Uaker Chemical: India Limited

u ak er C h em ical
India Limited
CHLORIDE CONTENT
QUAKER INDIA Test Method: CI 009(01/04)

This Test Method replaces QITM: CI 009(98/01)
1. Scope
1.1 This method has been developed to determine the chloride
content in rolling oil emulsion. It involves the chloride
ions, present in the coolant, being treated with an excess
of silver nitrate solution and the residual silver nitrate
being determined by titration with ammonium thiocyanate
solution. The chloride content is then calculated.
2. Interferences
2.1 The elements normally found in roll coolant do not
interfere with this method.
3. Chemicals
3.1 Concentrated nitric acid(70% pure);Triethanolamine or
nitrobenzene solvent.
3.2 Standard silvernitrate solution(0.0564M): dissolve 19.176g
silver nitrate(AgNO3)of AR grade in 2 litres of distilled
water and store in a dark bottle. Standardise it before use
(Note 1)
3.3 Ammonium thiocyanate, standard solution(0.0564M):
Dissolve4.1g Ammonium thiocyanate(NH4CNS) in distilled
water and dilute to 1 liter in a glass bottle. Standardise
it before use(Note 2).
3.4 Ferric alum indicator solution: Dissolve 40g of ferric
ammonium sulfate[Fe2(SO4)3,(NH4)2SO4,24H2O]in 50 ml distilled
water and acidify with 3ml of nitric acid. Dilute to
100ml. If necessary, filter and store the clear solution
in a glass bottle.
3.5 Sodium chloride standard solution[0.0564M]:dry AR grade

sodium chloride(NaCl) at 400-500oC for 30 minutes and cool
in a desiccator. Dissolve 3.298g dried NaCl in distilled
water and dilute to 1 liter in a volumetric flask.
Page 1 of 3
3.6 Potassium Chromate indicator solution(100g/L):Dissolve 10g
potassium chromate (K2CrO4), in distilled water and dilute
to 1 liter in a glass bottle.
4. Procedures
4.1 Add 50 ml of the emulsion sample to a 250 ml beaker.
4.2 Acidify with 15ml of conc. HNO3.
4.3 Heat, with occasional stirring, until the solution becomes
clear and yellow in colour with seperation of oil.
4.4 For the removal of separated oil, cool the solution and
filter through a Whatman 541 filter paper into a labeled
conical flask. Wash content of the filter paper thoroughly
with distilled water to ensure that there is no entrapment
of chloride ions.
4.5 To the filtrate, add, by means of a pipette, 25ml of freshly
standardized 0.564M silver nitrate solution(Note 3).
4.6 Add 1ml of triethanolamine or nitrobenzene(Note 4) and 1ml
of ferric alum indicator solution. Shake vigorously to
coagulate the precipitate.
4.7 Back tirate the excess silver nitrate present with freshly
standardized 0.0564M ammonium thiocyanate solution, by means
of a burette, to a salomon pink end point.
4.8 Calculate the chloride content# as shown:
Chloride content as ppm Cl(or mg/L)

= (ml 0.0564M AgNO3 - ml 0.0564M NH4CNS)*40
#
If the true normalities of AgNO3 and NH4CNS solutions are
not accurate to 0.0564M, then there required volumes must be
corrected by the formula VX/ O.0564( where X is the true
strength factor and V is the volume required of the
respective solutions) before putting into calculation.
5. Report
5.1 Report the chloride content to the nearest whole number
using unit ppm as Cl or mg/g as Cl.
NOTE1:Standardisation of silver nitrate solution:
Pipette out10ml of standard sodium chloride solution into a

250ml Erlenmeyer flask and dilute approximately to 100ml with
distilled water. Add six drops potassium chromate indicator and
titrate with silver nitrate to a salmon pink end point. Calculate
silver nitrate normality.
True normality of AgNO3 solution= (10*true NaCl solution

normality)/ ml titrant
page 2 of 3
NOTE2: Standardisation of ammonium thiocynate solution:
Ammonium thiocynate solution degenerates after a period of
time, and thus must be regularly standardized. Therefore,
pipette out 25ml freshly standardized silver nitrate
solution into a 250 ml Erlenmeyer flask. Bulk to
approximately 100ml with distilled water. Add 1 ml of
triethnolamine or nitrobenzene. Swirl and add a few drops
of ferric alum indicator. Titrate with ammonium
thiocyanate to a Salmon pink end point.
True normality of NH4CNS solution = 25* true AgNO3

normality/ ml titrant
NOTE3: 10ml of 0.0564M AgNO3 should be sufficient for chloride

levels up to 200mg/L
NOTE4: This method involves the chloride solution being treated

with an excess of AgNO3, and the residual AgNO3 being
determined by titration with NH4CNS. Now silver chloride
is more soluble than silver thiocyanate and would react
thus:
AgCl+ NH4CNS =AgCNS + NH4Cl
It is therefore necessary to remove the silver chloride by

the addition of a little nitrobenzene or triethanolamine.
The silver chloride becomes surrounded by a film of
solvent and thus becomes unreactive.
page 3 of 3

Uaker Chemical: India Limited

Uploaded by

Copyright:

Uaker Chemical: India Limited

Uploaded by

Document Information

Original Title

Copyright

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Uaker Chemical: India Limited

Uploaded by

Copyright:

u ak er C h em ical

QUAKER INDIA Test Method: CI 009(01/04)

3.5 Sodium chloride standard solution[0.0564M]:dry AR grade

Chloride content as ppm Cl(or mg/L)

NOTE1:Standardisation of silver nitrate solution:

Pipette out10ml of standard sodium chloride solution into a

True normality of AgNO3 solution= (10*true NaCl solution

True normality of NH4CNS solution = 25* true AgNO3

NOTE3: 10ml of 0.0564M AgNO3 should be sufficient for chloride

NOTE4: This method involves the chloride solution being treated

It is therefore necessary to remove the silver chloride by

You might also like