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The Solubility of Sucrose in Hydroalcoholic Solutions
192
JOURNAL OF THE
AMERICAN PHARMACEUTICAL ASSOCIATION
(13) White P. B. J . Palh. Bucl. 35 77(1932). (14) White' P. B.' ibid. 36 65(1'933j. (15) Ward,'M. K:, Pro;. d c . Exfill. Biol. Med., 67, 527 (1948). (16) Kolmer,,, J. S., and Boerner. F.. "Approved Laboratory Technic, 4th ed., Appleton-Century-Crofts, Inc., New York, 1945, p. 324. (17) United States Department of Agriculture, Food and
Vol. XLII, NO. 4
Drug Administration F u l a r 198(1931). (J8)Byrows, W.: Jordan-Burrows kextbook of Bacterlology, 15th ed., W. B. Saunders Co., Philadelphia, 1949, pp. 167-168. (19) Mellon, R. R., Hastings, W. S., and Anastasia, C., J . Immunol., 9, 365(1924). (20) Frobisher. M . , Jr.. J . Iirfeclious Diseuses, 38, 66 (1926).
The Solubility of Sucrose in Hydroalcoholic Solutions* By LOUIS A. REBER A report is presented on the solubility of sucrose in hydroalcoholic solutions, measured at 2 5 over the entire range of alcohol concentrations at intervals of approximately 10 per cent. Information is included concerning the effect of alcohol on the specific rotation of sucrose. NFORMATION on the solubility of sucrose in
hydroalcoholic solutions is incomplete.
Sei-
dell (1) reports data at 0, 14, and 40°,based on work done in the last century. Data at room temperature are entirely lacking. The International Critical Tables (2) contain similar information and also give the solubility of sucrose in 80 per cent alcohol lby volume) a t 20" as 37 Gm./L. of solution. This figure is based on the work of Hudson and Yanovsky (3), who claim that saturation was attained within five minutes after mixing. The solubility reported by these two workers appears to be entirely too low when compared with the values at other temperatures. The present investigation was undertaken to supply data on the solubility of sucrose in hydroalcoholic solutions at 25'. The entire range of alcohol concentrations, a t intervals of approximately 10 per cent, has been covered (Table I).
and was used in the solubility determinations without further purification. Method.-Determinations of solubility were performed by agitating an excess of solute with solvent contained in glass-stoppered bottles sealed with paraffin, in a bath maintained at 25" f 0.01'. The period of agitation was forty-eight hours or longer. The amount of sucrose dissolved was determined by evaporating a weighed amount of saturated solution to dryness and drying the residue in a vacuum oven a t 60". The drying was continued until the residues reached essentiallyconstant weight. At the same time that a sample of saturated solution was removed for analysis, another portion was used to determine the specific gravity in order to permit calculation of solubilities on both weight and volume bases. Measurements of the optical rotation of sucrose solutions were made to determine the effect of alcohol on the specific rotation of sucrose. As much as 50yo (by volume) of alcohol had no demonstrable effect; higher percentages caused an increase in specific rotation. In 80% alcohol (by volume) the specific rotation, [ a ] q ,rose to 67.5 as compared to 66.5 in aqueous solution. Browne and Zerban (4) report a similar but less pronounced effect of alcohol on the specific rotation of sucrose. I
EXPERIMENTAL Materials.-Hydroalcoholic solutions were prepared from distilled water and alcohol S. P. Absolute alcohol was also used as a solvent. In all cases, the percentage of alcohol was determined from measurement of the specific gravity, using a 50-ml. pycnometer. Sucrose was obtained from the National Bureau of Standards. It was checked for optical rotation
u.
*
Received September 5, 1952, from the Chemistry Department, Philadelphia College of Pharmacy and Science, Philadelphia, Pa. Presented to the Scientific Section. A. PH. A,, Philadelphia meeting. August, 1952.
10 20 30 40 50 60 70 80 90 100 PERCENT ALCOHOL (0 BY WEIGHT; A B Y VOLUME)
Fig. 1.-The solubility of sucrose expressed as Gm. of sucrose in 100 Gm. of solution.
SCIENTIFIC EDITION
April, 1953
193
TABLE I.-THE SOLUBILITY OF SUCROSE IN HYDROALCOHOLIC SOLUTIONS Alcohol in Solvent, Weight %
0.00
8.62 15.79 24.88 33.53 42.48 51.83 61.30 72.38 86.15 92.50 99.42
Alcohol in Solvent Volume’%”
0.00 9.48 19.42 30.24 40.18 49.99 59.67 68.93 79.00 90.36 95.05 99.65
---
100 Gm. of Soh.
Solubility as Gm. of Sucrose in 100 MI. 100 Gm. of of Soln. Solvent
100 MI. of Solvent
67.6 65.2 62.2 58.1 52.9 46.1 39.6 25.4 11.39 1.675 0.401 0.065
89.7 85.1 79.5 72.0 63.3 52.8 43.4 25.3 10.32 1.391 0.324 0.051
207.7 184.2 160.0 132.6 105.9 79.3 59.4 30.0 11.01 1.401 0.325 0.051
208.6 187.4 164.8 138.4 112.2 85.7 65.6 33.3 12.85 1.703 0.403 0.065
-
Density of Satd. Soln.. Gm./ml.
1,3274 1.3054 1.2775 1.2411 1.1976 1.1443 1,0949 0.9948 0.9060 0.8307 0.8070 0.7865
“ At 15.56’. RESULTS The results of the solubility measurements are given in Table I, and are expressed graphically in Figs. 1-4; all measurements are at 25” unless otherwise noted.
10 20 30 40 50 60 70 80 90 100 PEKCENT ALCOHOL (0BY WEIGHT; A BY VOLUME)
Fig. 2.-The solubility of sucrose expressed as Gm. of sucrose in 100 ml. of solution.
L *> A 220
200
6 180 Lo
160
$ 140
10 20 30 40 50 60 70 80 90 100 PERCENT ALCOHOL (0BY WEIGHT; A BY VOLUME)
Fig. $.-The solubility of sucrose expressed as Gnr. of sucrose in 100 ml. of solvent.
SUMMARY T h e solubility of sucrose in hydroalcoholic solutions has been determined at 25’. The entire range of alcohol concentrations, at intervals of approximately 10 per cent, has been covered.
g
40
20
PERCENT ALCOHOL (0BY WEIGHT; A BY VOI.UME)
Fig. 3.-The solubility of sucrose expressed as Gni. of sucrose in 100 Gm. of solvent.
REFERENCES .(I) Seidell, A., “Solubilities of Organic Compounds,” 3rd ed. D. Van Nostrand Co. New York,p. 713. (2) “International CrGical Tables,” Vol. 4, 1st ed., McGraw-Hill Book Co., New York. 1928, pp. 405-406. (3) Hudson, C. S., and Yanovsky, E., J . Am. Chem S a c , 39,1013(1917). (4) Browne, C . A , and Zerbao, F. W..“Physical and Chemical Methods of Sugar Analysis,” 3rd ed.. John Wiley and Sons, Inc., New York, 1941, p. 274.
JOURNAL OF THE
AMERICAN PHARMACEUTICAL ASSOCIATION
(13) White P. B. J . Palh. Bucl. 35 77(1932). (14) White' P. B.' ibid. 36 65(1'933j. (15) Ward,'M. K:, Pro;. d c . Exfill. Biol. Med., 67, 527 (1948). (16) Kolmer,,, J. S., and Boerner. F.. "Approved Laboratory Technic, 4th ed., Appleton-Century-Crofts, Inc., New York, 1945, p. 324. (17) United States Department of Agriculture, Food and
Vol. XLII, NO. 4
Drug Administration F u l a r 198(1931). (J8)Byrows, W.: Jordan-Burrows kextbook of Bacterlology, 15th ed., W. B. Saunders Co., Philadelphia, 1949, pp. 167-168. (19) Mellon, R. R., Hastings, W. S., and Anastasia, C., J . Immunol., 9, 365(1924). (20) Frobisher. M . , Jr.. J . Iirfeclious Diseuses, 38, 66 (1926).
The Solubility of Sucrose in Hydroalcoholic Solutions* By LOUIS A. REBER A report is presented on the solubility of sucrose in hydroalcoholic solutions, measured at 2 5 over the entire range of alcohol concentrations at intervals of approximately 10 per cent. Information is included concerning the effect of alcohol on the specific rotation of sucrose. NFORMATION on the solubility of sucrose in
hydroalcoholic solutions is incomplete.
Sei-
dell (1) reports data at 0, 14, and 40°,based on work done in the last century. Data at room temperature are entirely lacking. The International Critical Tables (2) contain similar information and also give the solubility of sucrose in 80 per cent alcohol lby volume) a t 20" as 37 Gm./L. of solution. This figure is based on the work of Hudson and Yanovsky (3), who claim that saturation was attained within five minutes after mixing. The solubility reported by these two workers appears to be entirely too low when compared with the values at other temperatures. The present investigation was undertaken to supply data on the solubility of sucrose in hydroalcoholic solutions at 25'. The entire range of alcohol concentrations, a t intervals of approximately 10 per cent, has been covered (Table I).
and was used in the solubility determinations without further purification. Method.-Determinations of solubility were performed by agitating an excess of solute with solvent contained in glass-stoppered bottles sealed with paraffin, in a bath maintained at 25" f 0.01'. The period of agitation was forty-eight hours or longer. The amount of sucrose dissolved was determined by evaporating a weighed amount of saturated solution to dryness and drying the residue in a vacuum oven a t 60". The drying was continued until the residues reached essentiallyconstant weight. At the same time that a sample of saturated solution was removed for analysis, another portion was used to determine the specific gravity in order to permit calculation of solubilities on both weight and volume bases. Measurements of the optical rotation of sucrose solutions were made to determine the effect of alcohol on the specific rotation of sucrose. As much as 50yo (by volume) of alcohol had no demonstrable effect; higher percentages caused an increase in specific rotation. In 80% alcohol (by volume) the specific rotation, [ a ] q ,rose to 67.5 as compared to 66.5 in aqueous solution. Browne and Zerban (4) report a similar but less pronounced effect of alcohol on the specific rotation of sucrose. I
EXPERIMENTAL Materials.-Hydroalcoholic solutions were prepared from distilled water and alcohol S. P. Absolute alcohol was also used as a solvent. In all cases, the percentage of alcohol was determined from measurement of the specific gravity, using a 50-ml. pycnometer. Sucrose was obtained from the National Bureau of Standards. It was checked for optical rotation
u.
*
Received September 5, 1952, from the Chemistry Department, Philadelphia College of Pharmacy and Science, Philadelphia, Pa. Presented to the Scientific Section. A. PH. A,, Philadelphia meeting. August, 1952.
10 20 30 40 50 60 70 80 90 100 PERCENT ALCOHOL (0 BY WEIGHT; A B Y VOLUME)
Fig. 1.-The solubility of sucrose expressed as Gm. of sucrose in 100 Gm. of solution.
SCIENTIFIC EDITION
April, 1953
193
TABLE I.-THE SOLUBILITY OF SUCROSE IN HYDROALCOHOLIC SOLUTIONS Alcohol in Solvent, Weight %
0.00
8.62 15.79 24.88 33.53 42.48 51.83 61.30 72.38 86.15 92.50 99.42
Alcohol in Solvent Volume’%”
0.00 9.48 19.42 30.24 40.18 49.99 59.67 68.93 79.00 90.36 95.05 99.65
---
100 Gm. of Soh.
Solubility as Gm. of Sucrose in 100 MI. 100 Gm. of of Soln. Solvent
100 MI. of Solvent
67.6 65.2 62.2 58.1 52.9 46.1 39.6 25.4 11.39 1.675 0.401 0.065
89.7 85.1 79.5 72.0 63.3 52.8 43.4 25.3 10.32 1.391 0.324 0.051
207.7 184.2 160.0 132.6 105.9 79.3 59.4 30.0 11.01 1.401 0.325 0.051
208.6 187.4 164.8 138.4 112.2 85.7 65.6 33.3 12.85 1.703 0.403 0.065
-
Density of Satd. Soln.. Gm./ml.
1,3274 1.3054 1.2775 1.2411 1.1976 1.1443 1,0949 0.9948 0.9060 0.8307 0.8070 0.7865
“ At 15.56’. RESULTS The results of the solubility measurements are given in Table I, and are expressed graphically in Figs. 1-4; all measurements are at 25” unless otherwise noted.
10 20 30 40 50 60 70 80 90 100 PEKCENT ALCOHOL (0BY WEIGHT; A BY VOLUME)
Fig. 2.-The solubility of sucrose expressed as Gm. of sucrose in 100 ml. of solution.
L *> A 220
200
6 180 Lo
160
$ 140
10 20 30 40 50 60 70 80 90 100 PERCENT ALCOHOL (0BY WEIGHT; A BY VOLUME)
Fig. $.-The solubility of sucrose expressed as Gnr. of sucrose in 100 ml. of solvent.
SUMMARY T h e solubility of sucrose in hydroalcoholic solutions has been determined at 25’. The entire range of alcohol concentrations, at intervals of approximately 10 per cent, has been covered.
g
40
20
PERCENT ALCOHOL (0BY WEIGHT; A BY VOI.UME)
Fig. 3.-The solubility of sucrose expressed as Gni. of sucrose in 100 Gm. of solvent.
REFERENCES .(I) Seidell, A., “Solubilities of Organic Compounds,” 3rd ed. D. Van Nostrand Co. New York,p. 713. (2) “International CrGical Tables,” Vol. 4, 1st ed., McGraw-Hill Book Co., New York. 1928, pp. 405-406. (3) Hudson, C. S., and Yanovsky, E., J . Am. Chem S a c , 39,1013(1917). (4) Browne, C . A , and Zerbao, F. W..“Physical and Chemical Methods of Sugar Analysis,” 3rd ed.. John Wiley and Sons, Inc., New York, 1941, p. 274.