4.2.2. Volumetric solutions EUROPEAN PHARMACOPOEIA 9.

Potassium bromate. KBrO3. (Mr 167.0). 2000300. Standardisation. To 25.0 mL of acetic acid add 0.5 mL of
[7758-01-2]. phenolphthalein solution R and titrate with 0.1 M sodium
Crystallise potassium bromate R from boiling water R. Collect hydroxide.
the crystals and dry to constant mass at 180 °C. 0.1 M Ammonium and cerium nitrate. 3000100.
Potassium hydrogen phthalate. C8H5KO4. (Mr 204.2). Shake for 2 min a solution containing 56 mL of sulfuric acid R
2000400. [877-24-7]. and 54.82 g of ammonium and cerium nitrate R, add five
Recrystallise potassium hydrogen phthalate R from boiling successive quantities, each of 100 mL, of water R, shaking after
water R, collect the crystals at a temperature above 35 °C and each addition. Dilute the clear solution to 1000.0 mL with
dry to constant mass at 110 °C. water R. Standardise the solution after 10 days.
Standardisation. To 25.0 mL of the ammonium and cerium
Sodium carbonate. Na2CO3 . (Mr 106.0). 2000500. nitrate solution add 2.0 g of potassium iodide R and 150 mL
[497-19-8]. of water R. Titrate immediately with 0.1 M sodium thiosulfate,
Filter at room temperature a saturated solution of sodium using 1 mL of starch solution R as indicator.
carbonate R. Introduce slowly into the filtrate a stream of Storage : protected from light.
carbon dioxide R with constant cooling and stirring. After
about 2 h, collect the precipitate on a sintered-glass filter 0.01 M Ammonium and cerium nitrate. 3000200.
(2.1.2). Wash the filter with iced water R containing carbon To 100.0 mL of 0.1 M ammonium and cerium nitrate add,
dioxide. After drying at 100 °C to 105 °C, heat to constant with cooling, 30 mL of sulfuric acid R and dilute to 1000.0 mL
mass at 270-300 °C, stirring from time to time. with water R.

Sodium chloride. NaCl. (Mr 58.44). 2000600. [7647-14-5]. 0.1 M Ammonium and cerium sulfate. 3000300.
To 1 volume of the saturated sodium chloride solution R add Dissolve 65.0 g of ammonium and cerium sulfate R in a
2 volumes of hydrochloric acid R. Collect the crystals formed mixture of 500 mL of water R and 30 mL of sulfuric acid R.
and wash with hydrochloric acid R1. Remove the hydrochloric Allow to cool and dilute to 1000.0 mL with water R.
acid by heating on a water-bath and dry the crystals to Standardisation. To 25.0 mL of the ammonium and cerium
constant mass at 300 °C. sulfate solution add 2.0 g of potassium iodide R and 150 mL
of water R. Titrate immediately with 0.1 M sodium thiosulfate,
Sulfanilic acid. C6H7NO3S. (Mr 173.2). 2000700. [121-57-3]. using 1 mL of starch solution R as indicator.
Recrystallise sulfanilic acid R from boiling water R. Filter and 0.01 M Ammonium and cerium sulfate. 3000400.
dry to constant mass at 100-105 °C.
To 100.0 mL of 0.1 M ammonium and cerium sulfate add,
Zinc. Zn. (Mr 65.4). 2000800. [7440-66-6]. with cooling, 30 mL of sulfuric acid R and dilute to 1000.0 mL
Content : minimum 99.9 per cent. with water R.
0.1 M Ammonium thiocyanate. 3000500.
Dissolve 7.612 g of ammonium thiocyanate R in water R and
04/2016:40202 dilute to 1000.0 mL with the same solvent.
Standardisation. To 20.0 mL of 0.1 M silver nitrate add 25 mL
of water R, 2 mL of dilute nitric acid R and 2 mL of ferric
ammonium sulfate solution R2. Titrate with the ammonium
thiocyanate solution until a reddish-yellow colour is obtained.
4.2.2. VOLUMETRIC SOLUTIONS
0.1 M Barium chloride. 3000600.
Volumetric solutions are prepared according to the usual Dissolve 24.4 g of barium chloride R in water R and dilute to
chemical analytical methods. The accuracy of the apparatus 1000.0 mL with the same solvent.
used is verified to ensure that it is appropriate for the intended Standardisation. To 10.0 mL of the barium chloride solution
use. add 60 mL of water R, 3 mL of concentrated ammonia R and
The concentration of volumetric solutions is indicated in terms 0.5-1 mg of phthalein purple R. Titrate with 0.1 M sodium
of molarity. Molarity expresses, as the number of moles, the edetate. When the solution begins to decolorise, add 50 mL
amount of substance dissolved in 1 L of solution. A solution of ethanol (96 per cent) R and continue the titration until the
which contains x moles of substance per litre is said to be x M. blue-violet colour disappears.
Volumetric solutions do not differ from the prescribed
0.05 M Barium perchlorate. 3000700.
strength by more than 10 per cent. The molarity of the
volumetric solutions is determined by an appropriate number Dissolve 15.8 g of barium hydroxide R in a mixture of 7.5 mL
of titrations. The repeatability does not exceed 0.2 per cent of perchloric acid R and 75 mL of water R, adjust the solution
(relative standard deviation). to pH 3 by adding perchloric acid R and filter if necessary. Add
150 mL of ethanol (96 per cent) R and dilute to 250 mL with
Volumetric solutions are standardised by the methods water R. Dilute to 1000.0 mL with buffer solution pH 3.7 R.
described below. When a volumetric solution is to be used
in an assay in which the end-point is determined by an Standardisation. To 5.0 mL of 0.05 M sulfuric acid add 5 mL
electrochemical process (for example, amperometry or of water R, 50 mL of buffer solution pH 3.7 R and 0.5 mL of
potentiometry) the solution is standardised by the same alizarin S solution R. Titrate with the barium perchlorate
method. The composition of the medium in which a solution until an orange-red colour appears. Standardise
volumetric solution is standardised should be the same as that immediately before use.
in which it is to be used. 0.025 M Barium perchlorate. 3009600.
Solutions more dilute than those described are obtained Dilute 500.0 mL of 0.05 M barium perchlorate to 1000.0 mL
by dilution with carbon dioxide-free water R of the with buffer solution pH 3.7 R.
least-concentrated solution that describes a standardisation.
The correction factors of these solutions are the same as those 0.005 M Barium perchlorate. 3010200.
from which the dilutions were prepared. Dilute 10.0 mL of 0.05 M barium perchlorate to 100.0 mL with
a buffer solution prepared as follows: to 15.0 mL of acetic
0.1 M Acetic acid. 3008900. acid R add 60.0 mL of 2-propanol R. Adjust to pH 3.7 with
Dilute 6.0 g of glacial acetic acid R to 1000.0 mL with water R. ammonia R and dilute to 100.0 mL with water R.

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

EUROPEAN PHARMACOPOEIA 9.0 4.2.2. Volumetric solutions

0.004 M Benzethonium chloride. 3000900. 1 mL of 1 M hydrochloric acid is equivalent to 53.00 mg of

Dissolve in water R 1.792 g of benzethonium chloride R, Na2CO3.
previously dried to constant mass at 100-105 °C, and dilute to 0.1 M Hydrochloric acid. 3002100.
1000.0 mL with the same solvent.
Dilute 100.0 mL of 1 M hydrochloric acid to 1000.0 mL with
Standardisation. Calculate the molarity of the solution from water R.
the content of C27H42ClNO2 in the dried benzethonium
chloride determined as follows. Dissolve 0.350 g of the dried Standardisation. Carry out the titration described for 1 M
substance in 30 mL of anhydrous acetic acid R and add 6 mL hydrochloric acid using 0.100 g of sodium carbonate RV
of mercuric acetate solution R. Titrate with 0.1 M perchloric dissolved in 20 mL of water R.
acid, using 0.05 mL of crystal violet solution R as indicator. 1 mL of 0.1 M hydrochloric acid is equivalent to 5.30 mg of
Carry out a blank titration. Na2CO3.
1 mL of 0.1 M perchloric acid is equivalent to 44.81 mg of 0.1 M Hydrochloric acid, alcoholic. 3008800.
C27H42ClNO2. Dilute 9.0 mL of hydrochloric acid R to 1000.0 mL with
0.01 M Bismuth nitrate. 3010000. aldehyde-free alcohol R.
Dissolve 4.86 g of bismuth nitrate pentahydrate R in 60 mL of 0.5 M Iodine. 3009400.
dilute nitric acid R and dilute to 1000.0 mL with water R. Dissolve 127 g of iodine R and 200 g of potassium iodide R in
Standardisation. To 25.0 mL of the bismuth nitrate solution, water R and dilute to 1000.0 mL with the same solvent.
add 50 mL of water R and titrate with 0.01 M sodium edetate Standardisation. To 2.0 mL of the iodine solution add 1 mL of
using 0.05 mL of a 1 g/L solution of xylenol orange R as dilute acetic acid R and 50 mL of water R. Titrate with 0.1 M
indicator. sodium thiosulfate, using starch solution R as indicator.
0.0167 M Bromide-bromate. 3001000. Storage : protected from light.
Dissolve 2.7835 g of potassium bromate RV and 13 g of 0.05 M Iodine. 3002700.
potassium bromide R in water R and dilute to 1000.0 mL with Dissolve 12.7 g of iodine R and 20 g of potassium iodide R in
the same solvent. water R and dilute to 1000.0 mL with the same solvent.
0.1 M Cerium sulfate. 3001100. Standardisation. To 20.0 mL of the iodine solution add 1 mL
Dissolve 40.4 g of cerium sulfate R in a mixture of 500 mL of of dilute acetic acid R and 30 mL of water R. Titrate with 0.1 M
water R and 50 mL of sulfuric acid R. Allow to cool and dilute sodium thiosulfate, using starch solution R as indicator.
to 1000.0 mL with water R. Storage : protected from light.
Standardisation. To 20.0 mL of the cerium sulfate solution, 0.01 M Iodine. 3002900.
add 1.6 g of potassium iodide R, 100 mL of water R and 40 mL Add 0.3 g of potassium iodide R to 20.0 mL of 0.05 M iodine
of dilute sulfuric acid R. Titrate immediately with 0.1 M sodium and dilute to 100.0 mL with water R.
thiosulfate using 0.8 mL of starch solution R as indicator.
0.1 M Lanthanum nitrate. 3010100.
0.02 M Copper sulfate. 3001200.
Dissolve 43.30 g of lanthanum nitrate R in water R and dilute
Dissolve 5.0 g of copper sulfate pentahydrate R in water R and to 1000.0 mL with the same solvent.
dilute to 1000.0 mL with the same solvent.
Standardisation. To 20 mL of the lanthanum nitrate solution,
Standardisation. To 20.0 mL of the copper sulfate solution add 15 mL of water R and 25 mL of 0.1 M sodium edetate.
add 2 g of sodium acetate R and 0.1 mL of pyridylazonaphthol Add about 50 mg of xylenol orange triturate R and about 2 g
solution R. Titrate with 0.02 M sodium edetate until the colour of hexamethylenetetramine R. Titrate with 0.1 M zinc sulfate
changes from violet-blue to bright green. Titrate slowly until the colour changes from yellow to violet-pink.
towards the end of the titration.
1 mL of 0.1 M sodium edetate is equivalent to 43.30 mg of
0.1 M Ferric ammonium sulfate. 3001300. La(NO3)3,6H2O.
Dissolve 50.0 g of ferric ammonium sulfate R in a mixture of 0.1 M Lead nitrate. 3003100.
6 mL of sulfuric acid R and 300 mL of water R and dilute to Dissolve 33 g of lead nitrate R in water R and dilute to
1000.0 mL with water R. 1000.0 mL with the same solvent.
Standardisation. To 25.0 mL of the ferric ammonium sulfate Standardisation. Take 20.0 mL of the lead nitrate solution
solution, add 3 mL of hydrochloric acid R and 2 g of potassium and carry out the determination of lead by complexometry
iodide R. Allow to stand for 10 min. Titrate with 0.1 M sodium (2.5.11).
thiosulfate, using 1 mL of starch solution R as indicator.
1 mL of 0.1 M sodium thiosulfate is equivalent to 48.22 mg 0.05 M Lead nitrate. 3009700.
of FeNH4(SO4)2,12H2O. Dilute 50.0 mL of 0.1 M Lead nitrate to 100.0 mL with water R.
0.1 M Ferrous sulfate. 3001400. 0.1 M Lithium methoxide. 3003300.
Dissolve 0.694 g of lithium R in 150 mL of anhydrous
Dissolve 27.80 g of ferrous sulfate R in 500 mL of dilute sulfuric
acid R and dilute to 1000.0 mL with water R. methanol R and dilute to 1000.0 mL with toluene R.
Standardisation. To 25.0 mL of the ferrous sulfate solution addStandardisation. To 10 mL of dimethylformamide R add
3 mL of phosphoric acid R and titrate immediately with 0.02 M 0.05 mL of a 3 g/L solution of thymol blue R in methanol R
potassium permanganate. Standardise immediately before use. and titrate with the lithium methoxide solution until a
pure blue colour is obtained. Immediately add 0.200 g of
1 M Hydrochloric acid. 3001800. benzoic acid RV. Stir to effect solution and titrate with the
Dilute 103.0 g of hydrochloric acid R to 1000.0 mL with lithium methoxide solution until the pure blue colour is again
water R. obtained. Protect the solution from atmospheric carbon
Standardisation. Dissolve 1.000 g of sodium carbonate RV in dioxide throughout the titration. From the volume of titrant
50 mL of water R, add 0.1 mL of methyl orange solution R used in the second titration ascertain the exact strength of the
and titrate with the hydrochloric acid until the solution just lithium methoxide solution. Standardise immediately before
becomes yellowish-red. Boil for 2 min. The solution reverts to use.
yellow. Cool and continue the titration until a yellowish-red 1 mL of 0.1 M lithium methoxide is equivalent to 12.21 mg
colour is obtained. of C7H6O2.

General Notices (1) apply to all monographs and other texts 567
4.2.2. Volumetric solutions EUROPEAN PHARMACOPOEIA 9.0

0.1 M Magnesium chloride. 3003400. 1 M Potassium hydroxide. 3009100.

Dissolve 20.33 g of magnesium chloride R in water R and dilute Dissolve 60 g of potassium hydroxide R in carbon dioxide-free
to 1000.0 mL with the same solvent. water R and dilute to 1000.0 mL with the same solvent.
Standardisation. Carry out the determination of magnesium Standardisation. Titrate 20.0 mL of the potassium hydroxide
by complexometry (2.5.11). solution with 1 M hydrochloric acid, using 0.5 mL of
phenolphthalein solution R as indicator.
1 M Nitric acid. 3003600.
Dilute 96.6 g of nitric acid R to 1000.0 mL with water R. 0.1 M Potassium hydroxide. 3004800.
Standardisation. Dissolve 1.000 g of sodium carbonate RV in Dissolve 6 g of potassium hydroxide R in carbon dioxide-free
50 mL of water R, add 0.1 mL of methyl orange solution R water R and dilute to 1000.0 mL with the same solvent.
and titrate with the nitric acid until the solution just becomes Standardisation. Titrate 20.0 mL of the potassium hydroxide
reddish-yellow ; boil for 2 min. The solution reverts to yellow. solution with 0.1 M hydrochloric acid, using 0.5 mL of
Cool and continue the titration until a reddish-yellow colour phenolphthalein solution R as indicator.
is obtained.
0.5 M Potassium hydroxide in alcohol (60 per cent V/V).
1 mL of 1 M nitric acid is equivalent to 53.00 mg of Na2CO3. 3004900.
0.1 M Perchloric acid. 3003900. Dissolve 3 g of potassium hydroxide R in aldehyde-free
Place 8.5 mL of perchloric acid R in a volumetric flask alcohol R (60 per cent V/V) and dilute to 100.0 mL with the
containing about 900 mL of glacial acetic acid R and mix. Add same solvent.
30 mL of acetic anhydride R, dilute to 1000.0 mL with glacial Standardisation. Titrate 20.0 mL of the alcoholic potassium
acetic acid R, mix and allow to stand for 24 h. Determine the hydroxide solution (60 per cent V/V) with 0.5 M hydrochloric
water content (2.5.12) without addition of methanol and, acid, using 0.5 mL of phenolphthalein solution R as indicator.
if necessary, adjust the water content to 0.1-0.2 per cent by
0.5 M Potassium hydroxide, alcoholic. 3005000.
adding either acetic anhydride R or water R. Allow to stand
for 24 h. Dissolve 3 g of potassium hydroxide R in 5 mL of water R and
dilute to 100.0 mL with aldehyde-free alcohol R.
Standardisation. Dissolve 0.350 g of potassium hydrogen
phthalate RV in 50 mL of anhydrous acetic acid R, warming Standardisation. Titrate 20.0 mL of the alcoholic potassium
gently if necessary. Allow to cool protected from the air, and hydroxide solution with 0.5 M hydrochloric acid, using 0.5 mL
titrate with the perchloric acid solution, using 0.05 mL of of phenolphthalein solution R as indicator.
crystal violet solution R as indicator. Note the temperature of 0.1 M Potassium hydroxide, alcoholic. 3005100.
the perchloric acid solution at the time of the titration. If the Dilute 20.0 mL of 0.5 M alcoholic potassium hydroxide to
temperature at which an assay is carried out is different from 100.0 mL with aldehyde-free alcohol R.
that at which the 0.1 M perchloric acid has been standardised,
the volume used in the assay becomes : 0.01 M Potassium hydroxide, alcoholic. 3009000.
Dilute 2.0 mL of 0.5 M alcoholic potassium hydroxide to
100.0 mL with aldehyde-free alcohol R.
t1 = temperature during standardisation, 0.05 M Potassium iodate. 3005200.
t2 = temperature during the assay, Dissolve 10.70 g of potassium iodate R in water R and dilute to
1000.0 mL with the same solvent.
Vc = corrected volume, Standardisation. Dilute 25.0 mL of the potassium iodate
V = observed volume. solution to 100.0 mL with water R. To 20.0 mL of this
solution add 2 g of potassium iodide R and 10 mL of
1 mL of 0.1 M perchloric acid is equivalent to 20.42 mg dilute sulfuric acid R. Titrate with 0.1 M sodium thiosulfate,
of C8H5KO4. using 1 mL of starch solution R, added towards the end of the
0.05 M Perchloric acid. 3004000. titration, as indicator.
Dilute 50.0 mL of 0.1 M perchloric acid to 100.0 mL with 0.001 M Potassium iodide. 3009200.
anhydrous acetic acid R. Dilute 10.0 mL of potassium iodide solution R to 100.0 mL
0.02 M Perchloric acid. 3009900. with water R. Dilute 5.0 mL of this solution to 500.0 mL with
water R.
Dilute 20.0 mL of 0.1 M perchloric acid to 100.0 mL with
anhydrous acetic acid R. 0.02 M Potassium permanganate. 3005300.
0.033 M Potassium bromate. 3004200. Dissolve 3.2 g of potassium permanganate R in water R and
dilute to 1000.0 mL with the same solvent. Heat the solution
Dissolve 5.5670 g of potassium bromate RV in water R and for 1 h on a water-bath, allow to cool and filter through a
dilute to 1000.0 mL with the same solvent. sintered-glass filter (2.1.2).
0.02 M Potassium bromate. 3004300. Standardisation. To 20.0 mL of the potassium permanganate
Dissolve 3.340 g of potassium bromate RV in water R and solution, add 2 g of potassium iodide R and 10 mL of dilute
dilute to 1000.0 mL with the same solvent. sulfuric acid R. Titrate with 0.1 M sodium thiosulfate, using
1 mL of starch solution R, added towards the end of the
0.0167 M Potassium bromate. 3004400. titration, as indicator. Standardise immediately before use.
Prepare by diluting 0.033 M Potassium bromate. Storage : protected from light.
0.0083 M Potassium bromate. 3004500. 0.1 M Silver nitrate. 3005600.
Prepare by diluting 0.033 M Potassium bromate. Dissolve 17.0 g of silver nitrate R in water R and dilute to
0.1 M Potassium hydrogen phthalate. 3004700. 1000.0 mL with the same solvent.
In a conical flask containing about 800 mL of anhydrous acetic Standardisation. Dissolve 0.100 g of sodium chloride RV in
acid R, dissolve 20.42 g of potassium hydrogen phthalate RV. 30 mL of water R. Titrate with the silver nitrate solution,
Heat on a water-bath until completely dissolved, protected determining the end-point potentiometrically (2.2.20).
from humidity. Cool to 20 °C and dilute to 1000.0 mL with 1 mL of 0.1 M silver nitrate is equivalent to 5.844 mg of NaCl.
anhydrous acetic acid R. Storage : protected from light.

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

EUROPEAN PHARMACOPOEIA 9.0 4.2.2. Volumetric solutions

0.001 M Silver nitrate. 3009300. 1 mL of 0.1 M sodium hydroxide is equivalent to 12.21 mg

Dilute 5.0 mL of silver nitrate 0.1 M to 500.0 mL with water R. of C7H6O2.
0.1 M Sodium arsenite. 3005800. 0.1 M Sodium hydroxide, ethanolic. 3007000.
Dissolve arsenious trioxide RV equivalent to 4.946 g of As2O3 To 250 mL of anhydrous ethanol R add 3.3 g of strong sodium
in a mixture of 20 mL of strong sodium hydroxide solution R hydroxide solution R.
and 20 mL of water R, dilute to 400 mL with water R and add Standardisation. Dissolve 0.100 g of benzoic acid RV in 2 mL
dilute hydrochloric acid R until the solution is neutral to litmus of water R and 10 mL of ethanol (96 per cent) R. Titrate
paper R. Dissolve 2 g of sodium hydrogen carbonate R in the with the ethanolic sodium hydroxide solution, using 0.2 mL
solution and dilute to 500.0 mL with water R. of thymolphthalein solution R as indicator. Standardise
0.1 M Sodium edetate. 3005900. immediately before use.
Dissolve 37.5 g of sodium edetate R in 500 mL of water R, add 1 mL of 0.1 M ethanolic sodium hydroxide is equivalent to
100 mL of 1 M sodium hydroxide and dilute to 1000.0 mL 12.21 mg of C7H6O2.
with water R. 0.1 M Sodium methoxide. 3007100.
Standardisation. Dissolve 0.120 g of zinc RV in 4 mL of Cool 175 mL of anhydrous methanol R in iced water R and add,
hydrochloric acid R1 and add 0.1 mL of bromine water R. in small portions, about 2.5 g of freshly cut sodium R. When
Drive off the excess of bromine by boiling, add dilute sodium the metal has dissolved, dilute to 1000.0 mL with toluene R.
hydroxide solution R until the solution is weakly acid or neutral
and carry out the assay of zinc by complexometry (2.5.11). Standardisation. To 10 mL of dimethylformamide R add
0.05 mL of a 3 g/L solution of thymol blue R in methanol R,
1 mL of 0.1 M sodium edetate is equivalent to 6.54 mg of Zn. and titrate with the sodium methoxide solution until a
Storage : in a polyethylene container. pure blue colour is obtained. Immediately add 0.200 g of
0.02 M Sodium edetate. 3006000. benzoic acid RV. Stir to effect solution and titrate with the
sodium methoxide solution until the pure blue colour is again
Dissolve 7.444 g of sodium edetate R in water R and dilute to obtained. Protect the solution from atmospheric carbon
1000.0 mL with the same solvent. dioxide throughout the titration. From the volume of titrant
Standardisation. Dissolve 0.100 g of zinc RV in 4 mL of used in the second titration ascertain the exact strength of the
hydrochloric acid R1 and add 0.1 mL of bromine water R. Drive sodium methoxide solution. Standardise immediately before
off the excess of bromine by boiling. Transfer the solution to a use.
volumetric flask and dilute to 100.0 mL with water R. Transfer
1 mL of 0.1 M sodium methoxide is equivalent to 12.21 mg
25.0 mL of the solution to a 500 mL conical flask and dilute
of C7H6O2.
to 200 mL with water R. Add about 50 mg of xylenol orange
triturate R and hexamethylenetetramine R until the solution 0.1 M Sodium nitrite. 3007200.
becomes violet-pink. Add 2 g of hexamethylenetetramine R
Dissolve 7.5 g of sodium nitrite R in water R and dilute to
in excess. Titrate with the sodium edetate solution until the
1000.0 mL with the same solvent.
violet-pink colour changes to yellow.
1 mL of 0.02 M sodium edetate is equivalent to 1.308 mg of Zn. Standardisation. Dissolve 0.300 g of sulfanilic acid RV in 50 mL
of dilute hydrochloric acid R and carry out the determination
1 M Sodium hydroxide. 3006300. of primary aromatic amino-nitrogen (2.5.8), using the
Dissolve 42 g of sodium hydroxide R in carbon dioxide-free sodium nitrite solution and determining the end-point
water R and dilute to 1000.0 mL with the same solvent. electrometrically. Standardise immediately before use.
Standardisation. Titrate 20.0 mL of the sodium hydroxide 1 mL of 0.1 M sodium nitrite is equivalent to 17.32 mg of
solution with 1 M hydrochloric acid using the indicator C6H7NO3S.
prescribed in the assay in which 1 M sodium hydroxide is used.
0.1 M Sodium periodate. 3009500.
If sodium hydroxide free from carbonate is prescribed, prepare
it as follows. Dissolve sodium hydroxide R in water R to give a Dissolve 21.4 g of sodium periodate R in about 500 mL of
concentration of 400-600 g/L and allow to stand. Decant the water R and dilute to 1000.0 mL with the same solvent.
clear supernatant, taking precautions to avoid the introduction Standardisation. In a stoppered flask, introduce 20.0 mL of the
of carbon dioxide, and dilute with carbon dioxide-free water R sodium periodate solution and add 5 mL of perchloric acid R.
to the required molarity. The solution complies with the Close the flask and shake. Adjust the solution to pH 6.4 using
following test. Titrate 20.0 mL of hydrochloric acid of the a saturated solution of sodium hydrogen carbonate R. Add
same molarity with the solution of sodium hydroxide, using 10 mL of potassium iodide solution R, close, shake and allow to
0.5 mL of phenolphthalein solution R as indicator. At the stand for 2 min. Titrate with 0.025 M sodium arsenite until the
end-point add just sufficient of the acid to discharge the pink yellow colour almost disappears. Add 2 mL of starch solution R
colour and concentrate the solution to 20 mL by boiling. and titrate slowly until the colour is completely discharged.
During boiling add just sufficient acid to discharge the pink
0.1 M Sodium thiosulfate. 3007300.
colour, which should not reappear after prolonged boiling.
The volume of acid used does not exceed 0.1 mL. Dissolve 25 g of sodium thiosulfate R and 0.2 g of sodium
carbonate R in carbon dioxide-free water R and dilute to
0.1 M Sodium hydroxide. 3006600. 1000.0 mL with the same solvent.
Dilute 100.0 mL of 1 M sodium hydroxide to 1000.0 mL with Standardisation. To 10.0 mL of 0.033 M potassium bromate,
carbon dioxide-free water R. add 40 mL of water R, 10 mL of potassium iodide solution R
Standardisation. Titrate 20.0 mL of the sodium hydroxide and 5 mL of hydrochloric acid R1. Titrate with the sodium
solution with 0.1 M hydrochloric acid, using the end-point thiosulfate solution, using 1 mL of starch solution R, added
detection prescribed for the assay in which the 0.1 M sodium towards the end of the titration, as indicator.
hydroxide is used.
0.5 M Sulfuric acid. 3007800.
Standardisation (for use in the assay of halide salts of organic
bases). Dissolve 0.100 g of benzoic acid RV in a mixture of Dissolve 28 mL of sulfuric acid R in water R and dilute to
5 mL of 0.01 M hydrochloric acid and 50 mL of ethanol (96 per 1000.0 mL with the same solvent.
cent) R. Carry out the titration (2.2.20), using the sodium Standardisation. Dissolve 1.000 g of sodium carbonate RV in
hydroxide solution. Note the volume added between the 2 50 mL of water R, add 0.1 mL of methyl orange solution R,
points of inflexion. and titrate with the sulfuric acid until the solution begins to

General Notices (1) apply to all monographs and other texts 569
4.2.2. Volumetric solutions EUROPEAN PHARMACOPOEIA 9.0

turn reddish-yellow. Boil for about 2 min. The colour of the until a pure blue colour is obtained. Immediately add 0.200 g
solutions reverts to yellow. Cool and titrate again until the of benzoic acid RV. Stir to effect solution, and titrate with
reddish-yellow colour reappears. the tetrabutylammonium hydroxide solution until the pure
1 mL of 0.5 M sulfuric acid is equivalent to 53.00 mg of blue colour is again obtained. Protect the solution from
Na2CO3. atmospheric carbon dioxide throughout the titration. From
the volume of titrant used in the second titration ascertain the
0.05 M Sulfuric acid. 3008000. exact strength of the tetrabutylammonium hydroxide solution.
Dilute 100.0 mL of 0.5 M sulfuric acid to 1000.0 mL with Standardise immediately before use.
water R. 1 mL of 0.1 M tetrabutylammonium hydroxide is equivalent
Standardisation. Carry out the titration described for 0.5 M to 12.21 mg of C7H6O2.
sulfuric acid, using 0.100 g of sodium carbonate RV, dissolved 0.1 M Tetrabutylammonium hydroxide in 2-propanol.
in 20 mL of water R. 3008400.
1 mL of 0.05 M sulfuric acid is equivalent to 5.30 mg of Prepare as described for 0.1 M tetrabutylammonium hydroxide
Na2CO3. using 2-propanol R instead of toluene R and standardise as
described.
0.1 M Tetrabutylammonium hydroxide. 3008300.
Dissolve 40 g of tetrabutylammonium iodide R in 90 mL of 0.05 M Zinc chloride. 3008500.
anhydrous methanol R, add 20 g of finely powdered silver Dissolve 6.82 g of zinc chloride R, weighed with appropriate
oxide R and shake vigorously for 1 h. Centrifuge a few precautions, in water R. If necessary, add dropwise dilute
millilitres of the mixture and test the supernatant for iodides. hydrochloric acid R until the opalescence disappears. Dilute to
If a positive reaction is obtained, add an additional 2 g of silver 1000.0 mL with water R.
oxide R and shake for a further 30 min. Repeat this procedure Standardisation. To 20.0 mL of the zinc chloride solution add
until the liquid is free from iodides, filter the mixture through 5 mL of dilute acetic acid R and carry out the determination of
a fine sintered-glass filter (2.1.2) and rinse the reaction vessel zinc by complexometry (2.5.11).
and filter with three quantities, each of 50 mL, of toluene R.
Add the washings to the filtrate and dilute to 1000.0 mL with 0.1 M Zinc sulfate. 3008600.
toluene R. Pass dry carbon dioxide-free nitrogen through the Dissolve 29 g of zinc sulfate R in water R and dilute to
solution for 5 min. 1000.0 mL with the same solvent.
Standardisation. To 10 mL of dimethylformamide R add Standardisation. To 20.0 mL of the zinc sulfate solution add
0.05 mL of a 3 g/L solution of thymol blue R in methanol R 5 mL of dilute acetic acid R and carry out the determination of
and titrate with the tetrabutylammonium hydroxide solution zinc by complexometry (2.5.11).

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