Indian Standard (First Revision) : Method of Chemical Analysis of Hydraulic Cement

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IS : 4032 – 1985
(Reaffirmed 2000))
( Reaffirmed 2005
Edition 2.1
(1998-05)
Indian Standard (Reaffirmed!2014)!
(Reaffirmed 2019)
METHOD OF CHEMICAL
ANALYSIS OF HYDRAULIC CEMENT
( First Revision )
(Incorporating Amendment No. 1)
UDC 666.971.4 : 543
© BIS 2004
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
Price Group 9
IS : 4032 – 1985
Indian Standard
METHOD OF CHEMICAL
( First Revision )
Cement And Concrete Sectional Committee, BDC 2
Chairman Representing
DR H. C. VISVESVARAYA National Council for Cement and Building Materials,
New Delhi
Members
ADDITIONAL DIRECTOR STANDARDS Research, Designs & Standards Organization
(B & S) (Ministry of Railways), Lucknow
DEPUTY DIRECTOR STANDARDS
(B & S) ( Alternate )
SHRI K. P. BANERJEE Larsen and Toubro Limited, Bombay
SHRI HARISH N. MALANI ( Alternate )
SHRI S. K. BANERJEE National Test House, Calcutta
CHIEF ENGINEER (BD) Bhakra Beas Management Board, Nangal Township
SHRI J. C. BASUR ( Alternate )
CHIEF ENGINEER (DESIGNS) Central Public Works Department, New Delhi
EXECUTIVE ENGINEER (D) III
( Alternate )
CHIEF ENGINEER (RESEARCH)- Irrigation and Power Research Institute, Amritsar
CUM-DIRECTOR
RESEARCH OFFICER (CONCRETE
TECHNOLOGY) ( Alternate )
DIRECTOR A. P. Engineering Research Laboratories, Hyderabad
JOINT DIRECTOR ( Alternate )
DIRECTOR Central Soil and Materials Research Station,
New Delhi
CHIEF RESEARCH OFFICER
( Alternate )
DIRECTOR (C&MDD-I) Central Water Commission, New Delhi
DEPUTY DIRECTOR (C&MDD-I)
( Alternate )
SHRI V. K. GHANEKAR Structural Engineering Research Centre (CSIR),
Roorkee
( Continued on page 2 )
© BIS 2004
This publication is protected under the Indian Copyright Act (XIV of 1957) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 4032 – 1985
( Continued from page 1 )
Members Representing
SHRI A. V. GOKAK Development Commissioner for Cement Industry
(Ministry of Industry), New Delhi
SHRI S. S. MIGLANI ( Alternate )
SHRI S. GOPINATH The India Cements Limited, Madras
SHRI T. TAMILAKARAN ( Alternate )
SHRI A. K. GUPTA Hyderabad Industries Limited, Ballabagarh
SHRI P. J. JAGUS Associated Cement Companies Ltd, Bombay
DR A. K. CHATTERJEE ( Alternate )
SHRI N. G. JOSHI Indian Hume Pipes Co Limited, Bombay
SHRI R. L. KAPOOR Ministry of Shipping and Transport (Roads Wing)
SHRI N. SIVAGURU ( Alternate )
SHRI S. K. LAHA The Institution of Engineers (India), Calcutta
SHRI B. T. UNWALLA ( Alternate )
DR A. K. MULLICK National Council for Cement and Building Materials,
New Delhi
SHRI K. K. NAMBIAR In Personal Capacity ( ‘Ramanalaya’ 11 First Cresent
Park Road, Gandhinagar, Adyar, Madras )
SHRI S. N. PAL M. N. Dastur and Company Private Limited, Calcutta
SHRI BIMAN DASGUPTA ( Alternate )
SHRI H. S. PASRICHA Hindustan Prefab Limited, New Delhi
SHRI Y. R. PHULL Indian Roads Congress, New Delhi; and Central Road
Research Institute (CSIR), New Delhi
SHRI M. R. CHATTERJEE ( Alternate )
DR MOHAN RAI Central Building Research Institute (CSIR), Roorkee
DR S. S. REHSI ( Alternate )
SHRI A. V. RAMANA Dalmia Cement (Bharat) Limited, New Delhi
DR K. C. NARANG ( Alternate )
SHRI G. RAMDAS Directorate General of Supplies and Disposals,
New Delhi
DR A. V. R. RAO National Buildings Organization, New Delhi
SHRI J. SEN GUPTA ( Alternate )
SHRI R. V. CHALAPATHI RAO Geological Survey of India, Calcutta
SHRI S. ROY ( Alternate )
SHRI T. N. SUBBA RAO Gammon India Limited, Bombay
SHRI S. A. REDDI ( Alternate )
DR M. RAMAIAH Structural Engineering Research Centre (CSIR),
Madras
DR A. G. MADHAVA RAO ( Alternate )
SHRI A. U. RIJHSINGHANI Cement Corporation of India, New Delhi
SHRI C. S. SHARMA ( Alternate )
SHRI H. S. SATYANARAYANA Engineer-in-Chief’s Branch, Army Heqadquarters,
New Delhi
SHRI V. R. KOTNIS ( Alternate )
SECRETARY Central Board of Irrigation and Power, New Delhi
SHRI K. R. SAXENA ( Alternate )
SUPERINTENDING ENGINEER Public Works Department, Government of
(DESIGNS) Tamil Nadu, Madras
EXECUTIVE ENGINEER
(SMD DIVISION) ( Alternate )
2
IS : 4032 – 1985
Indian Standard
METHOD OF CHEMICAL
( First Revision )
0. F O R E W O R D
0.1 This Indian Standard (First Revision) was adopted by the Indian
Standards Institution on 30 October 1985, after the draft finalized by
the Cement and Concrete Sectional Committee had been approved by
the Civil Engineering Division Council.
0.2 Standard methods of testing cement are essential adjuncts to the
cement specifications because faulty test methods may lead to
erroneous conclusions as to the quality of cement. The Cement and
Concrete Sectional Committee has, therefore, formulated methods of
chemical and physical tests of hydraulic cements in details in two
separate standards which could be referred to in each of the
specification for different types of hydraulic cement. This standard
covers methods of chemical analysis of hydraulic cement while
methods of physical tests are covered in IS : 4031-1968*.
0.3 This standard was first published in 1968. A need has been felt to
introduce rapid methods of chemical analysis of cement to cut down
the time taken for determination of major constituents. In this
revision, therefore, rapid complexometric (EDTA) methods developed
by National Council for Cement and Building Materials have been
included as alternate methods for estimation of CaO, MgO, Fe2O3 and
Al2O3 in ordinary and low heat Portland cement, rapid hardening
Portland cement, Portland slag cement and Portland pozzolana
cement. In case of dispute or doubtful marginal values, the
gravemetric methods for estimation of CaO, MgO and Al2O3 and
potassium permanganate method for estimation of Fe2O3 shall be
taken as referee method. For rapid complexometric methods of
analysis, photometric end point detector shall be used for better
detection of sharp end point where sufficient skill is not available.
0.4 This edition 2.1 incorporates Amendment No. 1 (May 1998). Side
bar indicates modification of the text as the result of incorporation of
the amendment.
*Methods of physical tests for hydraulic cement.
3
IS : 4032 – 1985
0.5 For the purpose of deciding whether a particular requirement of
this standard is complied with, the final value, observed or calculated,
expressing the result of a test or analysis, shall be rounded off in
accordance with IS : 2-1960*. The number of significant places
retained in the rounded off value should be the same as that of the
specified value in this standard.
1. SCOPE
1.1 This standard gives the procedure for the chemical analysis of the
different types of hydraulic cement.
1.2 In addition to the tests for chemical requirements prescribed in
different cement specifications, this standard also covers test for
determination of free lime in Portland cement, pozzolanicity test for
Portland pozzolana cement and staining test for masonry cement.
NOTE — Analysis of hydraulic cement may be done using rapid methods such as atomic
absorption spectrophotometer method ( see IS : 12813-1989† ) or X-ray fluorescence
spectrometer method ( see IS : 12803-1989‡ ), or calorimetric analysis ( see
IS : 12423-1988§ ) not covered in this standard. However, in case of dispute or doubtful
marginal values, the method given in this standard shall be taken as referee method.
2. SAMPLING
2.1 The samples of the cement shall be taken as per requirements of
IS : 3535-1966|| and the relevant standard specification for the type of
cement being tested. The representative sample of the cement selected
as above shall be thoroughly mixed before using.
3. REPRODUCIBILITY OF RESULTS
3.1 Blank determinations shall be made on the reagents for each
constituent in the cement and the corrections shall be applied where
necessary. In all cases check determinations shall be made and
repeated if satisfactory checks are not obtained. The difference
between check determinations shall not exceed 0.2 percent for silica
and alumina, and 0.1 percent for other constituents.
The difference between check determinations by EDTA method
shall not exceed 0.2 percent for calcium oxide and magnesia, 0.15
percent for alumina and 0.1 percent for ferric oxide.
*Rules for rounding off numerical values ( revised ).
†Method of analysis of hydraulic cement by atomic absorption spectrophotometer.
‡Method of analysis of hydraulic cement by X-ray fluorescence spectrometer.
§Method for calorimetric analysis of hydraulic cement.
||Methods of sampling hydraulic cements.
4
IS : 4032 – 1985
4. CHEMICAL ANALYSIS OF HYDRAULIC CEMENTS OTHER
THAN PORTLAND SLAG CEMENT AND PORTLAND
POZZOLANA CEMENT
4.1 Reagents and Special Solutions — Unless specified otherwise,
pure chemicals of analytical reagent grade shall be employed in tests,
and distilled water ( see IS : 1070-1977* ) shall be used where the use of
water as a reagent is intended. The following reagents and special
solutions of analytical reagent grades are required ( see IS : 2263-1979†
and IS : 2316-1968‡ ).
4.1.1 Reagents
4.1.1.1 Hydrochloric acid — sp gr 1.16 (conforming to IS : 265-1976§ ).
4.1.1.2 Nitric acid — sp gr 1.42 (conforming to IS : 264-1976||).
4.1.1.3 Sulphuric acid — sp gr 1.84 (conforming to IS : 266-1977¶ ).
4.1.1.4 Phosphoric acid — sp gr 1.7.
4.1.1.5 Hydrofluoric acid — 40 percent.
4.1.1.6 Ammonium Hydroxide — sp gr 0.90.
4.1.1.7 Acetic acid — glacial.
4.1.1.8 Diethylamine — liquid.
4.1.1.9 Sulphosalicylic acid — solid.
4.1.1.10 Potassium periodate — solid.
4.1.2 Dilute Solutions of Reagents — prepare the following dilute
solutions by diluting the reagent with distilled water.
4.1.2.1 Hydrochloric acid — 1 : 1, 1 : 3, 1 : 10 and 1 : 99 (by volume).
4.1.2.2 Nitric acid — 1 : 4, 1 : 33 (by volume).
4.1.2.3 Ammonium hydroxide — 1 : 1 and 1 : 6 (by volume).
4.1.2.4 Sulphuric acid — 1 : 3 (by volume).
4.1.2.5 Phosphoric acid — 1 : 3 (by volume).
4.1.2.6 Sodium hydroxide solution — 4 N (approximately). Dissolve
80 g of sodium hydroxide in 500-ml volumetric flask and make up to
the mark with distilled water.
4.1.2.7 Glycerol — 1 : 1 (by volume).
*Specification for water for general laboratory use ( second revision ).
†Methods of preparation of indicator solutions ( first revision ).
‡Methods of preparation of standard solution for colorimetric and volumetric
analysis ( first revision ).
§Specification for hydrochloric acid ( second revision ).
||Specification for nitric acid ( second revision ).
¶Specification for sulphuric acid ( second revision ).
5
IS : 4032 – 1985
4.1.2.8 Triethanolamine — 1 : 1 (by volume).
4.1.2.9 Ammonium Acetate — 50 percent solution. Weigh 50 g of amm-
onium acetate and make up the volume to 100 ml with distilled water.
4.1.3 Stannous Chloride Solution — Dissolve 50 g of stannous chloride
( SnCl2 ) in 100 ml of hydrochloric acid and dilute to one litre. Keep a
few pieces of pure metallic tin in contact with the solution.
4.1.4 Mercuric Chloride Solution — Prepare a saturated solution [5.6 g
of mercuric chloride ( HgCl2 ) in 100 ml of water should give a
saturated solution at ordinary room temperature].
4.1.5 Manganese Sulphate Solution — Dissolve 35 g of crystalline
manganese sulphate (MnSO4.4H2O) in 250 ml of water. Add 70 ml of
phosphoric acid (sp gr 1.7) and 65 ml of sulphuric acid (sp gr 1.84).
Dilute to 500 ml.
4.1.6 Standard Potassium Permanganate Solution — 0.05 N. Dissolve
about 1.5 g of potassium permanganate (KMnO4) in one litre of water.
Allow it to stand for a week; filter through asbestos mat and keep in a
dark place after standardizing it with pure sodium oxalate.
4.1.7 Ammonium Nitrate Solution — Dissolve 2 g of ammonium
nitrate (NH4NO3) in 100 ml of water.
4.1.8 Methyl Red — 0.1 percent solution.
4.1.9 Ammonium Oxalate Solution — Dissolve 50 g of ammonium
oxalate [ (NH4) 2 C2O4.H2O ] in one litre of water. Also prepare a
dilute solution containing one gram of salt per litre.
4.1.10 Ammonium Hydrogen Phosphate Solution — Dissolve 250 g of
ammonium hydrogen phosphate in one litre of water.
4.1.11 Barium Chloride Solution — Dissolve 100 g of barium chloride
(BaCl2.2H2O) in one litre of water.
4.1.12 Bismuth Nitrate Solution — Weigh about 4 g of bismuth nitrate
pentahydrate [ Bi (NO3)3.5H2O ] in 500-ml beaker. Add 20 ml of acetic
acid. Stir and dilute with about 40 ml water. Filter and transfer the
solution to one litre volumetric flask and make up the volume to the
mark with distilled water.
4.1.13 Buffer Solution — pH 10 — Dissolve 70 g of ammonium
chloride in 570 ml of ammonium hydroxide (sp gr 0.90) and make up to
one litre with distilled water.
4.1.14 Standard Zinc Solution — 0.01 M. Dissolve accurately weighed
0.6537 g of granulated zinc in a minimum quantity of dilute
hydrochloric acid (1 : 1). Make up to the mark with distilled water in
one litre volumetric flask.
6
IS : 4032 – 1985
4.1.15 Standard EDTA Solution — 0.01 M. Dissolve 3.7224 g of
disodium ethylenediamine tetra acetate dihydrate in 400 ml hot water
and make up the volume in one litre flask. Take 10 ml of standard zinc
solution in an Erlenmeyer flask. Add 20 ml buffer solution of pH 10 and
warm to 50 to 60°C. Add 50 mg Eriochrome Black-T indicator and titrate
with EDTA till the colour changes from wine red to clear blue. Note the
volume of EDTA used ( V ). Calculate the molarity of EDTA as follows:
0.01 × 10-
Molarity of EDTA = -------------------------
V
Adjust the molarity to 0.01 M, if required.
4.1.16 Eriochrome Black-T — Grind 100 mg of indicator with 10 g of
sodium chloride till homogeneous mixture is obtained and store in an
airtight polyethylene bottle.
4.1.17 Xylenol Orange — Grind 100 mg of indicator with 10 g of
potassium nitrate till a homogeneous mixture is obtained and store in
an airtight container.
4.1.18 Patton-Reeders Indicator — Grind 100 mg of indicator with 10 g
of sodium or potassium sulphate till a homogeneous mixture is
obtained and store in an airtight bottle.
4.1.19 Thymol Phthalexone Indicator — Grind 100 mg of thymol
phthalexone indicator with 10 g of potassium nitrate till a
homogeneous mixture is obtained and store in an airtight container.
4.1.20 Thymol Blue — 0.1 percent solution in ethyl alcohol ( W/V ).
4.2 Loss on Ignition — Heat 1.00 g of the sample for 15 minutes 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
temperature between 900° and 1000°C; cool and weigh. Check the loss
in weight by a second heating for 5 minutes and re-weigh. Record the
loss in weight as the loss on ignition and calculate the percentage of
loss on ignition to the nearest 0.1. Calculate the percent loss on
ignition as below:
Percent loss on ignition = loss in weight × 100
4.3 Silica
4.3.1 Transfer 0.5 g of the sample to an evaporating dish, moisten with
10 ml of distilled water at room temperature to prevent lumping, add 5
to 10 ml of hydrochloric acid, and digest with the aid of gentle heat and
agitation until the sample is completely dissolved. Dissolution may be
aided by light pressure with the flattened end of a glass rod. Evaporate
the solution to dryness on a steam-bath. Without heating the residue
any further treat it with 5 to 10 ml of hydrochloric acid and then with
an equal amount of water, or pour at once upon the residue 10 to 20 ml
7
IS : 4032 – 1985
of hydrochloric acid (1 : 1). Then cover the dish and digest for
10 minutes on the water-bath or hot-plate. Dilute the solution with an
equal volume of hot water, immediately filter through an ashless filter
paper (Whatman No. 40 or its equivalent), and wash the separated
silica (SiO2) thoroughly with hot water and reserve the residue.
4.3.2 Again evaporate the filtrate to dryness, baking the residue in an
oven for one hour at 105 to 110°C. Then treat the residue with 10 to
15 ml of hydrochloric acid (1 : 1) and heat the solution on water-bath or
hot-plate. Dilute the solution with an equal volume of hot water catch
and wash the small amount of silica it contains on another filter paper.
Reserve the filtrate and washings for the determination of combined
alumina and ferric oxide.
4.3.3 Transfer the papers containing the residues to a weighed
platinum crucible. Dry and ignite the papers, first at a low heat until the
carbon of the filter paper is completely consumed without inflaming,
and finally at 1 100 to 1 200°C until the weight remains constant.
4.3.4 Treat the ignited residue thus obtained, which will contain small
amounts of impurities, with 1 to 2 ml of distilled water, about 10 ml of
hydrofluoric acid and 2 drops of sulphuric acid and evaporate cautiously
to dryness. Finally heat the small residue at 1 050 to 1 100°C for a
minute or two; cool and weigh. The difference between this weight and
the weight of ignited sample represents the amounts of silica:
Silica percent = 200 ( W1 – W2 )
where
W1 = weight of silica + ( insoluble impurities – residue ), and
W2 = weight of impurities.
NOTE — For routine analysis, treatment with hydrofluoric acid may be omitted.
4.3.4.1 To this amount of silica, add the amount of silica recovered
from the residue derived from the combined precipitates of alumina
and ferric oxide as indicated under 4.3.5.
4.3.5 Add 0.5 g of sodium or potassium persulphate to the crucible and
heat below red heat until the small residue of impurities is dissolved in
the melt. Cool, dissolve the fused mass in water, and add it to the
filtrate and washings reserved for the determination of the combined
alumina and ferric oxide.
4.4 Combined Ferric Oxide and Alumina
4.4.1 To the filtrate reserved in 4.3.2 which shall have a volume of
about 200 ml, add a few drops of the methyl red indicator, and heat to
boiling, adding a few drops of bromine water or concentrated nitric
8
IS : 4032 – 1985
acid during boiling in order to oxidize any ferrous iron to the ferric
condition. Then treat with ammonium hydroide (1 : 1) drop by drop
until the colour of the solution becomes distinctly yellow and smells of
ammonia. Bring to boiling the solution containing the precipitates of
aluminium and ferric hydroxides and boil for one minute. In case of
difficulty from bumping experienced while boiling the ammoniacal
solution, substitute the one-minute boiling period by a digestion period
of 10 minutes on a steam-bath or a hot-plate of approximately the
same temperature as of a steam-bath. Allow the precipitate to settle
(which should not take more than 5 minutes), filter through an ashless
filter paper (Whatman No. 41 or equivalent) and wash with 2 percent
hot ammonium nitrate solution. Set aside the filtrate and washings.
NOTE — Two drops of methyl red indicator should be added to the ammonium nitrate
solution, followed by ammonium hydroxide (1 : 1) added dropwise until the colour
just changes to yellow. If the colour reverts to red at any time due to heating, it
should be brought back to yellow by addition of a drop of ammonium hydroxide (1 : 1).
4.4.2 Transfer the precipitate and filter paper to the same beaker in
which the first precipitation was effected. Dissolve the precipitate in
hot hydrochloric acid (1 : 3), dilute the solution to about 100 ml and
re-precipitate the hydroxides ( see Note ). Filter the solution and wash
the precipitate with two 10-ml portions of hot ammonium nitrate
solution. Combine the filtrate and washings, with the filtrate set aside
under 4.4.1 and reserve for the determination of calcium oxide.
NOTE — Alternatively, after the precipitate of the combined hydroxide is dissolved in
hydrochloric acid, it may be diluted up to 100 ml in a volumetric flask. A portion may
be used for precipitating and estimating the hydroxides and another portion may be
used for estimating ferric oxide (instead of dissolving the sample afresh).
4.4.3 Place the precipitate in a weighed platinum crucible, heat slowly
until the papers are charred and finally ignite to constant weight at
1 050 to 1 100°C taking care to prevent reduction, and weigh as
combined alumina and ferric oxide.
4.4.3.1 Calculation — Calculate the percentage of combined ferric
oxide and alumina by multiplying the weight in grams of the residue
by 200 (100 divided by weight of sample used):
R2O3 percent = weight of residue × 200
4.4.4 If silica is suspected to be carried into the filtrate used for this
estimation, proceed as given in 4.4.4.1.
4.4.4.1 Treat the residue in the crucible with a drop of water, about
5 ml of hydrofluoric acid and drop of sulphuric acid and evaporate
cautiously to dryness. Finally heat the crucible at 1 050 to 1 100°C for
1 or 2 minutes, cool and weigh. The difference between this weight and
the weight previously obtained represents the amount of residual
silica. Subtract this amount from the weight of ferric oxide and
9
IS : 4032 – 1985
alumina found under 4.4.3 and add the same amount to the amount of
silica found under 4.3.4.
4.5 Ferric Oxide
4.5.1 Method 1 ( Potassium Permanganate Method ) — To one gram of
the sample, add 40 ml of cold water and, while the mixture is being
stirred vigorously, add 15 ml of hydrochloric acid. If necessary, heat
the solution and grind the cement with the flattened end of a glass rod
until it is evident that the cement is digested fully. Heat the solution to
boiling and treat it with stannous chloride solution added drop by drop
while stirring, until the solution is decolourized. Add a few drops of
stannous chloride solution in excess and cool the solution to room
temperature. Rinse the inside of the vessel with water, and add 15 ml
of a saturated solution of mercuric chloride in one lot. Stir, add 25 ml
of manganese sulphate solution and titrate with standard solution of
potassium permanganate until the permanent pink colour is obtained.
Calculate iron as ferric oxide.
4.5.2 Method 2 ( EDTA Method )
4.5.2.1 Prepare filtrate as given in 4.3.2 and 4.3.5. Mix the filtrates
and make up the volume in a 250-ml volumetric flask.
4.5.2.2 Take 25 ml of solution reserved in 4.5.2.1 and add dilute
ammonium hydroxide (1 : 6) till turbidity appears. Clear the turbidity
with a minimum amount of dilute hydrochloric acid (1 : 10) and add a
few drops in excess to adjust the pH to approximately 1 to 1.5. Shake
well. Then add 100 mg of sulphosalicylic acid and titrate with 0.01 M
EDTA solution carefully to a colourless or pale yellow solution.
4.5.2.3 Calculation — Calculate the percentage of Fe2O3 as below:
1 ml of 0.01 M EDTA ≡ 0.7985 mg of Fe2O3
Iron oxide (Fe2O3) percent = 0.7985 ×V
----------------------------
W -
where
V = Volume of EDTA used in ml, and
W = Weight of the sample in g.
4.6 Alumina
4.6.1 Method 1 ( Gravemetric Method ) — Subtract the calculated
weight of ferric oxide and small amount of silica from the total weight
of oxides found under 4.4.3. The remainder is the weight of alumina
and small amounts of other oxides which are to be reported as alumina.
4.6.2 Method 2 ( EDTA Method ) — Take 25 ml of solution reserved
under 4.5.2.1 and titrate iron at pH approximately 1 to 1.5 with EDTA
10
IS : 4032 – 1985
using sulphosalicylic acid as indicator as given in 4.5.2.2. Add 15 ml
standard EDTA solution. Add 1 ml of phosphoric acid (1 : 3), 5 ml of
sulphuric acid (1 : 3) and one drop of thymol blue into the titration
flask. Add ammonium acetate solution by stirring until the colour
changes from red to yellow. Add 25 ml of ammonium acetate in excess
to obtain pH approximately 6. Heat the solution to boiling for one
minute and then cool. Add 50 mg of solid xylenol orange indicator and
bismuth nitrate solution slowly with stirring until the colour of the
solution changes from yellow to red. Add 2 to 3 ml of bismuth nitrate
solution in excess. Titrate with 0.01 M EDTA solution to a sharp
yellow end point red colour.
4.6.2.1 Calculation — Calculate the percentage of Al2O3 as below:
V = V1 – V2 – ( V3 × E )
where
V = Volume of EDTA for alumina in ml,
V1 = Total volume of EDTA used in the titration in ml,
V2 = Volume of EDTA used for iron ( see 4.5.2.2 ) in ml,
V3 = Total volume of bismuth nitrate solution used in the
titration in ml, and
E = Equivalence of 1 ml of bismuth nitrate solution ( see Note
below )
1 ml of 0.01 M EDTA ≡ 0.5098 mg of Al2O3
0.5098 × V-
Aluminium oxide (Al2O3) percent = -----------------------------
W
where
NOTE — Equivalence of bismuth nitrate solution is obtained as follows:
Transfer 100 ml of bismuth nitrate solution to a 500-ml flask and dilute with about 100 ml
distilled water. Add a few drops of thymol blue solution and ammonium acetrate solution
until the colour changes from red to yellow. Add 50 mg of xylenol orange indicator and
titrate with 0.01 M EDTA solution until the colour changes from red to yellow. The
equivalence (ml of EDTA) of 1 ml of bismuth nitrate solution is calculated as follows:
V4-
E = ---------
100
where
V4 = Volume of EDTA solution in ml.
4.7 Calcium Oxide
4.7.1 Method 1 ( Gravemetric Method ) — Acidify the combined filtrates
set aside under 4.4.2 with hydrochloric acid and evaporate them to a
11
IS : 4032 – 1985
volume of about 100 ml. Add 40 ml of saturated bromine water to the
hot solution and immediately add ammonium hydroxide until the
solution is distinctly alkaline. Boil the solution for 5 minutes or more,
making certain that the solution is at all times distinctly alkaline.
Allow the precipitate to settle; filter and wash with hot water. Wash the
beaker and filter once with nitric acid (1.33) that has been previously
boiled to expel nitrous acid, and finally with hot water. Discard any
precipitate (of manganese dioxide) that may be left on the funnel.
Acidify the filtrate with hydrochloric acid and boil until all the bromine
is expelled. Add 5 ml of hydrochloric acid, dilute to 200 ml, add a few
drops of methyl red indicator and 30 ml of warm ammonium oxalate
solution. Heat the solution to 70 to 80°C and add the ammonium
hydroxide (1 : 1) dropwise, while stirring, until the colour changes from
red to yellow. Allow the calcium oxalate precipitate to stand without
further heating for one hour, with occasional stirring during the first 30
minutes; filter through Whatman filter paper No. 42 or equivalent, and
wash moderately with cold 0.1 percent ammonium oxalate solution. Set
aside the filtrate and washings for estimating magnesia.
4.7.1.1 Dry the precipitate in a weighed, covered platinum crucible,
char the paper without inflaming, burn the carbon at as low
temperature as possible, and finally heat with the crucible tightly
covered in an electric furnace or over a blast lamp at a temperature of
1 100 to 1 200°C. Cool in a desiccator (to guard against absorption of
moisture by ignited calcium oxide) and weigh as calcium oxide. Repeat
the ignition to a constant weight.
4.7.1.2 Calculation — Calculate the percentage of CaO by multiplying
the weight in grams of 200 residue (CaO) by 200 [100 divided by the
weight of sample used (0.5 g)]:
CaO percent = weight of residue × 200
under 4.5.2.1 in a 250-ml concial flask. Add 5 ml of 1 : 1 glycerol with
constant stirring and 5 ml of diethylamine. To this add 10 ml of 4N
sodium hydroxide solution and shake well to adjust pH to highly
alkaline range of 12 or slightly more. Add approximately 50 ml of
distilled water and 50 mg of solid Patton-Reeder’s indicator. Titrate
against 0.01 M EDTA solution to a sharp change in colour from wine
red to clear blue ( see Note ).
4.7.2.1 Calculations — Calculate the percentage of CaO as below:
1 ml of 0.01 M EDTA ≡ 0.5608 mg of CaO
Calcium Oxide (CaO) percent = 0.05608 × 25 × V
-----------------------------------------------
W
12
IS : 4032 – 1985
where
V = Volume of EDTA used in ml, and
NOTE — Manganese interferes with the estimation of CaO. In presence of
manganese, the procedure specified in 6.7.2 may be adopted.
4.8 Magnesia
4.8.1 Method 1 ( Gravemetric Method ) — Acidify the filtrate set aside
under 4.7.1 with hydrochloric acid and concentrate to about 150 ml.
Add to this solution about 10 ml of ammonium hydrogen phosphate
(250 g/l) and cool the solution by placing in a beaker of ice water. After
cooling, add ammonium hydroxide drop by drop, while stirring
constantly, until the magnesium ammonium phosphate crystals begin
to form, and then add the reagent in moderate excess (5 to 10 percent of
the volume of the solution), the stirring being continued for several
minutes. Set the solution aside for at least 16 hours in a cool
atmosphere and then filter, using Whatman No. 42 filter paper or its
equivalent. Wash the precipitate with ammonium nitrate wash solution
(100 g ammonium nitrate dissolved in water, 200 ml of ammonium
hydroxide added and diluted to one litre). Place in a weighed platinum
crucible, slowly char the paper and carefully burn off the resulting
carbon. Ignite the precipitate at 1 100 to 1 200°C to constant weight
taking care to avoid bringing the pyrophosphate to melting. The
product of the weight of magnesia (MgO), pyrophosphate obtained and
a factor, 0.3621, shall be the magnesium content of the material tested.
4.8.1.1 Calculation — Calculate the percentage of MgO as below:
MgO percent = W × 72.4
where
W = grams of residue (Mg2P2O7), and
72.4 = molecular ratio of 2 MgO to Mg2P2O7 (0.362), divided by
weight of sample used (0.5 g) and multiplied by 100.
under 4.5.2.1. Add 5 ml of 1 : 1 triethanolamine with constant shaking
and 20 ml of buffer solution pH 10. Add 50 mg of the solid thymol
phthalexone indicator followed by approximately 50 ml of distilled
water. Titrate it against standard 0.01 M EDTA solution until the
colour changes from blue to clear pink. This titration gives the sum of
calcium and magnesium oxide present in the solution. Titre value of
magnesium oxide is obtained by subtracting the titre value of calcium
oxide from the total titre value.
13
IS : 4032 – 1985
4.8.2.1 Calculations — Calculate the percentage of MgO as given
below:
1 ml of 0.01 M EDTA 0.4032 mg of MgO
≡
0.04032 × 25 × ( V1 – V )
Magnesium oxide (MgO) percent = -----------------------------------------------------------------
W
where
V1 = Volume of EDTA used in this titration in ml,
V = Volume of EDTA used in CaO determination in ml, and
4.9 Sulphuric Anhydride — To one gram of the sample, add 25 ml of
cold water, and while the mixture is stirred vigorously add 5 ml of
hydrochloric acid. If necessary, heat the solution and grind the
material with flattened end of a glass rod until it is evident that the
decomposition of the cement is complete. Dilute the solution to 50 ml
and digest for 15 minutes at a temperature just below boiling. Filter
and wash the residue thoroughly with hot water. Set aside the filter
paper with the residue. Dilute the filtrate to 250 ml and heat to boiling.
Add slowly drop by drop, 10 ml of hot barium chloride (100 g/l) solution
and continue the boiling until the precipitate is well formed. Digest the
solution on a steam-bath for 4 hours or preferably overnight. Filter the
precipitate through a Whatman No. 42 filter paper or equivalent and
wash the precipitate thoroughly. Place the filter paper and the
contents in a weighed platinum or porcelain crucible and slowly
incinerate the paper without inflaming. Then ignite at 800 to 900°C,
cool in a desiccator and weigh the barium sulphate obtained, calculate
the sulphuric anhydride content of the material taken for the test.
4.9.1 Calculation — Calculate the percentage of SO3 as follows:
SO3 percent = W × 34.3
where
W = weight of residue (BaSO4) in g; and
34.3 = molecular ratio of SO3 to BaSO4 (0.343), multiplied
by 100.
4.10 Insoluble Residue — Digest the filter paper containing the
residue set aside under 4.9 in 30 ml of hot water and 30 ml of 2N
sodium carbonate solution maintaining constant volume, the solution
being held at just below the boiling point for 10 minutes. Filter and
wash with dilute hydrochloric acid (1 : 99) and finally with hot water
till the residue is free from chlorides. Ignite the residue in a tared
crucible at 900 to 1 000°C, cool in a desiccator and weigh.
14
IS : 4032 – 1985
4.11 Sodium Oxide and Potassium Oxide — This method covers
the determination of sodium oxide and potassium oxide by flame
photometry using direct intensity procedure.
4.11.1 Reagents and Materials
4.11.1.1 The following reagents and materials are required:
Calcium Carbonate — The calcium carbonate used in the
preparation of the calcium chloride stock solution ( see 4.11.1.2 )
shall contain not more than 0.020 percent total alkalies as sulphate.
Hydrochloric Acid (HCl) ( sp gr 1.19 ) — concentrated hydrochloric
acid.
Potassium Chloride (KCl)
Sodium Chloride (NaCl)
4.11.1.2 Preparation of solution
a) Calcium Chloride Stock Solution — Add 300 ml of water to
112.5 g of calcium carbonate in a 1 500-ml beaker. While stirring
slowly add 500 ml of hydrochloric acid. Cool the solution to room
temperature, filter into a 1-litre volumetric flask, dilute to one
litre, and mix thoroughly. This solution contains the equivalent to
63 000 ppm (6.30 percent) calcium oxide.
b) Sodium Chloride-Potassium Chloride Stock Solution — Dissolve
1.885 8 g of sodium chloride and 1.583 g of potassium chloride
(both dried at 105 to 110°C for several hours prior to weighing) in
water. Dilute to one litre in a volumetric flask and mix
thoroughly. This solution contains the equivalent of 1 000 ppm
(0.10 percent) each of sodium oxide and potassium oxide.
c) Standard Solution — Prepare the standard solutions prescribed
in Table 1 ( see Note ). Measure the required volume of sodium
chloride-potassium chloride stock solutions in calibrated pipettes
or burettes. The calcium chloride stock solutions may be
measured in appropriate graduated cylinders. Place each solution
in a volumetric flask, dilute to the indicated volume and mix
thoroughly.
NOTE — The solutions listed in Table 1 represent the minimum number required. A
greater number of solutions and different concentrations may be used provided there
is no more than 25 ppm difference between the alkali concentrations of any solution
and the solution containing the next larger amount of alkalies.
4.11.2 Laboratory Containers — All glassware shall be made of
borosilicate glass. All polyethyelene containers shall be made of a
high-density polyethylene having a wall thickness of at least one mm.
4.11.3 Flame Photometer — Any type of flame photometer may
be used, provided it may be demonstrated that the required degree of
15
IS : 4032 – 1985
TABLE 1 STANDARD SOLUTIONS
[ Clause 4.11.1.2 (c) ]
STANDARD CONCENTRATION VOLUME OF VOLUME OF FINAL
SOLUTION OF ALKALI CALCIUM NaCl-KCl VOLUME
NUMBER (EXPRESSED) CHLORIDE STOCK OF
AS Na2O OR K2O STOCK SOLUTION SOLUTION
IN STANDARD SOLUTION USED
SOLUTION USED
ppm ml ml ml
1 100 200 200 2 000
2 75 100 75 1 000
3 50 100 50 1 000
4 35 100 25 1 000
5 10 100 10 1 000
6 0 100 0 1 000
7 100 0* 100 1 000
*The calcium-free solution is for use only in determining the correct position of the
wavelength selector for maximum responses to sodium oxide and potassium oxide.
accuracy and precision as indicated below is obtained ( see Note ). The
instrument shall consist of an atomizer and burner; suitable pressure
regulating devices and gauges for fuel and air or oxygen; an optical
system consisting of suitable light-dispersing or filtering devices
capable of preventing excessive interference from wavelengths of light
other than that being measured; and a photosensitive indicating
device capable of measuring direct intensity.
NOTE — After such accuracy is established for a specific instrument, further tests of
instrument accuracy are not required except in cases of dispute when it has to be
demonstrated that the instrument gives results within the prescribed degree of
accuracy by a single series of tests using the designated standard samples. For
normal laboratory testing, it is recommended that the accuracy of the instrument be
routinely checked by the use of either a National Bureau of Standards ‘Standard
Cement’ or cement of known alkali content.
4.11.3.1 Precision of the instrument — To establish that an instrument
provides the desired degree of precision and accuracy, tests shall be
made with the NBS Standard Cement Sample No. 1013, 1015 and
1016, or any other cement samples having alkali oxide (Na2O) and
K2O contents equal to the appropriate certificate value for NBS
Standard Sample No. 1013, 1015 and 1016.
Using the procedures described in 4.11.3.2 make individual
determination with each of the three designated standard cements on
three different days. The average of the results for each alkali oxide
shall not differ from the appropriate certificate value by more than the
16
IS : 4032 – 1985
following amounts ( see Note ):
Sodium Oxide Potassium Oxide
(Na2O) (K2O)
NBS Standard Sample No.1 013 ± 0.02 ± 0.02
The maximum acceptable difference in the percentage of each alkali
between the lowest and highest value obtained shall be 0.04.
NOTE 1 — In the absence of NBS Standard Samples, samples of Indian cements
having alkali oxide contents (Na2O and K2O) and other requirements equivalent to
those of NBS Standard Sample No. 1013, 1015 and 1016 may be used.
NOTE 2 — The presence of silica (SiO2) in solution effects the accuracy of some flame
photometers. In cases where an instrument fails to provide results within the
prescribed degree of accuracy, outlined above tests shall be made on solutions from
which the SiO2 has been removed. For this removal, proceed as follows:
Place 1.000 ± 0.001 g of cement in a platinum evaporating dish and disperse with
10 ml of water using a swirling motion. While still swirling, add 5.0 ml of
hydrochloric acid all at once. Break up any lumps with a flat-end stirring rod and
evaporate to dryness on a steam-bath. Make certain that the gelatinous appearance
is no longer evident. Treat the residue with 2.5 ml of hydrochloric acid and about
20 ml of water. Digest on a steam-bath for 5 to 10 minutes and filter immediately
through a 9-cm medium texture filter paper into a 100-ml volumetric flask. Wash
thoroughly with repeated small amounts of hot water until the total volume of
solution is 80 to 95 ml. Cool to room temperature, dilute to the mark, and mix
thoroughly.
When it has been demonstrated that the removal of silica (SiO2) is necessary to
obtain the required accuracy described above for a specific flame photometer, silica
(SiO2) shall always be removed when making analysis that are used as the basis for
rejection of a cement for failure to comply with specification or where specification
compliance may be in question.
4.11.3.2 Calibration of apparatus — Detailed steps for putting the
instrument into operation will vary considerably with different
instruments and manufacturer’s instructions should be followed for
special techniques or precautions to be employed in the operation,
maintenance, or cleaning of the apparatus. Generally the apparatus
shall be calibrated in accordance with the procedure given below:
a) Turn on the instrument and allow it to warm up in accordance
with the manufacturer’s instructions (a minimum of 30 minutes
is required for most instruments). Adjust fuel and oxygen or air
pressures as required by the instrument being used. Light and
adjust the burner for optimum operation.
b) Where required, select the proper photocell for sodium oxide
(Na2O). For instruments with variable slit widths set the slit
17
IS : 4032 – 1985
opening at the previously determined optimum ( see Note ). Make
any other adjustments that may be necessary to establish the
proper operating conditions for the instrument.
NOTE — For instruments with a variable slit width, proceed with the slit between
fully closed and one fourth open as a preliminary test. Repeat with the slit width
at various settings to determine the smallest slit width that does not result in
instability of the galvanometer needle when set to give full scale readings with
standard solution No. 1. This setting represents the most favourable operating
conditions and should be used in all subsequent tests for a specific elements.
c) For filter instruments, select the proper filter for sodium oxide
(Na2O). For spectral dispersing devices find the correct position
on the wavelength dial for the element to be determined by
atomizing some of the calcium-free solution (solution No. 7) and
moving the wavelength selector slowly back and forth on each
side of the indicated wavelength ( see Note ) for the element until
the point of maximum transmission or intensity is noted. Set the
wavelength selector at the point. The sensitivity controls should
be set so as to give about 95 percent of full scale transmission for
this determination.
NOTE — Where the desired point for a specific element is not indicated, use a
wavelength of 589 mµ for sodium oxide (Na2O) and 767 mµ for potassium oxide
(K2O) as preliminary setting.
d) Rinse the atomizer with each solution prior to taking readings on
that solution. For instruments having total consumptions-type
atomizers rinse with distilled water between tests on each
solution.
e) Atomize standard solution No. 1 (100 ppm) and adjust the proper
gain or sensitivity controls to provide full scale readings (meter
reading of 100 or 100 percent transmittance).
f) Atomize standard solution No. 6 (0 ppm). For instruments
equipped with a zero adjustment knob, set the meter readings at
zero. For dial-transmission instruments record the indicated
minimum transmittance without further adjustment. Repeat the
procedure described in (e) and (f) until no further sensitivity or
zero adjustments are necessary to obtain the full scale reading
and zero (or the indicated minimum transmittance) when going
from one solution to the other.
g) Atomize standard solution No. 2 (75 ppm) and note the scale
reading. Check the zero of minimum reading with alkali-free
standard solution No. 6. Return to the 100 ppm standard solution
No. 1. These last two readings serve to evaluate the reading for
the 75 ppm standard. If they are within one scale division of zero
(or the predetermined minimum) and 100 (or other full scale
transmittance reading) respectively, the meter reading obtained
18
IS : 4032 – 1985
for the 75 ppm solution may be considered correct. If either the
reading for the 0 or 100 ppm standard solution is not within one
scale division of its predetermined value, then the previously
obtained meter reading for the 75 ppm solution No. 2 shall be
rejected. In the latter event, repeat the procedure described in (e)
and (f) and take another reading for the 75 ppm solution. Only
when the 0 ppm and 100 ppm readings are in proper agreement
both before and after taking readings on an intermediate
standard can be regarded as accurate.
h) Determine and record meter or transmission reading for the 50,
25 and 10 ppm solution following the same procedure given in (g).
j) Repeat the entire procedure given in (b) to (h) for potassium oxide
(K2O) making changes in filters, photocells, wavelength,
sensitivity, and slit width as required.
k) Plot calibration curves for each oxide, using suitable linear cross-
section paper with meter reading or transmittancy represented
on the ordinate and percentage of alkali oxide represented on the
abscissa. Draw a smooth curve through the points.
4.11.4 Procedure
4.11.4.1 Solution of cement — Place 1.000 ± 0.001 g of the cement
sample in a 150-ml beaker, disperse with 20 ml of water using a
swirling motion of the beaker. While still swirling, add 5.0 ml of
hydrochloric acid all at once. Dilute immediately to 50 ml with water.
Break up any lumps of cement remaining undispersed with a flat-end
stirring rod. Digest on the steam-bath or hot-plate for 15 minutes, then
filter through a medium texture filter paper into a 100-ml volumetric
flask. Wash beaker and paper thoroughly with hot water, cool contents
of the flask to room temperature, dilute to 100 ml, and mix the solution
thoroughly ( see Note 2 under 4.11.3.1 ).
4.11.4.2 Procedure for determination of sodium oxide — Warm up and
adjust the instrument for the determination of sodium oxide as
described in 4.11.3.2. Immediately following the adjustment and
without changing any instrumental setting, atomize the cement
solution and note the scale reading ( see Note 2 ). Select the standard
solution which immediately bracket the cement solution in sodium
oxide content and observe their readings. Their values should agree
within one division on the scale with the values previously established
during calibration of the apparatus. If not, reset the instrument
controls so that the original calibration point is obtained. Finally,
alternate the use of the unknown solution and the bracketing standard
solution until readings for the unknown agree within one division on
the transmission or meter scale and readings for the standards
19
IS : 4032 – 1985
similarly agree with the calibration points. Record the average of the
last two readings obtained as the value for the unknown solution.
NOTE 1 — The order in determining sodium oxide or potassium oxide is optional. In
all cases, however, the determination should immediately follow the adjustment of
the instrument for that particular constituent.
NOTE 2 — If the reading exceeds the scale maximum, either transfer a 50-ml aliquot
to a 100-ml volumetric flask or, if desired, prepare a new solution by using 0.500 g of
cement and 2.5 ml of hydrochloric acid (instead of 5.0 ml) in the initial addition of
acid. In case the silica has been removed from the 0.5 g sample of cement, treat the
dehydrated material with 1.25 ml of hydrochloric acid and about 20 ml of water, then
digest, filter and wash. In either case add 5.0 ml of calcium chloride stock solution
[ see 4.11.1.2 (a) ] before diluting to mark with water. Determine the alkali content of
this solution as described in 4.11.3.2 and multiply the percentage of alkali oxide
obtained by a factor of 2.
4.11.4.3 Procedure for determination of potassium oxide — Repeat the
procedure described in 4.11.4.2 except that the instrument shall be
adjusted for the determination of potassium oxide.
4.11.4.4 Calculations — From the recorded averages of meter readings
for potassium oxide and sodium oxide in the unknown sample, read
the percentage of each oxide from its respective calibration curve.
Report each oxide to the nearest 0.01 percent.
4.12 Water-Soluble Alkali
4.12.1 The determination of water-soluble alkali should not be
considered as a substitute for the determination of total alkali
according to 4.11. Moreover, it is not to be assumed that in this method
all water-soluble alkali in the cement will be dissolved. Strict
adherence to the procedure described is essential where there is a
specified limit on the content of water-soluble alkali or where several
lots of cement are compared on the basis of water-soluble alkali.
4.12.2 Procedure
4.12.2.1 Weigh 25 to 150 g of sample into a 400-ml beaker and add
250 ml of water ( see Note ). Stir thoroughly and let stand 30 min at
room temperature. Stir again and filter immediately through a
Buchner funnel which contains a well-seated retentive filter paper,
into a 500-ml filtering flask using slight vacuum. Without washing,
transfer the insoluble matter and the paper to the original beaker and
rinse the funnel with 150 ml of water into the beaker containing the
insoluble matter. Stir thoroughly and let stand 30 min at room
temperature. Stir and filter, as above, using a fresh filter paper. Again
return the insoluble matter and the paper to the original beaker. Wash
the funnel with 100 ml of water into the beaker containing the
insoluble matter. Stir thoroughly and let stand 30 min at room
temperature. Stir and filter as above. Quantitatively transfer the
filtrate to a suitable beaker. Acidify the filtrate with 5 ml of
20
IS : 4032 – 1985
concentrated HCl (sp gr 1.19). Stir until cloudiness disappears.
Evaporate the solution to about 400 ml. Cool to room temperature and
transfer quantitatively to a 500 ml volumetric flask. Dilute to 500 ml.
NOTE — The amount of sample taken for analysis should be based on the expected
water-soluble alkali content. Twenty-five grams should be used when the expected
percentage of either water-soluble alkali (Na2O or K2O) is 0.4 or more. When the
expected percentage of each water-soluble alkali is 0.06 or less, a 150-g sample
should be used. For intermediate amounts of water soluble alkali adjust the weight of
sample as follows:
Weight of sample = 8/A
where
A = expected percentage of the alkali present in largest amount.
This procedure gives a test solution containing approximately 80 ppm of the
alkali present in the largest amount.
4.12.2.2 Transfer a 50-ml aliquot of this solution to a 100-ml
volumetric flask. Add 9.0 ml of the stock CaCl2 solution (63 000 ppm
CaO) described in 4.11.1.2 (a) to the 100-ml flask, and dilute the
solution to 100 ml. Determine the sodium and potassium oxide content
of this solution as described in 4.11.4.2 and 4.11.4.3. Record the parts
per million of each alkali in the solution in the 100-ml flask.
4.12.3 Calculations
4.12.3.1 Calculate the percentage of water-soluble alkali expressed as
Na2O, to the nearest 0.01 as follows:
Total water-soluble alkali = A + E
A=W B
-------------------
× 10
D
C = -------------------
W × 10
E = C × 0.658
where
A = percentage of water-soluble sodium oxide (Na2O);
W = weight of cement sample, g;
B = parts per million of Na2O in the solution in the 100-ml
flask;
C = percent of water-soluble potassium oxide (K2O);
D = parts per million of K2O in the 100-ml flask;
E = percentage Na2O equivalent of the K2O; and
0.658 = molecular ratio of Na2O to K2O.
21
IS : 4032 – 1985
5. DETERMINATION ON FREE LIME IN PORTLAND CEMENT
5.1 Object — Three methods of test have been described for
determining free lime content in Portland cement, namely,
Ethanol-Glycerol Method, Ethanol-Glycerol Rapid Method and
Ethylene-Glycol Method. The method described under 5.2 is more
accurate and in cases of dispute, results obtained by this method shall
govern. The other two methods described under 5.3 and 5.4 are given
for these who wish to use shorter or more convenient procedures for
routine determination of free lime content in cement.
NOTE — The Indian Standard Specification for Portland Cement does not specify
requirements regarding free lime content in cement. The determination of free lime in
cement is important from the point of soundness of cement mortar or concrete and
from the point of view of leaching and efflorescence. Excessive free lime leads to
unsoundness in cement; it may also be one of the factors that cause leaching and
efflorescence in concrete and masonry work. No definite conclusions, however, have
been reached in regard to the optimum content of free lime in cement. The Cement and
Concrete Sectional Committee felt that a knowledge of the free lime content in cement
will guide the user specially in those cases where careful control over quality of
concrete or mortar needs to be exercised or where it will be disastrous to have leaching
and efflorescence defacing the exposed surface. This standard has been prepared with
a view to providing a method for determining free lime in cement clinker, cement, etc.
5.2 Ethanol Glycerol Method
5.2.1 Reagents — The following reagents are required.
5.2.1.1 Absolute ethanol — Absolute ethanol shall conform to the
requirements of IS : 321-1964*.
5.2.1.2 Glycerol — Glycerol shall be of the analytical reagent quality
conforming to a purity of about 99 percent. As normally, the water
contained in glycerol is not considered an impurity, it is preferable to
use anhydrous quality or alternatively, glycerol with not more than
5 percent of water. However, glycerol shall be free from acidic or
aldehydic matter. The specific gravity of glycerol when tested with a
pyknometer at 25°C shall be not less than 1.249.
5.2.1.3 Phenolphthalein indicator — Dissolve one gram of phenol-
phthalein in 100 ml of absolute ethanol and neutralize the solution
with sodium hydroxide dissolved in absolute ethanol.
5.2.1.4 Glycerol-ethanol solvent — Prepare a solution consisting of one
part by volume of glycerol and five parts by volume of absolute ethanol.
To each litre of this solution, add 2 ml of the indicator. The solvent
should be slightly alkaline ( see Note 1 ) to the indicator. If the solvent
is colourless, add a dilute solution of sodium hydroxide in absolute
ethanol until a slight pink colour appears. If the initial colour is pink,
remove it with the standard ammonium acetate solution ( see 5.2.1.5 )
*Specification for absolute alcohol ( revised ).
22
IS : 4032 – 1985
and then add the sodium hydroxide solution until a slight pink colour
appears. Heat 60 ml of the solvent to boiling. If the pink colour
persists, add one small drop of the standard solution of ammonium
acetate to the hot solvent. If the pink colour does not disappear, the
solvent contains too much alkali, which should be reduced. The
solvent, if allowed to stand for a considerable length of time, may
become slightly acidic and should be checked and, if necessary,
re-adjusted from time to time ( see Note 2 ).
NOTE 1 — While a solvent that is exactly neutral at the boiling point is the ideal, it is
difficult to prepare due to the end point not being sharp and the danger of adding too
much ammonium acetate. The error due to slight alkalinity is not more than
0.01 percent in a determination of free calcium oxide and may be disregarded. In
preparing the solvent, the end point may be observed better if the solvent is put in a
tall cylinder placed on white paper. The solvent may be observed from the top and
the colour matched with that of acidified solvent in a similar cylinder.
NOTE 2 — Glycerol and ethanol are highly hygroscopic. Every effort shall be made to
avoid exposing them and other materials unnecessarily to moisture and carbon
dioxide in air. Bottles with an outlet near the bottom or fitted with a siphon are
convenient. Alternatively, an automatic pipette attached to storage vessel can be
used. They can be filled to the top and protected with tubes containing soda lime.
Condensers may also be fitted with such tubes at the top.
5.2.1.5 Standard ammonium acetate solution ( 1 ml = 0.005 g calcium
oxide ) — Prepare the solution by dissolving 16 g of crystalline
ammonium acetate ( see Note ) in one litre of ethanol. Standardize this
solution by titrating against pure calcium oxide that is freshly
prepared by calcining pure calcium carbonate or calcium oxalate in a
platinum crucible at 900 to 1 000°C to constant weight. When the
calcined calcium oxide has cooled in a desiccator, perform the
operations described under 5.2.1.6 in quick succession.
NOTE — Ammonium acetate is generally sold in a damp in condition and should be as
dry as possible. It may be dried by placing over a dehydrating agent, such as, sulphuric
acid or fused anhydrous calcium chloride contained in a desiccator for two weeks or more.
5.2.1.6 Grind it in an agate mortar, weigh out 0.05 to 0.06 g into a dry
200 or 250 ml Erlenmeyer flask, and add to 60 ml of the glycerol
ethanol solvent to the flask ( see Note 1 ). In order to minimize the
danger of hydration and carbonation, separate samples of pure
calcium carbonate may be calcined in small sized platinum capsules.
The calcium oxide thus produced is cooled in a desiccator, re-weighed
for a check and introduced in the flask. The grinding of oxide may be
unnecessary if original calcium carbonate is in a finely powdered form.
Disperse the calcium oxide in the solution by shaking the flask and
attach a reflux condenser ( see Note 2 ). Boil the mixture. The
ebullition should be positive but not so violent as to cause bumping or
excessive evaporation. Then remove the condenser and immediately
titrate the solution, while near boiling, with the standard ammonium
23
IS : 4032 – 1985
acetate solution. Replace the condenser and boil the solution again.
Repeat the titrations at intervals ( see Note 3 ). Shake the flask
frequently between titrations to shorten the time required for the
boiling. The titration is complete when no further colour appears in the
solution during continuous boiling for one hour ( see Note 4 ). Calculate
the calcium oxide equivalent of the ammonium acetate solution in
grams per millilitre by dividing the weight of calcium oxide used by the
volume of solution required.
NOTE 1 — Sometimes pure calcium oxide will take on the bottom of the flask,
particularly if the glycerol is anhydrous. This trouble may be avoided putting a few
grams of clean, dry quartz sand in the flask before the introduction of calcium oxide
and solvent.
NOTE 2 — If a new stopper is used and has white powder on it, it should be thorou-
ghly washed before using. A glass tube about 6 mm in diameter and 50 to 100 cm in
length may be used as an air-cooled condenser, but a short condenser is not recom-
mended because a loss of alcohol is liable to occur through evaporation. In such a case
it is necessary to add neutralized ethanol from time to time to maintain the same
proportion of glycerol to ethanol. If the proportion is greater than one to three, a
partial decomposition of cement may take place. Instead of an ordinary flask, plain
tubing and a stopper, a flask with a ground-in glass stopper and condenser tube may
be used, preferably one with standard taper joint. A water-cooled condenser is the
most satisfactory and it may be as short as 30 cm. Some loss of alcohol may also occur
through dripping from the condenser during the titrations and should be
compensated for by the addition of neutralized ethanol.
NOTE 3 — In general, the intervals may be of 20 minutes but they will chiefly depend
on the rapidity of the dissolution of calcium oxide. They may be of 5 to 10 minutes in
the beginning and then be increased to 30 minutes or one hour in the end. If the
solution contains a large amount of dissolved calcium oxide and the boiling is continued
a long time without titration, crystals (probably of calcium glyceride) may form which
dissolve slowly and increase the time required for the completion of the titration.
NOTE 4 — The end point will not be the same for a hot solution and a cold solution,
especially when a large amount of calcium acetate is present. The titration should
always be carried out while the solution is boiling hot. If the end point is determined
accurately, the solution will turn pink upon cooling, and this can serve as evidence
that the end point has not been greatly overstepped.
5.2.2 Procedure — Weigh one gram of finely ground clinker or Port-
land cement ( see 5.2.2.1 ) into a flask, and add 60 ml of the solvent to
the flask and proceed as in the standardization of the ammonium
acetate solution ( see 5.2.1.5 ). The end point is considered to have been
reached when the content of free calcium oxide in the sample does not
increase by more than 0.05 percent during the last two hours of boiling.
5.2.2.1 The method is designed especially for fresh clinker. As the
method does not differentiate between free calcium oxide and free
calcium hydroxide, any free calcium hydroxide that may be present
will be included in the determination and calculated as free calcium
oxide. The method may be applied to cement or aged clinker, if desired,
but the possibility of the presence of free calcium hydroxide should be
kept in mind.
24
IS : 4032 – 1985
The sample shall be fine enough to pass completely through
75-micron IS Sieve. If it is not, take about 1.2 g of the sample and sieve
it through a small, clean, 75-micron IS Sieve. Grind the residue in an
agate mortar until it is fine enough to pass through the sieve. Mix the
ground residue with screened material thoroughly and grind the
mixture rapidly in the agate mortar for two or three minutes. Weigh
approximately about one gram of the ground mixture into the flask for
the determination of free calcium oxide. Avoid unnecessary exposure of
the sample to the atmosphere. If the sample is fine enough to pass
completely through the sieve, grind slightly over one gram as above
before weighing one gram for the determination.
5.2.2.2 No excess of ammonium acetate shall be added at any time
because an excess of it may react with calcium aluminate and silicates.
To avoid such excess, use a small burette or measuring pipette fitted
with a glass stopcock or a rubber pinchcock and small tip which
delivers about 50 drops per millilitre. If the titrations are far apart and
the reagent evaporates in the tip, a few drops may be discarded before
each titration and the drops used in titration may be counted and
converted in terms of millilitres. It is a good precaution to allow a slight
pink colour to remain in the solution after each of the early titrations.
Vigorous boiling is more essential with cement than with pure
calcium oxide and, if possible, should be so conducted that it is not
necessary to shake the flask vigorously at intervals. The flask should
not be shaken vigorously while it is disconnected from the condenser
because the solvent, if superheated, may boil, expel alcohol vapour and
then draw in air carrying water and carbon dioxide. A good procedure
is to bring the solution and sample to boiling rapidly over a Bunsen
flame in the beginning before placing the flask on a hot plate and
connecting it with the condenser. If there is a tendency to bump, it may
be reduced by adding glass beads or pure quartz sand to the flask or
putting a thin mat of asbestos between the flask and the hot plate.
If in the final titrations there is doubt as to the exact end point, add
a drop of the phenolphthalein indicator to the quiescent liquid in the
flask and carefully observe the point where the indicator strikes the
liquid. If no colour appears, the end point has been reached. If the
sample settles during boiling and leaves a partially clear layer of
solution, another way to overcome difficulty in discerning a change in
the colour of the solution is to swirl the flask after the addition of the
solution of ammonium acetate so as to avoid the dispersion of the
sample. A strong daylight lamp with a reflector may be used as an aid
in the discernment of the end point. The contents of the flask may be
matched with similar contents in another flask which contains an
excess of ammonium acetate.
25
IS : 4032 – 1985
If it is necessary to leave the determination incomplete, remove the
flask, add just enough ammonium acetate to discharge the pink colour
and stopper the flask tightly. When renewing the determination, boil
the mixture before repeating the titrations.
5.2.3 Calculation — Calculate the percentage of free calcium oxide to
the nearest 0.1 as follows:
Free calcium oxide (CaO), percent = EV × 100
where
E = CaO equivalent of the ammonium acetate solution in grams
per millilitre, and
V = millilitres of ammonium acetate solution required by the
sample.
5.3 Ethanol-Glycerol Rapid Method
5.3.1.1 Phenolphthalein indicator — Prepare the indicator as
described under 5.2.1.3.
5.3.1.2 Glycerol-ethanol solvent — Prepare the solvent as described
under 5.2.1.4. Either anhydrous barium chloride or sodium chloride is
used to accelerate the solution of free calcium oxide. If anhydrous
barium chloride is used, dissolve it in the solvent on the basis of one
gram per 60 ml of solvent before the solvent is neutralized ( see Note ).
If sodium chloride is used, add 0.5 g of it to the flask that contains
solvent and freshly prepared calcium oxide or sample at the beginning
of the standardization or the determination, as the case may be.
NOTE — A convenient way to prepare a large amount of solvent is to heat barium
chloride crystals at 120 to 130°C for several hours, dissolve them in hot glycerol (100
to 125°C) without grinding and mix the solution with ethanol. If the salt is
dehydrated at a much higher temperature, it may be slow to dissolve in hot glycerol
or solvent, even when ground.
5.3.1.3 Standard ammonium acetate solution ( 0.2 N ) — Prepare and
standardize a solution of ammonium acetate as described
under 5.2.1.5, using an accelerator as specified under 5.3.1.2.
5.3.2 Procedure — Determine free calcium oxide in clinker or Portland
cement as described under 5.2 using anhydrous barium chloride or
sodium chloride as an accelerator ( see 5.3.1.2 ). The end point is
considered to have been reached when the content of free calcium
oxide does not increase by more than 0.05 percent during the last hour
of boiling ( see Note ).
NOTE — If the boiling is too prolonged, the sample may be partially decomposed and
the end point may be obscured by coloured decomposition products.
26
IS : 4032 – 1985
5.3.3 Calculation — Calculate the percentage of free calcium oxide as
described under 5.2.3.
5.3.4 Result — This method has a tendency to give higher results than
the method described under 5.2. Result obtained by this method
should be checked with the other method wherever possible.
5.4 Ethylene-Glycol Method
5.4.1 The ethylene-glycol method is to be used only for estimating free
lime in fresh clinker and freshly ground cement but not with aged
cement.
5.4.2.1 Ethylene glycol shall not contain more than one percent of
water when determined as below:
Take 50 ml of ethylene glycol and 0.5 g of anhydrous copper in a
small flask and shake at intervals for one hour at room
temperature. A greenish-blue colour indicates the presence of water
and the glycol cannot be used. If the colour is only faint green, it
indicates that the water content is below one percent. If the water
content is below one percent, it can be removed by evaporation by
heating the glycol to 120°C for 1 to 2 hours.
5.4.2.2 Bromocresol green indicator — Bromocresol green is blue in
alkaline solution and changes through green and yellowish green to
yellow in acid solution. In aqueous solution, the various colours
correspond to the following pH values:
pH
Blue 5.2
Green 4.5
Yellow 3.8
5.4.2.3 Standard hydrochloric acid — 0.1 N.
5.4.3 Procedure
5.4.3.1 Take one gram of cement in a long-necked Pyrex flask of 100 ml
capacity and add 50 ml of ethylene glycol. Close the flask with a cork
stopper and heat the contents on a water bath for one-half hour to bring
calcium oxide into solution. Keep the temperature of the bath between
60 to 70°C and shake the flask vigorously every five minutes to prevent
the cement from forming lumps. Alternatively, very pure quartz sand
initially washed and thoroughly dried is added to the flask to prevent
the cement from baking. Morover, the cement-ethylene- glycol mixture
is put under the reflux condenser on a water bath at 60 to 70°C. In the
event of stubborn cement necessitating a long time to react, the time
can be cut-down by adding purest water-free methanol to the ethylene
27
IS : 4032 – 1985
glacol (say 15 cc of former to 30 cc of latter) when on boiling for one-half
to one hour under reflux, the solution is ready for titration.
5.4.3.2 Fit into a 5-cc Buchner funnel two filter papers. Carl Schleicher
and Schull No. 597 ‘Selecta’ or equivalent, moisten the paper with a
little ethylene glycol and such tightly against the funnel. Filter off the
solution from the flask quickly using suction, first pouring the clear
solution and then the cement on the filter. Wash the cement on filter
paper thrice with a 10 ml portion of glycol after filtration. Titrate the
filtrate against 0.1 N hydrochloric acid using 3 drops of 1 percent
bromocresol green in absolute alcohol as indicator ( see Note ).
NOTE — Instead of the Buchner funnel, it is possible to filter the solution through a
Jena sintered glass filter No. 3G3. Sintered glass filter should be used only once and
then washed with hydrochloric acid, followed by sodium carbonate solution and
distilled water.
5.4.3.3 Conduct a blank determination with known quantities of
calcium oxide by dissolving in glycol and titrating against 0.1 N hydro-
chloric acid as before. Prepare a graph showing the amount of 0.1 N
hydrochloric acid required for titrating glycol having different
quantities of calcium oxide.
5.4.4 Calculation — Calculate the percentage of calcium oxide present
in the sample by comparing the quantity of 0.1 N hydrochloric acid
required for titration with the graph and determining the equivalent
calcium oxide.
5.5 Precaution
5.5.1 Wherever leaching or bleeding of ethanol glycerol or ethylene
glycol is involved, avoid direct contact with flame. Heating over a bath
or hot plate is recommended.
6. CHEMICAL ANALYSIS OF PORTLAND SLAG CEMENT
6.1 Reagents and Special Solutions — The following reagents and
special solution of analytical reagent grades are required in addition to
those specified in 4.1.
6.1.1 Dilute Solutions of Reagents — Prepare the following dilute
solutions by diluting the reagent with distilled water.
6.1.1.1 Sodium nitrite — five percent (by weight).
6.1.1.2 Ammonium nitrite — two percent (by weight).
6.1.1.3 Phosphoric acid — 1 : 1 (by volume).
6.1.1.4 Ammonium nitrate wash solution — Hundred g of ammonium
nitrate and two hundred g of ammonium hydroxide mixed and diluted
to one litre with distilled water.
28
IS : 4032 – 1985
6.1.2 Standard Potassium Permanganate Solution — 0.03 N. Dissolve
about 0.94 g of potassium permanganate (KMnO4) in one litre of water.
Allow it to stand for a week; filter through asbestos mat and keep in a
dark place after standardizing it against pure sodium oxalate.
6.1.3 Standard Sodium Thiosulphate Solution — 0.03 N. Prepare a
solution of sodium thiosulphate on the basis of 7.4 g of sodium
thiosulphate (Na2S2O3 5H2O) per litre.
6.1.4 Standard Potassium Iodate Solution — 0.03 N. Prepare a
solution of potassium iodate and potassium iodide on the basis of
1.12 g of potassium iodate (KIO3) and 12 g of potassium iodide (KI) per
litre. Standardize the solution as in 6.1.4.1.
6.1.4.1 To a cool solution of one gram of potassium iodide in 300 ml of
water and 10 ml of hydrochloric acid in a 500-ml flask, add about 25 ml
of the standard potassium permanganate solution (0.03 N). Swirl the
solution gently, stopper the flask and let it stand for 5 minutes. Titrate
the liberated iodine with the standard sodium thiosulphate solution
until the colour nearly fades. Add 2 ml of the starch solution, continue
the titration until the blue colour is destroyed, and back-titrate with
the standard potassium permanganate solution (0.03 N) until the blue
colour just reappears. Repeat the titration with the potassium iodate
solution substitute for the potassium permanganate solution.
Calculate the sulphur equivalent of the standard potassium iodate
solution in grams per millilitre as follows:
× C × G × 0.0239 2-
E = A----------------------------------------------------------
B×D×F
where
E = sulphur equivalent of the potassium iodate solution g/ml,
A = weight in g of sodium oxalate used in the standardization of
the potassium permanganate solution,
C = volume in ml of potassium permanganate solution used in
the standardization of the potassium iodate solution,
G = volume in ml of sodium thiosulphate solution required by F,
B = volume in ml of potassium permanganate solution required
by A,
D = volume in ml of sodium thiosulphate solution required by C,
and
F = volume in ml of potassium iodate solution used in the
standardization of the potassium iodate solution.
NOTE — One millilitre of a normal solution of potassium permanganate or potassium
iodate is equivalent to 0.067 01 g of sodium oxalate or 0.016 03 g of sulphur. The
number 0.239 2 is obtained by dividing 0.016 03 by 0.067 01. The potassium iodate
29
IS : 4032 – 1985
and potassium permanganate solutions should be standardized frequently, but, as
the sodium thiosulphate solution is more stable the potassium iodate solution may
sometimes be standardized against the sodium thiosulphate solution alone and
without the last values of A, B, C and D being changed.
6.1.5 Starch Solution — To 100 ml of boiling water, add a cool
suspension of one g of soluble starch in 5 ml of water, and cool. And a
cool solution of one g of sodium hydroxide in 10 ml of water, then 3 g of
potassium iodide and mix thoroughly.
6.1.6 Ammoniacal Zinc Sulphate Solution — Dissolve 50 g of zinc
sulphate (ZnSO47H2O) in 150 ml of water and 350 ml of ammonium
hydroxide. Filter the solution after allowing it to stand for at least
24 hours.
6.1.7 Ammoniacal Cadmium Chloride Solution — Dissolve 15 g of
cadmium chloride (CdCl22 1--2- H2O) in 150 ml of water and 350 ml of
ammonium hydroxide. Filter the solution after allowing it to stand for
atleast 24 hours.
6.1.8 Standard Sodium Arsenite Solution — Dissolve 3.0 g of sodium
carbonate (Na2CO3) and then 0.90 g of arsenic trioxide (As2O3) in
100 ml of water. Heat the mixture until the solution is as complete as
possible. Filter the solution if it is not clear or it contains a residue.
Cool it to room temperature, transfer to a volumetric flask and dilute it
to one litre. Standardize the solution as given in 6.1.8.1.
6.1.8.1 Dissolve 0.58 g of potassium permanganate (KMnO4) in one
litre of water and standardize it against 0.03 g of pure sodium oxalate
(Na2C2O4). Put 30 ml of the potassium permanganate solution in a
250-ml Erlenmeyer flask. Add 60 ml of the dilute nitric acid (1 : 4) and
10 ml of a sodium nitrite solution (5 percent) to the flask. Boil the
solution until the nitrous acid is completely expelled. Cool the solution,
add sodium bismuthate and finish by titrating with standard solution
of sodium arsenite in the manner described under 6.10 for the
determination of manganic oxide.
NOTE — Each millilitre of the sodium arsenite solution is approximately equivalent
to 0.000 3 g of manganic oxide.
6.1.8.2 Calculate the manganic oxide equivalent of the standard
sodium arsenite solution in grams per millilitre as follows:
C = 0.03 × 0.236 × 30-
-----------------------------------------------
a×b
where
C = manganic oxide equivalent of the sodium arsenite solution
in g/ml,
30
IS : 4032 – 1985
a = volume in ml of potassium permanganate solution required
by 0.03 g of sodium oxalate, and
b = volume in ml of sodium arsenite solution required by 30 ml
of potassium permanganate solution.
6.2 Loss on Ignition — Loss on ignition shall be determined in
accordance with requirements of 4.2. Owing to the presence of sulphide
in slag cements which may be oxidised to sulphates, there may be a
gain instead of loss in some cases and this should be reported.
6.3 Silica — The method for determining silica in Portland slag
cement shall be the same as described in 4.3.
6.4 Combined Ferric Oxide and Alumina — The method for
determining combined ferric oxide and alumina in Portland slag
6.5 Ferric Oxide — The method for determining ferric oxide in
Portland slag cement shall be the same as described in 4.5.
6.6 Alumina — The method for determining alumina in Portland slag
6.7 Calcium Oxide
6.7.1 Method 1 ( Gravemetric Method ) — The method for determining
calcium oxide shall be the same as described in 4.7.1.
6.7.2 Method 2 ( EDTA Method ) — Take 10 ml of solution prepared as
given in 4.5.2.1 in a conical flask. Warm the solution on a hot plate and
add drop by drop 1 : 1 ammonium hydroxide with constant shaking till
a turbidity appears. Filter through Whatman filter paper No. 41 and
wash the filter paper 2 to 3 times taking 5 to 10 ml to distilled water
each time. Add 2 to 3 drops of nitric acid followed by about 50 mg of
solid potassium periodate. Keep the flask on water bath till pink colour
develops. Shake and allow to cool to room temperature. Add 5 ml of
1 : 1 glycerol with constant stirring and then 5 ml of diethylamine. Add
20 ml of 4 N sodium hydroxide solution and shake well to adjust the
pH to 12 or slightly more. Add approximately 50 ml of distilled water
and 100 mg of solid Patton — Reeders indicator and titrate against
0.01 M EDTA solution. The end point of titration is reached when one
to two drops of EDTA produce a sharp change in colour from violet to
blue. Calculate calcium oxide as given in 4.7.2.1.
6.8 Magnesia
6.8.1 Method 1 ( Gravemetric Method ) — The method for determining
magnesia in Portland slag cement shall be the same as described
in 4.8.1.
31
IS : 4032 – 1985
6.8.2 Method 2 ( EDTA Method ) — Take 10 ml of solution prepared as
given in 4.5.2.1 in a conical flask. Warm the solution on a hot plate and
add drop by drop 1 : 1 ammonium hydroxide with constant shaking till
a turbidity appears. Add 2 ml in excess. Filter the solution through
Whatman filter paper No. 41 in another conical flask. Wash the filter
paper with hot water 2 to 3 times, taking 10 to 15 ml aliquot each time.
Titrate against 0.01 M EDTA solution as in 4.8.2 and calculate
magnesium oxide as given in 4.8.2.1.
6.9 Insoluble Residue — The method for determining insoluble
residue in Portland slag cement shall be the same as described in 4.10.
6.10 Manganic Oxide
6.10.1 Take a sample of cement 1 to 3 g ( see Note 1 ), weigh and put it
into a 250-ml beaker and treat with 5 to 10 ml of water and then with
60 to 75 ml of diluted nitric acid (1 : 4). Boil the mixture until the
solution is as complete as possible. Add 10 ml sodium nitrite solution
(5 percent) and boil until the nitrous acid is completely expelled ( see
Note 2 ) taking care not to allow the volume of the solution to become
so small as to cause the precipitation of gelatinous silica. Ignore any
separated silica, but if there is still a red or brown residue, use more
solution of sodium nitrite to effect a complete decomposition and then
boil again to expel the nitrous acid. Filter the solution into a 250-ml
Erlenmeyer flask and wash the filter paper with water. The solution
should have a volume of 100 to 125 ml.
NOTE 1 — The amount of cement taken for analysis depends on the content of
manganese, varying from one gram for about one percent of manganic oxide to 3 g for
0.25 percent or less of manganic oxide.
NOTE 2 — When sodium nitrite is added, the expulsion of nitrous acid by boiling
should be complete. If any nitrous acid remains in the solution, it will react with the
added sodium bismuthate and decrease its oxidizing value. If there is any manganese
in the cement, the first small quantity of sodium bismuthate should bring out a
purple colour.
6.10.2 Cool the solution to room temperature. Add a total of 0.5 g of
sodium bismuthate in small quantities with intermittent shaking.
Complete adding, and shake the solution occasionally for 5 minutes
and then add 50 ml of cool dilute nitric acid (1 : 33) which has been
previously boiled to expel nitrous acid. Filter the solution through a pad
of ignited asbestos in a Gooch crucible or a carbon filter with the aid of
suction. Wash the residue four times with cool dilute nitric acid (1 : 33).
6.10.3 Titrate the filtrate immediately with the standard sodium
arsenite solution. The end point is reached when a yellow colour is
obtained free of brown or purple tints and it does not change upon
further addition of arsenic oxide. Calculate the manganese in the
cement as manganic oxide.
32
IS : 4032 – 1985
6.10.4 If a determination of calcium or magnesium is required in
addition to determination of manganese, the latter shall be eliminated
from the combined filtrate obtained in 4.4.2 in the alumina and ferric
oxide determination by the method laid down in 4.7.1.
6.11 Sulphur Trioxide
6.11.1 To one gram of the sample, add 25 ml of cold water, and while the
mixture is stirred vigorously, add 5 ml hydrochloric acid. If necessary,
heat the solution and grind the material with the flattened end of a
glass rod until the decomposition of the cement is complete. Dilute the
solution to 50 ml and digest for 15 minutes. Filter and wash the residue
thoroughly with hot water. Set aside the filter paper with the residue.
Dilute the filtrate to 250 ml and heat to boiling. Add slowly, drop by
drop, 10 ml of hot barium chloride (100 g/l) solution and continue the
boiling until the precipitate is well formed. Digest the solution on a
steam-bath for 4 hours or preferably overnight. Filter the precipitate
using Whatman No. 42 filter paper or its equivalent. Wash, place the
paper and contents in a weighed platinum or porcelain crucible, and
slowly incinerate the paper without inflaming. Then ignite at 800 to
900°C, cool in a desiccator and weigh the barium sulphate.
6.11.2 Calculate the percentage of sulphur trioxide to the nearest 0.1
as follows:
Sulphur trioxide percent = W × 34.3
where
W = weight in g of barium sulphate, and
34.3 = molecular ratio of sulphur trioxide to barium sulphate
(0.343 × 100)
6.12 Sulphur as Sulphide
6.12.1 Gas Generating Flask — Connect a dry 500-ml boiling flask with
a long-stem separating funnel and a small connecting bulb, by means of
a rubber stopper. Bend the stem of the funnel so that it does not interfere
with the connecting bulb, adjust the stem so that its lower end is close
to the bottom of the flask, and connect the opening of the funnel with a
source of compressed air. Connect the bulb with an L-shaped glass tube
and a straight glass tube about 20 cm in length. Insert the straight glass
tube in a tall-form, 400-ml beaker. A three-neck Woulfe bottle with a
long glass tubing in the middle opening, placed between the source of
compressed air and the funnel, is a convenient aid in the regulation of
the air flow. If the air contains hydrogen sulphide or sulphur dioxide, a
solution of lead acetate or some other suitable absorbent shall be used
in the bottle. Rubber used in the apparatus shall be of pure gum grade
low in sulphur and shall be cleaned with warm hydrochloric acid.
33
IS : 4032 – 1985
6.12.2 Procedure — Place 15 ml of the ammoniacal zinc sulphate
solution ( see Note 1 ) and 285 ml of water in the beaker. Put 5 g of the
sample ( see Note 2 ) and 10 ml of water in the flask and shake the flask
gently to wet and disperse the cement completely. This step and the
following one should be performed rapidly to prevent the setting of the
cement. Connect the flask with the funnel and bulb. Add 25 ml of the
stannous chloride solution through the funnel and shake the flask. Add
100 ml of hydrochloric acid (1 : 3) through the funnel and shake the
flask. During these shakings, keep the funnel closed and the delivery
tube in the ammoniacal zinc sulphate solution. Connect the funnel with
the source of compressed air, open the funnel, start a slow stream of air,
and heat the flask and contents slowly to boiling. Continue the boiling
gently for 5 or 6 minutes, cut off the heat, and continue the passage of
air for 3 or 5 minutes. Disconnect the delivery tube and leave it in the
solution for use as a stirrer. Cool the solution to 20 to 30°C
( see Note 3 ), and 2 ml of the starch solution and 40 ml of hydrochloric
acid (1 : 1), and titrate immediately with the standard potassium iodate
solution until a persistent blue colour is obtained ( see Note 4 ).
NOTE 1 — In general, zinc sulphate solution is preferable to cadmium chloride
solution because zinc sulphate is more soluble in ammonium hydroxide than
cadmium chloride. The cadmium chloride solution may be used when there is a doubt
as to the presence of a trace of sulphur as the yellow cadmium sulphide facilitates the
detection of a trace.
NOTE 2 — If sulphur content exceeds 0.20 or 0.25 percent, a smaller sample should
be used so that the titration with the potassium iodate solution will not exceed 25 ml.
NOTE 3 — The cooling is important, as the end point is indistinct in a warm solution.
A part of the ammonium hydroxide is lost during distillation and the remaining
ammonium hydroxide reacts with the acid, raising the temperature of the solution a
few degrees without rendering the end point uncertain.
NOTE 4 — If sulphur content is appreciable but not approximately known in advance,
the result may be low due to the loss of hydrogen sulphide during a slow titration. In
such a case the determination should be repeated with the titration carried out more
rapidly.
6.12.3 Calculation — Calculate the percentage of sulphur as follows:
Sulphur, percent = EV × 20
where
E = sulphur equivalent of the potassium iodate solution
in g/ml,
V = volume in ml of potassium iodate solution required by
the sample, and
20 = 100 divided by the weight of sample used (5 g).
NOTE — Sulphites, thiosulphates, and other compounds intermediate between
sulphides and sulphates are assumed to be absent. If such compounds are present,
they may cause an error in the determination.
34
IS : 4032 – 1985
7. CHEMICAL ANALYSIS OF PORTLAND POZZOLANA
CEMENT
7.1 Loss on Ignition — The loss on ignition of Portland pozzolana
cement shall be determined as specified in 4.2.
7.2 Magnesia
7.2.1 Method 1 ( Gravemetric Method ) — The method of determining
magnesia content in Portland pozzolana cement shall be the same as
that described in 4.8.1 except as given in 7.2.1.1 to 7.2.1.3.
7.2.1.1 Weigh out a quantity of the ignited sample equivalent to 0.5 g
of the moisture-free sample, calculated as follows:
Weight of ignited = ---------------------------------------------------------------------------------------------------------------
0.5 ( 100.00 – percentage loss on ignition -)
sample, g 100
NOTE — The ignited material from the loss on ignition determination may be used
for the sample.
7.2.1.2 Thorougly mix the sample with 4 to 6 g of sodium carbonate by
grinding in an agate mortar. Place a thin layer of sodium carbonate on
the bottom of a platinum crucible of 20 to 30 ml capacity, add the
cement-sodium carbonate mixture and cover the mixture with a thin
layer of sodium carbonate. Place the cover crucible over a moderately low
flame and increase the flame gradually to a maximum (approximately
1 100°C) and maintain this temperature until the mass is quiescent
(about 45 min). Remove the burner, lay aside the cover of the crucible,
grasp the crucible with the tongs, and slowly rotate the crucible so that
molten contents spread over the side and solidify as a thin shell on the
interior. Set the crucible and cover aside to cool. Rinse off the outside of
the crucible and place the crucible on its side in a 300-ml casserole about
one-third full of water. Warm the casserole and stir until the cake in the
crucible disintegrates and can be removed easily. By means of a glass
rod, lift the crucible out of the liquid, rinsing it thoroughly with water.
Rinse the cover and crucible with hydrochloric acid (1 : 3); then add the
rinse to the casserole. Very slowly and cautiously, add 20 ml
hydrochloric acid (sp gr 1.19) to the covered casserole. Remove the cover
and rinse. If any gritty particles are present, the fusion is incomplete and
the test should be repeated, using a new sample.
7.2.1.3 Evaporate the solution to dryness on a steam-bath. Remove
silica, the ammonium hydroxide group and calcium in accordance with
4.3.1, 4.3.2, 4.3.3, 4.3.4, 4.3.5, 4.4.1 and 4.7.1 respectively. Determine
magnesium oxide in accordance with 4.8.1.
7.2.2 Method 2 ( EDTA Method ) — Evaporate the solution under 7.2.1.2
to dryness on steam-bath. Remove silica as described in 4.3 and
35
IS : 4032 – 1985
make up the volume of 250 ml in a volumetric flask. Determine
magnesia as described in 4.8.2.
7.3 Sulphuric Anhydride — The method for determining sulphuric
anhydride of Portland pozzolana cement shall be the same as described
in 4.9, except that the sample used shall be moisture free and need not
be completely decomposed.
7.4 Insoluble Residue — Insoluble residue of Portland pozzolana
cement shall be determined as specified in 4.10.
8. POZZOLANICITY TEST FOR PORTLAND POZZOLANA
CEMENT
8.1 Purpose — The pozzolanicity test for checking pozzolanic cements
enables to observe the absence of hydrated lime in the cement pastes
under consideration, owing to the equilibrium which is established
between the lime and the alkalies present in the liquid phase in
contact with the pastes themselves which are preserved for a given
time at constant temperature.
NOTE — Under these conditions, the solutions which are in contact with the Portland
cement pastes are generally oversaturated or at least saturated with lime. In case of
cement pastes containing a suitable quantity of pozzolana the solutions in contact
have a lime content (after a given period), the value of which is always less than that
of the saturation, compared with the alkalinity of the solutions themselves.
Obviously such a behaviour depends upon the absence in the pozzolanic pastes of
hydrated lime, which is gradually fixed by the pozzolana.
8.2 Principle — Pozzolanic activity depends upon the fixation of
Ca (OH)2, released by the hydration of the cement, in the form of more
or less definite hydrates whose strength increases with time. In the
test described, pozzolanicity is assessed by comparing the quantity of
Ca (OH)2 present in a liquid phase in contact with the hydrated
cement, with the quantity of Ca (OH)2 capable of saturating a medium
of the same alkalinity. With a pozzolanic cement, the Ca (OH)2 in
solution is always lower than the saturation concentration.
8.2.1 Experiments show that by using 20 g of cement per 100 ml of
water at a temperature of 40°C, equilibrium is practically reached is
seven days. The application of the test thus requires knowledge of the
solubility at 40°C of Ca (OH)2 in a solution whose free alkalinity varies
from zero to about 100 milli-equivalents of strong base (OH) per litre.
8.2.2 The pozzolanicity test thus offers the advantage of controlling
the pozzolanic binder hydrated directly under conditions of use and
represents a method of controlling the pozzolanic behaviour of a
pozzolanic cement, that is the chemical and physical phenomenon
which tend to practically completely remove the lime of hydrolysis
from the binder.
36
IS : 4032 – 1985
8.3 Reagents
8.3.1 Distilled Water
8.3.2 Standard Hydrochloric Acid — 0.1 N.
8.3.3 Ammonia Solution — 0.5 N.
8.3.4 Ammonium Oxalate — in saturated solution.
8.3.5 Methyl Orange
8.3.6 Potassium Permanganate Solution — 0.05 N.
8.3.7 About 20 g paraffin wax (in case a glass flask is used).
8.4 Apparatus
8.4.1 Conical Flask — of 300 ml in alkali resisting glass or preferably
in plastics material, with a stopper of rubber or waxed cork capable of
being securely fitted to the latter so as to permit a vigorous shaking.
8.4.2 Funnel — with wide stem.
8.4.3 Filter — in sintered glass.
8.4.4 Conical Flask — of 250 ml with ground-glass stopper.
8.4.5 Beaker — of 250 ml.
8.4.6 Precision Pipette — of 50 and 100 ml.
8.4.7 Thermostatic Space — at 40 ± 2°C.
8.5 Procedure
8.5.1 In case a conical glass flask is used, coat the inside of the flask
with about 20 g of melted paraffin wax. Finally allow the surplus to
solidify at the bottom of the flask as it stands on a level surface.
8.5.2 With a pipette, introduce 100 ml of distilled water in the flask
and put the stoppered flask into a thermostat at 40°C until the
required temperature is reached (about 1 hour).
8.5.3 Then pour into the conical flask, using the funnel with a wide
stem, 20.00 ± 0.01 g of the cement to be tested. Close the container and
secure the stopper. Shake vigorously for about 20 seconds in order to
prevent the formation of cement lumps. Put the conical flask back into
the thermostat at 40°C, quite level in order to ensure that the cement
settles in a layer of even depth. All the operations outside the
thermostat shall be carried out as quickly as possible, to avoid any
appreciable lowering of the temperature of the contents of the flask.
37
IS : 4032 – 1985
8.5.4 After storage for seven days at 40°C, quickly filter the liquid
through sintered glass, collecting the filtrate in a conical flask with
ground-glass stopper. Cool the filtrate to room temperature and mix.
8.5.5 Pipette out 50 ml of the filtrate solution into a 250-ml beaker and
determine the total alkalinity against standard hydrochloric acid
(0.1 N), using methyl orange as indicator. Express the result in milli-
equivalents (OH) per litre. Now precipitate the calcium as oxalate in
ammonia solution, filter and wash with cold water. Titrate the calcium
oxalate obtained, using 0.05 N potassium permanganate solution.
Express the lime content in millimoles per litre.
8.6 Results — Express the total alkalinity and the calcium oxide
content in millimoles per litre. Report on a pozzolanicity diagram* ( see
Fig. 1 ), the point representing the calcium oxide content as a function
of the total alkalinity.
8.6.1 The cement under test is considered to be pozzolanic if the point
representing it lies below the solubility isotherm.
8.7 Retests — If the point obtained is on the isotherm or in the
immediate vicinity, re-start the test in the same conditions, but
leaving the conical flask in the thermostatic space during fourteen
days. In the case of slow but real pozzolanic activity, the test becomes
clearly positive.
9. STAINING TEST FOR MASONRY CEMENT
(DETERMINATION OF WATER-SOLUBLE ALKALI)
9.1 Procedure
9.1.1 To 150 g of sample of masonry cement in a 400-ml beaker, add
250 ml of distilled water. Stir thoroughly, let stand 30 min at room
temperature, and stir again. Filter through a Buchner funnel, transfer
the insoluble matter to the original beaker, and rinse the funnel with
150 ml of distilled water into the beaker containing the insoluble
matter. Stir thoroughly, let stand 30 min at room temperature, and
stir again. Filter as above and again return the insoluble matter to the
original beaker. Wash the funnel with 100 ml of distilled water into
the beaker containing the insoluble matter. Stir thoroughly, let stand
30 min at room temperature, and stir again. Filter as above. Acidify
the filtrate with 5 ml of concentrated hydrochloric acid (HCl,
sp gr 1 : 19). Stir until cloudiness disappears. Evaporate the solution
to about 400 ml. Cool to room temperature and transfer quantitatively
to a 500-ml volumetric flask. Dilute to 500 ml. Transfer a 50-ml aliquot
of this solution to a 100-ml volumetric flask.
*The pozzolanicity diagram (Fig. 1) has been established in inclined coordinates, it
may also be established in rectangular coordinates.
38
IS : 4032 – 1985
FIG. 1 POZZOLANICITY DIAGRAM — SOLUBILITY OF Ca(OH)2 IN THE

PRESENCE OF ALKALIES AT 40°C
9.1.2 Determine sodium oxide and potassium oxide in the solution
described in 9.1.1 following the procedure described in 4.11. Pour 9 ml
of the stock calcium chloride (CaCl2) solution 63 000 ppm (CaO)
[ see 4.11.1.2 (a) ] into the 100-ml flask, and dilute the solution to
100 ml. Determine the solution and potassium oxide content of this
solution as described in 4.11.4.2 and 4.11.4.3. Read the parts per
million of each solution in the 100-ml flask from the calibration curve.
9.2 Calculation — Calculate the percentage of water-soluble alkali as
sodium oxide (Na2O) to the nearest 0.01 as follows:
A = B/1 500
C = D/1 500
E = C × 0.658
Total water-soluble alkali = A + E
39
IS : 4032 – 1985
where
A = percentage of water-soluble sodium oxide (Na2O),
B = parts per million of Na2O in the solution in the 100-ml flask
( see 9.1.1),
C = percentage of water-soluble potassium oxide (K2O),
D = parts per million of K2O in the solution in the 100-ml flask
( see 9.1.1), and
E = percentage of Na2O equivalent to the K2O.
40
IS : 4032 – 1985
SHRI L. SWAROOP Orissa Cement Limited, New Delhi
SHRI H. BHATTACHARYYA ( Alternate )
SHRI S. K. GUHA THAKURTA Gammon Dunkerley and Co Ltd, Bombay
SHRI S. P. SANKARNARAYANAN ( Alternate )
SHRI G. RAMAN, Directorate General, BIS (Ex-officio Member)
Director (Civ Engg)
Secretary
SHRI N. C. BANDYOPADHYAY
Deputy Director (Civil Engg), BIS
Cement Subcommittee, BDC 2 : 1
Convener
DR H. C. VISVESVARAYA National Council for Cement and Building Materials,
New Delhi
Members
DR A. K. MULLICK ( Alternate to
Dr H. C. Visvesvaraya )
SHRI S. K. BANERJEE National Test House, Calcutta
SHRI SOMNATH BANERJEE Cement Manufacturers’ Association, Bombay
CHIEF ENGINEER (RESEARCH)- Irrigation Department, Government of Punjab,
cum-DIRECTOR Amritsar
RESEARCH OFFICER (CONCRETE
TECHNOLOGY) ( Alternate )
DIRECTOR Maharashtra Engineering Research Institute, Nasik
RESEARCH OFFICER ( Alternate )
DIRECTOR (C & MDD) Central Water Commission, New Delhi
DEPUTY DIRECTOR (C&MDD) ( Alternate )
SHRI A. V. GOKAK Development Commissioner for Cement Industry
(Ministry of Industry), New Delhi
SHRI S. S. MIGLANI ( Alternate )
SHRI P. J. JAGUS Associated Cement Co Ltd, Bombay
DR A. K. CHATTERJEE ( Alternate )
JOINT DIRECTOR, RESEARCH Research, Designs & Standards Organization
(B & S) (Ministry of Railways), Lucknow
DEPUTY DIRECTOR, RESEARCH
(B & S-I) ( Alternate )
SHRI R. L. KAPOOR Ministry of Shipping and Transport (Roads Wing)
SHRI W. N. KARODE Hidustan Construction Co Ltd, Bombay
SHRI S. R. KHANNA Directorate General of Technical Development,
New Delhi
SHRI S. K. GHOSH ( Alternate )
SHRI K. P. MOHIDEEN Central Warehousing Corporation, New Delhi
SHRI K. K. NAMBIAR In personal capacity ( 11 First Cresent Park Road,
Adyar, Madras )
41
IS : 4032 – 1985
SHRI Y. R. PHULL Central Road Research Institute (CSIR), New Delhi
SHRI M. R. CHATTERJEE ( Alternate )
SHRI A. V. RAMANA Dalmia Cement (Bharat) Ltd, New Delhi
DR K. C. NARANG ( Alternate )
DR A. V. R. RAO National Buildings Organization, New Delhi
SHRI J. SEN GUPTA ( Alternate )
LT-COL V. K. RAO Engineer-in-Chief’s Branch, Army Headquarters,
New Delhi
SHRI N. S. GALANDE ( Alternate )
SHRI S. A. REDDI Gammon India Limited, Bombay
DR S. S. REHSI Central Building Research Institute (CSIR), Roorkee
DR R. K. DATTA ( Alternate )
SHRI A. U. RIJHSINGHANI Cement Corporation of India Ltd, New Delhi
SHRI K. K. SOMANI Shree Digvijay Cement Co Ltd, Bombay
SHRI R. K. GATTANI ( Alternate )
SUPERINTENDING ENGINEER (D) Public Works Department, Government of
Tamil Nadu, Madras
SENIOR DEPUTY CHIEF
ENGINEER (GENERAL) ( Alternate )
SHRI L. SWAROOP Orissa Cement Ltd, New Delhi
SHRI H. BHATTACHARYA ( Alternate )
SHRI C. D. THATTE Gujarat Engineering Research Institute, Vadodara
SHRI J. K. PATEL ( Alternate )
SHRI V. M. WAD Bhilai Steel Plant, Bhilai
WORKS MANAGER (CEMENT) Rohtas Industries Ltd, Dalmianagar
Ad-Hoc Panel for Considering EDTA Method of Analysis and
Colorimetric Analysis of Cement, BDC 2 : 1 AP
Convener
SHRI S. K. CHOPRA In personal capacity ( S-436, Greater Kailash,
New Delhi )
Members
SHRI R. C. BHATNAGAR Central Road Research Institute (CSIR), New Delhi
DR (SMT) S. GUPTA ( Alternate )
DR A. K. CHATTERJEE Central Research Station (ACC), Thane
SHRI C. H. PAG ( Alternate )
DR D. K. DAS National Test House, Calcutta
42
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UDC 666.971.4 : 543

FIG. 1 POZZOLANICITY DIAGRAM — SOLUBILITY OF Ca(OH)2 IN THE

BUREAU OF INDIAN STANDARDS

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