Prepared by the Safety Advisory Group

SAG NL 75/02/E

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 §, 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.

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 warmup of the column system, stresses created by thermal expansion or contraction go un-relieved and splits or fractures are induced in pipework,

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.

PHONE +32 2 217 70 98

AVENUE DES ARTS 3 – 5 B-1210 BRUSSELS FAX + 32 2 219 85 14 E-mail : -

SAG NL 75/02/E – Page 2 commonly in small bore impulse lines. Delay will run the risk of erosion due to perlite swirl or pooling of liquid with subsequent expansion due to heating. such reference to or use of EIGA’s publications by its members or third parties are purely voluntary and not binding. performance or non performance. will assist in trouble-shooting and control of any incident. Regular logging of interspace purge parameters. Preventive measures Both design and safe operating practices contribute to the prevention of the abovementioned risks. While EIGA recommends reference to or use of its publications by its .eiga. During and after cool-down. Thermal stress relief design of cold box piping and components. Therefore. 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. 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. Proper risk assessments should be performed and contingency plans laid. flows. A healthy purge gas flow of nitrogen will keep the perlite dry and will provide early assistance in evaporating liquid pools. or simply the ingress of air itself to the interspace. the following factors should be considered during the lifetime of a cold box: • The existence of an active interspace purge at all times should be confirmed by the logging of purge gas flow. 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. including Codes of practice. EIGA or its members make no guarantee of the results and assume no liability or responsibility in connection with the reference to or use of information or suggestions contained in EIGA’s publications. EUROPEAN INDUSTRIAL GASES ASSOCIATION PHONE +32 2 217 70 98 AVENUE DES ARTS 3 – 5 B-1210 BRUSSELS FAX + 32 2 219 85 14 E-mail : info@eiga. 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. Relief systems The importance of relief systems in mitigating a cold box over-pressure incident is high. as the presence of oxygen in any proportion will probably indicate leakage. • • • • All technical publications of EIGA or under EIGA’s name. This is prevalent at the upper parts of the cold box. EIGA’s publications are subject to periodic review and users are cautioned to obtain the latest edition. the checking and maintenance of cold box purge arrangements will help to reduce the impact of a leak into the interspace. usually on the argon system but can occur at any location. Oxygen may also.www. . It will also be of value to record the constituents of the gas purge at the top of the ASU cold box. and time/temperature charts at various critical process points. the cold box should be monitored for signs of leaks as thermal contraction is maximum at this point. Over-pressure incidents typically occur during plant thawing in preparation for maintenance. in the absence of flow. Summary In summary. EIGA has no control whatsoever as regards. preferably flow and pressure. Plants should be shut down as soon as possible after an interspace leak is diagnosed. Documented plant defrosting plans are recommended and should define valves status. indicate condensing atmospheric air. Purge More importantly.

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