232ELEMENTALIMPURITIES-LIMITS（主要杂质控制）USP39.pdfVIP

Accessed from 10.6.1.1 by zpmtknv2s on Mon Aug 22 03:49:40 EDT 2016 268 á231ñ Heavy Metals / Chemical Tests USP 39 Method III pH 3.5 Acetate Buffer—Prepare as directed under Method I. Standard Preparation—Transfer a mixture of 8 mL of sulfuric acid and 10 mL of nitric acid to a clean, dry, 100-mL Kjeldahl flask, and add a further volume of nitric acid equal to the incremental volume of nitric acid added to the Test Preparation. Heat the solution to the production of dense, white fumes; cool; cautiously add 10 mL of water; and, if hydrogen peroxide was used in treating the Test Preparation, add a volume of 30 percent hydrogen peroxide equal to that used for the substance be- ing tested. Boil gently to the production of dense, white fumes. Again cool, cautiously add 5 mL of water, mix, and boil gently to the production of dense, white fumes and to a volume of 2 to 3 mL. Cool, dilute cautiously with a few mL of water, add 2.0 mL of Standard Lead Solution (20 mg of Pb), and mix. Transfer to a 50-mL color-comparison tube, rinse the flask with water, adding the rinsing to the tube until the volume is 25 mL, and mix. Test Preparation—Unless otherwise indicated in the individual monograph, use a quantity, in g, of the substance to be tested as calculated by the formula: 2.0/(1000L) in which L is the Heavy metals limit, as a percentage. If the substance is a solid—Transfer the weighed quantity of the test substance to a clean, dry, 100-mL Kjeldahl flask. [NOTE—A 300-mL flask may be used if the reaction foams excessively.] Clamp the flask at an angle of 45°, and add a sufficient