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CONDUCTANCE and VISCOSITY of CONCENTRATED AQUEOUS SALT SOLUTIONS a T 50.50 by M

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CONDUCTANCE and VISCOSITY of CONCENTRATED AQUEOUS SALT SOLUTIONS a T 50.50 by M 802 CHEMISTRY: RICE AND KRA US PROC. N. A. S. CONDUCTANCE AND VISCOSITY OF CONCENTRATED AQUEOUS SALT SOLUTIONS A T 50.50 By M. JOHN RICE, JR.,* t AND CHARLES A. KRAus METCALF RESEARCH LABORATORY, BROWN UNIVERSITY Communicated June 12, 1953. Our knowledge of the electrical conductance and the viscosity of con- centrated salt solutions is very limited. Campbell and Kartzmark1 have measured the conductance and the viscosity of solutions of silver nitrate and ammonium nitrate in water at 950 up to saturation. Seward2 has measured the conductance and viscosity of solutions of tetrabutylammonium picrate in butanol at 93° over the complete range from pure solvent to pure fused salt; Strong' has measured the conductance of some quaternary ammo- nium salts in benzene at 250 up to fairly high concentration but viscosity data are for the most part lacking. Moessen and Kraus4 have measured the conductance of solutions of tetrabutylammonium bromide and tri- methylammonium chloride in bromine at 250 to fairly high concentrations but there are no viscosity data for these solutions. The same is true of potassium iodide in iodine at 140°C. which was measured by Lewis and Wheeler.5 Cesium formate has been reported to be soluble to the extent of one mole of salt to one-half mole of water at 5'.6 However, this datum is in error; the limit of solubility is one mole of salt to approximately two moles of water. However, potassium formate is soluble to the extent of approxi- mately one mole of salt to 1.1 mole of water at 500. The conductance and viscosity of solutions of these two salts have been measured at 50.50 to near saturation. Solutions of the potassium salt were measured to lower concentration in order to approximate the value of A0. In the preparation of cesium formate, cesium chloride was converted to cesium nitrate by repeated treatment with nitric acid. After repeated recrystallizations, the nitrate was converted to carbonate by treatment with oxalic acid in the presence of a small amount of water and subsequent calcination. The carbonate was converted to fonnate by neutralization with formic acid and evaporating to dryness. The salt was recrystallized by dissolving it in 96%0 alcohol and adding ether to precipitate the desired proportion of salt. The final product was dried in vacuo at 1500 for 4-5 hours, m.p. 264°C. (corr.). The nitrate, when tested spectroscopically, showed no traces of metallic elements other than cesium. Potassium formate was prepared by neutralizing potassium carbonate with formic acid and evaporating to dryness. The salt was recrystallized from 96%o alcohol on addition of ether. The product was dried in vacuo at 1500 for 8 to 10 hours. This material was found to contain 1.5% water. Downloaded by guest on September 30, 2021 VOL. 39, 1953 CHEMISTRY: RICE A ND KRA US 803 The water could be completely removed by regrinding the salt and heating in vacuo at 1500 for 10 hours. When necessary, operations were carried out in a dry-box. The solutions were made up in the cells in which their conductance was measured. ThrIee cells of different constants were employed. Two of these were of the Erlenmeyer type with the electrode chamber attached to the outside of the flask. These cells were similar to those described by Daggett, Bair, and Kraus,7 although much smaller. The third cell con- sisted of two cylindrical tubes which were joined at the bottom by a 55-mm. length of smaller tubing of approximately 5 mm. diameter. The cylindrical cells were closed by ground glass caps which carried tubes at the ends of which were sealed platinum electrodes that normally projected into the solution. The cell constant of this cell was 38.430 and was independent of the precise setting of the caps or the volume of solution in the cell. This cell was provided with stopcocks so that the solution could be forced from one arm to the other by air pressure for the purpose of mixing. The other two cells had constants of 0.3081 and 10.669. Cell No. 1 was of approximately 300 cc. capacity and was used for meas- uring the most dilute solutions. A known weight of salt was introduced and weighed quantities of water were added successively. When the cell was full, the greater portion of the solution was withdrawn into a weight pipette and a new series of additions of water was begun. Cell No. 2 had a capacity of approximately 800 cc. and was used for intermediate concentrations. Measurements could be made with a minimum volume of 50 cc. of solution. The desired concentration range could be covered by merely adding known weights of water to a known weight of salt. Cell No. 3 had a capacity of approximately 100 cc. and measurements could be made with a very small volume of solution. The desired concentration range could be covered by merely adding successive weights of water. To determine the densities, known solutions were made up by adding known weights of water to known weights of salt in a large weighing bottle. Samples of these solutions were transferred to a pycnometer which had been calibrated at 50.50. Since the density of the solutions varies slightly from linearity, data are given for densities at a series of concentrations. The density of dry cesium formate was determined by weighing the de- hydrated salt in a pycnometer under hexane. From the weight of hexane and its density and the weight of salt, the density of the salt is readily com- puted. Assuming the density of hexane to be 0.6550, the density of the salt was found to be 2.99. The density of potassium formate was taken to be 1.91.8 Viscosities were measured with a modified Ostwald viscometer. The viscometer was provided with a ground glass cap and solutions were made up in the viscometer. The instrument was calibrated with water and the Downloaded by guest on September 30, 2021 804 CHEMISTRY: RICE AND KRA US PROC. N. A. S. time of efflux was determined as a function of volume of water. The vis- cometer with its contents was weighed on a sensitive balance. Concen- tration could be changed by addition of water and further dilution could be made by withdrawing a known weight of solution and then making fur- ther addition of water. Densities of solutions in water at 50.50 are given for cesium formate and potassium formate in tables 1A and 1B, respectively. Molal concentra- tions appear in column 1, molar concentrations in column 2, and densities in column 3. TABLE 1 DENSITY OF FORMATE SOLUTIONS AT 50.50C. (A) CESIUM FORMATE - .- (B) POTASSIUM FORMATE MOLAR MOLAR CONCENTRATION, C DENSITY CONCENTRATION, C DENSITY 0.00 0.9878 0.00 0.9878 1.193 1.142 3.967 1.160 2.414 1.303 5.643 1.232 4.892 1.613 9.452 1.392 9.068 2.147 TABLE 2 CONDUCTANCE OF FORMATE SOLUTIONS AT 50.50C. (A) CESIUM FORMATB - (B) POTAS$IUM FORMATE EQUIVALENT EQUIVALBNT MOLAR CONC. COND. MOLAR CONC. COND. 10.13 24.80 6.503 63.03 10.06 24.84 3.492 96.17 9.034 33.18 10.45 30.82 6.913 54.33 8.602 44.24 4.629 81.78 15.52 9.780 0.8104 138.1 13.66 14.65 0.5430 145.8 0.5999 142.2 0.3055 153.5 0.2722 154.2 3.231 98.84 0.1543 161.6 2.437 109.5 2.404 110.4 1.785 118.9 1.325 126.4 1.400 125.6 0.07471 168.7 0.01973 176.6- 0.01038 179.8 Conductance data for the cesium and potassium salts are presented in tables 2A and 2B, respectively. Molar concentrations are given in column 1 and equivalent conductances in column 2. Viscosities for solutions of cesium formate and potassium formate are given in tables 3A and 3B, respectively. Molar concentrations are given in column 1, relative viscosities in column 2, and absolute viscosities in centipoises in column 3. Downloaded by guest on September 30, 2021 VOL. 39, 1953 VCHEMISTR Y: RICE AND KRA US 805 In tables 4A and 4B are presented values of the conductance-viscosity product for the cesium and potassium salts, respectively, at rounded molar concentrations. In column 2 are given values of the ratios of moles of salt per mole of water. Values of equivalent conductance and of viscosity TABLE 3 ViscosITY OF FORMATE SOLUTIONS AT 50.50C. (A) CESIUM FORMATE- -(B) POTASSIUM FORMATS-. MOLAR CONC. *7 X 102 POISES MOLAR CONC. X X 102 POISES 9.605 2.612 13.95 5.173 8.203 1.809 8.224 1.463 6.834 1.338 6.090 1.028 3.989 0.8500 4.199 0.8277 2.808 0.7313 3.125 0.7296 5.819 1.117 15.64 8.223 1.784 0.6533 12.26 , 3.403 0.7496 0.5847 10.38 2.216 1.516 0.6245 TABLE 4 CONDUCTANCE-VISCOSITY PRODUCT OF FORMATES AT 50.5°C. MOLBS H20 PBR II X 102 MOLAR CONC. MOLE SALT CONDUCTANCE POISES A-7-PRODUCT (A) Cesium Formate 0.00 ... 192.9 0.5449 1.051 0.25 ... 157.2 0.560 0.879 1.00 0.01893 134.0 0.610 0.817 2.00 0.04080 115.5 0.670 0.774 4.00 0.09141 88.8 0.840 0.746 7.00 0.1981 52.8 1.37 0.723 9.00 0.3018 32.7 2.22 0.726 10.00 0.3704 25.0 2.95 0.738 (B) Potassium Formate 0.00 ..
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