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WORK INSTRUCTION Department. : QAD
Doc. No. : NL/SA/QAD/WI/26
ANALYSIS METHOD OF LIGHT / DENSE Page : 1 of 5
NIRMA SODA ASH
LIMITED

1. Purpose : To define the method for determination of chemical and physical parameters of light /
dense soda ash
2. Scope : Covers light/ dense soda ash received from soda ash bagging and in plant sample
3. Definitions/Abbreviation :
4. Description :

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To analyze following parameters.

4.1 Total alkalinity as Na2CO3

4.2 Matter insoluble in water
4.3 Sulphate as Na2SO4
4.4 Chloride as NaCl
4.5 Iron as Fe2O3
4.6 Bulk Density
4.7 Volatile matter
4.8 Moisture
4.9 Bicarbonate
4.10 Sample preparation for tests of parameters 4.1 to 4.9

4.1 Determination of Total Alkalinity as Na2CO3

4.1.1 Requirement
4.1.1.1 1N H2SO4
4.1.1.2 Methyl orange indicator
4.1.2 Method of test
Weigh accurately about 1.0 gm of the prepared sample (4.10) and transfer it completely 250 ml
Conical flask. Add about 100 ml of distilled water and a few drops of methyl orange indicator
solution and titrate with standard 1N H2SO4.

4.1.3 Calculation
B.R x N x 53 x 100
Total Alkalinity as Na2CO3 % by mass = -------------------------
W x 1000
4.2 Determination of Matter of insoluble in water
4.2.1 Requirement
4.2.1.1 Whatmann filter paper no 42

Prepared By Checked By Approved By Issue no. : 01

Signature Issue Date : 17.08.2004
Designation Sr.Chemist Consultant Rev. no. : 02
Date 04.03.2005 04.03.2005 04.03.2005 Rev. Date : 04.03.2005
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4.2.2 Method of Test
Weigh accurately 20 gm of the prepared sample(4.10). Transfer it to 500 ml glass
beaker. Add about 200ml distilled water and boil the solution for about 10 minutes.
Filter it through predried and preweigh( W1) whattman filter paper. Wash throughly
with hot water and dry it to constant weigh at 110+5 °C in oven. Cool the filter paper
and weigh(W2).( Preserve the filtrate for Sulphate test.)

4.2.3 Calculation
W2-W1 x 100
% Water insoluble = ------------------------
Weight of sample
Where,
W1 = Weight of filter paper
W2 =Weight of filter paper with residue

4.3 Determination of Sulphate as Na2SO4

4.3.1 Requirement
4.3.1.1 G4 crucible 50 ml
4.3.1.2 Electric oven
4.3.1.3 10 % BaCl2 Solution
4.3.1.4 Conc. Hydrochloric acid
4.3.1.5 5 % Picric acid

4.3.2 Method of Test

To the filtrate obtained (4.2.2) after determination of insoluble add conc.
Hydrochloric acid to make it acidic using methyl orange indicator. Boil the solution
and add 20 ml 1.5% picric acid and 10 ml of 10% BaCl2 solution to the boiling
solution. Boil again for 10 minutes. Let it stand for two hours and filtered through
previously dried and weighed G4 crucible. Wash the ppts. with hot water till Free
from chloride and dry it to constant weight at 105+2°C in oven. Cool the solution
and weigh.

4.3.3 Calculation
60.86 x weight of the ppts.
Sulphate as Na2SO4 = ------------------------------------
(Percent by mass ) weight of sample

4.4 Determination of Chloride as NaCl

4.4.1 Requirement
4.4.1.1 con.HNO3
4.4.1.2 0.1N standard silver nitrate
4.4.1.3 5 % K2CrO4
4.4.1.4 CaCO3

4.4.2 Method of Test

Weigh accurately 5.0 gm of the prepared samples (4.10) to a 250ml conical flask
and dissolve it in 100 ml-distilled water. Add a few drops of HNO3 to neutralize the
alkalinity and to it add 5.0 gm CaCO3 to neutralize the acidity. To this add a few
drops of nitrobenzene and titrate with 0.1N standard silver nitrate using K2CrO4
indicator till the endpoint is from yellow to brick red.

4.4.3 Calculation
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BR x N x58.46 x 100
Chloride as NaCl % by mass = --------------------------------
Wt of sample x 1000
4.5 Determination of Iron as Fe2O3
4.5.1 Requirement
4.5.1.1 Nessler cylinders 100 ml
4.5.1.2 Standard Iron solution 1ml = 0.1 mg
4.5.1.3 Con.Hydrochloric acid
4.5.1.4 5% Ammonium thiocynate
4.5.1.5 Ammonium per Sulphate

4.5.2 Method of test

Weigh accurately 1.00gm of the prepared sample (4.10) and dissolve it in about 20
ml of water and add about 5.0 ml hydrochloric acid (15 % hydrochloric acid) to
make it acidic and 30 mg Ammonium per Sulphate and boil to oxidize the iron. Cool
and transfer to 100 ml Nessler cylinder. Add 5 ml of 5% ammonium thiocynate,
dilute to the mark and stir well with glass road. In another nessler cylinder take
50ml DM water and add few drops of con hydrochloric acid to make it acidic. Add
5ml of 5% ammonium thiocynate and make the volume to mark (100 ml ) then add
standard Fe2O3 solution till the colour intensity of the sample matches to the
standard. Note the burette reading.

4.5.3 Calculation
ml. of standard solution x 1000
Iron as Fe2O3 PPM = ---------------------------------------------
Weight of sample taken for test

4.6 Determination of Bulk Density

4.6.1 Requirement
4.6.1.1 Trip drop density apparatus (As Per Akzo Doc No. EPP 1.908.047 )

4.6.2 Method of test

Use trip drop density apparatus made as per Akzo dimensions. Fill the metallic
funnel with light / dense soda which is closed from the bottom with a sliding plate.
Put cleaned metallic beaker at its bottom. Pull the sliding plate. The material will fall
in the beaker. Level the beaker with metallic plate. Weigh the material.

4.6.3 Calculation

Bulk Density g/l = 2 x material weight.

4.7 Determination of Volatile Matter :-

4.7.1 Requirement
4.7.1.1 Silica crucible
4.7.1.2 Electric bunsen burner

4.7.2 Method of test

Place about 2 gm of the material, without drying in a silica crucible and heat for
about one hour at a temperature of 250 to 300°C in an electric bunsen burner. Cool
in a desicator and weigh.
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4.7.3 Calculation
Loss in weight x 100
Volatile matter = -------------------------------------------
(Percent by Mass) Weight of sample taken for test

4.8 Determination of Moisture Content

4.8.1 Requirement
4.8.1.1 petric dish 3 ‘
4.8.1.2 Electric bunsen burner

4.8.2 Method of test

Moisture is determined only as and when required.
For this , first volatile is determined as per 4.7 and Bicarb is determined as per 4.9

4.8.3 Calculation

% Moisture = % V. M – { % Bicarb x 0.369 }

4.9 Determination of Bicarb in Soda ash

4.9.1 Requirement
4.9.1.1 1.0.1N standard NaOH
4.9.1.2 2.0.1N standard HCl
4.9.1.3 3.Phenolphthalein indicator
4.9.1.4 4.10% BaCl2 solution

4.9.2 Method of Test

Place 200 ml of 10 % BaCl2 solution in a 400-ml beaker and adjust pH to 8.8 by
adding 0.1 NaOH or 0.1 N HCl as the case may be. Into another beaker of 600 ml
Take 150 ml distilled water and add 5.0 ml 0.1 N NaOH. Add to it 4.0 gm Soda
sample and properly stir. Add to it BaCl2 solution slowly. Now, insert the electrode
of pH meter and start adding dropwise 0.1 N HCl along with stirring till pH 8.8 is
reached. This is end point.

4.9.3 Calculation
% NaHCO3 = 0.084 x ( 5 - B.R ) x 0.1 N x 25
or
5- BR x 0.21

4.10 Sample Preparation for tests of parameters 4.1 to 4.9

4.10.1 Requirement
4.10.1.1 Moisture Balance ( Scaltec )
4.10.1.2 Silica Crucible
4.10.1.3 Electric Bunsen Burner

4.10.2 Method of test:

1. All fresh calcined samples and bagging sample will be dried first in electronic
quick moisture determination apparatus (Scaltec) before carrying out test.
2. If the loss remains between 0.2 to 0.4 % proceed for tests. However if the loss
is more, required quantity of sample will be dried as explained in 4.7
3. Fresh soda from calciner/ FBD is mostly fully calcined. However in rare cases,
uncalcined material may come due to leakage of steam tubes. In such cases
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required quantity of soda will be dried as per 4.7.
4. On storage soda as bagging hygroscopic absorbs moisture. The absorption of
moisture and carbon dioxide proceeds until the formation of ultimate stable
forms, namely Na2CO3.NaHCO3.2H2O known as sesquicarbonate of soda (IS
251:1998). So all samples from long storage will be dried as per 4.7.

5. Quality Records:

Record No. Title Location Retention

Period

NL/SA/QAD/REG/07 Record register of Light / Dense Soda Ash QAD 06 month

bagging

NL/SA/QAD/REG/08 Dispatch Record Register of Light / Dense QAD 06 month

Soda Ash