SOLUBILITY OF FRUCTOSE DIPHOSPHATE SODIUM IN AQUEOUS ALCOHOL MIXTURES Yanfei Wang, Yuxiang Zhu , Xiaoyu Zhao, Zuoliang Sha Tianjin Key Laboratory of Marine Resources and Chemistry , College of Marine of Science and Technology, Tianjin University of Science and Technology, Tianjin, P.R. China (zsha@tust.edu.cn) Keywords: Solubility; Fructose Diphosphate Sodium; Solid-Liquid Phase Equilibrium 1.Introduction Solubility data of fructose diphosphate sodium compounds have a broad application and great importance in the pharmaceutical industry, such as the solvent selection for the reaction and separation process. However, a survey of the literature indicates that there is little work on fructose diphosphate sodium . Recently, more and more solubility data, determined by the laser monitoring observation technique, have been published, and the results agree with the known results[1-4]. 2. Experimental Section 2.1 Experimental Materials Fructose diphosphate sodium used in the experiments was supplied by Huatian Pharmaceutical Co. with the purity of 99.9 %( wt %). The mixed solvents were prepared with distilled water and alcohol (Analytically pure). 2.2 Apparatus and Procedure. The setup for solubility measurements is shown in Figure 1.The apparatus for solubility measurement is the same as that described in the literature(Li, Wang, 2001) . A laser beam was used to determine the solubility of the solute in the binary solvent mixture at a known temperature. The laser monitoring system consisted of a laser generator, a photoelectric transformer, and a light intensity display. The solubility apparatus consisted of a jacketed glass vessel maintained at a desired temperature by water circulated from water circulated from a water bath with a thermoelectric controller (type 501 . China) .Continuous stirring was achieved with a magnetic stir bar. The thermometer had an uncertainty of ± 0.05K. An analytical balance (type TG332A,China) with an uncertainty of ± 0.0001g was used during the measurement . 2 3 1 5 6 4 Figure 1.Experimental setup for the measurement of solubility: 1. Laser device 2. Thermometer 3. Jacketed thermometer cell 4. Magnetic stir plate 5. Laser receiver 6. Recorder At the beginning of the experiment, predetermined amounts of solute were transferred into the jacketed vessel, and the corresponding light intensity penetrated through the solution was recorded down and regarded as the maximum value when the temperature was set. Then additional solute of known mass was introduced into the vessel, and light intensity would decrease. If the intensity reaches the previous value , another previous was made . The above procedure was repeated until the intensity was below the maximum and constant for more than 30 min. Finally, the total amount of the solute added was used to compute the solubility . The method for solubility measurement was based on the fact that the light intensity penetrated through the solution would increase with the dissolution of the solute when the temperature was gradually increased . 2.3 Experimental data The solubility data of fructose diphosphate sodium in binary alcohol + water solvent mixtures at the temperature range from 303.15K to 333.15K are presented in Table 1. It can be seen that the solubility of fructose diphosphate sodium gradually increases with the increase of temperature, whereas it decreases with the increase of the fructose diphosphate sodium . X×10-6 450 400 alcohol 59.28% alcohol 39.18% alcohol 45.37% alcohol 50.53% alcohol 55.03% alcohol 35.17% 350 300 250 200 150 100 50 0 298 302 306 310 314 318 322 326 330 334 T/ K Figure 1 Solubility of fructose diphosphate sodium in binary alcohol + water solvent mixtures along temperature. 3.Data model regression 3.1The results of regression models Polynomial equation of experience x = A + B ×T + C ×T 2 + D ×T 3 + E ×T 4 (1) Where x is the mole fraction solubility of fructose diphosphate sodium in binary alcohol + water solvent mixtures , T is the absolute temperature (K) , and A , B ,C ,D and E are the mole parameters . The values of parameters A , B , C ,D and E are listed in Table 1. Table 1 Parameters of equation 3 for fructose diphosphate sodium in binary alcohol + water solvent mixtures w A B 10-5C 10-7D 10-10E R2 0.3517 -8.0731 0.1037 0.9982 -49.9455 10.6824 -8.5615 0.3918 0.7626 -0.009 4.09810 -0.8110 0.5987 0.9967 0.4537 -3.4285 0.0438 -21.0633 4.49033 -3.5875 0.9953 0.5053 1.1677 -0.0145 6.82108 -1.4155 1.1002 0.9999 0.5503 -0.8505 0.0108 -5.1470 1.0892 -0.8638 0.9980 0.5928 0.9603 -0.0120 5.6789 -1.1870 0.9298 0.9995 Apelblat model ln x1 = A + B / T + C ln(T ) Where x is the mole fraction solubility of fructose diphosphate sodium in binary alcohol + water solvent mixtures, T is the absolute temperature , and A , B and C are the mole parameters . The values of parameters A , B , C are listed in Table 2. Table 2 Parameters of equation 4 for fructose diphosphate sodium in binary alcohol + water solvent mixtures w A B C R2 0.3517 0.3918 0.4537 0.5053 0.5503 1250.77 1533.83 952.09 2023.39 -63894.63 -76636.50 -49224.54 -99892.63 -183.64 -225.89 -139.93 -298.24 1127.87 -58240.33 -165.63 0.9909 0.9962 0.9886 0.9968 0.9904 0.5928 1459.31 -73661.27 -214.82 0.9922 The experimental and the calculation values of two kinds of model were listed in Table 3,where T is the absolute temperature, δ x is the relative deviation, and xexp and xcal are the experimental and calculation values of the solubility, respectively. Table 3 The experimental and the calculation values of fructose diphosphate sodium . Polynomial Apelblat equation model T 10-5xexp 10-5xcal 10-5xexp 10-5xcal δx δx 303.58 308.45 313.15 317.95 322.45 327.75 332.35 8.47 12.18 16.32 25.20 31.02 38.06 40.45 8.13 12.15 17.31 24.13 31.24 38.31 40.35 298.73 303.57 308.39 313.2 318.03 322.86 327.71 332.48 3.48 5.93 8.49 11.44 16.57 19.10 21.66 24.01 3.60 5.57 8.60 12.15 15.80 19.16 21.95 23.91 298.75 303.59 308.31 313.08 317.97 322.89 327.68 2.68 5.03 7.48 8.79 12.40 16.28 17.83 2.71 5.08 7.07 9.41 12.37 15.64 18.39 W=0.3517 0.0406 0.0028 0.0602 0.0428 0.0069 0.0065 0.0027 W=0.3918 0.0338 0.0619 0.0118 0.0613 0.0470 0.0027 0.0129 0.0045 W=0.4537 0.0077 0.0087 0.0552 0.0703 0.0029 0.0395 0.0311 8.47 12.18 16.32 25.20 31.02 38.06 40.45 8.6 12.83 17.88 23.81 29.78 36.74 42.21 0.0149 0.0531 0.0951 0.0555 0.0401 0.0347 0.0433 3.48 5.93 8.49 11.44 16.57 19.10 21.66 24.01 3.74 5.92 8.72 12.01 15.57 19.01 21.98 24.07 0.0740 0.0030 0.0259 0.0491 0.0609 0.0052 0.0143 0.0022 2.68 5.03 7.48 8.79 12.40 16.28 17.83 3.55 5.18 7.16 9.51 12.20 15.06 17.81 0.3200 0.0286 0.0432 0.0817 0.0166 0.0751 0.0014 332.37 19.67 19.52 298.74 303.48 308.29 313.12 317.95 322.77 327.6 332.43 1.36 2.90 5.07 7.54 9.67 11.50 13.10 14.26 1.36 2.91 5.11 7.48 9.69 11.56 13.05 14.27 298.75 303.58 308.37 313.14 317.94 322.75 327.56 332.33 0.65 2.12 3.58 5.19 6.62 8.01 10.31 11.49 0.62 2.21 3.61 5.03 6.61 8.33 10.05 11.56 298.70 303.56 308.36 313.17 317.9 322.69 327.53 332.29 0.36 0.95 1.77 2.99 3.95 4.90 5.55 6.36 0.38 0.89 1.86 2.96 3.98 4.85 5.60 6.35 0.0077 W=0.5053 0.0019 0.0011 0.0063 0.0091 0.0017 0.0045 0.0043 0.0007 W=0.5503 0.0578 0.0392 0.0068 0.0322 0.0027 0.0387 0.0260 0.0060 W=0.5928 0.0409 0.0642 0.0466 0.0124 0.0056 0.0120 0.0086 0.0030 19.67 20.31 0.0325 1.36 2.90 5.07 7.54 9.67 11.50 13.10 14.26 1.89 3.20 4.99 7.17 9.49 11.64 13.29 14.19 0.38704 0.10084 0.01728 0.05012 0.01898 0.01144 0.01398 0.00491 0.65 2.12 3.58 5.19 6.62 8.01 10.31 11.49 1.50 2.35 3.46 4.83 6.44 8.21 10.03 11.74 1.2795 0.1050 0.0351 0.0707 0.0283 0.0237 0.0279 0.0217 0.36 0.95 1.77 2.99 3.95 4.90 5.55 6.36 0.83 1.35 2.02 2.85 3.77 4.73 5.64 6.37 1.2737 0.4195 0.1366 0.0491 0.0474 0.0364 0.0158 0.0002 4. Conclusion (1)The experimental results show that the solubility of fructose diphosphate sodium is a function of temperature, and solubility increase with an increase of temperature. (2) The solubility decreases with an increase of fructose diphosphate sodiumin in the solvent mixture, and the solubility in pure alcohol is the lowest.(3) The calculated solubilities of fructose diphosphate sodium show good agreement with the experimental values, and the experimental solubility and correlation equation in this work can be used as essential data and models in the purification process of fructose diphosphate sodium. References: [1] Hao, H. X.; Wang, J. K.; Wang, Y. L. Solubility of dexamethasone sodium phosphate in different solvents. J. Chem. Eng. Data 2004, 49, 1697-1698. [2] Li, D. Q.; Lin, Y. J.; Evans, D. G.; Duan, X. 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