EUROPEAN PHARMACOPOEIA 70 Sodium bromide Sodium calcium edetate EUROPEAN PHARMACOPOEIA 70
B. (ZD-bulenedioicacid Ifumaric acid),
mTu* ____.____
C. (2/ř51-2-5ulfaiivlbutaricdK.u acid (thiomalic add).
01/2008:0123 corrected 6.0
SODIUM BENZOATE
Natrii benzoas
C-HsNaOj M, 144.1
{532-32-1]
DEFINITION
Sodium benzenecarboxylate.
Content: MO per cent to 100.5 per cent (dried substance). CHARACTERS
Appearance: white or almost white, crystalline or granular powder or flakes, slightly hygroscopic. Solubility: freely soluble in water, sparingly soluble in ethanol (90 per cent V/V).
IDENTIFICATION
A It gives reactions (b) and |c) of benzoates (2.31)-B. It gives reaction (a) of sodium (2.3.1).
TESTS
Solution S- Dissolve 10 0 g in carbon dioxide-free water R and dilute to 100 ml. with the same solvent
Appearance of solution. Solution S is clear (2.2 1) and not more intensely coloured than reference solution Y„ (2.2.2, Method II). Acidity or alkalinity To 10 ml. of solution S add 10 ml. of carbon dioxide-free water R and 0.2 mL of phenolphthalein solution R. Not more than 0.2 mL of 0.J M sodium hydroxide or 0.1M hydrochloric acid is required to change the colour of the indicator.
Halogenated compounds: maximum 200 ppm tor ionised chlorine and maximum 300 ppm for total chlorine. All glassware used must be chloride-free and may be prepared by soaking overnight in a 500 g/L solution of nitric acid R, rinsed with water R and stored full of water R. It is recommended that glassware be reserved exclusively for this test.
Test solution To 20.0 mL of solution S add 5 mL of water R and dilute to 50.0 mL with ethanol (96 per cent) R. Determination of ionised chlorine
In three 25 mL volumetric flasks, prepare the following
solutions.
Solution (a). To 4.0 mL of the test solution add 3 mL of dilute sodium hydroxide solution R and 3 mL of ethanol (96 per cent) R. This solution is used to prepare solution A. Solution (b). To 3 mL of dilute sodium hydroxide solution R add 2 mL of water R and 5 mL of ethanol (96 per cent) R. Tins solution is used to prepare solution B. Solution (c). To 4.0 mL of chloride standard solution (8 ppm CI) R add 6 0 mL of water R This solution is used to prepare solution C.
In a fourth 25 mL volumetric flask, place 10 mL of water R. To each flask add 5 mL of ferric ammonium sulfate solution R5, mix and add dropwise and with swirling 2 mL of
nitric acid R and 5 mL of mercuric thiocyanate solution R. Shake. Dilute the contents of each flask to 25 0 mL with water R and allow the solutions to stand in a water-bath at 20 DC for 15 min. Measure at 460 nm in a 2 cm cell the absorbance (2.2.25) of solution A using solution B as the compensation liquid, and the absorbance of solution C using the solution obtained with 10 mL of water R as the compensation liquid The absorbance of solution A is not greater than that of solution C. Determination of total chlorine
Solution (a). To 10.0 mL of the test solution add 7.5 mL of dilute sodium hydroxide solution R and 0.125 g of nickel-aluminium alloy R and heat on a water-bath for 10 min. Allow to cool to room temperature, filter into a 25 mL volumetric flask and wash the filter with 3 quantities, each of 2 mL, of ethanol (96 per cent) R (a slight precipitate may form that disappears on acidification). Dilute the filtrate and washings to 25.0 mL with water R This solution is used to prepare solution A.
Solution (b). In the same manner, prepare a similar solution replacing the test solution by a mixture of 5 mL of ethanol (96 per cent) R and 5 mL of water R. This solution is used to prepare solution B. "
Solution (cl. To 6.0 mL of chloride standard solution (8 ppm Cl) R add 4.0 mL of water R. This solution is used to prepare solution C.
In four 25 mL volumetric flasks, place separately 10 mL of solution |u). 10 mL of solution (b), 10 mL of solution (c) and 10 mL of water R. To each flask add 5 mL of ferric ammonium sulfate solution R5, mix and add dropwise and with swirling 2 mL of nitric acid R and 5 mL of mercuric thiocyanate solution R. Shake. Dilute the contents of each flask to 25.0 mL with water R and allow the solutions to stand in a water-bath at 20 °C lor 15 min. Measure at 460 nm in a 2 cm cell the absorbance (2.2.25) of solution A using solution B as the compensation liquid, and the absorbance of solution C using the solution obtained with 10 mL of water R as the compensation liquid. The absorbance of solution A is not greater than that of solution C. Heavy metals [2.4.8): maximum 10 ppm.
2 0 g complies with test C. Prepare the reference solution using 2 mL of lead standard solution (10 ppm Pb) R. Loss on drying {2.2.32): maximum 2.0 per cent, determined on 1.00 g by drying in an oven at 105 aC.
ASSAY
Dissolve 0 250 g in 20 ml. of anhydrous acetic acid R, heating to 50 C if necessary. Cool. Using 0.05 mL of naphtholbenzein solution R as indicator, titrate with 0. J Mperchloric acid until a green colour is obtained.
1 mL of 0.1 M perchloric acid is equivalent to 14.41 mg of CHsNaOj.
SODIUM BROMIDE
Natrii bromidum
NaBr M, 102.9
17647-15-6]
DEFINITION
Content: 98.0 per cent to 100.5 per cent (dried substance). CHARACTERS
Appearance: white or almost white, granular powder or small, colourless, transparent or opaque crystals, slightly hygroscopic. Solubility: freely Soluble in water, soluble in alcohol.
01/2008:0190	•&		E o
corrected 6.0			oj
	So		WS
	o		T? D-
	2		
IDENTIFICATION
A. It gives reaction (a) of bromides [23 1) ft Solution S {see Tests) gives the reactions of sodium (2.3.1).
TESTS
Solution S. Dissolve 10.0 g in carbon dioxide-free water R prepared from distilled water R and dilute to 100 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 10 mL of solution S add 0.1 ml of
bromothymol blue solution Rl. Not more than 0.5 mL of 0 01 M hydrochloric acid or 0.01 M sodium hydroxide is required to change the colour of the indicator Bromates To 10 mL of solution S add 1 mL of starch solution R. 0.1 mL of a 100 g/L solution of potassium iodide R and 0.25 mL of 0.5 M sulfuric acid And allow to stand protected from light for 5 min. No blue or violet colour develops. Chlorides: maximum 0 6 per cent
In a conical flask, dissolve 1 000 g in 20 mL of dilute nitric acid R. Add 5 mL of strong hydrogen peroxide solution R and heat on a water-bath until the solution is completely decolourised. Wash down the sides of the flask with a little water R and heat on a water-bath for 15 nun Allow to cool, dilute to 50 mL with water R and add 5.0 mL of 0.1 M silver nitrate and 1 mL of dibutyl phthalate R. Shake and titrate with 0.1 M ammonium thiocyanate. using 5 mL of ferric ammonium sulfate solution R2 as indicator. Not more than 1.7 mL of 0.1 M silver nitrate is used. Note the volume of 0.1 M silver nitrate used (see Assay). Carry out a blank test Iodides To 5 mL of solution S add 0.15 mL of ferric chloride solution Rl and 2 ml. of methylene chloride R. Shake and allow to separate. The lower layer is colourless {2.2.2, Method I). Sulfates (2.4.13): maximum 100 ppm. 15 mL of solution S complies with the limit test for sulfates. Iron (2 4 9): maximum 20 ppm
5 mL of solution S diluted to 10 mL with water R complies with the limit test for iron.
Magnesium and alkaline-earth metals (2-4 7): maximum 200 ppm. calculated as Ca.
10.0 g complies with the limit test for magnesium and alkaline-earth metals. The volume of 0.01 M sodium edetate used does not exceed 5.0 mL.
Heavy metals (2.4.8): rnaximurn 10 ppm.
12 mL of solution S complies with limit test A- Prepare the
standard using lead standard solution (1 ppm Pb) R.
Loss on drying (2.232): maximum 3.0 per cent, determined on 1.000 g by drying in an oven at 105 °C for 3 h
ASSAY
Dissolve 2.000 g in water R and dilute to 100.0 mL with the same solvent To 10.0 mL of the solution add 50 mL of water R, 5 mL of dilute nitric add R. 25.0 mL of 0.1 M silver nitrate and 2 mL of dibutyl phthalate R. Shake. Titrate with 0.1 M ammonium thiocyanate. using 2 mL of ferric ammonium sulfate solution R2 as indicator and shaking vigorously towards the end-point
1 mL of 0.1 M silver nitrate is equivalent to 10.29 mg of NaBr ulate the percentage content of NaBr from the expression:
a -2-902 6
percentage content nf \ahi and NaCI obtained in the assay and calculated as NaBr?---^^ percentage content of Cl in the test for chlorides.
STORAGE
In an airtight container.
01/2006:0231
SODIUM CALCIUM EDETATE
Natrii calcii edetas
if, 374.3 (anhydrous substancel
Cj.HuCaN^NajOgAHjO (62-33-91
DEFINITION
Disodium ((ethylenedinitrilo)tetraacetato]calciatet2- J. Content; 98.0 per cent to 102.0 per cent (anhydrous substance). It contains a variable amount of water of crystallisation.
CHARACTERS
Appearance: white or almost white, hygroscopic powder Solubility- freely soluble in water, practically insoluble in ethanol (96 per cent).
IDENTIFICATION
First identification: A C, D. Second identification: B, C, D.
A. Infrared absorption spectrophotometry (2.2.24). Preparation: discs.
Comparison: sodium calcium edetate CRS.
B. Dissolve 2 £ in 10 mL of water R. add 6 mL of lead nitrate solution R, shake and add 3 mL of potassium iodide solution R No yellow precipitate is formed. Make alkaline to red litmus paper R by the addition of dilute ammonia R2 and add 3 mL of ammonium oxalate solution R. A white precipitate is formed.
C Ignite The residue gives reaction (b| of calcium {2.3.1).
D. Dissolve 0.5 g in 10 ml of water R and add 10 mL of potassium pyroantimonate solution R A white, crystalline precipitate is formed The formation of the precipitate is accelerated by rubbing the wall of the tube with a glass rod.
TESTS
Solution S. Dissolve 5.0 g in water R and dilute to 100 mL with the same solvent
Appearance of solution. Solution S is clear {2.2.1) and colourless (2.2.2, Method II). pll (2.2.3): 6.5 to S.O.
Dissolve 5.0 g in carbon dioxide-free water R and dilute to 25 mL with the same solvent
Impurity A. Liquid chromatography (2.2.29). Carry out the test protected from light.
Solvent mixture. Dissolve 10.0 g of ferric sulfate pentahydrate R in 20 mL of 0.5M sulfuric acid and add 780 mL of water R. Adjust to pH 2.0 with / M sodium hydroxide and dilute to 1000 mL with water R.
Test solution. Dissolve 0.100 g of the substance to be examined in the solvent mixture and dilute to 25.0 mL with the solvent mixture.
Reference solution. Dissolve 40 0 mg of nitrilotriacetic acid R (impurity A) in the solvent mixture and dilute to 100.0 mL with the solvent mixture. To 10 mL of this solution add 0.1 mLof the test solution and dilute to 100.0 mL with the solvent mixture. Column:
- size I - 0.10 m, 0 - 4.6 mm:
General Notices (1) apply to alt monographs and other texts
2915
2916
See the information section on general monographs (cover pages)