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Estimation of Chloride in Cement and Material

This document provides instructions for estimating chloride in cement and materials. It describes preparing silver nitrate and sodium chloride standard solutions and standardizing an ammonium thiocyanate solution. To determine chloride, a cement sample is dissolved and filtered. The filtrate is titrated with silver nitrate and ammonium thiocyanate. The volume of ammonium thiocyanate used is noted and used to calculate the chloride content based on the sample weight and volume of silver nitrate consumed. A blank titration is also performed to account for any chloride in reagents.

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saji kumar
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263 views

Estimation of Chloride in Cement and Material

This document provides instructions for estimating chloride in cement and materials. It describes preparing silver nitrate and sodium chloride standard solutions and standardizing an ammonium thiocyanate solution. To determine chloride, a cement sample is dissolved and filtered. The filtrate is titrated with silver nitrate and ammonium thiocyanate. The volume of ammonium thiocyanate used is noted and used to calculate the chloride content based on the sample weight and volume of silver nitrate consumed. A blank titration is also performed to account for any chloride in reagents.

Uploaded by

saji kumar
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOCX, PDF, TXT or read online on Scribd
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ESTIMATION OF CHLORIDE IN CEMENT AND MATERIAL

REAGENTS/CHEMICAL
1.
2.
3.
4.

NITRIC ACID CONC.


NITROBENZENE
POTASSIUM CHROMATE AS INDICATORS (0.2G K2CrO4)
SILVER NITRATE
0.025 N

PREPARATION

of SOLUTION

SILVER NITRATE (0.025 N)


1. Dry AgNO3 at 150 +/- for two hours and allow it to cool in a desiccators .
2. Weight accurately 4.2468 gms of it into a 250 m l beaker and dissolve in a little
qty. of distilled water .
3. Transfer it into a one litre Volumetric flask and make up to solution to one litre.
4. This solution needs standardization with standard Sodium chloride.
SODIUM CHLORIDE (0.025N)
1. Dry NaCl at 110 5 oC for one hours.and cool in a desiccators.
2. 1.4165 gms of its in a 250 ml beaker and dissolve in 50 distilled water .
3. Transfer it into one liter Volumtric Flask and make up the solution to one
litre.
AMMONIUM THIOCYNATE (0.025 N)
1. 1.9030 gms NH4SCN in a 250 ml beaker and dissolve in about 50 ml beaker ,
transfer it into one litre volumetric flask .this solution needs standaization
with standard AgNO3 solution.
Stardardisation of

0.025N AgNO3

1. Take 10 ml 0.025 N NaCl solution in a 250 ml conical flask .


2. Add 2 ml of Potassium Chromate as indicator.
3. Titrate with AgNO3 solution may be calculated using the equation
N1 x V1 = N2 x V2
Stardardisation of

0.025N NH4SCN

1. Pipette 20 ml of the standard 0.025 N AgNO3 into a conical flask , add 6N


HNO3. And add few drops of ferric alum indicator.
2. Add NH4SCN from burette,at first add white precipitation ,further addition of
solution a reddish brown cloud, which quickly disappear while shaking.at the
end point approaches the ppt became flocculent and settle easily .finally one

drop of thiocynate solution produce a faint brown colour which no longer


3.

disappears upon shaking. This is end point.

4. It is essential to shake vigorously during titration in order a correct results ,


because the freshly precipitate silver Thiocynate formed during the titration.
absorbs Ag+. these by causing a false end points which however disappears
with vigourous shaking
5. Calculate the normality of thiocynate solution,by using the
N3 xV3 =N4x V4
CHLORIDE DETERMINATION
1.
2.
3.
4.
5.

Dry the sample at 110 +/-10 oC for one hours & Cool in dessicator.
Take 2.0 +/- 0.050 gms to a 250 ml beaker.
Add 40 ml of distilled water and 10 ml of conc. HNO3
Heat to boiling & shake thoroughly.
Keep for a few minutes to settle and filter thoroughly Whatman filter

paper no.40 in conical flask.


6. Wash the filter paper thoroughly its content 4-5 times with a hot distilled
water.
7. To the fitrate 2 ml of nitrobenzene and 10 ml of 0.025N AgNO3 to the
filtrate with the help of microburtte.
8. Then, add 1 ml of ferric alum indicator.
9. Titrate with 0.025 N , NH4SCN to get a faint brown colour .
10.Note down the volume of NH4SCN used.
BLANK TEST
1. Take 100 ml distilled water in a conical flask
2. Add 10 ml conc.HNO3,10 ml of 0.025 AgNO3,2ml of Nitrobenzene, add 1
ml ferric alum.
3. Titrate with 0.025 N NH4SCN solution.
Let, Volume of NH4SCH = y
Blank = (10 y) ml.
CALCULATE & EXPRESSION OF RESULTS
Let volume of the NH4SCN

= x ml.

AgNO3 consumed by the chloride

Z = [ 10-(10-y)-X) ml
Chloride = Z x 0.08815
Wt. of the sample

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