Oin Ops Chem 011 Analytical Procedures For Raw Material

(For Internal Circulation)
COS-ISO-00-OIN/OPS/CHEM/011
Rev. No. : 0 January 2004
OPERATION INFORMATION NOTE
Analytical Procedures for Raw

Materials
CORPORATE OPERATION SERVICES
National Thermal Power Corporation Ltd.
NATIONAL THERMAL POWER CORPORATION LTD.

OPERATION & MAINTENANCE FORMAL DOCUMENTATION SYSTEM
OPERATION INFORMATION NOTE : COS-ISO-00-OIN/OPS/CHEM/011
Rev. No.: 0
Date : January 2004
Analytical Procedures for Raw

Materials
Approved for
Implementation by ..
GM (OS)
Date: ..
Enquiries to: Head of Corp. Operation Services
Analytical Procedures for Raw Materials

INDEX
S.N.
Contents
Page No.
1.
Introduction
2.
Superseded Documents
3.
Alum
4.
Ammonia Liquor
5.
Bleaching Powder
19
6.
Common salt
23
7.
Hydrazine 31
8.
Hydrochloric Acid
9.
Lime
10.
Soda Ash 42
11.
Sodium Hydroxide
46
12.
Sodium Hypochlorite Solution
56
13.
Sulphuric Acid
66
14.
Trisodium Phosphate
69
15.
Review
33
40
76
Page - 1
Rev. No.: 0

1.0
INTRODUCTION
The Manual of Analytical Procedures for Raw Materials was prepared by
Operation Services long back. The procedure of test of various chemicals has
been revised since then. The test methods given in this revised manual are suitable
for the chemicals given in the document COS-ISO-00-OIN/OPS/CHEM/007
Specifications for Water Treatment Chemicals. The latest methods of tests have
been included in this manual referred from BIS and from standard textbook. In the
revised version chemicals such as morpholine, sodium aluminate and sodium
hexametaphosphate are deleted, as these chemicals are not being used. Similarly
liquor ammonia, common salt, sodium hypochlorite and sulphuric acid are
included due to their wide use in power stations.
The manual serves as guidance for the assay analysis of bulk chemicals most
frequently used at power stations.
2.0
SUPERSEDED DOCUMENTS
Manual of Analytical Procedure for Raw Materials prepared by the Chemistry
Group of Operation Services.
3.0
ALUM
3.1 Sampling
The following procedure may be followed for sampling.
The sample must be taken in clean, dry and airtight glass or other suitable
container on which material has no action.
All the material of the same grade in a single consignment drawn from a single
batch of manufacture shall constitute a lot. If a consignment is declared or known
to consist of different batches of manufacture, the material from each batch shall
constitute a separate lot.
For ascertaining the conformity of the material in a lot to the requirements of the
specification, samples shall be tested from each lot separately. The number of
packages or slabs to be selected from lots of different sizes shall be in accordance
with column 1 and 2.
Page - 2
Rev. No.: 0
Lot Size (N)

up to 15
16 to 50
51 to 100
101 and above
Sample size (n)

3
5
8
15
Draw by suitable means a representative portion of the material, sufficient for

carrying out the tests from each package or slab selected. These portions shall
constitute the individual test sample.
From each of the individual test samples, a small but equal quantity of the
material shall be taken and thoroughly mixed to constitute the composite sample.
3.2 Prepared Sample.
Crush about 200g of the material rapidly to pass through 1.00 mm IS sieve (refer
IS. 460 1978); keep it in a clean glass stoppered weighing bottle. Use this
prepared sample for various tests to be carried out.
3.3 Assay analysis.
1. Determination of insoluble matter.
2. Determination of water-soluble aluminium compounds.
a) By gravimetry
b) By EDTA titration
3. Determination of soluble iron compounds.
4. Determination of basicity/ acidity.
3.4 Determination of Insoluble Matter
3.4.1
Principle.
A weighed sample is dissolved in acidified distilled water and filtered through a
gooch crucible, dried and weighed.
3.4.2
Reagents
1 N Sulphuric acid.
3.4.3
Procedure
Weigh accurately 10g of the prepared sample, mix with 10ml of 1N sulfuric acid
and dissolve in 100ml of water by stirring and warming if necessary. Filter
through a tared filter paper or a sintered glass crucible (G4) or a gooch crucible.
Wash the residue once with hot water slightly acidified with sulfuric acid and then
Page - 3
Rev. No.: 0
with hot water till it is free from soluble compounds and dry to constant mass at
105 110oC.
3.4.4
Calculation
Insoluble matter (% by mass) =
100M1
M
Where,
M1
M
=
=
Mass in gram of the residue.

Mass in gram of the prepared sample taken for the test.
.
3.5 DETRMINATION OF WATER SOLUBLE ALUMINIUM COMPOUNDS
(Preferred method)
3.5.1
Principle
Aluminium compounds are precipitated as hydroxide under alkaline conditions,
ignited at 1100 1200oC and weighed.
3.5.2
Reagents
i)
ii)
iii)
iv)
3.5.3
Ammonium Chloride
Concentrated Nitric Acid.
Ammonium Hydroxide (4N).
Methyl red indicator solution
Dissolve 0.1g of methyl red in 100ml of rectified spirit.
Procedure
Weigh accurately about 1g of the prepared sample and dissolve it in 100ml of
water. Filter to remove the undissolved matter and wash the filter paper
thoroughly. Add 5g of ammonium chloride and two drops of concentrated nitric
acid to the filtrate and washings, heat to boiling and add dilute ammonium
hydroxide, drop by drop until the solution smells faintly of ammonia and shows
distinct yellow colour on addition of two drops of methyl red indicator. Boil for
two minutes, filter immediately through filter paper (Whatmann No. 41or its
equivalent) and wash the residue with hot ammonium nitrate solution (2%) till the
filtrate is free from chloride. Dry the residue and ignite to constant mass at 1100
1200oC in a silica crucible.
Page - 4
Rev. No.: 0
3.5.4
Calculation
Water soluble Aluminium compounds
(as Al2O3) % by mass
=
Where,
M1 =
M2 =
A =
3.5.5
100M1 - 1.4297 A
M2
Mass in gram of the ignited residue.

Mass in gram of the prepared sample taken for the test.
% by mass of iron determined.
Alternate Method (By EDTA Titration)
3.5.5.1 Principle
An excess amount of 0.01M EDTA is added to a known volume of the sample.
Al3+ ions present in the sample will form complex with EDTA under favorable
conditions. The excess of EDTA is back titrated with 0.01M zinc sulphate. Since
alum solution is prepared in raw water, Ca++ and Mg++ will interfere in complex
formation. In order to avoid this interference a blank is prepared with raw water
and in same condition titrated with zinc sulphate. EDTA consumed for blank is
due to Ca++ and Mg++
3.5.5.2 Reagents
i)
ii)
iii)
iv)
v)
EDTA solution (0.01M)

Zinc Sulphate Solution (0.01M)
Ammonia Solution (1+5)
Hydrochloric acid (2N)
Erichrome Black T indicator (1% indicator in AR KNO3).
3.5.5.3 Procedure
Take 25ml of 5% alum solution and make up to 250ml in raw water. Take 10ml
dilute solution. Add 20ml of 0.01M EDTA (before using EDTA standardise it with
ZnSO4 using ammonia buffer). Adjust the pH 7 to 8 using a pH meter. The pH of
the solution initially is within 2 to 3 which can be raised to 7 to 8 range by adding
14 to 15 drops of 1+5 aqueous ammonia solution. Boil it for 5 to 7 minutes, cool
it to room temperature. Again adjust the pH in 7 to 8 range by adding a few drops
of 1+5 ammonia solution. Add 50mg indicator and immediately titrate with
0.01M zinc sulphate solution until the colour changes from blue to wine red. The
end point is very sharp. It will again change from slight red to blue again due to
the irreversible reaction set in between zinc-In and aluminium-In complex.
Run a blank in the same manner as above using raw water only. EDTA
consumption for complex formation in case of sample solution minus EDTA
Page - 5
Rev. No.: 0
consumption for complex formation in case of blank will give the amount of
EDTA consumed for complex formation with Al3+ only.
3.5.5.4 Calculation
Alum (% W/V)
=
=
3.5.6
Diff. Of EDTA (ml) x 0.27 x 25 x 4 x 12.33

1000
Diff. EDTA (ml) x 0.027 x 12.33
Reference
A Text Book of Quantitative Inorganic Analysis A. I. Vogel
3.6 Determination of Soluble Iron Compounds

3.6.1
Principle
Iron is estimated volumetrically by titration against standard potassium
dichromate solution using diphenylamine as indicator.
3.6.2
Reagents
1.
2.
3.
4.
5.
6.
7.
3.6.3
Concentrated Hydrochloric Acid

Stannous Chloride solution
Dissolve 6.0g of stannous chloride crystals (SnCl2.2H2O) in 60ml
concentrated hydrochloric acid and dilute with water to 100ml. Keep this
in a stoppered bottle.
Mercuric Chloride Solution Saturated.
Sodium Diphenylamine Sulphonate indicator solution: Dissolve 0.5g in
100ml water.
Standard Potassium Dichromate solution (0.05N)
Phosphoric acid.
Procedure
Weigh accurately 10g of the prepared sample and dissolve it in 50ml of water and
filter. To the filtrate add about 10ml of concentrated hydrochloric acid and heat to
boiling. Reduce the iron by adding stannous chloride solution until the yellow
colour of ferric chloride disappears. Do not add more than 2-3 drops of stannous
chloride in excess, cool the solution add rapidly 10 ml of mercuric chloride
solution and stir so that a little white precipitate of mercurous chloride forms
slowly indicating that slight excess of stannous chloride was present. Allow to
stand for five minutes. Add 5ml of phosphoric acid and dilute to 200-250ml with
water. Add 5 drops of diphenylamine indicator and titrate with standard potassium
Page - 6
Rev. No.: 0
dichromate solution until the colour of the solution changes to a deep blue which
does not fade on stirring.
3.6.4
Calculation
Soluble iron compounds (as Fe)
% By mass
5.584 x V x N
M
Where,
V
N
M
=
=
Volume in ml of saturated potassium dichromate solution

required for the titration to be made.
Normality of standard potassium dichromate solution
Mass in g of the prepared sample taken for the test.
3.7 Determination of Basicity/Acidity

3.7.1
Principle
It is estimated by titrating under specified conditions the sample solution against
standard sodium hydroxide solution using phenolphthalein indicator.
3.7.2
Reagents
1. Sulphuric acid (0.5N)
2. Potassium fluoride solution.
Having Relative density approximately 1.32, neutralized with potassium
hydroxide if acidic or with concentrated sulfuric acid if alkaline using
phenolphthalein solution as indicator.
3. Phenolphthalein indicator solution.
Dissolve 0.1g of phenolphthalein in 100ml of 60% rectified spirit.
4. Standard Sodium hydroxide solution (0.5N).
3.7.3
Procedure
Weigh accurately about 3g of the prepared sample and dissolve in 20ml of carbondioxide free water and 10ml of dilute sulfuric acid, cool the solution to 20oC and
add 20ml of potassium fluoride solution and 0.5ml of phenolphthalein indicator.
Titrate the solution against standard sodium hydroxide solution (V1) till the end
point, which is indicated by a pink colour persisting for 1 minute.
Carry out a blank titration without the sample (V2). If V2 is less than V1, the
sample is acidic.
3.7.4
Calculation
Basicity (as Al2O3)% by mass
(V2 V1) x N x E1
Page - 7
Rev. No.: 0
10M
Acidity (as H2SO4) % by mass
(V1 V2) x N x E2
10M
Where,
V1 = Volume in ml of standard sodium hydroxide solution used in
titration of the material.
V2 = Volume in ml of standard sodium hydroxide solution used in blank
titration.
N = Normality of sodium hydroxide solution.
E1 = Equivalent mass of Al2O3
E2 = Equivalent mass of H2SO4
M = Mass in g of the prepared sample taken for the test.
Page - 8
Rev. No.: 0
4.0
AMMONIA, LIQUOR
4.1
Determination of Ammonia
4.1.1 Method A
4.1.1.1 Principle
A weighed amount of ammonia is reacted with excess of acid and the remaining
acid is estimated by titrating against standard alkali.
4.1.1.2 Reagents
1. Standard sulphuric acid - 0.5 N.
2. Methyl red indicator.
Dissolve 0.5 g of water-soluble methyl red in water and dilute the solution to
one litre.
3. Caustic soda solution 0.5 N, freshly standardized.
4.1.1.3 Procedure
Accurately weigh a 15ml capacity ground glass stoppered weighing bottle
containing 10 to 12 ml of water. Open the ammonia bottle and insert a clean and
dry glass tube of about 5mm bore to half the height of the liquid and transfer 1 to
1.5ml of the material to the weighing bottle immediately replace the glass stopper
and weigh. Place the weighing bottle in about 200ml of water containing 50ml of
0.5 N sulphuric acid and a few drops of methyl red indicator.
Due to the mass of the water and ammonia contained in the bottle, it will remain
immersed in the acid. Open the stopper under the acid by manipulating with a
glass rod and titrate the excess of acid with standardised caustic soda solution to a
faint yellow end point.
Carry out a blank with all the reagents used for the test.
4.1.1.4 Calculation
Ammonia, percent by mass
1.703(V1 V2) x N
M
Where
V1 = volume in ml of standard sodium hydroxide solution used in the blank,
V2 = volume in ml of standard sodium hydroxide solution used in the test with the
material,
N = normality of standard sodium hydroxide solution, and
M = mass in g of the material taken for the test.
Page - 9
Rev. No.: 0
4.1.2 Method B
4.1.2.1 Reagents
1. Boric acid 2 percent.
2. Standard sulphuric acid solution 0.5N.
3. Methyl red 0.1 percent.
Dissolve 0.1g of methyl red in 95 percent (V/V) ethanol and make up to
100ml with the same ethanol.
4.1.2.3 Apparatus
Spherical glass ampoule of thin glass, of suitable capacity and shape, for
example, about 20-mm diameter, with one capillary end about 50 mm in length.
4.1.2.4 Procedure
Weigh the glass ampoule to the nearest 0.01g. Gently heat the spherical part of
the ampoule over a flame and dip the capillary end of the ampoule into the bottle
containing the laboratory sample. Ensure that the ampoule is almost completely
filled during cooling.
Withdraw the ampoule and dry the capillary tube carefully with filter paper. Seal
the end of the capillary tube, without loss of glass, with an oxidizing flame.
Allow the capillary tube to cool, wash it with water and wipe it carefully with
filter paper.
Weigh the sealed ampoule accurately and calculate, by difference, the mass of the
test portion.
Carefully place the ampoule containing the test portion into a 500 ml conical
flask, fitted with a ground glass stopper, to which 50ml of the boric acid solution,
about 250ml of water and several drops of the methyl red solution have been
added.
Stopper the conical flask and shake carefully so as to break the ampoule.
Unstopper the flask; rinse the stopper with water collecting the washings in the
same flask.
Using a glass rod, grind the pieces of the ampoule, in particular those parts of the
capillary tube, which may have remained unbroken. Remove the glass rod; rinse
it with water, collecting the washings in the same flask.
Titrate with the sulphuric acid solution until the indicator changes from yellow to
red.
Page - 10
Rev. No.: 0
4.1.2.5 Calculation
Ammonia (Percent by mass) =
1.703 x V x N
M
Where
N
V
M
=
=
=
Normality of sulphuric acid.

volume in ml of standard sulphuric acid used, and
mass in g of the material taken for the test.
4.2
Determination of Residue on Evaporation
4.2.1
Procedure
Measure 500 ml of the material in a volumetric flask. Add the whole material, in
small portions, to a platinum crucible or other suitable dish, and evaporate to
dryness on a steam bath, inside a fume cupboard. Dry the residue at 1052 degree
C to constant mass.
4.2.2
Calculation
Residue on evaporation, percent by mass
100 x M
VS
Where
M = mass in g of the residue,
V = volume in ml of the material taken for the test, and
S = relative density of the material.
4.3
Determination of Carbonate
4.3.1
Principle
The carbonate is precipitated as barium carbonate and the turbidity produced due
to the precipitation is compared with a known standard.
4.3.2
Apparatus
4.3.3
Nessler Cylinders 25ml capacity.

Reagents
1.
2.
4.3.4
Barium Hydroxide Solution saturated.

Standard Sodium Carbonate (Anhydrous) Solution 0.01 N.
Procedure
Weigh 1.5 g of the material, dilute to 20 ml with carbon dioxide-free water and
add 5ml barium hydroxide solution. Carry out a control test in the other solution,
20 ml of carbon dioxide-free water and 5ml of barium hydroxide solution.
Page - 11
Rev. No.: 0
The material shall be taken to have passed the test if the turbidity produced in the
test with the material is not greater than produced in the control test.
4.4
Determination of Chlorides
4.4.1
Principle
The chloride is precipitated as silver chloride and the turbidity produced due to
the precipitation is compared with a known standard.
4.4.2
Apparatus
Nessler Cylinders 50 ml capacity.
4.4.3
Reagents
1. Silver Nitrate Solution 0.1 N approximately.
2. Dilute Nitric Acid 4N approximately.
3. Standard Chloride Solution A
Dissolve 1.648 g of sodium chloride (dried at 105 2 degree C) in water and
dilute to 1000ml in a volumetric flask. One milliliter of this diluted solution
contains 1.0 mg of chloride (as Cl).
4. Standard chloride solution B
Dilute 10ml of standard chloride solution A to 1000ml with water. One
milliliter of this diluted solution contains 0.01 mg chloride (as Cl).
4.4.4
Procedure
Accurately weighs 20 g of the material and evaporate on a steam bath until
reduced to 1 ml. Then dilute with 50ml of water and add 1ml of dilute nitric acid
and 1ml of silver nitrate solution. Carry out a control test in the other Nessler
cylinder using 1 ml of standard chloride solution B, 1 ml of dilute nitric acid, 1ml
of silver nitrate solution and 50 ml of water. Wait for 5 minutes and compare the
opalescence in both the cylinders.
The material shall be taken to have passed the test if the opalescence produced in
the test with the material is not greater than that produced in the control test.
4.5
Determination of Phosphate
4.5.1
Principle
The sample is reacted with ammonium molybdate in an acid medium and the
resulting phosphomolybdate is reduced to molybdenum blue complex with
amino-naphtol-sulphonic-acid.
Page - 12
Rev. No.: 0
4.5.2
Apparatus
1. Spectrophotometer
2. Nessler cylinders
4.5.3
Reagents
1. Standard phosphate solution.
Dissolve 0.165g potassium dihydrogen phosphate dried at 105oC, in water,
dilute to 1000ml. Add 5ml of CHCl3 (1ml = 0.5mg PO4). Prepare standard
solution from the above stock having 1ml = 0.01mg PO4.
2. Strong acid solution
Cautiously add 300ml concentrated sulphuric acid to 600ml water. Cool and
add 4.0ml concentrated nitric acid and dilute to 100ml.
3. Phenolphthalein indicator
4. Ammonium molybdate solution
a) Dissolve 31.4g ammonium molybdate in 200ml of water.
b) Cautiously add 252ml of concentrated H2SO4 to 400ml of water, mix and
cool, add 3.4ml concentrated HNO3.
Add solution (a) to solution (b) and dilute to 1000ml.
5. Amino-naphtol sulphonic acid.
Weigh out separately 0.75g 1-amino-2-naphthol-4-sulphonic acid, 42g sodium
sulphite and 70g sodium metabisulphite. Pulverize the amino-naphthol
sulphonic acid with a small portion of sodium metabisulphite in a clean dry
mortar. Dissolve the remaining sodium metabisulphite and sodium sulphite in
900ml water, add to it ground amino-naphtol sulphonic acid sodium
metabisulphite mixture and stir to dissolve. Dilute to 1litre. Store in an amber
coloured bottle.
Note This solution is not stable. Do not keep longer than two weeks.
4.5.4
Procedure
Take 2,4,6,8 and 10ml standard solutions (1ml = 0.01mg) in Nessler cylinders and
add 2.0ml ammonium molybdate, mix well and after 5 minutes add 2.0ml amino
naphthol sulphonic acid and dilute to 50ml mark. Run a reagent blank. Measure
the absorbance at 660nm using 10mm cell and adjusting the blank to zero. Draw a
calibration curve against the concentration of PO4.
Take a suitable aliquot containing 0.02mg PO4 or more; evaporate on steam bath
until reduced to 1ml. Transfer quantitatively with water into a 100ml Nessler
cylinder. Add phenolphthalein indicator. If pink colour develops, neutralize it with
acid. Add 2.0ml ammonium molybdate reagent and mix well. After 5 minutes add
2.0ml amino naphthol sulphonic acid and dilute to 50ml mark, mix well. After 5
minutes measure the percentage transmittance at 660nm and from the graph find
out the amount of PO4.
Page - 13
Rev. No.: 0
4.5.5
Calculation
Phosphate (as PO4), percentage by mass
A x 100
V
Where
A
V
=
=
mg/l of PO4 from the calibration curve, and

volume in ml of the sample taken for the test.
4.6
Determination of Silicate
4.6.1
Principle
The sample is reacted with molybdate ion in an acidic medium and the resulting
green-yellow coloured complex is reduced to a blue complex with 1-amino-2naphthol-4-sulphonic acid the intensity of which is measured at a wavelength of
815nm.
4.6.2
Apparatus
1.
2.
4.6.3
Spectrophotometer.
Nessler cylinder.
Reagents
1.
2.
4.6.3
Dilute hydrochloric acid 1:1 (v/v).

Ammonium molybdate solution.
Dissolve 10g ammonium molybdate in water by warming and dilute to
100ml. Filter if necessary. Adjust pH 7 to 8 with silica free ammonia or
sodium hydroxide. Store the reagent in polyethylene bottle to stabilize.
3.
Oxalic acid solution 10 percent.
4.
Standard silica solution.
Dissolve 4.73g sodium metasilicate nonahydrate (Na2SiO3.9H2O) in water
and dilute to about 900ml. Check the concentration and adjust the solution
to contain 1000mg/l SiO2.
Dilute 10ml of this solution to 1000ml. One milliliter of this solution is
equivalent to 0.01mg SiO2.
5.
Reducing agent.
Dissolve 500mg 1-amino-2-naphthol-4-sulphonic acid and 1g of sodium
sulphite in 50ml water and add this to a solution of 30g sodium hydrogen
sulphite in 150ml water, filter into a plastic bottle.
Procedure
Take 2.5, 5,10,15 and 20ml standard solution (1ml = 0.01mg SiO 2). Add to each
1.0ml (1:1) HCl and 2.0ml ammonium molybdate reagent. Mix well and allow to
stand for 5 to 10 minutes. Add 5ml oxalic acid and mix. Wait for 2 minutes and
then add 2.0ml reducing agent. Make up volume to 50ml. Run a reagent blank.
Page - 14
Rev. No.: 0
After 5 minutes measure absorbance and draw a calibration curve against mg
SiO2.
Take 10g of the sample and evaporate on steam bath until the volume reduces to
1ml. Transfer quantitatively with water into a 100ml Nessler cylinder and proceed
as above (calibration curve). Find mg SiO2 from the graph.
4.6.4
Calculation
Silicate (as SiO2), percent by mass =
A x 100
M
Where
A
M
=
=
mg of SiO2 from the calibration curve, and

mass in gram of the sample taken for the test.
4.7
Determination of Sulphate
4.7.1
Apparatus
Nessler Cylinders 50 ml capacity.
4.7.2
Reagents
1.
2.
3.
4.
4.7.3
Ordinary Denatured Spirit

Dilute Hydrochloric Acid 1 N approximately.
Barium Chloride Solution
Prepare by dissolving 12 g of barium chloride crystals in water and making
up to 100 ml.
Standard Sulphate Solution
Dissolve 0.148 g of sodium sulphate in water and make up the solution to
1000ml. One milliliter of the solution contains 0.1 mg of sulphate (as SO4).
Procedure
Accurately weigh 50 g of the material and evaporate on a steam bath until reduced
to 1 ml, dilute with 40 ml of water and 10 ml of denatured spirit, and add 1 ml of
dilute hydrochloric acid. Mix and add 1ml of barium chloride solution, mix
immediately. Carry out a control test in the other Nessler cylinder by taking 1ml
of standard sulphate solution, 10 ml of denatured spirit, 40 ml of water and 1ml of
dilute hydrochloric acid; mix, add 1 ml of barium chloride solution and mix
immediately. Allow both the solutions to stand for 1 hour.
The limit prescribed in Table 1 shall be taken as not having been exceeded if the
turbidity produced with the material is not greater than that produced in the
control test.
Page - 15
Rev. No.: 0
4.8
Determination of Calcium and Magnesium
4.8.1
Principle
Presence of calcium and magnesium is checked as the consumption of EDTA
4.8.2
Reagents
1.
Ammonia-Ammonium Chloride Buffer Solution

Dissolve 67.5 g of ammonium chloride in 300 ml of water, add 570 ml of
strong ammonia solution and mix. Make up volume to 1 000 ml with water.
2. Sodium Sulphide Solution M/2 approximately.
3. EDTA Solution M/100.
Dissolve 4.0g of ethylene diaminetetraacetic acid disodium salt in water, add
20 ml of 1N sodium hydroxide solution, mix, and dilute to 1000 ml with
water.
4. Methylthymol Blue Indicator
Grind 0.1 g of methylthymol blue with 10 g of potassium nitrate. Add 25 to
50 mg of this mixture to 50 ml of the solution to be titrated.
4.8.3
Procedure
Weigh 80 g (89ml) of the material and evaporate on a steam bath until reduced to
1ml. Dilute to 100 ml with water and add 20 ml of ammonia-ammonium
chloride buffer solution, a further 20g of sample and 5 drops of sodium sulphide
solution. Titrate with 0.01M EDTA, using methyl thymol blue as indicator until
the blue solution becomes colourless or grey.
The material shall be taken to have passed the test if not more than 1ml of 0.01M
EDTA is required for titration.
4.9
Determination of Copper
4.9.1
Procedure
Accurately weigh 100g (110ml) of the material, evaporate on a steam bath until
volume is reduced to 2ml. Dilute with 20ml water and 5ml dilute sulphuric acid
(approximately 5N). Proceed for determination of copper by the Neocuproine
method as described in the Manual on analytical test procedures for water and
steam in thermal power stations (Revision 01) by Operation Services.
4.10
Determination of Iron
4.10.1 Principle
Iron is measured by the intensity of the colour developed with 2-2-Dipyridyl
solution using spectrophotometer at a wavelength of 530nm.
Page - 16
Rev. No.: 0
4.10.2 Apparatus
1. Spectrophotometer
4.10.3 Reagents
1.
2.
3.
4.
5.
6.
7.
Dilute sulphuric acid 1:1 (v/v)

Hydroxylamine hydrochloride solution 10 percent.
Ammonium acetate solution 20 percent.
2-2-Dipyridyl solution 1 percent in alcohol.
Ammonia solution (R.D. 0.93) 18 percent.
Standard iron solution A.
Dissolve 0.702g of ferrous ammonium sulphate [FeSO4(NH4)2SO4.6H2O]
in a small amount of water. Add 5ml of concentrated H2SO4 and dilute
with water up to the mark in a 1000ml volumetric flask, mix well (1ml =
0.1mg Fe).
Standard Iron Solution B.
Transfer 10ml of solution A to 1000ml volumetric flask and dilute to the
mark with water, mix well (1ml = 0.001mg = 1g Fe).
4.10.4 Procedure
Transfer 2,5,10,15 and 20ml of standard iron solution in 5 different 100ml
volumetric flasks. Add to each flask 2ml of (1:1) sulphuric acid, 2ml of 10 percent
hydroxylamine hydrochloride, shake and wait for 5 minutes. Add 10ml of 20
percent ammonium acetate solution and 1ml of 1 percent 2-2-Dipyridyl solution.
Then add 3.5ml of 18 percent ammonia solution and dilute to the mark, shake
well. Run a reagent blank. Allow to stand for 30 minutes and measure absorbance
at 530nm using 10mm cell. Draw a calibration curve of absorbance against
concentration of iron.
Accurately weigh 50g (57 ml) of the sample and reduce the volume to 15ml
evaporating on a steam bath. Transfer the material quantitatively with small
amount of water into 100ml volumetric flask. Add 2ml (1:1) sulphuric acid and
2ml hydroxylamine hydrochloride and shake well. Allow to stand for 5 minutes.
Add 10ml ammonium acetate solution, mix and add 1ml of 2-2-Dipyridyl
solution and 3.5 ml 18 percent ammonia solution. Dilute to the mark with water.
Run a reagent blank. Allow to stand for 30 minutes and measure absorbance at
530nm adjusting blank to zero. Find out iron from the graph.
4.10.5 Calculation
Iron (as Fe), percentage by mass
X
M x 104
Where
4.11
X
=
g iron from the graph, and
M
=
mass in gram of the sample taken for the test.
Determination of Heavy Metals
Page - 17
Rev. No.: 0
4.11.1 Apparatus
4.11.2 Reagents
1.
Dilute Hydrochloric Acid Solution- approximately 5 N.
2.
Dilute Ammonia Solution 30 percent (v/v).
3.
Dilute Acetic Acid Solution 30 percent (v/v)
5. Standard Lead Solution A.
Dissolve 0.160g of lead nitrate in 250 ml of water. One milliliter of the
solution contains 0.1 mg of lead.
6. Standard solution B
Dilute 50 ml of standard lead solution (A) to 500 ml with water. This
solution contains 0.01 mg of lead (as Pb).
4.11.3 Procedure
Accurately weigh 40 g (45 ml) of the material, boil until the volume is reduced to
15 ml, add 2.5 ml of dilute hydrochloric acid and boil for 2 minutes in the same
vessel. Cool, dilute to 20 ml and add 30 ml of water and 10 g (11ml) of the
sample. Pass hydrogen sulphide through the solution for a few seconds. Carry
out a control test in the other Nessler cylinder as follows. Mix 2.0 ml of the
standard lead solution B with 3ml of dilute acetic acid. Add standard iron
solution equivalent to the amount of iron present in the test solution, as per 4.10
dilute to 40 ml with water; add 10ml of dilute ammonia solution pass hydrogen
sulphide through the solution for a few seconds.
The material shall be taken to have not exceeded the limit given in Table 1 if the
turbidity produced in the test with material is not greater than that produced in the
control test.
4.12
Test for Reducing Substances
4.12.1 Reagents
1.
2.
Dilute Sulphuric Acid approximately 5 N.

Potassium Permanganate Solution 0.1 N.
4.12.2 Procedure
Weigh 10g (11ml) of the material, add 50 ml of dilute sulphuric acid and 1.0 ml of
0.01 N potassium permanganate solution and boil the mixture gently for 5
minutes.
Page - 18
Rev. No.: 0
The material shall be taken to have passed the test if the pink colour of potassium
permanganate is not completely discharged.
4.13
Test for Pyridine and Homologues

Measure the optical density of the sample in 1-cm quartz or silica cell at a
wavelength of 252 nm, using water blank. The optical density should not be
greater than 0.045.
4.14
Sampling of Ammonia, Liquor

Ammonia, liquor, is volatile and highly toxic and requires care in sampling. Use
care in opening the container as a portion of the contents may blow out violently
due to pressure of ammonia gas. Cool the container before opening, especially
during warm season. Hold it away from the eyes and then slowly remove the cap
or stopper.
The samples shall be placed in clean, dry and airtight screw cap polyethylene
bottles.
4.14.1 SCALE OF SAMPLING

All containers in a single consignment of the material of the same grade and
drawn from a single batch of manufacture shall constitute a lot. If a consignment
is declared to consist of different batches of manufacture, the containers
belonging to the same batch shall be grouped together and each such batch shall
constitute a lot. For ascertaining the conformity of the material to the requirement
of this specification, samples shall be tested for each lot separately.
The number of containers to be selected from a lot shall depend on the size of the
lot and shall be as given below.
Lot Size
Number of Containers To Be Selected
Up to 15
2
16 to 25
3
26 to 50
4
51
100
5
101 300
6
301 500
7
501 800
8
801 130
9
1301 and above
10
These containers shall be selected at random. In order to ensure the randomness of
selection the procedures given in IS: 4905-1968 shall be followed.
Page - 19
Rev. No.: 0
5.0
BLEACHING POWDER
5.1
Sampling
All the container in a single consignment of same grade of the material drawn
from a single batch of manufacture shall constitute a lot. If a consignment is
declared to consist of different batches of manufacture, the batches shall be
marked separately and the groups of containers in each batch shall constitute
separate lots. The number of containers to be selected from the lot shall depend
upon the size of the lot (N)
Lot Size (N)
28
9 27
28 64
65 125
126 216
217 343
344 512
513 729
730 1000
1001 1331
Sample Size (n)

2
3
4
5
6
7
8
9
10
11
These containers (n) shall be selected at random from the lot and in order to
ensure randomness of selection (also refer IS: 4905 1969), the following
procedure may be adopted.
Starting from any container count them in order 1,2,3,up to r where r is an
integral part of N/n. Every rth container thus counted shall be withdrawn to form
the sample.
5.2
Assay Analysis
1.
2.
3.
4.
Determination of available chlorine.

Determination of stability.
Determination of moisture.
Determination of particle size.
5.3
Determination of Available Chlorine
5.3.1
Principle
The sample is treated with an excess of potassium iodide and estimated
iodometrically using sodium thiosulphate and starch indicator.
Page - 20
Rev. No.: 0
5.3.2
Reagents
1.
2.
3.
4.
5.
5.3.3
Potassium dichromate solution (0.1N)

Carefully pulverize a quantity of potassium dichromate and dry at 110 5 o C
to constant weight. Dissolve 4.904g of the dried reagent in water to make
exactly one litre and mix thoroughly.
Standard sodium thiosulphate solution (0.1N).
Potassium Iodide.
Glacial acetic acid.
Starch indicator.
Triturate 1g of starch with 10ml of cold water and pour with constant
stirring into 200ml of boiling water. Allow to settle and use the clear
supernatant liquid.
Procedure
Weigh accurately about 2.5g of the sample and grind in a mortar with water till a
smooth paste is formed. Add 15 20ml of water and decant off the fine part into a
250ml flask. Again grind the material left behind and repeat the process of
decanting off till no gritty material is left. Wash the pestle and mortar in the same
flask. Make the solution to 250ml. Take 25ml of the solution add 2g of potassium
iodide crystals and 100ml of water and then add 2ml of glacial acetic acid and
titrate it against the standardized sodium thiosulphate solution till a pale yellow
colour is left. At this stage add starch indicator and continue the addition of
standard sodium thiosulphate solution till the blue colour disappears.
5.3.4
Calculation
Available chlorine % by weight
A x N x 35.46
W
Where,
A
N
W
=
=
Volume in ml of standard sodium thiosulphate solution

used.
Normality of standard sodium thiosulphate solution.
Weight in gram of sample taken for the test.
5.4
Determination of Stability
5.4.1
Principle
The sample is heated at 1002oC for 2 hours and available chlorine is determined.
The difference between available chlorine content before and after heating
represents stability of bleaching powder.
Page - 21
Rev. No.: 0
5.4.2
Procedure
Crush the material to powder. This operation shall be carried out with minimum
delay. Fill a test tube to a depth of 125mm with the sieved material and tap lightly
three times, close the mouth of the tube with rubber stopper carrying an air
condenser so that about 12mm of the tube projects below the stopper into the test
tube, place the test tube in a bath maintained at 100 2 oC for 2 hours. At the end
of this period, remove the test tube from the bath. Remove the stopper carrying
the air condenser and close the test tube with a solid stopper. After standing for 15
minutes, transfer the material to a glass bottle. Shake well and store.
Determine the available chlorine on the stored material.
5.4.3
Calculation
Stability
Where
W1
=
W2
=
W1 W2
W1
% by weight of available chlorine as determined in 5.4.

% by weight of available chlorine after heating.
5.5
Determination of Moisture
5.5.1
Procedure
Weigh accurately 15 20g of the sample in an open dry weighing glass, and place
it for 24 hours in a vacuum desiccator over fused anhydrous calcium chloride
under an absolute pressure of 30 40mm of mercury. Weigh the weighing glass
again. The decrease in weight corresponds to the moisture content of the sample.
5.5.2
Calculation
Moisture content % by weight
(W1 W2) x 100

W1
Where,
W1
W2
5.6
=
=
Weight of material taken before drying.

Weight of material after drying.
Determination of Particle Size

Weigh accurately 50g of the sample, place it over 1.7 mm IS sieve and shake it for
15 minutes. The weight of the material passing over the sieve gives the particle
size of the sample expressed as % by weight.
Page - 22
Rev. No.: 0
5.6.1
Calculation
Calculate the particle size as follows.
Material passing through 1.7 mm IS sieve
% by weight
(W1 W2) x 100

W1
Where
W1
W2
=
=
Weight of material taken for sieving.

Weight of the material retained over the sieve.
Page - 23
Rev. No.: 0
6.0
COMMON SALT
6.1
Sampling
Each individual heap or wagon shall constitute a separate lot.
For Packages
All the packages in a single consignment of common salt of the same grade,
drawn from a single batch of manufacture shall constitute a lot. If the
consignment is declared to consist of different batches, the batches shall be
marked separately and the group of containers in each batch shall constitute a
separate lot.
The number of packages (n) to be selected from the lot shall depend upon the size
of the lot (N) and shall be as under
Lot Size (N)
up to 50
51 to 100
101 to 150
151 to 300
301 and above
No. of packages to be
selected (n)
3
4
5
7
10
The packages shall be selected at random from the lot and in order to ensure the
randomness of selection, procedure given IS 4905 1968 may be followed.
Samples shall be tested for each lot, for ascertaining conformity of the material to
the requirements of this specification.
6.2
Preparation of Sample
A)
Crush 500g of the sample to pass through a 1mm sieve, dry in an air oven at
about 150oC for at least 4 hours. Cool in a desiccator and transfer to a clean
glass-stoppered weighing bottle kept in a desiccator for subsequent tests.
B)
Accurately weigh about 20g of the dried sample. Dissolve it in 200ml of

water in a beaker. Heat to boiling, filter and wash the paper free of chloride.
Cool and make up the solution to 1 litre. Use this solution for subsequent
tests.
6.3
Determination of Moisture Content
6.3.1
Procedure
Grind rapidly the material as received in an agate mortar approximately to a size
of 2.8mm sieve, but do not actually sieve. The material, which shall be in the
Page - 24
Rev. No.: 0
form of powder, shall be kept in an airtight container. Weigh accurately about 20g
of the material in the weighing bottle of about 30ml capacity, preferably wide
mouth squat type, previously dried and weighed. Dry in an oven at 140 to 150 oC
for at least 4 hours. Cool in a desiccator and weigh. Repeat drying, cooling and
weighing until constant mass is obtained.
6.3.2
Calculation
Moisture, percentage by mass
M1 M2 x 100
M1
Where
M1
M2
=
=
Mass in gram of the material taken for the test

Mass in gram of the material after drying.
6.4
Determination of Matter Insoluble in Water
6.4.1
Principle
A known amount of the material is dissolved in water and the solution is passed
through a sintered glass crucible. The weight of the material retained in the
crucible gives the insoluble.
6.4.2
Procedure
Accurately weigh about 20g of the dried sample, dissolve it in 200ml of water in a
beaker, heat to boiling and cool. Filter the solution through a weighed gooch or
sintered glass crucible (G4) and wash the residue till it is free from chlorides. Dry
the crucible along with the insoluble residue to constant mass.
6.4.3
Calculation
Matter insoluble in water
100 x M1
M2
Where
M1
M2
=
=
Mass in gram of the residue

Mass in gram of the sample taken for the test.
6.5
Determination of Total Chlorides
6.5.1
Principle
The sample is titrated with standard silver nitrate solution using potassium
chromate as indicator.
6.5.2
Reagents
1.
Potassium Chromate indicator solution 5 percent
2.
Standard silver nitrate solution 0.1N

Page - 25
Rev. No.: 0
6.5.3
Procedure
Transfer 10 ml of the sample solution prepared 6.2-(B) into a conical flask and
add 1ml of potassium chromate indicator solution. Titrate against standard silver
nitrate solution till the reddish brown tinge persists after brisk shaking. Carry out
a blank determination.
6.5.4
Calculation
Total chloride (as Cl) % by mass
Where
V
=
N
M
=
=
3.546 x VN
M
Volume in ml of standard silver nitrate solution used in the solution

with material corrected to the blank.
Normality of standard silver nitrate solution and
Mass in gram of the dried sample in 10ml of the solution taken for
the test.
Residual chloride is the chloride obtained by deducting the chloride attributed to

the other chlorides, such as magnesium chloride and calcium chloride. This is
calculated as follows:
Express the soluble carbonate as calcium carbonate. If there is excess of calcium
over calcium carbonate, combine all the calcium with sulphate radical and express
the result as percentage of calcium sulphate. If there is excess of sulphate over
what is required for calcium, combine the excess with magnesium and express the
result as percentage magnesium sulphate. Calculate the balance of magnesium as
magnesium chloride and deduct the chloride content corresponding to it from the
chloride content. Also deduct from the chloride content an amount of chloride
corresponding to potassium content and express it as percentage of potassium
chloride. Calculate the residual chloride as percentage of sodium chloride.
6.6
Determination of Calcium And Magnesium
6.6.1
Principle
The total hardness is determined using titration with EDTA and calcium is
separately determined using a calcium specific indicator like calcine. The
difference is calculated and expressed as magnesium.
6.6.2
Reagents
1.
Standard Calcium solution

Weigh 1.000g of calcium carbonate, dried at 120oC, and dissolve it in the
minimum quantity of dilute hydrochloric acid. Dilute the solution to one
litre in a graduated flask. One millilitre of this solution is equivalent to
0.4003mg of calcium (as Ca).
Page - 26
Rev. No.: 0
2.
Standard EDTA solution

Dissolve 3.72g of disodium ethylene diamine tetra acetate dihydrate in
water and dilute in a graduated flask to one litre. The solution shall be
standardized frequently against standard calcium solution following the
procedure as given for the sample.
3.
Dilute sodium hydroxide solution Approximately 10 percent
4.
Eriochrome Black T indicator
Dissolve 0.1g of the dye in 20ml of rectified spirit conforming to IS-324
1959. This solution shall be prepared fresh every week.
5.
Dilute Sodium Hydroxide Solution Approximately 10%.
6.
Murexide indicator solution.
Grind 0.2g of murexide with 10g of sodium chloride until the mixture is
homogenous. 0.2g of this mixture is suitable for 100ml of the sample
solution.
7.
Calcein Indicator
Grind thoroughly 0.1g of calcein and 0.06g of thymolphthalein with 10g
of potassium chloride.
8.
Ammonium chloride-Ammonium hydroxide buffer solution
Dissolve 67.5g of ammonium chloride in a mixture of 570ml of
ammonium hydroxide (sp. gr. 0.90) and 250ml of water. Also dissolve
separately a mixture of 0.931g of disodium ethylene diamine tetra acetate
dihydrate and 0.616g of magnesium sulphate (MgSO4.7H2O) in about
50ml of water. Mix the two solutions and dilute to one liter.
Note Five milliliters of buffer solution added to 50ml of distilled water should
not consume more than a drop of EDTA solution to change to distinct blue
with Eriochrome black T indicator.
6.6.3
Procedure
Standardization of EDTA solution Transfer 25ml of standard calcium solution
into a conical flask, add 25ml of water, 10ml of ammonium chloride-ammonium
hydroxide buffer solution, 5 drops of the eriochrome black T indicator solution
and titrate against the standard EDTA solution to a pure blue end point.
Titrate 25ml of the buffer solution with EDTA solution using eriochrome black T
indicator. Subtract the buffer correction for 10ml (usually it will be 0.1ml) from
the reading obtained in the standardization step and note the final titre value.
Calculate the calcium equivalent of 1ml of EDTA solution (say A).
Transfer exactly 100ml of the solution preserved in (B) into a 250ml conical flask,
add 10 ml ammonium chloride-ammonium hydroxide buffer solution, 5 drops of
eriochrome black T indicator solution and titrate against standard EDTA solution
till wine red colour of the solution changes to pure blue end point. Note the
volume of EDTA used in the titration.
Transfer exactly 100ml of the solution preserved in (B) into 250ml conical flask
add 5mg sodium hydroxide solution and stir well. Add 0.2g murexide (or 100 mg
calcein indicator) and titrate against standard EDTA solution till wine red colour
Page - 27
Rev. No.: 0
of the solution changes to pure blue end point with murexide (or green to purple
with mixed calcein indicator). Note the volume of the standard EDTA solution
used in the titration.
6.6.4
Calculation
Calcium (as Ca), percentage by mass =
Magnesium (as Mg), percentage by mass
AV2
M
=
0.6068 x A (V1 V2)

M
Where
A = Calcium equivalent in mg of 1ml of EDTA solution determined in
standardization titration.
V2 = Volume in ml of standard of EDTA solution used in calcium titration.
M = Mass in gram of the dried sample equivalent to the solution (B) used
for the titration.
V1 = Volume in ml of standard EDTA solution used in eriochrome black T
titration.
6.7
6.7.1
Gravimetric Method
6.7.1.1 Principle
The sulphate is precipitated as barium sulphate and the amount of sulphate present
is determined gravimetrically.
6.7.1.2 Reagents
1. Dilute hydrochloric acid approximately 4N.
2. Barium chloride solution approximately 10 percent.
6.7.1.3 Procedure
Dissolve about 10g of the preserved dry sample in about 400ml of water, filter
and wash the residue free from soluble salts. Collect the filtrate and washings.
Add 1 drop of methyl orange and 10ml of dilute hydrochloric acid or more till it
is pink and then boil. Add to the boiling solution, 10 to 12ml of barium chloride
solution drop by drop so that the addition is in slight excess and continue boiling
for 4 minutes to obtain a granular precipitate. Allow to stand for 4 hours and filter
through a weighed sintered glass crucible (G 4) or Gooch crucible. Wash the
precipitate till free from chloride and dry to constant mass at 105 to 110oC.
Alternatively, filter through Whatman No.42 filter paper and wash till it is free
from chloride. Ignite and determine as barium sulphate.
Page - 28
Rev. No.: 0
6.7.1.4 Calculation
Sulphate (as SO4), percent by mass =
41.13 x M1
M2
Where
M1
M2
6.7.2
=
=
mass in gram of barium sulphate, and

mass in gram of dried sample taken for the test.
Volumetric method.
6.7.2.1 Principle
The sulphate is precipitated with barium chloride and the excess of barium is
determined by titration against standard EDTA.
6.7.2.2 Reagents
1.
2.
3.
4.
5.
Standard barium chloride solution 0.05N

Dissolve 6.108g of barium chloride dihydrate (BaCl2.2H2O) in water and
make up to one litre.
Dilute hydrochloric acid approximately 1N.
Standard EDTA solution
Weigh 3.72g of disodium ethylene diamine tetra acetate dihydrate in water
and dilute in a graduated flask to one litre. The solution shall be
standardized frequently against standard barium chloride solution prepared
in (1.) using the procedure given for hardness. One milliliter of standard
EDTA solution is equal to 0.001374g of barium (Ba) or 0.00096g of
sulphate (SO4).
Eriochrome black T indicator solution Same as in Hardness test.
Ammonium chloride-ammonium hydroxide buffer solution same as in
hardness test.
6.7.2.3 Procedure
Pipette out 20ml of standard barium chloride solution into a conical flask, add 2
drops of hydrochloric acid and 10ml of ammonium chloride-ammonium
hydroxide buffer solution. Dilute it with water to about 50ml, add five drops of
eriochrome black T indicator solution and titrate against standard EDTA solution
to pure blue end point. Note the titre value (say, A)
Pipette out 100ml of the preserved sample solution and add two drops of
hydrochloric acid and heat to gentle boiling. To the hot solution add 20ml of
standard barium chloride solution. Boil gently for about 5 minutes and then cool
to room temperature. The solution will be neutral or slightly acidic when tested
with a litmus paper. Add 10ml of ammonium chloride-ammonium hydroxide
Page - 29
Rev. No.: 0
buffer solution and five drops of eriochrome black T indicator solutin. Titrate
against standard EDTA solution to pure blue end point. Note the titre value (say,
B).
6.7.2.4 Calculation
Sulphate (as SO4), percentage by mass
(on dry basis)
Where
A
V1
B
M
0.096 x (A+V1 B)
M
= volume in ml of standard EDTA solution used in first titration.

= Volume in ml of standard EDTA solution used in total Ca+ Mg
(as obtained in 6.6.3).
= volume in ml of standard EDTA solution used in second titration.
= Mass in gram of the dried sample in the test solution.
6.8
Test for Iron
6.8.1
Principle
Iron is converted to the ferric form and reacted with thiocyanate solution. The
colour developed is compared with the colour developed with a standard iron
solution.
6.8.2
Apparatus
6.8.3
Reagents
1.
2.
3.
4.
5.
6.8.4
Dilute hydrochloric acid Approximately 5N, free from iron.

Concentrated nitric acid.
Potassium thiocyanate solution 5 percent (m/v).
Dilute sulphuric acid approximately 5N.
Standard Iron solution.
Dissolve 2.81g of ferrous ammonium sulphate [FeSO4 (NH4)2SO4.6H2O]
in 10ml of dilute sulphuric acid and dilute with water to 1000ml. Transfer
10ml of the solution to 1000ml volumetric flask and dilute again up to the
mark. One milliliter of this solution is equivalent to 0.004mg of iron as Fe.
Procedure
Weigh accurately about 2g of the material and dissolve it in about 20ml of water.
Add about 5ml of hydrochloric acid in order to make the solution acidic and 2ml
of nitric acid, and boil to oxidize the iron salts. Cool and transfer to a Nessler
cylinder, add 5ml of potassium thiocyanate solution, dilute to the mark with water
Page - 30
Rev. No.: 0
and stir well. Into a second Nessler cylinder, add 5ml hydrochloric acid, 2ml
nitric acid, 5ml standard iron solution for the grade for resin treatment and 10ml
of standard iron solution for that used for softener regeneration, and 5ml
potassium thiocyanate solution. Dilute to the mark and stir well. Compare the
colour of the solution in the two cylinders.
The limit prescribed for iron shall be taken to have not been exceeded if the
intensity of colour produced with the sample is not greater than that produced by
the standard iron solution.
Page - 31
Rev. No.: 0
7.0
HYDRAZINE
7.1
Determination of Percentage Purity of Hydrazine
7.1.1
Principle
Hydrazine can be determined by titrating with standard solution of potassium
iodate.
7.1.2
Reagent
1.
2.
3.
4.
7.1.3
Potassium Iodate Solution (0.1M)

Hydrochloric Acid (2N)
Hydrochloric Acid (12N)
Chloroform.
Procedure
Weigh out about 1-2g of the hydrazine into a 100 ml volumetric flask containing
25ml of 2N hydrochloric acid dilute to 100ml mark with water and; mix well.
Pipette a 25ml aliquot of this solution into a 250ml glass stoppered erlenmayer
flask containing 30ml of 12N hydrochloric acid and 10ml of chloroform.
Titrate rapidly with 0.1M potassium iodate solution until the aqueous layer begins
to change from brown to a light yellow colour. Continue the addition of iodate
dropwise, stopper the flask and shake the solution vigorously after addition of
each drop. The end point is indicated when the purple iodine colour disappears
from the chloroform.
7.1.4
Calculation
Hydrazine, wt %
V x M x 32.05
W x10
Where
V
M
W
7.2
=
=
=
ml of iodate solution
Molarity of iodate solution
Weight of hydrazine in the aliquot in gram.
Sampling
All containers in a single consignment of the material drawn from a single batch
of manufacture shall constitute a lot. If a consignment is declared or known to
consist of different batches of manufacture, the batches shall be marked separately
and the groups of containers in each batch shall constitute separate lots. For
ascertaining conformity of the material in a lot to the requirements of this
Page - 32
Rev. No.: 0
specification, sample shall be tested of each lot separately. The number of
containers to be selected at random from lots of different sizes shall be as follows
Lot Size (N)
3 to 15
16 to 40
41 to 65
66 to 110
111 and above
Sample Size (n)

3
4
5
7
10
In order to ensure randomness of selection, the following procedure shall be

adopted:
Arrange all the containers in the lot in a systematic manner and
starting from any one, count them as 1,2,3,.. Up to r, where r is the integral
part of N/n (N and n being the lot size and sample size respectively). Every r th
container thus counted shall be with drawn to constitute the test sample.
Page - 33
Rev. No.: 0
8.0
HYDROCHLORIC ACID
8.1
Determination of Total Acidity
8.1.1
Principle
The strength of the acid sample is determined by carrying out acid alkali titration.
8.1.2
Apparatus
Lunge-Rey pipette:
If this pipette is not available a weighing bottle or a glass ampoule may be used.
8.1.3
Procedure
If lunge-Rey pipette or an ordinary weighing bottle is used for weighing the
sample, accurately weigh about 2-3g of the material in it. Transfer the sample to a
conical flask and dilute to 100ml with water. Add two drops of bromocresol green
or phenolphthalein indicator to the solution in the beaker or flask and titrate to the
end point with standard sodium hydroxide solution.
8.1.4
Calculation
Total acidity (as HCl) % by mass
V x N x 3.646
M
Where
V
N
M
=
=
=
Volume in ml of standard sodium hydroxide solution used.

Normality of standard sodium hydroxide solution.
8.2
Determination of Residue on Ignition
8.2.1
Reagents
Concentrated sulphuric acid
8.2.2
Procedure
In a platinum dish previously ignited at 800 oC cooled in a desiccator and weighed,
weigh to the nearest 10mg approximately, 100g of the sample. Evaporate most of
the acid (the final volume should amount to about 5-10ml) by carefully heating
the dish containing the test portion (on a sand bath). Then allow to cool to room
temperature, add 1ml of concentrated sulfuric acid and heat to dryness. Place the
dish containing the residue in an electric furnace heated at 8005oC and keep at
this temperature for about 15 minutes. Remove the dish from the furnace, cool in
Page - 34
Rev. No.: 0
a desiccator and weigh. Repeat the heating, cooling and weighing to constant
mass.
8.2.3
Calculation
Residue on ignition % by mass
M1 x 100
M2
Where
M1
M2
=
=
Mass in gram of the residue weighed.

8.3
8.3.1
Principle
Sulphate is estimated gravimetrically as barium sulphate and reported as H2SO4.
8.3.2
Reagents
1.
2.
8.3.3
Sodium carbonate AR Grade.

Barium chloride solution Approximately 10% (m/v).
Procedure
Weigh to the nearest 0.01g about 10g of the material (M1) in a porcelain dish, add
0.5g of sodium carbonate and evaporate to dryness. Moisten the residue with
about 1.000g of the material accurately weighed (M2), add 200ml of boiling water
and filter if necessary. Bring the contents to boil over a low flame and add slowly
with stirring 5ml hot barium chloride solution. Boil the contents for two minutes
and allow the precipitate to settle for 4 hours. Filter the supernatant liquid through
a tared sintered glass crucible or a tared gooch crucible and transfer the precipitate
carefully into the crucible. Wash thoroughly with hot water till the washings are
free from chlorides. Heat the crucibles at 105oC to 110oC to constant mass.
8.3.4
Calculation
Sulphate (as H2SO4) % by mass
42.02 M
(M1+M2)
Where
M
M1
M2
=
=
=
Mass in gram of the precipitate.

Mass in gram of the sample taken for the test initially.
Mass in gram of the sample added subsequently.
Page - 35
Rev. No.: 0
8.4
Determination of Iron (Bipyridyl Method)
8.4.1
Principle
Iron (II) forms a red coloured complex with 2,2 bipyridyl. The intensity of the
colour is measured at 522nm.
8.4.2
Apparatus
Spectrophotometer suitable for measurement at a wavelength of 522nm.
8.4.3
Reagents
1.
2.
3.
4.
5.
6.
8.4.4
Hydrochloric acid (1N).

Hydroxyl ammonium chloride solution
Dissolve 10g of hydroxyl ammonium chloride in water and dilute to
100ml.
2,2 bipyridyl solution
Dissolve 1g of 2,2 bipyridyl in 10ml dilute hydrochloric acid (1N) and
dilute to 100ml with water.
Standard Iron Solution (A)
Dissolve 0.7022g of ferrous ammonium sulphate hexa hydrate
[FeSO4(NH4)2SO4 .6H2O] in water in a 1000ml volumetric flask, add 4ml
of concentrated sulphuric acid and make up to the mark with water, one ml
of this solution contains 0.1mg of iron (as Fe).
Standard iron solution (B)
Take 100ml of standard iron solution A and dilute to 1000ml with water
in a volumetric flask. This dilute solution should be prepared fresh. One
ml of this solution contains 0.01mg of iron.
Ammonium acetate solution.
Dissolve30g of ammonium acetate in water and dilute to 100ml.
Procedure
Weigh accurately about 50g of the sample in a platinum or silica dish (100ml
capacity), place on a boiling water bath and carefully evaporate to dryness. Cool,
take up with 2ml hydrochloric acid and 25 ml of water and heat to facilitate
dissolution. Transfer quantitatively to a 100ml volumetric flask; dilute to mark,
mix and filter if necessary. Transfer an aliquot of the sample solution containing
between 50 to 500 microgram of iron to 100ml volumetric flask. Dilute to
approximately 50ml if necessary and then add successively 2ml of hydrochloric
acid solution, 2ml hydroxylammonium chloride solution and after 5 minutes 5ml
of ammonium acetate solution and 1ml 2,2 bipyridyl solution. Dilute to the
mark, mix and wait for 10 minutes. Carry out the measurement on the
spectrophotometer at a wavelength of about 522nm adjusting the instrument to
zero optical density using the blank standard as reference.
Page - 36
Rev. No.: 0
At the same time as the analysis, carryout a blank test. Using the same procedure
and quantities of all reagents employed in the test.
Prepare a Calibration curve by taking the quantities of standard iron solution
indicated below in a series of eleven 100ml volumetric flask.
Volume of standard iron
Solution B of iron (Fe)
ml
0
5
10
15
20
25
30
35
40
45
50
Corresponding Mass
microgram
0
50
100
150
200
250
300
350
400
450
500
The first solution will be used as reference. Add to each volumetric flask an
amount of water sufficient to make up total volume to 50 ml, then 2 ml of
hydrochloric acid solution (1N), 2ml of hydroxyl ammonium acetate solution and
1ml of 2,2-bipyridyl solution. Dilute to mark, mix thoroughly & wait for 10
minutes. Carryout the photometric measurement as stated earlier using reference.
Prepare a calibration curve by plotting iron content as abscissa and corresponding
values of absorbance as ordinate.
8.4.5
Calculation
Iron contents (as Fe)% by mass
m x 100 x 100
VxM
Where
m = Mass in gram of iron determined in the aliquot of sample solution.
V = Volume in ml of the sample taken for colour reaction.
M = Mass in gram of the test portion.
8.5
Determination of Free Chlorine & Bromine
8.5.1
Principle
Free chlorine and bromine is estimated iodometrically by reacting with potassium
iodide and titrating equivalent amount of released iodine with sodium thiosulfate
solution.
Page - 37
Rev. No.: 0
8.5.2
Reagents
1.
2.
3.
4.
8.5.3
Potassium Iodide 10% solution

Potassium Iodide crystals.
Sodium Thiosulfate solution (0.1N)
Starch indicator solution.
Make a paste of 0.5g of starch with 2.5ml of water. Pour the paste in small
quantities into 200 ml water. Boil for 15 minutes with stirring, preserve in
small containers previously sterilized in boiling water for 2 hours.
Procedure
Place about 20ml of the test sample in a 100ml conical flask, add 50ml of water,
one crystal of potassium iodide, 0.5ml of starch solution & stir. If a blue colour
indicating iodine liberation appears, proceed for determination of free chlorine
and bromine as under. If no colour develops, it indicates absence of free chlorine
and bromine.
Weigh about 50g of the sample accurately in a weighing bottle. Transfer the test
portion to a 500ml capacity conical flask having ground glass stopper, containing
about 100ml of water; stopper the flask and cool. Add to the conical flask 100ml
of potassium iodide solution; stopper the flask and shake. Allow to stand for 2
minutes & then add 1ml of starch solution titrate the liberated iodine until the blue
colour disappears.
Since iron may interfere in the determination, carryout a blank determination
using 100 ml of water and adding to it a water soluble ferric iron salt equivalent to
that contained in 50g of the sample. Add other reagents as added to the sample.
Subtract the volume of sodium thiosulfate solution required for titration from the
volume required with the sample.
8.5.4
Calculation
Free Chlorine & bromine (as Cl)% by mass =
Where
V =
m =
M =
V x m x 100
M
Volume in ml of 0.1N Sodium thiosulfate solution used in titration.

(Corrected for the blank)
Mass in g of chlorine corresponding to 1ml of 0.1N sodium
thiosulfate solution (theoretical value, 1 ml = 0.00355g of Cl.)
mass in g of test portion.
Page - 38
Rev. No.: 0
8.6
Determination of Sulphites
8.6.1
Principle
The measured sample is added to standard iodine solution and excess of iodine is
titrated with standard sodium thiosulphate solution.
8.6.2
Reagents
1.
Standard iodine solution 0.1 N

freshly standardized.
2.
Standard
sodium
thiosulphate
solution. 0.1 N freshly standardized.

3.
Starch
Solution
as
in previous
experiment
8.6.3
Procedure
Introduce successively into a 500 ml stoppered conical flask 100ml of freshly
boiled water and 10ml of standard iodine solution. Add while cooling about 50 g
of the sample 0.01g weighed accurately. Stopper the flask mix after 2 minutes,
titrate the excess iodine with standard sodium thiosulphate solution, adding 5ml of
starch towards the end of the titration.
8.6.4
Calculation
Sulfites (as SO2) % by mass =
0.3203 (10 V)
M
Where
V = Volume in ml of standard sodium thiosulphate solution used in titration.
M = Mass in g of the material taken for the test.
8.7
Sampling
All containers in a single consignment of the material of the same grade drawn
from a single batch of manufacture shall constitute a lot. If a consignment is
declared to consist of different batches of manufacture, the batches shall be
marked separately and the groups of containers in each batch shall constitute
separate lots. Samples shall be tested from each lot separately for judging the
conformity of the material to the requirements of the specification. For this
purpose, five containers shall be selected at random from each lot.
NOTE--- If the number of containers in a lot is eight or less, the number of
containers to be selected and the criteria for conformity of the lot to the
specification requirements shall be as agreed to between the purchaser
and supplier.
Page - 39
Rev. No.: 0
The containers shall be selected at random and to ensure randomness of selection,
random number tables shall be used (see IS 4905: 1968). In case random number
tables are not available, the following procedure may be used:
Starting from any container in the lot, count them as 1,2,.., up to r, and so on,
where r is the integral part of N(N being the number of container in the lot). Every
rth container thus counted shall be withdrawn to constitute a sample.
8.7.1
Sampling Tube
The sampling tube shall be made of glass and shall be 20 to 40 mm in diameter
and 350 to 750 mm in length. The upper and lower ends are conical and reach 6 to
12 mm diameter at the narrow ends. For drawing the samples, the apparatus is
first closed at the top with a thumb or a stopper and lowered till a desired depth is
reached. It is then opened for a short time to admit the material and is finally
closed and withdrawn.
For small containers, the size of the sampling tube may be altered suitably.
Page - 40
Rev. No.: 0
9.0
LIME
9.1
Determination of Available Lime (As CaO)

Two methods have been prescribed for the determination of available lime. For
routine analysis, the iodine method may be used but in case of dispute, the sugar
method shall be used.
9.1.1
Iodine Method
9.1.1.1 Reagents
1.
2.
3.
Standard sodium thiosulphate solution 0.1 N recently standardized.

Standard iodine solution
0.1 N, recently standardized against standard Sodium thiosulphate solution
Starch iodine solution.
Triturate 5g of starch and 0.01g of mercuric iodide with 30 ml of cold water
and slowly pour it with stirring, into 1 litre of boiling water. Boil for 3
minutes. Allow the solution to cool and decant off the supernatant clear
liquid.
9.1.1.2 Procedure
Weigh accurately about 1g of the material into a glass-stoppered conical flask and
add about 30ml of boiling water. Shake for 5 to 10 minutes. Cool the solution
and add an amount of iodine solution sufficient to provide an excess of about 5ml
and stir occasionally until the lime has gone in solution. Any insoluble silica
present is easily distinguished from the milky-appearing lime. When the solution
of lime is complete (about 10 minutes required), dilute the solution in a
volumetric flask to 500 ml. Pipette out 25 ml of the solution and titrate the excess
iodine with standard sodium thiosulphate solution, adding starch indicator
towards the end of the titration. Carryout a blank determination using exactly the
same amount of iodine solution as with sample.
9.1.1.3 Calculation
Available lime (as CaO) percent by weight =
56.08 x ( V1 V2) N
W
Where
V1 = Volume in ml of standard sodium thiosulphate solution used with the blank.
V2 = Volume in ml of standard sodium thiosulphate solution used with the
material.
N = Normality of standard sodium thiosulphate solution, and
W = weight in gram of the material taken for the test.
Page - 41
Rev. No.: 0
9.1.2
Sugar Method
9.1.2.1
Reagents
1.
2.
3.
4.
5.
9.1.2.2
Rectified Spirit Conforming to IS : 323 1959.

Standard hydrochloric acid 0.1N.
Standard sodium hydroxide solution 0.1N
Sugar solution approximately 15%, in carbondioxide free water.
Phenolphthalein indicator solution.
Dissolve 0.5g of phenolphthalein in 100ml of rectified spirit.
Procedure
Weigh accurately about 1g of the finely powdered material into a 500ml

volumetric flask and wet it with the minimum amount of rectified spirit. Shake
with about 400ml of sugar solution for 3 hours. Dilute to volume. Filter through a
coarse dry filter paper (Whatman No. 40 or its equivalent) into a dry flask.
Discard the first 25ml of the filtrate. Pipette out 50ml from the filtrate into another
flask to which 50ml of standard hydrochloric acid is added and titrate with
standard sodium hydroxide solution using phenolphthalein as indicator.
Run a blank using 50ml of sugar solution and 50ml of standard hydrochloric acid.
9.1.2.3 Calculation
Available lime (as CaO) percentage by weight
Where
A
=
B
=
N
W
9.2
=
=
28.04 x (A B) N
W
Volume in ml of standard sodium hydroxide solution used in blank

Volume in ml of standard sodium hydroxide solution used with the
material.
Normality of standard sodium hydroxide solution.
Weight in gram of the material taken for the test.
Reference
1514: 1990 Methods of sampling and Test for quick lime and hydrated lime.
Page - 42
Rev. No.: 0
10.0
SODA ASH
10.1
Sampling
In any consignment of one grade of soda ash, all the containers of the same size
and drawn from a single batch of manufacture shall constitute a lot. If a
consignment of one grade of soda ash is known to consist of different batches of
manufacture or of different sizes of containers, then the containers belonging to
the same batch and size shall be grouped together and each group shall constitute
a separate lot.
For ascertaining the conformity of the lot to the requirements of the specification,
tests shall be carried out for each lot separately. The number of container (n) to be
selected for this purpose shall depend on the size of the lot (N) and shall be in
accordance with Table below.
The containers shall be selected at random from the lot and in order to ensure
randomness of selection, the following procedure is recommended for use.
Arrange all the containers in the lot in a systematic manner and starting from any
container, count them as 1,2,3., etc, up to r and so on, where r is the integral
part of N/n. Every rth container thus counted shall be withdrawn to give sample for
tests.
Lot Size (N)
up to 15
16 to 40
41 to 65
66 to 110
111 and above
10.2
No. of containers to be
selected (n)
3
4
5
7
10
Prepared sample
Dry about 35g of the material in a weighing bottle. Heat for about 1 hour at a
temperature of 250oC 300 oC. Cool in a desiccator. Repeat until mass remains
constant.
10.3
Determination of Total Alkalinity
10.3.1 Reagents
1. Sulfuric acid 1N
2. Methyl orange Indicator solution
Dissolve 0.01g of methyl orange in100 ml of water.
Page - 43
Rev. No.: 0
10.3.2 Procedure
Weigh accurately 1g of the prepared sample as given in 10.2 Transfer it
completely to 500ml conical flask and dissolve it in a 100ml of water. Add 4
drops of methyl orange indicator solution and titrate with standard sulfuric acid.
10.3.3 Calculation
Total alkalinity (as Na2CO3)
By mass
5.3 x A x N
M
Where,
A = Volume in ml of sulfuric acid used in the titration.
N = Normality of standard sulfuric Acid.
M = Mass in gram of the prepared sample taken for the test.
10.4
10.4.1 Procedure
Weigh accurately about 10g of the prepared sample. Transfer it to a 400ml beaker,
add about 200ml of freshly boiled distilled water and boil the solution for about
10 minutes. Filter through a weighed sintered glass crucible (G No. 4) or Gooch
crucible. Wash thoroughly with hot water and dry to constant mass at 11050C.
10.4.2 Calculation
Matter insoluble in water, percent by mass = 100M1
M2
Where
M1=mass in g of the residue, and
M2=mass in g of the prepared sample taken for the test.
10.5
Determination of Sulphates
10.5.1 Reagents
1. Conc. Hydrochloric Acid
2. Barium Chloride Solution 10 percent.
10.5.2 Procedure
Dissolve about 10g of the prepared sample accurately weighed, in 100ml of water
and add hydrochloric acid to make the solution slightly acidic. Boil well to
decompose the carbonates. Cool, filter through a folded filter paper and wash the
filter paper thoroughly, collecting the filtrate and washings to about 250ml, boil
Page - 44
Rev. No.: 0
and add 10ml of hot barium chloride solution to the boiling solution. Boil again
for 2 minutes, let it stand for 4 hours and filter through a tared Gooch crucible.
Wash the precipitate free from chloride and dry to constant mass at 1052oC.
10.5.3 Calculation
Sulphates (as Na2SO4), percent by mass
60.86C
M
Where
C
M
10.6
=
=
mass in gram of the precipitate, and

mass in gram of the prepared sample taken for the test.
Determination of Chloride
10.6.1 Principle
The chloride is precipitated with silver nitrate in presence of the nitric acid and
the excess silver nitrate is estimated by titration against standard Thiocyanate
using iron III salt as indicator.
10.6.2 Reagents
1.
2.
3.
4.
5.
Conc. Nitric Acid See IS. 264-1976.

Standard Silver Nitrate Solution 0.1 N.
Nitrobenzene. (A.R Grade).
Standard Ammonium Thiocyanate Solution 0.1N.
Ferric Ammonium Sulphate Indicator saturated solution.
10.6.3 Procedure
Transfer about 2g of the prepared sample weighed accurately, to a conical flask,
neutralise with nitric acid and then add 5ml of the acid in excess. Add 20ml of
standard silver nitrate solution. Add 3ml of nitrobenzene and shake vigorously.
Titrate with standard ammonium thiocyanate solution using ferric ammonium
sulphate indicator until the colour of indicator changes from colourless to faint
distinct reddish brown colour.
10.6.4 Calculation
Chloride (as NaCl), percent by mass =
5.845 (20N1 VN2)

M
Where
10.7
N1 = normality of standard silver nitrate solution

V = volume in ml of standard ammonium thiocyanate solution used.
N2 = normality of standard ammonium thiocyanate solution, and
M = mass in g of the prepared sample taken for the test.
Page - 45
Rev. No.: 0
10.7.1 Apparatus
1. Nessler Cylinders 100ml capacity.
10.7.2 Reagents
1.
2.
3.
4.
5.
Dilute Hydrochloric Acid- approximately 15 percent (m/V).

Ammonium persulphate
Potassium thiocyanate solution, 5%.
Dilute sulphuric acid 10%.
Standard Iron Solution
Dissolve 0.490 g of ferrous ammonium sulphate [FeSO4(NH4)2SO4.6H2O] in
10 ml of One millilitre of the dilute solution is equivalent to 0.1 mg of iron (as
Fe2O3).
10.7.3 Procedure
Weigh accurately 1.00 g of the prepared sample and dissolve it in about 20 ml of
water. Add about 5ml of hydrochloric acid to make it acidic and 30 mg of
ammonium persulphate and boil to oxidize the iron. Cool and transfer to a
Nessler cylinder, add 5ml of potassium thiocyanate solution, dilute to the mark
with water, and stir well. In to a second Nessler cylinder, add 5ml of hydrochloric
acid and 30 mg of ammonium persulphate, 5ml of potassium thiocyanate solution
and 0.7ml of standard iron solution. Dilute to mark with water. Compare the
colour of the solution in the two cylinders.
The limit prescribed shall be taken as not having been exceed if the intensity of
colour produced with the prepared sample is not greater than that produced by the
standard iron solution.
Page - 46
Rev. No.: 0
11.0
SODIUM HYDROXIDE
11.1
Calculation of Results on Dry Basis

The results in procedures outlined have been calculated on the basis of the
material as received. To convert it on dry basis, the following procedure may be
followed.
For the purpose of this standard, add the percentage of carbonates (as Na 2CO3),
chlorides (as NaCl). Sulphates (as Na 2SO4) and Silicates (as SiO2), and treat the
total as the total dry solid content of the solution. On this basis calculate the
content of the different components on the determined components on the dry
basis. If the total percentage of the determined components of a solution is 50.4
and the percentage of sodium hydroxide contents is 50.2, the percentage of
sodium hydroxide on dry basis will be
50.2 x 100
99.6
50.4
Again in the above example, if the iron content is 10ppm the content of iron on
dry basis will be
10 x 100
19.8ppm
50.4
11.2
Sampling
Precautions shall be taken to protect the samples, the material being sampled, the
sampling instrument and the containers for samples from adventitious
contamination, particularly from absorption of water and carbondioxide. The
sample shall be placed in a clean, dry and airtight alkali resistant glass container
or preferably in a PVC container.
All the container in a single consignment of the material drawn from a single
batch of manufacture shall be marked separately and the groups of containers in
each batch shall be constituting separate lots.
Samples shall be tested from each lot separately for judging the conformity of the
material to the specified requirements. The number of containers (n) to be
selected at random from lots of different sizes (N) shall be as under.
Lot Size (N)
3 to 50
51 to 200
201 to 400
401 to 650
651 and 1000
No. of packages to be
selected (n)
3
4
5
6
7
Page - 47
Rev. No.: 0
The containers shall be drawn at random from the lot, and to ensure randomness,
the following procedure may be adopted.
Arrange all the containers in the lot in a systematic manner, and starting from any
one, count them as 1,2,up to r. Where r is the integral part of N/n. Every rth
container thus counted shall be included in the sample till the required number of
containers specified is taken out.
11.3
Prepared Sample Solution

Weigh accurately about 50g of caustic soda (solid or liquid) in a glass weighing
bottle with ground glass stopper.
11.3.1 Solid material

Dissolve the material in approximately 200 ml of water & cool it to room
temperature, transfer the solution quantitatively to a 500 ml volumetric flask and
dilute nearly to mark, recool then dilute to the mark and mix thoroughly. The
solution prepared will be needed for the subsequent tests.
11.3.2 Liquid Material
Transfer the weighed material directly to a 500-ml volumetric flask and dilute
nearly to the mark, cool to room temperature, then dilute to the mark and mix
thoroughly.
11.4
Determination of Carbonates
(Double Indicator Method)
11.4.1 Reagents
1.
Standard Hydrochloric acid 1N &

0.1N.
2.
3.
Methyl orange indicator solution

Dissolve 0.1g of methyl orange in 100ml of water.
Phenolphthalein Indicator Dissolve
0.1g of phenolphthalein powder in 60ml of rectified spirit and dilute with
water to 100ml.
11.4.2 Procedure
Pipette out 25ml of the prepared sample solution into a control flask and add 2-3
drops of phenolphthalein indicator. Titrate it against standard hydrochloric acid
solution (1 N) upto a little before the end point, Take this reading as (A). Further
titrate it against standard hydrochloric acid (0.1N) till the pink colour just
disappears. Take this reading as (B). Then add 2-3 drops of methyl orange
Page - 48
Rev. No.: 0
indicator and continue titration against standard hydrochloric acid (0.1N) to a
reddish orange colour. Take this reading as (C).
11.4.3 Calculation
Carbonate (as Na2CO3) % by mass
212 (C-B) x N
M
Where
N = Normality of standard hydrochloric acid (0.1N)
M = Mass of the material taken in 11.3 for making the stock solution.
11.5
Determination of Sodium Hydroxide
11.5.1 Principle
The known amount of sample is titrated against standard hydrochloric acid using
methyl orange as indicator.
11.5.2 Reagents
1.
2.
Standard hydrochloric acid (1N).

Methyl orange indicator solution
Dissolve 0.1 g of methyl orange in 100ml of water.
11.5.3 Procedure
Transfer exactly 20ml of the sample solution in a 500ml conical flask. Add
approximately 80ml of water and 5 drops of methyl orange indicator solution and
titrate it against standard hydrochloric acid until the colour of indicator changes
from yellow to orange.
11.5.4 Calculation
Total alkalinity % by mass (B)
V x N x 99.9925
M
Where
V = volume in ml of standard hydrochloric acid solution used
N = Normality of standard hydrochloric acid solution.
Sodium hydroxide (as NaOH) % by mass = B (A x 40/53)
Where
A = Carbondioxide content (as Na2CO3) as calculated
B = Total Alkalinity
Page - 49
Rev. No.: 0
Page - 50
Rev. No.: 0
11.6
Determination of Chlorides
11.6.1 Principle
The sample is titrated with standard silver nitrate solution using ferric alum as
indicator.
11.6.2 Reagents
1.
2.
3.
solution (0.1 N).
4.
5.
solution.
Concentrated nitric acid

Standard silver nitrate solution (0.1N).
Standard ammonium thiocyanate
Nitrobenzene
Ferric Ammonium sulphate saturated
11.6.3 Procedure
11.6.3.1 For Solid Caustic Soda
Weigh accurately about 15g of the material; dissolve it in about 50 ml of distilled
water in a conical flask. Neutralize it with concentrated nitric acid and then add
5ml of the acid in excess. Add 5ml of nitrobenzene and shake vigorously. Pipette
into this 20 ml of standard silver nitrate solution. Tirate it against standard
ammonium thiocyanate solution using ferric ammonium sulphate as indicator.
11.6.3.2 For Caustic Soda lye
Weigh accurately a quantity of the material containing not more than 0.05 g of
chlorides (as NaCl) & carryout the test as prescribed above.
11.6.4 Calculation
1. For Caustic Soda, Pure grade
Chlorides (as NaCl) % by mass
5.845 (20N1 VN2)

M
5.845 (20N1 VN2)

M
2. For caustic Soda Lye

Chlorides as (NaCl) % by mass
Where
N1 =
V =
N2 =
Normality of standard silver Nitrate solution.

volume in ml of standard ammonium thiocyanate solution
used in the specified procedure.
Normality of standard ammonium thiocyanate solution.
Page - 51
Rev. No.: 0
M =
11.7
Mass of in g of the material taken for the test.
Determination of Silicates
11.7.1 Reagents
1.
2.
3.
4.
Concentrated hydrochloric acid.

Dilute hydrochloric acid (6N).
Sulphuric acid (18N).
Concentrated Hydrofluoric Acid. About 48%.
11.7.2 Procedure
Weigh about 25g of the material to the nearest 0.1g, transfer it to a 600ml beaker
and dissolve in 200 ml of water neutralize it with concentrated hydrochloric acid,
& then add 10 ml in excess. Evaporate it to dryness on a water bath. Bake the
residue for one hour at 110oC. Cool & then add 10ml of concentrated
hydrochloric acid and 200ml of water. Heat the solution to boiling and filter it
through a filter paper. (whatmann No. 40 or equivalent). Wash the residue with
hot dilute hydrochloric acid and then with hot water until the residue is free from
chlorides. Evaporate the filtrate to dryness, repeating the above procedure, except
that the residue is washed only with hot water, until free from chlorides. Place the
residue from both the above procedure together with the filter paper in a tared
platinum crucible Dry, char and ignite to constant mass, Add two drops of
sulphuric acid and 2-3ml of hydrofluoric acid to the residue in the platinum
crucible. Evaporate to dryness and drive off the excess sulphuric acid, cool and
weigh again to constant mass.
11.7.3 Calculation
Silicates (as SiO2) % by mass =
100 (M1 M2)

M
Where
M1 = Mass in g of the residue before the addition of concentrated
hydrofluoric acid and drying.
M2 = Mass in g of the residue after the addition of concentrated
hydrofluoric acid and drying.
11.8
Determination of Sulphates
11.8.1 Principle
The sample is acidified and treated with barium chloride solution and estimated
gravimetrically.
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11.8.2 Reagents
1.
2.
Concentrated Hydrochloric acid.

Barium Chloride Solution (10%).
11.8.3 Procedure
Weigh accurately about 10g of the material and dissolve it in 100ml of water.
Add sufficient quantity of concentrated hydrochloric acid to neutralize and add an
excess of aid in the solution. Boil it to decompose the carbonates. Filter the
resulting solution through a folded filter paper thoroughly collecting both the
filtrate and washing in a 500-ml beaker. Dilute it to 250ml boil and add 10 ml of
hot barium chloride solution to the boiling solution. Boil it again for 2 minutes,
let it stand for 4 hours and then filter through a tared sintered glass crucible (G4)
or a tared gooch crucible and precipitate to free it from chlorides and dry to
constant mass at 105 110oC.
Excess barium chloride is necessary to reduce the solubility of barium sulphate.
Precipitation in hot solution by the addition of barium chloride in a slow stream
with stirring minimizes the mechanical occlusion of barium chloride and gives a
coarse precipitate which is less soluble in acid.
11.8.4 Calculation
Sulphates (as Na2SO4) % by mass
60.86 x M1
M2
Where
M1 = Mass in g of the precipitate
M2 = Mass in g of the material taken for test.
11.9
11.9.1 Principle
Iron is estimated in the sample by comparing the colour produced on reaction
with potassium thiocyanate and compared with standards.
11.9.2 Apparatus
1. Nessler cylinders 100ml capacity.
11.9.3
Reagents
1. Concentrated hydrochloric acid.
2. Ammonium persulphate.
3. Potassium thiocyanate (5% solution).
Page - 53
Rev. No.: 0
4. Standard Iron solution.
Dissolve 0.702 g of ferrous ammonium sulphate hexahydrate in 100ml of
water and 10 ml of concentrated sulphuric acid and dilute with water to
1000ml mark. Transfer 100ml, of this solution to 1000ml volumetric flask
and dilute again to 1000ml mark. 1ml of this solution is equivalent to 0.01 mg
of iron (as Fe).
11.9.4 Procedure
1. For Caustic Soda Solid
Transfer 25ml of the prepared sample solution by a pipette, dilute to 50 ml and
acidify it with concentrated hydrochloric acid. Add 30g of ammonium per
sulphate and boil to oxidize the iron. Cool and transfer to a Nessler cylinder,
add 2ml of potassium thiocyanate solution and dilute to 100ml mark with
water. In another Nessler cylinder, take the same amount of concentrated
hydrochloric acid, ammonium persulphate and potassium thio-cyanate
solution, as used with the material and dilute to about 85ml. From a burette
add standard iron solution in small portions at a time so that after dilution to
100ml , the colour obtained matches with that obtained with the material.
2. For Caustic Soda Lye
Weigh accurately an amount of the material containing not more than
0.035mg of iron (as Fe) and carryout the test as mentioned above.
11.9.5 Calculation
1.
For Caustic Soda (pure)

Iron (as Fe) ppm
200 x V
M
Where
V = volume in ml of standard iron solution used.
2.
For Caustic Soda Lye

Iron (as Fe) ppm
10 x V
M
Where
V = volume in ml of standard iron solution used.
M = mass in g of the material taken for the test.
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11.10 Determination of Copper
11.10.1 Principle
The test of copper is carried out by comparing the colour developed usually
against a standard solution of copper.
11.10.2 Reagents
1. Concentrated Sulphuric acid.
2.
pH indicator paper.
3.
Ammonium chloride.
4.
Concentrated Ammonium Hydroxide.
5.
Citric Acid solution.
Dissolve 10.0g of Citric acid (monohydrate) crystals in 100ml of water.
6. Ammonium Hydroxide (3N).
7. Gum Acacia Suspension.
Dissolve 1.0g of gum acacia in 100 ml of boiling water, filter and dilute to
200ml. The solution should be prepared fresh.
8. Tetra Sodium pyrophosphate solution, Dissolve 4.0 g of tetra sodium
pyrophosphate in 100ml of water.
9. Sodium Diethyl Dithio Carbamate solution
Dissolve 0.2g of the sodium diethyl dithiocarbamate in water and make up the
volume to 100ml.
10. Standard copper solution.
Dissolve 0.3928g of copper sulphate pentahydrate (CuSO4.5H2O) in slightly
acidified water and make up the volume to 1000ml in volumetric flask.
Pipette out exactly 10ml of the solution in a 100ml volumetric flask and make
up the volume to 100ml mark. One ml of this solution is equivalent to 0.01mg
of copper.
11.10.3 Procedure
Weigh about 10g material to the nearest 0.1g and transfer it into a 400ml beaker.
Dissolve it in about 20 ml of water & then neutralize with concentrated sulphuric
acid using pH indicator paper. To the neutralized solution add ammonium
chloride and concentrated ammonium hydroxide to precipitate out iron. Heat the
solution to coagulate the precipitate, Filter the precipitate through a Gooch
crucible with an asbestos mat and wash the residue twice with water. Collect the
filtrate and washing in a beaker cover the beaker with a watch glass and then
evaporate it to a volume of about 70ml. Transfer the solution to 100ml Nessler
cylinder. To this add 2ml citric acid solution and add dilute ammonium hydroxide
until a drop of this solution turns the colour of PH indicator paper to PH of about
8.5 Mix the solution thoroughly & then add 10ml of gun acacia suspension, 5ml
of tetra sodium pyrophosphate solution and 10ml of the sodium diethyl
dithiocarbamate solution and dilute to 100ml mark with distilled water.
Page - 55
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To another Nessler cylinder add 2ml of citric acid solution dilute ammonium
hydroxide (till PH 8.5), 10ml gum acacia suspension, 5ml of tetra sodium
pyrophosphate solution, 10ml of sodium diethyl dithio carbamate solution and
then 2ml of standard copper solution. Make upto 100ml mark with distilled water
and mix well. Compare the colour produced in the two cylinders after 10
minutes.
The limit prescribed shall be taken, as not having exceeded if the intensity of
colour produced in the test with the material is not greater than that in the control
test.
11.11 Determination of Manganese
11.11.1 Principle
The colour produced by the test sample on treatment with phosphoric acid,
potassium periodate is compared with reference solution containing standard
manganese solution.
11.11.2 Apparatus
Nessler Cylinder 100 ml capacity
11.11.3 Reagents
1.
2.
3.
Phosphoric acid 85% (manganese free).

Potassium periodate.
Standard Manganese Solution.
Dissolve 0.3077 g of manganese Sulphate monohydrate (MnSO4.H2O) in
water, add 1ml of concentrated sulphuric acid and make up in a volume to
1000ml mark in a volumetric flask. Pipette 10ml of this solution into a
100ml volumetric flask and make upto the mark. 1ml of this solution is
equivalent to 0.01 mg of manganese.
11.11.4 Procedure
Weigh out about 10g of the material to the nearest 0.1g and transfer it into a
400ml beaker and dissolve in about 40ml water. To this solution, add 10-15 ml of
phosphoric acid and 0.6-0.8g potassium periodate. Heat the solution to boiling.
Boil for 20 minutes. Cool solution to room temperature; Transfer the solution to a
100ml Nessler cylinder. Make up to the mark with distilled water and mix well.
Compare the colour with that in the other Nessler cylinder containing 1ml of
standard manganese solution in place of the test solution treated similarly under
similar conditions with the same amount of reagents for the same time as in the
test solutions, and make upto 100ml mark.
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The limit prescribed shall be taken, as not having exceeded if the intensity of
colour produced in the test with the material is not greater than that in the control
test.
11.12 Determination of Matter Insoluble in Water
11.12.1 Reagents
1.
Concentrated hydrochloric acid.
11.12.2 Procedure
Weigh accurately about 50 g of the material and transfer it into a 600ml beaker,
add 300 ml of water and stir until dissolved. Add concentrated hydrochloric acid
till the solution is just alkaline to phenolphthalein. Bring to boil and allow the
solution to settle on the hot plate for 15 minutes. Filter through a weighed gooch
crucible (G4) and wash with hot water to free it from alkali allowing water to
drain completely after each washing. Dry it in an oven for one hour at 105-110oC.
Cool it in a dessicator and weigh.
11.12.3 Calculation
Matter insoluble in water, % by mass =
100 x M1
M2
Where
M1 = Mass in g of the insoluble residue
M2 = Mass in g of the material taken for the test.
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12.0 SODIUM HYPOCHLORITE SOLUTION

12.1 Sampling Instrument
Sampling Tube
It is made of thick glass and is 20 to 40mm in diameter and 400 to 800mm in
length. The upper and lower ends are conical and reach 5 to 10mm diameters at
the narrow ends. Handling is facilitated by two rings at the upper end. For taking
sample, the apparatus is first closed at the top with the thumb or a stopper and
lowered until the desired depth is reached. It is then opened for a short time to
admit the material and finally closed and withdrawn.
For small containers, the size of the sampling tube may be altered suitably.
12.2
Scale of Sampling
In any consignment, all the containers of the same size belonging to the same
batch of manufacture shall constitute a lot. If a consignment is known to consist
of different sizes of containers, the containers belonging to the same batch and
same size shall be grouped together and each such group shall constitute a
separate lot.
For ascertaining the conformity of the material in a lot to the requirement of this
specification, test shall be carried out for each lot separately. For this purpose the
number of containers to be selected from a lot shall be in accordance with the
table below.
Scale of sampling
Lot Size (N)
up to 15
16 to 50
51 to 100
101 to 300
301 and above
selected (n)
2
3
4
5
6
These containers shall be selected at random from the lot. In order to ensure the
randomness of selection, random sampling procedure as given in IS : 4905: 1968
shall be followed.
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12.3 Determination of Relative Density

12.3.1 Principle
Relative density shall be determined by a capillary-stoppered relative density bottle, but
subject to agreement between the purchaser and the supplier, a Twaddle or Baume
hydrometer may also be used.
12.3.2 Procedure
Clean the bottle with a saturated solution of chromic acid in concentrated sulphuric acid
followed by washing with alcohol. Dry the bottle; cool it to room temperature and
weigh. Fill the weighed bottle with water and place it in the constant temperature bath
maintained at 25.0 0.5oC for an hour. Then insert the capillary stopper, which has also
been brought to 25.0 0.5oC. Wipe excess liquid from the top of the stopper, remove the
bottle from the bath, wipe the outside to dryness, and bring to room temperature and
weigh. The difference between the mass of the filled and empty bottle gives the water
equivalent, that is, the mass in air of the water contained in the bottle at 25.0 0.5 oC.
Empty the bottle, rinse several times with alcohol and finally with ether. Remove the
ether fumes with the aid of an air blast and permit the bottle to dry thoroughly. Fill the
bottle with the material, warming both the material and bottle to assist filling and removal
of air bubbles, and then bring the bottle and contents to 25.0 0.5oC. When the
temperature is constant, insert the capillary to 25.0 0.5oC and remove excess liquid
from the top of the stopper. Remove the bottle from the bath, wipe the outside dry, and
bring to room temperature and weigh.
12.3.3 Calculation
Relative density (at 25o/25oC)
M3 M1
M2 M1
Where
M1
M2
M3
12.4
=
=
=
mass in g of the empty relative density bottle;

mass in g of water at 25oC and the relative density bottle; and
mass in g of sodium hypochlorite solution at 25 oC and the relative
density bottle.
AVAILABLE CHLORINE
12.4.1 Principle
The sample is added to an acidified solution of potassium iodide and the released iodine
is titrated with standard sodium thiosulphate solution to the usual starch end point.
Page - 59
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12.4.2 Reagents
1.
2.
3.
4.
5.
Glacial Acetic Acid

Standard Potassium Iodate Solution 0.1 N.
Starch Indicator Solution 0.5 percent.
Mix 0.5 g of soluble starch with 5ml of cold water and add 95 ml of boiling
water. Mix, cool and store in a glass bottle. Replace frequently or add 0.1
percent salicylic acid to the starch solution to minimize deterioration.
Potassium Iodide iodate free.
Standard Sodium Thiosulphate Solution (Hypo) 0.1 N.
Dissolve 25g of sodium thiosulphate (Na2S2O3.5H2O) crystals in freshly
boiled and cooled water, and dilute to 1000ml.
NOTE The solution is more stable if the glassware is cleaned with sulphuric
or chromic acids and thoroughly rinsed with water.
5.1
Standardization of sodium thiosulphate solution

Weigh accurately 3.567g of dry potassium iodate (KIO 3) and transfer to a
1000ml volumetric flask. Dissolve in water, mix thoroughly and make up to
the mark. This solution will be exactly 0.1 N. To standardize the sodium
thiosulphate solution, carefully pipette out a 50ml aliquot of the potassium
iodate solution into a 250ml conical flask and dilute to 100ml with water. Add
1g of potassium iodide crystals. When it is dissolved, add 15ml of 0.1 N
hydrochloric acid and titrate immediately with the sodium thiosulphate
solution. When the solution becomes light yellow, add 1ml of starch indicator
solution and complete the titration to the disappearance of the blue colour.
Standardize at least monthly. Calculate the normality of the sodium
thiosulphate solution as follows:
Normality = (50 x 0.1) / A
Where A is the volume, in ml, of standard sodium thiosulphate solution
required for titration.
12.4.3 Procedure
Dissolve 2 to 3 g of potassium iodide crystals in 50 ml of water in a 250ml
conical flask. Add 10 ml of acetic acid, and then pipette out the aliquot of sample
into the solution, keeping the tip of the pipette beneath the surface of the solution
until drained. Titrate at once with 0.1N standard sodium thiosulphate solution
until the iodine colour is nearly gone, and then add 1ml of starch indicator to the
disappearance of the blue colour.
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12.4.4 Calculation
Available chlorine (as Cl), percent
Mass by volume
Sodium hypochlorite (as NaOCl), percent
mass by volume
=
=
(AN x 0.035 46) x 100

V
(AN x 0.037 22) x 100
V
where
12.5
N
V
=
=
volume in ml of standard sodium thiosulphate solution

required for titration of the sample;
normality of the standard sodium thiosulphate solution; and
volume in ml of original sample in aliquot used.
TOTAL CHLORINE
12.5.1 Principle
All hypochlorites and chlorates present are reduced to chloride by sodium meta
bisulphite in the presence of nitric acid. The total chlorine is then determined by
Volhard method.
12.5.2 Reagents
1. Iron Indicator Solution.
Dissolve 6.25g of ferric ammonium sulphate [Fe2 (SO4)3.(NH4)2
SO4.24H2O] in 50 ml of water and add 45ml of nitric acid.
2. Concentrated Nitric Acid See IS 264: 1976.
3. Standard Sodium Chloride Solution 0.05N.
Dissolve 2.923 g of pure sodium chloride (NaCl) in water and dilute to
1000ml.
4. Standard potassium thiocyanate solution 0.05N.
Prepare a 0.05N solution of potassium thiocyanate (KCNS) and
standardize against 0.05N standard silver nitrate.
5. Standard Silver Nitrate Solution 0.05 N.
Dissolve 8.5 g of silver nitrate (AgNO3) in water and dilute to 100ml.
Store in an amber-coloured glass-stoppered bottle. Standardize the
solution as follows:
Standardisation of silver nitrate solution.
Pipette out 25ml of the standard 0.05 N sodium chloride solution into a 250-ml
conical flask resting on a white porcelain tile, and add 1 ml of potassium
chromate indicator. Add the silver nitrate solution slowly from a burette, swirling
the liquid constantly until the red colour formed by the addition of each drop
begins to disappear slowly; this is an indication that most of the chloride has been
Page - 61
Rev. No.: 0
precipitated. Continue the addition dropwise until a faint but distinct reddishbrown colour persists after vigorous shaking.
Determine the indicator blank correction by adding 1ml of the indicator to a
volume of water equal to the final volume in the titration and then silver nitrate
solution until the colour of the blank matches to that of the solution titrated. The
indicator blank correction should not amount to more than 0.03 to 0.1 ml of silver
nitrate solution. Repeat the titration with two further 25ml portions of the sodium
chloride solution. The titration readings should agree within 0.1 ml.
6. Sodium Metabisulphite (Na2S2O5) Powder.
7. Potassium Chromate 5 percent (m/v).
12.5.3 Procedure
To a 250ml beaker add 50 ml of water and about 0.5g of sodium metabisulphite
powder. Then pipette into the mixture a sample aliquot of the same size as used
for available chlorine and chlorate. Add about 10 drops of nitric acid to acidify
the solution and boil until the entire sulphur dioxide has been expelled. Cool to
room temperature and add 5ml of iron indicator solution. From a burette add 0.5
ml of 0.05 N potassium thiocyanate solution (see Note 1). Then titrate to complete
decolourisation with 0.05 N silver nitrate solution. Filter off the precipitate by
suction and wash three times with water (see Note2). Finally, back titrate the
filtrate and washings with 0.05 N potassium thiocyanate solution until a faint
reddish colour persists.
NOTES
1. The small amount of potassium thiocyanate solution serves as an indicator to
show when an excess of standard silver nitrate solution has been added. The
back titration is continued from the same burette and the total volume of
potassium thiocyanate solution used is noted and used in the calculation.
2. For less accurate work the filtration may be avoided by adding 1 ml of
nitrobenzene to coagulate the suspension before back-titrating the excess silver
nitrate solution.
12.5.4 Calculation
Total chlorine (as Cl), percent by volume
(CN1 DN2) x 3.546

V
Where
C = volume in ml of standard silver nitrate solution required for titration
of the sample;
D = volume in ml of standard potassium thiocyanate solution required for
back-titration;
N1 = normality of standard silver nitrate solution;
N2 = normality of standard potassium thiocyanate solution; and
V = volume in ml of original sample in aliquot used.
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12.6
Free Alkali
12.6.1 Principle
The sample is added to a neutralized, mixed solution of barium chloride and
hydrogen peroxide, which precipitate any carbonate and reduces the hypochlorite
to chloride. The free alkali is then titrated with standard hydrochloric acid using
phenolphthalein indicator.
12.6.2 Reagents
1. Barium Chloride Solution 10 percent (m/v).
Dissolve 100g of barium chloride (BaCl2.H2O) in water and dilute to 1000ml.
Filter, if the solution is turbid.
2. Standard Hydrochloric Acid 0.1 N.
3. Hydrogen Peroxide Solution 3 percent (v/v).
4. Phenolphthalein Indicator Solution 0.5 percent (m/v).
Dissolve 0.5g of phenolphthalein in 60ml of 95 percent ethyl alcohol and
dilute to 100ml with water.
5. Sodium Hydroxide Solution 0.4 percent (m/v).
12.6.3 Procedure
Place 50ml of barium chloride solution and 30ml of hydrogen peroxide solution in
a 250ml conical flask, add 10 drops of phenolphthalein indicator solution and
neutralize with caustic soda solution. Introduce into this neutral mixture 10ml of
the liquid bleach, shake or stir vigorously for 1 minute, and titrate caustic soda
solution with 0.1 N hydrochloric acid until the pink colour disappears.
12.6.4 Calculation
From alkali (NaOH), g/l
(V1N x 40)
V
Where
V1
12.7
volume in ml of standard hydrochloric acid solution

required for titration of sample;
N
=
normality of standard hydrochloric solution acid; and
V
=
volume in ml of original sample solution in aliquot used.
FREE SODIUM CARBONATE
12.7.1 Principle
For determining free sodium carbonate, a number of determinations like total
alkalinity, free sodium hydroxide and sodium bicarbonate are required. Finally,
free carbonate is estimated from the data obtained.
Page - 63
Rev. No.: 0
12.7.2 Total Alkalinity (as Sodium Monoxide)
12.7.2.1 Reagents
1. Standard hydrochloric acid 0.1 N.
2.
Dilute hydrogen peroxide solution 10 percent.
3.
Standard sodium hydroxide solution 0.1 N.
4.
Mixed indicator
Mixture of 3 parts of 2 percent of methyl red in alcohol and 1 part of 0.1
percent of bromocresol green in alcohol.
12.7.2.2 Procedure
Use a volume of sample solution to require at least 10 ml of 0.1 N standard
hydrochloric acid for titration. Add the sample to three times its volume of
hydrogen peroxide solution, previously neutralized with 0.1 N sodium
hydroxide solution, using methyl red-bromocresol mixed indicator solution.
Add a few drops more of the indicator solution and titrate to the end point with
0.1 N hydrochloric acid.
12.7.2.3 Calculation
Total alkalinity (as sodium monoxide), g/l
V1 x N x 31
V
Where
V1
N
V
=
=
=
volume in ml of standard hydrochloric acid;

normality of hydrochloric acid; and
12.7.3 Free Sodium Hydroxide

12.7.3.1 Reagents
Dilute barium chloride solution 10 percent (m/v).
12.7.3.2 Apparatus
pH meter
12.7.3.3 Procedure
Place 50 ml of barium chloride solution and 30 ml of hydrogen peroxide
solution in a 250ml beaker and, using a pH meter, bring the pH to 7.5-with 0.1
N sodium hydroxide solution. Introduce into this solution 10ml of the sample
solution, stir vigorously for 1 min, and ttirate with 0.1 N hydrochloric acid to a
pH of 7.5 while continuing to stir the solution
Page - 64
Rev. No.: 0
Sodium hydroxide (as NaOH), g/l =
V1 x N x 40
V
Where
V1
N
V
=
=
=
Volume in ml of standard hydrochloric acid;

Normality of hydrochloric acid and
Volume in ml of original sample solution in aliquot used.
12.7.3 Sodium Bicarbonate

If no free sodium hydroxide is found, sodium bicarbonate may be present and can
be determined as follows.
Place in a 250ml conical flask a volume of 0.1N sodium hydroxide solution equal
to the volume of 0.1N hydrochloric acid required for the determination of total
alkalinity. Into this solution, add by pipette the same volume of sample solution as
used for the determination of total alkalinity. In a 250 ml beaker, place 50ml of
barium chloride solution, 30ml hydrogen peroxide and 10 drops of
phenolphthalein indicator solution, neutralize with 0.1N sodium hydroxide
solution. Add this neutralized solution to the prepared sample solution and shake
vigorously for 1min. Titrate the excess sodium hydroxide with 0.1N hydrochloric
acid to the disappearance of the pink colour.
Sodium bicarbonate (as NaHCO3) g/l
(V1N1 V2N2) x 84
V
Where
V1
N1
V2
N2
V
=
=
=
=
=
volume in ml standard hydroxide solution;

normality of sodium hydroxide solution;
volume in ml of hydrochloric acid;
normality of hydrochloric acid; and
If sodium hydroxide is present, calculate free sodium carbonate as follows:

Free sodium carbonate (as Na2CO3), g/l
= [Total alkalinity 0.775 (sodium hydroxide)] x 1.709
If sodium bicarbonate is present, calculate free sodium carbonate as follows:
Free sodium carbonate (as Na2 CO3), g/l
= [Total alkalinity 0.369 (sodium bicarbonate)] x 1.709
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12.8
IRON
12.8.1 Apparatus
12.8.2 Reagents
1.
2.
3.
Ammonium Persulphate.
Butonolic Potassium Thiocyanate Solution
Dissolve 10g of potassium thiocyanate in 10ml of water. Add sufficient nbutanol to make up to 100ml and shake vigorously till the solution is clear.
Standard Iron Solution A
Dissolve 0.7022g ferrous ammonium sulphate [FeSO4(NH4)2SO4.6H2O] in
100ml of water, add 5ml of 1:5 (v/v) sulphuric acid followed by potassium
permanganate (0.2 percent, m/v) until a slight pink coloration remains
after stirring well. Dilute with water to 1000ml and mix thoroughly. One
millimeter of this solution contains 0.1 mg of iron as Fe.
Standard Iron Solution B
Take 100 ml of the standard iron Solution A and dilute to 1000ml with
water in a 1000ml volumetric flask. This dilute solution should be
prepared fresh. One millimeter of this solution contains 0.01mg of iron
(as Fe).
4.
12.8.3 Procedure
12.8.3.1 For Grade 1
Weigh 50.0g of the material and evaporate almost to dryness. Dilute it to 30 ml;
add about 30 mg of ammonium persulphate and 15ml of butanolic potassium
thiocyanate solution. Make up to 50 ml, shake vigorously for about 30 seconds
and allow the layers to separate. Carry out a control test in another Nessler
cylinder using 2ml of standard iron Solution B. Compare the intensity of the
colour produced in the butanol layers in the two cylinders.
12.8.3.2 For Grade 2
Carry out the test as given for Grade I, using 5ml of the standard iron Solution B
for the control test.
The limit prescribed is taken as not having been exceeded if the intensity of
colour produced with the material is not greater than that produced in the
control test.
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12.9
SODIUM CHLORATE
12.9.1 Principle
Sodium chlorate is reduced with sodium bromide in 8N hydrochloric acid. After
dilution and addition of potassium iodide, the released iodine (equivalent to the
hypochlorate plus chlorate) is titrated with standard sodium thiosulphate solution
and starch indicator.
12.9.2 Reagents
1.
2.
3.
4.
5.
6.
Concentrated Hydrochloric Acid See IS 265: 1987.

Sodium Bromide Solution 10 percent (m/v).
Potassium Iodide Solution 10 percent (m/v).
Standard Sodium Thiosulphate Solution 0.05 N,
Starch Indicator Solution 0.5 percent (m/v).
Sodium Bicarbonate pure grade (see IS 2124: 1974).
12.9.3 Procedure
Pipette out an aliquot of the sample (same amount as used for available chlorine
determination) into a ground glass stopped flask, add 1 ml of concentrated
hydrochloric acid and 0.3g of pure sodium bicarbonate to expel all the air from
the vessel. Then add 20ml of sodium bromide solution followed by 80 ml of
concentrated hydrochloric acid. Stopper the bottle and shake well. Allow
standing for 10 minutes. Add 20 ml of 10 percent potassium iodide solution and
titrate immediately the liberated iodine against 0.05 N sodium thiosulphate
solution using a few drops of starch indicator solution.
Run a blank with all the reagents except the sample by proceeding in the same
manner as that of the test.
12.9.4 Calculation
Sodium chlorate (As NaCIO2), g/l
Where,
V2 =
V1 =
N =
V =
(V2 V1) x N x 17.75

V
volume in ml of sodium thiosulphate, solution used for the test;

volume in ml of sodium thiosulphate solution used for the blank;
normality of sodium thiosulphate solution; and
12.9.5 Reference
A Text Book of Quantitative Inorganic Analysis A.I. Vogel
Page - 67
Rev. No.: 0
13.0
SULPHURIC ACID
13.1
DETRMINATION OF TOTAL ACIDITY
13.1.1
Principle
The material is titrated against standard sodium hydroxide solution using methyl red as
indicator.
13.1.2
Apparatus
Lunge-Rey Pipette
If this pipette is not available, a weighing bottle or a glass ampoule may be used.
13.1.3
1.
2.
13.1.4
Reagents
Standard Sodium Hydroxide Solution, 1 N, freshly standardized.
Methyl Red Indicator
Dissolve 1g of methyl red in 95 percent (v/v) ethanol and dilute to 100ml with
the same ethanol.
Procedure
Accurately weigh about 2g of material with Lunge-Rey Pipette or weighing
bottle. Carefully place the weighing bottle containing the test portion into a
conical flask containing 300ml of cold water. Open the weighing bottle with a
glass rod under water, stopper the flask and shake well. Cool the flask during this
operation. Keep cooling and shaking until the vapours are completely absorbed.
Remove the stopper and rinse it with water, withdraw the glass rod and wash it
with water, collecting the washings in the conical flask. Add two drops of methyl
red indicator solution and titrate to the end point with standard sodium hydroxide
solution.
13.1.5
Calculation
Total acidity (as H2SO4), percent by mass
V x N x 4.904
M
Where
V
N
M
=
=
volume in ml of standard sodium hydroxide solution used

for the titration.
normality of standard sodium hydroxide solution, and
mass in g of the sample taken for the test.
Page - 68
Rev. No.: 0
13.2
13.2.1
13.2.2
DETERMINATION OF RESIDUE ON IGNITION

Procedure
Weigh to the nearest 10mg about 50g of the sample in a platinum or silica dish of
100ml capacity, previously ignited at 80050oC, cooled in a desiccator and
weighed. Evaporate the acid carefully on a sand-bath, heating the dish containing
the test portion. Heat to dryness. Place the dish containing the residue in an
electric furnace heated at 80050oC and keep at this temperature for about 15
minutes. Remove the dish from the furnace heating, cooling and weighing till
constant mass is obtained.
Calculation
Residue on ignition, percent by mass =
M1 x 100
M2
Where
M1
M2
13.3
=
=
mass in g of the residue weighed, and

Mass in g of the sample taken for the test.
DETERMINATION OF IRON
13.3.1 Procedure
Weigh accurately about 50g of the sample in a platinum or silica dish (100ml
capacity). Place on a sand bath and carefully evaporate to dryness. Cool take up
with 2ml of hydrochloric acid and 25ml of water and heat to facilitate dissolution.
Transfer quantitatively to a 100ml one mark volumetric flask, dilute to the mark,
mix and filter, if necessary.
Proceed as described in 8.4 similar to hydrochloric acid.
13.4
DETERMINATION OF LEAD
13.5
Procedure
Prepare a solution of the sample as in the case of 13.3.1 using nitric acid for
dissolving the evaporated residue. Proceed for the determination of lead using
atomic absorption spectrophotometer as per procedure applicable to the
instrument.
13.6
SAMPLING
All the containers in a single consignment of the same grade drawn from a single
batch of manufacture shall constitute a lot. If a consignment is declared to consist
of different batches of manufacture, the batches shall be marked separately and
the groups of containers in each batch shall constitute separate lots.
Page - 69
Rev. No.: 0
Samples shall be tested from each lot separately for judging the conformity of the
material to the requirements of the specification. The number of containers to be
selected from the lots of different sizes shall be in accordance with the table
below.
Lot Size (N)
up to 15
16 to 25
26 to 50
51 to 100
101 to 300
301 to 500
501 to 800
801 to 1000
selected (n)
2
3
4
5
6
7
8
9
Page - 70
Rev. No.: 0
14.0
TRI SODIUM PHOSPHATE
14.1
14.1.1
Principle
A weighed quantity of the sample is dissolved in water and filtered through a
tared sintered crucible. The residue is dried and weighed.
14.1.2
Procedure
Weigh accurately about 10-20g of the material and dissolve in about 150 ml of
water. Filter the insoluble matter, if any through a tared sintered glass crucible
(G-4) or a Gooch crucible. Wash the residue thoroughly with water till it is free
from all soluble compounds and dry to constant mass at 105-110 oC. Cool in a
desiccator and weigh to constant mass.
14.1.3
Calculation
Matter insoluble in water % by mass =
100 M1 / M2
Where
M1
M2
=
=
Mass in g of the residue

Mass in g of the material taken for test.
14.2
Determination of Phosphate Contents
14.2.1
Principle
The method involves the formation of phosphomolybdic acid in a solution free
from ammonium salts followed by its precipitation as the salt of quinoline.
Finally the quinoline phosphomolybdate is titrated with sodium hydroxide using
mixed indicator solution.
14.2.2
Reagents
1.
Quinoline Hydrochloride solution.

Add 20ml of purified quinoline to 500ml of hot water acidified with 25ml
concentrated hydrochloric acid cool & dilute to 1 liter.
Quinoline used shall be purified and distilled as follows: Dissolve the
technical grade quinoline in concentrated hydrochloric acid and add
excess zinc chloride solution. This precipitate quinoline as a complex salt
[(C9H7N)2. ZnCl4] in well-defined crystals. Separate and wash the crystals
with cold dilute hydrochloric acid. Regenerate the pure quinoline by
Page - 71
Rev. No.: 0
sodium hydroxide solution. Dry and distil to yield pure and distilled
quinoline.
2.
3.
4.
5.
14.2.3
Citromolybdate reagents
(a) Dissolve 150 g of sodium molybdate (Na2MoO4.2H2O) in 400ml of
water.
(b) Dissolve 250g of citric acid in 250ml to 300ml of water and 280ml of
concentrated hydrochloric acid.
Pour with stirring solution (a) to (b). Cool & filter through a filter pad. A
slight greenish colour is obtained on mixing which may deepen when
exposed to sunlight. Add in drops a 0.5% (m/v) solution of potassium
bromate to discharge the colour. Store the solution in colored, airtight,
stoppered glass bottles in the dark.
Mixed Indicator solution
Mix 3 volumes of alcoholic phenolphthalein solution and 1 volume of
alcoholic thymol blue solution.
Standard Sodium Hydroxide Solution Carbonate free, 0.5 N and 0.1 N.
Standard Hydrochloric acid 0.5N & 0.1N.
Procedure
Weigh accurately about 2g of the sample into a 250ml measuring flask & add 50
ml of carbondioxide free water. Boil the solution gently for 30 minutes. Cool to
room temperature and make up the volume to 250ml with Carbondioxide free
water. Filter the solution through a filter paper discarding the first 15ml. Transfer
25 ml of the filtered solution by means of a pipette into a 250ml beaker. Add
50ml of Citro-molybdate reagent and heat to boiling. Add 5 drops of quinoline
hydrochloride solution with constant stirring during the addition. Again heat to
boiling and add quinoline hydrochloride solution dropwise with constant stirring
until 2ml have been added. To the gently boiling solution, add quinoline
hydrochloride solution stirring few milliliters a time with constant stirring until a
total of 60ml has been added. A coarsely crystalline precipitate is obtained.
Allow to stand on a hot plate for 15 minutes & then cool to room temperature.
Filter through a filter paper & wash the flask & precipitate with cold water until
they are free from acid.
Transfer the filter paper & the precipitate to the original flask and rinse the funnel
with water into the flask. If necessary wipe the funnel with a small piece of damp
filter paper to ensure complete removal of the precipitate &place the paper in
flask. Dilute to about 100ml with water. Stopper the flask and shake it
vigorously until the pulp & the precipitate are completely disintegrated. Remove
the stopper & wash it with water, returning the washings to the flask. From a
burette add 50ml of 0.5N standard sodium hydroxide solution, shaking the flask
during addition. Shake vigorously until all the precipitate dissolves. Add 1ml of
mixed indicator solution and titrate the excess of sodium hydroxide solution with
Page - 72
Rev. No.: 0
0.5 N hydrochloric acid until the indicator changes from violet to green, blue &
then sharply to yellow.
Carryout a blank determination using all reagents, without the sample and using
exactly. 0.1N standard sodium hydroxide solution & 0.1 N standard hydrochloric
acid instead of 0.5N acid and 0.5N alkali.
14.2.4
Calculation
Phosphate (as P2O5) % by mass
0.136
M
[(V1 V2) {(V3 V4) / 5]
Where
V1
V2
V3
V4
M
= Volumes in ml of 0.5 N sodium hydroxide solution used with the

sample.
= Volume in ml of 0.5 N hydrochloric acid used with the sample
= Volume in ml of 0.1 N sodium hydroxide used in the blank.
= Volume in ml of 0.1N hydrochloric acid used in the blank.
= Mass in g of the material contained in the solution taken or the
test.
14.3
Determination & Phosphate, Carbonate and Free Sodium Hydroxide
14.3.1
Principle
In an aliquot of the solution of material, total alkali and phosphate are titrated
with a standard acid. The acid phosphate formed is precipitated with silver nitrate
and the free acid liberated is titrated with alkali which gives the phosphate
contents. In another aliquot of the solution, carbonates & phosphates are
precipitated with barium chloride and free alkali is determined by titration with
standard hydrochloric acid.
14.3.2
Reagents
1.
2.
3.
4.
5.
6.
7.
8.
Barium Chloride Solution (10%).

Phenolphthalein indicator solution.
Dissolve 0.1 g of phenolphthalein in 100ml of 60 % rectified spirit.
Standard hydrochloric acid 0.1N.
Methyl orange indicator solution.
Dissolve 0.01 g of methyl orange in 100ml of water.
Silver Nitrate Solution (5%).
Benzyl Alcohol.
Methyl red indicator solution.
Dissolve 0.15g of methyl red in 500ml of water.
Standard Sodium Hydroxide solution 0.1N.
Page - 73
Rev. No.: 0
14.3.3
Procedure
Weigh accurately about 5g of the material and dissolve it in water. Filter off
insoluble, if any, and make up the filtrate and the washings to 250ml in a
volumetric flask.
Transfer 25ml aliquot of this solution to a conical flask & add 40-50ml of barium
chloride so that all the phosphate & the carbonates are precipitated off. Add 0.2
ml of phenolphthalein indicator and titrate with standard hydrochloric acid to
colorless end point (V1).
Transfer another 25ml. Aliquot of the solution to a 250ml beaker, add 1 drop of
methyl orange indicator and titrate with standard hydrochloric acid to light pink
end point (V2).
Add sufficient silver nitrate solution to precipitate all the phosphate (35-40 ml are
usually sufficient), 2ml of benzyl alcohol to coagulate all the precipitate and 0.5
ml of methyl red indicator. Titrate the liberated nitric acid with standard sodium
hydroxide solution. The end point shall be from red to yellow (V3).
14.3.4
Calculation
Phosphates (as P2O 5) % by mass
V3 x 3.55 / M
Free Sodium hydroxide (as NaOH) % by mass
V1 x 4.0 / M
Carbonate (as Na2CO3), % by mass
(V2 V3 V1) x 5.30

M
Where
V1}
V2}
Explained in the procedure.
V3}
14.4
DETRMINATION OF SOLUBLE IRON COMPOUNDS
14.4.1
Principle
Iron is determined calorimetrically by measuring the transmittance of reddish

violet colour produced by Ferrous and ferric iron with thioglycollic acid at pH 10.
14.4.2
Apparatus
1.
Spectrophotometer.
2. One mark graduated flasks. 100ml capacity.
Page - 74
Rev. No.: 0
14.4.3
Reagent
1.
2.
3.
4.
5.
14.4.4
Hydrochloric acid - approximately 5 N.

Dilute Sodium Citrate Solution (1M)
or Ammonium Citrate Solution (2M). Dissolve 29.4 g of Sodium citrate
in 100ml of water or 43.0 g of ammonium citrate in 100ml of water.
Ammonium hydroxide
approximately 16 N.
Thioglycollate reagent.
Add 20ml of ammonium hydroxide to 30ml of water, and then add a
mixture of 10ml of thioglycollic acid and 40 ml of water.
Standard Iron Solution.
Dissolve 0.702 g of ferrous ammonium sulphate hexahydrate in 10 ml of
dilute sulphuric acid (10% v/v) and dilute with water to 1000ml. One ml
of this solution contains 0.01mg of Iron (as Fe).
Procedure
Take several aliquot of the standard iron solution in one mark graduated flasks
(100ml capacity) and add to each of these flasks 4ml of sodium citrate solution or
2ml of ammonium citrate solution, 5ml of thioglycollate reagent and 15ml of
ammonium hydroxide swirling after each addition. Dilute to the mark and mix
well. After 10 minutes determine the absorbance against a reagent blank at
535nm using 5 cm cell (use 1 cm cell if the colour is too strong). Draw a
calibration curve by plotting concentration (in microgram/ml) against absorbance.
Weigh accurately about 1g of the material and dissolve in 20 ml of water. Add
5ml of dilute hydrochloric acid, stir slowly with a glass rod, cover with
watchglass and boil gently for 15-20 minutes, Cool & transfer to a Nessler flask.
Add 4ml of sodium citrate solution or 2 ml of ammonium citrate solution 5ml of
thioglycollate reagent and 15ml of ammonium hydroxide.
Dilute to mark and after 10minutes determine the absorbance at 535 nm using
5cm cell (use 1cm cell if the colour is too strong). Read the concentration (in
microgram /ml) of this solution from the calibration curve and calculate the total
amount of soluble iron present (as Fe).
14.5
Determination of Nitrogen Compounds
14.5.1
Apparatus
14.5.2
Reagents
1.
Sodium Hydroxide Solution approximately 10 percent.

Page - 75
Rev. No.: 0
2.
3.
4.
5.
14.5.3
Devardas Alloy
Consisting of copper 50 parts, aluminium 45 parts and zinc 5 parts.
Nessler Solution
Dissolve 10g potassium iodide In 10ml of ammonia free water, and add to it
slowly with stirring saturated mercuric chloride solution until a slight
permanent precipitate forms. Add 30g of potassium hydroxide and when it
has dissolved, add 1ml more of mercuric chloride solution, and dilute to
200ml more of ammonia free water. Allow to settle overnight; decant the
clear solution and keep it in a bottle closed with a well-fitting rubber
stopper.
Dilute Hydrochloric Acid approximately 5N.
Standard Ammonium Chloride Solution
Dissolve 0.382g of ammonium chloride in water and make up to exactly
1000ml. One millilitre of this solution contains 0.01mg of nitrogen (as N).
Procedure
Weigh 1.0 g of the material and dissolve in 50ml of water. Add 20ml of sodium
hydroxide solution, 0.5g of powdered Devardas alloy and allow to stand for 2
hours in a distillation flask protected from loss or gain of ammonia. Then slowly
distil 30 to 35ml into 5ml of water containing 1-drop dilute hydrochloric acid.
Transfer to a Nessler cylinder; add 1ml of sodium hydroxide solution and 2ml of
Nessler solution. Make up the volume to 50ml mark. Carry out a control test in
another Nessler cylinder using for comparison 1ml of standard ammonium
chloride solution in place of the material and the same quantities of other reagents
in the same total volume of the reaction mixture.
The limit prescribed can be considered as not having been exceeded if the
intensity of the colour produced in the test with the material is not greater than
that produced in the control test.
14.6
Detrmiantion of Sulphates
14.6.1
Reagents
1.
2.
14.6.2
Dilute Hydrochloric Acid approximately 5N.

Barium Chloride Solution about 10 percent.
Procedure
Weigh accurately about 10g of the material and dissolve in 100ml of water and
2ml of dilute hydrochloric acid. Filter, if necessary; heat the filtrate to boiling;
add slowly, with constant stirring, 5ml of barium chloride solution; and allow to
stand overnight. Filter, wash the precipitate with hot water and ignite at about
800oC. Cool and weigh till constant mass is obtained.
Page - 76
Rev. No.: 0
14.6.3
Calculation
Sulphates (as SO4), percent by mass =
41.15 M1 / M2
Where
M1
M2
14.7
=
=
mass in g of the precipitate, and

mass in g of the material taken for the test.
Determination of Soluble Silica

The method detailed in Section 4.6 may be adopted.
14.8
Determination of Chloride
14.8.1
Apparatus
14.8.2
Reagents
1. Nitric Acid concentrated.
2.
Silver Nitrate 10 percent solution in water.
3.
Standard Chloride Solution
Dissolve 824.1mg sodium chloride (AR Grade, dried at 140oC) in chloride
free water and dilute to 1000ml. One milliliter of this solution contains
500g of chloride as Cl.
14.8.3
Procedure
Dissolve 1g of the sample in 20ml of water and add 3ml of concentrated nitric
acid to 50ml in a Nessler cylinder. The turbidity produced shall not be greater
than that produced by 2ml of standard chloride solution for technical grade and
1ml of AR Grade of material diluted to the same with all the reagents.
14.5
Sampling
All the containers in a single consignment of the material drawn from a single
batch of manufacturer shall constitue a lot. If a consignment is declared or known
to consist of different batches of manufacture, the batches shall be marked
separately and the groups of containers in each batch shall constitute separate lots.
Samples shall be tested for each lot for ascertaining the conformity of the material
to the requirement of the specification.
The number of containers (n) to be selected at random form the lot shall depend
on the size of the lot & shall be in accordance as under.
Page - 77
Rev. No.: 0
Lot Size (N)

up to 15
16 to 40
41 to 110
111 to 180
181 to 300
301 to 500
501 to 800
801 to 1000
Samples in size (n)

3
4
5
6
7
8
9
10
These containers shall be chosen at random from the lot. For random selection
the following procedure should be followed [Refer IS 4905 (1968)]. Arrange all
the containers in the lot in a systematic manner and starting from any container
count them as 1,2,3upto r where r is the integral part of N/n. Every r th
container thus counted shall be withdrawn to constitute the sample.
14.6
Reference
Specifications for Tri Sodium Phosphate IS 573 1992 (fourth revision).
15.0
REVIEW
The Head of Corporate Operation Services will be responsible for reviewing this
document on a 3 yearly basis, or as and when required
Page - 78
Rev. No.: 0
Errata
Correction in the following document may please be made at
appropriate places.
Document title: Analytical Procedures for Raw materials
Document No. : COS-ISO-00-OIN/OPS/CHEM/011
Clause 3.1:
The sample size for lot size (N) of 101 & above
should be read as 13. Due to a printing error it has
been wrongly mentioned as 15 in the document.
Clause 14.8.3:
The procedure should be read as follows:

Dissolve 1g of the sample in 20ml of water and
add 3ml of concentrated nitric acid and 1 ml of
10% silver nitrate solution. Dilute to 50ml in a
Nessler cylinder The turbidity produced shall not
be greater than that produced by 2ml of standard
chloride solution for technical grade and 1ml of
AR Grade of material diluted to the same with all
the reagents.
The underlined sentence in bold italics has been
omitted from the above clause due to a printing
error.
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OPERATION INFORMATION NOTE

Analytical Procedures for Raw

CORPORATE OPERATION SERVICES

National Thermal Power Corporation Ltd.

NATIONAL THERMAL POWER CORPORATION LTD.

Date : January 2004

Analytical Procedures for Raw

Analytical Procedures for Raw Materials

Sodium Hypochlorite Solution

Analytical Procedures for Raw Materials

Lot Size (N)

Sample size (n)

Draw by suitable means a representative portion of the material, sufficient for

Mass in gram of the residue.

National Thermal Power Corporation Ltd.

Mass in gram of the ignited residue.

Alternate Method (By EDTA Titration)

EDTA solution (0.01M)

Diff. Of EDTA (ml) x 0.27 x 25 x 4 x 12.33

3.6 Determination of Soluble Iron Compounds

Concentrated Hydrochloric Acid

Volume in ml of saturated potassium dichromate solution

3.7 Determination of Basicity/Acidity

National Thermal Power Corporation Ltd.

National Thermal Power Corporation Ltd.

National Thermal Power Corporation Ltd.

Normality of sulphuric acid.

Determination of Residue on Evaporation

Nessler Cylinders 25ml capacity.

Barium Hydroxide Solution saturated.

mg/l of PO4 from the calibration curve, and

Dilute hydrochloric acid 1:1 (v/v).

mg of SiO2 from the calibration curve, and

Ordinary Denatured Spirit

National Thermal Power Corporation Ltd.

Determination of Calcium and Magnesium

Ammonia-Ammonium Chloride Buffer Solution

Dilute sulphuric acid 1:1 (v/v)

Test for Reducing Substances

Dilute Sulphuric Acid approximately 5 N.

Test for Pyridine and Homologues

Sampling of Ammonia, Liquor

4.14.1 SCALE OF SAMPLING

National Thermal Power Corporation Ltd.

Sample Size (n)

Determination of available chlorine.

Determination of Available Chlorine

Potassium dichromate solution (0.1N)

Volume in ml of standard sodium thiosulphate solution

% by weight of available chlorine as determined in 5.4.

(W1 W2) x 100

Weight of material taken before drying.

Determination of Particle Size

(W1 W2) x 100

Weight of material taken for sieving.

National Thermal Power Corporation Ltd.

Accurately weigh about 20g of the dried sample. Dissolve it in 200ml of

Determination of Moisture Content

Mass in gram of the material taken for the test

Determination of Matter Insoluble in Water

Mass in gram of the residue

Determination of Total Chlorides