, tobacco, plastics, wood,
paper, pulp, rubber, textiles, pesticides, pharmaceuticals, dyes, coal,
metals (such as aluminum, chromium, iron, magnesium and zinc),
and fossil-fuel power generation [3].
When these dusts are ignited, they
can produce a fireball 810 times
larger than the original volume of
the cloud in the absence of confinement. Conversely, in a confined environment, explosive pressures can
increase to as high as 810 times
the original pressure.
Control measures
Every dust has unique physical and

chemical characteristics that impact
its level of hazard. Physical characteristics include size, shape and
moisture content, among others.
Chemical characteristics include
flammability or combustibility, explosibility, susceptibility to thermal
degradation and instability, susceptibility to ignition, and chemical re60
Figure 2. Even dust-mitigating equipment can be the source of explosion

hazards if not correctly installed and
maintained
activity. It should be noted that the

physical characteristics of the dust
also effect the chemical characteristics. For example, as particle size
and moisture content decrease, the
maximum explosion potential and
maximum rate of pressure rise per
unit time increases and the minimum ignition energy (MIE) generally decreases [4]. The dust-explosion hazardous classes (ST) range
from 0 (no explosion potential) to
3 (very strong explosion potential).
Testing of representative dust samples is the best method to classify
dust materials. Typically, the cost
of testing is recovered in reduced
engineering-control costs.
To control dust and particulate
matter, vacuum systems with various forms of filtrations and particleremoval devices have been designed
and installed in industry. The engineering and design behind some of
these systems can be very detailed
and intricate. The key to their design is to move the dust and air at
a velocity fast enough to keep the
dust or particulate matter suspended and moving inside of transport ductwork until they reach the
filter mechanism or cyclone separator. At this point, they are removed
from the air to an acceptable level
before the air is released back into
the facility or outside environment.
These mechanical air-purifying
systems are intended for removing dust and particulate matter. An
important aspect to their function,
besides proper design, is proper
maintenance specifically chang-
Figure 3. Extra care must be taken any

time personnel have direct contact with potentially combustible dusts or solids, for example,
when pouring a bag of reactant into a vessel
ing filters and keeping the system

clean. This ensures that dust and
particulate matter do not build up in
the equipment and cause a hazardous fire and explosion scenario; this
is the reason they were installed in
the first place. In addition to proper
design, the installation of explosionprotection (such as venting or suppression systems), explosion-isolation, and spark-detection systems
may be required, depending upon
the properties of the dust being collected. One might think this is obvious; however, systems installed to
mitigate dust and particulate matter have historically been involved
in fire and explosion incidents, as
seen in the dust-collector explosion
in Figure 2.
In some cases, dust is removed
through a wet-scrubbing arrangement where the dust or air stream
comes into intimate contact with
water, and the dust is removed from
the air stream. The dust may be
dissolved in the water or may create a slurry. In either case, this type
of collection requires further treatment of the water solution or sludge
for environmental purposes.
In addition to vacuum-bag or
filter systems, water and various
polymer-additive systems have also
been used to control dust, mainly in
coal, mining and dirt-road applications. These systems typically consist of a water-only, water-polymer
solution or oil-based liquid that is
laid down or sprayed onto a surface
by a nozzle-manifold or firehoselike system.
Avoiding incidents
Due to the number of incidents related to combustible dust there

have been 281 major events reported
from 19802005, which have killed
119 workers, injured another 718
workers, and destroyed many industrial facilities [3,5] OSHA reissued
its CPL 03-00-008 Combustible Dust
National Emphasis Program (NEP)
on March 11, 2008. Although OSHA
does not yet have its own standard
pertaining to combustible dust, the
agency cites combustible-dust hazards, including fire deflagration, explosion and related hazards under
the General Duty Act of 1970. This
act states that an employer shall
furnish to each of his employees employment and a place of employment
which are free from recognized hazards that are causing or are likely to
cause death or serious physical harm
to his or her employees [6], and relies
on NFPA standards for the recognition of such hazards. This includes
the statement that employers must
furnish each employee with a place
of employment that is free from recognized hazards that are causing, or
are likely to cause, death or serious
physical harm. In 20072009, OSHA
conducted approximately 1,100 combustible-dust inspections and issued
over 4,900 citations for both combustible-dust hazards and other safety
violations. From these violations, the
following list summarizes some of
the General Duty Violations issued
by the OSHA inspectors [7]:
Dust collectors were located
inside buildings that lacked
proper explosion-protection systems, including for venting and
suppression purposes
The rooms with excessive dust accumulations were not equipped
with explosion-relief venting distributed over the exterior walls
and roofs of the buildings
The horizontal surfaces, including
those on beams, ledges and screw
conveyors at elevated surfaces,
were not minimized to prevent accumulation of dust
Equipment, such as grinders,
shakers, mixers and ductwork,
were not maintained to minimize
escape of dust into the surround-
Figure 4. The dust explosion pentagon represents the conditions that can
lead to a catastrophic event
ing work area. This becomes especially problematic when employees may have direct contact with
powder or dusty materials, such
as when pouring bags into reactors or vessels (Figure 3). Also,
the employer did not prevent the
escape of dust from the packaging
equipment, creating a dust cloud
in the work area
Interior surfaces where dust accumulations could occur were not
designed or constructed to facilitate cleaning or to minimize combustible-dust accumulations. Regular cleaning frequencies were not
established for walls, floors and
horizontal surfaces, such as ducts,
pipes, hoods, ledges and beams
Compressed air was periodically
used to clean up the combustibledust accumulation in the presence
of ignition sources
Explosion vents on dust collectors and bucket elevators were
directed into work areas and not
vented to a safe, outside location away from platforms, means
of egress or other potentially
occupied areas
Process hazard analysis (PHA)
was not conducted to determine
whether the process hazards necessitated the installation of approved devices, such as explosionprotection systems, interlocked
rotary valves, deflagration vents
and flame-front diverters
The employer did not provide
adequate maintenance and design of dust-collector systems,
which created insufficient air aspirations, low duct velocities and
blocked ducts
Even with OSHA implementing the
NEP program, combustible-dust
related incidents continue to be a
major industrial problem in the U.S.
and globally. There were over 500
combustible-dust related incidents

reported in 2011 in the U.S. alone
[8]. That number does not include
the events associated with grain elevators or coal-fired power plants, or
smaller flash fires that were quickly
extinguished, as well as other nearmisses that failed to be reported.
From the above list, some good
rules of thumb and generally accepted good engineering practices for facilities that contain
dust and particulate matter from
production are [9]:
Implement appropriate engineering designs and controls to minimize the presence of dust and to
prevent the dust explosion pentagon (Figure 4) from occurring
Perform
manufacturer-recommended maintenance on all equipment to ensure that it is functioning as designed
Implement good housekeeping
practices, including using surfaces
that minimize dust accumulation,
periodic inspections for hidden
areas of dust accumulation and
controlling sources that could
cause dust to become airborne
to maintain a clean, dust-free
working environment
Follow other measures, including:
bonding of equipment to ground
to control static electricity; controlling smoking and sources of
open flames and sparks; managing friction and other sources for
mechanical sparks
Provide hazard recognition training for employees per OSHA
3371-08 2009
Establish overall safe work practices, such as proper electricalarea classifications, physical barriers for the hazard, cleaning that
does not generate dust clouds
and locating relief valves away
from dust
Report and record any and all
incidents or near-misses, as
they are a valuable tool and resource for preventing larger, more
serious incidents
With all these recommendations,
regulations, reported incidents
and near-misses, facilities should
strongly consider use of competent personnel and knowledge-
61
able individuals to provide testing,
hazard assessments, risk analysis
studies and engineered solutions
to minimize or control dangerous dusts and particulate matter
in manufacturing.
To achieve process-safety excellence, employees must be genuinely
proficient and competent in their
requisite technical disciplines, and
appropriate levels of knowledge
must be embedded in key positions
throughout an organization with

a mechanism for longevity. Or, put
more simply, organizations must
have the right people, with the
right skills, implementing appropriately designed process-safety programs, motivated by the right organizational culture, in the right way.
Results are far-reaching and broad,
affecting finances, the environment
and most of all, workforce safety.
Properly managing dust protects
References
5. U.S. Chemical Safety and Hazard Investigation Board, Investigation Report: Combustible Dust Hazard Study, Report No. 2006-H-1,
November 2006.
6. OSHA General Duty Act of 1970, Sec. 5
Duties, 1970.
7. OSHA Status Report on Combustible Dust
NEP, October 2009.
8. National Fire Incident Reporting System.
(NFIRS) Combustible Dust Policy Institute,
2011 Combustible Dust Related Incidents
Fact Sheet, April 2013.
9. OSHA, Combustible Dust in Industry: Preventing and Mitigating the Effects of Fire
and Explosions, SHIB 07-31-2005.
1. OSHA Standard 1910: Personal Protective

Equipment, 19982011.
2. NFPA 654: Standard for the Prevention of
Fire and Dust Explosions from the Manufacturing, Processing and Handling of Combustible Particulate Solids, 2013.
3. OSHA, Combustible Dust: an Explosion Hazard, OSHA website, https://www.osha.gov/
dsg/combustibledust.
4. Amyotte, P., An Introduction to Dust Explosions: Understanding the Myths and Realities of Dust Explosions for a Safer Workplace, Elsevier, 2013.
the workforce, facility and the environment, while maintaining stakeholder confidence and encouraging
compliance with all legislation and
avoiding regulatory intervention.
Eliminating or minimizing dust is
a small investment compared to the
costs of the harm that can occur if
not appropriately addressed.
Edited by Mary Page Bailey
Author
Walter S. Kessler is a senior process engineer and
safety specialist at Chilworth
Technology, Inc., a DEKRA
Company (113 Campus Drive,
Princeton, N.J. 08540; Phone:
609-799-4449; Email: walter.
kessler@dekra.com). He has
20 years of experience in process design, development and
improvement, process control,
logic-controller programming,
process-hazard analysis, layers-of-protection
analysis (LOPA), safety-integrity levels (SIL)
and process safety management in petroleum
refineries, gas and chemical plants, as well as
pharmaceutical, manufacturing and wastewater
facilities. Kessler holds a B.S.Ch.E. from Pennsylvania State University and is currently obtaining a Ph.D. at the University of Houston.
The Chemical Engineering bookstore

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63
Solids
Environmental
Processing
Manager
Avoiding Static Sparks

In Hazardous Atmospheres
Relatively simple steps can be taken to mitigate risks
associated with static electricity in process plants
Graham Tyers, Newson Gale Inc.
e are all familiar with the

effects of static electricity in
everyday life the sharp
spark we experience as we
approach a metal file cabinet or the
crackle we feel as we remove a garment
made of synthetic material. While these
effects are largely harmless, in the
chemical process industries (CPI),
whenever flammable or combustible
atmospheres are present, uncontrolled
discharges of static electricity can be
potentially disastrous.
The National Fire Protection Assn.
(NFPA; Quincy, Mass.; www.nfpa.org)
tracks the causes of all industrial
fires and explosions reported to U.S.
fire departments. Roughly 280 incidents/year in the U.S. are attributed
to static electricity, and these result
in significant damage to property, lost
production, injuries and even fatalities. According to the U.K. Institute
of Chemical Engineers, roughly 350
incidents per year are caused by static
electricity. And this figure is probably
conservative, as more such incidents
likely occur but go unreported, or do
not have an electrostatic cause substantiated during the investigation.
Case in point
One major industrial fire at a totefilling operation at a chemical distribution facility in Des Moines, Iowa,
was investigated in 2008 by the U.S.
Chemical Safety Board (CSB; Washington, D.C.; csb.gov), and the cause
was determined to be static electricity.
(the full report is available at csb.gov).
CSB concluded that a combination of
technical and procedural factors led to
an uncontrolled static discharge, which
created a fire that spread rapidly to a
wood-framed warehouse, igniting a
large volume of flammable and com44
Figure 1. Many self-testing groundbustible liquids. One employee and

ing clamps also monitor cable condione firefighter were injured. The main tion back to the designed ground point,
warehouse structure was destroyed,
and will alert the operator if the cable
the operators business was signifihas worked itself loose or is broken
cantly interrupted, and surrounding
businesses were evacuated.
tance of the object, this may result in
significant levels of energy being available for discharge well above the
Best practices
Anyone responsible for, or working minimum ignition energy (MIE) of the
in, potentially explosive atmospheres surrounding flammable atmosphere.
(Class I, II or III) is aware of the fact Typical MIE values (Table 1) vary acthat all potential sources of ignition, cording to whether the flammable atincluding naked flames, hot surfaces mosphere comprises vapor, dust or gas,
and electrical sparking must be elimi- but many commonly used solvents and
nated. Today, a variety of safety codes other flammable chemicals have MIEs
and guidelines (discussed below) spec- that are relatively low on the order
ify safe working practices in hazardous of 1 mJ or less. If the isolated conducareas, and provide specific guidance tor then comes into proximity with another object at a lower potential, much
on how to control static electricity.
The risk of static electricity is ever- of this energy could be released in the
present, as it is generated continu- form of an incendive spark.
Of course, in order for there to be
ously, whenever surfaces come into
contact and then separate. Examples static ignition of the flammable atmoinclude liquids flowing through pipe- sphere, there would need to also be a
lines or filling into drums and tanks, suitable concentration of fuel (vapor,
powder dropping down a chute, and dust or gas) in air, but for the purposes
even a person walking across an insu- of safe plant design, the very fact that
there is an identified flammable atmolating floor.
The extent of charge generation in sphere should suggest that this is posindustrial processes is usually very sible or likely.
Despite these potential hazards, the
low, typically no greater than 1
104 Amp. However, these generated danger associated with static electriccharges become a problem in hazard- ity can be effectively mitigated by folous areas when allowed to accumu- lowing national and industry codes
late on objects that are not at ground of practice, technical standards, and
(earth) potential. Unfortunately, many working practices such as NFPA
of today's paints, coatings, gaskets, 77 (Recommended Practice on Static
seals and other non-conductive mate- Electricity), and NFPA 30 (Flammable
rials are sufficiently insulating so and Combustible Liquids Code) that
they actually prevent the proper dis- specify proper grounding and bonding
techniques. Such techniques work on
sipation of static charge.
Without proper engineering and the assumption that if a) conductive
worker training, charges can quickly or static-dissipative plant, equipment
build up to a very high potential, with and materials are used, and b) these
voltages in excess of 30 kV not being materials are properly bonded and
uncommon. Depending on the capaci- grounded, it will be impossible for
Chemical Engineering www.che.com JUNE 2009
Table 1. Typical MIE values

Material
(gas/vapor or
powder/dust)
Carbon disulfide
Methanol
Xylene
Toluene
Propane
Ethyl acetate
Zirconium
Epoxy resin
Aluminum
Sugar
Wheat flour
Minimum
Ignition Energy
(MIE), mJ
0.009
0.14
0.20
0.24
0.25
0.46
5.00
9.00
10.00
30.00
50.00
Note 1: Minimum ignition energy (MIE) is defined

as the minimum energy that can ignite a mixture
of a specified flammable material with air or oxygen, measured by a standard procedure.
Note 2: MIE values are provided for guidance
only specific MIE data for any material
should be verified.
Source: NFPA, IchemE
dangerous levels of static electricity

to accumulate and result in an uncontrolled discharge.
NFPA 77 and NFPA 30 are extremely useful, in that they provide
practical examples of common operations, and detail effective ways
to eliminate, control or mitigate the
problem. Where today's recommendations tend to converge is in the recommendation to always use conductive or
static dissipative materials, and to ensure effective bonding and grounding.
In this context, the term conductive
would apply to metal materials, such
as stainless or carbon steel, aluminum and others, and static-dissipative may indicate rubber or plastics
that have been formulated with some
added semi-conductive additives.
Bonding means linking these objects together by means of a suitably
strong conductor (wire), and grounding refers to a true ground/earth
connection that is applied to one or
more of the bonded objects. When one
or both of these techniques is applied,
and while a low resistance connection
between the objects and ground is
maintained, operators are able to prevent dangerous levels of static charge
from accumulating.
Hidden dangers
In any type of flammable atmosphere

there may be hidden dangers lurking
in the form of so-called isolated conductors. These are conductive objects that
are either inherently or accidentally
insulated from earth. The insulation
effectively keeps any static electricity buildup from safely discharging,
thereby resulting in accumulation of
charge on the object.
Isolated conductors may arise from
Figure 2. FM/ATEXapproved grounding

clamps, when properly
bonded and grounded,
can control static
buildup
Figure 3. Static ground-verification and interlock

systems are essential for certain critical applications
such as loading/unloading tanker trucks and rail cars,
IBCs, fluid bed dryers, mixers, transfer equipment and
other process equipment that have a high explosion
potential, applications with a high likelihood of static
charge accumulation in a very-low-MIE flammable atmosphere, and situations in which low-conductivity liquids
or highly resistive powders are being handled
metal flanges, fittings or valves in

pipework systems; portable drums,
containers or vessels; tanker trucks,
rail cars and intermediate bulk containers (IBCs); and even people. During day-to-day operations at industrial
facilities, isolated conductors are probably the most likely source of static ignition incidents.
Fortunately, the problems associated with isolated conductors can be
remedied by effective grounding and
bonding. In the case of fixed installations such as pipe work, storage tanks
and so forth, this is relatively simple
to implement. However, these preventive measures are more difficult to implement with mobile/portable objects,
such as drums, IBCs and tankers. In
these instances, purpose-designed
temporary grounding and bonding devices must be used, with strict procedures to ensure that they are always
in place prior to starting the process.
For instance, specific types of
clamps and devices for grounding
and bonding portable or mobile plant
equipment, drums and containers are
recommended in NFPA 77, and such
grounding clamps and devices generally should employ sharp contact
points. These contact points should
be made of a wear-resistant material,
have positive spring pressure, and be
universally adaptable to a wide range
of plant objects.
In some cases, these grounding
clamps and devices may have additional third-party notified-body testing such as Factory Mutual (FM) or
the European ATEX Directive (Figure
2). If these units are properly specified
and correctly used, in most cases the
user can be reasonably sure of effective static control.
In all situations it is also important to periodically test the control

measures used, to check the condition
of the clamp, contact and cable, and
to verify the all-important connection back to the grounding point (bus
bar). Instruments like Ohm testers or
multi-meters are useful for performing such verifications, but, of course,
these will need to be approved as intrinsically safe instruments if you are
working live in a hazardous area.
According to the recommendations
in the latest edition of NFPA 77, the
maximum resistance to ground in
conductive (metal) bonding systems
should be tested to 10 Ohms or less.
With all-metal systems and tight connections, it should be easy to achieve
this level of resistance to ground.
While higher resistance levels may
be theoretically low enough for static
charge removal from conductive objects, resistance levels higher than
two-digit figures in all-metal systems
usually indicate problems, such as corrosion, loose or broken connections or
a buildup of coating or insulating materials somewhere in the system. Any
such readings should be immediately
investigated and rectified.
The presence of semi-conductive or
so-called static-dissipative materials
may also exhibit higher resistance
levels, owing to their varying characteristics (which in some cases may be
as high as 1 108 Ohms).
Additional considerations
Even when the appropriate static

safety equipment has been specified,
there are some further concerns that
must be addressed by all those responsible for operations within hazardous
areas. In operational terms, attaching
45
a grounding clamp to a plant obRecommended
ject is always a physical action.
resources
Thus, there is always a risk that
Useful
guidance
on minimizing fire and
even if operators diligently carries
explosion hazards, and managing static
out their duties per the companyelectricity in process plants, can be found
recommended safety procedures,
at these websites.
no one can ever be sure that the
NFPA77, NFPA30
www.nfpa.org
clamp has made good enough
Chemical Safety Board
www.csb.gov
contact with the object. For inIchemE
www.icheme.org
stance, the clamp has to make
OSHA
www.osha.gov
a low enough resistance contact
with the conductive object to enable any static that is generated to be forming its intended function of safely
safely dissipated to ground before it dissipating any static electricity that
is generated.
can accumulate to dangerous levels.
These specialized clamps employ
The fact remains that many conductive objects that are capable of accumu- intrinsically safe electronic monitorlating high static charges also have in- ing circuits that are powered from a
sulating layers on their surfaces, which low-energy battery. The circuit is only
may prevent this low resistance con- completed when the clamp achieves
tact. Examples include paints and coat- a low resistance contact onto the obings on drums, tank vehicles and other ject to be grounded, and the operator
mobile plant equipment, or product receives visual confirmation of this
buildup caused by normal working con- via a light/indicator (usually a flashditions (for instance where insulating ing LED). The self-testing grounding
liquids, powders and other materials clamp also monitors cable condition
are part of the operation or process). As back to the designed ground point,
a result, many grounding and bonding and will also fail to register a permisclamps show very high resistance read- sive signal if the cable has worked
ings when clamped to conductive objects itself loose or is broken (Figure 1). In
with insulating surfaces. Worse still, if order to be safely used in hazardous
the company tries to cut costs by using locations, these clamps should be apstandard welding clamps or lightweight proved as intrinsically safe devices
alligator clips for static grounding and carry the appropriate Hazardous
(instead of purpose-designed clamps), Area Certification, for instance, from
these devices have an even higher Factory Mutual (FM), Underwriters
failure rate with potentially grave Laboratories (UL), or the Canadian
Standards Authority (CSA).
consequences.
To move to an even higher level of
During an internal audit (using an
approved Ohm meter) of ground con- security, static ground verification sysnections in its flammable-liquids area, tems are available that not only give
one major chemical company actually visual verification to the operator, but
determined that only 85% of the de- that provide interlock switching convices had acceptable low resistance tacts that may be linked to process
levels, or proper ground. Therefore, pumps, valves, alarm/shutdown/con15% of their ground connections failed trol systems, as well. This means that
to meet the proper levels, and as a re- the process cannot be started until
sult were at risk to the process area the conductive object has been safely
grounded, and, if at any time during the
and operating personnel.
To solve this problem, NFPA 77 sug- operation the condition changes (due to
gests that intrinsically safe, self-check- a clamp falling off or wire breaking for
ing grounding and bonding clamps be instance), the system automatically
used. From an operators point of view, switches to the non-permissive state
these devices are employed in exactly and shuts down the process.
Systems employing interlocks can
the same way as conventional grounding clamps. Where they differ is in also prevent accidents that would oththe way that they reassure the opera- erwise result when operators approach
tor that the clamp has not only been plant objects that are already carrying
physically attached, but is also per- accumulated static charges. In this
46
Figure 4. If staticdissipative footwear is

specified, it can also
be tested for ongoing
effectiveness using
test stations that test
the ground leakage
from the individual,
via the footwear, to
ground. These devices
help prevent incorrect shoes from being
used in static-sensitive environments
case, the process cannot be initiated

until proper grounding is established,
thereby ensuring that any generated
static electricity is safely dissipated to
ground. These systems are generally
fed from a line feed 110/120-V a.c.
power supply, and employ approved
intrinsically safe barriers to limit the
monitoring circuit down to safe levels.
They must also have proper hazardous location and safety certification.
Static ground-verification and interlock systems are typically used in critical/ultra-safety applications, such as
loading/unloading tanker trucks and
rail cars, IBCs, fluid bed dryers, mixers,
transfer equipment and special process
machines that have a high explosion
potential. They are also useful wherever there is a high likelihood of static
charge accumulation in very low MIE
flammable atmospheres, or where lowconductivity liquids or highly resistive
powders are being handled (Figure 3).
Static ground-verification clamps
and interlock systems also tend to
have an important beneficial effect
on the operators using them. Since
they build an additional check into
the operation, their use helps to reinforce the static safety procedures of
the company in short, the operator
is more likely to observe the correct
procedures, as he or she is kept aware
of the need to properly control static
electricity on a daily basis.
One final element of the static safety
audit is the static accumulating characteristics of people working in the
hazardous area. If the human body is
insulated from natural contact with
the ground, either by non-conducting
shoes, insulating floors or both, then
static charge can start to accumulate
as the person walks along the floor.
After just a few steps, a fairly high po(Continues on p. 49)
Avoiding Static Sparks In Hazardous Atmospheres (Cont. from p. 46)
tential may develop (especially in dry,
low-humidity atmospheres).
If the person now approaches a conductive material at either ground or a
lower electrical potential, a spark may
be promoted. It is generally thought
that sparks from people can reach energies as high as 30 mJ sufficient
to ignite almost all flammable vapors
and gases, and many sensitive combustible powder (dust) atmospheres.
In order to control this, it is necessary to ground the employees working
in sensitive hazardous areas. This can
take the form of ground wrist-straps
for sedentary workers, or specialized
static-dissipative (SD) safety shoes for
personnel who need to move around to
carry out their tasks. In the case of the
latter, it is also necessary for the floor
materials to be sufficiently conducting to allow a ground leakage path
to safely dissipate any static charge as
each foot contacts the ground.
In the U.S., SD footwear is manufactured according to ASTM F2413-05,
which specifies maximum and minimum levels for ground leakage via the
shoe. According to ASTM, it should be
sufficiently low to allow static charges
to be safely dissipated to ground, but

sufficiently high to afford some protection against electric shock. If SD
footwear is specified, it can be tested
for ongoing effectiveness using test
stations that test the ground leakage
from the individual, via the footwear, to
ground. These devices help prevent incorrect shoes from being used in staticsensitive environments (Figure 4).
In general, proper mitigation of
static electricity risk in hazardous
areas demands a holistic approach to
plant, process and personnel safety.
Any multi-part control program is
only as good as the weakest link in the
chain. As the speed and scale of modern manufacturing and distribution
techniques increase, and the range of
materials used and processed grows,
this basic approach to safety will become even more important.
More detailed information on this
subject may be found in industry
safety guidelines, such as NFPA 77,
and OSHA Regulations, Section 1910,
which provide safety managers with
practical guidance for specific situations. It is also important to remember
that proper grounding and bonding may
not be enough on their own to ensure
completely safe operations. Depending
on the materials involved it may some-
times be necessary to also employ other

protection measures like static charge
neutralization, inert gas blanketing (to
remove the flammable atmosphere),
and to look at process related ways to
minimize charge generation and maximize charge dissipation rates.
Controlling static electricity in hazardous areas may be simple in theory,
but in practice requires a thorough
knowledge of processes and operations,
sound engineering controls, properly
specified safety equipment and properly trained operational staff.
Author
Graham Tyers is president
of Newson Gale Inc. (www.
newson-gale.com), a manufacturer of static control equipment for hazardous areas (460
Faraday Ave., Unit B, Suite 1,
Jackson, NJ 08527). He has
worked in the specialist field
of electrostatic control and
hazardous atmospheres for
nearly 20 years. His industry
background is in monitoring
and control systems, and general electrical equipment for potentially explosive atmospheres. Tyers
is a member of the NFPA, ESDA, and ISA. He regularly conducts training and presents to industry
and safety groups on the subject of static electricity and hazardous areas. In addition to his technical subject background, he holds a Diploma in
Business Management (Open University, United
Kingdom). As part of the management team of
Newson Gale in the U.K., Graham was awarded
the Queens Award for Enterprise in 2005. He now
heads up Newson Gales North American Operations, based in New Jersey.
49
Feature Report
Piping Design for

Hazardous Fluid Service
William M. Huitt
W.M. Huitt Co.
ncorporating fire safety into plant

design takes on two fundamental
goals: to prevent the occurrence
of fire and to protect the initially
uninvolved piping and equipment
long enough for operations personnel to perform their duties and for
emergency responders to get the fire
under control. While it is impractical
to completely eliminate the potential
risk of an accidental fire in a complex
process-plant facility that is expected
to handle and process hazardous
chemicals, it is reasonable to assume
that certain aspects of design can be
incorporated to reduce that risk.
Designing facilities that use and
store hazardous chemicals requires
a demanding set of requirements, at
times beyond what can practically be
written into industry codes and standards. It is ultimately the responsibility of the engineer of record (EOR)
and the owner to fill in those blanks
and to read between the lines of the
adopted codes and standards to create a safe operating environment,
one that minimizes the opportunity
for fire and its uncontrolled spread
and damage.
This article will not delve into the
various trigger mechanisms of how a
fire might get started in a process facility, but will instead discuss containment and control of the fuel component
of a fire that resides in piping systems
that contain combustible, explosive or
flammable fluids.
In the design of piping systems containing such fluids, there are critical
aspects that need additional considerations beyond those involved in the
design of piping systems containing
non-hazardous fluids. There are two
key safety aspects that need to be
incorporated into the design, namely
system integrity and fire safety.
36
Extra considerations and precautions are needed

beyond the requirements of codes and standards
System integrity
System integrity describes an expectation of engineering that is integrated

into the design of a piping system in
which the selected material of construction (MOC), system joint design,
valve selection, examination requirements, design, and installation have
all been engineered and performed in a
manner that instills the proper degree
of integrity into a piping system. While
this approach is certainly needed for
the piping design of so-called normal
fluid service it is absolutely critical for
hazardous fluid systems.
The design of any piping system, hazardous or non-hazardous, is based, in
large part, on regulations and industry
accepted standards published by such
organizations as the American Society of Mechanical Engineers (ASME)
and the American Petroleum Institute
(API). The standards published by
these organizations include tables that
establish joint-pressure ratings based
on MOC and temperature. Where the
joint-design consideration for hazardous fluid services departs from that of
non-hazardous fluid services is in gasket and seal material specifications.
This is due to the need for sealing
material to contain hazardous chemicals for as long as possible while surrounded by a fire or in close proximity
to a fire. The effect of heat from a fire on
an otherwise uninvolved piping system
can only be delayed for a relatively short
period of time. And the first thing to fail
will be the mechanical type joints.
Depending on the type of fire and
whether the piping is directly in the
fire or in close proximity, the window of
opportunity, prior to joint seal failure,
for an emergency response team to get
Chemical Engineering www.che.com June 2010
the fire under control is anywhere from

a few hours to less than 30 minutes. As
you will see, a number of factors dictate
the extent of that duration in time.
A system in which the gasket material is selected on the basis of material
compatibility, design pressure, and
design temperature may only require
a solid fluoropolymer. In a fire, this
non-metallic material would readily
melt, allowing the contents of the pipe
to discharge from the joint once sealed
by the gasket. Specifying a gasket that
is better suited to hold up in a fire for
a longer period of time gives the emergency responders time to bring the initial fire under control, making it quite
possible to avoid a major catastrophe.
Fire-safe system
Preventing the potential for a fire

requires operational due diligence
as well as a proper piping-material
specification. However, controlling
and restricting the spread of fire
goes beyond that. Results of the assessment reports of catastrophic
events coming from the U. S. Chemical Safety and Hazard Investigation
Board (CSB; Washington, D.C.) have
shown that many of the occurrences
of catastrophic incidents have actually played out through a complex
set of circumstances resulting from
design flaws, instrumentation problems, pipe modifications, inadequate
fire-proofing and human error.
Events, such as a fire, are not necessarily then the result of a hazardous
fluid simply escaping through a leaky
joint and then coming into contact with
an ignition source. There are usually a
complex set of events leading up to a
fire incident. Its subsequent spread,
Incident No. 1
Valero-McKee Refinery,
Sunray, Tex., Feb. 16, 2007
ithout going into great detail as to the circumstances that led up to this incident, piping
handling liquid propane in a propane deasphalting (PDA) unit ruptured. The location of the rupture was in a section of isolated piping that had been
abandoned in place several years prior. A valve, intended to isolate the active flow of liquid propane from
the abandoned-in-place piping, had been unknowing left partially open due to an obstruction inside the
valve. Water had gradually seeped in past the valve
seat over the years and being heavier than the liquid Figure 1.
propane, settled at a low-point control station where
it eventually froze during a cold period. The expanding ice inside the pipeline subsequently cracked the
pipe. When the temperature outside began to warm,
the ice thawed allowing liquid propane to escape
from the active pipeline, through the partially closed
valve, and out the now substantial crack. The resultant cloud of propane gas drifted toward a boiler
house where it found an ignition source. The flame of
the ignited gas cloud tracked back toward its source
where the impending shockwave from the explosion
ripped apart piping attached to the PDA extractor
columns causing ignited propane to erupt from one
of the now opened nozzles on the column at such a
velocity as to create a jet fire.
The ensuing jet fire, which is a blow-torch like Figure 2.
flame, discharged toward a main pipe rack approximately 77 ft away, engulfing the pipe rack in the jet fire. As the
temperature of the non-fire-proofed structural steel of the pipe rack
reached its plastic range and began to collapse in on itself, the
piping in the rack, which contained additional flammable liquids,
collapsed along with it (Figure 1).
Due to the loss of support and the effect of the heat, the pipes in
the pipe rack, unable to support its own weight, began to sag. The
allowable bending load eventually being exceeded from the force
of its unsupported weight, the rack piping ruptured spilling its flammable contents into the already catastrophic fire. The contents of
the ruptured piping, adding more fuel to the fire, caused the flames
to erupt into giant fireballs and thick black smoke.
The non-fire-proofed support steel (seen on the left in Figure 1
and on the right in Figure 2) was actually in compliance with API
recommendations. Those recommendations can be found in Publication 2218 Fireproofing Practices in Petroleum and Petrochemical Processing Plants; API Publications 2510 Design and
Construction of LPG Installations; and 2510A Fire-Protection
into a possible catastrophic event, can

then be the result of inadequate design requirements that extend beyond
the piping itself.
While this discussion touches only
on piping issues, know that this is
only a part of the overall integration
of safety into the design of a facility
that handles hazardous fluids. What
follows are recommended piping design considerations that are intended
to substantially reduce the risk of
the onset of fire and its uncontrollable spread throughout a facility. In
discussing the spread of fire, it will
be necessary to include discussion regarding the needs for disciplines other
A collapsed pipe rack as a result of heat from a jet flame
The same collapsed pipe rack as Figure 1 seen from above
Considerations for the Design and Operation of Liquefied Petroleum Gas (LPG) Storage Facilities. In these issues of the publications it was recommended that pipe-rack support steel within 50 ft
of an LPG vessel be fire proofed. The collapsed support steel was
approximately 77 ft from the extractor columns, which is beyond
the 50-ft recommended distance.
While the EOR was in compliance with the governing code, with
regard to fire proofing, there may have been a degree of complacency in defaulting to that minimum requirement. This goes back
to a point made earlier in which it was said that industry standards
are not intended to be design manuals. They instead provide,
the minimum requirements necessary to integrate safety into the
design, fabrication, inspection, installation, and testing of piping systems Proprietary circumstances make it the imperative
responsibility of the EOR or the owner to make risk assessments
based on specific design conditions and go beyond the minimum
requirements of an industry code or standard when the assessment
results and good engineering practices dictate.
than piping, namely fire proofing of

structural steel.
General codes and standards
From a fire-safety standpoint, some

requirements and industry regulations are stipulated in the International Fire Code (IFC), published by
the International Code Conference
(ICC) under IFC 3403.2.6.6. There are
also requirements by the National Fire
Protection Assn. (NFPA) under NFPA
1 and NFPA 30. Test requirements for
fire-rated valves can be found under
API 607 Fire Test for Soft Seated
Quarter Turn Valves. Starting with
the 4th edition of this API standard,
it was added that, among other things,

the tested valve has to be operated
from fully closed to fully open after
the fire test. Prior to the 4th edition
a soft-seated fire-rated valve had to
only remain sealed when exposed to
fire without having to be operated, or
rotated. Additional fire test requirements can be found as published by the
BSI Group (formerly known as British
Standards Institution) as BS-6755-2
Testing of Valves. Specification for
Fire Type-Testing Requirements, and
FM Global FM-7440 Approval Standard for Firesafe Valves.
With exception to the specific requirements covered in the valve test-
37
Feature Report
ing standards, the codes and standards
mentioned above provide generalized
requirements that touch on such key
aspects of safety as relative equipment location, mass volume versus
risk, electrical classifications, valving,
and so on. They cannot, and they are
not intended to provide criteria and
safeguards for every conceivable situation. Designing safety into a particular
piping system containing a hazardous
liquid goes beyond what should be expected from an industry-wide code or
standard and falls to the responsibility of the owner or EOR. As ASME
B31.3 states in its introduction, The
designer is cautioned that the code is
not a design handbook; it does not do
away with the need for the designer or
for competent engineering judgment.
When designing piping systems to
carry hazardous liquids, the design
basis of a project or an established
protocol for maintenance needs to
incorporate a mitigation strategy
against two worse-case scenarios: (a)
A leak at a pipe joint containing a
hazardous liquid, and (b) The rupture
or loss of containment, during a fire,
of surrounding hazardous piping systems, not otherwise compromised that
would add fuel to the fire.
The occurrence of those two failures, one initiating the incident and
the other perpetuating and sustaining the incident, can be minimized or
eliminated by creating a design basis
that provides the following:
Added assurance against the potential for joint failure
Added assurance of containment
and control of a hazardous liquid
during a fire
Safe evacuation of a hazardous liquid from the operating unit under
distress
Fire prevention through design
Piping joints. When designing piping systems to contain hazardous liquids, one of the key objectives for the
design engineer should be taking the
necessary steps to minimize the threat
of a leak, steps beyond those typically
necessary in complying with the minimum requirements of a code. There are
certainly other design issues that warrant consideration, and they will be
touched on much later. However, while
38
PTFE
envelope
Primary
sealing
element
Profiled
inner ring
Monel*
windings
Secondary
sealing element
Flexible
graphite filler
* Monel is a registered trademark of international Nickel
the pipe, valves, and instrumentation

all have to meet the usual criteria of
material compatibility, pressure, and
temperature requirements there are
added concerns and cautions that need
to be addressed.
Those concerns and cautions are
related to the added assurance that
hazardous liquids will stay contained
within their piping system during
normal operation and for a period of
time during a fire as expressed in such
standards as API-607, FM-7440, and
BS-6755-2. Designing a system, start
to finish, with the intent to minimize
or eliminate altogether the potential
for a hazardous chemical leak will
greatly help in reducing the risk of fire.
If there is no fuel source there is no
fire. In the design of a piping system,
leak prevention begins with an assessment of the piping and valve joints.
There are specified minimum requirements for component ratings,
examination, inspection, and testing
that are required for all fluid services.
Beyond that, there is no guidance
given for fire safety with regard to the
piping code other than a statement in
B31.3 Para. F323.1 in which it states,
in part: The following are some general considerations that should be
evaluated when selecting and applying
materials in piping: (a) the possibility
of exposure of the piping to fire and
the melting point, degradation temperature, loss of strength at elevated
temperature, and combustibility of the
piping material under such exposure,
(b) the susceptibility to brittle failure
or failure from thermal shock of the
piping material when exposed to fire
or to fire-fighting measures, and possible hazards from fragmentation of the
material in the event of failure, (c) the
ability of thermal insulation to protect
piping against failure under fire exposure (for example, its stability, fire resistance, and ability to remain in place
during a fire).
The code does not go into specifics on
this matter. It is the engineers respon-
Carbon steel
outer ring
Figure 3. If flanged
joints are necessary, it is
suggested that fire-safe
spiral-wound type gaskets with graphite filler
be specified
sibility to raise the compliance-level

requirements to a higher degree where
added safety is warranted and to define
the compliance criteria in doing so.
Joints in a piping system are its
weak points. All joints, except for the
full penetration buttweld, will de-rate
a piping system to a pre-determined
or calculated value based on the type
of joint. This applies to pipe longitudinal weld seams, circumferential welds,
flange joints and valve joints such as
the body seal, stem packing, and bonnet seal, as well as the valve seat.
For manufactured longitudinal weld
seams, refer to ASME B31.3 Table
A-1B for quality factors (E) of the
various types of welds used to manufacture welded pipe. The quality factor
is a rating value, as a percentage, of
the strength value of the longitudinal
weld in welded pipe. It is used in wall
thickness calculations as in the following equations for straight pipe under
internal pressure:

(1)

(2)
Where:
c = sum of mechanical allowances
D = outside dia. of pipe
d = inside dia. of pipe
E = quality factor from Table A-1A
and A-1B
P = internal design gage pressure
S = stress value for material from
Table A-1
t = pressure design thickness
W = weld-joint strength-reduction
factor
y = coefficient from Table 304.1.1
Also found in Para. 304 of B31.3 are
wall thickness equations for curved
and mitered pipe.
With regard to circumferential
welds, the designer is responsible
for assigning a weld-joint reduction
factor (W) for welds other than longitudinal welds. What we can do, at
Incident No. 2: Formosa Plastics Corp.,

trailer being towed by a forklift operator
down a pipe rack alley in the Olefins II
operating unit of Formosas Point Comfort
facility attempted to back the trailer up into an
open area between pipe rack support columns
in an effort to turn the rig around. When the
operator, in the process of pulling back into
the pathway, began to pull forward the trailer
struck a protruding 2-in. blow-down valve on
a vertically mounted Y-strainer that was connected to a 4-in. NPS liquid propylene line
subsequently ripping the valve and nipple
from the strainer (Figure 4). Liquid propylene
under 216 psig pressure immediately began
discharging into a liquid pool from the 2-in. opening and partially
vaporizing into a flammable cloud.
The flammable cloud eventually found an ignition source, ignited
and exploded, in-turn igniting the pool of liquid propylene. The
fire burned directly under the pipe rack and an attached elevated
structure containing process equipment and piping. About 30 min
into the event, non-fire-proofed steel sections of the pipe rack and
the elevated structure containing process equipment collapsed
(Figure 5). The collapse caused the rupture of equipment and additional piping containing flammable liquids, adding more fuel to
an already catastrophic fire. The flare header was also crimped in
the collapse and ruptured, causing flow that should have gone to
the flare stack to be discharged into the heart of the fire. The fire
burned for five days.
Again, as in Incident No. 1, you can see in Figure 5 the result
of insufficient fire proofing of steel beams and columns in close
proximity to process units. And fire protection does not apply
only to vertical columns. As you can see, it is not sufficiently
effective to have the vertical columns protected while the horizontal support steel is left unprotected and susceptible to the heat
from a fire.
Another key factor in the Formosa fire was the ambiguous decision by the designer to orient the Y-strainer blow-down in such a
position of vulnerability. While there is absolutely nothing wrong
with installing the Y-strainer in the vertical position, as this one
was, they are normally installed in a horizontal position with the
blow-down at the bottom, inadvertently making it almost impossible to accidentally strike it with enough force to dislodge the
valve and nipple.
However, orienting the blow-down in such a manner, about the
vertical axis, should have initiated the need to evaluate the risk and
make the determination to rotate the blow-down about its vertical
axis to a less vulnerable location, or to provide vehicle protection
least for this discussion, is to provide,

as a frame of reference, some quality
rankings for the various circumferential welds based on the stress intensification factor (SIF) assigned to
them by B31.3. In doing so, the full
penetration buttweld is considered
to be as strong as the pipe with an
SIF = 1.0. The double fillet weld at a
slip-on flange has an SIF = 1.2. The
socketweld joint has a SIF = 2.1. Any
value in excess of 1.0 will de-rate the
strength of the joint below that of the
pipe. With that said, and assuming
an acceptable weld, the weld joint,
and particularly the full penetration
buttweld, is still the joint with the
highest degree of integrity. In a fire,
4-in. Propylene
product line
Column
Point Comfort, Tex., Oct. 6, 2005
Strainer
Pipe
nipple
2 ft
Figure 4. The impact point (left)

showing the damaged Y-strainer
Figure 5. Collapse of non-fire-proofed structural steel
around the blow-down in the form of concrete and steel stanchions.

Both of these precautionary adjustments were overlooked.
The plant did perform a hazard and operability study (HAZOP)
and a pre-startup safety review (PSSR) of the Olefins II operating
unit. In the CSB report, with regard to process piping and equipment, it was stated that, During the facility siting analysis, the
hazard analysis team [Formosa] discussed what might occur if a
vehicle (for instance, fork truck, crane, man lift) impacted process
piping. While the consequences of a truck impact were judged
as severe, the frequency of occurrence was judged very low
(that is, not occurring within 20 years), resulting in a low overall
risk rank [The ranking considered both the potential consequences
and likely frequency of an event]. Because of the low risk ranking,
the team considered existing administrative safeguards adequate
and did not recommend additional traffic protection.
the last joint type to fail will be the

welded joint.
The threaded joint has an SIF =
2.3 and requires a thread sealant
applied to the threads, upon assembly, to maintain seal integrity. With
flame temperatures in a fire of around
2,7003,000F the thread sealant will
become completely useless if not vaporized, leaving bare threads with no
sealant to maintain a seal at the joint.
The flange-joint-sealing integrity,
like the threaded joint, is dependent
upon a sealant, which, unlike the
threaded joint, is a gasket. Flange
bolts act as springs, providing a constant live load so long as all things
remain constant. Should the gasket
melt or flow due to the heat of a fire,

the initial tension that was given the
bolts when the joint was assembled
will be lost. Once the gasket has been
compromised the sealing integrity of
the joint is gone.
Knowing that the mechanical type
threaded and flange joints are the
weak points in a piping system, and
the primary source for leaks, it is suggested that their use be minimized to
the greatest extent possible. Consider
the following design points:
Do not specify flange joints solely for
installation purposes
Specify flange joints only where required for equipment connections
and for break-out spools
39
Feature Report
Discharge
to safe area
Line D
Slope
RD-1
If a lined pipe system is required,

use the type requiring the liner to be
fused, a coupling installed and one
that is suitable for multi-axis bending
Threaded joints should be limited
to instrument connections and then
only if the instrument is not available with a flange or welded connection. If a threaded connection is used,
it should be assembled without thread
compound then seal-welded. This may
require partial dismantling of the instrument to protect it from the heat of
the welding process.
It is recommended that piping systems be welded as much as possible and
flanged joints be minimized as much as
possible. That includes using welded
end valves and inline components
where possible. If flanged joints are
necessary for connecting to equipment
nozzles, flanged valves, inline components, or needed for break-out joints, it
is suggested that a spiral-wound type
gasket with graphite filler be specified.
This material can withstand temperatures upwards of 3,000F. There are
also gasket designs that are suitable
for when a fluoropolymer material is
needed for contact with the chemical,
while also holding up well in a fire.
These are gaskets similar in design to
that shown in Figure 3.
Valves. A fire-rated valve meeting the
requirements of API 607 (Fire Test
for Soft Seated Quarter Turn Valves)
is designed and tested to assure the
prevention of fluid leakage both internally along the valves flow path, and
externally through the stem packing,
bonnet seal, and body seal (where a
multi-piece body is specified). Testing
under API 607 subjects a valve to well
defined and controlled fire conditions.
It requires that after exposure to the
fire test the valve shall be in a condition that will allow it to be rotated
from its closed position to its fully
open position using only the manual
operator fitted to the test valve.
Quarter turn describes a type of
valve that goes from fully closed to
fully open within the 90 deg rotation
of its operator. It includes such valve
types as ball, plug, and butterfly with
a valve seat material of fluoropolymer,
elastomer, or some other soft, non-metallic material.
Standards such as FM-7440 and
40
XV-1
Line A
Flammable
liquid in
VA-1
Operating unit
battery limits
LT-1
SG-1
VA-6
VA-3
Flammable
liquid to
recovery
VA-4
PG-1
XV-2
VA-5
Flammable
liquid out
Line B
VA-2
Pump
Line C
XV-3
XV-4
Figure 6. A simplified P&ID used in the discussion about process systems
BS-6755-2, touched on earlier, apply

to virtually any valve type that complies with their requirements. Under
the FM and BS standards, valve
types such as gates, globes, and piston valves with metal seats can also
make excellent fire-rated valves when
using a body and bonnet gasket and
stem packing material similar in temperature range to that of a graphite or
graphite composite.
Process systems. At the onset of a fire
within an operating unit, initially unaffected process piping systems should
not be a contributor to sustaining and
spreading what is already a potentially
volatile situation. There are basic design concepts that can be incorporated
into the physical aspects of a process
system that will, at the very least, provide precious time for operators and
emergency responders to get the situation under control. In referring to the
simplified piping and instrumentation
diagram (P&ID) in Figure 6, there are
seven main points to consider:
1. Flow supply (Line A), coming from
the fluids source outside the operating unit, needs to be remotely shut off
to the area that is experiencing a fire
2. The flow path at the systems use point
valves (VA-1) needs to remain open
3. The flow path at drain and vent valves
(VA-2) needs to remain sealed
4. The external path through stem
packing and body seals needs to remain intact during a fire
5. The bottom outlet valve (XV-2) on a
vessel containing a flammable liquid should have an integral fusible
link for automatic shut-off, with its
valve seat, stem packing and body
seals remaining intact during a fire
6. Pipeline A should be sloped to allow
all liquid to drain into the vessel
7. The liquid in the vessel should be

pumped out to a safe location until
the fusible link activates, closing the
valve. There should be an interlock
notifying the control room and shutting down the pump
Those seven points, with the help of
the P&ID in Figure 6, are explained
as follows:
Point 1. The supply source, or any
pipeline supplying the operating unit
with a flammable liquid, should have
an automated, fire-rated isolation
valve (XV-1) located outside the building or operating unit area and linked
to the units alarm system with remote
on/off operation (from a safe location)
at a minimum.
Point 2. Any point-of-use valve (VA-1)
at a vessel should remain open during a fire. The area or unit isolation
valve (XV-1) will stop further flow to
the system, but any retained or residual fluid downstream of the automatic shut-off valve needs to drain to
the vessel where the increasing overpressure, due to heat from the fire,
will be relieved to a safe location, such
as a flare stack, through RD-1. If the
Valves, XV-1 and VA-1, are closed in a
fire situation the blocked-in fluid in a
heated pipeline will expand and potentially rupture the pipeline; first at the
mechanical joints such as seals and
packing glands on valves and equipment, as well as flange joints, and then
ultimately the pipe itself will rupture
(catastrophic failure). During a fire, expanding liquids and gases should have
an unobstructed path through the piping to a vessel that is safely vented.
Point 3. Valves at vents and drains
(VA-2 & VA-6) need to be fire-rated and
remain closed with seals and seat intact
for as long as possible during a fire.
Incident No. 3: BP Refinery,

Texas City, Tex., July 8, 2005
High-temperature
n the design layout of a duplex heathydrogen to furnance
exchanger arrangement (Figure 7) in the
resid-hydrotreater unit of the BP Refinery in
Preheat gas
Texas City, Tex., the designer duplicated the
fabrication dimensions of the 90-deg fabricated elbow-spool assemblies shown in FigFigure 8. Severed 8-in.
Heat
ure 7 as Elbows 1, 2, and 3. While the pipe
NPS hydrogen piping
exchanger A
sizes and equipment nozzle sizes were the
Elbow 3
same, permitting an interchangeability of the
(failure location)
fabricated elbow spool assemblies, the service
Elbow 2
conditions prohibited such an interchange.
Bolted flange
The shell side conditions on the upstream
(typical)
side (at Elbow 1) were 3,000 psig at 400F.
The shell side conditions on the downstream
11/4 chrome
side (at Elbow 3) were 3,000 psig at 600F.
alloy piping
The intermediate temperature at Elbow 2
was not documented. In the initial design,
Elbow 1
the material for Elbow 1 was specified as carbon steel
carbon steel, Elbow 3 was specified as a
Heat
exchanger B
1 - 1/4 chrome/moly alloy. The reason for
the difference in material of construction
(MOC) is that carbon steel is susceptible to
Preheat gas
high temperature hydrogen attack (HTHA)
to separator
above ~450F at 3,000 psig, therefore the
Low-temperature
chrome/moly alloy was selected for the
3,000 psig
higher temperature Elbow 3.
hydrogen feed
11/4 Chrome alloy pipe
At 3,000 psig and temperatures above
Carbon steel pipe
450F hydrogen permeates the carbon steel
and reacts with dissolved carbon to form Figure 7. Heat exchanger flow diagram
methane gas. The degradation of the steels
The one thing you can take
tensile strength and ductility due to decarburization, coupled
with the formation of methane gas creating localized stresses, away from this incident is: Do
not dimensionally replicate
weakens the steel until it ultimately fatigues and ruptures.
In January 2005, scheduled maintenance was performed on the piping spools or assemblies of
heat exchanger assembly. The piping connected to the heat ex- different materials. The other
changers was dismantled and stored for the next 39 days. After underlying, but significant
maintenance was completed, the piping was retrieved from stor- component you can also take
away is this: In the initial de- Figure 9. Fragments of
age and reinstalled.
the failed 8-in. NPS carbonThe elbows of different material were not marked as such and sign of a plant facility the ensteel spool
gineer
of
record
will
routinely
the maintenance contractor was not warned of the different
MOC for the elbows. Elbows 1 and 3 were unknowingly in- hold formal design reviews
stalled in the wrong locations. On July 8, 2005, approximately that will include all key personnel with vested interest in the projfive months after re-installing the piping around the heat ex- ect. In doing so, include, among the attendees, key operations
changers, the elbow in the #3 position catastrophically failed as and management plant personnel from one of the owners operating facilities, if available. These individuals typically bring a
shown in Figure 8.
As you can see in Figure 9 the carbon steel, after becoming lot of insight and knowledge to a review. Whereas the designers
progressively weakened by HTHA, fractured on the inside of may not have the wherewithal to think along the lines of issues
the pipe and catastrophically failed. The incident injured one that might pertain to a facility turnaround, the plant personnel
person in operations responding to the emergency and cost the will. These are issues that they normally think long and hard
company $30MM.
about. Make use of this resource.
Point 4. During a fire, another source

for valve leakage is by way of stem
packing and body seal, as mentioned
earlier. Leakage, at these seal points,
can be prevented with valves that are
not necessarily fire-rated, but contain
stem packing and body seal gasket
material specified as an acceptable
form of graphite (flexible graphite,
graphoil and so on). This is a fire-safe
material which is readily available in
non-fire-rated valves.
Point 5. The valve on the bottom of
the vessel should be fire-rated with a
fusible link or a fail closed position.
Relying on an air or electric operated

valve actuator may not be practical. A
fusible link is most certainly needed
on a manually operated valve. The
contents of a vessel containing a hazardous liquid needs to get pumped to
a safe location during a fire until such
time as the fusible link is activated,
closing the tank bottom valve, or the
pump fails. All valved gage and instrument connections (SG-1) mounted on
a vessel should have a graphite-type
stem packing and body-seal-gasket
material at a minimum. Flange gaskets at these gage and instrument con-
nections should be of a spiral-wound

fire-safe gasket type similar to those
mentioned earlier. Specialty tankbottom valves (XV-2) should be given
special consideration in their design
by considering a metal-to-metal seat,
or a piston valve design along with
fire-rated seal material.
Point 6. As mentioned in Point 2, the
residual fluid in Line A, after flow has
been stopped, should be drained to
the vessel. To help the liquid drain,
the pipeline should be sloped toward
the vessel. The intent, as mentioned
above, is to prevent sections of any
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42
Feature Report
pipeline that do not contain a relief
device from being blocked and isolated
during a fire. If the piping system for
flammable fluid service is designed
properly, the contents will be able to
drain or expand into a vessel where
over-pressurization can be relieved
and safely vented.
Point 7. It will be necessary to evacuate as much of the hazardous fluid as
possible from tanks and vessels in the
fire area to a safe location. The pumpout should continue until there is inadequate pump suction head, or until
the fusible link on XV-2 is activated.
At that time the pump interlocks
would shut down the pump.
With regard to tank farms, the following is a suggested minimum consideration for a safe design: Drain
valves should be of a fire-rated type.
Tank outlet valves should be of a firesafe type with a fusible link. Tank
nozzles used for gages or instrument
connections should have, at a minimum, valves containing stem packing and seal gasket material specified
as an acceptable form of graphite, as
mentioned above, or some other firesafe material. Gaskets used at nozzle
flange joints should be a fire-safe gasket similar to the spiral wound gaskets mentioned earlier or the gasket
shown in Figure 3.
Inline valves in piping downstream
of the tank outlet valve, such as pump
transfer lines and recirculation lines,
do not necessarily need to be firerated, but should have stem packing
and seal gasket material that is firesafe as mentioned earlier.
Situations will arise that do not fall
neatly into what has been described
above. If there is any doubt with regard
to valving then default to a fire-rated
valve. Each piping system identified
as needing to be fire-safe should be
designated as such. Where individual
fire-safe valves are to be strategically
located in a system, they should be
designated on their respective P&IDs
either by notation or through the assigned pipe material specification.
The pipe-material specification should
be indicated on each pipeline of the
P&ID. The specification itself should
therefore be descriptive enough for
the designer to know which valve to
apply at each location.
Lessons learned from incidents
While this particular discussion is specific to piping leaks and joint integrity
it bares touching on a few subjects that
are integrally associated with piping
safety: pipe rack protection, protecting
piping from vehicle traffic, and designing for disaster (HAZOP).
In Incident Number 1 (box, p. 37),
the onset of a fire that might otherwise
have been quickly controlled becomes
a catastrophic event because piping
mounted on the unprotected structural
steel of a pipe rack, outside the extent
of the initial occurrence, becomes collateral damage adding more fuel to the
fire causing it to sustain itself, increase
in intensity and continue to spread.
In Incident Number 2 (box, p. 39), an
unprotected and protruding pipeline
component (Y-strainer) is damaged,
causing a major leak that operating
personnel were unable to stop. The ensuing fire lasted for five days.
In Incident Number 3 (box, p. 41),
two dimensionally identical spool
pieces were designed for a system in
which the two were fabricated from
different materials because their service conditions were very different. It
can only be assumed that this was an
erroneous attempt at trying to achieve
duplication of pipe spools in an effort
to assist the fabricator in their productivity of pipe fabrication. Instead it
ultimately caused injury to one person
and cost the plant owner $30MM.
Edited by Gerald Ondrey
Author
W. M. (Bill) Huitt has been
involved in industrial piping design, engineering and
construction
since
1965.
Positions have included design engineer, piping design
instructor, project engineer,
project
supervisor,
piping department supervisor,
engineering manager and
president of W. M. Huitt Co.
(P.O. Box 31154, St. Louis,
MO 63131-0154; Phone: 314-966-8919; Email:
wmhuitt@aol.com; URL: www.wmhuitt.com),
a piping consulting firm founded in 1987. His
experience covers both the engineering and
construction fields and crosses industrial lines
to include petroleum refining, chemical, petrochemical, pharmaceutical, pulp and paper,
nuclear power, biofuel, and coal gasification.
He has written numerous specifications, guidelines, papers, and magazine articles on the
topic of pipe design and engineering. Huitt is
a member of ISPE (International Society of
Pharmaceutical Engineers), CSI (Construction
Specifications Institute) and ASME (American
Society of Mechanical Engineers). He is a member of three ASME-BPE subcommittees, several
task groups, an API task group, and sits on two
corporate specification review boards.
DuPont
Solids
Environmental
Processing
Manager
Chemical
Protective Clothing
ISO 16602 offers a much-needed,
common global language for expressing
protective clothing performance
Susan Lovasic, DuPont
hemical protective garments

are available in a wide variety of fabrics and designs that
provide varying levels of protection for chemical process industries
(CPI) workers, who may be exposed to
chemicals in the form of vapors, liquids and particles. While other forms
of personal protective equipment
such as safety glasses and hard hats
are highly regulated in the U.S. and
Canada, the performance of chemical
protective clothing is not. An international standard for classifying chemical-protective-clothing performance,
however, is available in ISO 16602. The
ISO 16602 Standard (Protective clothing for protection against chemicals
Classification, labelling and performance requirements) provides an
objective system to appropriately test,
classify and label chemical-protectiveapparel products. This article shows
how ISO 16602 can be used as a tool to
help with the selection of appropriate
chemical protective clothing by providing an objective means of defining the
performance of chemical protective apparel in situations involving potential
exposure to chemical hazards.
Since, in North America, chemical
protective clothing is not assessed by
a comprehensive standard that quantifies the performance of garments,
safety and health professionals selecting chemical protective clothing can
only rely upon manufacturers claims
to choose the appropriate garments.
Unfortunately, the performance of
chemical protective clothing can vary
by manufacturer and there is no established means to compare the performance of the various garments on the
market. There is also no standard lan-
guage in place that describes either the

overall performance of the protective
ensemble or the performance of the
individual components against types
of different chemical hazards. While
some standards do exist for hazardous
materials (Hazmat) emergencies, little
regulation exists regarding routine industrial workplace applications. This
void in recognized standards for everyday, industrial-use chemical protective
clothing can lead to confusion and uncertainty for the safety professionals
who must select the appropriate apparel for a given hazard or application.
Established by the International Organization for Standardization (ISO),
the requirements outlined in ISO
16602 provide a common language for
the performance of chemical protective clothing. While ISO 16602 was introduced fairly recently (in 2007), it is
already recognized and accepted internationally, and is poised to become the
global language for expressing chemical-protective-clothing performance.
By offering a common, global classification system and a standard presentation of the performance data,
ISO 16602 can simplify the selection of
chemical protective apparel by safety
and occupational health professionals.
Standardizing the protective clothing performance data allows objective
evaluation and comparison of the various garments available in the marketplace, rather than relying solely upon
vendors claims. Although ISO 16602
permits a range of performance levels
for a series of key properties, it also
establishes a minimum level of performance for each major type of hazard.
ISO 16602 defines performance requirements based on results obtained
from existing test-method standards.

Many companies are multinational
and do not have access to the same
chemical protective apparel in each
location even though they may be
engaged in the same work tasks and
therefore have the same needs for
protective clothing. The ISO 16602
description of chemical-protectiveclothing performance is vital to these
businesses as it provides a common
description that can be used to select the appropriate, locally available
products. In addition, ISO 16602s objective performance levels allow safety
professionals a means of identifying
and selecting higher performing garments if a specific selection of chemical protective clothing fails to perform
as intended in the work environment
for which it was chosen.
Clothing selection
The first, and most critical, step to

selecting appropriate chemical protective clothing is the completion of
an accurate hazard assessment. By
identifying the task, the surroundings, the chemical(s) and any hazards
beyond chemical exposure, a hazard
assessment provides a basis for understanding what chemical protective
clothing and other personal protective
equipment (PPE) are necessary to protect the workers operating in specific
situations. The environment, chemical hazard and work activity must be
considered in order to be able to select the most appropriate protective
clothing including the fabric, seam
type and garment design most suitable. Without adequate protection
from chemical protective apparel and
proper work practices, the likelihood
Chemical Engineering www.che.com March 2011
51
of a worker being exposed to potentially harmful chemicals increases.
Conversely, overprotecting a worker
with unnecessary clothing can be burdensome and result in heat stress, reduced field of vision, restricted mobility and increased physical exertion for
the wearer, as well as possibly higher
purchasing costs for the employer.
Every work situation is unique,
and the ISO 16602 Standard does not
consider all specific hazards that may
be present in the work environment.
Safety and occupational health professionals need to consider hazards that
are specific to their work conditions
and then look to ISO 16602 to find the
minimum requirements for chemical
protective garments for that type of
situation. ISO 16602 focuses exclusively on typical chemical hazards
and protective clothing requirements
for such hazards so the work situation
may also require additional forms of
PPE, such as footwear, gloves, face protection, fall protection and respirators.
When evaluating protective clothing
performance under ISO 16602, gloves,
footwear and respirators must be included in the whole-garment ensemble testing. It is important to validate
that any additional PPE components
will work properly with the chemical
protective clothing selected for use.
Types of clothing
The ISO 16602 standard is based upon

a series of types and classes. ISO 16602
designates minimum performance levels for six types of chemical hazards.
The type is the overarching system,
with chemical protective clothing fitting into one of the six different types.
The garment type designation is based
upon the physical state of the hazard,
for example vapors, liquids, aerosols
or particles (Figure 1).
When setting the requirements for
each type in ISO 16602, the entire garment is tested as well as the individual
components. During the whole-garment
tests, a human subject wears the test
garment and accompanying PPE, such
as gloves, boots and respirator. The
human subject is exposed to non-hazardous test chemicals while in an enclosed chamber performing a series of
movements meant to simulate actual
work activities. This whole-garment
52
testing is used to validate the barrier

performance of the entire ensemble
against a specific type of chemical
threat (gas, liquid or particle). Wholegarment testing is conducted for each
ISO 16602 type, and the exposure conditions for the tests vary according to
the hazard defined by that type. Note
again that the test chemicals are nonhazardous and are used to essentially
determine how much of a similar phase
chemical will leak into the suit. The
whole-garment tests do not evaluate
the chemical permeation properties of
the garments. This is assessed in the
class testing portion of ISO 16602.
For example, the Type 3 whole-garment test is conducted by having the
test subject march in place with exaggerated arm-pumping movements,
while slowly turning, in front of a highpressure, high-volume liquid spray
nozzle. This liquid is tinted with a dark
color to be visible if it penetrates the
test garment. Once the high-pressure
liquid exposure portion of the test is
completed, the outer test garment is
carefully removed and an inner indicator garment is checked for evidence of liquid penetration, which is
evident by staining from the dark liquid. Beyond the whole-garment tests,
additional tests are conducted on the
garments fabric(s) and components to
qualify the class performance level for
the garment against specific chemical
challenges and the physical demands
of the task and work surroundings.
ISO 16602 defines different class levels of performance for each type of protection as described below.
Classes of clothing
Within each of the six garment types,

there are also requirements directed
at the mechanical, barrier and basic
flammability properties of the fabrics
and components used to make chemical
protective clothing. Laboratory tests
are used to determine the mechanical
durability, the barrier against specific
chemical hazards, and ease of ignition
of the garment materials. The results
of these tests will fall into a unique
performance class. Each type within
ISO 16602 specifies a combination
of barrier and durability tests levels,
establishing a minimum performance
class for each of the tests to meet the
specific type requirements. A higher

class rating denotes a higher level of
performance for that property.
The flammability requirements
outlined in ISO 16602 establish a
minimum performance level of flame
spread once the material is ignited; it
does not qualify an ensemble as suitable for protection against heat and
flame hazards. Specific evaluation of
chemical protective clothing for heat
and flame protection is not in the purview of ISO 16602. In North America,
relevant standards specifically related
to protective clothing for use near fire
and electric-arc hazards are NFPA
2112 (Standard on Flame-Resistant
Garments for Protection of Industrial
Personnel Against Flash Fire) and
NFPA 70E (Standard for Electrical
Safety in the Workplace).
The class tests are as important as
the whole-garment tests described earlier. Both are integral to evaluating the
overall integrity and expected performance of chemical protective clothing.
This integrated rating system aids the
selection of the most appropriate chemical protective apparel for specific work
tasks. Testing the whole garment and
the individual components separately
ensures the sum of the parts is able to
provide the appropriate protection.
Applying ISO 16602
While understanding ISO 16602 is

critical for safety and occupational
health professionals, it must also be
applied consistently and correctly in
the workplace. Consider the task of
opening a flange in a process pipe containing a hazardous liquid under pressure. Even though the pipe should be
depressurized and drained as much as
possible before the flange is removed,
this activity would likely require an
ISO 16602 Type 3 garment for protection against the possibility that pressurized liquid exposure might occur.
The Type 3 whole-garment jet test
would have demonstrated the liquidpenetration resistance of the ensemble and the performance of the connections between the garment and other
items of PPE, such as gloves, boots
and respirator. The chemical barrier
performance of the suit material and
components should have been determined with permeation tests using
Six types of CPC outlined in ISO 16602
Type 1
Type 2
Type 3
Type 4
Type 5
Type 6
Limited
protection
against
liquid mist
Protection
against
airborne,
solid
particulate
chemicals
Protection
against
liquid
aerosols
Protection
against
pressurized
liquid
chemicals
Non
gas-tight
protection
Gas-tight
protection
against
chemicals
and vapors
and toxic
particles
Type indication doesnt tell you everything

about the performance of the CPC. It only
tells that it meets the minimum requirements of a particular type certification
Figure 1. Do not assume that the terms gas-tight and liquid-tight refer to absolute barrier performance in chemical protective clothing (CPC). They can oversimplify
the level of barrier provided by such garments. Instead, these terms should be considered as vapor-protective and liquid-protective, respectively
the specific chemical that is in the process piping. The mechanical durability
of the suit against the rigors of the job
would have been assessed with the
mechanical-strength laboratory tests
outlined in ISO 16602. The hazard assessment and experience of the safety
and occupational health professional
would lead to the selection of a garment with a specific performance class
in each of the barrier and mechanical
tests, plus the type requirement.
Another example can be found in
work situations where exposure to
hazardous particles might be likely
to occur, such as sanding lead-based
paints or mold-abatement work. For
protection against airborne hazardous
particles, a Type 5 ensemble would be
the obvious choice, barring any other
hazard or complications. Most likely,
the garment would be a one-piece coverall with an attached hood, but nothing in ISO 16602 precludes a multiplepiece ensemble, such as a separate
jacket, hood and pants. ISO 16602
does not specify the design of the ensemble; it specifies the level of performance. As with the previous case, the
nature of the work task will determine
the class of mechanical durability required for the work activity and environment. Note that the use of a respirator might also be required when
working near airborne particles.
Labeling
In addition to delineating performance

standards for chemical protective
clothing, ISO 16602 also sets minimum requirements for the labeling
and documentation for such garments.
Chemical-protective-clothing
labels
complying with ISO 16602 must be
permanently attached to the garment
and should include the manufacturers
contact information, the garment style

and model number, the ISO 16602
type, the date of manufacture, size
and care instructions. With each garment, the manufacturer should provide complete instructions that include
safety considerations and limitations,
user instructions and all inspection,
warranty, and maintenance information. Since ISO 16602 does not require
third-party certification to claim compliance, the safety and occupational
health professional should request and
examine validation reports provided by
the garment manufacturer that support all performance claims made for
the chemical protective clothing. Use of
ISO 16602 by garment manufacturers
can provide objective information that
enables safety and occupational health
professionals to select the most-appropriate chemical-protective clothing for
their employees.

Author
Susan Lovasic is a senior
research associate for DuPont Protection Technologies
(5401 Jefferson Davis Highway, Richmond, Va., 23234;
Phone: 804-383-5060; Email:
susan.l.lovasic@usa.dupont.
com). Since 1996, her research efforts have focused
on protective apparel applications to help protect wearers
against chemical, thermal
and fire hazards. In her role, Lovasic has conducted extensive research to assess the critical
properties of protective apparel ranging from
assessment of comfort and durability properties
of protective garments to instrumented, thermal
mannequin fire and electric-arc flash testing.
She has worked for DuPont since 1984 in both
research and marketing capacities across a variety of businesses. Lovasic holds four U.S. patents
associated with materials used for fabrics and
clothing for electric arc, flame and fire protection.
She is a member of several professional societies
including the AIChE, National Fire Protection
Association (NFPA), American Society for Testing and Materials (ASTM), American Association of Textile Chemists and Colorists (AATCC),
and the American Society of Safety Engineers
(ASSE). Lovasic received her B.S.Ch.E. from
Pennsylvania State University.
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53
Solids Processing
Environmental
Manager
Managing Material Safety

Data Sheets in the Workplace
While regulatory agencies
outline requirements for
communicating chemical
hazards, the format of compliance
is up to the employer.
Software tools can be helpful aids
in meeting these requirements
Karen E. Lintz
Wercs Professional Services, LLC
o ensure the health and safety

of workers, the U.S. Occupational Safety and Health Administration (OSHA) adopted
the Hazard Communication Standard
(HCS) in 1983. Initially designed to
protect workers in the manufacturing
sector, the HCS was expanded in 1987
to cover all industries where workers
could be exposed to hazardous chemicals. This article gives an overview of
the OSHA requirements for material
safety data sheets (MSDSs) and describes ways to meet these requirements with automated software tools.
Hazard communication program
All manufacturers and importers of

chemicals are required to review the
known physical and health hazards
of the chemicals they make or import
to determine if they are hazardous.
This process is known as hazard assessment. The manufacturers and
importers must have a process for
collecting and assessing this information, and then generating MSDSs.
While OSHA only requires MSDSs for
chemicals that are hazardous according to its definition, these data sheets
are also often written for non-hazardous materials.
When the MSDSs have been developed, the manufacturer must make
Material safety
data sheets are
an essential part
of hazard communication programs
them available to downstream users

of the chemicals, including its own
employees, distributors and customers. A written hazard-communication
program is also required to share this
information with employees through
training and the use of MSDSs and
warning labels. The written program
must describe how the requirements
for labels, MSDSs and employee training are going to be met in the facility.
This hazard communication program is
key to meeting OSHAs requirements.
Employee training
Under the HCS, all employees have

the right to know about chemical hazards in the workplace, and how they
can protect themselves against both
the physical and health hazards associated with exposure. Employees
must know the identities of the hazardous chemicals in their workplace

and where they can find the MSDSs
for the chemicals.
The HCS dictates that employees
be trained at least once a year, but
additional training should also be
conducted whenever a new hazardous chemical is introduced into the
workplace. The training must include
educating employees in the proper
use of the hazardous chemicals. Both
the physical and health hazards of
the chemicals should be included, as
well as information on how employees
can protect themselves from exposure.
Employees need to know the physical
properties of the chemicals, how to detect a spill or release of the chemical,
and what measures to take if a spill
occurs.
Chemical Engineering www.che.com November 2007
53-55 CHE 11-07.indd 53
53
10/25/07 7:30:12 PM
Employee access to information
According to OSHA, all employees
must have direct access to MSDSs for
the hazardous chemicals that are in
their work areas during their normal
working hours. Employers must ensure that employees are provided with
an MSDS for every chemical to which
they may be exposed, and employees
must receive training on any new
chemicals before the chemicals are introduced into the workplace. MSDSs
may be provided to employees as paper
copies contained in centrally located
binders or through computerized systems. Alternatives to paper copies are
permitted, as long as employees have
immediate access to the MSDSs. Maintaining paper copies of MSDSs in a
back-up method to electronic systems
is often a good practice.
Information requirements
To ensure that employees can properly handle hazardous chemicals in

the workplace, the HCS requires that
each MSDS include information about
the chemical that will allow employees
to quickly identify the chemical, recognize the possible hazards of exposure,
and take precautions to protect themselves against exposure. The HCS is a
performance-oriented standard, which
means that OSHA provides very few
requirements for the format of MSDSs.
However, the HCS does specify that
MSDSs must be available in English, and must include the following
information:
The product name as it appears on
the container label: This allows employees to quickly locate the proper
MSDS for the chemical they are
handling
The names of all of the hazardous
chemicals in the product that are
present at a concentration of greater
than 1% (0.1% for carcinogens): Nonhazardous chemicals may also be
listed, but full disclosure of a products formulation is not required
The physical and chemical characteristics of the chemical, such as its
physical form, color, odor, flash point
and vapor pressure: To ensure safe
handling, employees must be able to
recognize how a product is supposed
to look and behave
The physical hazards of the product,
54
such as flammability and reactivity:

This information may be important
for proper handling, storage, and
disposal of a chemical
The known acute (immediate or
shortterm) and chronic (longterm)
health hazards of the chemical
The signs and symptoms of exposure: Some chemicals do not have
good warning properties, such as a
smell, so employees must be able to
recognize any expected health effects from overexposure to a hazardous chemical
Any medical conditions that may
be aggravated by exposure to the
chemical: Employees with pre-existing medical conditions may need
to take additional steps to ensure
their safety when working with a
chemical
The routes of exposure for the hazardous chemical: This information is
important when choosing the proper
personal protective equipment to be
worn while handling a hazardous
chemical. Severe irritants or chemicals that can be absorbed through
the skin may require specific gloves
or protective clothing, while products
that are respiratory hazards may
need special ventilation or respiratory protection for safe handling
The exposure limits for the hazardous chemical, including the OSHA
permissible exposure limit, the
ACGIH (American Conference of
Governmental Industrial Hygienists) threshold limit value (TLV),
or a recommended exposure limit
developed by the manufacturer of
the hazardous chemical: This information is critical to ensure that
employees are not overexposed to
hazardous chemicals during the
workday
The classification of the chemical as
a known or potential carcinogen by
OSHA, NTP (National Toxicology
Program), or IARC (International
Agency for Research on Cancer)
Precautions for safe handling and
use, including hygiene practices and
cleanup procedures
Appropriate engineering controls
and personal protective equipment
Emergency and first aid procedures
The date the MSDS was prepared
The name, address and telephone
number of the party responsible for

preparing the MSDS
The MSDS may also provide additional regulatory information for the
hazardous chemical. SARA (Superfund Amendments and Reauthorization Act) hazard classifications, CERCLA (Comprehensive Environmental
Response, Compensation and Liability Act) reportable quantities (RQs),
transportation information, global
inventory compliance, and environmental hazards or effects are often
included in MSDS. When these documents are written to the ANSI (American National Standards Institute)
standard guidelines, they will meet
OSHA requirements and provide the
user with additional helpful toxicology
and regulatory information.
Updating the MSDS
In the U.S., there is no specific timeframe requirement for updating

MSDSs. When the document is prepared, it must include the most upto-date information about the chemical hazards based on the available
scientific evidence at that time. If a
manufacturer becomes aware of new
significant information regarding a
chemicals hazards, the manufacturer
has three months to update its MSDS.
This updated version must be provided
to customers with the next shipments
of the hazardous chemical. To ensure
compliance with this requirement,
manufacturers must closely monitor
global chemical regulations as well as
new reports of adverse health or environmental effects associated with
chemical exposure.
MSDS management software
While there are no requirements for

generating MSDSs through specific
software, many companies utilize software tools or programming to produce
and manage their MSDSs.
Using dedicated MSDS-management software has several distinct
advantages over word processing: increased MSDS-production efficiency;
enhanced MSDS-language consistency; better formulation management; and ease of distribution.
Global market. In todays global
market, having a system that supports
alternate templates and languages to
53-55 CHE 11-07.indd 54
10/25/07 7:30:37 PM
meet the requirements for specific regions or countries is a must. All global
product information can be stored in
MSDS management software, allowing for the quick and easy production
of MSDSs for any country or region.
Rules or logic tools. Automated tools
can decrease the need for manual data
entry and manipulation. By using appropriate software, information can be
automatically entered into the MSDS
based on system rules or logic. This
not only increases the efficiency of
MSDS production but the consistency
of MSDS information as well.
Impact of regulatory changes. The
impact of changes in regulations can
be quickly determined through the
use of automated impact analyses
and update tools. These tools can ensure that all affected products are reviewed, and required changes are applied appropriately. These tools can be
configured to apply to local, regional,
state, federal and global changes, de-
pending on the needs of the user.

MSDS distribution tools. Automated MSDS distribution tools are
also a very useful part of an automated
system. MSDSs can be automatically
mailed, faxed, emailed, or sent to a
web viewer based on predetermined
criteria.
Through proper training, procedures,

and automated software tools, we can
ensure that our employees and customers always receive the most upto-date information for the chemicals
they use.
n

Author
Looking forward
Requirements for MSDSs will continue to grow and change. New initiatives, regulations and health-effect
information make it necessary for regulatory professionals to continually be
on the lookout for anything that may
impact their MSDSs. New guidelines
or classification systems, such as the
Globally Harmonized System of Classification and Labeling of Chemicals
(GHS), will impact how we communicate and classify information. Regulatory professionals must keep abreast
of not only the OSHA requirements for
MSDSs, but also global requirements.
Karen Lintz is the director of regulatory services for

Wercs Professional Services
(WPS); (Phone (800) 572-6501
or (518) 640-9220; Email:
info@thewercs.com; Fax; (518)
640-9299), where she provides
regulatory guidance in support of software content and
implementation. Prior to this
position, Lintz was a regulatory specialist at GE Silicones. In earlier positions, Lintz followed patients in human clinical
cancer-treatment trials as a study coordinator at
the Cancer Center of Albany Medical Center, developed and reviewed clinical protocols and case
report forms as a data manager at Frontier Science and Technology Research Foundation, Inc.,
and worked as a product safety specialist at the
Carborundum & Advanced Materials Division of
BP Chemicals. Lintz holds a B.A. in biology from
Lycoming College and an M.A. in pharmacology,
toxicology and therapeutics from the State University of New York at Buffalo.
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53-55 CHE 11-07.indd 55
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10/25/07 7:31:04 PM
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Dust Explosions:
Prevention &
Protection
Feature
Cover
Story
Report
Ignition source
Figure 1. All three legs of the combustion triangle

must be presnt for combustion to start
Amrit Agarwal
Pneumatic Conveying Consulting
reventing dust explosions is not

rocket science, and still these
disasters occur. This article is
written to help prevent these
accidents. It describes how and why
these explosions happen and what can
be done to avoid them.
Why they occur
Dust explosions occur when three

conditions are present simultaneously. The first is that there is a dust
cloud of a combustible material (the
fuel). The second is that there is sufficient quantity of oxygen. The third is
that there is an ignition source of sufficient strength. When all three conditions combine, there is combustion
and then an explosion if the combustion takes place in a closed environment, such as a bin, silo, dust collector or even a building.
A large piece of wood, once ignited,
will burn slowly, releasing its heat over
a long time. But if this piece of wood is
cut in small pieces, the combustion rate
increases because the total contact surface area between the wood particles
and the air has increased. If the wood
pieces are cut up in very small pieces,
such as 0.1 mm or less, and the particles
form a dust cloud so that each particle
has sufficiently large volume of air giving enough space for its unrestricted
burning, the combustion rate will be
very fast. If such an explosive combustion of dust takes place inside process
equipment or work rooms, the pressure
26
Understand what causes these disasters

and then put these practical measures in place
in the fully or partly enclosed space may
rise rapidly and the process equipment
or building may burst open. Figure 1 is
called a combustion triangle because it
has these three legs. It shows that a dust
explosion can be prevented by eliminating any one of these three conditions.
Within the above three conditions,
there is one more condition to consider.
It is the concentration of dust particles in a dust cloud. For a dust explosion to take place, dust particles must
be present in sufficient quantities in
the closed gas space. The minimum
quantity or concentration is called the
lower explosive concentration (LEC).
(This term is synonymous with the
term lower explosive limit, or LEL,
that is used for combustible gases). In
addition to LEC, there is also an upper
explosive concentration (UEC) and
an optimum explosive concentration
(OEC). At or above UEC, dust particles are so close to each other that
they can burn but cannot cause a dust
explosion. At the OEC, the severity of
a dust explosion is at the maximum.
Dust explosions occur because this
combustion takes place in a closed air
space. During a dust explosion, dust
particles burn and turn into vapor,
which expands and burns other particles. The gaseous products of combustion cannot vent out from the space,
thereby resulting in an increase in internal pressure. This increase in pressure results in bursting of the container in which combustion is taking
place. In the closed vessel, pressure

rises during an explosion because of
the expanding vapor. The maximum
pressure (Pmax) that is developed depends upon a dust property called the
explosivity index (Kst). Each dust has
its own Kst value. The higher the Kst,
the higher the explosivity and the
higher the pressure that is generated.
Values of Kst and Pmax are found by a
standardized laboratory test.
A combustible dust cloud will not
start to burn unless it is ignited by a
source of heat of sufficient strength.
The most common ignition sources are
smoldering or burning materials; open
flames such as from welding, cutting,
matches and so on; hot surfaces such
as hot bearings, dryers, heaters, compressors and so on; heat from mechanical impacts; and electrical discharges,
arcs and electrostatic discharges.
A combustible dust must first be ignited before it can initiate a dust explosion. The source of ignition must have
a minimum ignition energy (MIE).
This is the energy that is required to
initiate ignition of a dust particle. The
lower the MIE, the higher the combustibility of the dust. An MIE of less
than 10 mJ is considered a low MIE.
Materials that can give dust explosions are natural organic materials,
such as grains, cottons, linens and
sugar; synthetic organic materials, such
as plastics, pigments and pesticides;
coal and peat; and most metals such as
aluminum, magnesium and zinc.
Collecting data on plant design and

explosive properties of dusts being handled
Explosive properties
It is important to know what the explosive properties of the

dusts being handled are, so that the plant in which these
dusts are used is designed correctly. These properties include
the following considerations:
Particle size of the dust, including its particle size distribution, if it has a range of different sizes
ticles during the process? If so, what will be the particle

size after breakage?
Explosive properties, such as Pmax, Kst, MIE, auto ignition
temperature, LEC, and particle size distribution of sub200 mesh dust
Does the material contain combustible gases such as hydrocarbons? This will result in hybrid mixtures that are
more explosive
Defining explosivity
A number of parameters define the

explosive characteristics of combustible solids.
Explosivity indices (Pmax and Kst).
The explosivity of dusts is measured
in terms of two deflagration indices,
namely the maximum deflagration
pressure (Pmax) and the normalized
maximum rate of pressure rise (Kst).
These indices are measured in a
closed, spherical test vessel (Figure
2). Pmax is the maximum pressure developed in a standardized test vessel
during a dust explosion. Kst measures
the severity of a dust explosion. It is
related to the rate of pressure rise due
to a dust explosion in a standardized
test vessel. The higher the value of Kst,
the greater the severity of the dust explosion. Kst is defined by Equation (1)
in bars-m/s:
K st =
dp 1/ 3
V
dt

Where:
p = Pressure in the test vessel, bar
t = Time, s
V = Volume of the test vessel, m3
(1)
dp
=R
ate of pressure rise in the test
dt
vessel
Heat of combustion. The heat of combustion of the material is an impor-
It is important to know how the plant is being designed to make it safe

against a dust explosion. Collect data such as the following:
How is the material handled in the plant? Will there be segregation
of different sized particles, resulting in concentration of very fine

particles?
Will dust accumulate in process equipment, such as dust collectors?
Is the material fragile? Will it break up into smaller par-
Can the material cause static charges?
Plant design aspects
Are there gravity falls of material in the plant? These falls can cause
a dust cloud
Is grinding equipment being used? Grinders create dusts and unless
properly designed, can emit dust in the surrounding atmosphere
Pneumatic conveying can break up fragile particles into dusts. Is it

being used?
If the process can emit dust inside a building, does the building have
a dust collection system that prevents accumulation of dust on building surfaces?
tant parameter because it determines

the amount of heat that is liberated in
the explosion. Heat is liberated due to
oxidation of the material. Metals such
as aluminum and magnesium have
much higher heat generation than organic dusts and coal. The result is that
the temperatures of flames of metallic dusts such as aluminum and magnesium are very high compared with
those of flames of organic dusts.
Particle size and particle size distribution (PSD). Explosiveness of a
dust depends upon the particle size.
In general, particles larger than about
400 microns or about 35 mesh, can
burn, but not explode. Particles larger
than 120 mesh can burn and explode,
but the severity of the dust explosion
is not very high. Particles smaller than
200 mesh are most explosive and are
used to determine the dusts explosive
properties such as its Kst, MIE and
LEC values.
As the particle size of a sub-200
mesh dust decreases, dust becomes
more and more explosive for the following reasons:
Its MIE decreases
Its Pmax and Kst increase
Hybrid mixtures are mixtures of combustible gases, oxygen and combustible dusts. Hybrid mixtures are much
more explosive than mixtures of combustible dusts and oxygen.
Dust classes. NFPA (National Fire

Protection Association) classifications
for various dusts are Class 1, Class 2
and Class 3. Class 1 is the least explosive dust, and Class 3 is the most explosive dust. Examples of these three
classes of dusts are as follows:
Class 1 dusts (Kst = 1200 bar-m/s):
Coal, flour, starch, sugar, grain, powdered milk, polyethylene, polypropylene, epoxy resin and sulfur
Class 2 dusts (Kst = 201300 barm/s): Organic pigment, wood, cellulose and cork
Class 3 dusts (Kst > 300 bar-m/s): Aluminum, magnesium and calcium
explosion protection
and prevention
If the data on the material being handled show that its dust is explosive,
steps must be taken to prevent a dust
explosion. These steps are given below.
Precautionary methods
Implement proper housekeeping procedures to minimize formation of a

dust cloud anywhere in the building
or inside process equipment. Meanwhile, minimize the probability of
having a source of ignition by adopting safe housekeeping procedures
and proper electrical classification.
These two methods are described in
more detail below.
27
Cover Story
28
20,000
120
15,000
60
5,000
30
60
dp
dt
120
160
Time, ms
240
dt
10,000
dp
90
, psi/s
PMAX
Pressure, psi
1. Control dust emissions and accumulation. Good housekeeping

should be maintained at all times in
buildings and other confined spaces to
keep them free from dust concentrations. Good housekeeping is essential
to prevent accumulation of dusts inside buildings or in structures, because these accumulations can result
in secondary dust explosions.
Dust should not be allowed to accumulate in layers on equipment, building walls, floors or structural members. Install building venting and dust
collection if good housekeeping cannot
be maintained. The preferred method
for dust removal is by means of properly designed vacuum-cleaning equipment. Dispersion of the dust, which
results in formation of a dust cloud,
must be prevented.
Meanwhile, keep the following best
practices in mind:
Dust tight process: All process components must be dust tight
Dust collection: For process components that cannot be made dust
tight, vent hoods and dust collectors
must be installed to remove and collect emitted dust
Pneumatic-conveying system design:
All equipment and piping must be of
dust-tight design to avoid emission
of dust. Piping must be designed to
withstand the maximum explosion
pressure without exceeding twothirds of the burst pressure. In case
of a filter element failure, blower
outlets and dust-collector outlets
are located outside closed buildings
to prevent formation of a dust cloud
inside a building or a structure.
2. Control ignition sources. Equipment design and arrangement, good
maintenance and good housekeeping
are all necessary to minimize the potential for ignition of dusts by electrical equipment or other equipment that
might have high surface temperatures.
In the U.S., all electrical installations and equipment designs should
meet the requirements prescribed in
the U.S. National Electrical Code. This
code classifies processing or manufacturing areas involving combustible
materials according to class, group
and division.
Class refers to broad categories of
combustible materials, where Class
150
-5,000
300
= Rate of pressure rise in the test vessel
Figure 2. In typical tests results, Pmax is the top peak of the red line, while the
maximum rate of pressure rise (dp/dt) is used with Equation (1) to determine Kst
I includes all combustible vapors

and gases, and Class II includes all
combustible dusts
Group further defines the classes
based on the ease of ignition or the
rate of combustion of the combustible material
Division specifies the time periods,
frequency and length, during which
the combustible material is present
Unclassified areas are areas that
contain no significant amount of
combustible material at any time.
Electrical equipment installed in
unclassified areas should meet certain minimum standards to maintain operability and prevent personnel hazards
Once it has been determined that a particular area may contain combustible
materials, it is necessary to classify the
area according to Division and Group.
Division 1 locations are defined as
those where flammable or combustible mixtures are normally present
in sufficient quantities to present a
hazard
Division 2 locations are those where
flammable or combustible mixtures
are not normally present, but might
be present as the result of infrequent
malfunctioning of equipment
Based on the physical characteristics
of the materials handled, flammable
vapors or gases are assigned to Groups
A, B, C or D, and combustible dusts are
assigned to Groups E or G.
Bonding and grounding: Energy
levels far greater than 15 mJ, easily sufficient to ignite some dusts, are
obtainable via spark discharges from
ungrounded conductors. To dissipate
static electricity, adequate bonding and
grounding must be provided for solids
handling equipment and components,
including conveying, feeding, blending
and storage systems. Bonding is the
process of electrically connecting conductive components together so that
these are at the same electrical potential, and no sparks can occur between
them. Equipment such as a baghouse
can be comprised of a number of individual components: bag cages, bag
clamps, bag grounding wire and so on.
In such cases, it is important that each
of the components is properly grounded
and integrity of the grounding system
is routinely checked. Resistance to
ground shall be measured and documented for each major component.
Equipment skin-temperature limi-
tations: In addition to establishing a

number of other design and installation requirements, the skin (outside
surface) temperature of any equipment should not exceed 80% of the
auto ignition temperature (AIT) for
the dust being used.
Maintenance: Maintenance must
be provided to assure the integrity of
dust-tight electrical equipment. Periodic inspection is required to detect
and remove buildup of combustible
dusts inside the electrical equipment.
Design methods
When handling explosive dusts, the

following standards are used to design
the dust-explosion prevention or protection systems:
NFPA 68: Explosion venting
NFPA 69: Explosion prevention
NFPA 497M: Electrical classification of gases, vapors and dusts for
electrical equipment in hazardous
(classified) locations
NFPA 650: Pneumatic conveying
systems for handling of combustible
materials
NFPA 654: Fire and explosion prevention in chemical, dye, pharmaceutical and plastics industries
The use of these standards is described
below in more detail.
Explosion suppression systems. Explosion suppression systems prevent
high explosive pressures from developing in vessels by suppressing an explosion from starting at its source. These
systems consist of a detector system that
senses the start of an explosion, a pressurized container with an extinguishing
medium, and a fast-opening valve that is
activated by a pressure sensor through
a control-monitoring unit. The extinguishing medium is dispersed into the
protected vessel in a very short time in
order to reduce the expected maximum
pressure to a substantially lower level.
The detectors that trigger the explosionsuppression system are able to start the
suppression system rapidly. There are
three different types of sensors: thermoelectric, optical and pressure. Pressure
sensors are used more widely. The containers of the extinguishing medium are
equipped with fast-acting valves, which
open fully within milliseconds after the
activation signal is given. The valves
are designed to uniformly distribute the
whole contents of the extinguishing medium within a very short time.

To prevent flashback from occurring, a positive method of isolating the
explosion is required. For this isolation, devices such as mechanical decouplers, or fast-acting shut-off valves
are used to isolate the vessel.
The explosion-suppression method
is cost prohibitive for large equipment
and vessels, such as bins and silos. It
also requires diligent upkeep of the
control systems so that timely operation of the valves is not affected.
Explosion pressure containment.
Explosion pressure containment is a
technique to protect small-sized equipment by designing it to withstand the
internal pressure that is generated by
an explosion. This technique is cost
prohibitive for large vessels such as
bins and silos.
Vessels designed for explosion pressure containment are to be designed
and constructed according to the
ASME Pressure Vessel Code.
The design pressure of the vessel is
based on either the ultimate strength
of the vessel or on the yield strength
of the vessel.
The vessel is designed so that the
peak explosion pressure is less than
two thirds of the vessel burst pressure. Vessel design pressure is calculated by using the method given in
NFPA 69:
Pr =
1.5 Pmax
Fu

(2)
Where:
Fu = Ratio of ultimate stress divided
by the stress generated at the design pressure
Pr = Vessel design pressure to prevent
vessel rupture, psig
Pmax = Maximum deflagration pressure, psig
Note: If it is desired that the vessel
not be damaged as a result of the explosion, then Fy (the ratio of the yield
stress divided by the stress at the design pressure) should be substituted
for the ultimate stress in the above
equation. Yield stress is the stress at
which that the material deforms permanently; ultimate tensile stress is
the stress at which it breaks.
Inerting. This design method is used
to prevent dust explosions by reducing
the oxygen concentration to less than

that needed to support an explosion.
It is the preferred design method for
ignition-sensitive dusts. Ignition sensitive dusts are those whose sub-200mesh fraction has an MIE less than
10 mJ. It is also used for hybrid dusts
(dusts containing combustible gases).
When sufficient inert gas (typically nitrogen) is introduced, the
volumetric concentration of oxygen
is reduced to such a level that no ignition of the dust, combustible-gas
and air mixture can occur. The inert
gas must not be contaminated by air
or hydrocarbons.
A minimum safety factor of 2-vol.%
should be provided below the limiting
oxygen concentration (LOC) if either
of the following are true:
Oxygen-limiting control equipment,
analyzers and interlocks are installed to take positive action to prevent formation of an explosive mixture in the event of a failure (with a
pre-alarm and a shutdown alarm)
Or, if interlocks are not installed,
alarms should be provided, and
operating procedures should be
in place to prevent formation of a
mixture exceeding the maximum
oxygen concentration above which
deflagration can take place
If oxygen analyzers and alarms are
not used, the maximum oxygen concentration shall be maintained at no
more than 60% of the LOC, alarms
must be provided on loss of the inert
gas flow or pressure, and the oxygen
concentration must be checked on a
regularly scheduled basis. The integrity and consistency of all inerting
facilities must be established by periodic checking of the oxygen concentration. Low-flow alarms should be used
if procedures cannot be relied upon to
ensure that the inert gas is turned on.
For those operations relying entirely on control of oxidant as the
means of explosion protection (for instance, no explosion venting or other
methods for explosion protection are
provided), the percent O2 and inertgas flow systems should be considered as critical controls.
Maximum oxygen concentrations for
typical dusts can be found in NFPA 69.
Dust explosion venting method. This
method is used to prevent catastrophic
29
Cover Story
damage to equipment and facilities by
properly venting a dust explosion to the
outside atmosphere. It assumes that oxygen, a combustible mixture and a sufficiently strong ignition source are present so that a dust explosion can occur.
Catastrophic vessel failure is prevented
by providing rupture panels on vessels
for pressure relief and for discharge of
the explosive material, and by designing rupture panels so that the peak explosion pressure is less than two thirds
of the vessel burst pressure.
The rupture panels are also called
vents. Vents are openings in a vessel
through which combustion-generated
gases can expand and flow out. These
vents serve to limit the deflagration
pressure so that damage to the enclosure is limited to an acceptable level or
is eliminated entirely. The area of the
vents must be large enough to limit
the explosion pressure to a safe level.
Vents are designed so that they rupture and blow out, thus reducing the
pressure inside the vessel to a level
that is below the rupture-pressure
rating of the vessel.
The rate of pressure rise is an important parameter in the venting of
an explosion. It determines the time
that is available for the products of
combustion to escape from the enclosure and for the pressure to dissipate.
The higher this rate, the greater the
venting area that is required.
The vessel or equipment must be
designed to withstand the maximum
pressure attained during the venting
process without catastrophic failure.
Some yielding of the vessel or equipment is acceptable during a vented deflagration. For example, partial failure
of the roof-to-shell seam of a vessel is
not considered catastrophic failure.
Maximum pressure during venting
(Pred) should not exceed two thirds of
the static burst pressure of the protected equipment. If Pred exceeds 10
psig, an ASME Code vessel is required.
The vent opening pressure (Pstat)
should be set as low as practical to
minimize the rise in internal vessel pressure before the explosion is
vented. This reduces the potential for
damage, and for a given vent size, will
result in a lower maximum pressure
during venting. However, Pstat must
be high enough to prevent premature
30
opening of the vent by the combination of normal vessel-operating pressures and wind loads.
The following method for calculating
required venting area (Av, m2) is given
in NFPA 68 and here in Equation (3):
Av = a V 2 / 3 ( K st ) ( Pred )
b
(3)
Where:
Av = Required venting area, m2
a = 5.71 104 exp(2 Pstat)
b = 0.978 exp(0.105 Pstat)
c = 0.687 exp (0.0226 Pstat)
V = Empty vessel volume, m3
Kst = Dust deflagration index, bar-m/s
Pred = The reduced pressure (the maximum pressure actually developed in
the vessel during a vented explosion),
barg. The maximum pressure developed during a vented deflagration
(Pred) should not exceed 2/3 burst of
the vessel burst pressure.
Pstat = Pressure at which the relief device opens, barg. This is the pressure
at which the vent is expected to open.
It should be at least 0.5 psi greater
than the peak operating pressure of
the equipment. The minimum Pstat
used in the venting equations is 0.1
barg (1.45 psig).
The following best practices should
be observed for vents:
Vents should be designed to give a
free, unobstructed opening during a
deflagration
Access of personnel to areas that could
be exposed to fireballs coming out
from the deflagration vents should be
restricted unless deflector shields are
provided. Shields should not interfere
with the venting process
Panels shall be adequately tethered
by using chains or cables, where practical, to prevent them from becoming
missiles during the venting process
Vent panels should be located so
that they are not obstructed by the
solids level in the vessel. For example, by ensuring that the vent panel
bottoms are at least 1 ft higher than
the maximum solids level
Where side vent panels are used,
they should be symmetrically arranged around the perimeter of the
vented vessel
All equipment using explosion relief
panels should be located outside of
closed structures or buildings. If this
is not possible and the equipment

volume exceeds 8 ft3, the equipment
is to be vented to the outside through
a properly designed duct
Vent panels should be manufactured
by vendors who have special expertise in their design and testing
Vents can fail by rupture (for instance, metal fails in tension), or
they can fail by blowing out from
their frames or by failure of their
fasteners. When fasteners are used,
avoid spring-loaded latching devices
because they are not reliable
Buildings. Buildings that have properly designed and maintained dust
handling and process equipment do
not require explosion venting. However, damage-limiting construction of
the building is desirable. In locations
where environmental dust-concentration conditions exist, such as due to
poor maintenance and housekeeping,
building explosion venting should be
provided, as given in NFPA 68.
Dust collectors and bag houses.
Dust collectors and bag houses pose
significant dust explosion hazards because they inherently have a dusty
internal environment. Their tube
sheets and bag cages must be properly
bonded and grounded to prevent ignition caused by static charges. Properly
designed explosion vents should be
provided on the dusty side of the dust
collector. Dust collectors should be located outside of buildings or located
close to external walls. When installed
above bins and silos as bin vent filters,
use a rotary valve to prevent propagation of a dust explosion into the bin or
silo. When handling low-MIE dusts use
the inerting method, as described previously, instead of explosion vents.
Author
Amrit Agarwal is a consulting engineer with Pneumatic
Conveying Consulting (7 Carriage Road, Charleston, WV,
25314; Phone: 304-553-1350,
Email: polypcc@aol.com). He
started his consulting work
after retiring from The Dow
Chemical Co. in 2002 as a
senior research specialist. He
has more than 47 years of design and operating experience
in bulk solids handling and pneumatic conveying. He holds an M.S. in mechanical engineering from the University of Wisconsin-Madison,
and an M.B.A. from the West Virginia College of
Graduate Studies in Charleston.
Solids Processing
Prevent Explosions During Transfer

Of Powders Into Flammable Solvents
Martin Glor
Swiss Institute for the Promotion of Safety & Security
xplosion prevention must be

a primary objective wherever the process of transferring powders into flammable
solvents is utilized, irrelevant of the
industry and existing practices, in accordance with regulatory guidelines
such as the ATEX directives (Directive
94/9/EC, 1994 and Directive 1999/92/
EC, 1999), which prevail in Europe.
The addition of powders such as
catalysts, pigments and other reactants into a reactor, hopper or large
container is an extremely common operation within the chemical process industries (CPI). Frequently, the vessel
into which the powder is being added
will already be charged with flammable solvents in large amounts, or contain residual levels from previous use
or intermediate cleansing procedures.
The presence of flammable solvents
may create an explosive vapor atmosphere both within the vessel and in
the immediate environment, depending on the flashpoint of the solvent,
the temperature of the liquid and
the ambient temperature outside the
container. Equally significant are the
nature of the powder and the act of
transferring it. Whatever the combustibility of the powder, the combination
of the powders characteristics in addition to the transfer, increases the
potential for formation of an explosive
dust/air mixture, both in the container
and in the immediate surroundings.
The amalgamation of flammable solvent vapors and explosive dust/air
88
71
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Explanations of the development and

characteristics of explosive atmospheres
and the potential for an explosion to occur
are given, along with the advantages
and disadvantages of preventative practices

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Figure 1. The affiliation between methanols
mixtures can form a volatile vapor-pressure (VP) curve, the explosive range of
hybrid mixture.
its vapor and its flashpoint (FP) is similar to that
The presence of such ex- of most commonly used solvents. The majority of
plosion hazards, further common solvents have flashpoints below room temExplosive range of solvents also tends to
supported by incident sta- perature.
increase with increasing temperature. Note T(LEL)
tistics, corroborates the fact and T(UEL) are the respective temperatures at meththat this type of operation anols LEL and UEL
is clearly one of the most
hazardous within the CPI. Even if following basic principle: Prevent the
all effective ignition sources gener- formation of explosive atmospheres
ally considered common and insignifi- Where prevention due to the nacant, including those ignition sources ture of the process and materials is
related to electrical equipment, me- precluded, then the following criteria
chanical load, open flames, cutting, apply:
welding and smoking, have been ex- I gnition sources must be avoided
itigation of the detrimental effects
cluded through the introduction of M
precautionary measures, the hazard
of an explosion must be a priority to
of electrostatic ignition sources inherensure the health and safety of opent in the powder transfer will still
erators
remain a viable possibility for causing In conjunction with the above factors,
an explosion.
frequent reviews of the practices and
In short, the probability of an ex- processes in place must be carried
plosion occurring within the trans- out, the primary goal of which should
fer process is high. Furthermore the be to avoid propagating explosions. If
severity of such an explosion could any part of the process changes, then
be disastrous, especially when the additional reviews and precautionary
number of operators that would be di- measures should be introduced.
rectly exposed to the initial blast wave
and subsequent fireball are taken Probability and cause
into consideration. Serious, if not life Determining the risk of an explosion
threatening, burns are possible, espe- hazard is very important in assessing
cially in the presence of a dust cloud or how a process should be carried out
hybrid mixture explosion.
and whether adequate precautionIt is therefore paramount to ensure ary measures are in place. In order
that appropriate organizational, oper- to calculate the explosion risk assoational and technical systems relating ciated with charging a powder into a
to the nature of the process and the reactor already containing flammable
materials in use are in place in con- solvents, two main criteria need to be
junction with ATEX directives and the established:
Chemical Engineering www.che.com October 2007
88-95 CHE 10-07.indd 88
9/29/07 5:46:49 PM

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Figure 2. The vapor pressures of most commonly

used solvents reach the concentration of 20% of the
LEL at temperatures 3040 K below the flashpoint (FP)
T
he ignition sensitivity of the explosive atmosphere, which is categorized by the minimum ignition
energy (MIE)
The probability of an explosion occurring at different locations (highest probability during transfer of
powder into a flammable solvent occurs in the reactor above the solvent
surface, such as where vapors exist,
and at the manhole where powder
is charged into the reactor and turbulence is high, coupled with vapor
release from within the reactor).
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Figure 3. The opening of any access port and the addition

of the powder itself will cause a reactors previously inerted
atmosphere to be lost [10]
Factors such as the solvent vapor

pressure, powder characteristics
and ventilation are key
Once these criteria have been established, the risk of a specific ignition
source, such as static electricity, to create
an explosion can also be determined.
For most commonly used solvents,
the affiliation between their vaporpressure curve, explosive range of
their vapor and their flashpoints (FPs)
are well recognized (Figure 1). The
majority of universal solvents, including white spirit, toluene, acetone, ethyl
Excellence in solids-liquid separation and vacuum drying
acetate, ethanol, methanol and isopropanol, have flashpoints below room

temperature. The explosive range of
solvents tends also to increase with
increasing temperature.
Explosive dust clouds formed during
the transfer of powders can be located
within the reactor or at the point of
entry into the reactor, for instance
at the manhole and its surrounding
area. Particle size and distribution,
moisture content, concentration and
explosivity of the powder in its tumultuous state when being charged to the
Problems with
poor flowing
powder or
bulk solids?
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Solids Processing
reactor, make up the powder characteristics, which can then be expressed
in terms of the lower explosion limit
(LEL), MIE and minimum ignition
temperature (MIT).
When a dust cloud mixes with flammable solvent vapors, which can happen within the reactor or at the manhole, a hybrid mixture is formed. The
explosion risks of hybrid mixtures
have been extensively reported [1].
However, the most relevant points
regarding their characteristics are as
follows:
A
solvents MIE is generally much
lower than that of a pure powder;
therefore, when a hybrid mixture is
formed, its MIE as a rule will be somewhere between the two and tends to
veer towards the lower range, even if
the flashpoint of the solvent is above
ambient temperature
Regardless of whether the concentrations of the dust cloud and solvent
vapor are below their own LELs,
C
Ma
hybrid mixture is an entirely separate entity that may well be within

the explosive range
There are exceptions regarding
the explosive properties of a hybrid
mixture, specifically the MIE. If for
instance the vapor concentration is
below 20% of the LEL of the solvent,
the MIE of the pure powder would then
be representative of the explosion risk
for the hybrid. The vapor pressure,
temperature, LEL and flashpoint of
solvents are used in conjunction with
each other to determine the probability of a hybrid mixture forming under
any specific environmental conditions.
The 3040 K rule applies to this calculation, in that the vapor pressure
reaches a concentration of 20% of the
LEL at temperatures 3040 K below
the flashpoint of most commonly used
solvents (Figure 2).
Vapor atmospheres can also be created by charging powder where solor CY
solvent
Y vents
CM MY
CMY K residue, and therefore
vapors are not already present in the

reactor, as the powder itself may contain solvent residue capable of creating a vapor atmosphere. If solvent
residue in a powder is present at less
than 0.5% (by weight), the risk of a hybrid mixture being formed can be negated as a rule. The exception is when
the powder is ground up, allowing the
desorption of vapors and, therefore,
creating a vapor atmosphere.
A powders dispersibility and
method of transfer will affect whether
an explosive dust cloud will be present
within the whole reactor and in the
region around the manhole, consequently (and dependent on the presence of solvent vapors), hybrid mixtures may be formed throughout the
reactor as well as in and around the
manhole.
In the case of toluene or methanol,
which are solvents with flashpoints
only slightly below ambient temperature, the entire gas phase within the
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Inlets and outlets where you want them
Electropolished surfaces
Carbon or stainless steel
Perforated stainless baskets
Wire mesh linings optional
Filter bags to 1 micron
Inner baskets/bags for
2-stage action optional
Centrifugal separator action
Rosedale Products, Inc.

3730 W. Liberty Road, Ann Arbor, MI 48103
800-821-5373 or 734-665-8201 Fax 734-665-2214
filters@rosedaleproducts.com www.rosedaleproducts.com

90
88-95 CHE 10-07.indd 90
9/29/07 5:54:09 PM
reactor for instance, from

the liquid surface to the point
of entry (manhole) can be
filled with an explosive atmosphere. In their gas phases,
solvents are at their most ignition-sensitive concentration.
This is especially the case for
toluene. 4MVJDF
Conversely, if a solvent has
a low flashpoint (high vapor
pressure at room temperature)
the environment within the reactor will tend to be saturated.
In this instance the most explosive range will occur around
the manhole. However, if large
amounts of powder are conveyed into a reactor containing
a solvent with a low flashpoint,
the entrainment of air associated with the operation may
also cause the atmosphere
within the reactor to become
explosive.
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Process ignition sources
Static electricity. The occurrence of static electrical dis*TPMBUJPOWBMWF

charges at different locations
and during distinct phases of
the powder-transfer process,are
dependent on the methods
used for transferring the pow- Figure 4. There are a number of common lock systems available for transferring powder
der and charging it into the into an inerted reactor
reactor. Although electrostatic
ignition sources associated with the B
rush discharges from any non-con- B
rush discharges from the powder
packaging, the equipment and the opductive bag, bin, drum, container,
heap formed on top of the liquid
erators can in theory be removed with
and so on, from which the powder is
phase within the reactor
Cone discharges from the powder
the use of conductive materials, reliatransferred into the reactor
ble earthing and other such measures, Spark discharges from any conducheap formed on top of the liquid
discharges associated with the prodtive but not earthed auxiliary device
phase
ucts will remain. Substantial changes
used in the transfer procedure, in- Mechanical sparks and hot surto the product properties would be recluding, but not limited to, shovels, faces. A mixer is normally running
quired in order to remove the electrofunnels, chutes and pipes
in the reactor during the transfer of
static ignition sources within specific Spark discharges from the operator, powders into a liquid phase, to preproducts.
if he is not adequately earthed
vent lumps from forming and to blend
Details regarding the incendiary Brush discharges from any non-con- the products together. The rotating
properties of the electrostatic disductive auxiliary devices, such as mechanical seal on the agitators axis
charges related to gases, vapors, dusts
shovels, funnels, chutes and pipes
is a potential ignition source, and a
and hybrid mixtures are given in Ref. Brush discharge from the dust cloud hot surface potentially present on the
[2, 3].
formed within the reactor during axis is another that cannot be ruled
Typical possible discharges include
powder transfer
out. Additionally, mechanical faults
Spark discharges from any conduc- of the agitator, mechanical sparks
the following:
S
park discharges from any conductive but not earthed fixtures and fit- caused by the operation of the agitive but not earthed (grounded) bag,
tings within the reactor
tator, and hot surfaces that can be
bin, drum, container, and so on, from Brush discharges from the charged generated are also potential ignition
which the powder is transferred into
solvent, suspension or emulsion pre- sources of the explosive atmosphere
the reactor
loaded in the reactor
within a reactor.
88-95 CHE 10-07.indd 91
91
9/29/07 5:55:32 PM
Solids Processing
Table 1. advantages and disadvantages of the different powder transfer methods
Prevention of explosive atmosphere

Transfer to closed reactor, inerting possible
Entrainment of air with powder transfer highly
improbable
Entrainment of air within bulked product
excluded
Repeated inerting not required for transfer of
large quantities
Inert atmosphere maintained after transfer
Diffusion of flammable gases or vapors to surroundings excluded
Formation of dust cloud in surroundings not
expected
Other advantages
Required space (particularly above the reactor) low
Easy to clean
Mobile transfer system
Transfer into pressurized systems
Not depending on flow properties of powder
GMP (good manufacturing practice)
conformity
Transfer over large distances
Investments
Charge moist or solvent wet powder
For multipurpose applications
Provides manufacturing flexibility
Automated operation
Environmental Health & Safety
Manual
transfer
Docking
Specially
Two
Bucket/ FIBC
Vacuum
Screw
station
Rotary
chain
disvalve
transfer
designed
conveyor
valve
for conconveyor charge system
with lock
system
tainers
++
++
++
++
++
+++
++
+++
+++
++
+++
+++
+++
+++
+++
+++
+++
++
+++
++
+++
+++
+
++
+++
++
++
++
++
+++
+++
+++
+++
+++
+++
+
+
+
+
+
+
+
+
++
++
+
+
+
++
++
++
+
+++
+
+
+
+
+
+
+
+
++
+
++
+
++
+
++
+
+
+
++
+
++
+
+++
+++
+++
++
+++
(No); + (Sometimes); ++ (Usually); +++ (Yes)
Avoiding explosive
atmospheres
If an explosion occurs, not only is it

likely to cause significant damage to
equipment and the infrastructure of
the plant, but even worse, jeopardize
personnel and expose them to possible
injury or even death, which is unacceptable. It is clear, therefore, that operations where the transfer of powder
into reactors containing flammable
solvents, even where very sensitive
powders with MIEs below 10 mJ are
being transferred into solvent-free
vessels, should no longer be carried
out using open methods.
As previous sections have outlined,
it is nearly impossible to prevent the
formation of explosive atmospheres.
Also, the exclusion of effective ignition
sources from a process is not simple
and can in no way be a guaranteed
measure against explosion risks. In
this day and age, it is necessary to
utilize every possible precaution to
92
prevent explosions from happening in

order to reliably protect both personnel and plant.
In order to attain the required level
of safety for such transfer operations,
powders must be conveyed under inert
conditions, especially when the recipient vessel is preloaded with flammable
solvents. Inert conditions exist where
the oxygen content of the reactor is at
a level below the limiting oxygen concentration (LOC), where explosions
are no longer possible [1].
Reduction in the oxygen content
of a vessel is achieved with the addition of carbon dioxide, nitrogen or any
other inert gas (Ref. [6] expands on
the technical aspects of this practice).
However, as illustrated in Figure 3,
the opening of any access port and
the addition of the powder itself will
cause the reactor's previously inerted
atmosphere to be lost. The opening of
the manhole allows the inert atmosphere within the reactor to diffuse
into the surrounding environment

thus increasing the level of oxygen.
The addition of powder also increases
the oxygen level within the reactor
due the entrainment of oxygen within
the powder itself, and as a result of
the turbulence caused by the powder
swirling around in the oxygen-rich atmosphere outside and at the manhole
of the reactor. The LOC within the
reactor is compromised and the risk
of explosion is again present. Modern
technology provides the solution to
these problems; using any type of lock
to transfer the powder into an inerted
reactor is a safer operation.
Figure 4 illustrates some of the more
common lock systems available today.
Table 1 compares some of the existing
lock systems against criteria for prevention of an explosive atmosphere.
Notably, oxygen enrichment within the
reactor is a fundamental problem associated with all the lock systems, with
the exception of the Powder Trans-
88-95 CHE 10-07.indd 92
9/29/07 5:56:01 PM
$
$
$
$
7N
%LHN
% LHN
$POUBJONFOU
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and containment
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Consideration of the
safety aspects related
154%$4
to the transfer of pow
ders into flammable
%PDLJOHTZTUFN

atmospheres must also
154
incorporate measures

-BNJOBSGMPXCPPUI
that take the toxic
3PUBSZWBMWF
ity and the reactivity

of the powder being
4BGFUZ
0
1,000 2,000 3,000 4,000 5,000 6,000
transferred into ac"NPVOUPGQPXEFSUSBOTGFSSFE LH
count, especially within
the pharmaceutical inFigure 5. Oxygen enrichment during
Figure 6. Unlike specially designed powder
dustry. These factors,
transfer of powder into a preinerted vessel.
transfer systems, most contemporary methods
in addition to the everC1: Oxygen concentration in the reactor
for contained transfer of powders tend to be
before the transfer, V1: volume of the gas
more focused on the containment aspect and
more stringent quality
phase in the reactor before the transfer, D1:
do not incorporate the added need for improvcontrol and production
bulk density of the powder transferred, D2:
ing the safety of the process with regard to
standards, make the
skeletal density of the powder transferred
explosion risks
need for containment
fer System (PTS), as more powder is etal density) and/or large volumes of inevitable and should also make mantransferred into the reactor. Oxygen powders are being transferred. Figure ual handling obsolete.
enrichment is increasingly highlighted 5 illustrates the effect of oxygen enrichCurrently, the addition of powders
when products with low bulk density ment in the reactor due to the oxygen into reactors through open manholes
(apparent density as opposed to skel- entrained within the powder.
is still the norm in the CPI. The in*TPMBUPS

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88-95 CHE 10-07.indd 93
93
9/29/07 5:57:12 PM
Extract Technologies
Extract Technologies
Solids Processing
troduction of alternatives to
this method (Figure 6) tend to
be more focused on the containment aspect and do not incorporate the added need for improving the safety of the process with
regard to explosion risks.
Most contemporary methods Figure 7. Containers may be equipped with
for contained transfer of pow- flexible intermediate bulk containers (FIBC) fitders use gravity as the impetus ted with docking devices that enable a receiver
to charge the powder into a re- to be connected or disconnected in an almost
airtight manner
actor, which requires that multistory facilities be built. The powder is acteristics or high moisture content.
delivered to a higher floor and falls Cleaning and validation is an inherthrough a chute (due to the natural ent problem and increases proportioneffects of gravity) directly into the ately with the length of the chute.
production equipment. The problem of
Gravity charging as a process, itcontainment around the loading zone self, can be a safety issue. The process
is addressed by incorporating a lami- cannot be rendered completely inert
nar flow booth, for example, into the and the problems associated with inarea and a drum-lifting system within creasing the oxygen concentration
that to avoid the need for manual han- within the reactor are, significant, as
dling. In these instances, operators previously discussed. The use of inert
must still wear personal protective gases to reduce the oxygen content
equipment including full body suits, introduced to the reactor via the powmasks and, depending on the toxicity der is costly as large volumes of gases,
of the powder, external respiratory ap- such as nitrogen, are required with
paratuses.
this system. To counterbalance these
Alternatively, containers may be inadequacies, more solutions are reequipped with automatic connect- quired. Sophisticated instrumentaing valves (active and/or passive) or tion may need to be incorporated into
flexible intermediate bulk containers the system to monitor oxygen levels,
(FIBC; Figure 7) fitted with docking for instance, but it in turn increases
devices that enable a receiver to be the cost, and affects the reliability of
connected or disconnected in an almost the process by requiring calibration,
airtight manner. These systems enable maintenance and other repairs that
large quantities of powder (in excess of necessitate downtime. Or, the system
100 kg) to be transferred and reduce itself may have to be modified; chargthe requirement for manual handling. ing the powder into an empty reactor
This method is also suitable for proc- may address most of the safety issues,
esses where intermediate products but the efficiency of the process will
that require storage or isolation be- be compromised. The following points
tween phases.
illustrate the detrimental effects of
A product with high toxicity will re- charging powder into a reactor in the
quire more containment. Glove boxes absence of solvents:
roduction of static electricity as
offer one of the few practical solutions P
to protect the operator, product and
powder is introduced under dry conenvironment (Figure 8). The cost, howditions
ever, of this solution can often be pro- Damage to the reactor lining due to
hibitive, especially considering that
abrasion or corrosion
most glove boxes are rigidly designed Risk of damage to the agitator seal
for a specific use, require a large dedior the agitator itself due to large
cated area within the plant and are
amounts of solids at the bottom of
not ergonomically designed, therefore
the reactor
Increased mixing cycle and problemcausing operators discomfort.
The chutes used for charging the
atic product homogenization due to
powder into the reactors often get
the formation of agglomerates
clogged, so bridging can occur, espeATEX and other applicable standcially if the powder has poor flow char- ards determine the delimitation of
94
Figure 8. Glove boxes offer one of the

only solutions to protect the operator,
product and environment from a product
with high toxicity
zones within a process environment;

the choice of equipment, its setup and
the methodology employed within a
plant can directly impact the determination of zones. Therefore certain
zones may be downgraded, for example, where the plant would then benefit from operational advantages and
associated economic benefits.
Common to the majority of powder handling systems is the lack of
a physical barrier between the reactor and other production equipment
thus rendering the peripheral units
neither pressure nor explosion proof.
The operating pressure of the recipient vessel, temperature and presence
of flammable atmosphere are serious
safety risks, especially when charging
powder and even more so when powder is charged by gravity. There is an
increased risk of the powder loading
area developing an explosive atmosphere, which must therefore be classified as an explosive zone.
Economic constraints faced within
the process industry create a diversity
of challenges; from the conception and
implementation of a flexible production unit which complies with current quality control and safety legislation and is also capable of adapting to
changing demands in the marketplace
and future changes in policies to
maintaining the lowest possible overheads. Existing process systems that
may need updating to comply with
legislation and increase productivity
face even tougher fiscal dilemmas, as
the nature of such systems lend themselves to modification and often stipulate entirely new systems.
Having established that gravity
charging systems are fundamentally
unsafe, manufacturers face the predicament of a loss of productivity versus significant costs associated with
88-95 CHE 10-07.indd 94
9/29/07 5:57:44 PM
Deitrich Engineering Consultants
long distances (horizontally

and vertically). The problems
of designing new plants or
processes have to be solved by
discussing and considering all
arguments mentioned.
If a system is installed directly onto a reactor (or other
process equipment), for instance, the two systems can
be operated in isolation from
each other. The technology
should not only act to reduce
the oxygen content of the
powder before it is discharged
into the reactor, but also to
keep the atmosphere within
the reactor inert while powder is being charged into it by
Figure 9. Specially designed powder transfer
using nitrogen or other inert
systems specifically address the safety risks regas. Equipment should allow
lated to transferring powders into solvents
powder to be safely charged
addressing the inherent operative into a reactor, even one that contains
risks. The solution for manufacturers solvents or operates under pressure
is to use a system capable of isolating without the risk of explosions or gas
process equipment during the filling leaks.
stage and transferring powder in a
contained way.
Conclusions
A technology providing a total solu- Historically, operations where powtion to the problems faced by manufac- ders are transferred into reactors
turers including safety, containment have resulted most conspicuously in
and productivity has to be chosen. fires and explosions. The risks are inThe concept should lead to actively creased significantly where flammable
conveying powder of any characteris- solvents are also present within the
tics without using gravity, effectively process. A large proportion of such opin the same way liquids can be han- erations are still carried out manually,
dled. The principle used has to allow thus exposing the personnel involved
the transfer of powder from any recep- to immense safety risks.
tacle (container, drum, big bag, silo,
Either in the presence or absence of
process equipment and so on) over flammable gases or vapors, the MIE of
the powder and the method of transfer

can create the risk of an explosion. In
order to increase the safety of these
processes, transfer of powders should
be carried out in closed systems, the
recipient vessel should be inerted,
every precaution should be taken during and after the transfer to maintain
the lowest possible oxygen concentrations within the reactor, and the systems should be separated by a physical barrier.
Most gravity-based transfer systems offer poor levels of safety overall,
and risks are further compounded by
the nature of the material being transferred and the process conditions. This
is true to such an extent that an operation that is considered safe under
one set of parameters can be destabilized by changing one small aspect
of the system. A system that does not
use gravity, eliminates oxygen from
the powder, and has a physical barrier
between itself and the reactor during
loading can provide a safe solution for
powder transfer independent of the
nature of the powder and the process
parameters.
The importance of process optimization in conjunction with ever changing
safety and quality criteria means that
in order for manufacturers to effectively function in a competitive marketplace, the process technology they
choose to apply must be flexible, and
guarantee full safety of their personnel, product and equipment regardless
of the process parameters and powder
characteristics.
References
Author
1. Bartknecht, W., Explosionsschutz, Grundlagen und Anwendung, Springer Verlag Berlin, Heidelberg, New York, 1993.
2. BGR 132: Avoidance of Ignition Hazards
Due to Static Electricity, Hauptverband
der gewerblichen Berufsgenossenschaften,
Fachausschuss Chemie der BGZ, March
2003.
3. CENELEC: Technical Report CLC/TR 50404
Electrostatics Code of Practice for the
Avoidance of Hazards Due to Static Electricity, June 2003.
4. ATEX 95: Directive 94/9/EC of the European
Parliament and of the Council of 23 March
1994 on the approximation of the laws of the
Member States concerning equipment and
protective systems intended for use in potentially explosive atmospheres, 1994.
5. ATEX 137: Directive 1999/92/EC of the European Parliament and of the Council of 16
December 1999 on minimum requirements
for improving the safety and health protec-
tion of workers potentially at risk from explosive atmospheres (15th individual Directive
within the meaning of Article 16(1) of Directive 89/391/EEC), 1999.
6. ESCIS (Expert Commission for Safety in the
Swiss Chemical Industry): Booklet 8, Inerting Methods and Measures for the Avoidance of Ignitable Substance-Air Mixtures
in Chemical Production Equipment and
Plants, 1993.
7. Fishwick, T., Loss Prevention Bulletin, 171,
7, 2003.
8. Glor, M., Journal of Loss Prevention in the
Process Industries, 14, pp. 123128, 2001.
9. Glor, M., Proceedings of the 11th Symposium
Loss Prevention 2004, Praha, Congress Centre, pp. 22332241, May 31June 3, 2004.
10. Hoppe, T. and Jaeger, N., Proceedings of 39th
Loss Prevention Symposium of the American
Institute of Chemical Engineers, April 1014,
2005, Atlanta, Ga., 2005.
Martin Glor is a member

of the Executive Committee of the Swiss Institute for
the Promotion of Safety &
Security (WKL-32.3.01., P.O.
Box, CH-4002 Basel, Switzerland; Phone: +41 (0)61
696 22 11; Fax: +41 (0)61 696
70 72; Email: martin.glor@
swissi.ch). He has been with
the Swiss Institute for the
Promotion of Safety & Security and a member
of the Executive Committee, Head of Risk Consulting since 1997. Before that, he worked with
Ciba-Geigy AG in Basel, Switzerland, serving as
head of the explosion technology/electrostatics
dept. Glor is the author and coauthor of several
books on electrostatics and a large number of
publications in the field of explosion technology
and electrostatics. Meanwhile, he is either the
chairman or member of numerous international
committees and the recipient of several prestigious professional awards. He holds a Ph.D. in
experimental physics from the University of
Basel, Switzerland.
88-95 CHE 10-07.indd 95
95
9/29/07 5:58:22 PM
Solids
Environmental
Processing
Manager
Preventing
Dust Explosions
Risk management programs are critical
for safe handling and processing of combustible dust
as well as for OSHA regulatory compliance
Geof Brazier and Mitch Rooker
BS&B Safety Systems, LLC
ousehold items, such as

breakfast cereal, flour, corn
starch and sugar are so common that many were left
surprised after the 2008 combustibledust explosion at a sugar refinery in
Georgia. Heard in much of the early
media coverage was the question How
could sugar explode?
Plant explosions are, thankfully, not
routine occurrences. However, when
they do occur, it is the unusual event
often a combination of abnormal
events that is typically the trigger.
This article outlines some of the guidelines that are available to help prevent
dust explosions. It also offers a list of
factors to consider when choosing explosion vent technology to minimize
combustible-dust-explosion hazards.
The facts are that in the U.S. and
elsewhere, the chemical process industries (CPI) are working to minimize the risk of combustible dust explosions by following a revised suite of
National Fire Protection Association
(NFPA) standards, that are recognized by the U.S. Occupational Safety
and Health Administration (OSHA).
A documented combustible-dust, riskmanagement program that is regularly updated, forms the cornerstone of
a plants owner/operator responsibility
to provide a safe workplace. Identification of areas of risk, along with implementation of prevention and protection strategies, achieves compliance
with these safety standards.
OSHAs Combustible Dust National
Emphasis Program (NEP) and the NF-
PAs current standards define best engineering practices and are designed to
protect both personnel and plant from
combustible dust explosions. These
standards are typically adopted by state
fire marshals, insurance companies,
consultants and their legal representatives and are referenced by the OSHA
NEP. OSHA can and does issue safety
citations in relation to combustible dust
risks. Its citations are based on the General Duty Clause whereby the owner/
operator of a facility shall provide a safe
workplace, as well as by reference to
specific NFPA standards including 61,
68, 69, 86, 484, 499, 654, and 664.
OSHAs NEP
OSHA introduced the Combustible

Dust National Emphasis Program in
October 2007 issued by the Directorate
of Enforcement Programs and revised
it on March 11, 2008 with directive
number CPL 03-00-008*. This document describes OSHAs policies and
procedures regarding inspection of facilities that handle combustible dust
as well as their expectations regarding
owner/operator compliance with U.S.
safety standards. The scope is national
and administered by national, regional
and area offices of OSHA or the officials of participating state programs.
Its focus includes the following three
technical areas of risk management:
1) Dust control
2) Ignition control
3) Injury and damage control
Dust control. To summarize, dust
control is achieved by the implementation of appropriate combinations
* Available for review on www.bsbipd.com
Figure 1. This photo

shows the effects of
pneumatic transport of
powder to a silo through
a hose not designed
to conduct away static
electricity. The friction
caused by static electricity has created enough
heat to cause a hole to
form.Code compliance
with OSHA requires continuous monitoring of
potential ignition hazards,
including the control
of static electricity and
process equipment hot
spots, similar to the pictured example
of housekeeping and dust collectionand-filtration measures. These measures are combined with inspection to
ensure that they remain effective. A
layer of dust that is only 1/32-in. thick
is a concern when it covers 5% or more
of a workplace floor area that has
dust-laden structural members, such
as joists and I-beams. Successful dust
control reduces fugitive emissions of
combustible dusts, which in turn cuts
the dust explosion risk.
Quantification of a combustible
dust risk requires that the characteristics of the material be identified
by test. Key parameters include the
maximum explosion pressure (Pmax),
the deflagration index (Kst) and the
minimum ignition energy (MIE) of the
dust. Prevention and protection strategies must also be based on knowledge
of process conditions, such as dust concentration, airflow velocity, operating
pressure, temperature and humidity.
The higher the Kst value, the faster
the rate of pressure rise due to combustion. Kst values above 600 are
considered extremely explosive. Most
common plant dusts have Kst values
between 100 to 150. Even if a plant
owner/operator knows the characteristics of a particular dust, a sample must
be tested under NFPA 68. Particle size
can profoundly affect explosive properties, as the finer the dust, the higher
the Kst value. For example, sugar has
a recorded Kst value of about 138. Of
more concern with regard to the potential damage to process equipment
is the fact that a fine-sugar-dust explosion will generate a pressure in excess
of 100 psi within an enclosed volume in
less than 100 milliseconds. Other key
49
parameters include particle size, with
smaller particles equating to more
rapid combustion and easier ignition.
The reason is that more surface area
is freely accessible by the surrounding
air to support combustion.
Ignition control. Understanding and
monitoring for potential ignition hazards at a plant provides a first layer
of protection to the facility. Essential
measures include proper grounding
and bonding of equipment and ducting, appropriate wiring of electrical
equipment, the control of static electricity (see Avoiding Static Sparks in
Hazardous Atmospheres, CE, June
2009, pp. 4449) and monitoring of
process equipment hot spots (Figure
1). Preventive maintenance programs
ensure that such design safety measures remain effective.
Review of dust-explosion loss history
proves that it is important to consider
normal and potential abnormal circumstances while evaluating processes
within a facility. Many times a dust
explosion is the result of an abnormal
event, such as when an automated process fails and it is replaced by a temporary, manual activity. Other times
it could be a consequence of a change
in product packaging. For example, an
operator at a manual bag-emptying
station receives a shrink wrapped pallet of bags. Instinctively, he walks toward the pallet, across a concrete floor,
while wearing appropriately specified
conducting shoes. The surrounding
metal equipment is grounded. The operator stands on shrink-wrap-packaging material (an insulator) as it is unwrapped, tears open a bag of material
and empties it into an adjacent hopper.
As the dry powder flows, static charge
builds on the now insulated operator
until there is sufficient electrical potential to release a spark having sufficient energy to ignite the dust present
in the emptying station.
Injury and damage control. The
OSHA NEP anticipates the deployment of specialty technology to mitigate the effects of a dust explosion.
Referenced techniques fall into the
following four areas:
Prevention: Detection of sparks and
embers traveling through a dust
collection system can lead to their
quenching before reaching an area
50
Figure 2. Isolation introduces a barrier to flame

propagation that can prevent
a primary dust explosion from
amplifying into a secondary fire
and explosion in an interconnected piece of equipment. This
example shows chemical barrier
isolation on a 36-in.-dia. duct
Figure 3. In
this illustration,
the explosion
suppression system extinguishes
the fireball as it
occurs, rapidly
injecting a heatquenching agent
into the tanks and
duct to extinguish
the fireball. The
outside world
does not hear or
see the fireball.
The readings from
the sensor and
monitor are the
only indication
that an explosion
has occurred
of high dust-explosion risk, such as

a filtration unit
Isolation: Introducing a barrier to
flame propagation can prevent a
primary dust explosion in one piece
of equipment from amplifying into
a typically more-severe secondary
event in a connected item of equipment. Solutions include chemical
isolation (particularly well-suited
to large or irregular-shaped ducting) and mechanical isolation barriers (Figure 2), such as pinch valves,
knife gate valves and rotary airlocks
Venting: Pressure relief is provided
to process equipment and to building
structures by releasing the products
of combustion to the atmosphere in
a safe trajectory. Flameless venting
provides for over-pressure protection without the release of flame
or particulates to the atmosphere
when following the requirements of
NFPA68-2007
Suppression: Explosion effects can
be minimized by injecting a flame
quenching agent into process equipment to arrest the combustion process explosion suppression equipment responds rapidly to prevent
the full development of a dust explosion, preventing a destructive overpressure from developing (Figure 3)
In addition, an emergency action plan

with properly maintained exit routes
ensures the right safety response for
protection of personnel.
Understanding the risks
The course of action to minimize combustible-dust-explosion hazards begins, preferably, in the planning stages
of a process by identifying the risks,
determining the explosive reactivity
of the combustible process dust, and
implementing a combination of both
prevention and protection measures.
Economic considerations favor the
use of explosion vent technology in
terms of cost of equipment and installation. However, many factors must be
considered before choosing explosion
vents. Consider the following application factors:
Can the flame ball that is ejected
from an open vent be accepted? It
will usually extend 30 to about 100 ft in
length and about half this in diameter.
An 1,800-ft3 vessel venting from a single
position will produce a flame ball over
100 ft in length and 50 ft in diameter.
Simple free venting must be directed to
a safe location where personnel will not
be present and other equipment cannot
be damaged (Figure 4).
If venting equipment is installed
Figure 4. The photo shows explosion

venting of a dust collector.A vented
flameball is a mass of dust and combustion gases over 2,000F that may extend
30100 ft from the point of exit. Simple
free venting must be to a safe location
where personnel will not be present and
other equipment cannot be damaged
indoors, can a vent duct to a safe

outdoor location be provided?
Vent ducts will always increase the
required vent area, and their use may
not allow smaller process volumes at
higher Kst values to be protected by
venting at all.
Can the required vent area be accommodated? As well as requiring the
space for vent installation, can the reaction forces during venting be sustained
and, for tall equipment, can a nearthrust, neutral vent arrangement (topsidewall-mounted vents) be achieved to
prevent collapse during relief?
If there are process inlets and outlets to the protected equipment,
are these protected to prevent
propagation of the dust explosion
to other equipment or work areas?
Authors
Geof Brazier serves as president of Industrial Protection
Devices, LLC and as the director of product and market
development for BS&B Safety
Systems, LLC (7455 East
46th St., Tulsa, OK 74145;
Phone: 918622-5950; Email:
gbrazier@bsbsystems.com).
He holds more than 20 U.S.
patents in the areas of pressure-relief and industrial
wireless devices. Brazier also collaborates with
the Minnesota Workplace Safety Consultation organization in providing seminars about OSHAs
Combustible Dust NEP. He was educated at the
University of Bristol in England as a physicist.
Mitch Rooker is a senior
development engineer at
BS&B Safety Systems LLC
and along with his co-author,
serves as a member of the
NFPA Committee on Explosion Protection Systems. He
has more than 30 years of experience in research, design
and development of industrial
products and many patents in
the area of overpressure protection. He holds a degree in Mechanical Engineering from the University of Oklahoma.
Standards are now very clear in requiring isolation of vented equipment

to prevent secondary explosions. Secondary explosion risks are typically
much greater in their potential for
damage and destruction.
Can the clean up of a vented explosion be accepted? Depending upon
the design basis adopted, a vented
explosion may require replacement of
capital equipment components that
have become damaged by the pressure
wave, resulting in loss of production
while delivery is awaited. Most vented
equipment is designed with a pressure relief area that prevents failure
of the equipment structure. A higher
vent area is always required to protect
equipment within its design pressure.
What will the neighbors think?
A vented explosion is a spectacular
event that will draw considerable
community attention.
What if the process material is
toxic or hazardous? A vented re-
lease must simply be avoided for certain materials.

As illustrated by the previous series
of questions posed for a vented-dustexplosion application, each process
needs to be considered both alone and
as a component of a production facility to ensure that the right explosion
protection and prevention technology
is implemented. There are always options for dust-explosion-risk management. The technical solutions adopted
must take proper account of the practical needs of each process and the consequences of safety system operation.
Some final rules of thumb include:
plan for the abnormal; and maintain
a strict management of change policy
that will catch the potential consequences of product material changes,
hardware changes, and procedural
changes. Dust-explosion-risk management requires periodic detailed review,
even at the best-protected facility.

For custom fabrication,

Mueller is the obvious choice.
Specialty isnt just our name,
its what we do. For over 50
years, Mueller Steam Specialty
has been the preferred source
for the widest variety of special
service valves and strainers
in the industry. This capability
is further enhanced with the
addition of in-house fabrication. Using state-of-the-art cutting, fabricating, and welding
equipment, our ASME-certified
craftsmen manufacture to our
customers specific needs.
Quality is assured by in-house,
dedicated Design Engineering
professionals.
Designed, Engineered and
Manufactured in the USA
muellersteam.com
A Watts Water Technologies Company
51
Feature Report
Engineering
Practice
Compressed Gases:
Managing Cylinders Safely
Richard Palluzi
ExxonMobil Research & Engineering
ompressed gas cylinders are

widely used in research, pilot
plant, laboratory and smallscale manufacturing and processing operations as a way to provide
a convenient, economical and safe
source of high-pressure gases for various applications. These gases can be
inert, flammable, toxic or oxidizing (or
mixtures of any or all), and are typically supplied at pressures from 800
to 6,000 psig, with 2,250 psig being
common. A compressed gas is defined
by the U.S. Department of Transportation (DOT) as any materials or mixtures in containers having an absolute
pressure in excess of 40 psi at 70F, or
in excess of 104 psi at 130F.
Cylinder basics
Gas cylinders have several major components, including the cylinder body,
a steel or aluminum cylinder with a
strengthened, threaded neck, a flat
bottom rim for standing level, the
valve assembly to control the gas flow,
and a protective cap. Each cylinder is
stamped with its design information,
as shown in Figure 1. Items of particular interest include the cylinder size
(which is required for calculating the
content volume), the cylinder maximum design pressure, and the cylinder test date.
If it is past the test date indicated
on the cylinder, the cylinder can be
transported and the contents can still
be used, but the unit cannot be refilled. Nearly all manufacturers label
their cylinders with a stick-on label
that provides the type of information
shown in Figure 2.
Different manufacturers refer to
their cylinders by a variety of different terms, and not all manufacturers
provide all sizes. The most common
sizes are shown in Table 1.
In the U.S., gas cylinder design and
construction is governed by DOT codes.
52
Follow these recommendations to ensure the safe

handling, storage and use of gas cylinders
Rarely does a user need to worry about
how a given cylinder is designed. One
exception, however, is when the user
is asking for a specialty cylinder for
a non-standard application, such as
a specialty gas made specifically for
a one-time application, a sample of a
new mixture, or similar one-of-a-kind
uses. Specialty cylinders that are significantly past their date (by two years
or more), should not be used; rather,
they should returned to the supplier
as soon as this fact has been discovered. Cylinders provided by specialty
suppliers for non-standard sources
should be confirmed to be adequately
designed before being accepted.
Gas cylinders are designed to be
transportation vessels not pressure
vessels. As such, they are not usually
intended to replace a well-designed
pressure vessel. In particular, DOT
design standards are not intended
to adequately cover pressure cycling.
Most DOT vessels will only be rated
for ~60% of the comparable American Society of Mechanical Engineers
(ASME) rating. Hence, before using
any gas cylinder as a pressure vessel
(such as an accumulator), the design
should be reviewed by both a pressure
vessel expert and the vessel manufacturer. In most cases, using the cylinder
will not prove to be the best course.
For these applications, a properly designed and constructed ASME-code
vessel is the proper choice.
Pressure relief
Gas cylinders are protected from overpressure in several ways. A pressurerelief device is always installed in the
neck of the cylinder (Figure 1). A variety of such devices may be used, depending on the supplier and the gas:
A rupture disk (CGA code CG-1).
This device consists of a thin piece of

metal that is designed to burst and
release the cylinder contents to the
atmosphere. The rupture disk setting may not exceed the minimumDOT-required test pressure of the
cylinder, which is usually 167% (5/3)
of the cylinder service pressure. It
may not exceed 4,500 psig for the
DOT-3E or CTC-3E specification cylinders, nor be less than 105% of the
cylinder test pressure, or greater
than 80% of the minimum burst
pressure for DOT-39 cylinders.
A fusible link (CGA code CG2 or
3). This device relies on a metal link
that is designed to melt at a given
temperature and release the cylinder contents to the atmosphere. Fusible links are generally set between
165 and 220F.
A combination rupture disk and
fusible link (CGA code CG 4 or
5). In this design, a fusible plug is
provided on the atmospheric side
of the rupture disk. The burst pressure of the disk may not exceed the
minimum DOT-required test pressure of the cylinder, and the fusible
link must melt or extrude between
157 and 220F. Such an assembly
is designed to prevent a release in
the event of a small external fire (in
which case the fusible link may fail
but the pressure not rise sufficiently
to burst the rupture disk), or a premature failure of the rupture disk
(in which case the fusible link will
remain intact).
A spring-loaded relief device
(CGA code CG7). This device is
designed to open when the pressure exceeds a set value and to close
again once the excess pressure is
relieved. These are relatively uncommon in most gas cylinders due
8
1a
1
1b
1c
Figure 2. The
manufacturers label
provides critical information to assist
the end user
3
4
6
5
DOT3AA-2265
AH-89694
MC
3 H 32
Table 1. Common Cylinder Dimensions and capacities

Size
DOT
specifications
Nominal dimensions* (Excluding

valve & cap), in.
Average tare
weight, lb
Average
internal
volume, ft3
3AA2400
9 x 55
137
1.76
3AA2265
9 x 51
119
1.55
3A2015
7 x 33
57
0.56
D-1
3A2015
7 x 19
26
0.26
3AA2015
4 x 17
0.10
4X
3AA2015
4 x 13
6.6
0.075
L.B.I.
3E1800
2 x 12
0.015
L.B.
3E1800
2 x 12
0.015
Medical E
3AA2015
4 x 26
14
0.16
BX
3AA6000
10 x 51
300
1.49
BY
3AA3500
9 x 51
187
1.53
3A480
10 x 49
85
1.93
3A480
10 x 36
90
1.28
3A480
8 x 22
33
0.53
AA
4AA480
15 x 52
160
4.46
A1
4BW240
16 x 50
75
3.83
A-2
4BW240
22 x 48
167
7.64
8/8AL
12 x 41
185
2.36
3A1800
24 x 90
1,108
15.83
106A800X
30 x 82
2,254
25.82
106A500X
30 x 82
1,400
25.64
A(Al)
3AL2216
10 x 52
90
1.64
B(Al)
3AL2015
8 x 48
48
1.04
C(Al)
3AL2216
7 x 33
32
0.56
D-1(Al)
3AL2216
7 x 16
15
0.21
4X(Al)
3AL1800
4 x 10
3.3
0.057
3BN400
7 x 45
88
0.65
D-1
3BN400
7 x 22
48
0.28
D-2
3BN400
5 x 15
10
0.10
55 gal
UN1A1
24 x 45
175
7.35
10 gal
UN1A1
14 x 29
50
1.34
5 gal
UN1A1
9 x 24
25
0.67
High pressure
1
1a
1b
1c
2
3
4
5
6
7
8
Cylinder shut-off valve packing nut

Cylinder shut-off valve
CGA outlet connection
Cylinder pressure-relief device
(relief valve, rupture disk or fusible link)
CGA outlet cap to protect threads
and keep clean
Threaded cylinder collar to accept
protective metal cap
DOT specification (3AA) and service
pressure (2,265 psig)
Manufacturers serial number
Manufacturer's symbol (MC)
Test date (3/89)
Cylinder cap
Figure 1. Key components of an

appropriately appointed compressedgas cylinder are shown here
to their larger size, higher cost and

greater complexity. The relief device setting must be greater than
75% and less than 100% of the
cylinders minimum test pressure
with a reseating pressure greater
than the pressure in a normally
charged cylinder at 130F. The relief
device on DOT-39 cylinders must
not exceed 80% of the minimum
burst pressure of the cylinder nor
be less than 105% of the cylinder
test pressure.
Meanwhile, heating is often required
for calibration gases (to prevent condensation) and liquefied petroleum
gases (to vaporize the liquid or increase
the delivery pressure). No matter
which type of device is used, the potential for cylinder overheating remains a
concern. In all cases, gas cylinder
heating should be carried out by
indirect methods using steam, hot
water, hot air enclosures or similar
heated enclosures.
While some manufacturers supply
electric heating blankets, these should
be considered a higher-risk alternative. The electric heating elements
often operate well above the fusible-
Low pressure
C2H2
A
HCI and bulk electronic gases

Y
H2S
T
SO2, C2H5Cl, Cl2, CH3Cl

T
Aluminum
Nickel
Stainless steel
*These dimensions are not exact. They should not be used for engineering
drawings or equipment specifications.
53
link, relief-valve or rupturedisk setting (8001,100F is
common) even when operating
at lower temperatures. Hence
the heating elements rely on
the control system (whether automatic or manual) to limit the
cylinder temperature to a value
below that required to initiate
the relief device. The Box on p.
58 shares some simple guidelines for safe hot-box design.
Regulations and codes
Wall
Cylinders not adequately supported

Wall
Adjustable bay
storage rack
Wall
Secured storage in
public access area
Eye bolt
Figure 3. Unless they are properly secured, compressed-gas

cylinders can fall and present a hazard in the workplace. Examples of
proper procedures for securing gas
cylinders are shown here
In the U.S., specific requireChain

Latch
ments from the Occupational
Safety and Health AdministraDetail: eye bolts, chain,
Individually supportrd
and latch
cylinders
tion (OSHA) for gas cylinders
are rather minimal:
Meanwhile, the National Fire Pro- reaching 52C (125F) or above on
OSHA 1910.101 (a) requires routine
inspections per DOT regulations tection Association (NFPA) addresses hot summer days.
[49CFR parts 171179, and 14CFR gas cylinder usage in several codes.
Exterior storage areas should be
The the two most prominent are kept clear of weeds, grass and similar
part 103]
OSHA 1910.101 (b) requires that NFPA-55: Storage, Use and Handling combustible vegetation for at least 15
in-plant handling, storage and utili- of Compressed and Liquefied Gases ft around the perimeter of the cylinder
zation shall be per Compressed Gas in Portable Cylinders, and NFPA-45: storage area. Flash ground fires can
Fire Protection for Laboratories Using easily span this distance in a matter of
Association CGA P-1-1965
OSHA 1910.101 (c) requires all cyl- Chemicals. NFPA-55 is intended more minutes far too fast for emergency
for industrial applications, focusing responders to intervene effectively.
inders to have safety-relief devices
Similarly, in several other parts, on larger volumes and manufacturAll storage areas should also be
OSHA 29CFR provides some more- ing applications. In fact, NFPA-55 clearly marked as No Smoking areas.
specific requirements for larger-size specifically excludes laboratory appli- Protection against vehicular collision
installations that are typical of full- cations and storage in 1.1.2 (0) from is also necessary. Remember that the
the scope of the standard. NFPA-45 delivery vehicle may well be the most
scale industrial plants:
1910.253 Oxygen-Fuel Gas Welding addresses cylinders in detail in Chap- likely source of the collision so facilities
ter 11 but explicitly excludes pilot should plan accordingly for positive
and Cutting
plants in 1.1.2 (2). Where pilot plants protection that is designed to withstand
1910.102 (Acetylene)
are covered remains somewhat un- the strongest anticipated collision.
1910.103 (Hydrogen)
certain. Some organizations apply
1910.104 (Oxygen)
Regardless of where the gas cylNFPA-45 (despite the specific exclu- inders are stored, they should all be
1910.105 (Nitrous Oxide)
These are generally for larger site- sion), others apply NFPA-55 despite properly secured from falling (Figure
what seems to not be the intent, and 3). Except when stored in a properly
wide or plant-wide installations.
Meanwhile, DOT addresses cylin- some apply neither.
designed central storage facility with
ders in depth in several regulations
their metal protective caps on, gas cyl(namely, 49CFR parts 171179 and Proper storage
inders should not be secured in large
14CFR part 103), but these are gen- Storage areas should be located away groupings. When the chain or rope is
erally restricted to the transportation from sources of excessive heat and removed, it is possible for a group of
aspects and do not affect laboratory potential ignition. Care is required to cylinders to fall, creating a hazard.
research or other end-use applica- ensure that all cylinders are protected Cylinders should be secured in smaller
tions except with regard to receiving against heating above 52C (125F). groups of not more than 46 cylinders,
cylinders or shipping out materials in Storage areas should also be secured as an added precaution.
cylinders. DOT regulations do prohibit against unauthorized personnel and
When installed for use, all gas cylinrefilling of any cylinder without the must be properly ventilated. They ders should be individually secured at
manufacturers permission (although should be located at least 30 ft from 1/2 to 3/4 of their height to a fixed supobtaining the manufacturers permis- any air intakes at the facility.
port. Movable benches, rolling tables
sion in this litigious age can prove to
Exterior storage areas should al- and similar objects should never be
be challenging). Fortunately, such ap- ways have a roof to keep cylinders used as supports. A cylinder-transport
plications, while rare, may need addi- out of direct sunlight. Even cooler cart, while very useful for transporting
tional time and effort to be addressed. climates can result in cylinders cylinders safely, should never be used
54
Table 2. NFPA-55 Maximum Allowable Quantity of Gases per Control Area
(Quantity Thresholds for Gases Requiring Special Provisions)
Material
Unsprinklered areas
No gas cabinet, gas
room, or exhausted
enclosure
Sprinklered areas
Gas cabinet, gas
room, or exhausted
enclosure
No gas cabinet, gas

room, or exhausted
enclosure
Gas cabinet, gas

room, or exhausted
enclosure
Corrosive gas
Liquefied
68 kg (150 lb)
136 kg (300 lb)
136 kg (300 lb)
272 kg (600 lb)
Non-liquefied
23 m3 (810 ft3)
46 m3 (1,620 ft3)
46 m3 (1,620 ft3)
92 m3 (3,240 ft3)
Flammable
0 L (0 gal)
170 L (45 gal)
170 L (45 gal)
170 L (45 gal)*
Oxidizing
170 L (45 gal)
340 L (90 gal)
340 L (90 gal)
681 L (180 gal)
Cryogenic fluid
Flammable gas
Liquefied
114 L (30 gal)
227 L (60 gal)
227 L (60 gal)
454 L (120 gal)
Non-liquefied
28 m3 (1,000 ft3)
56 m3 (2,000 ft3)
56 m3 (2,000 ft3)
112 m3 (4,000 ft3)
0 kg (0 lb)
2.3 kg (5 lb
0 kg (0 lb)
4.5 kg (10 lb)
Highly toxic gas

Liquefied
Non-liquefied
m3
(0
ft3)
0.6
m3
(20
ft3)
m3
(0
ft3)
1.1 m3 (40 ft3)
Nonflammable gas
Liquefied
No limit
No limit
No limit
No limit
Non-liquefied
No limit
No limit
No limit
No limit
Oxidizing gas
Liquefied
57 L (15 gal)
114 L (30 gal)
114 L (30 gal)
227 L (60 gal)
Non-liquefied
43 m3 (1,500 ft3)
85 m3 (3,000 ft3)
85 m3 (3,000 ft3)
170 m3 (6,000 ft3)
0 kg (0 lb)
0 kg (0 lb)
1.8 kg (4 lb)
3.6 kg (8 lb)
Pyrophoric gas
Liquefied
Non-liquefied
m3
(0
ft3)
m3
(0
ft3)
1.4
m3
(50
ft3)
2.8 m3 (100 ft3)
Toxic gas
Liquefied
68 kg (150 lb)
136 kg (300 lb)
136 kg (300 lb)
272 kg (600 lb)
Non-liquefied
23 m3 (810 ft3)
46 m3 (1,620 ft3)
46 m3 (1,620 ft3)
92 m3 (3,240 ft3)
0.5 kg (1 lb)
1 kg (2 lb)
Unstable reactive (Detonable) gas, Class 3 or Class 4

Liquefied
Non-liquefied
0 kg (0 lb)
0
m3
(0
0 kg (0 lb)
ft3)
m3
(0
ft3)
0.3
m3
(10
ft3)
0.6 m3 (20 ft3)
Unstable reactive (Non-detonable) gas, Class 3

Liquefied
1 kg (2 lb)
2 kg (4 lb)
2 kg (4 lb)
4 kg (8 lb)
Non-liquefied
1.4 m3 (50 ft3)
3 m3 (100 ft3)
3 m3 (100 ft3)
6 m3 (200 ft3)
227 L (60 gal)
227 L (60 gal)
454 L (120 gal)
Unstable reactive gas, Class 2

Liquefied
Non-liquefied
114 L (30 gal)

21
m3
(750
ft3)
43
m3
(1,500
ft3)
43
m3
(1,500
ft3)
85 m3 (3,000 ft3)
Unstable reactive gas, Class 1

Liquefied
No limit
No limit
No limit
No limit
Non-liquefied
No limit
No limit
No limit
No limit
Note: The maximum quantity indicated is the aggregate quantity of materials in storage and use combined.
*A gas cabinet or exhausted enclosure is required. Pressure-relief devices or stationary or portable containers shall be vented directly outdoors or to
an exhaust hood.
as a support for a cylinder without its

protective cap in place.
All storage areas should also be
well-ventilated. While laboratories
usually have high exhaust rates that
are capable of handling routine leaks
from gas cylinders, some may be inadequate to handle significant releases, particularly for toxic or lique-
fied gases. Enclosed interior storage

spaces are a particular concern as the
modest exhaust capacity provided is
often overwhelmed by even a small
leakage (and would be unable to safely
evacuate a full cylinder release). Accidental releases, while rare in properly
designed systems, do occur. As such,
exterior storage areas should not be
overly enclosed. The best designs are

open on all four sides. When this is not
practical, then no more than two sides
should be enclosed, or special provisions for cross-ventilation should be
provided, as shown in Figure 4.
The area electrical classification of
cylinder storage areas is a function of
the gases stored and the ventilation
55
Table 3. NFPA-45 Gas Cylinder Limitations

Gas
For a laboratory work

area of 500 ft2 or less
internal cylinder
volume
For a laboratory work

area > 500 ft2
internal cylinder
volume per ft2 area
Flammable
6 scf
0.012 ft3
Oxidizing
6 scf
0.012 ft3
Liquefied flammable gas
1.2 scf
0.0018 ft3
NFPA health hazard 3 or 4 gas
0.3 scf
0.0006 ft3
Lecture bottles
25 total
rate. If the flammable gas storage is
significant or the ventilation rate low,
it may be prudent to classify the area
as Class I Division 2. If only a small
quantity of flammable materials is involved, if the ventilation rate is high
or in an unenclosed exterior location
then General Purpose (ordinary) classification is usually adequate. Note
that in many cases, cylinder storage areas have only minimal electrical equipment and fixtures, typically
lighting. Hence, electrically classifying
the area as Class I Division 2, while
conservative, may be an appropriate
and very low-cost solution.
All storage areas should also have
easy access that is free of extended
ramps and enclosed spaces. Consider
that a release of even an inert gas
in an elevator, for example, could be
enough to cause asphyxiation.
Cylinder placement
How many cylinders can be used in

a laboratory? Table 2 provides the
NFPA-55 requirements. Table 3 provides NFPA-45 requirements. Local
building codes may mandate even
more stringent levels.
NFPA-45 provides some additional
guidance. For instance, it specifies
that cylinders not required for current operations shall be stored outside the laboratory work area. Highhazard gases shall be kept in a hood
or other continuously ventilated enclosure. (A high-hazard gas is one that
has an NFPA health hazard rating of
3 or 4 or 2 with no physiological warning properties.)
So what is the best location for gas
cylinders used in laboratory and research applications? While it has been
common practice for years to place
cylinders directly in labs, this may
not necessarily be the best approach.
For instance, it is difficult to maintain
the required separation of flammable
and oxidizing materials required in a
standard laboratory. Hazardous gas
cylinders are often placed outside
hoods. All cylinders have a tendency
to end up in escape paths or along
major traffic corridors. Gas cabinets
are expensive, and are both spaceand exhaust-intensive. They also are
not foolproof in preventing a fire or
explosion in the (admittedly unlikely)
56
event of a major cylinTop view

der leak.
Even worse, cylinProvide
ders are often moved
ventilation
holes
or gaps
around to obscure
corners, alcoves, cabinets and closets with
minimal ventilation or
inadequately designed
and constructed, ventilated cabinets and
boxes that do not meet the safety requirements of a bona fide gas cabinet.
The preferred placement for cylinders used in a research or laboratory
setting should be as follows:
Outside the laboratory or pilot plant
area with the gas piped to its final
use location
In a specially designed, gas-cylinder
-storage area in the facility, with the
gas piped in to its final use. This
may be adjacent to the area served,
or some distance away, depending on
what makes most sense safety wise
and economically
Inside a specially designed gas cabinet that meets the requirements of
NFPA-55
Inert gas cylinders, while posing significantly fewer dangers than those
containing flammables, toxics or oxidizing agents still pose some risks and
should follow these same guidelines.
The argument that a lone cylinder of
helium for a gas chromatograph poses
a trivial or acceptable risk may be
valid, but even a single cylinder improperly piped or secured can pose a
hazard. And, since this lone cylinder
often tends to accumulate additional,
more-hazardous brothers and sisters
over time, sound engineering design
precedent should be established and
maintained from the beginning.
Gas cabinets are commonly used
for those desiring to keep their cylinders in the laboratory. NFPA-55 provides prudent requirements for such
a setup:
Such cabinets must be at negative
pressure with respect to the laboratory, and have an average face ve-
Side view
Holes or
gaps for
cross
ventilation
Figure 4.
Proper ventilation is an important design
consideration
when storing
gas cylinders,
even in exterior
storage areas
Raised
floor
locity across the open doors of 200

ft/min, with a 150 ft/min minimum
at any point
Self-closing access doors and noncombustible windows are required
The interior must be equipped with
sprinkler systems
The cabinet must be labeled as to its
contents
NFPA-55 requires that toxic gases
shall be treated to neutralize or dilute
the effluent to below toxic levels that
are considered to be life-threatening.
Many organizations rely on the dilution effect of the exhaust and dispersion from the exhaust stack well above
grade to achieve this effect. However,
this may not be possible with very toxic
gases or larger cylinder volumes.
Cylinder piping
Cylinders need to be properly piped to

their final use location to ensure safe
operation. A suggested minimum piping schematic is shown in Figure 5. No
system should ever be supplied from a
gas cylinder without a regulator to set
the feed pressure. However, it is not
safe to rely on a regulator alone to prevent a system from overpressure. Operator error and regulator failure can
lead to a failure of the downstream
equipment with dangerous or even
fatal consequences.
Instead, a relief device of some type
should be used. It may be a springloaded device (Figure 5) or a rupture
disk (for higher-purity or lower-maintenance applications), or a similar relief device. The relief device needs to
be properly sized to handle a regulator
failure, which produces flows as much
PR
PR
PI
Relief Vent
valve
Globe
valve
Check
valve
Excess flow
prevention
valve
Gas
cylinder
Figure 5. Shown here is the recommended,

minimum cylinder-piping array that should
be used for compressed-gas cylinders
as an order-of-magnitude higher than

the maximum regulator-design flow.
The relief device vent should be piped
to a safe location, typically an exhaust
duct or vent stack. Both will need
to have their sizing confirmed
as adequate.
The purpose of a manual globe valve
around the relief device (as shown in
Figure 5) is to allow manual venting
and purging during cylinder changes
and system maintenance. It also allows the system pressure to be lowered
through venting, in the event that the
supply pressures are inadvertently set
too high. This valve should always be a
slow-opening, multiple-turn globe type
to prevent a sudden depressurization.
The excess-flow-prevention valve
should be mandatory on all piping systems involving flammable and toxic
systems. It is intended to shut off (or
at least limit the flow to an acceptable
smaller rate) in the event of a system
or component failure. Some facilities
allow a manual bypass around this device, to allow initial filling at a higher
rate without tripping the device, or to
allow the excess-flow-prevention valve
to be reset if tripped.
However, this is not the most appropriate approach. Too often, the manual bypass is left open, defeating the
capabilities and intent of the excessflow-prevention valve. If a bypass is
required, it should be of the deadman
type (requiring the operator to hold it
open), or be on a timer that closes the
bypass automatically after a minute
or two.
The check valve is intended to prevent backflow into the gas cylinder
from a source of higher pressure. If
such a source is not present, then one
might naturally consider eliminating
the check valve; however, it should be
a standard part of all gas cylinder installations, as higher-pressure sources
Globe
valve
Ball
valve Regulator
Regulator
Gas
cylinder
PI
Ball
valve
Check Ball
valve valve
Relief Vent
valve
PR
Relief Vent
valve
Globe
valve
Globe Check
valve valve
Excess flow
prevention
valve
PI
Purge
gas
supply
Regulator
Figure 6. The recommended, minimum cylinder-piping

array with purge capabilities is provided here
often appear down the road and create problems if the check valve is
not installed.
The manual ball valve is intended
to provide a fast means to shut off the
gas cylinder in an emergency situation, and also allows the system to be
easily locked out and tagged for maintenance. In this case, both the gas cylinder shutoff valve and the ball valve
should be closed, and the manual vent
valve should be opened to vent the
system, completing the double blockand-bleed setup.
Many organizations like to add
a second block valve immediately
downstream of the gas cylinder and
before the regulator, to enable the
isolation of the system for change
out and maintenance. In this case,
the valve must be rated for the full
cylinder pressure.
Purge streams are also common
on higher-purity systems (Figure
6). Since purge systems are usually
lower-pressure gas supplies, it is important to provide the back flow and
relief protection shown. The purgesystem vent should also be treated as
a potentially hazardous stream and
piped to the same vent location as the
purged hazardous gas.
Piping should be run in areas where
it is to be expected. Routing pipe above
offices, personnel corridors and supply rooms can lead to unfortunate
incidents later, in the event that the
piping is assumed to be something
innocuous. At best it can lead to service interruptions; at worst to accidents. Similarly, piping should not be
run above suspended ceilings unless
the space is ventilated as part of the
laboratory. Small leaks can develop
into very hazardous situations over
extended periods in unventilated
areas. Even if ventilated, all welded
systems should be strongly considered
above suspended ceilings particularly for flammable or toxic gases. All

valves above the ceiling should be of
the packless or bellow-type seal. Better yet, no valve should be allowed in
these areas.
Open all cylinder valves slowly.
Pressurizing a system, particularly
for the first time or following maintenance always presents a high potential risk. If the valve does not open by
hand or with the manufacturer-supplied wrench, do not attempt to force
it with a pipe wrench or similar tool
that might be capable of transmitting
too much force. Such efforts can result
in unscrewing or at least loosening the entire valve assembly, with
results ranging from leaks to catastrophic failure.
Stand clear of all outlet piping while
opening the cylinder until the pressure has equalized. If there is going to
be a failure, it usually happens in the
first moments of pressurizing. While
such an occurrence is extremely rare,
this is still a prudent and essentially
no-cost safety measure.
Cylinder connections
All cylinders come with special threads

on the outlet. In the U.S., these threads
follow standards that are developed
by the Compressed Gas Association
(CGA), and are often called CGA fittings. CGA fittings should never be
modified or changed, as they are designed to minimize the chance of unsafe connections.
CGA fittings should never be forced
if they do not fit properly. They are very
effective for pure gases, but are less
foolproof with mixtures since different
vendors have different practices for
assigning thread types to a particular
gas mixture. Care must be taken before
connecting a new cylinder to
ensure compatibility.
57
Adaptors are available to ensure a
proper fit between a CGA fitting and
the existing pipe thread. However,
these must be used with extreme care
as they essentially allow the bypassing of safeguards.
Labeling
Gas cylinder piping should be clearly

labeled as to its contents. The location
of the feed cylinder should be posted
at the point of final use to allow emergency responders to know where to go
in order to shut off the cylinder. Similarly, the location should be posted at
the cylinder unless it is obvious (for
instance, strapped to the device), so
the user knows what impact the shutoff of a specific cylinder may have.
Never rely on the vendors color coding as it typically vary between vendors. Make sure each gas cylinder is
carefully checked to confirm its contents from the label affixed to the cylinder before placing it in service.
Empty cylinders
Empty cylinders should be kept separately from full cylinders. Mark empty
cylinders as soon as possible; as a
rule-of-thumb (until the situation can
be verified), always assume a cylinder
is full and act accordingly to ensure
safety, even when it is marked empty.
Cylinders should not be used at pressures below ~25 psi, to prevent gases
from being drawn from the system
into the cylinder and creating an inadvertent hazard for the vendor when
refilling the cylinder. The remaining
useable volume in a cylinder can be
found from the following formula:
Actual volume = [(Actual pressure)
(Initial volume)]/Initial pressure
Emergency response
All organizations using gas cylinders

should have procedures in place for
how to deal with leaking cylinders. The
type of gas (inert, flammable or toxic)
will obviously be a major factor, as
will the cylinder location, rate of leakage, ventilation and numerous other
incident-specific factors. Waiting to develop a plan once a leaking cylinder has
been found, with no basis from which
to work, is a recipe for a very poor and
usually ill-conceived, response.
58
Guidelines for safe hot-box design

These tips will ensure safe hot-box design for gas cylinders that require heating.
Ensure the enclosure has adequate over-temperature protection that is independent
of the control system. A separate sensor, alarm and shutoff are the minimum required.
The alarm should be latching (for instance, requiring a person to manually reset it),
and should require someone to deliberately reset the alarm before heating can resume.
Ensure that the temperature control and alarm systems are interconnected and enabled
to allow the hot box to heat.
Confirm the placement of the over-temperature sensor carefully to ensure it monitors
the hottest area. All too frequently, the device can be placed out of the way in a significantly cooler corner. Confirm the enclosure does not have such substantial temperature
differentials to create a problem.
Provide adequate audible and visual alarms to signal a problem to the operating
personnel. Take immediate automatic action to shut down all heat sources in the event
of a high temperature.
Ensure the enclosure has adequate ventilation to prevent small leaks from building
up to become a major hazard. Typical ventilation rates are 1 ft3/min per square foot
of floor area, with 150 ft3/min as a suggested minimum. In general, exhaust ventilation
should be provided at floor level. In larger installations (over 100 ft2), both high- and
low-point exhaust should be provided.
Make sure all heating elements are protected against direct impingement on the cylinder. Particular care should be paid to ensuring that a heavy cylinder cannot be pushed
against a heater. Many mechanical guards to prevent this accident are clearly inadequate when compared to the forces they need to withstand when struck by a 300-lb
cylinder in motion.
Ensure the hot box is completely constructed of non-combustible materials. Fire-retardant materials are not adequate. This includes doors, ramps and racks.
Managing the inventory
All organizations should inventory

their cylinders at least annually. This
allows the user to identify unused cylinders, spot potential problems with
older cylinders, and reduce demurrage
charges (the rental fee the supplier
charges on the cylinders). Return any
damaged, suspect or unneeded cylinders immediately to the supplier.
Consider establishing retention
times on cylinders with corrosive
gases. Six to twelve months are common but each case needs to be individually evaluated. In general, no cylinder should be kept for more than 36
months. If it has not been used in that
time, either it is not required or the
amount of gas has been oversized.
Develop procedures to force individuals to dispose of cylinders before personnel transfer to other sites, to avoid
accumulating un-owned cylinders
around the facility. Failure to do so is
not only costly in terms of continued
demurrage charges, but is potentially
very dangerous. Most organizations
have their own horror stories of aged
gas cylinders that were found in unexpected locations.
Cylinders cannot be tossed in the
garbage, but must be returned to the
supplier. Note, however, that some
new small calibration-gas and mixedgas cylinders are designed for single
use, and are intended to be disposed of
when empty.
Gas cylinders are common and very
safe if installed and operated properly.
However, despite their widespread use
in research, they always hold the potential for accidents and injuries if not
properly handled.
Author
Richard Palluzi is a distinguished engineering associate at ExxonMobil Research
& Engineering Co. (1545
Route 22 East, Annandale, NJ
08801; Phone: 908-730-2323),
responsible for the design,
construction and support of
pilot plants and laboratories
for the firms research site in
Clinton, N.J., and consulting
on pilot-plant issues throughout ExxonMobil worldwide. The author of two
books, 30 articles and 40 presentations on all
phases of pilot plant and laboratory safety and
operations, he is a member of AIChE, ISA, the
American Soc. of Safety Engineers and the National Fire Protection Assn., and was recently
elected to the last-named organizations committee on NFPA-45 Fire Protection for Laboratories
Using Chemicals. He teaches three pilot-plant
training courses for AIChE, and is a past chair
of the AIChE Pilot Plant Committee, as well as
of the Clinton sites Safe Operations Team. Also,
he currently chairs ExxonMobils Pilot Plant and
Laboratory Safety Standards Committee. Palluzi
has consulted for both the U.S. Dept. of Energy
and Dept. of Defense on research-related issues.
He holds B.S.Ch.E. (1974) and an M.S.Ch.E.
(1976) from Stevens Institute of Technology.
Reduce Hazards in
Process Vacuum Systems
Stanley S. Grossel
Process Safety and Design
Consultant
acuum conditions for many

unit operations including
distillation, evaporation, drying, crystallization, filtration
and more are typically achieved
using the following three approaches:
Steam ejector systems
Mechanical vacuum pumps
Integrated vacuum systems (which
combine steam ejectors and mechanical vacuum pumps)
This article is the second part of a
two-part series,1 and provides practical guidance for addressing during
design and operation some of the
most commonly encountered hazards
and maximizing the overall safety of
these systems.
This section reviews the potential
hazards that can occur with process
vacuum pumps and systems. These
include chemical sources of hazards,
explosion-related hazards and physical sources of hazards. They are discussed below, and are based on material in Reference 1.
Chemical sources of hazards
Chemical reactions and explosions. All possible chemical reactions

that a vacuum system might encounter at any point in mechanical vacuum
pump systems should be considered
particularly those that could result in
a fire or explosion (deflagration). And
such an analysis should consider these
scenarios during normal use, potential
misuse and failure conditions.
For instance, experience has shown
that explosions have occurred in situations involving materials that were
not originally considered by the system designer, and in which the failure
mode of that particular scenario had
not been taken into account. During
this analysis, the reactions that should
be considered include homogeneous,
heterogeneous and abnormal reactions. Two other sources of chemical
hazards are toxic and corrosive mate1. Editors note: Part 1 of this two-part article appeared in the September 2012 issue (pp. 5966).
Reduce explosion risks, and chemical

and physical hazards, to ensure safer operation
of vacuum pumps and related systems
rials. Each of these chemical sources
of hazards is also discussed below.
Homogeneous reactions. Homogeneous
reactions occur in the gas phase between two or more gas molecules. If
such reactions are possible in a given
manufacturing process, the process
pressure and reactant concentrations
must be carefully controlled to prevent excessive reaction rates.
Heterogeneous reactions. Heterogeneous reactions require a solid surface
(a catalyst) to occur. Most heterogeneous reactions become homogeneous
at higher pressures, normally at pressures well below atmospheric pressure.
This means that the way in which the
gases react inside the process equipment will not necessarily relate to the
way that they react when compressed
by a mechanical vacuum pump.
Abnormal reactions. Abnormal reactions can occur when chemicals come
into contact with gases or materials
that the designer did not anticipate.
This can occur, for example, when
there is a leak that either allows atmospheric gases (air) to leak into the system, or toxic, flammable, or explosive
gases to leak into the atmosphere.
To prevent the occurrence of abnormal reactions, high-vacuum applications should typically maintain a leak
tightness of 1 105 mbar-L/s (1
103 Pa-L/s), or lower. It must be ensured that all valves in the system are
leak-tight across their seats.
In estimating an acceptable airleakage rate, do not overlook the implications of process contamination
by air leakage. If leakage into the
vacuum system could in any way adversely affect the process, or create a
safety hazard, the acceptable air leakage may be considerably less than
that presented in Ref. 1, pp. 8386, for
medium- and high-vacuum systems.

Consideration should be given to the
fact that gases that do not normally
come into contact with each other during the process cycle may be mixed in
the pumping system and exhaust piping. It is possible that water vapor or
cleaning solutions may be present in
the process equipment after routine
maintenance procedures due to the
equipment having been washed and
cleaned. Water vapor may also enter
the system from exhaust ducts and
exhaust scrubbers.Where solvents are
used to flush process deposits from the
vacuum system, it is important to ensure that the selected solvent is compatible with all the process materials
in the vacuum system.
Explosion-related hazards
Explosions can occur in vacuum

pumps. The most common causes of
violent rupture of a vacuum system
due to an explosion results from the
ignition of flammable materials, or the
blockage or restriction of the pump exhaust. In general, the source of explosion hazards in vacuum systems fall
into one of the these categories:
Oxidants
Flammable materials
Pyrophoric materials
Unstable materials
Oxidants. Oxidants, such as oxygen,
ozone, fluorine and others are often
pumped using vacuum pumps. Oxidants readily react with a variety of
substances and materials. The reaction often produces heat and an increased gas volume with a potential
for fire and overpressure in the pump
or exhaust system. The practices discussed below are recommended to
minimize the potential for an explosion in pumps handling oxidants:
47
1. Always use perfluoropolyether
(PFPE) lubricant in pumps that are
used to pump oxygen in concentrations above 25 vol.% in an inert gas.
Although PFPE lubricants are preferred, hydrocarbon-based lubricants
may be used if a suitable inert purge
is used to guarantee that the oil is not
exposed to unsafe levels of oxidant.
2. If it is not desired to use PFPE lubricants in oil-sealed rotary vane or
piston vacuum pumps, dilute the oxidant to a safe concentration using an
inert gas (dry nitrogen). However, this
approach is only feasible for relatively
low flowrates of oxidant gases.
3. One must install safety features in
a mechanical pump system to ensure
that the minimum flow of the dilution
gas required to reduce the oxidant
concentration to a safe level is always
available, and to ensure that the flow
of oxidant does not exceed the maximum allowed flowrate. The safety system must be designed so that the flow
of oxidant stops immediately if these
conditions are not met.
Flammable materials. Many gases
are flammable and can explode (deflagrate) if they are within the flammability limits, and there is an ignition
source of sufficient energy available
(for instance, from a localized heat
source). It may be possible to reduce
the explosion hazard if the concentration of flammable gases is lowered
by introducing an inert gas at several
points within the pump or system.
Another way to reduce the probability of an explosion is to eliminate potential ignition sources. It may be difficult to eliminate all ignition sources
because there is often a possibility of
static discharge or friction hot spots
where rotating machinery is used.
Where it is not possible under abnormal conditions to avoid the flammable
zone, the equipment must be designed
to contain any resulting explosion
without rupturing or transmitting a
flame to the environment. This is typically achieved by installing a flame arrester on the exhaust piping.
Pyrophoric materials. A number of
gases (such as silane, phosphine and
others) are pyrophoric that is, they
are spontaneously flammable in air at
atmospheric pressure, so combustion
could occur if the gases were to come
48
in contact with air anywhere in the

vacuum system. This can happen if
air leaks into the system, or if the system exhaust comes in contact with the
atmosphere. In a confined space (such
as an exhaust duct, a dust filter, or an
oil box of a mechanical pump) combustion can cause an explosion.
If, in addition to pyrophoric materials, an oxidant is also present in the
process, the probability of an explosion
occurring at both atmospheric and process conditions increases greatly. Similarly, if oxidants from other processes
are vented through a common extraction (treatment) system, combustion or
an explosion could result. It is necessary, therefore, that an independent
extraction system be used when pyrophoric materials are pumped.
While the use of PFPE lubricants in
the pump will not prevent the ignition
and explosion of pyrophoric materials, it
will help to minimize the risk of a subsequent oil fire. However, PFPE lubricants can absorb process gases which,
in the case of pyrophoric materials, can
lead to local ignition when the lubricant is exposed to air. The probability of
this occurring can be reduced by using
a dry vacuum pump, which contains no
lubricant in the swept volume.
Unstable materials. Sodium azide is
occasionally used in the preparation of
products for freeze drying and other
manufacturing processes. Sodium azide
can produce hydrozoic acid, the vapors
of which can react with heavy metals to
form unstable metal azides, which may
then explode spontaneously.
Brass, copper, cadmium, tin and zinc
are commonly used in many components in vacuum pumps, accessories
and piping. If ones process system uses
or produces sodium azide, it must be ensured that the gas path in the process
system does not contain heavy metals.
Toxic materials. Toxic materials are
not necessarily explosive in nature, but
they are hazardous to ones health, and
thus require special care. The following
methods for handling them in vacuum
pump systems should be considered:
Gas dilution: Systems can be installed to allow the dilution of toxic
process gases as they pass through
the vacuum pump and into the exhaust piping. Dilution may be used
to reduce the concentration of the
gas to below its toxic limit

Leak detection: Many vacuum pumps
are generally designed to be leak
tight to a level of < 1 103 mbarL/S (< 1 101 Pa-L/s). However,
the leak-tightness of the adjoining
process system cannot be ensured
and thus should be checked with a
reliable leak-detection method (such
as helium mass-spectrometry leak
detection) to confirm the integrity of
the vacuum and exhaust systems
Shaft sealing (dry pumps): Many
vacuum pumps use a gas purge to
ensure that process gases do not
enter the gearbox, and thereby, potentially escape into the atmosphere.
The integrity of the purge gas supply must be ensured when handling
toxic gases. Non-venting regulators
must be used in combination with a
non-return check valve
Shaft sealing (other pumps): Oilflooded shaft-seal designs (for instance, for mechanical booster pumps
and rotary vane pumps) minimize
the risk of process gas leakage (or, of
the in-leakage of air), and can provide a visual warning (oil leakage or
oil level reduction) before a hazard
arises. Other seal designs may not
give adequate warning of failure
Magnetic drives: Where total hermetic sealing is required, dry vacuum pumps can be fitted with a
magnetic drive employing a ceramic
containment vessel (housing); this
eliminates the need for shaft sealing
on the motor input shaft
If pressure-relief valves or rupture
disks are used to relieve excess pressure, ensure that they are safely
vented into a suitable exhaust system
to prevent the toxic gas from escaping
into the atmosphere and possibly coming in contact with people.
Corrosive materials. Corrosive gases
generally attack the material they are
in contact with by the mechanism of
ion exchange, a process that can only
happen in the presence of a suitable
liquid solvent (such as water). This
mechanism cannot occur when the
material is in the vapor phase, even if
a suitable solvent is present.
The possibility of corrosion occurring in mechanical vacuum pumps
should be considered when carrying
out a hazard analysis.
Edwards Vacuum Pumps
Figure 1. Prudent design, operating and maintenance strategies are needed to

minimze the potential hazards associated with all types of vacuum systems
Many vacuum pumps are not designed to resist wet corrosive materials. Therefore, the following points
should be considered:
Anhydrous materials: The removal
of a liquid solvent (water) will prevent corrosion. However, special
care must be taken to prevent the
ingress of wet air from the exhaust
of the vacuum pump, especially
when the pump is stopped and air
is sucked back into the pump. An
inert purge should be used as part
of the shutdown procedure in order
to flush corrosive vapors out of the
system prior to shutdown
Dilution: Use a suitable dilution gas
to prevent condensation of corrosive
vapors and thus prevent the possible resulting corrosion
Temperature: Increase the pumpand exhaust-line temperature to
prevent condensation and, therefore,
corrosion. Where the low temperature of the incoming gas flow could
lead to condensation and subsequent
corrosion, an inert gas purge should
be used to avoid condensation
Corrosion of safety equipment: Where
safety critical equipment (such as
flame arrester elements, temperature sensors, safety relief valves and
so on) could be damaged by corrosive
products in the process gas flow, their
materials of construction must be selected to avoid this hazard
Phase changes: Unplanned phase
changes can result in condensation
and possible corrosion. Consideration
of changes in temperature and pressure is required to avoid this hazard
Unplanned reactions: These can lead
to the generation of corrosive products. Careful consideration should
be given to the possibility of cross
contamination when equipment is
used for more than one purpose
To minimize hazards from chemical
sources and to minimize explosion hazards, attention should be paid to the
items listed below to ensure safe operation of vacuum pumps and systems:
Consider all possible chemical reactions within your system
Make allowance for abnormal chemical reactions, including those that
could occur under fault conditions
Refer to material safety data sheets
when you assess the potential hazards associated with your process
materials
Use dilution techniques to minimize
reactions with oxidants and flammable materials
Use dry vacuum pumps if flammable
materials could enter the flammable
zone under abnormal conditions
Use the correct type of lubricant in
your pump when you pump oxidants,
and consider the use of a dry pump
Do not use heavy metals in the gas
path of your system if your process
uses or produces sodium azide
Take specific care when handling
toxic, corrosive, or unstable materials
Ensure that the concentration of
flammable materials in the vacuum
system does not permit these materials to enter the flammable zone.
During operation, there should be
a suitable supply of inert gas (nitrogen) to achieve dilution to a safe
level under all foreseeable operating
conditions and failure modes
Ensure that exhaust blockages cannot occur during operation, either
because of mechanical components
(such as valves or blinds) or because
of process materials or byproducts
depositing in pipelines, filters and
other exhaust components
Use only PFPE (perfluoropolyether)
oils to lubricate pump mechanisms
that are exposed to high concentrations of oxygen or other oxidants.
Other types of oils sold as nonflammable may only be suitable for
use with concentrations of oxidants
up to 30% v/v
Ensure that the accidental overpres-
sure of a deliberately closed and isolated vacuum system cannot occur,

for instance, as a result of a fault in
a pressure regulator or purge control system
Where the pumped product can react
violently with water, it is recommended that a cooling fluid other than
water (for example, a heat transfer
fluid) be used in the cooling circuit
Physical sources of hazards
Exhaust system over-pressure. The

most common physical hazard is an
over-pressurized exhaust due to a
blockage or restriction in the exhaust
system. All high-vacuum pumps are
specifically designed to operate with
high outlet-to-inlet compression ratios. They are designed to exhaust to
atmospheric pressure, or to a pressure
only slightly higher. If the exhaust is
restricted or blocked, many typical vacuum pumps can generate an exhaust
pressure in excess of 7 barg (101.6 psig).
This can lead to failure of the pump or
other components in the system.
In addition to the potential overpressure caused by the operation of
the pump, the introduction of a compressed gas (such as a purge or dilution gas) can also over-pressure the
system if the exhaust system is restricted or blocked.
Where a vacuum pump is fitted with
a flame arrester on the exhaust side, it
is essential that the exhaust back pressure does not exceed the maximum
limit stated in the vacuum system's
instruction manual. A regularly scheduled maintenance program should be
instituted to ensure that process deposits do not block the exhaust system
and flame arrester. In addition, it may
be desirable to install a pressure sensor located between the pump and the
flame arrester to detect if a blockage is
occurring and to sound an alarm.
Phase change. Another cause of
overpressure is sublimation or phase
change, which can lead to blockage of
process piping. The instruction manual
supplied with a vacuum pump should
be read for information on the maximum and recommended continuous
backpressure, and the exhaust system
should be designed so that these limitations can be met.
Some recommendations for oil-
49
sealed rotary vane and piston pumps,
dry pumps, and exhaust system design
are summarized below:
For oil-sealed rotary vane and piston
pumps, design the exhaust system
so that the pump is never subjected
to a back-pressure greater than 1
bar gauge (14.5 psig). Under normal operating conditions, the pump
should not run continuously with a
back-pressure of more than 0.35 bar
gauge (5.1 psig)
Many dry pumps also generate high
exhaust pressures when the exhaust
system is blocked or restricted. One
well-known dry-pump manufacturer
recommends that its dry pumps
should not be operated with an exhaust pressure higher than 0.3 bar
gauge (4.4 psig). If there is a risk of
high exhaust pressures occurring,
this vendor recommends that the
system incorporate an exhaust pressure switch to shut down the pump
and prevent the recommended pressure from being exceeded
It is recommended that the exhaust
system be designed to withstand
an internal pressure of at least 1.3
bar gauge (18.9 psig) for oil-sealed
pumps and at least 10 bar gauge
(14.5 psig) for dry pumps, unless
over-pressure relief is provided.
If a vacuum pump exhaust system
contains accessory components that
might cause restrictions or blockages
the protection methods shown in the
Table (p. 53) should be provided.
Inlet overpressure. The most common cause of over-pressure in vacuumpump inlet piping is the introduction of
compressed gas (such as purge gases)
when the pump is not operating. If
components in the inlet piping are not
suitable for the pressures that result,
the piping will rupture and process
gases will leak from the system.
Care must be taken before connecting compressed gas supplies to the
vacuum system through pressure regulators, which are designed to provide
a low-pressure flow so that the regulated pressure is within the pressure
rating of the vacuum system. The nonventing regulators most commonly
used will cause the pressure within
the vacuum system to rise to the pressure of the gas supply to the regulator, if operated under conditions where
50
there is no process gas flow through

the system. These two methods can
help to prevent over-pressurization:
Reduce the pressure and allow the
gases to bypass the pump into a
freely vented exhaust volume
Monitor the pressure of the vacuum
system and use a positive-closure
valve to shut off the supply of compressed gas at a preset pressure level
Inlet overpressure can also result from
incorrect vacuum pump operation,
and special precautions must be taken
until it has been established that the
pump is operating correctly.
If the direction of rotation of the
pump is incorrect and the pump is
operated with the inlet blocked or restricted, the pump will generate high
pressure in the inlet piping. This could
result in rupture of the pump, the piping and components in the piping.
Always use a blanking plate (line
blind) loosely secured by screws to the
pump inlet until it has been established that the direction of rotation for
the pump is correct.
Operation at high rotational speeds
could result in pump break-up. Do not
operate the pump at rotational speeds
above the maximum designed speed of
rotation; this is particularly important
where frequency inverters are used for
speed control.
General design practices
More details about the design practices

described below can be found in Ref. 1.
Pressure ratings in a system. Vacuum systems and piping are designed
to operate with internal pressures
below atmospheric pressure. In practice, however, it is necessary to design
the system (pump and piping) for use
with internal pressures above atmospheric pressure as well. It may be necessary to incorporate pressure relief
devices to prevent over-pressurization.
Exhaust systems must always be designed to produce the smallest possible
backpressure to the pump during operation. It is important, however, to design
the exhaust system with an adequate
pressure rating; it must be suitable for
the pressures that can be generated by
the pump and by the introduction into
the system of a compressed gas, and be
suitable for use with the overpressureprotection measures used.
Where the vacuum system is used to

handle a vapor or gas mixture in the
flammable range, and where there is
a potential ignition source, the pump,
piping and associated vessels should
have a minimum design pressure of
10 bar gauge (145 psig).
Eliminate stagnant volumes. A stagnant volume is any closed volume in a
vacuum pipe or component that is not
subjected to a through flow of gas. Examples are the gear box of a mechanical booster pump or the gauge head of
an instrument. Valved piping and nitrogen-gas inlet pipes can also become
stagnant when they are isolated.
Stagnant volumes must be taken
into account when one considers the
mixture and reaction of process gases
that are not normally present together
in the process vessel. A stagnant volume is not purged and may be filled
with process gases as the pressure in
the system rises and falls. In this way,
gases that pass through the system at
one stage of the process can be retained.
These may then react with gases from
a subsequent phase of the process.
Thorough evacuation of the process
chamber between episodes involving
the introduction of incompatible gases
will lower the risk of an explosion.
Special care must be taken when
considering cross-contamination in
stagnant volumes, especially when the
pressure is relatively high (close to atmospheric pressure) and the gases are
potentially explosive. In particular, one
should consider the hazard of buildup
in filters and separators. Where appropriate, use high-integrity, continuous
flows of inert purge gas to reduce the
probability of cross-contamination.
When pumping flammable gases, it
is possible for stagnant volumes to fill
with potentially explosive gases or vapors that cannot be removed by normal
purging. When an ignition source may
also be present, specific purging of the
stagnant volume should be considered.
Sources of potentially explosive gas
or vapor mixtures. When a flammable
gas or vapor is mixed with the correct
concentration of oxygen or other suitable oxidant, it will form a potentially
explosive mixture, which will ignite in
the presence of an ignition source.
While it is generally apparent if a
pumped gas or vapor is potentially
Table. Options for protecting

vacuum pump exhaust systems
Component
Valve in
exhaust
Exhaust
scrubber
Flame
arrester
Oil mist filter
Protection method
Interlock the valve so that its piping is always open when the pump is operating
Incorporate a pressure relief bypass
Incorporate a pressure relief bypass
Incorporate a pressure monitor or sensor and interlock this with the pump motor
so that the pump is shut down when the exhaust pressure is too high
Provide an exhaust pressure measurement or a differential-pressure measurement
Incorporate a pressure-relief device
explosive, there are some conditions

where a potentially explosive mixture
is produced due to conditions that
were not considered when the process
was designed. One must identify all
possible sources of potentially explosive mixtures that could be generated
by the process vacuum equipment. Examples are listed:
Cross-contamination. Where a vacuum pump is being used for a number of duties, it is possible that its
use with individual gases or vapors
is safe, but if the pump is not purged
before use with another gas or vapor,
then cross-contamination could occur
with unexpected reactions
Cleaning fluids. An application may
be viewed as benign, but the use of
flammable cleaning fluids and the
subsequent drying by evacuation
through the vacuum pump can create a potentially explosive mixture
Unexpected material. On house
vacuum duties where the vacuum
pump is used to provide a distributed vacuum system, it is possible
to pump flammable gases or vapors
that were not considered during system design. These gases or vapors
may have autoignition temperatures
that are lower than the internal
temperatures of the vacuum pump
Dissolved vapors. Low autoignitiontemperature vapors generally have
high vapor pressures. Pumping
these vapors at pressures above the
vapor pressure will generally result
in internal dry-pump stage temperatures below the autoignition point.
However, it is possible for these vapors to become absorbed in a liquid
with a lower vapor pressure, and for
them to be released as the pressure
falls below the vapor pressure of the
dissolved vapors. At this lower pressure, it is possible for the internal
dry-pump stage temperature to exceed the autoignition point
Air leakage. The accidental ingress
of air or oxidant into a vacuum system may change the concentration
of a flammable gas or vapor and create a potentially explosive mixture
Flammable sealing liquids. Where a

flammable liquid is used as the sealing liquid in a liquid-ring vacuum
pump, air ingress will create a potentially explosive internal mixture
Avoiding the flammable zone. A
flammable gas or vapor will only create a potentially explosive atmosphere
if it is combined with sufficient air or
oxygen (or another oxidant, such as
chlorine) and the concentration of the
vapor in the mixture lies between the
lower flammability limit (LFL) and
the upper flammability limit (UFL).
To be potentially explosive, it is
also necessary for the concentration
of oxygen to be above the limiting oxidant concentration (LOC). There are
several strategies that can be used to
avoid operating with gas mixtures in
the flammable region. The choice of
strategy will depend on the outcome of
the hazard analysis for the process and
the pumping system. Recommended
strategies include the following:
Maintain the flammable gas concentration below the LFL. This is
accomplished by diluting the flammable mixture with an inert gas
(usually nitrogen) that is introduced
into the pump inlet and/or purge
connections. Refer to NFPA 69 [2]
for recommendations as to what
percentage of the LFL the flammable concentration should be maintained. The required integrity of the
dilution system and of any alarms or
interlocks will depend on the nature
of the hazards that would result if
the dilution system were to fail
Maintain the oxidant concentration
below the LOC. This mode of operation requires the use of oxygen-concentration monitoring of the pumped
gases to ensure safe operation. To
minimize the risk of flammable gas
accidentally entering the flammable
zone, a safety margin below the LOC
should be maintained. NFPA 69
[2] presents recommendations for
these safety margins. The preferred
method of maintaining the oxidant
(usually oxygen) level below the
LOC is to carry out both rigorous ex-
clusion of air and oxygen from

the process and pump system,
and dilution of the pumped gas
with an inert purge gas (usually nitrogen) that is introduced into the pump inlet or purge
connections, if needed. The required
integrity of the air/oxygen-exclusion
measures (for example, purging)
and of any alarms or interlocks will
depend on the hazardous zone that
would result, were the exclusion and
dilution systems to fail
Precautions typically required to rigorously exclude air from the process and
pump system include the following:
Eliminate air leaks. Use a leak detector or conduct a pressure-rise test
Remove all air from the system before
the start of the process. Before any
flammable gas is admitted into the
process, the system should be fully
evacuated and purged with an inert
gas (usually nitrogen) to remove all
air from the system. At the end of
the process, repeat this procedure
before the system is finally vented
to the atmosphere
Maintain the integrity of shaft-seal
gas. For dry-vacuum pumps, ensure
that any shaft-seal gas cannot be
supplied with, or contaminated by,
air under any circumstances (for
dry-vacuum pumps). In addition,
ensure that any gas ballast port is
either sealed, or only used to introduce inert gas
Follow instructions and maintain
proper lubrication. For wet vacuum
pumps (rotary piston or rotary vane
pumps), maintain the shaft seals in
accordance with the manufacturers
instructions, and use a pumped, pressurized oil-lubrication system with
an alarm that indicates the loss of oil
pressure. This system may comprise
an external accessory to provide filtered and pressurized lubricating oil,
with a pressure switch. Ensure that
any gas ballast port is either sealed,
or only used to introduce inert gas.
Provide an adequate purge of inert
gas to the oil box, to remove air before
the start of the process
Maintain the drive-shaft seal for
vacuum booster pumps (such as the
Roots pump). Maintain the primary
drive shaft seal fully in accordance
with the manufacturers instruc-
51
tions, and ensure that any purge or
breather port connections can only
be used to introduce inert gas
Guard against reverse flow. Ensure
that the system operating procedures and protective equpment protect the system from any reverse air
flow that might result from a pump
failure. Ensure that any pumped
flammable gases are safely disposed of at the final vent from the
pump exhaust. Ensure that flammable gas mixtures cannot occur in
the exhaust piping. This is done by
using suitable inert-gas purging of
the piping before the start of, and
after the end of, the flammable gas
process, and by the use of adequate
inert-gas purging during operation,
to prevent turbulent back-mixing of
air down the exhaust
Maintain the flammable gas concentration above the UFL. Where the
flammable gas concentrations are
very high, operation above the UFL
can be used. Procedures for doing this
are given in NFPA 69 [2]. To maintain
the oxygen at a safe level, rigorous
exclusion of air and oxygen from the
process and pump system is required.
This can be accomplished by dilution
of the pumped gas with an inert gas
(usually nitrogen) or by addition of
enrichment flammable gas (NFPA
69 discusses the use of methane for
this), introduced into the pump inlet
and/or purge connections
Use of flame-arrester protection
systems. When dry vacuum pumps
are used for pumping gases or vapors
that could enter the flammable zone
under abnormal conditions, exhaust
flame arresters should be installed to
quench any resulting flame front in
the event of an ignition. Flame arresters should be closely coupled to the exhaust connections.
Where there is the possibility of continuous burning within a dry vacuum
pump, special precautions should be
taken. Such conditions could occur due
to a continuous ignition source resulting from the accidental pumping of a
gas or vapor with an auto-ignition temperature lower than the internal pump
temperatures. In this case, one must
use a PT100 or equivalent temperature-sensing device on the pump side
of each flame arrester to detect a burn
52
condition, and adopt a suitable flamesuppression strategy to make the system safe in the event of a burn being
detected. The suitable strategy depends
on the application, but could include
the following:
Stopping the supply of fuel. Closing
a valve located on the inlet of the
dry vacuum pump will prevent the
supply of fuel (process gas or vapor)
into the vacuum pump
Stopping the source of ignition. Stopping the pump by turning off power
to the motor will bring the pump to
a halt in approximately 10 seconds
Inerting the area of the burn. The
rapid addition of inert gas into the
area of the burn (typically, but not
always located in the exhaust manifold of the pump) will eliminate the
flame. Note that it is possible for a
flame to reignite if the source of ignition is not removed
Piping design
This section discusses design practices for piping components used with
mechanical vacuum pumps.
Bellows. Bellows are short, thinwalled components with deep convolutions. They are used to reduce the
transfer of vibration from a pump to a
vacuum system. They are available in
metal, rubber or plastic construction.
Always install bellows in a straight
line with both ends rigidly constrained. When installed correctly, the
bellows can withstand a small positive
internal pressure (refer to the Instruction Manual supplied with the bellows
for details). Note: Do not use bellows
on dry vacuum-pumps exhausts: use
braided flexible bellows (see below).
Braided flexible bellows. Braided flexible bellows are bellows with an outer
protective layer of woven stainlesssteel braid. They are suitable for use
as exhaust connections on dry pumps
and other applications where there is
significant gas pulsation or the possibility of high gas pressures.
Braided flexible bellows are intended
for installation in static systems. They
are not suitable for repeated flexing, as
this could cause fatigue failure. When
a braided flexible bellows is installed,
one must comply with the minimum
bend radius given in the manufacturerss instruction manual.
Flexible hoses. Flexible hoses have

a thicker wall section and shallower
convolutions than bellows. Flexible
hoses provide a convenient method
for the connection of vacuum system
components and help to compensate
for misalignment or small movements
in rigid vacuum piping. Flexible hoses
can be formed into relatively sharp
bends that will hold their position.
Flexible hoses are intended for installation in static systems. They are
not suitable for repeated flexing, as
this could cause fatigue failure. When
flexible hoses are used, use the shortest possible length and avoid unnecessary bends. Do not use flexible hoses
on dry pump exhausts.
Anchor points. Piping and piping components must be anchored correctly. For
example, if bellows are anchored incorrectly, they will not reduce the vibration
generated by the pump, and this could
lead to fatigue in the piping.
Seals. Where there is the possibility of positive pressure occurring in
any part of the vacuum system (even
under failure conditions), one must use
trapped O-ring type seals, which are
capable of withstanding the expected
vacuum and positive pressures.
Physical over-pressure
protection
Over-pressure can be caused by a restriction or blockage in the vacuum

system or in one of its components.
The over-pressure may also occur as a
result of compressed-gas flow from the
pump or from external compressed gas
supplies (such as those for a dilution
system). There are two main methods
of over-pressure protection, as follows:
Pressure relief. Rupture disks or
pressure-relief valves may be used
to relieve an overpressure situation.
These devices must be provided with
discharge piping to convey the relief
device discharge fluid to a safe location
(where plant personnel are not usually
located), and the vent line should have
no restrictions. If the process produces
solid byproducts, the pressure-relief
devices must be inspected on a regularly scheduled basis to ensure that
they are not blocked or restricted.
Over-pressure alarm or trip. This
method of protection is used by several
vacuum-pump system manufacturers.
This type of protection can be used for

any vacuum-pump system, but it is
particularly suitable for systems that
produce solid byproducts.
Since the use of an alarm or trip
system forms part of a primary safety
system, it must incorporate a design
of high integrity. One should not rely
on a simple pressure switch or sensor
installed in a flow line, as the condensation of solid particles or corrosion of
the sensor can cause the device to fail
without indication of the failure.
It is also recommended that a sensor be used that incorporates a nitrogen purge flow to the sensor. A purge
flow keeps the sensor relatively free
from blockage, and such a sensor is designed so that, if the sensor is blocked,
the nitrogen supply pressure is high
enough to operate the pressure alarm
and trip. The normal settings for such
devices are usually no higher than 0.3
bar gauge (4.35 psig) and no greater
than 0.4 bar gauge (5.80 psig).
The control system should be designed so that both the pump and any
gas inlets (which are capable of pressurizing the system above its maximum operating pressure) are shut
down when the trip point is reached.
Purge systems. The correct use of
a purge (usually nitrogen) can ensure
that corrosive products are removed,
preventing them from damaging the
vacuum pump, and also from plugging
or damaging protective systems such
as flame arresters. In addition, the
removal of process gases ensures that
undesired and potentially dangerous
chemical reactions do not occur between process gases and vapors used
in different process cycles.
n
References
1. Edwards Ltd., Safety Manual-Vacuum Pump
and Vacuum (corporate manual).
2. NFPA 69, Standard on Explosion Prevention
Systems, National Fire Protection Association, Quincy, Mass., 2008.
Acknowledgements
The author wishes to thank J.L. Ryans of Eastman Chemical Co. (Kingsport, Tenn.) for his review of the draft of this article and for his helpful comments and recommendations. I should
also like to acknowledge the assistance of the
following people, who provided technical information used during the development of this article: Peter N. Lodal (Eastman Chemical Co.),
John Campbell (SIHI Pumps Americas), Mark
Nichols (Edwards Ltd.), and Eric Johnson (Graham Manufacturing Co.).
Author
Stanley S. Grossel is president of Process Safety
and Design, Inc. (4 Marble Court, Unit 9, Clifton,
N.J. 07013-2212; Phone: 973-779-3668; Email:
psadi28@aol.com). He provides consulting services related to process safety and loss prevention,
storage and handling of bulk solids and powders,
air pollution control, and process design of batch
plants. Prior to his 1993 retirement, Grossel spent
25 years in the Engineering Dept. of Hoffman-LaRoche, in a variety of roles. He was honored as the
only Senior Engineering Fellow ever to be designated by Hoffman-LaRoche. Grossel is a fellow of
AIChE, and holds AIChEs Norton Walton/Russell Miller Award for outstanding contributions to
loss prevention. He has lectured and been published widely, and has authored major standards
and guidelines. Grossel is also a contributor on
process safety to the 7th Ed. of Perry's Chemical
Engineers Handbook. He holds a B.S.Ch.E. from
City College of New York and an M.S.Ch.E. from
Drexel Inst. of Technology, and has completed
courses toward a doctoral degree.
Get Chemical Engineerings plant cost index to improve plant cost estimates
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521.7
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734.7
731.7
620.8
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437.2
379.5
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788.9
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53
What is aN SIS?
Tolerable Risk
While determined risk is generally well understood, tolerable
risk can be the missing link to complete risk assessments
Mike Schmidt
Emerson Process Management
afety instrumented systems (SIS)

are in the spotlight these days.
More companies have come to recognize the importance of recently
published consensus standards, and recent fatal accidents tied to the failure of
instrumented safeguards have brought
further attention. The result is that facilities all over the world are looking at their
safety interlocks and concluding that
what they really need is a full-blown SIS.
As some work to upgrade their SISs,
they find plenty of guidance available for
the early steps process hazard analysis
(PHA), consequence analysis, and layers
of protection analysis (LOPA) and also
guidance for the later steps component
selection, failure probability and SIL
(safety integrity level) verification calculations, and system-design guidelines. A
disconnect comes when end users have developed their lists of safety instrumented
functions (SIFs) and are asked to assign
an SIL to each one (Table 1).
Detailed design of an SIS cannot begin
until each SIF has been assigned an SIL.
This is the point in the process where
many are tempted to throw up their
hands in despair and want to arbitrarily
assign everything as SIL 3. This is not the
answer. At the very least, it fails to comply
with the letter and the spirit of the standards, but worse, it misallocates resources
to overdesign when these resources could
be better used to reduce risk elsewhere.
The disconnect occurs because SIL assignment depends on a comparison of
two values: determined risk, about which
much has been written; and tolerable risk,

which is frequently invoked but rarely
presented in terms that are useful for SIL
assignment. Instead, the literature usually contains some variation of this statement: Each organization is responsible
for establishing its own risk-tolerance
criteria. Some organizations have corporate risk-tolerance criteria that speak to
the total corporate risk, but many have
no risk-tolerance criteria at all. It is still
a rare organization that has established
risk-tolerance criteria that are actually
useful at the level of a process unit, where
the SIS resides.
Recommended approach
A typical approach to SIL assignment,

but certainly not the only one, is to use
a risk matrix. Risk is a product of consequence and likelihood. As shown in Table
2, consequence and likelihood categories,
like the SILs themselves, are separated
by orders of magnitude. The challenge for
each company then, is to define the consequences that are considered serious and
the benchmark frequency (f).
Many companies already use some type
of matrix, usually to prioritize recommendations from HazOps (hazard and operability reviews) or other PHAs. An example
of this is shown in Table 3, where a rating of 1 would mean something should be
done immediately, and a 10 would mean
that no action is required.
Typical likelihood categories include
terms such as frequent, occasional, seldom, remote and unlikely but what do
they mean? A company may leave it to the
individual participants in the PHA to decide for themselves.
Table 1. Safety Integrity Levels

Probability of
Failure on Demand
(PFDAVG)
10-4 > PFD > 10-5
10-3 > PFD > 10-4
10-2 > PFD > 10-3
10-1 > PFD > 10-2
10,000 < RRF 100,000

1,000 < RRF < 10,000
100 < RRF < 1,000
10 < RRF < 100
Some companies define these terms, but

may use frequency intervals that are not
uniformly spaced. A typical set might be:
Event occurs once a year
Event occurs once every 10 years (~1
order of magnitude)
Event occurs once every 50 years (~
order of magnitude)
Event occurs once every 150 years (~
order of magnitude)
Not likely to occur
The same holds true for the severity in the
consequence categories; a typical (nonlinear) arrangement might be:
Loss of life; damage over $1 million
Lost-time injury; damage over
$500,000
Medical treatment; damage less than
$500,000
Minor injury; near miss; poor quality
No injury, impact on process
Converting an existing matrix
To convert an existing matrix to an SILassignment matrix, the first step is to adjust the likelihood categories so they are
Table 2. Risk Matrix

Consequences (per event)
Risk Reduction
Factor (RRF)
Likelihood
Safety
Integrity
Level
SIL 4
SIL 3
SIL 2
SIL 1
Various acronyms are used in discussions about

safety instrumented systems (SISs). While these
acronyms are defined in the text of this article,
a little more explanation is warranted.
The acronym SIL stands for safety integrity level. Each SIL represents the difference
between the process risk without an SIF, and
the risk deemed tolerable. An SIF is a safety
instrumented function and consists of the sensors, logic solvers, and final elements necessary to detect a particular hazardous condition
and cause the process to go to a safe state. Its
important to note that SILs apply to each SIF,
not to the SIS as a whole.
An SIS is a collection of all the sensors,
logic solvers, and final elements necessary to
address all the SIFs in a process, hence the
word system. SILs establish the required reliability of an SIF. Once a safety instrumented
function is designed, reliability calculations
can show if the SIF is reliable enough to reduce
the risk to a tolerable level.
Safety integrity levels range from 1 to 4, but
it should be noted that SIL 4 is not recognized
in all SIS standards. Instead, there is an expectation that the process will be re-designed to
reduce the risk. An SIS can also include SIFs
that are not SIL rated. Various users refer to
them as N/R (not rated) or SIL 0 handy
terms, albeit not defined in any standards.
f > High
< 0.01 x > 0.01 x > 0.1 x > 1 x

> 10 x
Serious Serious Serious Serious Serious
N/R
SIL 1
SIL 2
SIL 3
SIL 4
High > f > 0.1 High N/R
N/R
SIL 1
SIL 2
SIL 3
f < 0.1 High
N/R
N/R
SIL 1
SIL 2
N/R
f =Benchmark frequency
Chemical Engineering www.che.com September 2007
69-74 CHE 9-07.indd 69
69
8/29/07 5:43:13 PM
Table 3. An example of a
matrix for PHAs
one order of magnitude apart. After that,

consequence categories should be adjusted
so they are also one order of magnitude
apart. The intervals could be 1.5, 15 and
150 years, or 5, 50 and 500 years, as long
as they are an order of magnitude apart.
The next step is to define the consequence categories. The universally used
scale and absolutely required by the
SIS standards is of consequences to personnel. But other important consequence
scales, like community, societal or environmental consequences, may also show
up in one of these matrices. Just keep in
mind that as an SIF for reducing the risk
of a specific hazard is evaluated, the consequences of that hazard must be evaluated
on each scale. The event will have the same
frequency, regardless of the types of consequences considered, and the consequence
that results in the highest SIL rules.
While some organizations want to consider site and operability consequences of
a hazard in their analyses, there are serious disadvantages to keep in mind. One, it
puts a dollar scale on the same matrix as
environmental, health and safety (EHS)
consequences, and it is not a big leap for
a plaintiffs attorney to equate the EHS
consequences to the dollar amounts. Also,
functions that strictly protect against economic loss dont need to be burdened with
the documentation requirements of the
SIS. Organizations are usually better off
to leave the economically driven functions
in the basic process control system and
avoid giving them SIL ratings.
Consequence categories
If classifying likelihoods into categories

that are separated by orders of magnitude is hard, its nothing compared to
separating consequences into categories.
Once a benchmark frequency is defined
as a number, dividing or multiplying it
by ten is straightforward. Development of
consequence categories, however, requires
agreement on what consequence is ten
times worse than another.
In the early twentieth century, H.W.
Heinrich [1] proposed the idea that for
each fatality there were many incidents
with less serious consequences, and that
for each incident with less serious consequences, there were even more near
misses. From that simple observation
grew the notion that if we could be more
alert to near misses and reduce them, we
would necessarily reduce the incidence of
70
Likelihood
1
2
3
4
5
5
5
8
9
10
10
Severity (Consequence)
4
3
2
1
4
3
2
1
7
6
4
2
8
7
6
3
9
8
7
4
10
9
8
5
Table 4. Relative cost of
consequences
Fatalities
Serious injuries
Injuries (reportables)
First aids (non-reportables)
1.0x
0.1x
0.01x
0.001x
more severe consequences. This led to the

now familiar, safety pyramid (Figure 1).
While the premise of the safety pyramid has recently been called into question, Heinrichs original observation is
still valid: near misses, first aids, and
fatalities are each separated by about an
order of magnitude (Table 4).
Many have published cost estimates associated with increasing levels of injury,
with costs ranging from a few hundred dollars for a first-aid injury to a million dollars for a fatality. What the various scales
have in common is that severity of consequences, when reduced to dollars, seems to
be separated by orders of magnitude.
Once likelihood and consequence categories that are separated by orders of
magnitude have been established, an SILassignment matrix can be developed. An
example of a blank table is given in Table
5. All that remains is to associate an SIL
with each cell in the matrix.
What is a tolerable risk?
SILs represent the residual risk between

what is left after all other layers of protection have been applied to a hazard, and
the tolerable risk. But what is the tolerable risk? Consider this: Whether or not
your company has established a tolerable
risk criterion for your facility, what do you
believe it should be? How infrequently
would a fatality occur for you to be able
to describe your facility as safe? Once a
year? Once every three years? Once every
5,000 years? Once every million years?
The ALARP principle (Figure 2) was developed by the Health and Safety Executive of the U.K. It states that risks should
be reduced to a level that is As low as
reasonably practicable. The ALARP principle first divides risk into three areas:
Intolerable Risk at the high end, Negligible Risk at the low end, and the Tolerable Risk that falls between the two. Risk
in the middle region can be tolerated as
long as all cost-effective measures to reduce risk have been put into place. Any-
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H.W. Heinrich [1]
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FIGURE 2. The ALARP principle, developed
in the U.K., states that risks should be reduced
to a level that is as low as reasonably practicable
one operating a process with risks in the

tolerable risk region must demonstrate
that they have achieved the lowest risk
possible, taking into consideration cost
versus risk reduction.
Government mandates
Some countries have mandated upper and

lower levels for tolerable risk. Most countries that have set these levels use the
average level of risk faced by the entire
workplace population, regardless of occupation, as the upper limit for tolerable
risk. In many developed countries, that
is the equivalent of one fatality per year
per 1,000 workers. This upper boundary represents the level of fatality rate
already tolerated in industries such as
underground mining or deep-sea fishing.
The lower boundaries are generally two
or three orders of magnitude lower.
The Netherlands took a similar approach, but then declared that workplace
risk should be 1% of general risk, because
it is not voluntary risk. This results in levels that are 100 times lower than those
chosen by most countries that set levels.
These levels, as shown in Figure 3, are
sometimes called bright lines, especially
when discussed in the U.S., where there
has been no success in setting tolerable
risk levels. The argument was made that
a strict bright line approach to decision
making is vulnerable to misapplication
since it cannot explicitly reflect uncer-
69-74 CHE 9-07.indd 70
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Likelihood
Table 5: SIL Assignment Matrix,without SILs

Consequences (per event)
5
4
3
2
< 0.1 in- 0.1 injuries 0.1 disability 0.1 fatality
juries 1 first aid
1 Injury
1 disability
1 near miss 10 first aids 10 injuries
1. Frequent
(>1 event/1.5 years)
2. Occasional
(>1 event/15 years)
3/4. Seldom/Remote
(>1 event/150 years)
5. Unlikely
(<1 event/150 years)
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FIGURE 3. Government mandates defining
tolerable risk are often referred to as bright
lines. The color coding here refers back to
the 3 levels in the ALARP principle as shown
in Figure 2. The U.S. does not set tolerable
risk levels, nor offer guidelines
FIGURE 4. CPI benchmarks show that

large, multinational companies tend to set
levels consistent with government mandates. Smaller companies tend to operate in
wider ranges and implicitly at higher levels
of risk
Table 6: Voluntary risks

Smoking
9.7 x 10-3/yr or 9,700 fatalities per year per million smokers
Automobile accident
Lightning strike
1.4 x 10-4/yr or 140 fatalities per year per million people

1.5 x 10-7/yr or 15 fatalities per 100 years per million people
tainty about risks, variation of susceptibility within a population, community

preferences and values, or economic considerations all of which are legitimate
components of any credible risk management process. In other words, in the U.S.,
tolerable risk remains very much subject
to the political process.
CPI benchmarks
Almost all major companies in the chemical process industries (CPI) have guidelines for tolerable risk, but they are
generally considered highly confidential.
No company is going to announce to the
public, for example, that they would tolerate up to one fatality per year per ten
thousand workers.
Some companies, especially smaller
ones, do not have explicit guidelines. However, the risk they tolerate can be inferred
from the risk reduction measures they
have in place. Smaller companies without explicit guidelines generally tolerate
greater levels of risk than their larger
counterparts and this isnt inappropriate.
A small company, struggling to establish
itself or to make payroll, is going to look at
the amount of risk that it can and must
tolerate to get through the next year very
differently from a company that is look-
69-74 CHE 9-07.indd 71
ing out over the next 100 years. A small

company with a single plant will look at
a single event that occurs once every 250
years and may very well decide that once
every 250 years might as well be never.
A large company, with 50 similar plants
around the world would look at that same
risk as once every 250 years for each plant,
but once every 5 years for the corporation,
and make a very different decision about
whether the risk is tolerable (Figure 4).
Voluntary and natural risks
The levels mandated by governments,

or self-imposed by companies, can best
be understood in terms of some of the
risks to which people voluntarily expose
themselves. That is not to say that risks
like these should ever be compared to
process risks in a public setting, which
would likely inflame the audience. But,
for ones own understanding, it is helpful
to know that the upper level for ALARP is
typically set at 1 x 103 per year, or almost
ten times lower than the risk to which
smokers expose themselves. If a chemical
process had the same risk as smoking, it
would be considered an intolerable risk.
On the other hand, dying from a lightning strike would generally be considered
a negligible risk. If you consider your own
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8/29/07 5:45:12 PM
personal risk management strategies,

chances are that you have not invested in
lightning protection at your home. Even
in your plant, the lightning protection is
for electrical equipment, not personnel.
The risk of a fatality in a car accident is
within the ALARP region. Of course driving has the potential for fatalities, but the
risk is tolerable because the convenience
or benefit is worth it. If it wasnt, society
would insist on lower speed limits and
more safety features in cars.
Example A: 1 fatality/100 years
Lets get back to SIL assignment. While

each of us has a different level of personal
tolerable risk, when asked how small the
average frequency for a fatality would
need to be for a plant to be considered
safe, it is not at all uncommon for people
to pick 100 years. This is longer than any
one persons career but short enough to be
meaningful in terms of the life of a facility. So consider a facility with a tolerable
fatality rate of one per 100 years.
Likelihood
Table 7. completed risk matrix for example A

5
4
3
2
< 0.1
0.1 injuries 0.1 disability 0.1 fatality
injuries 1 first aid
1 Injury
1 disability
1. Frequent
N/R
SIL 1
SIL 2
SIL 3
(1 event/1.5 years)
2. Occasional
N/R
N/R
SIL 1
SIL 2
(1 event/15 years)
3/4. Seldom/Remote N/R
N/R
N/R
SIL 1
(1 event/150 years)
5. Unlikely
N/R
N/R
N/R
N/R
Further assume that at this facility,

the workforce includes 250 workers who
would be exposed to process risks:
(1 year/250 man-years) (1 fatality/100
years) = 1 fatality/25,000 man-years
= 4 x 105 fatalities/man-year
= total tolerable risk
In this case the total tolerable risk is one
fatality per 25,000 man-years, or 4 x 105
fatalities per man-year, which falls in the
middle of the tolerable risk region.
Process risk is only part of risk
Note that the tolerable risk established

above is for all fatalities in the plant. However, not all fatalities result from process
safety risks, that is from process hazards.
There are still the slips, trips and falls,
the housekeeping issues, the electrical
1
fatality
10 disabilities
Redesign
SIL 3
SIL 2
SIL 1
safety and confined-space entry issues,

and transportation-related fatalities.
For Example A, assume that half of the
risk comes from process safety risks or
process hazards. If total tolerable risk is
4 x 105 fatalities/man-year, then process
safety risk is half of that, or 2 x 105 fatalities/man-year.
Although weve assumed that no more
than half of the risk comes from the process hazards, we need to consider all of
the process hazards that could lead to a
fatality. Unless there is only one potentially fatal hazard, not all of the process
safety risk can be allocated to a single
hazard. One approach is to assume workers are each exposed to a certain number
of potentially fatal hazards, say five, and
then distribute the risk budget over
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72
69-74 CHE 9-07.indd 72
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8/29/07 5:46:39 PM
those five hazards in establishing SIL selection criteria. Other hazards, although
not expected to be fatal, can then use the
same criteria. If total process safety risk
is 2 x 105 fatalities/man-year, then:
N/R: 4 x 106 fatalities/man-year
SIL 1: 4 x 105 fatalities/man-year
SIL 4 or re-design: > 4 x 102 fatalities/
man-year
Putting a stake in the ground
With the tolerable risk criteria settled,

then the next step is to assign an SIL to
one of the cells in the matrix. For this example, lets look at cell 22 in Table 5.
We want to consider the risk at the middle of the cell. Since the scale is logarithmic, the middle of the cell on the likelihood
scale is the log (geometric) mean of 1.5
and 15 years, or 4.7 years. The log mean of
0.1 fatalities per event and 1 fatality per
event is 0.32 fatalities per event.
Doing the math, the center of our target cell has a risk of 2.7 x 104 fatalities
per man-year. Going back to our tolerable
risk criteria, that is less than 4 x 104, so
it translates to SIL 2.
Once we can assign SIL 2 to that cell,
completing the rest of the matrix is easy
(Table 7). The cell to the left is one order
of magnitude less risk, so it is SIL 1. Everything to the left of that is not rated.
Similarly, the cell below is one order of
magnitude less risk, so it is also SIL 1.
Everything below that cell is not rated.
Filling in the rest of the matrix follows
the same logic.
When were finished, we have a risk
matrix that can be used for SIL assignment for all SIFs, whether or not fatal
consequences are anticipated.
Interestingly enough, when the risk
matrix is finished, it spells out the criteria for assigning an SIL to an SIF without
ever explicitly acknowledging a tolerable
risk. The tolerable risk is only implied.
Example B: 1 x 106 fatalities/man-yr
Now consider Plant B. It is very similar to

Plant A, with the same number of exposed
workers and the same number of poten-
1
fatality
10 disabilities
Redesign

, " / , / "
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i`}iV
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Table 8. comleted risk matrix for example b

5
4
3
2
< 0.1
0.1 injuries 0.1 disability 0.1 fatality
injuries 1 first aid
1 Injury
1 disability
1. Frequent
SIL 2
SIL 3
Redesign
Redesign
(1 event/1.5 years)
2. Occasional
SIL 1
SIL 2
SIL 3
Redesign
(1 event/15 years)
3/4. Seldom/Remote N/R
SIL 1
SIL 2
SIL 3
(1 event/150 years)
5. Unlikely
N/R
N/R
SIL 1
SIL 2
SIL 3
tially fatal hazards. In this case, however,

senior management has declared that risk
needs to be reduced to the level considered negligible on the ALARP diagram
(Figure 2). That is, less than one fatality
per million man-years.
The portion of total risk to an individual attributable to process safety risk
would again be half, or 5 x 107 fatalities
per man-year. Once again, with each individual worker exposed to about five
potentially fatal hazards, the threshold
for avoiding an SIL-rated SIF is 1 x 107
fatalities per man-year.
Likewise, SIL 1 is less than 106, SIL 2 is
less than 105, and SIL 3 is less than 104.
In the CPI, anything larger than 104 would
need to be redesigned to reduce the hazard
before a safety instrumented function for
risk reduction was even considered.
Looking at the middle of the same cell,
we still end up with a risk of 2.7 x 104
fatalities per man-year. The plant is the
same, so the risk is the same. Whats different is the tolerable risk. In the case of
Plant B, the tolerable risk is set at a much
lower level, and so in this case, the risk
is not quite low enough to meet the SIL
3 rating:
(1 event/4.7 years) (0.32 fatalities per
event) (1 yr/250 man-years) = 2.7 x 104
fatalities/man-year
SIL rating = SIL 4 or redesign
As in the first example, the rest of the
matrix is easily populated. Because of the
difference in tolerable risk, the SIL assignments have shifted toward the lower
left-hand corner of Table 8.
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Variations to consider
A variation to consider, depending on risk

philosophy, is what part of a cell to benchmark to. In our examples, we took the center of a cell. If the upper right corner is
used instead, the result will be an SIL assignment that is higher by one level. This
is clearly a more conservative approach.
Another variation to consider is the
number of categories for both likelihood
and for consequence. Typically, a 5 x 5 matrix is the largest workable matrix, with

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69-74 CHE 9-07.indd 73
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a larger matrix, the team doing risk assessment will probably spend more time
debating categories than is warranted. By
the same token, if the matrix is smaller
than 3 x 3, it is unlikely to have enough
detail to be worthwhile.
In general, it is a good idea to extend
the matrix far enough to the left to get a
column of all non-rated SIFs, or else all the
SIFs, regardless of risk, will end up being
SIL rated. By the same token, there is no
reason to extend the matrix farther to the
left than a column that is all N/R, or farther to the right than is all redesign.
Business results achieved
When a company establishes a risk

matrix for SIL assignment, the matrix
receives a fairly broad distribution. To
the extent that the company is uncomfortable publicizing its tolerable risk
criteria, the risk matrix approach to
SIL assignment does not require an explicit statement of tolerable risk.
Because likelihood and consequence
only need to be estimated to the nearest less under-specification with intolerably

order of magnitude, most SIL assign- high risk, and much less over-specificaments can be made without using de- tion with resulting misallocation of limtailed and expensive quantitative risk- ited safety resources.
analysis techniques. It is usually easy to

get agreement, based solely on the expe- Reference
rience of the risk-assessment team, that 1. Heinrich, H.W., Industrial Accident Prevention: A Scientific Approach, 4th ed., McGraw-Hill, N. Y., 1959.
an event is likely to occur between 10 and
Author
100 years, rather than spend the time deMike Schmidt is a principal
termining whether it will be once every
consultant with Emerson Process
37 years or once every 54 years.
Management at the Refining and
Chemical Industry Center in St.
Since it is usually easy to get agreeLouis (641 Lambert Pointe Drive,
ment in the middle regions of consequence
Hazelwood, MO 63042; Phone:
314-872-6069; Fax: 314-872-8686;
and likelihood, quantitative risk analyEmail:
mike.schmidt@emerson
process.com). His responsibilities
sis can be reserved for the more extreme
include facilitating HazOps and
situations, such as hazards that are either
other PHAs, consequence analysis, facilitating LOPAs, reviewing
expected to be very, very rare, or to have
and preparing SRSs (SIS safety requirements specivery, very large consequences. And even in fications), and performing SIL calculations. Schmidt
on process design and optimization and teaches
those cases, the quantitative analysis only consults
in all these areas. In addition to being a registered PE
needs be done if there is a question about in several states, Schmidt is a CFSE. He has been with
Emerson for over ten years, and has been working in the
the SIL assignment of a particular SIF.
CPI since 1977. The majority of his career has been in
Finally, risk matrix is easy to apply, operating companies, including Union Carbide, Rohm
Haas, and Air Products. He is the author of several
and will result in hazards and their asso- and
articles on process design and process safety, and is currently
serving on the CCPS committee that is preparing
ciated risks being treated similarly from
a guideline book
on tolerable risk
and onPM
the API
com- 1
Ad 385-3c ChemEng:Layout
1 7/20/07
2:08
Page
project to project. This will result in much mittee on overfill
protection.
Problems with
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385-3c
69-74 CHE 9-07.indd 74
8/29/07 5:50:14 PM
PI
Solids
Environmental
Processing
Manager
Cooling water
return
Condensate
Follow this guidance to ensure that steam ejector

systems, mechanical vacuum pumps and integrated
vacuum systems are designed, operated and
maintained to ensure process safety
Stanley S. Grossel
Process Safety & Design Consultant
his article is the first in a twopart series, in which the types

of process vacuum equipment
(steam ejector systems and
mechanical vacuum pumps) are discussed.1 Emphasis is given on how
they are constructed and operate, and
how to design associated parts of the
systems (such as foundations, suction
piping, discharge piping, and so on), to
ensure safe operation.
Many unit operations including
distillation, evaporation, drying, crystallization, filtration, and others are
often conducted under vacuum conditions. To achieve the desired vacuum,
the following three process- vacuum
systems can be used:
Integrated vacuum systems (which
combine steam ejectors and mechanical vacuum pumps)
Available capacities and operating
ranges for vacuum pumps and vacuum
pumping systems that are most often
used in process operations throughout
the chemical process industries (CPI)
are listed in the Table on p. 60 [1].
This article reviews the hazards associated with steam ejector systems
and mechanical vacuum pumps, and
recommends design and operating
practices that can be taken to prevent
or mitigate these dangers.
1. Editors note: This is the first half of a twopart article. Part 2 is scheduled to appear in the
October 2012 issue.
Steam ejector systems are generally categorized into one of four basic
types: single-stage, multi-stage noncondensing, multi-stage condensing,
and multi-stage with both condensing
and non-condensing stages.
For many years, steam ejector systems dominated process applications
thanks to their simplicity, low purchase cost, good reliability and their
ability to be designed for very large capacities (in excess of 1,000,000 acfm)
and be operated at very low pressures
in the micron range (for instance, sixstage units are routinely designed for
suction pressures in the range of 310
microns). They also are available in a
variety of materials of construction.
Steam ejector systems are ideal for
wet-vacuum and highly corrosive applications. As a result, they are still
being used instead of mechanical
vacuum pumps in applications that
require a reliable vacuum system that
can tolerate corrosive chemicals, liquid slugs and solids carryover.
Safety considerations. In general, there are very few safety problems associated with the operation
of steam ejector vacuum systems.
However, one safety issue associated
with their design is the potential for
back-streaming of steam into the process equipment.
For instance, steam ejectors normally use a steam bleed to control
the suction pressure. If the process
TI
TI
To seal pot
Steam
supply
Condensate
Aftercondenser
Vacuum Systems:
Recommendations
For Safe Operation
PI
YZ intercondenser
Suction
Cooling water
supply
To seal pot
Gate valve
PI Pressure indicator
Four-way valve
TI Temperature indicator
Steam trap
Piccolo connection
FIGURE 1. Shown here is a schematic

of a three-stage steam ejector system
with inter-condensers (Reprinted with
permission from Ref. 1)
contains a water-reactive chemical

(such as acetic anhydride), a steam
bleed is not acceptable. If the ejector
should backfire, this will push steam
back into the process and could result
in a possibly violent reaction, which
could overpressure the system.
To avoid this problem, a nitrogen
bleed can be used to control the suction pressure. If the jet should back
fire, nitrogen will prevent the steam
from reaching the process. However,
using nitrogen to control an existing
multi-stage ejector may not be technically feasible. If nitrogen is to be used
to control a multi-stage jet, the user
must indicate this when writing the
performance and equipment specifications for the steam ejector.
Using nitrogen to control the suction pressure of the first stage that
which is closest to the process will
affect the design of subsequent stages,
and using nitrogen to control suction
pressure can significantly affect the
design of the inter-condensers. If the
back flow of steam or water into the
process equipment from the ejector
system can cause a serious safety or
quality problem, then a liquid separator (a so-called knockout pot) may be
installed between the ejector system
and the process equipment.
Another possible safety problem
may result from the loss of the intercondenser cooling medium (usually
water), which could lead to overpressure of the system.
Chemical Engineering www.che.com september 2012
59
In instances where suction gases,
or materials entrained in the suction
gases, might freeze inside the ejector,
ejectors with external heating jackets
can be specified.
Instrumentation. It is good engineering practice to provide adequate
instrumentation to monitor and control the operation of the steam ejector
system. The following instrumentation items are recommended for monitoring and controlling the vacuum
system, and to support troubleshooting efforts:
Control system for controlling the
steam bleed to maintain the desired
vacuum level
Pressure gage on the main steamsupply line
Steam pressure gage on each
ejector
Suction pressure gage on the inlet to
each ejector
Vacuum gage to monitor absolute
pressure at the process vessel
A flowmeter to monitor the water
flow to each inter-condenser
Temperature gages on the inlet and
outlet water lines to and from each
shell-and-tube inter-condenser
Temperature indicator in the barometric leg from each barometric
condenser
Design options. Mechanical vacuum

pumps usually are classified as either
wet pumps or dry pumps. The following lists show which mechanical
vacuum pumps are wet and which are
dry [2]:
Wet pumps:
Oil-sealed rotary vane (single- and
dual-stage)
Oil-sealed rotary piston
Liquid ring
Dry pumps:
Rotary claw
Rotary lobe (Roots)
Rotary scroll
Rotary screw
Rotary vane
Rotary piston
Diaphragm
Oil-sealed vacuum pumps. Both
rotary-vane
and
rotary-piston
vacuum pumps rely on oil for the
following functions:
To seal the internal clearances be60
Table 1. Capacity and operating range for vacuum pumps

and vacuum pumping systems commonly used in process
applications
Type
Blind or
base pressure
Lower limit for

process applications
Single unit
capacity
range, ft3/min
Single ejectors
One stage
50 torr
75 torr
101,000,000
Two stages
4 torr
10 torr
Three stages
800 micron* 1.5 torr
Four stages
100 micron
250 micron
Five stages
10 micron
50 micron
Six stages
1 micron
3 micron
Liquid-ring pumps
60F water-sealed:
One stage
50 torr
75 torr
318,000
Two stages
20 torr
40 torr
Oil-sealed
4 torr
10 torr
Air ejector first stage
2 torr
10 torr
Rotary-piston pumps
One stage
5 micron
100 micron
3800
Two stages
0.001 micron 10 micron
Rotary-vane pumps
Operated as a dry compres20 torr
50 torr
206,000
sor
Oil-sealed, rough-vacuum
0.5 torr
20 torr
50800
pump
Oil-sealed, high-vacuum
pump:
One stage
5 micron
100 micron
3150
Two stages
0.001 micron 10 micron
Rotary-lobe blowers:
One stage
100 torr**
300 torr
3030,000
Two stages
10 torr**
60 torr
Integrated pumping systems
Ejector-liquid ring pump
1 micron
3 micron
100100,000
Rotary-blower, liquid-ring
1.0 torr
5 torr
10010,000
pump
Rotary-blower, rotary-piston
0.1 micron
0.10 torr***
10030,000
pump
Rotary-blower, rotary-vane
20 micron
200
10030,000
pump
micron****
* 1.0 micron = 0.001 torr
**Based on intercooled design that uses gas admitted to a trapped discharge pocket to cool the blower
***Based on using a two-stage, rotary-piston pump as the backing pump
****Based on a two-stage, rough-vacuum, rotary-vane design that exhibits a
base pressure of approximately 0.5 torr
Source: Ref. 1
tween rotary components and housing to reduce gas slippage

To transfer the heat of gas compression away from wear surfaces
To lubricate the rotary internals
To flush away moisture
To inhibit corrosion of internal
parts
During operation, an oil-sealed

pump compresses the gas to a pressure that is slightly higher than atmospheric to expel it through the exhaust
valve. At this pressure, and at an operating temperature of 70100C, active gases readily attack pump bearings, seal materials and the oil. The
Outlet
Seal
0.0001-in.
clearance
Separator
baffle with
screen
Inlet
Discharge
valve
Inlet
Rotor
Discharge
Vanes
Slide
pin
Oil level
view port
Piston
Cam
Automatic
decanting
arrangement
Stator
FIGURE 2. Shown here is a schematic of the internals of a rotary-vane vacuum

pump (left) and a rotary-piston vacuum pump (right) (Reprinted with permission
from Ref. 1)
selection of an appropriate oil for the

application is critical for good pump
maintenance.
This dependency on the oil for internal lubrication is a limiting factor in
the use of these types of pumps in the
CPI. The integrity of the oil must be
maintained to avoid internal damage
that could cause contaminant buildup.
Particulates in the oil must be filtered
out ahead of the vacuum pump, and
water or solvent vapors must either be
removed ahead of the pump by using
pre-condensers, or prevented from
condensing within the pump by the
use of gas ballasting (air stripping) or
oil distillation.
For oil-sealed, rotary-vane vacuum
pumps, a variety of oils are available,
each with very different properties.
The sealing oil used in such pumps
that are destined for chemical service
has several additional requirements.
For instance, it must:
Be inert to chemical attack by
acids, bases, halogens and halogeninduced aging)
Be resistant to strong oxidants such
as oxygen, chlorine and fluorine
Possess good solvent power for problematic, mostly organic constituents
of pumped media, such as oligomers,
polymers, resins, crystalline decomposition or reaction products
Both oil-sealed, rotary-vane and piston vacuum pumps need periodic oil
changes. The chief purpose of changing of the oil is to remove particles that
either originate from aging of the oil
or particles that are generated by the
process (such as dust, decomposition
products, and other contaminants).
When either an oil-sealed rotaryvane or rotary-piston vacuum pump

is improperly installed a hazardous
condition can result. The following
installation practices will minimize
potential problems with these types of
oil-sealed vacuum pumps [1]:
Foundations. The foundation design
will depend on the type and size of the
oil-sealed pump. If the pump is inherently balanced, it can be mounted on
any floor that is able to support the
weight of the pump. However, pumps
that are partially balanced, should
be installed with vibration mounts
or matting between the base and the
floor. If the pump is not balanced, the
base should be securely fastened to a
concrete foundation with anchor bolts
and grouting. The pump manufacturer
should be consulted when designing
the pump foundation. It is always good
engineering practice to install flexible,
bellows-type connectors in the suction
and discharge piping; these can help
to isolate the rest of the system from
pump vibration.
Suction piping. Certain precautions
must be taken when installing the suction piping for an oil-sealed vacuum
pump. Care must be taken to prevent
any backstreaming of pump oil into
the process vessel and to prevent process liquids and solids from reaching
the pump. Backstreaming of oil is especially significant with larger pumps.
Baffles and traps are frequently installed in the suction line to prevent
this from happening.
Cold traps, knockout pots, wet scrubbers, and bag filters are some of the
devices used to protect the pump from
liquids and particulates in the suction stream. The degree of protection

necessary will depend on the process
application. If the upstream knockout pot is not continuously drained, a
high-level sensor should be installed
to automatically stop the pump or
close an isolation valve to prevent any
overflow from the knockout pot from
reaching the pump.
Oil-sealed vacuum pumps must be
protected from flooding if the oil flow
does not automatically stop when the
pump is shut down. To prevent flooding, a valve can be installed in the
suction line to admit air or nitrogen
to break the vacuum when the pump
stops. This prevents the siphoning of
oil from the reservoir when the oil is
not being discharged from the pump
by the normal pumping action. A zerospeed switch or solenoid valve is used
to actuate the air or nitrogen bleed
and close the isolation valve. Closing
the isolation valve allows the process
to remain under vacuum and allows
the vacuum in the pump to be broken
more quickly.
Flooding may be avoided with some
oil-sealed pumps by sealing the discharge line using a barometric leg
or a discharge check valve. This allows the system to pull a vacuum on
the oil reservoir so that oil siphoning
stops. A check valve or knockout pot
must be installed in the suction line to
prevent reverse flow from carrying oil
into the process vessel. A knockout pot
is recommended for critical applications where carryover of oil into the
process vessel might result in a fire
or explosion.
Discharge piping. Condensable vapors
that pass through an oil-sealed pump
tend to condense in the discharge line.
The discharge piping should slope
away from the pump, and a drip-leg
or knockout pot should be installed
in the discharge line to prevent the
backflow of condensate into the pump.
Backpressure on the pump should
be minimized.
Serious mechanical damage can result if the pump is operated against
a closed discharge valve. Discharge
valves are therefore not recommended
unless the pump must discharge into
a common exhaust header. If a discharge valve is required, an interlock
61
(that ensures that the exhaust valve is
open before the pump can be started)
is recommended; in fact, this is a condition of the warranty for some vacuum-pump manufacturers.
A fine mist of oil drops is emitted
with the exhaust gases that are discharged from an oil-sealed pump. Exhaust filters are normally installed
to eliminate this oil mist. The most
popular design has removable filter
elements and can be mounted anywhere in the discharge line. Units are
available that can remove up to 99.9%
of the exhausted oil mist. Oil mist filters should not be allowed to become
blocked, as hazardous over-pressures
could occur. A differential pressure
sensor and alarm can be installed on
oil mist filters to monitor their operation and detect potential blockages.
If the oil mist is contaminated with
organic compounds from the process
gas, especially if they are toxic, then
an activated carbon filter should be installed after the oil mist filter. The activated carbon filter will remove these
contaminants by adsorption.
Pump cooling. Oil-sealed pumps must
be cooled to remove the absorbed heat
of compression. Both water- and aircooled models are available. Air-cooled
models should be installed in an area
that will allow an ample flow of fresh
air to reach the pump. The jackets on
water-cooled pumps usually contain
small clearances that can plug with
solids. A strainer or filter should be
installed in the cooling water supply
line to remove any solids. A regulating
valve should be installed in the cooling-water supply line to control the
pump operating temperature. A hightemperature cutout switch is sometimes installed to protect the vacuum
pump from overheating.
Movement of oil and flammable
vapor droplets from oil-sealed vacuum
pumps has been known to generate a
static charge, which could lead to a fire
or explosion [3]. To avoid or minimize
this potential hazard, it is critical to
inert the exhaust stream with nitrogen to eliminate oxygen or reduce it to
below the limiting oxygen concentration (LOC).
Also, in many cases, it is prudent to
use nitrogen to dilute the gas stream
upstream of the pump inlet to move it
62
out of the flammable range. It is critical that the nitrogen supply source be
free of oxygen. There have been a few
instances where the nitrogen supply
was compromised, allowing in air that
can lead to an explosion [3]. For pyrophoric gases, such as silane, special
care must be taken to prevent air or
oxygen from entering the system.
Liquid-ring vacuum pumps
Liquid-ring vacuum pumps are widely

used in the CPI. They are available
as single-stage (one or two impellers
in parallel) or two-stage (two impellers in series) units. This type of pump
does not require internal lubrication
of the impellers, since they do not contact the housing. The sealant liquid,
used for both sealing and cooling, can
be virtually any liquid that is compatible with the process gas. For instance,
water, low-viscosity oils, glycols and
many process solvents such as toluene, xylene, methanol, ethanol, propanol, butanol and ethylbenzene have
been used as sealants in liquid-ring
pumps. Other liquids have also been
used, such as ethylene glycol and propylene glycol, and even sulfuric acid.
The motor horsepower must be corrected for the sealant viscosity and
density (see Reference 1, p. 273). These
sealants can be recirculated in a full
recovery system that includes a gasliquid separator tank and a heat exchanger to cool the sealant liquid. Even
higher vapor-pressure sealants can
be used if a low-temperature coolant
(such as glycol solution) is used in the
heat exchanger to reduce the sealant
liquid temperature. This recovery system allows process materials to be collected in the pump and either returned
to the process or collected for disposal,
thereby minimizing contamination of
other liquids or the environment.
The most advantageous property of
liquid-ring vacuum pumps is the fact
that they are nearly isothermal. The
liquid in the pump provides an ample
heat sink for the removal of the heat
of compression. This means that the
temperature rise in the casing is very
small. It is a function of the characteristics of the sealant fluid used, its
temperature, flowrate, and of course,
the process gas conditions. The resulting low internal temperatures provide
improved safety, especially when compressing explosive gases and fluids.

Generally, internal temperatures
in liquid-ring vacuum pumps are the
lowest of most mechanical vacuum
pumps. Hence, gases exit at almost
the same temperature, or in some
cases, at a lower temperature than
they enter the vacuum pump. Further,
since the gases handled are in direct
contact with large amounts of sealant liquid, even if touching of internal parts (the rotor with the casing)
occurs, the resulting sparks are not
hot enough or of sufficient duration
to cause explosions or ignition of even
the most hazardous gases. This provides a significant safety advantage,
especially when handling easily ignitable gas streams. The occurrence of an
explosion within liquid-ring vacuum
pumps handling flammable vapors is
very unlikely as the sealant liquid in
the pump casing acts as a hydraulic
flame arrester, quenching any flame
that may be generated and preventing
it from propagating.
However, one of the major drawbacks
of liquid-ring vacuum pumps is that
they must cope with cavitation when
running at low inlet pressure. If cavitation is allowed to continue over long
periods of time, serious damage can be
done to the pump. The amount of cavitation can be affected by the sealant
liquid, sealant temperature, impeller
speed, blade angle and inlet pressure.
For a given pump and sealant liquid,
cavitation can normally be suppressed
by bleeding air (or nitrogen) into the
pump inlet to raise its total pressure
above the vapor pressure of the sealant at operating temperatures.
All liquid-ring pump units have auxiliary equipment such as a vapor-liquid separator, a sealant recirculation
pump, a sealant cooler, and various
instrumentation items, relief devices
and valving.
Some advantages and disadvantages of liquid-ring pumps are summarized below:
Advantages:
Has a simple design that uses only
one rotating assembly
Can be fabricated from any castable
material
Creates
minimal
noise
and
vibration
In this sector liquid moves outward,

draws gas from inlet ports
into rotor chambers
In this sector liquid moves inward,

compresses gas in rotor chambers
Inlet
connections
Body
Liquid
Inlet
port
Inlet
port
Rotating
liquid
compressant
Rotor
Discharge
ports
In this sector
compressed gas
escapes at discharge ports
Experiences little increase in the

temperature of the discharged gas
Experiences no damage from liquid
or small particles in the process gas
Enables simple maintenance and
rebuilding
Uses a relatively slow rotational
speed (1,800 rpm or less), which
maximizes operational life
Can use any type of liquid for the
sealant fluid in situations where
co-mingling of the sealant with the
process vapor is permissible
Has no lubricating liquid in the process equipment to be contaminated
Can accommodate both condensable
and non-condensable gases while
operating as both a vacuum pump
and condenser
Disadvantages:
Mixing of the condensed gas/vapor
with the sealing liquid, which requires external equipment to separate them
The risk of cavitation requires a
portion of the process load to be
noncondensable under operating
conditions
High power consumption requires
large motors to form and maintain
the liquid ring
Achievable vacuum is limited by the
vapor pressure of the sealant liquid
at the operating temperature
The power consumption of a liquidring pump is normally higher than
that of other types of mechanical
vacuum pumps
The proper installation of a liquid-ring
vacuum pump is critical to its operation and maintenance. The following
recommendations should be followed
to ensure proper installation [1, 4]:
Foundations and pump checking.
Discharge
connections
FIGURE 3.
This figure
shows a crosssectional view
(above) and
general view of
assembly (right)
of a liquid-ring
vacuum pump
(Reprinted with
permission from
Ref. 1)
Since liquid-ring pumps do not usually create vibration problems, special

foundations are not required. Pumps
that are about 50 hp or above are best
placed on a concrete pad. Smaller units
may be mounted on existing floors and
skids. On pumps of all sizes, the base
should be leveled and the coupling
alignment should be checked during
installation. On belt-driven models,
the sheaves should be aligned and the
proper v-belt tensions set according to
the manufacturers instructions. After
the motor has been wired, the pump
rotation must be checked to ensure
that the polarity is not reversed. Do
not test the polarity without liquid in
the pump.
Suction piping. A check valve or a
valve that closes automatically when
the motor is shut down should be installed in the suction line to prevent
dumping of the liquid from the pump
back into the upstream process vessel in the event of pump failure. This
check valve will also serve to prevent
any backflow of air into the upstream
process vessel.
Where protection against backstreaming air is critical due to process
requirements, the vent and drain on
the separator should be barometrically

sealed. This can be accomplished by
discharging to a seal pot or by installing a vertical run in the suction line to
serve as a barometric leg between the
pump and the process vessel. If the
suction line is used as a barometric
leg, the vacuum pump discharge must
be sealed beneath the liquid level in
the separator.
A vacuum relief device should be
installed in the suction line on pumps
that are not automatically controlled.
Otherwise, the pump may cavitate during operation at low suction pressures
or when it is dead-headed by mistake.
The vacuum relief valve should be connected to a supply of inert gas (usually
nitrogen) if admitting air to the system is unacceptable.
If inlet spray nozzles are used to
condense incoming vapors, the nozzles
should be located in the suction piping
as close as possible to the pump. An
enlarged pipe section or a small vessel
may be needed to provide contacting
space between the spray liquid and incoming vapors.
Discharge piping. The pump and
discharge piping must be installed to
minimize backpressure on the pump.
63
Both the compressed gases and the
sealing liquid are discharged through
the pump discharge connection, and
the discharge piping must be sized
for two-phase flow. Piping of the same
diameter as the discharge connection
will usually be adequate, but a larger
line may be required if the distance
to the vapor-liquid separator is more
than a few feet. The discharge piping should never rise more than 23
ft above the pump before the gas and
liquid are separated. The discharge
piping should be designed so that it is
free to drain after a shutdown.
Pump draining. The pump casing
should be drained to the shaft level
before a liquid-ring pump is started.
Starting the pump when it is completely filled with liquid will overload
the motor and place undue mechanical
stresses on the shaft and rotor. Shaft
failure is not uncommon on large liquid-ring pumps operated in this way.
A solenoid valve installed in the sealant supply line to the pump is the best
way to stop the flow of sealant when the
pump is shut down. It will not be necessary to drain any residual liquid from
the casing. If sealant is recirculated
from the vapor-liquid separator, the
sealant will automatically drain to the
shaft level if the separator is designed
with an overflow nozzle at the pump
shaft level. The sealant may be manually drained to the shaft level through
a hole drilled in the pump casing or by
a drain in the sealant supply line.
If the pump is located outdoors or
in unheated buildings, it should be
completely drained for freeze protection during prolonged shutdowns.
Similarly, the pump must never be restarted dry; it must be partially filled
with sealant liquid. This may necessitate a bypass around the solenoid
valve in the sealant supply line.
Sealant piping. There are three possible arrangements for sealant flow
to liquid ring pumps: Once-through
(no recovery), closed loop (recirculated
sealant) and partial recirculation system (partial recovery).
Once-through arrangement. A oncethrough installation does not necessarily imply that none of the sealant
is recovered; rather, the term simply
refers to the absence of any return
piping from the vapor-liquid separa64
Edwards
Vacuum
FIGURE 4. This is a cutaway

view of a rotary-claw type dry
vacuum pump, showing all
components of the pump
tor drain to the pump-sealant supply

connection. This is a common arrangement where conservation or contamination of the seal liquid is not a
concern.
The line supplying sealant to the
pump should contain a shut-off valve
followed by a strainer with a blowdown valve to remove particulates. An
automatic solenoid valve may be installed in the supply line, interlocked
with the pump motors operation, to
prevent flow of sealant to the pump
in case the motor stops running, (in
this case, if the motor stops, the valve
closes to prevent the pump casing
from filling with liquid).
If a solenoid valve is used, a bypass
should be installed to allow some sealant to be introduced before starting
(when the pump has been completely
drained). The sealant flow can be regulated manually or automatically.
The manual method regulates the
flow by a globe valve (upstream of
an orifice), which uses pressure drop
across the orifice to set the desired
pressure to the pump. The orifice is
usually chosen so that the proper flow
to the pump is set by maintaining a
pressure drop of 5 to 10 psi across the
orifice. Automatic control is achieved
by using a flow controller to maintain
a constant pressure drop if the sealant
supply pressure tends to fluctuate.

Closed loop (total recirculated sealant) arrangement. In this arrangement the system is designed to operate as a closed loop with no addition
of fresh sealant. Only the vapors that
condense in the pump need to be removed from the system. In actual
practice, however, some fresh sealant
is often continually added to control
the concentration of low boilers or
other contaminants in the sealant or
to make up for evaporative losses from
the system.
A heat exchanger is installed in this
system to remove the heat of compression and condensation from the sealant before it is reintroduced into the
pump. The heat exchanger is normally
water cooled, but any suitable coolant can be used. Often, the system is
provided with a sealant recirculation
pump. This allows more flexibility in
the design and operation of the vacuum system. The sealant cooler can be
designed for a higher pressure drop,
which results in better heat transfer
and reduced fouling. A recirculation
pump must operate at suction pressures that are too high to siphon
an adequate flow of sealant from the
separator and in operations involving
frequent or prolonged evacuation. A
recirculation pump is often used for
systems in which several vacuum

pumps share a common separator.
The fresh sealant makeup line is installed in much the same way as for
a once-through installation. In addition, a check valve should be installed
in the makeup line to prevent reverse
flow if makeup supply pressure is lost
while the vacuum pump is operating.
The recirculation line should contain a strainer and one or more temperature gages. The strainer removes
solids that would otherwise accumulate in the sealant. Temperature gages
should be installed on both sides of
sealant coolers to monitor heat exchanger performance.
Partial recirculation (partial recovery) arrangement. A partial recirculation system has no sealant cooler.
Fresh solvent makeup is used as the
heat sink. A portion of the total sealant flow is supplied as cold makeup
and the rest is recirculated from the
separator. The fresh and recirculated
streams mix and come to some intermediate temperature before entering
the vacuum pump. The desired temperature is controlled by varying the
ratio between the two streams until a
satisfactory temperature is reached. A
partial recirculation arrangement can
reduce fresh sealant requirements
by 50% or more compared with oncethrough systems, depending on the
temperature of the fresh stream.
The recommendations about piping
design and filters given in the section
on closed-loop arrangements apply
here as well.
Potential hazards and options to
prevent or mitigate them. Listed
below are some potential hazards of
liquid-ring vacuum pumps and measures that can be used to prevent or
mitigate them [5]:
The escape of flammable or toxic
vapors from failed mechanical seals
can create external hazardous conditions. Liquid-ring vacuum pumps
handling non-hazardous vapors
usually are provided with single mechanical seals. If these pumps handle flammable or toxic vapors, then
double mechanical seals should be
installed with seal-welded connections to eliminate leak paths
Improper installation, mounting,
and alignment of pumps: This can
cause damaging vibration, which

can lead to potential seal or other
mechanical failures and leakage to
the environment of internal fluids
(sealant, gas or both)
Improper installation of piping
can result in external loads on the
casing leading to pump failure, or
again, leakage of internal fluids to
the atmosphere
Liquid-ring pumps use seal liquids that are in direct contact with
the process gases, and if the gases
pumped are flammable or toxic, the
discharged gases and sealants will
potentially also be hazardous
Since seal liquids are in direct contact with the process gases, liquid
ring pumps act as mixers in a sense,
and any potential reactions between
the seal liquid and the process gas
must be considered
Gases and seal liquids are discharged together and proper separation must be done if the gases are to
go to subsequent processes. If gases
or vapors condense or dissolve in the
seal liquid, consideration must be
given to selecting the proper materials of construction for the discharge
system to resist attack by any of
the gases present in the process gas
stream to the pump, or introduced
and/or formed in the seal liquid
Seal liquids, if recirculated, will
become saturated to equilibrium
states with the process gases being
pumped. As a result, the overflows
from a liquid-ring pump system
must be treated as a hazardous liquid if the gases are flammable or
toxic. Since, in many cases the seal
liquid is reused in the system, the
concentrations of contaminants can
increase with time
Since compression in a liquid-ring
vacuum pump is essentially isothermal, this means that any vapors or
gases exiting will be saturated with
the seal liquid and that any potentially hazardous vapors or gases
may condense and be discharged as
liquids to the discharge system
Proper materials of construction
must be selected if liquid-ring
pumps use seal liquids that are corrosive (such as sulfuric acid) or if the
process gases contain corrosive components
Liquid-ring vacuum pumps are not

generally built for high pressures
and use non-live sealed gasket systems for the most part. This means
that if pressure can rise in hazardous systems quickly, the liquid ring
system is often the lowest pressure
component, and must be protected
from the rise or particular design
variations made, to ensure that they
are resistant to maximum pressures
that may occur
Dry vacuum pumps
Dry vacuum pumps have been used

since the 1980s, originally in the semiconductor industry, then in the pharmaceutical industry, and now in other
chemical process applications. They
have several advantages, as follows:
No contamination of the process
caused by backstreaming of sealing
liquids or lubricating oils
No contamination of evacuated gas
with sealing liquid or lubricant
Due to lack of condensation (which
is assured because the pump runs
hot), the pump can be fabricated of
standard, inexpensive cast iron
They have a rugged rotor design
which is constructed of sturdy cast
iron, or ductile iron, without any
flimsy rotating components
Noncontact design: Timing gears
are oil lubricated in a sealed-off end
chamber to synchronize the rotors
for proper phasing and noncontacting operation
High operational speed: Operation
at high speeds reduces the ratio of
gas slip to displacement, increases
net pumping capacity and reduces
ultimate pressure. To accomplish
this, the rotors are well balanced
They can be designed with multiple
staging
The pump can discharge to the atmosphere
They can be used for handling corrosive gases
They can be used for handling flammable gases as the pumps are designed for containment of an internal explosion for this service
However, they also have the following
drawbacks:
They cannot handle particulates,
nor slugs of liquid
They may require a silencer
65
They may discharge gases at high
temperatures, in some cases as high
as 350400C. Newer designs allow
running at lower temperatures and
have precise temperature control
Some models are difficult to repair
or rebuild
They may require a gas purge for
cooling or to protect the bearings
and seals from the process gas
Due to the high operating temperature, some process materials such as
monomers, may have a tendency to
polymerize
An excellent overview of dry vacuum
pumps is presented by Ryans and
Bays [6]. Two types of vacuum pumps
that are used in high and ultra-high
vacuum applications are the turbomolecular pump and diffusion pump.
However, they are not discussed in
this article.
Author
References
1. Ryans, J.L., and Roper, D.L., Process Vacuum

System Design and Operation, McGraw-Hill
Book Co., New York, N.Y.1986.
2. Chew, A.D., Mechanical Vacuum Pumps,
BOC Edwards paper.
3. Private communication (email) of July 8, 2011
from Mark Nichols of Edwards Limited.
4. Aglitz, A., and others, Installing liquid ring
vacuum pumps, Chem. Eng., November 1996.
5. Private communication (email) of August 11,
2011 from John Campbell of SIHI Pumps
Americas.
6. Ryans, J., and Bays, J., Run clean with dry
vacuum pumps, Chem. Eng. Prog., pp. 3241,
October 2001.
7. Edwards Ltd., Safety Manual-Vacuum
Pump and Vacuum Systems, 2008.
8. NFPA 69, Standard on Explosion Prevention Systems, National Fire Protection Association, Quincy, Mass., 2008.
Stanley S. Grossel is president of Process Safety

and Design, Inc. (4 Marble Court, Unit 9, Clifton,
N.J. 07013-2212; Phone: 973-779-3668; Email:
psadi28@aol.com). He provides consulting services related to process safety and loss prevention,
storage and handling of bulk solids and powders,
air pollution control, and process design of batch
plants. Prior to his 1993 retirement, Grossel spent
25 years in the Engineering Dept. of Hoffman-LaRoche, in a variety of roles. He was honored as the
only Senior Engineering Fellow ever to be designated by Hoffman-LaRoche. Grossel is a fellow of
AIChE, and holds AIChEs Norton Walton/Russell
Miller Award for outstanding contributions to loss
prevention. He has lectured and been published
widely, and has authored major standards and
guidelines. Grossel is also a contributor on process
safety to the 7th Ed. of Perry's Chemical Engineers Handbook. He holds a B.S.Ch.E. from City
College of New York and an M.S.Ch.E. from Drexel
Inst. of Technology, and has completed courses toward a doctoral degree.
Acknowledgements
lowing people who provided technical

information that was used in writing
this article: Peter N. Lodal (Eastman
Chemical Co.), John Campbell (SIHI
Pumps Americas), Mark Nichols (Edwards Ltd.), and Eric Johnson (Graham Manufacturing Co.).
The author wishes to thank J.L. Ryans

of Eastman Chemical Co. (Kingsport,
Tenn.) for his review of the draft of
this article and for his helpful comments and recommendations. I also
acknowledge the assistance of the fol-
September 2012
Literature Review
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Minimizing Fire Risk at CPI Facilities Volume 2

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Minimizing Fire Risk at CPI Facilities

Focus on Plant Hazards

A Checklist for Safer Chemical Batch Reactions .................................................................................. 10

Designing Safer Process Plants ............................................................................................................. 12

Preventing Self-Heating and Ignition in Drying Operations ................................................................ 17

Facts at Your Fingertips: Gas Hazard Definitions and Data .................................................................. 20

Clearing the Air About Respiratory Protection ..................................................................................... 26

Eye-and-Face Personal Protective Equipment ..................................................................................... 32

Managing Compliant MSDSs and Labels ............................................................................................. 36

Design Safer Solids Processing Plants ................................................................................................. 39

Finding the Right Gloves To Fit the Application ................................................................................... 45

Dust Control in the Chemical Processing Industries ........................................................................... 49

Avoiding Static Sparks In Hazardous Atmospheres ............................................................................ 53

Piping Design for Hazardous Fluid Service .......................................................................................... 57

Chemical Protective Clothing ................................................................................................................ 64

Managing Material Safety Data Sheets in the Workplace ................................................................... 67

Dust Explosions: Prevention & Protection ............................................................................................ 70

Prevent Explosions During Transfer Of Powders Into Flammable Solvents ...................................... 75

Preventing Dust Explosions ................................................................................................................... 83

Compressed Gases: Managing Cylinders Safely ................................................................................. 86

Reduce Hazards in Process Vacuum Systems ...................................................................................... 93

Tolerable Risk .......................................................................................................................................... 100

Vacuum Systems: Recommendations For Safe Operation ................................................................. 106

How to Handle Hydrogen

ydrogen is widely employed

Process-unit layout, piping, instrumentation/control

When gas is released or escapes from

CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006

ing pressurized liquid hydrogen may

Key considerations that must be taken

brittlement. Therefore, post-weld annealing is recommended to restore the

Some important factors in determining the location for a hydrogen facility

CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006

TABLE 1. PIPING SYSTEMS FOR HYDROGEN

Piping materials and designs should be in compliance with ANSI/ASME B31.1,

sources of information that relate hydrogen

All hydrogen lines should be labeled as HYDROGEN, with flow-direction arrows

of 100 and a maximum of 216 lb/ft2.

CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006

Piping and supply lines

TABLE 2. INSTRUMENTATION AND CONTROL

FOR HYDROGEN-HANDLING SYSTEMS

Shut off the hydrogen supply and open vent line

2. On high pressure in the

Shut off the hydrogen supply and open vent line

3. On low speed of reactor

Shut off the hydrogen supply and open vent line

Shut off the hydrogen supply and open vent line

5. On flame out of the flare

Shut off the hydrogen supply and open vent line

An excess flow valve is required to

Control and monitoring

Minimum instrumentation and control practices for hydrogen plants are

strument sensors. Examples of critical safety instruments installed with

In any hydrogen-using facility, provision must be made for safe disposal of

CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006

should be commenced upon the introduction of hydrogen gas in the process

CHEMICAL ENGINEERING WWW.CHE.COM APRIL 2006

This tank should be sized for at least

Most fires in hydrogenation facilities

sified as Class I, Division 1, Group

A fire protection system is required for

extinguish small fires. As precaution

A hydrogenation or other hydrogenusing facility is designed safely if it

Dynamic process simulation