Method of Analysis

Thimerosal

C9H 9HgNaO2S 404.81 Mercury, ethyl(2-mercaptobenzoato-S)-, sodium salt. Ethyl (sodium o-mercaptobenzoato)mercury [54-64-8]. Thimerosal contains not less than 97.0 percent and not more than 101.0 percent of C9H9HgNaO2S, calculated on the dried basis. Packaging and storage Preserve in tight, light-resistant containers. USP Reference standards USP Thimerosal RS. Identification A: Infrared Absorption . B: To a solution (1 in 100) add a few drops of silver nitrate TS: a pale yellow precipitate is formed. Loss on drying Dry it in vacuum over phosphorus pentoxide to constant weight: it loses not more than 0.5% of its weight. Ether-soluble substances Shake 500 mg, accurately weighed, with 20 mL of anhydrous ethyl ether for 10 minutes. Filter, evaporate the ether in a tared container, dry the residue in vacuum over phosphorus pentoxide, and weigh: the weight of residue does not exceed 4 mg (0.8%). Mercury ions Iodide reagent [note Prepare fresh daily; keep the stopper in the flask and protect from light.] Dissolve 33.20 g of potassium iodide in 75 mL of water in a 100-mL volumetric flask, dilute with water to volume, and mix. Standard preparation Transfer about 190 mg of mercuric chloride, accurately weighed, to a 200-mL volumetric flask, and dissolve in 100 mL of water. Dilute with water to volume, and mix. Transfer 5.0 mL of this solution to a 50-mL volumetric flask, dilute with water to volume, and mix. The concentration of mercuric chloride in the Standard preparation is about 95 g per mL. Test solution Transfer about 500 mg of Thimerosal, accurately weighed, to a 100 mL volumetric flask, add water to volume, and mix to dissolve. Test preparation A volume, and mix. Test preparation B Transfer 10.0 mL of the Test solution to a 50mL volumetric flask, dilute with water to Transfer 10.0 mL of the Test solution to a 50-mL volumetric flask, add 5.0 mL of the
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Standard preparation, dilute with water to volume, and mix. Procedure [note Protect all solutions from light prior to determining their absorbances.] Label five 10-mL volumetric flasks C, D, E, F, and R. Transfer 5.0 mL of Test preparation A to flasks C and D, transfer 5.0 mL of Test preparation B to flasks E and F, and transfer 5.0 mL of water to flask R. Dilute flasks C and E with water to volume, and mix. Dilute flasks D, F, and R with the Iodide reagent to volume, and mix. Concomitantly determine the absorbances of the solutions in 1-cm cells at the wavelength of maximum absorbance for the tetraiodomercurate ion at about 323 nm (located from the similarly determined UV spectrum of a solution prepared by mixing 1.0 mL of the Standard preparation with 5.0 mL of Iodide reagent and diluting with water to 10.0 mL), with a suitable spectrophotometer, using water as the blank. Record the absorbances of the solutions in flasks C, D, E, F, and R as AC, AD, AE, AF, and AR, respectively. Calculate the percentage of mercury ions by the formula: (200.59 / 271.50)(5C / W)(AU / AS) in which 200.59 is the atomic weight of mercury, 271.50 is the molecular weight of mercuric chloride, AU is the absorbance of the test specimen obtained by the equation: AS is the absorbance of the Standard obtained by the equation: AS = (AF AR AE AU)

C is the concentration, in g per mL, of mercuric chloride in the Standard preparation; and W is the weight, in mg, of Thimerosal taken: the limit is 0.70%. Readily carbonizable substances more color than Matching Fluid J. Dissolve about 200 mg in 5 mL of sulfuric acid TS: the solution has no

Assay [note The Standard preparation and the Assay preparation may be diluted quantitatively with water, if necessary, to obtain solutions of suitable concentrations adaptable to the linear or working range of the instrument.] Standard preparation Dissolve an accurately weighed quantity of USP Thimerosal RS in water, and dilute quantitatively with water to obtain a solution having a known concentration of about 1 mg per mL. Assay preparation Transfer about 100 mg of Thimerosal, accurately weighed, to a 100-mL volumetric flask, add 25 mL of water, and mix to dissolve. Dilute with water to volume, and mix. Procedure Concomitantly determine the absorbances of the Standard preparation and the Assay preparation, at the mercury resonance line of 254 nm, with a suitable atomic absorption spectrophotometer (see Spectrophotometry and Light-Scattering ), equipped with a mercury hollow-cathode lamp and an air

*acetylene flame, using water as the blank. Calculate the quantity, in mg, of C9H9HgNaO2S in the portion of Thimerosal taken by the formula: 100C(AU / AS) in which C is the concentration, in mg per mL, of USP Thimerosal RS in the Standard preparation; and AU and AS are the absorbances of the Assay preparation and the Standard preparation, respectively. USP32*NF27 Page 3723 Pharmacopeial Forum: Volume No. 34(5) Page 1197
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