Sodium Saccharin

Soluble Saccharin

C7H4NNaO3SnH2O (n=2 or 0)

Mol. Wt. dihydrate

241.20

anhydrous 205.17
monosodium 3-oxo-1,2-benzisothiazoline 1,1-dioxide

dihydrate

6155-57-3

anhydrous 128-44-9
Content

Sodium Saccharin, when dried, contains 99.0 101.0% of soluble

saccharin (C7H4NNaO3S).
Description

Sodium Saccharin occurs as colorless to white crystals or powder,

having an extremely sweet taste.

Identification

(1)

To 10 ml of Sodium Saccharin solution (1 10), add 1 ml of

diluted hydrochloric acid (1 3), allow to stand for 1 hour, and filter the white
crystalline precipitate formed. Wash the residue on the filter paper thoroughly with
water, dry at 105for 2 hours, and measure the melting point. It is 226230.
(2)

Mix 20 mg of Sodium Saccharin with 40 mg of resorcinol, add 10 drops of

sulfuric acid, and heat gently until the color of the mixture changes to dark green. Cool,
and dissolve in 10 ml of water and 10 ml of sodium hydroxide solution (1 25). The
solution emits a green fluorescence.
(3)

Dissolve 0.1 g of Sodium Saccharin in 5 ml of sodium hydroxide solution (1

25), evaporate to dryness while gently heating, and fuse, being careful to avoid
carbonizing. Continue heating until the odor of ammonia no longer develops. Cool,
dissolve in about 20 ml of water, neutralize with diluted hydrochloric acid (1 10),
filter, and then add 1 drop of ferric chloride solution (1 10) to the filtrate. A purple
to red-purple color develops.
(4)

Sodium Saccharin solution (1 10) responds to all tests for Sodium Salt as

described in the Qualitative Tests.

Purity

(1)

Clarity and color of solution

Colorless, clear (powder 1.0 g, water

1.5 ml). Colorless, clear (powder 1.0 g, ethanol 70 ml).

(2)

Free acid and free alkali

Weigh 1.0 g of Sodium Saccharin, dissolve in 10 ml

of freshly boiled and cooled water, and add 1 drop of phenolphthalein TS. No pink color
develops. Add 1 drop of 0.1 mol/l sodium hydroxide. A pink color develops.
(3)

Heavy metals

Not more than 10 g/g as Pb (2.0 g, Method 1, Control

solution Lead Standard Solution 2.0 ml).

Not more than 4.0 g/g as As2O3 (0.50 g, Method 1, Apparatus B).

(4)

Arsenic

(5)

Benzoate and salicylate

Weigh 0.5 g of Sodium Saccharin, dissolve in 10 ml

of water, and add 5 drops of acetic acid and 3 drops of ferric chloride solution (1 10).
No precipitate is formed, and no purple to red-purple color develops.
(6)

o-Toluenesulfonamide Not more than 25 g/g as o-toluenesulfonamide.

Test Solution Weigh 10 g of Sodium Saccharin, dissolve in 50 ml of water, and

extract three times with 30 ml of ethyl acetate each time. Combine all the ethyl acetate
layers, and wash with 30 ml of sodium chloride solution (1 4), and add about 10 g of
anhydrous sodium sulfate, and shake. Transfer the ethyl acetate layer quantitatively
to an eggplant-type flask, evaporate the ethyl acetate, and dissolve the residue in 1.0
ml of a solution of caffeine in ethyl acetate (1 4,000).

Control Solution Measure 1.0 ml of a solution of o-toluenesulfonamide in ethyl

acetate (1 4,000), remove the ethyl acetate while heating on a water bath, and
dissolve the residue in 1.0 ml of a solution of caffeine in ethyl acetate (1 4,000).

Procedure

Perform Gas Chromatography on the test solution and the control

solution under the conditions given below. The ratio H/Hs of the peak height of

o-toluenesulfonamide (H) of the test solution to the peak height of caffeine (Hs) does
not exceed the ratio H/Hs of the peak height of o-toluenesulfonamide (H4) of the
control solution to the peak height of caffeine (Hs).

Operating Conditions
Detector: Hydrogen flame ionization detector.
Column packing material
Liquid phase: 3% of the amount of support is diethylene glycol succinate
polyester.
Support: 177- to 250- mm diatomaceous earth for gas chromatography.
Column tube: Glass or stainless steel tube 1 m in length and 34 mm in
internal diameter.
Column temperature: Constant temperature of 195205.
Carrier gas and flow rate: Use nitrogen. Adjust the column temperature and
the flow rate of the carrier gas so that the caffeine peak appears after
about 6 minutes.
Loss on Drying

Not more than 15.0% (120, 4 hours).

Assay

Weigh accurately about 0.3 g of Sodium Saccharin, previously dried,

dissolve in 20 ml of acetic acid for nonaqueous titration, and titrate with 0.1 mol/l
perchloric acid (indicator: 2 drops of crystal violetacetic acid TS) until the color of the
solution changes from purple through blue to green. Perform a blank test in the same
manner, and make any necessary correction.
1 ml of 0.1 mol/l perchloric acid = 20.517 mg of C7H4NNaO3S