Prepared by the Safety Advisory Group
Table of Contents
1. Compatibility of Gas and Cylinder Material ........................................................................Page 1
2. ASU Cold Box Over-pressurisation .....................................................................................Page 1
1. Compatibility of gas and cylinder
material
Some months ago a small aluminium cylinder
suddenly burst in a laboratory causing a release of
the gas and property damage. A few weeks later
another aluminium cylinder, a lecture bottle, burst
at another gas company causing minor property
damage. None of the accidents caused any injury.
In both cases the cylinder contained ethylene
chloride, a gas which must not be filled in
aluminium cylinders!
The standard EN ISO 11 114-1 on Transportable
gas cylinders – Compatibility of cylinder and valve
materials with gas contents – Part1: Metallic
materials and in the EIGA Technical Note
TN 507/90, Compatibility of Gas Cylinders and
Valve Materials with Gas Contents, as well as in
the ADR § 4.1.4.1, Packaging Instruction, clearly
state that ethylene chloride must not be filled in
aluminium cylinders. The two accidents made the
Safety Advisory Group concerned about the
implementation of official standards and industrial
practices (EIGA documents). Therefore we ask all
EIGA members to review their management
systems to ensure that external documents are
properly considered and implemented as required.
2. ASU Cold Box Over-pressurisation
There has been a series of accidents reported to
the Safety Advisory Group (SAG) of EIGA that are
concerned with ASU cold box over-pressurisation.
In these accidents, due to some fault in the
cryogenic process equipment, there is a leak of
gas or liquid into the interspace between the
column system and the cold box. This in turn
causes the cold box to be over-pressurised.
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SAG NL 75/02/E
Where the over-pressurisation protection
equipment is inadequate or the leakage and
evaporation rate exceeds the venting capacity, this
can lead to a release of insulant or, in extreme
cases, a failure of the metal cladding. In a powder
(perlite) insulated box this can, and has been
known to, expel all of the insulant. Even in cases
where over-pressurisation equipment has worked,
loss of insulant powder can still occur.
Incidents of this type pose different types of
hazard, the chief of which is the mobilisation of the
powder insulant. Even if the original leak is not
sufficient to cause the cold box to over-pressure,
the gas release can induce swirling of the powder
which in turn causes erosion and further damage
to the pipework and vessels within the cold box.
Additionally, the gases are very cold and can lead
to:
• Cracks in the cold box structure.
• The formation of large ice patches/blocks on
the outside of the cold box.
However, the predominant risks arise in any one of
three particular circumstances:
1 At the first start of the plant following
construction.
2 At the commencement of plant warm-up prior to
maintenance.
3 Shortly after the conclusion of maintenance
activities.
Typically there are two mechanisms for the failures
to propagate. Firstly, it is observed that pools of
cryogenic liquid are trapped within encrusted
insulant and these expand violently when exposed
to warmer temperatures as de-perliting
progresses. Secondly, during cool-down or warm-
up of the column system, stresses created by
thermal expansion or contraction go un-relieved
and splits or fractures are induced in pipework,
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 SAG NL 75/02/E – Page 2

commonly in
small bore impulse lines. This is prevalent at the Summary
upper parts of the cold box, usually on the argon
system but can occur at any location. In summary, the following factors should be
considered during the lifetime of a cold box:
Preventive measures
• The existence of an active interspace purge at
Both design and safe operating practices all times should be confirmed by the logging of
contribute to the prevention of the above- purge gas flow.
mentioned risks.
• Thermal stress relief design of cold box piping
Relief systems and components.

The importance of relief systems in mitigating a
cold box over-pressure incident is high. The
location of the chosen system on the cold box
faces is as important as the design basis for the
sizing and number of devices. A typical design
basis would be the maximum flow for the purge
and/or failure of an instrument line and/or a hole in
a liquid phase line.
• Over-pressure incidents typically occur during
plant thawing in preparation for maintenance.
Proper risk assessments should be performed
and contingency plans laid. Documented plant
defrosting plans are recommended and should
define valves status, flows, and time/-
temperature charts at various critical process
points.

Purge • Plants should be shut down as soon as

possible after an interspace leak is diagnosed.
More importantly, the checking and maintenance Delay will run the risk of erosion due to perlite
of cold box purge arrangements will help to reduce swirl or pooling of liquid with subsequent
the impact of a leak into the interspace. A healthy expansion due to heating.
purge gas flow of nitrogen will keep the perlite dry
and will provide early assistance in evaporating • During and after cool-down, the cold box
liquid pools. Regular logging of interspace purge should be monitored for signs of leaks as
parameters, preferably flow and pressure, will thermal contraction is maximum at this point.
assist in trouble-shooting and control of any
incident. It will also be of value to record the
constituents of the gas purge at the top of the ASU
cold box, as the presence of oxygen in any
proportion will probably indicate leakage. Oxygen
may also, in the absence of flow, indicate
condensing atmospheric air, or simply the ingress
of air itself to the interspace.

All technical publications of EIGA or under EIGA’s name, including Codes of practice, Safety procedures and any other technical information contained in
such publications were obtained from sources believed to be reliable and are based on technical information and experience currently available from
members of EIGA and others at the date of their issuance.
While EIGA recommends reference to or use of its publications by its members, such reference to or use of EIGA’s publications by its members or third
parties are purely voluntary and not binding. Therefore, EIGA or its members make no guarantee of the results and assume no liability or responsibility in
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EIGA has no control whatsoever as regards, performance or non performance, misinterpretation, proper or improper use of any information or suggestions
contained in EIGA’s publications by any person or entity (including EIGA members) and EIGA expressly disclaims any liability in connection thereto.
EIGA’s publications are subject to periodic review and users are cautioned to obtain the latest edition.

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