C7H5NO3S 183.19
1,2-Benzisothiazol-3(2H)-one, 1,1-dioxide.
1,2-Benzisothiazolin-3-one 1,1-dioxide [81-07-2].
Saccharin contains not less than 99.0 percent and not more than 101.0 percent of C7H5NO3S, calculated on the dried basis.
Packaging and storage: Preserve in well-closed containers. Store at room temperature.
Clarity of solution: [NOTE: The Test solution is to be compared to Reference suspension A and to water in diffused daylight 5 minutes after preparation of Reference suspension A.]
Hydrazine solution: Transfer 1.0 g of hydrazine sulfate to a 100-mL volumetric flask, dissolve in and dilute with water to volume, and mix. Allow to stand for 4 to 6 hours.
Amine of methen solution: Transfer 2.5 g of amine of methen to a 100-mL glass-stoppered flask, add 25.0 mL of water, insert the glass stopper, and mix to dissolve.
Primary opalescent suspension: [NOTE: This suspension is stable for 2 months, provided it is stored in a glass container free from surface defects. The suspension must not adhere to the glass and must be well mixed before use.] Transfer 25.0 mL of Hydrazine solution to the Amine of methen solution in the 100-mL glass-stoppered flask. Mix, and allow to stand for 24 hours.
Opalescence standard: [NOTE: This suspension should not be used beyond 24 hours after preparation.] Transfer 15.0 mL of the Primary opalescent suspension to a 1000-mL volumetric flask, dilute with water to volume, and mix.
Reference suspensions: Transfer 5.0 mL of the Opalescence standard to a 100-mL volumetric flask, dilute with water to volume, and mix to obtain Reference suspension A. Transfer 10.0 mL of the Opalescence standard to a second 100-mL volumetric flask, dilute with water to volume, and mix to obtain Reference suspension B.
Test solution: Dissolve 5.0 g of test material in about 20 mL of a 200 g per L solution of sodium acetate, dilute with the same solution to 25 mL, and mix.
Procedure: Transfer a sufficient portion of the Test solution to a test tube of colorless, transparent, neutral glass with a flat base and an internal diameter of 15 mm to 25 mm to obtain a depth of 40 mm.
Similarly transfer portions of Reference suspension A, Reference suspension B, water, and a 200 g per L solution of sodium acetate to separate matching test tubes. Compare the Test solution, Reference suspension A, Reference suspension B, water, and a 200 g per L solution of sodium acetate in diffused daylight, viewing vertically against a black. [NOTE—The diffusion of light must be such that Reference suspension A can readily be distinguished from water and that Reference suspension B can readily be distinguished from Reference suspension A.] The Test solution shows the same clarity as that of water, or the 200 g per L solution of sodium acetate, or its opalescence is not more pronounced than that of Reference suspension A.
Color of solution:
Standard stock solution: Combine 3.0 mL of ferric chloride, 3.0 mL of cobaltous chloride, 2.4 mL of cupric sulfate, and 1.6 mL of dilute hydrochloric acid (10 g per L).
Standard solution: [NOTE: Prepare the Standard solution immediately before use.] Transfer 1.0 mL of Standard stock solution to a 100-mL volumetric flask, dilute with dilute hydrochloric acid (10 g per L) to volume, and mix.
Test solution: Use the Test solution from Clarity of solution.
Procedure: Transfer a sufficient portion of the Test solution to a test tube of colorless, transparent, neutral glass with a flat base and an internal diameter of 15 mm to 25 mm to obtain a depth of 40 mm.
Similarly transfer portions of the Standard solution, a 200 g per L solution of sodium acetate, and water to separate matching test tubes. Compare the Test solution, the Standard solution, a 200 g per L solution of sodium acetate, and water in diffused daylight, viewing vertically against a white background. The Test solution has the appearance of water or the 200 g per L solution of sodium acetate, or is not more intensely colored than the Standard solution.
Identification: Infrared Absorption 197K .
Melting range: between 226C and 230C.
Loss on drying: Dry it at 105C for 2 hours: it loses not more than 1.0% of its weight.
Readily carbonizable substances: Dissolve 200 mg in 5 mL of sulfuric acid (between 94.5% and 95.5% [w/w] of H2SO4), and keep at a temperature of 48C to 50C for 10 minutes: the solution has no more color than Matching Fluid A, when viewed against a white background.
Residue on ignition: not more than 0.2%. Ignition temperature: 600C ± 50C.
Heavy metals: 0.001%.
Limit of toluenesulfonamides:
Internal standard solution: Dissolve 25 mg of caffeine in methylene chloride, and dilute with the same solvent to 100 mL.
Reference solution: Dissolve 20.0 mg of USP o-Toluenesulfonamide and 20.0 mg of USP p-Toluenesulfonamide in methylene chloride, and dilute with the same solvent to 100.0 mL. Dilute 5.0 mL of the solution with methylene chloride to 50.0 mL. Evaporate 5.0 mL of the final solution to dryness in a stream of nitrogen. Dissolve the residue in 1.0 mL of the Internal standard solution.
Test solution: Suspend 10.0 g of the substance to be examined in 20 mL of water, and dissolve using 5 mL to 6 mL of 10 N sodium hydroxide. If necessary, adjust the solution with 1 N sodium hydroxide or 1 N hydrochloric acid to a pH of 7 to 8, and dilute with water to 50 mL. Shake the solution with four quantities each of 50 mL of methylene chloride. Combine the lower layers, dry over anhydrous sodium sulfate, and filter. Wash the filter and the sodium sulfate with 10 mL of methylene chloride. Combine the solution and the washings, and evaporate almost to dryness in a water bath at a temperature not exceeding 40C. Using a small quantity of methylene chloride, quantitatively transfer the residue into a suitable 10-mL tube, evaporate to dryness in a stream of nitrogen, and dissolve the residue in 1.0 mL of the Internal standard solution.
Blank solution: Evaporate 200 mL of methylene chloride to dryness in a water bath at a temperature not exceeding 40C. Dissolve the residue in 1 mL of methylene chloride.
Chromatographic system: The gas chromatograph is equipped with a flame-ionization detector and contains a 0.53-mm × 10-m fused silica column, coated with G3 phase (film thickness 2 Gm). The injection port, column, and detector temperatures are maintained at about 250C, 180C, and 250C, respectively; and nitrogen is used as the carrier gas at a flow rate of about 10 mL per minute. The injector employs a split ratio of 1:2.
Procedure: Inject about 1 GL of the Reference solution. Adjust the sensitivity of the detector so that the height of the peak due to caffeine is not less than 50% of the full scale of the recorder. The substances are eluted in the following order: o-toluenesulfonamide, p-toluenesulfonamide, and caffeine. The test is not valid unless the resolution between the peaks due to o-toluenesulfonamide and p-toluenesulfonamide is at least 1.5. Inject about 1 GL of the Blank solution. In the chromatogram obtained, verify that there are no peaks with the same retention times as the internal standard, otoluenesulfonamide, and p-toluenesulfonamide. Inject about 1 GL of the Test solution and 1 GL of the Reference solution. If any peaks due to o-toluenesulfonamide, and p-toluenesulfonamide appear in the chromatogram obtained with the Test solution, the ratio of their areas to that of the internal standard is not greater than the corresponding ratio in the chromatogram obtained with the Reference solution (10 ppm of o-toluenesulfonamide and 10 ppm of p-toluenesulfonamide).
Limit of benzoate and salicylate: To 10 mL of a hot, saturated solution of it add ferric chloride, dropwise: no precipitate or violet color appears in the liquid.
Assay: Accurately weigh about 500 mg of Saccharin, dissolve in 40 mL of alcohol, add 40 mL of water, mix, add PhPh, and titrate with 0.1 N sodium hydroxide. Perform a blank titration, if necessary, and make the appropriate correction. Each mL of 0.1 N sodium hydroxide is equivalent to 18.32 mg of C7H5NO3S.
o-Benzosulfimide; Gluside; 1,2-Benzisothiazole-3(2H)-one-1,1-dioxide
C7H5NO3S Formula wt 183.18
INS: 954 CAS: [81-07-2]
DESCRIPTION
Saccharin occurs as white crystals or as a white, crystalline powder. Its solutions are acid to litmus. One gram is soluble in 290 mL of water at 25C, in 25 mL of boiling water, and in 30 mL of alcohol. It is slightly soluble in chloroform and in ether, and it is readily dissolved by dilute solutions of ammonia, solutions of alkali hydroxides, or solutions of alkali carbonates with the evolution of carbon dioxide.
Function: Nonnutritive sweetener.
Specifications of Saccharin BP Ph Eur Grade:
C7H5NO3S --- 183.2 --- CAS 81-07-2
Action and use: Sweetening agent.
DEFINITION
1,2-Benzisothiazol-3(2H)-one 1,1-dioxide.
Content: 99.0 per cent to 101.0 per cent (dried substance).
CHARACTERS
Appearance: White or almost white, crystalline powder or colourless crystals.
Solubility: Sparingly soluble in boiling water and in ethanol (96 per cent), slightly soluble in cold water. It dissolves in dilute solutions of alkali hydroxides and carbonates.
IDENTIFICATION
First identification: C
Second identification: A, B, D, E
A. A saturated solution, prepared without heating, turns blue litmus paper red.
B. Melting point: 226C to 230C.
C. Infrared absorption spectrophotometry.
Comparison Saccharin CRS.
D. Mix about 10 mg with about 10 mg of resorcinol add 0.25 mL of sulfuric acid and carefully heat the mixture over a naked flame until a dark green colour is produced. Allow to cool, add 10 mL of water and dilute sodium hydroxide solution until an alkaline reaction is produced. An intense green fluorescence develops.
E. To 0.2 g add 1.5 mL of dilute sodium hydroxide solution evaporate to dryness and heat the residue carefully until it melts, avoiding carbonisation. Allow to cool, dissolve the mass in about 5 mL of water, add dilute hydrochloric acid until a weak acid reaction is produced and filter, if necessary. To the filtrate add 0.2 mL of ferric chloride solution. A violet colour develops.
TESTS
Solution S: Dissolve 5.0 g in 20 mL of a 200 g/L solution of sodium acetate and dilute to 25 mL with the same solution.
Appearance of solution: Solution S is clear and colourless.
o- and p-Toluenesulfonamide: To pass the test by Gas chromatography.
Limits:
-o-toluenesulfonamide: the ratio of its area to that of the internal standard is not greater than the corresponding ratio in the chromatogram obtained with the reference solution (10 ppm),
-p-toluenesulfonamide: the ratio of its area to that of the internal standard is not greater than the corresponding ratio in the chromatogram obtained with the reference solution (10 ppm).
Readily carbonisable substances: Dissolve 0.20 g in 5 mL of sulfuric acid and keep at 48-50C for 10 min. When viewed against a white background, the solution is not more intensely coloured than a solution prepared by mixing 0.1 mL of red primary solution, 0.1 mL of blue primary solution and 0.4 mL of yellow primary solution with 4.4 mL of water.
Loss on drying: Maximum 1.0 per cent, determined on 1.000 g by drying in an oven at 105C for 2 h.
Sulfated ash: Maximum 0.2 per cent, determined on 1.0 g.
