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Bromatometry

This document describes procedures for titrating potassium bromate and using it to determine the amount of sodium salicylate in a sample. Potassium bromate is prepared as a primary standard solution. It is then used in a back-titration reaction along with potassium bromide to generate bromine, which reacts with phenol produced from sodium salicylate. The surplus bromine is then titrated with sodium thiosulfate using starch as an indicator. The amount of sodium thiosulfate used allows for calculating the percentage of sodium salicylate originally present in the sample.

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Mohamed Dahmane
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5K views2 pages

Bromatometry

This document describes procedures for titrating potassium bromate and using it to determine the amount of sodium salicylate in a sample. Potassium bromate is prepared as a primary standard solution. It is then used in a back-titration reaction along with potassium bromide to generate bromine, which reacts with phenol produced from sodium salicylate. The surplus bromine is then titrated with sodium thiosulfate using starch as an indicator. The amount of sodium thiosulfate used allows for calculating the percentage of sodium salicylate originally present in the sample.

Uploaded by

Mohamed Dahmane
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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1

Titration with Potassium Bromate

Potassium bromate is primary standard.


Potassium bromate can be used as oxidising agent for inorganic reducers
determination. For direct titration with potassium bromate are used specific redox indicators
or various azo-dyes, which are destroyed by bromate ion surplus (disappearance colour).
Mixture of potassium bromate and potassium bromide in acidified solution applies
for back-titration of organic compounds. This mixture produces bromine, which react with
aryl radicals in organic compounds structure. End point in bromatometric back-titration is
established iodometric-like titration with sodium thiosulfate, with starch serving as the
indicator.

I. Preparation the primary standard solution (0,1 N potassium bromate)

1. Calculate a primary standard sample (mPBT) for preparation 250 ml of solution:


N V meq PB
mPBT = . M.m. KBrO3 = 167,001 g;
1000
mass of potassium bromate equivalent meqPB = M/6.
2. Weight potassium bromate sample on hand balance with 0,1 g accuracy and put powder
into weighting bottle.
3. Weight weighting bottle with potassium bromate on analytical balance.
4. Transfer the potassium bromate into volumetric flask and weight empty weighting bottle
on analytical balance. Calculate the potassium bromate sample weight mPBP.
5. Add 40-50 ml of distilled water to volumetric flask, dissolve potassium bromate and
establish exact volume of solution with water.
6. Calculate precision normal concentration of prepared standard solution of potassium
m 1000
bromate: NPB = .
V meq BP
7. Calculate the correction factor for prepared 0,1 N potassium bromate solution: CFPB =
m PBP
.
m PBT

II. Sodium Salicylate Determination

In acid solution sodium salicylate transfer to phenol:


OH OH
COONa COOH

2 + H SO = + Na2SO4
2 4

OH
OH
COOH
H2SO4
2 2 + 2CO2 + H2O

Formed phenol reacts with bromine that produced by bromate-bromide mixture:


2

KBrO3 + 5KBr + 3H2SO4 = 3Br2 + 3K2SO4 = 3H2O

OH OH
Br Br
+ 3Br2 = + 3HBr

Br

Bromine surplus is titrated with sodium thiosulfate after potassium iodide addition:

Br2 + 2KI = 2KBr = I2

I2 + 2Na2S2O3 2NaI + Na2S4O6

1. Load a burette with 0,1 N standard sodium thiosulfate solution.


2. To conical flask pour in 10 ml aliquot of sample (VS), add pipette using 10 ml of prepared
0,1 N potassium bromate standard solution (VPB), add 10 ml of 10 % potassium bromide
solution, and add 10 ml of 1 M H2SO4 solution.
3. Cover the flask with a stopper and put into dark place at 10 min.
4. Add 10 ml of 10 % potassium iodide solution and titrate the sample with thiosulfate until
the solution becomes pale yellow. Introduce 5 drops of starch indicator, and titrate with
constant stirring to the disappearance of the blue colour.
5. Read the burette mark (VST).
6. Repeat titration also two times. Calculate the median volumes of used sodium thiosulfate
standard solution.
7. Calculate sodium salicylate percentage in sample:

(VPB N PB VST N ST ) meq SodSal


xSodSal = 100%
VS

M.m. Sodium salicylate = 160,11; meqSodSal = M/6.

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