Thursday, July 2, 2009

repeating this procedure to remove any trace of hydrogen peroxide. Cool, add cautiously 10 ml of water wash the sides

spectrophotomelry. Appendix 5.2 with- a furnace as atomic generator and measuring at 309.3 nm and using as standard solutions, a suitable range of dilutions in water of aluminium standard solution (10 ppm AI further diluted, as necessary, with a solution containing 0.17% w/v of magnesium nitrate and 0.05% w/v of octoxinol 10 in a solution of nitric acid containing 1% S w/v of HNO3 Prepare suitable dilutions of the preparation being examined and human albumin for aluminum validation RS with water Dilute the solutions, as necessary, with the magnesium nitrate-octoxir octoxinol10-nitric acid solution used for dilution of the standard solution. The test is valid only if the aluminium content determined for human albumin for aluminium validation RS is within 20% of The stated value NOTE-Wash all equipment with a solution containing 20% w/v of nitric acid before use and use plastic containers only to prepare all solutions ALGlNlC ACID Polymannuronic Acid Alginic acid is a hydrophilic colloidaE mixture of polyuronic acids, [(C8H8O8),l composed of residues of d-mannuronicacid and L-guluronic acid extracted with dilute alkali from various species of brown seaweeds (Fam Phaeophyceae) Category Pharrnaceutical aid (viscosity increasing agent). Description White to yellowish-white, fibrous powder, odourless Solubility Insoluble but swells in water, practically insoluble or very slightly soluble in ethanol (95%) and in organic solvents It is soluble in alkaline solutions Storage Store in tightly-closed containers STANDARDSAlgnic Acid contains not less than 19.0 percent and not more than 25.0 percent of carboxylic acid groups (CooH), calculated with reference to the dried substance Identification A. To 5 ml of a 0 75% w/v solubon in 0.1 M sodium hydroxide add 1 ml of calcium chloride solution, a gelatinous precipitate is formed B. To 5 ml of the solution obtained in test A add 1 ml of 2M sulphuric acid, a gelatinous precipitate is formed C: To about 5 mg in-a test-tubE add 5 ml of water, 1 ml of a freshly-prepared 1% w/v solution of 1,3-naphthalenedioI in ethanol (95%) and 5 ml of hydrochloric acid Heal the mixture to boiling, boil gently for 3 minutes and cool to about 15* Transfer the contents of the test-tube to a small separator with the aid of 5 ml of water and extract with 15 ml of di-isopropyl ethier, the dis-isopropyl either exract exhibits a deep purple colour which is more intense than that exhibited by a blank prepared in the same manner without the substance being examined pH Between 1.5 and 3.5, determined in a 3.0% w/V dispersion in water, Appendix 8.11.Arsenic Mix 2.0 g with 5 ml of sulphuric acid, add a few glass beads and digest at a temperature not exceeding 120" until charring begins Additional sulphuric acid may be added if necessary but the total volume of acid added should not exceed 1.0ml Add cautiously, dropwise. hydrogen peroxide solution (100 vol) allowing the reaction to subside and again heating between addition of Orops Discontinue heating rf foaming becomes excessive When the reaction has abated, heat cautiously rotating the Mask occasionally Maintain oxidising conditions at all times during the digestion by adding small quantities of the hydrogen peroxide solution whenever the mixture turns brown or darkens Continue the digestion until the organic matter has been destroyed, gradually raising the temperature until fumes of sulphur trioxide are copiously evolved and the solution becomes colourless or has only a light straw colour Cool, add cautiously 10 ml of water mix, and again evaporate till there is strong fuming, repeating this procedure to remove any trace of hydrogen peroxide. Cool, add cautiously 10 ml of water wash the sides of the flask with a few ml of water and dilute with water to 35 ml. The resulting solution complies with the limit test for arsenic, Appendix 3.9 (5 ppm)Heavy metals Not more than 40 ppm, determined on 0.5 g by Method B and using nitric acid Sp.in place of sulphuric acid Sp. to wet the sample Appendix 3 12 Acid value. Not less than 230,calculated with reference to the dried substance and determined in the following manner. Weigh accurately about 1g and suspend in a mixture of 50 ml of water and 30 ml of a 4.4% w/v solution of calcium acetate Shake vigorously, allow the mixture to stand for 1 hour, add phenolphthalein solution and titrate the liberated acetic acid with 0.1M sodium hydroxide Perform a blank determination and make any necessary correction Calculate the acid value from the expression 5.611 A/W in which A is the volume, in ml, of 0.1 M sodium hydroxide consumed and W is weight, in g. of the sample Ash Not more than 4.0%. determined on 0.5 g, Appendix 3.38 Loss on drying Not more than 15.0%, determined on 0.1 g by drying in an oven at 105* for 4 hours, Appendix 0.6 Micrabial limits 0.1 g is free from Eschenchia coli and 10.0 g is free from salmonellae. Appendix

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