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Vapor Pressures of Hydrogen, Deuterium, and Hydrogen Deuteride and Dew-Point Pressures of Their Mixtures

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Vapor Pressures of Hydrogen, Deuterium, and Hydrogen Deuteride and Dew-Point Pressures of Their Mixtures ------------------- ~~ --------~------------ Journal of Research of the National Bu reau of Standards Vol. 47, No. 2, August 1951 Resea rch Paper 2228 Vapor Pressures of Hydrogen, Deuterium, and Hydrogen Deuteride and Dew-Point Pressures of Their Mixtures 1 Harold J. Roge 2 and Robert D. Arnold The vapor pressures of H 2 , ED, and D2 have been measured from near their t riple poin ts to their critical points. The H 2 and D2 samples were catalyzed to or tho-para equilibrium at 20.4 0 K. Tables suitable for in terpolation have been prepared to r epr esen t the r esults both in centimeter-gram-second and in engin eering units. MeasUl"ements of dew-point pressures of severa l binary mixtures have been made at several pressures below atmospheric. Observed pressures were about 3 percent above those predicted by the law of ideal solutions. <t 1. Introduction e-H2 [6]. Likewisc, deuterium catalyzed to eq uilib­ rium at 20.4° Ie (0.022 para-Dz, 0.978 ortho-D2) is :Many papers dealiJlg with the vapor pressures of designaLe d e-D 2• It is worth while Lo emphasize various isotopic varieLies of hydrogen have appeared that e-H2 and e-D2 were in ortho-para equilibrium since Dennison [1] 3 co rrectly explained the behavior only at 20.4 0 Ie, and that the composition did not of ortho and para forms in 1\:)27, and since Urey, change as the temperaLure was raised or lowered Brickwedcle , ancl .Murphy [2] announced the con­ during the course of lhe rneasurements. It had centration of deuterium in 1932. So far as we are been hopedlo measure the vapor pressure of llormal, aware, hO\-'lever, no meaSlll'ements extending above or high-temperatme-equili brium hydrogen (0.25 para­ the range of ordinary mercury manometry had H 2, 0.75 ortho-H2) and deuterium (0.3333 para-D2' been reported until quite r ecently, when White, 0.6667 ortho-Dz), bu t time did not permit. There Friedman, and Jolmston [3] published data for nor­ are no separale ortho and para varieties of HD. mal hydrogen extending up to the critical point, and a preliminary report of the present work 2. Vapor-Pressure Measurements appeared [4]. Grilly [5] has measured the vapor pressures of the normal varieties of hydrogen, deu­ 2.1. Apparatus and Methods terium, and tritium up to approximately 3 atm. Vapor pressures of mixtures had bern neglected, The apparatus and methods werc substantially the there being no information on deviations from the same as those recently used to measure the vapor laws of ideal solutions other than that pu blished by pressure of oxygen and are describcd in reference [8]. Woolley, Scott, and B rickwedde [6, p. 454] for mix­ The diaphragm cell used for pa,rt of the work on tures of ortho and para hydrogen. oxygen was not employed. The present paper, and one on eritical co nstants After part of the present work was completed, it [7], being published simultaneollsly, comprise a full was noted that the floating nickel sleeves and mag­ report of a program of determination of Lhe proper­ netic detectors were not indi.cating eorrectly the ties of the hydrogens undertaken at Lhe Bureau difference in height of the two mcrcury meniscuses early in 1950. The work reported in this paper con­ inside the stainless steel U-tube. This was verified sisted of two parts: the measurement of vapor pres­ by taking X -ray pi ctures of the meniseuses. The ni ckel sleeve at the Hg-H 20 interface (height h2 ) was sures of H 2, HD, and D2 from low pressures to their critical points; and the measurement of the dew found to be functioning properly, supported entirely points of a number of binary mixtures of the same above the mercury by the surface tension of the substances at pressures below 1 atm. The vapor­ latter. The sleeve at the Hg-H2 interface (height h\), pressure meaSLU"ements and the dew-point meaS LU"e­ however, had been wetted by the mercury and had ments were performed with difre rent apparatuses, sunk into it. Measurements afrected by this dif­ and are discussed separately, the vapor-pressure fieul ty were calcul ated from the value of h2 only, by h d h2 ~ measurements being presented in section 2 and the using a curve of versus plotted from data dew-point measurements in section 3. Except for a taken before the Lrouble developed. There was a few preliminary measurements, all the vapor pres­ considerable range of overlap of the piston-gage sures reported for H2 and D2 are for samples catalyzed measurements with the mercury manometer and the to ortho-para equilibrium at the boiling point of mercury manometer-barometer measurements, in normal hydrogen (20.4° K ). Hydrogen so catalyzed which the various methods were cross-checked from time to time. (0.979 para-H2, 0.021 ortho-H ) has been designated z The resistance thermometer (L14) that developed a leak during the O measurements was removed and 1 This research was supported in part by the Atomic Energy Commission. 2 , Present address, Leeds & Northrnp Co., Philadelphia, Pa. replaced by Lll and L28. With the exception of a J Figures in brackets indicate the Iitcrature references at the end of this paper. few check measurements, all the temperatures in the 63 ",I ~ I ,.---.--,.----,--,.--,13000 1-------,/--11200 0 u / 11000 10000 'l E 800 E 9 000 l" 600 ~ -----18000 ~<::J /<:i l" "- co . I FIGURE 1. A comparison 400 7 000 E of the vapor pressures of E ordinaTY hydrogen, hydro­ n - T2 200 gen de1lteride, deuterium, 6000 ~ and tritium. 0 5000 Cl) 12 13 15 16 21 22 23 24 25 0: "' T oK -------1 4 000 3000 I • Critical point o Triple point I( 2000 rooo 4 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 4 0 TOK present work were measured with platinum resistance Mass Spectrometry Section of the Bureau for thermometer Lll. This thermometer is one of the analysis. The results are presented in connection original group used to define the Bureau's tempera­ with the discussion of the measurements on each ture scale below 90 0 K . Its calibration is discussed particular substance. in [9]. One improvement was made over the methods 2.2. Ortho-para Catalysis used in the oxygen measurements. Rather than The catalyst was N d20 3 furnished by the Bureau's make alternate measurements of pressure and of Inorganic Chemistry Section. It was a pale blue thermometer resistance, it was found more accurate powder prepared by firing neodymium oxalate at and more convenient to observe the resistance ther­ 800 0 C. To avoid contaminating the Hz with D 2, mometer continuously, keeping the piston gage the catalyst used for D2 was removed and replaced balanced until conditions had been steady for several by a fresh sample before measurements on H 2 were minutes.' A valve in the pressure-transmitting line begun. Each sample was contained in a cylindrical was then closed after which all the readings asso­ glass chamber of about 1.6-cm inside diameter and ciated with the l;ressure measurement could be made 15-cm3 volume. Connections were made by two at leisure. glass t ubes, one ending at the top and the other near The method of computing pressures was the same the bottom of the chamber. About 10 cm3 of as that used for O2 except that no correction was catalyst was placed in each chamber and confined made for the hydrostatic pressure of hydrogen vapor. with plugs of glass wool. The catalyst was prepared The maximum correction (at the critical point) in for use by evacuating for several hours near 440 0 the case of O2 was 6.5 mm Hg. It was estimated C, and flushing with small portions of the H 2 (o~' D.2) that the corresponding figure for D2 would be about to be measured. It was surrounded by hqUld 1 mm Hg, with the values for HD and H 2 propor­ hydrogen before use, after which the entire sample tionately less. of H 2 or D 2 to be measured was condensed on it. Preparation and purity of th e samples. The H2 A toepler pump was used to circulate the gas so that was taken from the supply generated by electrolysis all the material would come in contact with the of H 20 for use in this laboratory's hydrogen liquefier. catalyst. When gas was transferre.d from the cat­ The HD was prepared for us by Abraham Fookson, alyzing chamber to the cryostat, It was removed Philip Pomerantz, and Edwin H . Rich, who used tlu·ouo·h the tube extending to the bottom of the the reaction chamber, so that only material that had be~n in I close contact with the catalyst would be obtall1ed. During the catalytic conversi~n , sam:rles were co~­ ~ densed in the cryostat from tIme to tIme and theIr The D2 was obtained from the Stuart Oxygen Co. vapor pressures were observed; they were then re­ Both the HD and the D2 were purified by distillation circulated until no further change in vapor pressure by Fookson, et al. A more complete report of their was observed. The time required to reach ortho­ work is published elsewhere [10]. para equilibrium in the presence of the catalys~ at A number of samples taken at various stages of the 20.4 0 K appeared to be short compared to the tIme vapor-pressure measurements were submitted to the required to introduce and remove the sample.
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