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Farmaceutische Analyse
Titratievoorbeelden
Assay
Dissolve 0.150 g in 15 ml of glacial acetic acid R in a flask with a stopper fitted with a valve.
Add 15 ml of dilute hydrochloric acid R and 1 g of zinc powder R. Close the flask. Allow the mixture to stand for 60 min, protected from
light, with occasional shaking.
Filter the solution over a cotton
wad, wash with three quantities, each of 10 ml, of carbon dioxide-free water R. Add 0.1 ml of ferroin R
and immediately titrate the combined filtrate and washings with 0.1 M ammonium and cerium nitrate.
Assay
TEST
Dissolve a quantity of the powder containing 0.15 g of Ascorbic Acid as completely as possible in a mixture of 30 ml of water and 20 ml
of 1M sulphuric acid and titrate with 0.1M ammonium cerium( IV) sulphate VS using ferroin solution as indicator.
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Iodine (25g)
To 10 ml add 30 ml of water and 50 ml of hydrochloric acid and titrate with 0.05M potassium iodate VS until the dark brown solution
which is produced becomes pale brown.
Add 1 ml of amaranth solution and continue the titration until the red colour just changes to pale yellow.
From the number of ml of 0.05M potassium iodate VS required subtract half the number of ml of 0.1M sodium thiosulphate VS required in
the Assay for iodine.
Assay
Mix a quantity containing 0.7 g of Sodium Amidotrizoate with 12 ml of 5M sodium hydroxide and 20 ml of water , add 1 g of zinc powder
and boil under a reflux condenser for 30 minutes.
Cool, rinse the condenser with 30 ml of water , filter through absorbent cotton and wash the flask and the filter with two 20-ml quantities
of water .
To the combined filtrate and washings add 80 ml of hydrochloric acid , cool and titrate with 0.05M potassium iodate VS until the dark
brown solution becomes light brown.
Add 5 ml of chloroform and continue the titration, shaking well after each addition, until the chloroform becomes colourless. 1
Determine the weight per ml of the injection, Appendix V G , and calculate the percentage w/v of sodium amidotrizoate, C11H8I3N2
NaO4.
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Assay
Gently boil 0.12 g under a reflux condenser with 20 ml of 2M sodium hydroxide for 30 minutes.
Wash the combined extracts with 20 ml of 0.1M sodium hydroxide and add the washings to the main aqueous phase, discarding the organic
layer.
To the aqueous solution add 25 ml of 0.0333M potassium bromate VS , 5 ml of a 12.5% w/v solution of potassium bromide and 10 ml of
hydrochloric acid and immediately stopper the flask.
Titrate the liberated iodine with 0.1M sodium thiosulphate VS using starch mucilage , added towards the end of the titration, as indicator.
The difference between the titrations represents the amount of potassium bromate required.
The volume of 0.0333M potassium bromate VS used is equivalent to half of the volume of 0.1M sodium thiosulphate VS required for the
titration.
Assay
Add 5.0 ml of a 500 g/l solution of ethylene glycol R and allow to stand protected from light for 20 min.
Using 0.5 ml of phenolphthalein solution R as indicator, titrate with 0.1 M sodium hydroxide. Carry out a blank titration.
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1 ml of 0.1 M sodium hydroxide is equivalent to 9.21 mg of C3H8O3.
Sorbitol
Reducing sugars.
Heat so that boiling begins after 4 min and maintain boiling for 3 min.
Cool rapidly and add 100 ml of a 2.4 per cent V/V solution of glacial acetic acid R and 20.0 ml of 0.025 M iodine.
With continuous shaking, add 25 ml of a mixture of 6 volumes of hydrochloric acid R and 94 volumes of water R and, when the
precipitate has dissolved, titrate the excess of iodine with 0.05 M sodium thiosulphate using 1 ml of starch solution R as indicator, added
towards the end of the titration.
Assay
Dissolve 0.400 g in water R and dilute to 100.0 ml with the same solvent.
To 10.0 ml of the solution add 20.0 ml of a 21.4 g/l solution of sodium periodate R and 2 ml of dilutesulphuric acid R and heat on a water-
bath for exactly 15 min.
Cool and add 3 g of sodium hydrogen carbonate R a little at a time and 25.0 ml of 0.1 M sodium arsenite. Mix.
Add 5 ml of a 200 g/l solution of potassium iodide R and allow to stand for 15 min.
Titrate with 0.05 M iodine until the first trace of yellow colour appears.
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Assay
To 0.150 g in a 250 ml round-bottomed flask add 5 ml of strong sodium hydroxide solution R, 20 ml of water R, 1 g of zinc powder R and
a few glass beads. Boil under a reflux condenser for 60 min. Allow to cool and rinse the condenser with 20 ml of water R, adding the
rinsings to the flask. Filter through a sintered-glass filter and wash the filter with several quantities of water R. Collect the filtrate and
washings. Add 40 ml of dilute sulphuric acid R and titrate immediately with 0.1 M silver nitrate. Determine the end-point
potentiometrically (2.2.20), using a suitable electrode system such as silver-mercurous sulphate.
Definition Compound Magnesium Trisilicate Tablets contain, in each, 250 mg of Magnesium Trisilicate and 120 mg of Dried Aluminium
Hydroxide. They have a peppermint flavour.
To a quantity of the powder equivalent to two tablets add 7 ml of hydrochloric acid and 7 ml of water , stir and heat on a water bath for 15
minutes, stirring occasionally.
Add 30 ml of hot water , mix and filter whilst hot, washing the filter well with hot water .
Cool the combined filtrate and washings and dilute to 100 ml with water .
Add 0.2 ml of methyl red solution , neutralise to the orange colour of the indicator with 1M sodium hydroxide and heat on a water bath for
30 minutes.
Cool, add 3 g of hexamine and titrate the excess of disodium edetate with 0.05M lead nitrate VS using xylenol orange solution as indicator.
To 25 ml of the solution reserved in the Assay for aluminium add 1 g of ammonium chloride and 10 ml, or a quantity sufficient to
redissolve the precipitate that is produced, of triethanolamine .
Add 150 ml of water and 5 ml of ammonia buffer pH 10.9 and titrate immediately with 0.05M disodium edetate VS using mordant black
11 solution as indicator.
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Disperse 1 g in a mixture of 20 ml of hydrochloric acid and 20 ml of water with the aid of gentle heat, filter, wash the filter with water ,
cool the combined filtrate and washings and dilute to 100 ml with water (solution A).
Neutralise 10 ml of solution A to congo red paper with 5M sodium hydroxide , add 50 ml of 0.05M disodium edetate VS , heat on a water
bath for 30 minutes, cool, add 3 g of hexamine and titrate the excess of disodium edetate with 0.05M lead nitrate VS , using xylenol orange
solution as indicator, to a purplish red colour.
Add 1 g of sodium fluoride to the resulting solution, heat on a water bath for 15 minutes, cool and continue the titration to a purplish red
colour.
The volume of 0.05M lead nitrate VS used in the second titration represents the amount of disodium edetate liberated from the complex.
Each ml of 0.05M disodium edetate VS is equivalent to 1.349 mg of Al.
The difference between the volume of 0.05M disodium edetate VS added in the Assay for aluminium and the total volume of 0.05M lead
nitrate VS used represents the amount of zinc present. Each ml of 0.05M disodium edetate VS is equivalent to 4.068 mg of ZnO.
Amfimetrische titraties
Assay
Add 5 ml of acetate buffer pH 2.8 , 120 ml of chloroform and 5 ml of dimethyl yellow oracet blue B solution and titrate with 0.005M
dioctyl sodium sulphosuccinate VS , swirling vigorously. Near the end point add the titrant dropwise and, after each addition, swirl
vigorously, allow to separate and swirl gently for 5 seconds.
The end point is indicated when the colour of the chloroform layer changes from green to pinkish grey.
The difference between the titrations represents the amount of dioctyl sodium sulphosuccinate required.
Assay
To a quantity of the powder containing 24 mg of Codeine Phosphate add 5 ml of 5M sodium hydroxide and 15 ml of water , shake for 2
minutes and extract with three 50-ml quantities of chloroform .
Wash each extract with the same 10 ml of water , filter through absorbent cotton previously moistened with chloroform and evaporate the
combined extracts to about 60 ml on a water bath in a current of air.
Cool, add 25 ml of water , 5 ml of acetate buffer pH 2.8 and 5 ml of dimethyl yellow �oracet blue B solution and titrate with 0.01M
dioctyl sodium sulphosuccinate VS with vigorous swirling until near the end point, then add the titrant dropwise and, after each addition,
swirl vigorously, allow to separate and swirl gently for 5 seconds.
The end point is indicated by the appearance of a permanent pinkish grey colour in the chloroform layer.
The difference between the titrations represents the amount of dioctyl sodium sulphosuccinate required.
Calculate the content of C18H21NO3,H3 PO4,�H2O using the result obtained by dissolving 40 mg of codeine phosphate BPCRS in 25 ml
of water and 5 ml of acetate buffer pH 2.8 , adding 60 ml of chloroform and 5 ml of dimethyl yellow �oracet blue B solution, shaking
well to dissolve the codeine phosphate and completing the method described above beginning at the words 'and titrate...'.
For aspirin
To a quantity of the powder containing 0.8 g of Aspirin add 20 ml of water and 2 g of sodium citrate and boil under a reflux condenser for
30 minutes.
Cool, wash the condenser with 30 ml of warm water and titrate with 0.5M sodium hydroxide VS using phenolphthalein solution R1 as
indicator.
Definition
Emulsifying cetostearyl alcohol (type A) is a mixture which contains not less than 80.0 per cent of cetostearyl alcohol and not less than 7.0
per cent of sodium cetostearyl sulphate, both calculated with reference to the anhydrous substance. A suitable buffer may be added.
Assay
Cetostearyl alcohol
Disperse 0.300 g in 25 ml of methylene chloride R. Add 50 ml of water R and 10 ml of dimidium bromide-sulphan blue mixed solution R.
Titrate with 0.004 M benzethonium chloride, using sonication and heating and allowing the layers to separate before each addition, until
the colour of the lower layer changes from pink to grey.
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1 ml of 0.004 M benzethonium chloride is equivalent to 1.434 mg of sodium cetostearyl sulphate.
Assay
To 20 ml add 45 ml of water , 0.2 ml of hydrochloric acid and dilute potassium permanganate solution dropwise until a permanent pink
colour is produced.
Add 10 ml of hydrochloric acid and 3 ml of a 10% w/v solution of ammonium thiocyanate and titrate with 0.1M titanium ( III) chloride VS
maintaining a steady flow of carbon dioxide through the flask.
Assay
Dissolve 0.200 g in 5 ml of alcohol R and add 20.0 ml of 0.1M hydrochloric acid . Using 0.05 ml of methyl red solution R as indicator,
titrate with 0.1M sodium hydroxide until a yellow colour is obtained.
Assay
Dissolve 0.170 g in 10 ml of mercuric acetate solution R, warming gently. Add 50 ml of acetone R and 1 ml of a saturated solution of
methyl orange R in acetone R. Titrate with 0.1M perchloric acid until a red colour is obtained.
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Assay
Dissolve 0.170 g in 30 ml of alcohol R. Add 5.0 ml of 0.01M hydrochloric acid . Carry out a potentiometric titration (2.2.20 ), using 0.1M
sodium hydroxide . Read the volume added between the two points of inflexion.
Gehalte: Los op ongeveer 250 mg, nauwkeurig gewogen, in 10 ml water en titreer, na toevoegen van kaliumchromaat, met zilvernitraat.
Assay
Dissolve 0.350 g in 50 ml of a mixture of equal volumes of anhydrous acetic acid R and chloroform R. Titrate with 0.1 M perchloric acid
determining the end-point potentiometrically (2.2.20).
Assay
Dissolve 0.130 g in 30 ml of anhydrous acetic acid R. Titrate with 0.1 M perchloric acid, determining the end-point
potentiometrically (2.2.20).
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Assay
Dissolve 0.3000 g in a mixture of 10 ml of chloroform R and 20 ml of acetic anhydride R. Titrate with 0.1M perchloric acid ,
determining the end-point potentiometrically (2.2.20 ).
Assay
Dissolve 0.3000 g in a mixture of 50 ml of anhydrous acetic acid R and 20 ml of acetic anhydride R and add 5 ml of mercuric acetate
solution R. Titrate with 0.1M perchloric acid , determining the end-point potentiometrically (2.2.20 ).
Assay
Dissolve 0.3 g in a mixture of 50 ml of anhydrous acetic acid and 20 ml of acetic anhydride , add 10 ml of mercury ( II) acetate
solution and carry out method I for non-aqueous titration, Appendix VIII A , using crystal violet solution as indicator. Each ml of
0.1M perchloric acid VS is equivalent to 19.87 mg of C20H24N2O2 ,2HCl.
Assay Dissolve 0.45 g in 15 ml of water . Add 25 ml of 0.1M sodium hydroxide VS and extract with three 25-ml quantities of
chloroform . Wash the combined chloroform extracts with 20 ml of water , combine the aqueous solutions and reserve for the test
for Titratable cation. Dry the chloroform extracts with anhydrous sodium sulphate , evaporate to dryness at a pressure of 2 kPa
and dissolve the residue in 50 ml of anhydrous acetic acid . Carry out method I for non-aqueous titration, Appendix VIII A , using
crystal violet solution as indicator. Each ml of 0.1M perchloric acid VS is equivalent to 21.13 mg of C20H24N2O 2,H2SO4.
Codeine Hydrochloride
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Assay
Dissolve 0.3 g in a mixture of 10 ml of anhydrous acetic acid and 20 ml of 1,4-dioxan . Carry out Method I for non-aqueous titration,
Appendix VIII A , using 7 ml of mercury(<-- II>) acetate solution and determining the end point potentiometrically. Each ml of
0.1M perchloric acid VS is equivalent to 33.58 mg of C18H21NO3,HCl.
Codeine Phosphate
Assay
Dissolve 0.350 g in a mixture of 10 ml of anhydrous acetic acid R and 20 ml of dioxan R. Titrate with 0.1M perchloric acid using 0.05
ml of crystal violet solution R as indicator.
Dissolve 0.350 g in a mixture of 10 ml of anhydrous acetic acid R and 20 ml of dioxan R. Titrate with 0.1 M perchloric acid using
0.05 ml of crystal violet solution R as indicator.
Gehalte: Droog ongeveer 500 mg, nauwkeurig gewogen. Bepaal het gewichtsverlies en bereken hieruit het watergehalte. Los het
gedroogde poeder op in een mengsel van 8 ml neutrale spiritus en 2 ml water, voeg toe 10 ml chloroform en titreer het mengsel na
toevoegen van fenolftaleine met alkali.
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Assay
Dissolve 0.300 g in 30 ml of anhydrous acetic acid R and add 6 ml of mercuric acetate solution R. Titrate with 0.1 M perchloric
acid using 0.05 ml of crystal violet solution R as indicator.
Assay
In order to avoid overheating in the reaction medium, mix thoroughly throughout and stop the titration immediately after the end-
point has been reached.
Dissolve 0.200 g in 3.0 ml of anhydrous formic acid R and add 50.0 ml of acetic anhydride R. Titrate with 0.1 M per-chloric acid,
determining the end-point potentiometrically (2.2.20).
pKa 1,8
Assay
Dissolve 0.250 g in 20 ml of anhydrous acetic acid R and add 50 ml of acetic anhydride R. Titrate with 0.1 M perchloric acid,
determining the end-point potentiometrically (2.2.20).
Free pentobarbital.
Not more than 3.5 per cent. Dissolve 2.00 g in 75 ml of dimethylformamide R, heating gently if necessary. Add 0.25 ml of a 10 g/l
solution of thymol blue R in dimethylformamide R. Titrate with 0.1 M sodium methoxide until the colour changes from olive-green
to blue. Carry out a blank titration.
Assay
Dissolve 0.200 g in 15 ml of a 127.5 g/l solution of silver nitrate R in pyridine R. Titrate with 0.1 M ethanolic sodium hydroxide until a
pure blue colour is obtained, using 0.5 ml of thymolphthalein solution R as indicator. Carry out a blank titration.
C15H10Cl2N2O2 Mr 321.2
Assay
Dissolve 0.250 g in 30 ml of dimethylformamide R. Titrate with 0.1 M tetrabutylammonium hydroxide, determining the end-point
potentiometrically (2.2.20). Protect the solution from atmospheric carbon dioxide throughout the titration.
23 december 1999
Staf Farmaceutische Analyse 5e-jaar
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