Amendment No. 2 March 2010 TO Is 4032: 1985 Method of Chemical Analysis of Hydraulic Cement

AMENDMENT NO.
2 MARCH 2010
TO
Free amendment provided by BIS via BSB Edge Private Limited to JBS TESTING SOLUTIONSJalandhar([email protected]) 157.39.86.185
IS 4032 : 1985 METHOD OF CHEMICAL ANALYSIS OF
HYDRAULIC CEMENT
( First Revision )
(Page 4, clause 2.1) ― Insert the following at the end:
‘2.2 Preparation of Sample for Analysis ― Keep about 10 g sample in a large

glass Petri dish and spread it evenly into a thin layer. Put it in the oven
maintained at 105 ± 5°C for one hour to remove any superficially adsorbed
moisture. Take it out and keep in a desiccator and cool it to room temperature
for chemical analysis.’
(Page 7, clause 4.1.20) ― Insert the following at the end:
‘4.1.21 Nitrobenzene
4.1.22 Potassium Chromate Indicator ― Dissolve 0.2 g in 100 ml of distilled

water.
4.1.23 Silver Nitrate Solution ― 0.025 N. Dry silver nitrate at 120°C for two
hours and allow to cool in a desiccator. Weigh out accurately 4.246 7 g in a 250
ml beaker, dissolve in little quantity of distilled water and transfer in a one-litre
volumetric flask and make up to the mark.
4.1.23.1 Standardization of 0.025 N silver nitrate solution ― Silver nitrate may

be standardized to check its normality by titrating with a standard solution of
0.025 N sodium chloride.
Preparation of 0.025 N Sodium Chloride ― Dry sodium chloride at 600 ± 50°C

for 50 min and cool in a desiccator. Weigh 1.461 5 g in a 250-ml beaker.
Dissolve in about 50 ml water. Transfer in a one-litre volumetric flask and make
up to one litre.
Take 10 ml of 0.025 N sodium chloride solution in a 250-ml conical flask. Add

2 ml of potassium chromate indicator. Titrate with silver nitrate solution to
slight brick red colour end point. The exact normality of silver nitrate may be
Price Group 2
1
Amend No. 2 to IS 4032 : 1985
calculated using the equation:
N1V1 = N2V2
where
N1 = normality of sodium chloride that is 0.025,
V1 = 10 ml,
N2 = normality of silver nitrate solution, and
V2 = volume of silver nitrate required.
4.1.24 Ferric Alum Indicator ― A saturated solution of ammonium iron (III)

sulphate dodecahydrate [NH4Fe(SO4)12H2O] in distilled water (about 40
percent) is made, to which few drops of 6 N nitric acid are added. 1 ml of this is
used in the titration.
4.1.25 Ammonium Thiocyanate Solution ― 0.025 N. Weigh accurately 1.903 0 g

in a 250-ml beaker, dissolve in about 50 ml water and transfer in a one-litre
volumetric flask. Make up to one litre. This solution needs standardization with
standard silver nitrate solution.
4.1.25.1 Standardization of ammonium thiocyanate solution ― Pipette 20 ml of

standard 0.025 N silver nitrate solution into a 250-ml conical flask, add 5 ml of
6 N nitric acid and 1 ml of ferric alum indicator. Run in the ammonium
thiocyanate solution from a burette. At first a white precipitate is produced,
rendering the liquid a milky appearance and as each additional drop of
thiocyanate falls in, it produces a reddish-brown cloud, which quickly
disappears on shaking. As the end point approaches, the precipitate becomes
flocculent and settles easily; finally one drop of the thiocyanate solution
produces a faint brown colour, which no longer disappears upon shaking. This is
the end point. It is essential to shake vigorously during titration in order to
obtain correct results, because the freshly precipitated silver thiocyanate formed
during the titration adsorbs silver ions, thereby causing a false end point, which
however, disappears with vigorous shaking. Calculate the normality of the
thiocyanate solution by using the normality equation:
N3V3 = N4V4
where
N3 = normality of silver nitrate that is 0.025,
V3 = 20 ml,
N4 = normality of ammonium thiocyanate, and
V4 = volume of ammonium thiocyanate required.
2
Amend No. 2 to IS 4032 : 1985
(Page 7, clause 4.2) ― Substitute the following for the existing:
‘4.2 Loss on Ignition ― Heat about 1 g of oven-dried sample, m1 (accurately

weighed up to four decimal places) for 15 min in a weighed and covered
platinum crucible (a porcelain crucible may also be used) of 20 to 25 ml
capacity by placing it in a muffle furnace at a temperature of 950 ± 25°C; cool
and weigh. Check the loss in weight by a second heating for 5 min and reweigh
(m2). Calculate the loss on ignition as below:
(m1 - m2 ) ´ 100
Percent loss on ignition =
m1
Round off the calculated value and report up to 1 decimal place.’
(Page 7, clause 4.3.1, line 1) ― Substitute ‘Transfer about 0.5 g - 1.0 g, W

(accurately weighed up to four decimal places) of oven dried sample’ for
‘Transfer 0.5 g of the sample’.
(Page 8, clause 4.3.4) ― Substitute the following for the existing formula:
(W1 - W2 ) ´ 100
‘Silica, percent = ’
W
(Page 9, clause 4.4.3.1) ― Substitute the following for the existing
formula:
Weight of residue ´ 100
‘R2O3, percent = ’
W
(Page 12, clause 4.7.1.2) ― Substitute the following for the existing
formula:
Weight of residue ´ 100
‘CaO, percent = ’
W
(Page 13, clause 4.8.1.1) ― Substitute the following for the existing:
W1 ´ 36.22
‘MgO, percent =
W
where
W1 = grams of residue (Mg2P2O7), and
36.22 = molecular ratio of 2 MgO to Mg2P2O7 (0.362 2) × 100’
3
Amend No. 2 to IS 4032 : 1985
(Page 21, clause 4.12.3.1) ― Insert the following at the end:
‘4.13 Chloride
4.13.1 The sample is boiled with dilute nitric acid, thereby dissolving all the
chlorides present. Excess standard silver nitrate solution is added to it. The
chlorides react with silver nitrate forming silver chloride. Excess of silver nitrate
is then back titrated with standard ammonium thiocyanate solution. Ferric alum
is used as an indicator which gives reddish-brown colour at the end point. The
reactions involved are:
Ag+ + Cl– = AgCl
Ag+ + SCN– = Ag SCN
When the reactions are complete, the slightest excess of thiocyanate produces a
reddish-brown colouration due to the formation of complex ferric-thiocyanate
ion:
Fe+++ + SCN = [FeSCN]++
4.13.2 Procedure
4.13.2.1 Dry the sample at 110°C for 1 hour and cool in a desiccator. Take 2 g of
sample accurately weighed up to fourth decimal place in a 250-ml beaker. Add
about 40 ml of distilled water and 10 ml concentrated nitric acid. Heat to boil
and shake thoroughly. Keep for few minutes to settle and then filter through
Whatman No. 40 filter paper in a conical flask. Wash the filter paper along with
its contents 4-5 times with hot distilled water. Reject the insoluble in the funnel.
To the filtrate add 2 ml of nitrobenzene and 10 ml 0.025 N silver nitrate solution
with the help of a micro burette. Then add 1 ml of ferric alum indicator. Titrate
with 0.025 N ammonium thiocyanate solution to get a faint brown colour as
described in 4.1.25.1. Note down the volume of ammonium thiocyanate used.
As the reagents and distilled water, etc, used in the exercise may contain some
chloride as an impurity, it is essential to subtract this to get the actual chloride
content in the sample. For this a blank run is done as given in 4.13.2.2.
4
Amend No. 2 to IS 4032 : 1985
4.13.2.2 Blank ― Take 100 ml distilled water in a conical flask. Add 10 ml
concentrated nitric acid + 10 ml 0.025 N silver nitrate solution, 2 ml
nitrobenzene and 1 ml ferric alum. Titrate with 0.025 N ammonium thiocyanate
solution.
Let ammonium thiocyanate required be y ml
Blank = (10 – y) ml
4.13.3 Calculation
Let ammonium thiocyanate used in the sample titration be x ml
Silver nitrate consumed by the chlorides, Z = [10 – (10 – y) – x ] ml

Z ´ 0.035 46 ´ 0.025 ´ 100
Percent chloride, Cl =
Mass of sample
NOTE ― The calculation is based on the normalities of silver nitrate and ammonium
thiocyanate to be exactly same, that is, 0.025. In case the normalities differ, then correction
may be applied using appropriate factor.
4.13.4 Repeatability and Reproducibility
The standard deviation of repeatability of the method is 0.005 percent. The

standard deviation of reproducibility is 0.010 percent.’
(Page 34, clause 6.12.3) ― Insert the following at the end:
‘6.13 The method for determining chloride content in Portland slag cement shall
be the same as described in 4.13.’
(Page 36, clause 7.4) ― Insert the following at the end:
‘7.5 The method for determining chloride content in Portland slag cement shall
be the same as described in 4.13.’
(CED 2)
Reprography Unit, BIS, New Delhi, India
5

Amendment No. 2 March 2010 TO Is 4032: 1985 Method of Chemical Analysis of Hydraulic Cement

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AMENDMENT NO.

(Page 4, clause 2.1) ― Insert the following at the end:

‘2.2 Preparation of Sample for Analysis ― Keep about 10 g sample in a large

(Page 7, clause 4.1.20) ― Insert the following at the end:

4.1.22 Potassium Chromate Indicator ― Dissolve 0.2 g in 100 ml of distilled

4.1.23.1 Standardization of 0.025 N silver nitrate solution ― Silver nitrate may

Preparation of 0.025 N Sodium Chloride ― Dry sodium chloride at 600 ± 50°C

Take 10 ml of 0.025 N sodium chloride solution in a 250-ml conical flask. Add

4.1.24 Ferric Alum Indicator ― A saturated solution of ammonium iron (III)

4.1.25 Ammonium Thiocyanate Solution ― 0.025 N. Weigh accurately 1.903 0 g

4.1.25.1 Standardization of ammonium thiocyanate solution ― Pipette 20 ml of

‘4.2 Loss on Ignition ― Heat about 1 g of oven-dried sample, m1 (accurately

(Page 7, clause 4.3.1, line 1) ― Substitute ‘Transfer about 0.5 g - 1.0 g, W

Ag+ + Cl– = AgCl

Ag+ + SCN– = Ag SCN

Fe+++ + SCN = [FeSCN]++

Let ammonium thiocyanate required be y ml

Let ammonium thiocyanate used in the sample titration be x ml

Silver nitrate consumed by the chlorides, Z = [10 – (10 – y) – x ] ml

4.13.4 Repeatability and Reproducibility

The standard deviation of repeatability of the method is 0.005 percent. The

(Page 34, clause 6.12.3) ― Insert the following at the end:

(Page 36, clause 7.4) ― Insert the following at the end:

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