Cryogenic Storage

Cryogenic Storage of Ammonia

Sachin D Chavan

Abstract
Gases such as ammonia, chlorine, LPG, propane, propylene, ethane, ethylene etc need to be stored
at low temperatures. Cryogenic storage of such fluids is a well developed science with its own com-
plexities. This article talks about critical points related to cryogenic storage, especially about am-
monia. This article describes in brief typical configuration of storage system, various codes, de-
sign guidelines, commissioning and recommissioning procedures, etc.

Sachin Dinkar Chavan is a chemical engineer and an alumnus of Tatyasaheb Kore Institute of Engineering
& Technology. He is presently Sr Engineer-Business Development, with Uhde India Pvt Ltd. He has handled
LSTK proposals for Ammonia Cryogenic Storage Systems. He worked with NOCIL RCD, Melog Speciality
Chemical Pvt Ltd, Ion Exchange India Ltd.

76 Chemical Industry Digest. October 2012

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 Cryogenic Storage

C
ryogenic is a Greek word meaning “the produc- cryogenic storage, viz:
tion of freezing cold,” however, the term is used A) Single Wall Tank
today as a synonym for the low temperature state.
B) Double Wall Tank
It is not well defined at what point on the temperature
scale refrigeration ends and cryogenic begins. C) Double Integrity Cup-In Tank
There are number of gases that require cryogenic stor- Let us review each one separately.
ages e.g. ammonia, chlorine, LPG, propane, propylene, A) Single wall tank
ethane, ethylene, natural gas, oxygen, nitrogen, hydrogen
These are the tanks with one steel bottom and wall
etc.
designed to contain the full liquid level of ammonia. In-
In this article we have described about the different sulation is provided on the external surface to minimize
types of ammonia storages methods, typical configura- heat leakage Fig A1. External containment is provided in
tion of storage systems, various codes and standards, de- the form of dyke wall to contain the liquid coming out
sign guidelines, guarantees involved, commissioning & due to rupture of inner tank. From Health, Safety and En-
recommissioning procedures, hazardous area classifica- vironment perspective single wall tanks are not recom-
tion, safety aspects, ammonia transportation challenges mended and hence these are no longer built. Existing
and opportunities for cryogenic storages. Single wall tanks are being replaced with Double Integ-
rity Cup-In Tanks. See Fig A2.
Types of ammonia storage tanks
Liquid ammonia is usually stored either at ambient B) Double wall tank
temperature under high pressure or at -33oC under atmo- The outer tank is intended to contain refrigerated prod-
spheric pressure. In some cases, it is also stored at inter- uct leakage from inner tank but is not intended to con-
mediate temperatures and pressures (semi-refrigerated). tain any vapor resulting from product leakage from the
O Pressurised storage (pressure: 12 – 18 kg/cm2 g) at inner tank which means, it will be released to atmosphere
ambient temperature for small capacities (up to 100 through flare. See Fig B1 and Fig B2. The outer container
MT) is in horizontal pressure vessels. is normally provided in the form of “Bund wall” of height
O Semi-refrigerated stor-
age is in spheres for ca-
pacities up to 2000 MT Carbon Concrete for carbon
Carbon
(pressure 4 – 6 kg/cm2 steel steel steel weather
container container protection
g).
Ammonia Ammonia
O Atmospheric pressure discharge discharge line
Insulation Insulation
storage is at -33oC for line

large capacities (2000

MT and higher). There Concrete Concrete
foundation foundation
are three different
Fig A1. Single wall with external insulation Fig A2. Single wall with external wall
types of tanks for such
Fig 1. Single wall tanks

Carbon Carbon steel Carbon Carbon steel

steel outer tank steel outer tank
inner tank inner tank
Ammonia Ammonia
discharge line discharge line
Insulation Insulation

Concrete Concrete
foundation foundation

Fig B1. Double wall Tank Fig B2. Double wall tank with common roof
Fig 2. Double wall tanks

Chemical Industry Digest. October 2012 77

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 Cryogenic Storage

Roof

Mineral wool

Suspended deck
Liquid Ammonia
PUF Insulation with Cup
aluminium cladding
Outer tank

Annular space

PCC
Perlite concrete
Concrete deck

Foam Glass
Sand Layer

Fig C. Ammonia storage tank. Double integrity cup-in-tank (typical sketch)

corresponding to hold equivalent amount of liquid in the the following:

storage tank.
C) Double Integrity Cup-In Tank
This Double Integrity Cup-In provides extra vapor
space of 15 – 20% depending on tank dimensions which
is very useful for maintaining tank pressure within op-
erating limits especially under emergency condition. The
presence of ammonia vapor in the annular space between
the cup and shell acts as an insulating media and helps
in reducing the heat ingress from outside. See Fig C.
The tank is designed as per the API 620, Appendix R.
The outer tank is insulated with rigid polyurethane foam
insulation that is formed in-situ. The bottom insulation
is foam glass and Perlite Concrete which is a load bear-
ing insulation. The top of the cup is insulated by min-
eral wool/fiber glass wool insulation which is spread on
a suspended deck. Insulation thickness is determined to
limit the tank boil off within 0.04 wt% per day.
The tank is equipped with two pressure relief valves
to safeguard against overpressure. Isolation valves are
provided with suitable mechanical interlock. Also the
tank is equipped with two vacuum relief valves to safe-
guard the tank against vacuum isolation valves are pro-
vided with suitable mechanical interlock.
The tank rests on elevated foundation for a free pas-
sage of air from below, so as to avoid freezing of founda-
tion. A staircase tower with platform landing up to tank
top is provided to access tank’s top nozzles.
System Configuration
The cryogenic ammonia storage system comprises of
O Ship Unloading Arm
O Cross country pipe line
O Atmospheric Ammonia Storage Tank (Double Integrity
Cup-In Tank)
O Ammonia Refrigeration System (Includes Screw com-
pressors, Condensers, Receiver etc.)
O Ammonia transfer pumps
O Flare system
O Ammonia drain tank
O Ammonia pre-heater (If applicable)
O Road/Rail loading/unloading station (If applicable)
O All Utility equipment (Cooling tower with Side stream
filters, Instrument air compressor system, DG System
etc.) – Considering stand alone storage system
O Electrical & Instrumentation system
Applicable Codes and standards
Cryogenic storage tank have to confirm to these codes
and standards;
O ASME, Sec. VIII, Div. 1 code for pressure vessels (re-
ceiver and drain tank) and heat exchangers
O TEMA Class R code for ammonia heat exchangers
O API 619 for ammonia refrigeration screw compressors
O API 610, 10th Edition for ammonia pumps
O API-RP 520/2000, ASME Sec. VIII, Div. 1 for safety
valves

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 Cryogenic Storage
O ASTM/ASME Sec. II for material specification
O API 620 Appendix R Feb 2008 edition + Addendum
1 2009 + Addendum 2 2010 for storage tank and DIN
4119 sheet 1 & 2 (1961) for roof structure
O API 520/521 for flare
O IEC/IS standards for electrical equipment
O ISA and DIN standards for Instruments
O Insulation as per DIN/ANSI
O Fire protection as per local regulations
Design Guidelines
Design guidelines to be followed include:
O Pressure safety/vacuum relief valve should be inter-
locked in such a way that if one of the valve is taken
out for maintenance then the other valve should be
in line. Also they must be provided with mechanical
interlock.
O All the first isolation valves are required to be welded
type on the tank side. The flange valves always have
danger of gasket failure.
O The vacuum and pressure safety valve shall be flange
type.
O While cooling the tanks from ambient temperature to
-33 0C the tank will undergo the differential expan-
sion therefore the stairways and the tank protection
rail shall be independently supported.
O The nozzle orientation of the tank particularly shall
be in such a way that the liquid inlet to the tank and
the vapor outlet from the tank shall be away from the
each other. This will reduce the liquid droplets in the
vapor line.
O The nozzles for the level indicator and the pump suc-
tion shall be away from each other. Pump under run-
ning condition will cause drop in the liquid level,
therefore if the liquid level indicator is away from the
pump suction it will have better accuracy in the level
measurement.
O The filing nozzle pipe shall be with perforation and
the filling pipe shall extend up to cup bottom so that
splashing is avoided during the filling operation.
Guarantees involved in cryogenic storage
System
O Tank Capacity
O Tank Boil-Off
O Liquid ammonia receipt from ship/plant
Chemical Industry Digest. October 2012
O Transfer rate of liquid ammonia to user plant
O Electric power
Commissioning & recommissioning proce-
dure
Important steps to be taken during commissioning and
recommissioning.
1. Hydrotest, either up to 70 or 100%, depending on the
design code.
2. Purge with nitrogen until the measured oxygen in the
discharge gas is less than 4%.
3. Then purge with ammonia gas until the measured oxy-
gen in the discharge gas is less than 0.5%.
4. Cool the tank down to as low a temperature as pos-
sible, at a cooling rate lower than 1oC/hr.
5. Measure the temperature in the bulk volume of the
tank, away from the gas inlet.
6. Within one week after commissioning and when con-
ditions are stable, take samples for water and oxygen
analysis from the ammonia liquid in the tank and
analyse them.
Decommissioning procedure
1. Empty the tank to the absolute minimum liquid level.
2. Evaporate the remaining ammonia in a way that en-
sures uniform and slow heating, not exceeding 1oC/
hour.
3. Measure the temperature in the bulk volume of the
tank, away from the gas inlet. Give careful consider-
ation to temperature measurements at the lower levels
of the tank during decommissioning.
4. Purge with warm ammonia gas or nitrogen until all
liquid ammonia is removed. The bottom area may need
to be cleaned before it is possible to get all the ammo-
nia gas out.
Hazardous Area Classification
Ammonia storage tank and associated facility falls un-
der Class 1 and Zone-2.
O Class 1 – For flammable liquids, gases and vapors
O Zone 2 – Area in which explosive gas atmosphere is
not likely to occur under normal operations and if it
does occur it will exist for short period only.
Gas Group
O All gases and vapors are classified in to 4 major
groups namely, I, IIA, IIB, IIC as per IS 2206. The clas-
sification is based on the minimum ignition energy re-
quired to raise the temperature of gas locally to attain
79
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 Cryogenic Storage
its ignition temperature. Ammonia falls under the gas
group – IIA.
Temperature Class
O Ammonia falls under the temperature class – T1
Ammonia Transportation
A) By Ship
O Sizes of ships generally range between 2000 MT to
46500 MT.
O Ships are equipped with refrigeration facilities and
pumps. Similar to those of storage tanks.
O They are designed for carrying multiple liquids of dif-
ferent density and temperature.
B) By Rail/Road
O Cryogenic liquid is transported by the rail tankers
(BTAL) for short distance. It is unloaded into the stor-
age tank via flash vessel or surge drum to control the
pressure in the tank.
O Generally, rail/road tanker loading station has follow-
ing facilities
H Liquid loading arm
H Vapor return arm
O Shut-off valve interlocked with the flow controller on
loading line and also with emergency stop switch
O Flow measurement, recorder and control system for the
safe loading into the tanker
O Drain Pot (if required)
Safety Aspects
Safety of the cryogenic tanks is of prime importance.
These tanks are designed for double integrity as against
the normal tanks of API 650 which are designed for single
containment. These tanks have inner cup to contain the
liquid and also have an additional outer tank to contain
the liquid in case of cup failure. Utmost care is to be taken
80 Chemical Industry Digest. October 2012
while designing the inner cup as well as outer
tank as both inner and outer tanks will be sub-
jected to various different load combinations.
O These tanks are subjected to low tempera-
tures and accordingly are equipped with vari-
ous critical features like special anchorage and
its attachment, ability to handle differential
expansion, special insulation for outer tank/
tank bottom/suspended deck etc. In view of
this, various stringent requirements for mate-
rials, fabrication/welding, inspection and test-
ing of tank must be considered which are dif-
ferent and stringent from normal API 650 Atmospheric
Storage Tanks.
O Storage tank design is required to meet high safety
standards and flare system is strongly recommended.
O The flare system consists of an adequately sized pipe-
line (assessed for critical condition) routed to a dis-
tant location (as per local applicable rules) and re-
leased at a height and burnt with a pilot gas (usually
LPG or NG).
O To limit the risk of over pressure in cryogenic reser-
voirs, it is essential to maintain a sufficiently low tem-
perature (-33oC) during storage and also while filling
the tank, even if small quantities are involved relative
to the volumes stored. Protective equipment such as
bursting and valves, correctly dimensioned, must also
play their role.
O Safety measures and equipment, such as emergency
controls must be permanently accessible, even in de-
graded situations.
O The redundancy of the equipment reduces the prob-
ability of major accidents but does not exclude it. Mul-
tiplication of the various types of barrier (alarms,
servo-system, emergency operating procedures, fail
safe security system) while avoiding common sources
of failure particularly when the stakes are high or the
installations are particularly dangerous. These are
some of the most effective ways of reducing major
risks, but they do not necessary eradicate them. Bear-
ing in mind the quantities stored in cryogenic reser-
voirs, the potential sources of danger in these instal-
lations are numerous; therefore the measures taken on
the technical, organizational and human fronts to pre-
vent accidents should be proportionate to these.
O Remote shut-off valves on liquid ammonia main inlet
and outlet line to/from ammonia storage tank should
be installed.
O Refrigeration system should be based on reliable screw
compressors with stand-by options.
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 Cryogenic Storage Cryogenic Storage

O Adequate fire water grid and water curtain around

ammonia pumps, compressor house and loading/
unloading stations should be provided.
O Thermal relief valves should be installed on the am-
monia lines where there is any possibility for block-
age or heat ingress.
O Ammonia leak detection system should be provided
for storage installation.
O Lighting protection and earthing protection should be
considered for storage tank.
O Emergency power is should be provided to one refrig-
eration holding compressor to maintain tank pressure
during power failure.
O Wind direction indicator should be provided.

Challenges & Opportunities

O Ammonia Stints (That’s good and bad)
O Storing millions of gallons of ammonia presents envi-
ronmental, health & safety concerns
O Ammonia handling is very energy intensive and com-
petitive
O Energy prices are hitting ammonia manufacturing and
handling very hard
O Many of the facilities were built in the old days and
need to be upgraded to newer technology
O Due to the very low temperature these liquefied gases CHEMICAL INDUSTRY DIGEST
cannot be managed using normal equipments and
thus require specially made equipments, known as
Highlights - November 2012
cryogenic equipments. Commonly used cryogenic
equipments are tanks, valves, compressors and Articles
pumps.

Advanced Materials
The global market size of all cryogenic equipment (not

Mechanical Equipment
limited to ammonia) is estimated to be $11 billion in 2011.
Cryogenic tank has the largest market and majority of
R&D/ Innovation
cryogenic equipment market revenue come from those

Multivariable Predictive Control
tanks. After tanks, valves are the second largest revenue
contributor in cryogenic market followed by compressors
Erection & Commissioning Challenges
and then pumps.
Plus Regular Features and much more . . . .

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Chemical Industry Digest. October 2012 81

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