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Heat Capacities and Thermodynamic Properties of Ammonium and Potassium Thiocyanates from 5 to 340 K T

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Heat Capacities and Thermodynamic Properties of Ammonium and Potassium Thiocyanates from 5 to 340 K T J. Chem. Thermodynamics 1970, 2,417429 Heat capacities and thermodynamic properties of ammonium and potassium thiocyanates from 5 to 340 K t CECIL E. VANDERZEE Department of Chemistry, University of Nebraska, Lincoln, Nebraska 68508, U.S.A. and EDGAR F. WESTRUM, Jr. Department of Chemistry, University of Michigan, Ann Arbor, Michigan 48104, U.S.A. (Received 12 December 1969) The heat capacities of ammonium and potassium thiocyanates were determined by adiabatic calorimetry over the range 5 to 340 K, and associated thermodynamic functions were computed from the results. At 298.15 K, the heat capacities C&al K- ’ mol-1 and entropies S”/cal K-l mol-1 are 29.98 and 33.52 for NH&CN and 21.16 and 29.70 for KSCN. In both salts, the heat capacity contribution from libration of the thiocyanate ions may be represented by two Einstein functions up to 250 K. The torsional motion of the ammonium ion increases rapidly above 100 K and contributes more than 6 cal K-l to the heat capacity above 250 K. Adjuvant data on potassium thiocyanate solutions lead to S” = (34.23+0.3) cal K-’ mol-’ for SCN-(aq) at 298.15 K. 1. Introduction Ammonium halide crystals exhibit transitions in the solid state below 300 K which are related to the orientation and motion of the ammonium ion. It was of interest to examine the heat capacity of ammonium thiocyanate crystals to establish whether similar behavior occurred for ammonium ions in an environment of rod- or pear- shaped anions. Such studies were also made on potassium thiocyanate for comparison of lattice and internal contributions from the thiocyanate ion. A further purpose of this study was to determine the thermodynamic functions for these salts and the entropy of the aqueous thiocyanate ion, as a check on the entropies of SCN-(aq) and HNCS(g) based on studies by Brandenburg.‘” 2. Experimental CALORIMETRIC PROCEDURES Measurements were made by adiabatic calorimetry at temperatures between 5 and 330 K for ammonium thiocyanate and between 5 and 350 K for potassium thiocyanate, using the Mark II cryostat described elsewhere. (‘) The automatic adiabatic shield t This work was supported in part by the Division of Research of the U.S. Atomic Energy Commission. 418 C. E. VANDERZEE AND E. F. WESTRUM, JR. control system has also been described previously. (‘) The gold-plated copper calori- meter used in this study (laboratory designation W-42) has a capacity of 93 cm3 and has horizontal radial vanes for thermal equilibration within the sample. The calori- metric sample of ammonium thiocyanate had a mass of 66.0128 g. and its heat capa- city ranged from 91.41 per cent of the total at 16.48 K to 79 per cent at 103 K and increased to 84 per cent at 330 K. Buoyancy corrections were based on a density of 1.31 g cmF3. Helium at a pressure of 63 Torr at 300 K was used to facilitate equili- brium in the calorimeter. The calorimetric sample of potassium thiocyanate had a mass of 74.446 g, based on a density of 1.886 g cm -’ for buoyancy corrections. It was enclosed with helium gas at a pressure of 75 Torr at 300 K, and its heat capacity ranged from 82 per cent of the total at 10 K to 75 per cent at 168 K and increased gradually to 78 per cent at 350 K. A capsule-type strain-free platinum thermometer (laboratory designation A-5) located within the. entrant well of the calorimeter was used for temperature measurements. All measurements of mass, temperature, resist- ance, potential, and time are referred to standardizations and calibrations performed at the National Bureau of Standards. PREPARATION AND CHARACTERIZATION OF SAMPLES Reagent grade ammonium thiocyanate (Baker Analyzed, Lot. No. 34157) was recrystallized once from 50 per cent aqueous methanol and twice from methanol. The solutions were brought to saturation at about 80 “C, then cooled to between 0 and 5 “C. The crystals were recovered in a sintered glass funnel, rinsed with cold methanol, and dried under vacuum over potassium hydroxide pellets. After a preliminary drying, the crystals were broken to uniform size in an agate mortar, dried at 60 “C for two hours, then held in a vacuum desiccator over potassium hydroxide pellets under high vacuum for ten days. The material was loaded into the calorimeter under conditions of about 48 per cent relative humidity, at which the material is not appreciably hygro- scopic. Subsequent evacuation of the calorimeter and flushing with helium was expec- ted to eliminate any traces of water absorbed from the atmosphere during loading. Examination of the heat capacity behavior of the sample near the freezing temperature of methanol indicated 0.05 mass per cent methanol entrapped in the crystals, as calcu- lated from the excess energy absorption (1.2 cal mol- ‘) in Series I (table 1) by attribu- ting the excess to melting of the CH,OH+ NH,SCN eutectic at about 167 K. The excess heat capacity and entropy from this source would be negligible below 160 K, and were estimated at 0.01 cal K- ’ mol- ’ from 170 to 273 K, rising to 0.02 cal K- ’ mol-’ at 330 K. The estimated excess enthalpy would range from 1.2 cal mol-l at 170 K to 2.4 cal mol-’ at 273 K and to 3 cal mol- ’ at 330 K. No adjustment for this effect was made in the tabulated results (tables 1 and 2). Reagent grade potassium thiocyanate (Baker Analyzed) was recrystallized three times from methanol. The crystals were collected on a sintered-glass filter, rinsed with cold methanol, and given a preliminary drying under vacuum over potassium hydroxide pellets. The crystals were then broken to uniform size in an agate mortar, and dried six hours at 90 to 110 “C. They were subsequently stored under vacuum over potassium hydroxide pellets. Calorimeter loading conditions and procedures were the same as THERMODYNAMICS OF AMMONIUM AND POTASSIUM THIOCYANATES 419 for the ammonium thiocyanate. Examination of the heat capacity behavior of the sample near the freezing temperature of methanol showed no detectable amount (less than 0.003 per cent) of methanol entrapped in the crystals. TABLE 1. Experimental heat capacity of ammonium thiocyanate and potassium thiocyanate Ammonium thiocyanate, NH,SCN Series I 237.88 25.57 55.92 7.709 31.44 3.461 112.36 14.78 247.80 26.35 59.67 8.288 34.43 4.031 118.45 15.43 257.46 27.07 127.98 16.40 266.90 27.77 Series IV Series V 137.67 17.34 276.12 28.44 5.62. 0.022 61.45 8.556 146.89 18.21 285.16 29.09 6.27 0.034 64.65 9.026 156.46 19.08 294.02 29.69 6.82 0.044 68.33 9.532 166.35 20.03 302.71 30.28 7.46 0.062 72.93 10.139 175.89 20.67 311.24 30.84 8.15 0.086 78.44 10.867 185.13 21.43 320.56 31.43 8.93 0.121 84.34 11.642 194.50 22.18 330.63 32.04 9.89 0.177 90.51 12.387 204.01 22.93 10.99 0.245 217.17 24.03 12.18 0.333 Series VI 228.25 24.82 Series 111 13.48 0.459 89.36 12.257 34.60 4.059 14.90 0.619 95.90 12.990 Series II 35.95 4.316 16.48 0.821 102.84 13.755 172.59 20.40 38.03 4.698 18.1' 1.059 110.17 14.563 182.66 21.23 39.93 5.042 19.97 1.344 117.14 15.30 197.39 22.00 42.10 5.425 21.69 1.645 124.74 16.07 201.82 22.76 44.52 5.847 23.31 1.932 133.64 16.95 210.97 23.47 46.75 6.230 25.03 2.248 219.88 24.18 49.28 6.654 26.89 2.596 228.57 24.85 52.50 7.175 28.99 2.990 Potassium thiocyanate, KSCN Series I 175.49 16.98 Series III 29.17 2.969 96.06 13.009 183.87 17.28 5.53 0.015 31.80 3.578 102.37 13.435 192.85 17.59 6.46 0.024 34.81 4.289 111.96 14.040 202.41 17.93 7.39 0.036 38.57 5.155 122.14 14.622 211.81 18.25 8.41 0.057 42.95 6.117 131.91 15.13 221.06 18.56 9.26 0.083 47.46 7.052 141.34 15.59 230.17 18.85 10.08 0.114 52.26 7.957 150.49 16.00 239.89 19.16 Il.02 0.150 57.50 8.843 159.41 16.37 250.20 19.50 11.96 0.198 65.00 9.967 169.61 16.77 260.34 19.82 12.91 0.260 72.57 10.876 181.05 17.19 270.33 20.15 13.94 0.343 79.37 11.609 192.22 17.57 280.18 20.50 15.06 0.441 87.02 12.340 203.15 17.96 289.87 20.85 16.23 0.576 94.98 12.940 213.86 18.32 299.42 21.21 17.54 0.744 104.63 13.584 224.37 18.66 308.82 21.61 19.02 0.957 234.68 19.00 318.07 21.99 20.64 1.221 327.16 22.45 22.56 1.568 Series II 336.11 22.93 24.69 1.992 167.94 16.69 344.88 23.47 26.88 2.459 420 C.
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