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By Eric W. Spencer Cryogenics may be defined as low temperature technology, or the science of ultralow temperatures. To distinguish between cryogenics and refrigeration, a commonly used measure is to consider any temperature lower than - 73.3°C (- 1OO°F) as cryogenic. Although there is some controversy about this distinction, and some who insist that only those areas within a few degrees of absolute zero may be considered as cryogenic, the broader definition will be used here. Low temperatures in the cryogenic area are primarily achieved by the liquefaction of gases, and there are more than twenty-five which are currently in use in the cryogenic area; i.e., gases which have a boiling point below -73.3°C (- 1OO°F). However, the, seven gases which account for the greatest volume of use and applications in research and industry are helium, hydrogen, nitrogen, fluorine, argon, oxygen, and methane (natural gas). Cryogenics is being applied to a wide variety of research areas, a few of which are: food processing and refrigeration, rocket propulsion fuels, spacecraft life support systems, space simulation, microbiology, medicine, surgery, electronics, data processing, and metalworking.
TABLE I- Properties of Cryogenic Fluids.
Gas Helium-3 Helium-4 Hydrogen Deuterium Tritium Neon Nitrogen Carbon monoxide Fluorine Argon Oxygen Boiling Boiling Volume Point Point Expansion Flammable Centigrade Kelvin to Gas -269.9 -268.9 -252.7 -249.5 -248.0 -245.9 -195.8 -192.0 -187.0 -185.7 -183.0 3.2 4.2 20.4 23.6 25.1 27.2 77.3 81.1 86.0 87.4 90.1 757 to 1 757 to 1 851 to 1 ... ... 1438 to 1 696 to 1 ... 888 to 1 847 to 1 860 to 1 No No Yes Yes Yes No No Yes No No No Toxic No(a) No(a) No(a) Odor No No No
Radioactive No Radioactive No No(a) No(a) Yes Yes No(a) No(a) No No No Sharp No No
.7 183.1 190.3 -89.1 -103.. As with most chemicals. from approximately 553 to 1 for carbon dioxide. Table I contains a more complete summary of the properties of cryogenic fluids.4 -151.1-Difluoroethylene Carbon dioxide -161.5 -88.. However.0 -83... . . and personnel. HAZARDS There are four principal areas of hazard related to the use of cryogenic fluids or in cryogenic systems.. -459. 553 to 1 Yes No No Yes No Yes No No Yes No Yes No Yes No No No(a) No(a) Yes Yes No(a) No(a) Yes No(a) No(a) Yes Yes No(a) No(a) Yes Yes(a) No No No Yes No Sweet Pungent Sweet No Pungent Garlic No Ether Mild Pungent Chlorotrifluoromethane -81.. ..8 -100..0 169. Cryogenic fluids (liquefied gases) are characterized by extreme low temperatures.3 172. and may even cause some . (b) Sublimes.6 184. These are: flammability.0 191..3 145 161. The flammability hazard is obvious when gases such as hydrogen.5°C (-109°F) for carbon dioxide to -269.0 -78 5(b) 111......1 189..0 189. the fire hazard may be greatly increased when gases normally thought to be non-flammable are used. 666 to 1 ..4 0°K = -273.8 -128 -111..9 -109. All categories of hazard are usually present in a system concurrently... but can act as an asphyxiant by displacing air needed to support life. even harmless materials can be toxic or poisonous if taken in sufficient quantities under the right circumstances. The presence of oxygen will greatly increase the flammability of ordinary combustibles. ranging from a boiling point of -78.7 121. Another common property is the large ratio of expansion in volume from liquid to gas.3 164. materials.Methane Krypton Tetrafluoromethane Ozone Xenon Ethylene Boron trifluoride Nitrous oxide Ethane Hydrogen chloride Acetylene Fluoroform 1.69°F.6 578 to 1 700 to 1 .16°C..3 -85. 573 to 1 . .0 -84. and acetylene are considered.6 194. high pressure gas. and must be considered when introducing a cryogenic system or process.0 -84. .8 188. to 1438 to 1 for neon. .9°C (-454°F) for helium. (a) Nontoxic. methane.
Liquefied inert gases such as liquid nitrogen or liquid helium are capable. high pressure gas. The eyes are especially vulnerable to this type of exposure. Section VIII Unfired Pressure Vessels may be used as a specific guide to the selection of materials to be used in cryogenic service. While a number of the gases in the cryogenic range are not toxic. monel. Extremely cold metal surfaces are also capable of condensing oxygen from the atmosphere. The rate of evaporation will vary. bronze. Wood or asphalt saturated with oxygen has been known to literally explode when subjected to mechanical shock. container design. experimental evaluation should be performed before the materials are used in the system. When properties of materials which are being considered for cryogenic uses are unknown. and causing oxygen enrichment or entrapment in unsuspected areas. copper. brazing. so that eye protection is necessary. Mylar.noncombustible materials like carbon steel to burn readily under the right conditions. These same factors must also be considered in the design of transfer lines and piping systems. Prolonged contact with these temperatures will cause embrittlement of the exposed members because of the high water content of the human body. depending on the characteristics of the fluid. The large expansion ratio from liquid to gas provides a source for the build-up of high pressures due to the evaporation of the liquid. The American Society of Mechanical Engineers' Boiler and Pressure Vessel Code. Personnel hazards exist in several areas where cryogenic systems are in use. or not to be found in the known guides. Once the materials are selected. and Nylon. brass. there is always some gas present in the container. Teflon. Some metals which are suitable for cryogenic temperatures are stainless steel (300 series and other austenitic series). Kel-F. Finally. and environmental conditions of the atmosphere. they are all capable of causing asphyxiation by displacing the air necessary for the support of life. chemical reactivity between the fluid or gas and the storage containers and equipment must be studied. A very brief contact with fluids or materials at cryogenic temperatures is capable of causing burns similar to thermal burns from high temperature contacts. Of prime concern is bodily contact with the extreme low temperatures involved. of condensing oxygen from the atmosphere. the method of joining them must receive careful consideration to insure that the desired performance is preserved by using the proper soldering. or welding techniques and materials. The high pressure gas hazard is always present when cryogenic fluids are used or stored. Materials must be carefully selected for cryogenic service because of the drastic changes in the properties of materials when they are exposed to extreme low temperatures. Even oxygen . Since the liquefied gases are usually stored at or near their boiling point. under the right conditions. insulating materials. Non-metal materials which perform satisfactorily in low temperature service are Dacron. and aluminum. Container capacity must include an allowance for that portion which will be in the gaseous state. and material failures previously discussed must be avoided. while other materials may improve their properties of ductility. Materials which are normally ductile at atmospheric temperatures may become extremely brittle when subjected to temperatures in the cryogenic range. Exposure of personnel to the hazards of fire. asbestos impregnated with Teflon.
and high-topped shoes should be worn. rooms. bracelets. There is no fine line of distinction between the four categories of hazards. Work areas. personnel should avoid wearing anything capable of trapping or holding a cryogenic fluid in close proximity to the flesh. rings. GENERAL PRECAUTIONS Personnel should be thoroughly instructed and trained in the nature of the hazards and the proper steps to avoid them. A more desirable arrangement would be hand protection of the potholder type. an impervious apron or coat. it would be advisable to provide for the cryogenic system or equipment to be shut down automatically as well as to sound a warning alarm. When toxic gases are being used. and sufficiently large to be easily tossed off the hand in case of a spill. or the contamination of an oxidant by a fuel. when flammable gases are being used. When there is a possibility of personal contact with a cryogenic fluid. or laboratories should be suitably monitored to automatically warn personnel when a dangerous condition is developing. extreme care should be taken to avoid contamination of a fuel with an oxidant. they should be impervious. When practical. full face protection. As further prevention. and personal protective equipment required. potential ignition sources must be carefully controlled. This should include emergency procedures. or other jewelry should not be permitted when personnel are working with cryogenic fluids. This is particularly important when working with liquid or gaseous oxygen. cuffless trousers. Equipment and systems should be kept scrupulously clean and contaminating materials avoided which may create a hazardous condition upon contact with the cryogenic fluids or gases used in the system. safety devices. As the primary defense against fire or explosion. operation of equipment. Watches. suitable respiratory protective equipment should be readily available to all personnel. chambers. They should thoroughly know the location and use of this equipment. knowledge of the properties of the materials used. Gloves may or may not be worn. and they must be considered collectively and individually in the design and operation of cryogenic systems. Mixtures of gases or fluids should be strictly controlled to prevent the formation of flammable or explosive mixtures.may have harmful physiological effects if prolonged breathing of pure oxygen takes place. but if they are necessary in order to handle containers or cold metal parts of the system. Basically. STORAGE .
and a manual valve to relieve pressure before removing the device. Generally. .6 to 26 gallons). Cryogenic fluids with boiling point below that of liquid nitrogen (particularly liquid helium and hydrogen) require specially constructed and insulated containers to prevent rapid loss of product from evaporation. the containers are usually cylindrical with dished ends. and the outer vessel contains liquid nitrogen which acts as a heat shield to prevent heat from radiating into the inner vessel. and usually have a capacity of 10 to 100 liters (2. and to prevent an ice plug from forming in the neck.Storage of cryogenic fluids is usually in a well insulated container designed to minimize loss of product due to boil-off. The glass container is similar in construction and appearance to the ordinary Thermos bottle. and adequately vented to permit the escape of evaporated gas. The inner neck as shown in the illustration. The most common container for cryogenic fluids is a double-walled. one inside the other. Both the metal and glass Dewars should be kept covered with a loose-fitting cap to prevent air or moisture from entering the container. Exposed glass porions of the container should be taped to minimize the flying glass hazard if the container should break or implode.) long near the center of the tubing.54 cm ( I in. there is an automatic pressure relief valve. of either metal or glass. These are special Dewar containers which are actually two containers. but the evacuated space is generally filled with powdered or layered insulating material. and to allow built-up pressure to escape. should be kept closed with a loose fitting. Dewar vessels of this type must be strictly and regularly maintained to prevent the loss of product. evacuated container known as a Dewar flask. These containers arc also of double-walled evacuated construction. the lower portion will have a metal base which serves as a stand. Metal containers are generally used for larger quantities of cryogenic fluids. Containers must bc constructed to withstand the weights and pressures that will be encountered. 1). which approximates the shape of the sphere but is less expensive to build. Also. Piping or transfer lines should be doublewalled evacuated pipes to prevent the loss of product during transfer. yet is loose enough to vent any pressure which may have developed (Fig. Larger capacity storage vessels are basically the same double-walled containers. This prevents the entry of air and moisture. non-threaded brass plug which prevents air or moisture from entering the container. The inner container is usually spherical in shape because this has been found to be the most efficient in use. Most suppliers are now using a special fitting to be used in the shipment of Dewar vessels. For economic reasons. The liquid nitrogen fill and vent lines should be connected by a length of gum rubber tubing with a slit approximately 2. The liquid helium or hydrogen is contained in the inner vessel. and usually contain some adsorbent material in the evacuated space. while the slit will permit release of gas pressure. Containers should also bc equipped with rupture discs on both inner and outer vessels to release pressure if the safety relief valves should fail.
toxic or inert gas in the work area. Chicago. Chicago. "Industrial Gas Data. If it is not possible to empty all lines. New York.. East Rutherford." Conference on Special Risk Underwriters'. Transfer of liquids from the metal Dewar vessels should be accomplished with special transfer tubes or pumps designed for the particular application. ACKNOWLEDGEMENT: Reprinted from the Journal of the American Society of Safety Engineers. 11 (8). Massachusetts.. M. 15-19. The cap must be kept on at all times to prevent entry of moisture and air. tilting to pour the liquid may damage the container. An Introduction to Low Temperature Physics. Jackson. and Kuni. Braidech." Linde Company. (1960) "Precautions and Safe Practices for Handling Liquefied Atmospheric Gases. "Precautions and Safe Practices for Handling Liquid Hydrogen. Evaporation of the liquid in a section of line may result in pressure build-up and eventual explosion. (1960)." Anchor Books.. Some newer style Dewar vessels are equipped with a pressure relief valve. 111. "Matheson Gas Data Book. D. New Jersey.. Hoare. . Reaming should be performed with a hollow copper rod. Piping or transfer lines should be so constructed that it is not possible for fluids.to become trapped between valves or closed sections of the line. "Near Zero. New York." Linde Company. (1962)... and at least twice daily. London. Illinois. (1960). and pressure gauge for the inner vessel. they must be equipped with safety relief valves and rupture discs. shortening its life. The Matheson Co. (1961). which will form an ice plug. with a marker or stop to prevent damaging the bottom of the inner container. Doubleday & Co." 47th edition. Inc. New York." Linde Company." Marsh & McLennan. Since the inner vessel is mainly supported by the neck. Inc. MacDonald. August." Air Reduction Sales Co. or creating a hazard due to container failure at a later date. Neary. C. "Handling Cryogenic Fluids. New York." Butterworths. "Hazards/Safety Considerations in Cryogenic (Super Cold) Operations.. K. "Experimental Cryophysics... 1963. R. (1961). proper consideration must be given to the properties of the gas being vented. (1961). New York. Vol. Acton.The liquid nitrogen outer jacket should be kept filled to maintain its effectiveness as a radiant heat shield. Venting should be to the outdoors to prevent an accumulation of flammable. REFERENCES "Cryogenics. The liquid helium fill (inner neck) should be reamed out before and after transfer. (1961). Inc. Mathew M. When venting storage containers and lines.
New Jersey. M." A Summary Report of the Cryogenic Safety Conference. R. (1959). Zenner." in Advances in Cryogenic Engineering. (1962). . W. (1959). editor "Advances in Cryogenic Engineering. Pennsylvania.Scott. K. Van Nostrand Company. Inc. Princeton. H. and Dulce. Allentown. New York. Russeil B. "Safety Engineering as Applied to the Handling of Liquefied Atmospheric Gases.. G. Applied Cryogenic Engineering. D.. "Cryogenic Engineering. Plenum Press. Vance.." John Wiley h Sons. "Cryogenic Safety." D. Timmerhaus.. (1961)." 7. W. Plenum Press. New York. Incorporated. (1960). Air Products.. Inc" New York. Editors. 6..
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