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Apparatus for Water Detection Using a Radioactive Tritium Labelled Reactant

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Apparatus for Water Detection Using a Radioactive Tritium Labelled Reactant United States Patent [is] 3,655,982 Gelezunas [45] Apr. II, 1972 [54] APPARATUS FOR WATER DETECTION OTHER PUBLICATIONS USING A RADIOACTIVE TRITIUM Holtman et al., " Radiometric Determination of Moisture in •Gases," Radioisotope Tracers in Industry and Geophysics, LABELLED REACTANT Symposium Proceedings Prague 1966, International Atomic [72] Inventor: Vincent L. Gelezunas, Devon, Pa. Agency, Vienna 1967, pp. 261-270. Thompson, R. C., Nucleonics, " Biological Applications of [73] Assignee: General Electric Company Tritium," Vol. 12,No. 9, Sept. 1954, pp. 31-35. [22] Filed: Jan. 29,1969 Primary Examiner—James W. Lawrence [21] Appl.No.: 795,111 Assistant Examiner—Davis L. Willis Attorney—William G. Becker, Paul F. Prestia, Allen E. Am- gott, Henry W. Kaufmann, Frank L. Neuhauser and Oscar B. [52] U.S. CI 250/106 T, 23/255 E, 250/43.5 MR, Waddell 250/83.6 FT [51] Int.Cl G21h 5/02 [57] ABSTRACT [58] Field of Search 250/106 T, 83.6 FT, 43.5 R; 23/232 C, 232 E, 255 E A method and apparatus for detecting water using an ap- propriate radioactive labelled alkaline earth hydride as a reac- tant. Fluid from a gas liquid or solid sample to be tested is [56] References Cited passed through a bed of the reactant. The water present in the UNITED STATES PATENTS sample reacts with the reactant forming a radioactive product whose radioactivity is then measured to give a quantitative 3,118,735 1/1964 Favreetal 23/230 determination of the amount of water in the sample or a qualitative determination of the presence of water. 3 Claims, 3 Drawing Figures Patented April 11, 1972 3,655,982 f—iq.Z. INVENTOR: Vincent L. Gelezunas, by ' A. AGENT 3,655,984 1 2 APPARATUS FOR WATER DETECTION USING A radioactivity ofthe end products. Means 17 are also provided RADIOACTIVE TRITIUM LABELLED REACTANT for determining the parameters of the gas flow through the DAPirromixmthe ixiurMnnv radioactivity detector which are used to determine the water BACKUKUUNDUt THt, llSVLN HON concentration in the input sample. For qualitative analysis, de- The subject invention relates to the field of fluid detection ^ tection of any radioactivity above background in the reaction and, in particular, to methods and apparatus for detecting the products indicates the presence of water in the sample, concentration or presence of water. The reactant is a radioactive labelled-alkaline earth hydride There are many different methods of detecting water con- from the group consisting of calcium hydride, strontium centration including IR and mass spectrometers, alumina ,n hydride, and barium hydride. Radioactive labelling may be ac- hygrometer, electrolysis, and gas chromatography. However, complished by a simple exchange reaction as follows. Hydride all of these are quite limited in sensitivity, with the best having powder is exposed to a mixture of tritium and hydrogen gas in a sensitivity limit of about 10"8 micrograms per liter. Also, the a closed system at about 350° C. for approximately 48 hours, instruments used in these methods are generally quite com- The specific activity of the final product depends on the quan- plicated and have limited thermal and shock resistance. Water 15 tity and the ratio of tritium to hydrogen in the initial gas mix- detectors using radioactive labelled calcium carbide and bari- ture. In the preferred embodiment, tritium labelled calcium um carbide as reactants have been tried, but are limited for hydride is used because it is inexpensive and readily (commer- many purposes in terms of their sensitivity, selectivity and cially) available in a chemically pure form. The primary reac- ability to provide consistent results as the reactant is being tions of calcium tritide with water are as follows: 3 3 depleted. Heretofore water detection systems free of the 20 CaH2 + 2 H2'0 - Ca(Oh')2 + 2 H'H (d 3 1 3 foregoing limitations have been unknown. CaH2 + H2'0 — CaO + 2H H <2) From these reactions it can be seen that the products of the SUMMARY OF THE INVENTION reactions are calcium hydroxide, calcium oxide and molecules accordingly, it is an object of the subject invention to pro- ^IV* °fhydr°f"' ™e„reactions of calcium hydride vide a highly sensitive water detection means. 25 (without tntium) are substanti^y the same as reactions (1) a d f Another object of the subject invention is to provide a " ^)° the above except that H2« is formed instead of HH he h ro 11 m oiecu,es fr01 the cac u tn lde n d highly selective method and apparatus for water detection. i ' J ^ f t " „ ' T ' * , Still another object of the subject invention is to provide a the reaction product mixture may contain H, , H>3 and H 'H» water detector which is quite simple in operation and which . .S»ce specific activity of the reactent mixture which is has a high tolerance for mechanical shock 30 indicative of the concentration of radioactive trit.de in the ture 18 known A further object of the subject invention is to provide a ™* ' the Reactivity detected gives a qUan- method and apparatus for detecting water of a sample over a titative measurement of the amount of tritium (H ) m the wide concentration range. product gas, the amount of water m the input sample can be The subject invention satisfies the above-stated objects by determined. .... .. ... .. 35 D nn rat the sub e 1 providing a chemical/radiological water detector and water " 8 °Pf i°"f u J f. mention, either or both detection process. A fluid sample is passed through a reactant tactions < ). and (2) or a hydration reaction of the calcium bed containing a suitable radioactive labelled alkaline earth °xlde or ca>"um hydroxide may occur. General y, die higher hydride reactant. The radioactivity of the gaseous reaction ]he temperature of the reaction, the greater the tendency will products is then measured by a suitable device. The amount of 40 be for reaction (2) to take place m preference to reaction (1) radioactive material in the gaseous products and hence the 40 and the lesser the tendency will be for a hydration reaction to amount of radioactivity detected is proportional to the water take Place' duej° the reactlon ,raes and equilibrium concentration of the input sample. In the preferred embodi- c?nstants reactions reactions (1) and (2) will take ment the reactant used is tritium labelled calcium hydride. Place >?uch more readily and rapidly than the hydration reac- One or more parallel reaction beds may be provided to allow 45 tl0n/' 11 « desu-able for reactions (1) and {2 to occur in the detector to operate over two or more ranges. ° preference tothe hydration reactions because the hydration The subject matter which is regarded as the present inven- ^^l^0 Pfven* ™ater ln the samP,e fr°"} refctlnS tion is particularly pointed out Mid distinctly claimed in the wlth the hydnde t0 hydrogen gas which would lead to an concluding portion ofthe specification. erroneous determination ofthe water concentration. FIG. 2 shows an embodiment of the subject invention for BRIEF DESCRIPTION OF THE DRAWINGS use with a gas sample. The sample is ducted by pipe 13 to , reaction bed 14 of radioactive labelled calcium hydride. The The present invention, however, both as to organization and sample gas and reaction bed 14 are preferably heated to a method of operation, together with further objects and ad- predetermined temperature by any appropriate heating means vantages thereof, may best be understood by reference to the such ^ resistance heater 20 which is connected to a power description taken in connection with the accompanying source 22, as shown in FIG. 2. The product of the reaction in drawings in which: . , bed 14 is gaseous hydrogen, including the radioactive FIG. 1 is a block diagram of the process of the subject in- hydrogen isotope tritium (H3), which is piped via a tube 15 to vent'on; ... , detector chamber 24. Radioactivity detector 16 is used in con- FIG. 2 is a schematic view of one embodiment of the ap- 6Q junction with detector chamber 24 to provide a quantitative paratus ofthe subject invention; and r indication of the amount of radioactive material, i.e., tritium, FIG. 3 is a schematic view of the preferred embodiment of in ^ gaseous reaction products or a qualitative indication of the subject invention. the presence of radioactive material. DESCRIPTION OF THE PREFERRED EMBODIMENTS _ ^ny type of radioactivity detector sensitive to the type of 65 radiation emitted by tritium (beta particle) may be used for a FIG. 1 shows in block diagram form the steps of the basic stationary setup; this may conveniently be an ionization water detection process of the subject invention. Briefly, the chamber. However, for more mobile operation, a compact fluid sample 12 containing the fluid whose water concentra- radiation detector such as an avalanche semiconductor radia- tion is to be determined is ducted to a reaction bed 14 contain- tion detector 16, as shown in FIG. 2, may be used, ing a suitable radioactive labelled reactant in substantial 70 If a continuous sample is to be taken, an open-ended detec- stoichiometric excess to allow a reaction to take place. A tor chamber, such as that shown in FIG. 2, is used; and for a radioactivity detector 16 then measures the amount of sample, of a discrete volume a detector chamber closed at one radioactive material produced by the reaction is proportional end is used. In either case, in order for the water concentra- to the amount of water in the input sample, the water concen- tion to be determined, the volume of the detector chamber, tration in the sample is determined as a function of the 75 the pressure and temperature of the gases therein, the specific 3,655,982 activity of the calcium hydride in the reaction bed and the valves 26,28,30,32 in pipes 13,13' and tubes 15,15' respec- radioactivity of the gases within the detector chamber (as in- tively.
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