You are on page 1of 2

Silver nitrate


The chromatographic procedure may be carried out using : a non-metallic column 0.25 m long and 4.6 mm in internal diameter packed with a suitable anion-exchange resin (30 m to 50 m ), as mobile phase at a flow rate of 1.2 ml/min a solution prepared as follows : dissolve 0.508 g of sodium carbonate R and 0.05 g of sodium hydrogen carbonate R in water R and dilute to 1000 ml with the same solvent, a conductivity detector, a loop injector. Inject 25 l of the test solution and 25 l of the reference solution. When the chromatograms are recorded in the prescribed conditions, the retention times are : sulphate about 8 min and chloride about 4 min. In the chromatogram obtained with the test solution the area of any peak corresponding to sulphate is not greater than that of the corresponding peak in the chromatogram obtained with the reference solution (4.0 per cent calculated as sodium sulphate). Iron (2.4.9). Dilute 2 ml of solution S to 40 ml with water R. 10 ml of the solution complies with the limit test for iron (400 ppm). Heavy metals (2.4.8). To 20 ml of solution S, add 50 mg of hydroxylamine hydrochloride R and 1 ml of concentrated ammonia R. Adjust to pH 3.5 by adding dilute ammonia R2, monitoring the pH potentiometrically. Dilute to 25 ml with water R. 12 ml of the solution complies with limit test A for heavy metals (25 ppm). Prepare the standard using lead standard solution (1 ppm Pb) R. Loss on ignition. Not more than 25.0 per cent, determined on 0.200 g in a platinum crucible by heating at 100 C to 105 C for 1 h and then at 1000 C for 2 h. ASSAY To the residue obtained in the test for loss on ignition add 0.2 ml of sulphuric acid R and a quantity of alcohol R sufficient to moisten the residue completely. Add 6 ml of hydrofluoric acid R and evaporate to dryness at 95 C to 105 C, taking care to avoid loss from sputtering. Wash the inside of the crucible with 6 ml of hydrofluoric acid R and evaporate to dryness again. Ignite at 900 C, allow to cool in a desiccator and weigh. The difference between the mass of the final residue and that of the mass obtained in the test for loss on ignition corresponds to the mass of SiO2 in the test sample. 01/2005:0009

TESTS Solution S. Dissolve 2.0 g in water R and dilute to 50 ml with the same solvent. Appearance of solution. Solution S is clear (2.2.1) and colourless (2.2.2, Method II). Acidity or alkalinity. To 2 ml of solution S add 0.1 ml of bromocresol green solution R. The solution is blue. To 2 ml of solution S add 0.1 ml of phenol red solution R. The solution is yellow. Foreign salts. To 30 ml of solution S, add 7.5 ml of dilute hydrochloric acid R, shake vigorously, heat for 5 min on a water-bath and filter. Evaporate 20 ml of the filtrate to dryness on a water-bath and dry at 100-105 C. The residue weighs not more than 2 mg (0.3 per cent). Aluminium, lead, copper and bismuth. Dissolve 1.0 g in a mixture of 4 ml of concentrated ammonia R and 6 ml of water R. The solution is clear (2.2.1) and colourless (2.2.2, Method II). ASSAY Dissolve 0.300 g in 50 ml of water R and add 2 ml of dilute nitric acid R and 2 ml of ferric ammonium sulphate solution R2. Titrate with 0.1 M ammonium thiocyanate until a reddish-yellow colour is obtained. 1 ml of 0.1 M ammonium thiocyanate is equivalent to 16.99 mg of AgNO3. STORAGE Store in a non-metallic container, protected from light. 01/2005:1470

SIMETICONE Simeticonum
DEFINITION Simeticone is prepared by incorporation of 4 per cent to 7 per cent silica into poly(dimethylsiloxane) with a degree of polymerisation between 20 and 400. Simeticone contains 90.5 per cent to 99.0 per cent of poly(dimethylsiloxane). PRODUCTION Poly(dimethylsiloxane) is obtained by hydrolysis and polycondensation of dichlorodimethylsilane and chlorotrimethylsilane and the silica is modified at the surface by incorporation of methylsilyl groups. CHARACTERS A viscous, greyish-white, opalescent liquid, practically insoluble in water, very slightly soluble to practically insoluble in ethanol, practically insoluble in methanol, partly miscible with ethyl acetate, with methylene chloride, with methyl ethyl ketone and with toluene. IDENTIFICATION A. Examine by infrared absorption spectrophotometry (2.2.24). Absorption maxima are observed at 2964 cm 1, 2905 cm 1, 1412 cm 1, 1260 cm 1 and 1020 cm 1. Examine the substances as thin films between sodium chloride R plates. B. Heat 0.5 g in a test-tube over a small flame until white fumes begin to appear. Invert the tube over a second tube containing 1 ml of a 1 g/l solution of chromotropic acid, sodium salt R in sulphuric acid R so that the fumes reach the solution. Shake the second tube for about 10 s and heat on a water-bath for 5 min. The solution is violet.

SILVER NITRATE Argenti nitras

AgNO3 Mr 169.9 DEFINITION Silver nitrate contains not less than 99.0 per cent and not more than the equivalent of 100.5 per cent of AgNO3. CHARACTERS A white, crystalline powder or transparent, colourless crystals, very soluble in water, soluble in alcohol. IDENTIFICATION A. 10 mg gives the reaction of nitrates (2.3.1). B. 10 mg gives the reaction of silver (2.3.1). 2412

See the information section on general monographs (cover pages)



Dimeticone Test solution. Place about 50 mg (E) in a screw-capped 125 ml cylindrical tube, add 25.0 ml of toluene R, swirl TESTS manually to disperse and add 50 ml of dilute hydrochloric Acidity. To 2.0 g add 25 ml of a mixture of equal volumes of acid R, close the tube and place on a vortex mixer ; shake for 5 min. Transfer the contents of the tube to a separating ethanol R and ether R previously neutralised to 0.2 ml of funnel, allow to settle and transfer 5 ml of the upper layer bromothymol blue solution R1, and shake. Not more than 3.0 ml of 0.01 M sodium hydroxide is required to change the to a screw-capped test tube containing 0.5 g of anhydrous sodium sulphate R. Cap and shake vigorously manually. colour of the solution to blue. Centrifuge to obtain a clear test solution. Defoaming activity Reference solution. Introduce about 0.20 g of Foaming solution. Dissolve 5.0 g of docusate sodium R in dimeticone CRS in 100.0 ml of toluene R. Prepare the 1 litre of water R (warm to 50 C if necessary). reference solution in the same way as for the test solution, Defoaming solution. To 50 ml of methyl ethyl ketone R using 25.0 ml of the dimeticone solution obtained above. add 0.250 g of simeticone, warm to not more than 50 C Prepare a blank by shaking 10 ml of toluene R with 1 g of with shaking. anhydrous sodium sulphate R. Centrifuge the resulting suspension. Into a 250 ml cylindrical tube about 5 cm in diameter introduce 100 ml of foaming solution and 1 ml of defoaming Record the infrared absorption spectra for the test solution and the reference solution in 0.5 mm cells, from 1330 cm 1 solution. Close tightly and fix the tube on a suitable to 1180 cm 1, and determine the absorbance of the band at oscillating shaker that complies with the following 1260 cm 1 (2.2.24). conditions : Calculate the percentage content of dimeticone using the 250 to 300 oscillations per minute, expression : angle of oscillation of about 10, oscillation radius of about 10 cm. Shake for 10 s and record the time between the end of the shaking and the instant the first portion of foam-free liquid AM = absorbance of the test solution, surface appears. AE = absorbance of the reference solution, This duration does not exceed 15 s. C = concentration of the reference solution, in Mineral oils. Place 2.0 g in a test-tube and examine in milligrams per millilitre, ultraviolet light at 365 nm. The fluorescence is not more intense than that of a solution containing 0.1 ppm of quinine E = mass of the substance to be examined, in sulphate R in 0.005 M sulphuric acid examined in the same milligrams. conditions. Phenylated compounds. Dissolve 5.0 g with shaking in 10.0 ml of cyclohexane R. Determine the absorbance of 01/2005:1563 the solution between 200 nm and 350 nm (2.2.25) using cyclohexane R as the compensation liquid. The corrected SIMVASTATIN absorbance (absorbance measured at the maximum between 250 nm and 270 nm minus the absorbance measured at 300 nm) is not greater than 0.2. Simvastatinum Heavy metals. Mix 1.0 g with methylene chloride R and dilute to 20 ml with the same solvent. Add 1.0 ml of a freshly prepared 0.02 g/l solution of dithizone R in methylene chloride R, 0.5 ml of water R and 0.5 ml of a mixture of 1 volume of dilute ammonia R2 and 9 volumes of a 2 g/l solution of hydroxylamine hydrochloride R. At the same time, prepare a standard as follows : to 20 ml of methylene chloride R add 1.0 ml of a freshly prepared 0.02 g/l solution of dithizone R in methylene chloride R, 0.5 ml of lead standard solution (10 ppm Pb) R and 0.5 ml of a mixture of 1 volume of dilute ammonia R2 and 9 volumes of a 2 g/l solution of hydroxylamine hydrochloride R. Immediately C25H38O5 Mr 418.6 shake each solution vigorously for 1 min. Any red colour in the test solution is not more intense than that in the DEFINITION standard (5 ppm). Simvastatin contains not less than 97.0 per cent and not Volatile matter. Not more than 1.0 per cent, determined on more than the equivalent of 102.0 per cent of (1S,3R,7S, 1.00 g by heating in an oven at 150 C for 2 h. Carry out the 8S,8aR)-8-[2-[(2R,4R)-4-hydroxy-6-oxotetrahydro-2H-pyran-2test using a dish 60 mm in diameter and 10 mm deep. yl]ethyl]-3,7-dimethyl-1,2,3,7,8,8a-hexahydronaphthalen-1-yl 2,2-dimethylbutanoate, calculated with reference to the dried ASSAY substance. A suitable antioxidant may be added. Silica. Not more than 7 per cent, determined on not less than 20.0 mg. Heat the substance to be examined to 800 C CHARACTERS A white or almost white, crystalline powder, practically increasing the temperature by 20 C/min under a current insoluble in water, very soluble in methylene chloride, freely of nitrogen R at a flow rate of 200 ml/min and weigh the soluble in alcohol. residue (silica). C. The residue obtained in the test for silica under Assay, gives the reaction of silicates (2.3.1). General Notices (1) apply to all monographs and other texts 2413