Sodium benzoate EUROPEAN PHARMACOPOEIA 6.

Reference solution (d). To 7.5 ml of reference solution (a) CHARACTERS

add 2.5 ml of water R. Appearance : white or almost white, crystalline or granular
Blank solution. 10 ml of water R. powder or flakes, slightly hygroscopic.
To the test solution, reference solutions (b), (c) and (d) Solubility : freely soluble in water, sparingly soluble in
and the blank solution, add 2.5 ml of a freshly prepared ethanol (90 per cent V/V).
235 g/l solution of sodium hydroxide R and mix. Add
dropwise in 0.2 ml increments a 38.0 g/l solution of cupric IDENTIFICATION
chloride R, shaking vigorously after each addition, until the A. It gives reactions (b) and (c) of benzoates (2.3.1).
solutions become slightly turbid. Then add 0.2 ml of the B. It gives reaction (a) of sodium (2.3.1).
38.0 g/l solution of cupric chloride R. Stopper and shake
vigorously for 1 min. Dilute to 25.0 ml with water R and TESTS
mix. Centrifuge for 2 min. Measure the absorbance (2.2.25) Solution S. Dissolve 10.0 g in carbon dioxide-free water R
of the supernatant solution of a 1 cm layer at 635 nm. and dilute to 100 ml with the same solvent.
Use the solution prepared from the blank solution as the Appearance of solution. Solution S is clear (2.2.1) and not
compensation liquid. Draw a calibration curve and calculate more intensely coloured than reference solution Y6 (2.2.2,
the content of glycerol in the sample. Method II).
Loss on drying (2.2.32) : maximum 2.0 per cent, determined Acidity or alkalinity. To 10 ml of solution S add 10 ml of
on 1.000 g by drying over diphosphorus pentoxide R at a carbon dioxide-free water R and 0.2 ml of phenolphthalein
pressure not exceeding 0.7 kPa for 24 h. solution R. Not more than 0.2 ml of 0.1 M sodium hydroxide
ASSAY or 0.1 M hydrochloric acid is required to change the colour
of the indicator.
Gold. Heat 0.2 g with 10 ml of sulphuric acid R and continue
to boil gently until a clear, pale yellow liquid is produced. Halogenated compounds : maximum 200 ppm for ionised
Cool, add about 1 ml of nitric acid R dropwise and boil for chlorine and maximum 300 ppm for total chlorine.
1 h. Cool, dilute to 70 ml with water R, boil for 5 min and All glassware used must be chloride-free and may be
filter. Wash the residue of gold with water R at 60 °C. Dry prepared by soaking overnight in a 500 g/l solution of
and ignite at a temperature of at least 600 °C for 3 h. Weigh nitric acid R, rinsed with water R and stored full of water R.
the residue and calculate the percentage content of Au. It is recommended that glassware be reserved exclusively
for this test.
Sodium. Evaporate to dryness the filtrate and washings
obtained in the assay for gold, moisten with sulphuric acid R Test solution. To 20.0 ml of solution S add 5 ml of water R
and ignite at 600 ± 50 °C for 3 h. and dilute to 50.0 ml with ethanol (96 per cent) R.
1.000 g of residue is equivalent to 0.324 g of Na. Determination of ionised chlorine
In three 25 ml volumetric flasks, prepare the following
STORAGE solutions.
In an airtight container. Solution (a). To 4.0 ml of the test solution add 3 ml
of dilute sodium hydroxide solution R and 3 ml of
IMPURITIES ethanol (96 per cent) R. This solution is used to prepare
Specified impurities : A, B, C. solution A.
A. maleic acid, 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. This solution is used to prepare
solution B.
B. (2E)-butenedioic acid (fumaric acid), Solution (c). To 4.0 ml of chloride standard solution
(8 ppm Cl) 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 sulphate
C. (2RS)-2-sulphanylbutanedioic acid (thiomalic acid). 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
01/2008:0123 25.0 ml with water R and allow the solutions to stand in
corrected 6.0 a water-bath at 20 °C for 15 min. Measure at 460 nm in
a 2 cm cell the absorbance (2.2.25) of solution A using
SODIUM BENZOATE solution B as the compensation liquid, and the absorbance
of solution C using the solution obtained with 10 ml of
Natrii benzoas 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
C7H5NaO2 Mr 144.1 for 10 min. Allow to cool to room temperature, filter
[532-32-1] into a 25 ml volumetric flask and wash the filter with
3 quantities, each of 2 ml, of ethanol (96 per cent) R
DEFINITION
(a slight precipitate may form that disappears on
Sodium benzenecarboxylate. acidification). Dilute the filtrate and washings to 25.0 ml
Content : 99.0 per cent to 100.5 per cent (dried substance). with water R. This solution is used to prepare solution A.

2890 See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 6.0 Sodium bromide

Solution (b). In the same manner, prepare a similar Appearance of solution. Solution S is clear (2.2.1) and
solution replacing the test solution by a mixture of 5 ml colourless (2.2.2, Method II).
of ethanol (96 per cent) R and 5 ml of water R. This Acidity or alkalinity. To 10 ml of solution S add 0.1 ml of
solution is used to prepare solution B. bromothymol blue solution R1. Not more than 0.5 ml of
Solution (c). To 6.0 ml of chloride standard solution 0.01 M hydrochloric acid or 0.01 M sodium hydroxide is
(8 ppm Cl) R add 4.0 ml of water R. This solution is used required to change the colour of the indicator.
to prepare solution C.
Bromates. To 10 ml of solution S add 1 ml of starch
In four 25 ml volumetric flasks, place separately 10 ml of solution R, 0.1 ml of a 100 g/l solution of potassium
solution (a), 10 ml of solution (b), 10 ml of solution (c) iodide R and 0.25 ml of 0.5 M sulphuric acid and allow to
and 10 ml of water R. To each flask add 5 ml of ferric stand protected from light for 5 min. No blue or violet colour
ammonium sulphate solution R5, mix and add dropwise develops.
and with swirling 2 ml of nitric acid R and 5 ml of
mercuric thiocyanate solution R. Shake. Dilute the Chlorides : maximum 0.6 per cent.
contents of each flask to 25.0 ml with water R and allow In a conical flask, dissolve 1.000 g in 20 ml of dilute nitric
the solutions to stand in a water-bath at 20 °C for 15 min. acid R. Add 5 ml of strong hydrogen peroxide solution R
Measure at 460 nm in a 2 cm cell the absorbance (2.2.25) and heat on a water-bath until the solution is completely
of solution A using solution B as the compensation liquid, decolourised. Wash down the sides of the flask with a little
and the absorbance of solution C using the solution water R and heat on a water-bath for 15 min. Allow to cool,
obtained with 10 ml of water R as the compensation dilute to 50 ml with water R and add 5.0 ml of 0.1 M silver
liquid. The absorbance of solution A is not greater than nitrate and 1 ml of dibutyl phthalate R. Shake and titrate
that of solution C. with 0.1 M ammonium thiocyanate, using 5 ml of ferric
ammonium sulphate solution R2 as indicator. Not more
Heavy metals (2.4.8) : maximum 10 ppm.
than 1.7 ml of 0.1 M silver nitrate is used. Note the volume of
2.0 g complies with test C. Prepare the reference solution 0.1 M silver nitrate used (see Assay). Carry out a blank test.
using 2 ml of lead standard solution (10 ppm Pb) R.
Iodides. To 5 ml of solution S add 0.15 ml of ferric chloride
Loss on drying (2.2.32) : maximum 2.0 per cent, determined solution R1 and 2 ml of methylene chloride R. Shake and
on 1.00 g by drying in an oven at 105 °C. allow to separate. The lower layer is colourless (2.2.2,
Method I).
ASSAY
Sulphates (2.4.13) : maximum 100 ppm.
Dissolve 0.250 g in 20 ml of anhydrous acetic acid R,
heating to 50 °C if necessary. Cool. Using 0.05 ml of 15 ml of solution S complies with the limit test for sulphates.
naphtholbenzein solution R as indicator, titrate with 0.1 M Iron (2.4.9) : maximum 20 ppm.
perchloric acid until a green colour is obtained.
5 ml of solution S diluted to 10 ml with water R complies
1 ml of 0.1 M perchloric acid is equivalent to 14.41 mg with the limit test for iron.
of C7H5NaO2.
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
01/2008:0190 alkaline-earth metals. The volume of 0.01 M sodium edetate
corrected 6.0 used does not exceed 5.0 ml.
Heavy metals (2.4.8) : maximum 10 ppm.
SODIUM BROMIDE 12 ml of solution S complies with limit test A. Prepare the
standard using lead standard solution (1 ppm Pb) R.
Natrii bromidum Loss on drying (2.2.32) : maximum 3.0 per cent, determined
on 1.000 g by drying in an oven at 105 °C for 3 h.
NaBr Mr 102.9
ASSAY
[7647-15-6]
Dissolve 2.000 g in water R and dilute to 100.0 ml with
DEFINITION the same solvent. To 10.0 ml of the solution add 50 ml of
Content : 98.0 per cent to 100.5 per cent (dried substance). water R, 5 ml of dilute nitric acid R, 25.0 ml of 0.1 M silver
nitrate and 2 ml of dibutyl phthalate R. Shake. Titrate
CHARACTERS with 0.1 M ammonium thiocyanate, using 2 ml of ferric
Appearance : white or almost white, granular powder or ammonium sulphate solution R2 as indicator and shaking
small, colourless, transparent or opaque crystals, slightly vigorously towards the end-point.
hygroscopic. 1 ml of 0.1 M silver nitrate is equivalent to 10.29 mg of NaBr.
Solubility : freely soluble in water, soluble in alcohol. Calculate the percentage content of NaBr from the
expression :
IDENTIFICATION
A. It gives reaction (a) of bromides (2.3.1).
B. Solution S (see Tests) gives the reactions of sodium a = percentage content of NaBr and NaCl obtained in
(2.3.1). the assay and calculated as NaBr,
TESTS b = percentage content of Cl in the test for chlorides.
Solution S. Dissolve 10.0 g in carbon dioxide-free water R
prepared from distilled water R and dilute to 100 ml with STORAGE
the same solvent. In an airtight container.

General Notices (1) apply to all monographs and other texts 2891