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Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”

Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 5328 (1969): Method of test for determination of

chemical composition of asbestos fibre [CED 53: Cement
Matrix Products]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS: 5328 - 1969
( Reaffirmed 2001 )

Indian Standard
METHOD OF TEST FOR
DETERMINATION OF CHEMICAL
COMPOSITION OF ASBESTOS FIBRE
( Second Reprint MAY 1990 )

UDC 666.961 : 543

@ Copyright 1970

BUmAU OF INDrAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Gr 5 June 1970
 ..

IS: 5328 - 1969

Indian Standard
METHOD OF TEST FOR
DETERMINATION OF CHEMICAL
COMPOSITION OF ASBESTOS FIBRE

Cement and Concrete Sectional Committee, BDC 2

Chairman Re$vcsenting

.%IRI J. DATT The Concrete Association of India, Bombay

Members

SHRI M. A. MEHTA (Alternate to

Shri J. Datt) ’
SWRI A. P. BAGCHI Sahu Cement Service, New Delhi
SHRI P. S. BHATNAGAR Bhakgelh% Beas Design Organization, New

SHRI A. M. SINGAL (Alternate)

DR S. K. CHOPRA Central Building Research Institute (CSIR),
Roorkee
SHRI J. S. SHARMA (Altenlate)
DIRECTOR Central Road Research Institute (CSIR), New
Delhi
DR R. K. GHOSH (Altcmatc)
DIRECTOR (CSM) Central Water t Power Commission, New
Delhi
DIRECTOR (DAMS III) (Alternate)
DIRECT~R:IN-CHARGE (NR) Geological Survey of India, Lucknow
DR R. I<. GHOSH Indian Road Congress, New Delhi
DR R. R. HATTIANGADI The Associated Cement Companies Ltd, Bombay
SHRI P. J. JAGUS (AZtcrnatc)
JOINT DIRECTOR, STANDARDS Research, Designs & Standards Organization,
(B t S) Ministry of Railways, Lucknow
DEPUTY DIRECTOR, STAN-
DARDS (B & S) (Alternate)
SHRI S. B. JOSHI S. B. Joshi & Co, Bombay
SHRI M. T. KANSE Directorate Gene+ of Su plies & Disposals
SHRI KARTIK PRASAD Roads Wing, Ministry of $ ransport C Shipping
SHRI S. L. KATHURIA (Alternate)
SHRI S. N. MUKERJI National Test House, Calcutta
SHRI E. K. RAMCHANDRAN (AIteunatc)

(Continued on page 2)

BUREAU OF INDfAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC
NEW DELHI 110002
IS : 5328 - 1969

(Continued from page 1)

Members Representing
SHRI M. L. NANDA Central Public Works Department
SUPERINTENDINGENGINEER,
2nd CIRCLE (A ltevnate)
SHRI ERACH A. NADIRSHAH The Institution of Engineers (India)
SHRI K. K. NAMBIAR In personal capacity (‘ Ramanalaya ’ 16, First
Crescent Park Road, Gandkinagar, Adyar,
Madras 20)
BRIG NARESH PRASAD Engineer-in-Chief’s Branch, Ministry of Defence
COL J. M. TOLANI (Alternate)
SHRI RABINDER SINGH National Buildings Organization, New Delhi
SHRI B. D. AHUJA (Alternate)
PROF G. S. RAMASWAMY StructztLepgineering Research Centre (CSIR),

DR N. S. BHAL (Alternate)
SHRI T. N. S. RAO Gammon India Ltd, Bombay
SHRI S. R. PINHEIRO (Alleynafe)
REPRESENTATIVE M. N. Dastur & Co (Private) Limited, Calcutta
REPRESENTATIVE The India Cement Ltd, Madras
SHRI K. G. SALVI Hindustan Housing Factory, New Delhi
SHRI C. L. KASLIWAL (Attevnate)
SECRETARY Central Board of Irrigation BEPower, New Delhi
SHRI L. SWAROOP Dalmia Cement (Bharat) Ltd, New Delhi
SHRI A. V. RAMANA (Altevnate)
DR I-I. C. VISVESVARAYA Cement Research Institute of India, New Delhi
SHRI R. NAGARAJAN, Director General, IS1 (Ex-oflcio Member)
Director (Civ Engg) (Secretary)

Asbestos Cement Products Subcommittee, BDC 2 : 3

Convener

DR H. C. VISVESVARAYA Cement Research Institute of India, New Delhi

_ Members
SHRI N. H. BHAGWANANI Engineer-in-Chief’s Branch, Ministry of Defence
DEPUTY DIRECTOR,STANDARDS Research, Designs & Standards Organization,
(B 8~ S) Ministry of Railways, Lucknow
ASSISTANT DIRECTOR,STAN-
DARDS (B & S/M) (~b%ate)
ENGINEEB ~F~UCER I (A) Central Public Works Department
SHRI V, PODDAR Rohtas Industries Ltd, Dalmianagar
SHRI M. P. VEXMA (Altewate)
SHRI K. V. RAMASESHAN Shree Digvijay Cement Co Ltd, Ahmedabad
SHRI V. V. RANGNEKAR Directorate Gener’al of Supplies & Disposals
REPRESENTATIVE The Hyderabad Asbestos Cement Products Ltd.
Hyderabad
SHRI R. S. SHARMA Geological Survey of India, Calcutta
SHRI S. K. SWAMI The Asbestos Cement Ltd. Bombay
SHRI P. B. NAYER (Alternate)
SHRI N. VENKATARAMAN Hilldustan Ferodo Ltd, Bombay

(Continued on page 20)

2
 IS: 5328 - 1969

Indian Standard
METHOD OF TEST FOR
DETERMINATION OF CHEMICAL
COMPOSITION OF ASBESTOS FIBRE

0. FOREWORD

0.1 ‘1‘1~s Indian Standard was adopted by the In&m Standards Tnstitu-
tion on 13 August 1969, after the draft litlnlizcd by the Ccmcnt and Con-
crete Sectional Committee had b&n approved 1)~ the Civil Engineering
Division Council.

0.2 A series of Indian Standards on testing procedures of asbestos fibre is

being formulated so as to provide standard methods for obtaining physical
and chemical properties of asbestos fibre which is used for manufacturing
various asbestos cement (AC) products like AC sheets, AC pipes, etc.
These testing procedures will be useful both for mine owners and the
manufacturers of AC products provided they have the facilities to make
these tests with reasonable accuracy and the personnel with the required
degree of laboratory experience.

0.3 In the formulation of this standard due weightage has been given
to international co-ordination among the standards and practices prevail-
ing in different countries in addition to relating it to the practices. in the
field in this country. This has been met by basing the standard on
‘ Testing procedure for chrysotile asbestos fibrc’ jointly published by
American Textile Institute, Mineral Fibre Products Bureau and Quebec
Asbestos Mining Association.

0.4 This standard is one of the three Indian Standards on testing of

asbestos fibre published so far. IS:3632-1969* and IS:4844-1968t are
the other two standards published under this series.

0.5 In reporting the results of a test or analysis made in accordance

with this standard, if the final value, observed or calculated, is to be
rounded off, it shall be done in accordance with IS:2-1960:.
 IS : 5328 - 1969

1. SCOPE
1.1 This standard covers the methods for the quantitative analysis for
(a) silica, (b) ferrous oxide, (c) ferric oxide, (d) alumina, (e) calcium oxide,
(f) magnesium oxide, (g) sodium oxide, (h) carbonates, and (j) water
of crystallization in asbestos fibre.

2. OUTLINE OF METHOD
2.1 The samples are treated as silicates not decomposed by acids and are,
therefore, fused with sodium carbonate to convert to soluble sodium
salts. From the hydrochloric acid solution of the melt, silica is first
removed bv clehydration and precipitation. The filtrate containing iron
and aluminium plus calcium and magnesium is treated with bromine water*
to oxidize the iron to the ferric state and the latter together with the
aluminium is precipitated with ammonia and ignited. To differentiate
between ferric oxide and alumina, the ignited residue is fused with
potassium pyrosulphate and the iron in the melt determined volumetri-
cally. Another aliquot portion of the solution of the melt is used for
determination of alumina by use of 8-hydroxyquinoline. The filtrate
resulting from the ferric exide and alumina precipitation contains calcium
(if present) and magnesium. The calcium is precipitated from this
filtrate, after the latter is acidified, as calcium oxalate. The latter is
ignited and weighed as calcium oxide.
2.2 The filtrate after removal of the calcium is acidified with concen-
trated nitric acid and evaporated to dryness to ensure removal of ammo-
nium salts as the latter will prevent complete precipitation of the
magnesium. The residue is dissolved in dilute hydrochloric acid and
the magnesium precipitated with ammonium-hydrogen phosphate in
ammoniacal solution. The precipitate is carefully Ignited and weighed as
magnesium pyrophosphate. The water of crystallization is determined
by ignition loss and corrected for carbonate content.

3. SAMPLING
3.1 The sample shall be the laboratory test sample in accordance with
IS: 4844-1968t.

4. PREPARATION OF LABORATORY TEST SPECIMEN

4.1 Quarter the laboratory sample down to approximately 25 g. Divide
the 25 g sample into ten approximately equal portions and sub-divide
*If bromine water is not available, the oxidation can be affected with a few
drops of concentratecj nitric acid or hydrogen peroxide.
tMethod of sampling and preparation of asbestos fibre for laboratory test
purposes.

4
 IS: 5328 - 1969

these portions into halves. Combine a half of each of the ten poitions
and mix thoroughly. Repeat this procedure until the sample weight is
reduced to approximately 3 g. On a smooth and clean area spread the
3 g sample into a thin layer over an area of approximately 20 X
20 cm, in such a manner that pinches may be taken from all parts.
Extract with tweezers five bundles of long fibre free from rock, grit or
dust, each weighing about Q-5 g. Spread into a thin layer and extract
at least five bundles of the fibre from different parts so that when these
are combined and dried to constant weight at 110°C the test specimen
will weigh 0.5 + O-02 g.

5. PREPARATION OF SAMPLE

5.1 Apparatus

5.1.1 Agate Mortar and Pestle - 125 ml capacity.

5.1.2 Platinum Crucible - 30 ml capacity.
5.1.3 Oven - 110°C.
5.1.4 Electric Furnace - 925’ +- 25°C.
5.1.5 Chemical Balance
5.1.6 Pprcelain Crucible - 20 ml capacity.
5.1.7 Cam1 Hair Brush
5.1.8 Desiccator

5.2 Reagents

5.2.1 Sodium Carbonate - solid.

5.3 Procedure-The test specimen is placed in a tared porcelain crucible

and after being brought to constant weight at 110°C is cooled in a desicca-
tor and weighed on a sensitive balance to the fourth decimal place.
This weight minus the tare is the sample weight (IV) for (a) silica,
(b) ferric oxide, (c) alumina, (d) calcium oxide, and (e) magnesium oxide.
Different samples shall be used for carbonates and WYter of crystalliza-
tion. The crucible with specimen is then placed in a furnace at 925’
f 25°C for one hour. After cooling, the specimen is reduced to as fine
a mesh as possible with an agate mortar and pestle. About 3.0 g of
sodium carbonate are added and ground intimately with the specimen
for an intimate mixture. The contents of the mortar are then transfer-
red to a 30 ml capacity platinum crucible using a camel hair brush to
sweep the last of the mixture from the mortar. Successive small amounts
of additional sodium carbonate are then ground in the mortar and trans-
ferred in like manner to the platinum crucible, to ensure removing of

5
 7.

IS: 5328 - 1969

the last trace of specimen from mortar to the crucible. Then sprinkle
a little additional sodium carbonate on top of the intimate mix of
powdered specimen and the sodium carbonate. Place a platinum lid on
the crucible.

6. DETERMINATION OF SILICA BY THE HYDROFLUORIC

ACID (GRAVIMETRIC) METHOD

6.1 Apparatus
6.1.1 Platjnzrm Crucible
6.1.2 Platinum Wire
6.1.3 Casserole - 300 ml.
6.1.4 Glass Triangle
6.1.5 Vented Chamber - 110°C.
6.1.6 Filter Paper - Whatman No. 40.
6.1.7 Water-Bath
6.1.8 Meker Burner
6.1.9 Vented Hood

6.2 Reagents
6.2.1 Dillste Hydroch.loric Acid - 2 N and 6 N.
6.2.2 Concentrated Hydrochloric Acid - specific gravity 1*16.
6.2.3 Cortcentrated .Sulphzwic Acid - specific gravity 1.84.
6.2.4 Hydrojuoric Acid - 40 percent.
6.3 Procedure
6.3.1 Heat the covered platinum crucible containing the intimate mix
of powdered specimen and fiux at first over a small flame to drive out
any.moisture present. Gradually raise the temperature until the highest
heat of a good Meker burner is obtained. As soon as the mass
melts quietly and there is no further evolution of carbon dioxide, the
decomposition is complete. CFFJ
6.3.2 Wind a piece of platinum wire into a spiral and insert it
into the fused mass. Remove the flame, allow the crucible to cool
in the air somewhat and then play a stream of water upon the
outside of the crucible. As soon as the crucible does not hiss when
the water strikes it, quickly introduce enough water into the crucible
to cover the melt. After about a minute carefully pull on the wire;
usually the melt can be @hdrawn from the crucible. If it does not
come out easily, it can often be loosened by carefully heating the
crucible.

6
 is: 5328 - 1969

6.3.3 Place the meit in a 300 ml casserole, add 25 ml of water,

cover the casserole and carefully add 25 ml of 6 N hydrochloric acid.
A lively evolution of’ carbon dioxide at once takes place, but as the
silicic acid separates, the inner part of the cake gradually becomes
coated with a film of silicic acid which protects it from the further
action of the acid. Consequently, it is necessary to break up the cake
from time to time by means of glass rod, until finally there is no
evolution of gas and no more hard lumps remain.
63.4 After the evolution of carbon dioxide has nearly ceased, wash off
the under side of the watch-glass, raise it by placing a glass triangle
under it, and evaporate to dryness. Heat the residue for at least
an hour at 110°C to dehydrate the silica.
6.3.5 Moisten the dry powder with concentrated hydrochloric acid
(specific gravity 1.16) and allow the covered dish to stand 10 minutes
at the ordinary temperature in order that the basic salts and oxides
formed during the evaporation and drying may once more be changed
to chlorides. Then warm gently, dilute with 100 ml of water, heat to
boiling, and after the silicic acid has settled, filter through a well fitted
filter paper, Whatman No. 40. Wash the residue three or four times
by decantation with hot 2 N hydrochloric acid, then transfer to the filter
and wash with hot water until free from chloride. Place the precipitate
in a platinum crucible and set aside for few minutes. The separation
of the silicic acid is not quite complete; as much as 2 mg may
remain in the filtrate. To remove this, once more ‘evaporate the solution
to dryness on the water-bath, and age in heat at 110°C for an hour,
moisten the residue with 5 ml of concentrated hydrochloric acid, and
allow to stand for not more than 15 minutes. Warm, dilute to 100 ml,
heat to gentle boiling, and filter through a new and correspondingly
small filter paper, washing with hot 2 N hydrochloric acid and with
water as before. Reserve the filtrate and analyse it for ferric oxide,
alumina, calcium oxide and magnesium oxide.
63.6 Combine the filter papers obtained in 6.3.5 and ignite them in a
platinum crucible. Keep the temperature low until all the carbon is
consumed, and do not allow the filter papers to catch fire. Finally, cover
the crucible and ignite over a Meker burner, cool and weigh as impure
silica.

6.3.7 The silica thus obtained is not absolutely pure. Moisten the
impure silica with water, add a drop of concentrated sulphuric acid
(specific gravity 1.18) and about 5 to 10 ml of pure hydrofluoric acid.
Place the crucible in an air bath and evaporate under a hood until
no more vapours are expelled. Remove the excess sulphuric acid by
heating over a free flame. Raise the temperature gradually and finally
heat the crucible over a Meker burner and again weigh.

7
IS: 5328 - 1969

6.3.8 Repeat the treatment with sulphuric and hydrofluoric acids,

without adding any more water, until the contents of the. crucible
(usually ferric oxide and alumina) are at a constant weight. Deduct
this amount from the weight of impure silica and add it to the pre-
cipitate obtained with the ammonia in the subsequent analysis.

6.4 Calculations - The percentage of silica shall be calculated by the

following formula :

Weight in g of silica
Silica, percent =
Weight in g of sample (W) x loo

7. DETERMINATION OF FERROUS OXIDE BY

VOLUMETRIC METHOD

7.1 Apparatus

7.1.1 Heater
7.1.2 Platinum Crucible - 30 ml capacity with lid.
7.1.3 Bwette - 50 ml capacity.
7.1.4 Porcelain Basin and Wide Mouth Beakev

7.2 Reagents

7.2.1 HydroJuoric Acid

7.2.2 Concentrated Sulphuric Acid - specific gravity l-84.
7.2.3 Boric Acid Solution - saturated.
7.2.4 Potassium Permanganate Solution - standard, 1 ml is equivalent
to 0.0056 g of iron.
7.3 Procedure -Take 0.5 g fibre from the laboratory sample in a
30 ml platinum crucible fitted with lid. Mix 10 ml of hydrofluoric
acid and 10 ml of concentrated sulphuric acid and place the platinum
crucible in a heater. At first heat slowly with the lid fully covering the
crucible and then heat sfrongly avoiding turbulance of the liquid.
After about 15 minutes, when the fibre is decomposed, take the platinum
crucible out of the heater and cool in a ice-cold water-bath in a
porcelain basin or in a wide mouthed beaker. After cooling,’ drop the
crucible and the contents carefully into a wide mouthed flask containing
230 ml of cold (15%) saturated boric acid solution. Titrate the cold
mass with standard potassium permanganate solution.

8
 IS:5328-1969

7.4 Calculations -Determine ferrous oxide percentage by the following

formula:

Volume of potassium
Ferrous oxide, = permanganate in ml x 0~0056 x 1.28 x 1Do
percent
Weight of sample in g

8. DETERMINATION OF FERRIC OXIDE

8.1 Apparatus

8.1.1 Meker Bwner

8.1.2 Platinum Crucible
8.1.3 Platinum Wire
8.1.4 Silica Crucible
8.1.5 Two Burettes -each of 5 ml capacity.
8.1.6 Filter Paper - Whatman No. 40.

8.2 Reagents

8.2.1 Bromine Water

8.2.2 Ammonizcm Chloride ‘Solution - 2 N.
8.2.3 Ammonium Hydroxide Solution -‘2 N.
8.2.4 Hydrochloric Acid Solution - 2 N.
8.2.5 Ammonium Nitrate - 2 percent (rev/v).
8.2.6 Potassium Pyrosulphate - solid.
8.2.7 Dilute Hydrochloric Acid - 1 :l (v/v).
8.2.8 Stannous Chloride Solution - Prepare by dissolving 15 g tin metal
in 350 ml hot concentrated hydrochloric acid (specific gravity l-19) and
dilute to one litre.
8.2.9 Mercuric Chloride Solution - saturated.
8.2.10 Diphenylamine Ilzdicator - Dissolire one gram in 100 ml sulphuric
acid (specific gravity 1.84).
8.2.11 Potassium Dichromate. Afifwoximatelv 0.1 N - Dissolve 4.9 g
of potassium dichromate in water-and dilute- to one litre. Standard&
against a known weight of pure iron using same method as in 8.3.
8.3 Procedure -Treat the filtrate obtained under 6.3.5 as indicated
in 8.3.1 to 8.3.5.

9
IS: 5328 - 1969

8.3.1 Oxidize the iron back to the ferric state by adding bromine
water (or a few drops of concentrated nitric acid) and boiling until
the excess of the latter is expelled. Add 10 ml of 2 N ammonium
chloride solution and several drops of methyl red indicator, and precipitate
the aluminium and iron from the boiling hot solution by adding
dilute ammonia free from carbonate until the solution turns yellow.
Allow the precipitate to settle, filter and wash twice by decantation
with hot water.

8.3.2 Redissolve by running hot 2 N hydrochloric acid through the

filter paper into the beaker containing the greater part of the precipi-
tate. Repeat the precipitation with ammonia as under 8.3.1, and after
filtering and washing by decantation, transfer the precipitate to the
filter paper and wash with water containing 2 percent ammonium nitrate
until free from chloride. Reserve the filtrate for calcium oxide and
magnesium oxide determination.

8.3.3 Allow the precipitate to drain as completely as possible, and

ignite wet in the crucible containing the residue obtained under 6.3.8.
After igniting strongly over a Meker burner, weigh the crucible; its
contents represent the sum of alumina and ferric oxide.

NOTE - The percelitage of total ferric oxide and alumina may be obtained
by the following formula:

Weight. of alumina
Total alumina and fer- and ferric oxide contained in the crucible
ric oxide, percent = X100
Weight of sample (W)

8.3.4 Fuse the mixed oxides with potassium pyrosulphate ,in a silica
crucible using 15 to 20 times as much potassium. Before starting the
fusion, heat the potassium in the silica crucible until fumes of sulphur
trioxide evolve. Add the mixture of oxides to anhydrous potassium
pyrosulphate and heat slowly with a small flame until complete fusion
occurs. Add further small amount of additional pyrosulphate. When
the fusion is complete, make a spiral from a platinum wire and insert
in the melt; When solidified, remove by pulling the wire. Dissolve the
melt in hydrochloric acid (1 : 1 by vol) stirring until all is dissolved.
Dilute this solution to a definite volume and take one-half of it for the
ferric oxide and the other half of it for the alumina determina-
tion.

8.3.5 Heat the liquid taken for the ferric oxide to about 80°C and
while still hot reduce the ferric iron by adding stannous chloride
drop by drop from a burette until the yellow colour of the ferric chloride
just disappears, using a white piece of. paper under the beaker for a

10
better background of colour change. Cool the solution to 15°C Z&C&
while stirring, add 10 ml of mercuric chloride solution. Formation af Ct
light silky precipitate indicates that the conditions are correc6. Stir the
solution vigorously for one ’ minute, add 3 drops of diphenylamine
indicator solution and dilute to 150 to 200 ml with cold distilled water.
Titrate with a standardized solution of potassium dichromate until
the blue colour persists. The concentration of the potassium dichromate
solutoin should be such that one millilitre of the standard solution is equi-
valent to 0.005 6 g iron.

8.4 Calculations -Determine the ferric oxide percentage by the follow-

ing formula :

Volume of potassium
Ferric oxide, dichromate titer in.--ml_---_ 2x 1.43 x loo
x ~005 6x--.--.
percent =
Weight of sample JIf’J

9. DETERMINATION OF ALUMINIUM
OXIDE

9.1 The percentage of aluminium oside shall be obtained by the differ-

ence in the percentage of the total ferric osidc ;trrd aluminium oxide
(see 8.3.3) and the percentage of ferric oxide (see 8.4).

10. DETERMINATION OF CALCIUM OXIDE BY OXALATE

(GRAVIMETRIC) METHOD

10.1 Apparatus

10.1.1 Beaker - 600 ml capacity.

10.1.2 Glass Funnel

10.1.3 Platinum Cmcible

10.1.4 Filter Paper - Whatman No. 40.

10.1.5 Meker Burner

10.1.6 Desiccator

10.2 Reagents

10.2.1 Hydrochloric Acid Solution - 3 N.

11
IS: 5328 - 1969

20.2.2 Ammonilcm Oxalate Sol&ion - 0.5 N.

10.2.3 Ammonium Hydroxide Solution - 2, N.

10.3 Procedure

10.3.1 Make the filtrate, obtained from 3.3.2, acidic with hydrochloric
acid. Bring to a volume of 400 ml, heat to 80” to 9O”C, and slowly
add, while stirring, 30 ml of hot O-5 N ammonium oxalate solution.
Slowly add ammonium hydroxide solution until the solution is slightly
ammoniacal and allow the precipitate to stand several hours before
filtering.

10.3.2 If considerable magnesium is present in the solution, some

magnesium oxalate will come down with the calcium oxalate. Redissolve
the calcium oxalate precipitate and repeat the precipitation, using a
filter paper for filtering off the precipitate. When all the solution has
passed through the filter paper, wash the precipitate with about 15 ml
hot water. Then rinse the precipitate back into the original beaker
by holding the funnel in an inverted position and directing a stream
of hot water against it. Replace the funnel in the support and wash
the filter paper ‘with about 25 ml of hot 3 N hydrochloric acid. Heat the
acid in a test tube, pour it upon the upper edge of the paper, and
catch the liquid as it runs through the filter paper in the beaker con-
taining the precipitate. Finally, wash the filter paper with a little hot
water (and with dilute ammonia if it is to be used again for filtering
the next precipitate).

10.3.3 Heat the dilute acid in the beaker and add a little more acid
if necessary to dissolve the precipitate completely. Dilute the solution
to about 250 ml and repeat the precipitation *of the oxalate at the
boiling temperature, adding ammonia and 5 ml more of the ammonium
oxalate reagent.

10.3.4 Use a filter paper for collecting the precipitate. Wash the
precipitate with hot water until free from chloride, and reserve the
filtrate for the magnesium determination. Transfer the filter paper con-
taining the precipitate to a weighed platinum crucible. Ignite carefully
with the flame at the mouth of the crucible until the precipitate is dry,
and then heat with a small flame at the base of the crucible until all
the paper is decomposed without letting it take fire. Then gradually
raise the temperature and heat over a Meker burner for an hour
with the crucible in an upright position and covered. Cool to about
lOO”C, place in a desiccator, and weigh after 15 minutes, Repeat the
heating until after cooling a constant weight is obtained. The calcium
oxide is somewhat hygroscopic but is not difficult to weigh if it has

12
 IS: 5328 - 1969

been washed free from chloride. Assume weight constant if it agrees

within 0.2 mg with the previous weight.
10.4 Calculations - Determine calcium oxide percentage by the following
formula :
Weight of calcium oxide
Calcium oxide, percent = ---. - ------- -~-.---- ,---,~- x 100
Weight of sample {lb)

11. DETERMINATION OF MAGNESIUM OXIDE

11.1 Apparatus

11.1.1steam Bath or Hot Plate

11.1.2 Beaker and Watch-Glass
11.1.3 Filter Paper --‘Whatman No. 40.

11.2 Reagents

11.2.1 Concentrated Nitric Acid - specific gravity 1.5.

11.2.2 Concentrated Hydrochloric Acid - specific gravity 1.16.
11.2.3 Diammonium Hydrogen Phosphate - solid.
11.2.4Phenolphthalein Indicator
11.2.5 Ammonium Hydroxide Sol&on - 1.5 N.
11.2.6 Concentrated Ammonium H@oxide - specific gravity 0.90.
11.2.7 Ammonium Nitrate Solution. - saturated.

11.3 Procedure

11.3.1 Add 75 ml of concentrated nitric acid to the combined filtrate

and washings reserved under 10.3.4, and evaporate co dryness on the
steam bath or hot plate. Do not boil the solution or there will be loss
by spattering. Keep the beaker covered with a watch-glass supported
above the upper rim of the beaker. A glass triangle, or glass supports
which are made for this purpose, should be used to support the watch-
glass. To the small residue obtained, add 2 ml of concentrated hydro-
chloric acid and 2.5 ml of water. Heat nearly to boiling and, after a
few minutes, filter off the silica residue through a small filter paper.
Wash the beaker, and filter paper thoroughly with hot water. The
silica comes from the action of reagents on reagent bottles or on the
beaker used in the analysis.

13
 .
IS: 5328 - 1969

11.3.2 Dilute the solution to about 150 ml; add about l-2 g of
diammonium hydrogen phosphate dissolved in a little water and a few
drops of phenolphthalein indicator solution. Heat nearly to the boiling
point, and then slowly add 1.5 N ammonium hydroxide solution until
a faint pink colour is obtained and a slight precipitation takes .place.
Stir well for about a minute, touching the sides of the beaker as little
as possible. When the precipitate has become distinctly crystalline, add
more ammonium hydroxide solution until a deep colour is obtained
with the phenolphthalein. Allow the solution to cool, then add one-fifth
the solution’s volume of concentrated ammonium hydroxide and allow to
stand overnight.
11.3.3 Filter off the magnesium ammonium phosphate precipitate.
After washing it with 1.5 N ammonium hydroxide solution moisten
with a saturated solution of ammonium nitrate in 1.5 N ammonium
hydroxide solution, dry and ignite very slowly and carefully at 1 000” to
1 100°C and weigh. The precipitate contains 36.21 percent magnesium oxide.
11.4 Calculations - Determine magnesium oxide percentage by the
following formula:
Magnesium
o x i d e, Weight of magnesium pyrophosphate (Mg2P20,) x O-362 1 x 1oo
percent = -- -.
Weight of sample (W)

12. DETERMINATION OF SODIUM OXIDE

12.1 Apparatus

12.1.1 Platiuunz Dish artd Platinum Crucible

12.1.2 Stout Platinacm Wire
12.1.3 &d&&r or Hot PLate
12.1.4 Water-Bath
12.1.5 Meker Burner
12.1.6 Mechanical Stirrer
12.1.7 Sintered Bed Glass or Porcelain Crucible - IG-4.
12.1.8 Drying Oven

12.2 Reagents

12.2.1 Dilute Sul~huric d&d - 1: 5 (v/v).

12.2.2 Concentrated Hydrojzcoric Acid - specific gravity 1.16.

14
 12.2.3 Barium Hydroxide
12.2.4 Barium Chloride
12.2.5 Ammonium Carbonate
12.2.6 Ammolzium Hydroxide
12.2.7 Hydrochloric Acid
12.2.8 Uratiyl Acetate
12.2.9 Zinc Acetate
12.2.10 Sodium Zinc Uranyl Acetate
12.2.11 Absolute Alcohol
12.2.12 Ether or Acetone

12.3 Procedure
12.3.1 Take one gram of the sample powder in a platinum crucible.
Pour about 5 ml of dilute sulphuric acid (1: 5, V/V), mix it with the
powder by means of a glass rod or stout wire of platinum. Add 5 ml
of concentrated hydrofluoric acid and evaporate until the sulphuric acid
begins to escape. Repeat the evaporation with more hydrofluoric acid
until the mineral is wholly decomposed. Then expel most of the
sulphuric acid by heating over a radiator or hot plate. The expulsion
of fluorine also should be thorough.
12.3.2 Heat the sulphate residue until fumes of sulphur trioxide entirely
cease. Thus oxides or salts of iron, aluminium, titanium and phosphorus
are rendered insoluble in water. Take the contents of the crucible
with hot water in a beaker and wash the crucible thoroughly with
hot water so that the transferring of the material from crucible to
beaker is quantitative. Filter and wash the residue ‘on the filter paper
thoroughly with hot water four or five times. Reject the residue.
Once a clear solution is ‘obtained from the residue, precipitate the
sulphate ion by barium chloride solution in slight excess. Without
filtering, evaporate the liquid to dryness, take up with a little hot
water and add alkali-free barium hydroxide solution until the solution
is alkaline. In order to render the magnesium more insoluble again
evaporate to dryness without filtering. Stir the residue up with water,
filter and wash with a dilute alkali-free barium hydroxide solution.
Warm the filtrate and precipitate most of the excess barium by
ammonium hydroxide and ammonium carbonate. Repeat the operations
until all the barium is removed. Then evaporate the final filtrate to.
dryness in a platinum dish and moisten the residue with a drop of hydro-
chloric acid. Evaporate until ammonia ceases to evolve, ignite
very carefully till the residue just starts melting and weigh the alkali
chlorides after cooling the dish in a desiccator which still contains a
little magnesium as a basic chloride. If on dissolving of the chlorides

*i 15
IS: 5328 - 1969

in a little water any residue is seen, filter and wash with water.
Evaporate the filtrate to dryness and weigh as alkali chlorides.
12.3.3 Determination of Sodium as Sodium-Zinc Uranyl Acetate Hexa-
hydrate -Add. water to the residue obtained in 12.3.2 until the whole
of it dissolves and evaporate on a water bath to about 1.5 ml. Add
15 ml of zinc uranyl acetate (prepared as indicated in 12.3.3.1) and
stir vigorously, preferably mechanically, for at least 30 minutes. Allow
to stand for. one hour, and filter through a weighed sintered bed glass
or porcelain filtering crucible. Wash the precipitate four times with
2-ml portions of the precipitating reagent (allow the wash liquid to
drain completely before adding the next portion), then ten times with
95 percent alcohol saturated with sodium-zinc uranyl acetate at room
temperature (2-ml portions) and finally with a little dry ether or
acetone. .Dry for 30 minutes only at 55” to 60°C. Weigh as sodium zinc
uranyl acetate hexahydrate [NaZn(U09)s(C1H,0&6HZO].
12.3.3.1 Prepcration of zinc uranyl acetate - The reagent is prepared
by mixing equal volumes of solutions A and B and filtering after
standing overnight.
Solution A= Dissolve i0 g of crystallized uranyl acetate [UO&H,O;)s
2H10] in 4 ml of glacial acetic acid and 100 ml of water
(warming may be necessary).
Solution B= Dissolve 60 g of crystallized zinc acetate [Zn(CaHaOJp3HIO]
in 3 ml,of glacial acetic acid and 100 ml of water.
12.4 Calculations - Determine the percentage of sodium oxide using the
following formula :
Sodium oxide, percent =&x WxlOO
where
W = the weight of sodium-zinc uranyl acetate obtained from
one gram of the sample.

13. DETERMINATION OF CARBON DIOXIDE FROM

CARBONATES

13.1 Apparatus

13.1.1 Chemical Balance

13.1.2 Knorr Alkalimeter - consisting of the following parts, connected
suitably. A typical arrangement of the above is given in Fig. 1.
a) Gas washing bottle, A - containing concentrated sulphuric acid
which serves both to indicate the rate of flow and to prevent
any water vapour entering the system from the atmosphere.

16
 IS: 5328 - 1969

b) Dry&z tube OY cylinder. B - filled two-thirds with soda-asbestos

absorbent (ascarite) and one-third with a drying agent to
remove all carbon dioxide from the air.
4 KIZOYYalkalimeter unit, C-which consists of dropping funnel,
a distillation flask, and a condenser fitted with standard taper
joints to form a unit assembly.
4 Gas washing bottle, D - containing a solution of 5 to 10 percent
by weight of silver sulphate in concentrated sulphuric acid. This
serves to absorb any water vapour that escapes from the con-
denser and to remove any hydrochloric acid from the evolved
gases.
4 Drying tube, E - containing copper sulphate to absorb any
hydrogen sulphide generated by the absorption of hydrochloric
acid.
f) Drying tube, F -filled with a suitable drying agent to effect
complete drying.
EdAbsorption tube, G - filled two-thirds with soda-asbestos absor-
bent (ascarite) and one-third with a drying agent to absorb the
carbon dioxide.
h) Absorption tzlbe, H - filled with a drying agent and soda-asbestos
absorbent (ascarite) in the reverse direction to prevent carbon
dioxide from entering the system.
j) Trap, J - to prevent back-flow of water from the aspirator.
k) Valve OY pinched tubing, K - to control the rate of air flow
pulled through the system by the aspirator.

FIG. 1 KNORR ALKALIMETER FOR DETERMINATION OF

CARBON DIOXIDE

17
IS: 5328 - 1969

13.2 Reagents

13.2.1 Concentrated Su@huric Acid - specific gravity. 1.84.

13.2.2 Soda-Asbestos Absorbent (Ascarite)
13.2.3 Silver Sulfihate Solution - 10 percent by weight.
13.2.4 Copper Sulphate - solid.
13.2.5 Diltite Hydrochloric Acid - 1: 1 (v/v).

13.3 Sampling-The sample shall be taken in the same manner

as the laboratory test sample from which specimens were taken
for the preceding analysis. A specimen shall be taken, weighing
approximately one gram and dried to constant weight at 110°C weighing
to the nearest O*OOl g. Let this sample weigh W grams.
13.4 Procedure

13.4.1 Check the gas-flow train to ensure freedom from leaks. Aspirate
a current of air through the system at the rate of about two bubbles
per minute for a period of 10 minutes. Stop the air current and
remove the absorption tubes. Place the ttibes within the balance case
and allow it to stand for several minutes. When ready for weighing,
open the stopcock momentarily and close. Weigh and repeat the above
procedure. The second weight should agree with the first to within
0.005 g. If it does not, repeat this process until the two successive
weighings agree. When a constant weight is reached, replace the ab-
sorption tubes in the gas train.

13.4.2 Transfer about one gram of the sample, weighed to the nearest
0.001 g, to the distillation flask. Wash down any adhering particles
on the inside neck of the flask with distilled water. Add enough
distilled water to the flask so when the apparatus, ,& ?-e&nnected
the tip of the dropping funnel will be submerged about 5 to 10 mm.
Place 50 ml of hydrochloric acid (1 :l) in the dropping funnel and
replace the guard gas-absorption tube at the top of the funnel. Start
the flow of water in the condenser and open all stopcocks except
the one on the dropping funnel. Turn on the aspirator for medium
suction. Adjust the stopcock on the dropping funnel so that the suction
draws the acid slowly into the flask. When all the acid is in the flask,
fully open the funnel stopcock and pull air through the system at the
rate of two or three bubbles per second. After the reaction in the
flask has subsided, warm the contents gently to boiling. When steam
starts to condense in the condenser, turn off the heat. Continue to
draw air through the apparatus for 30 minutes. Reweigh the absorption
bulb as before. The gain ‘in weight represents the carbon dioxide in the
sample.

18
 IS: 5328 - 1%9

13.5 Calculations -Determine the carbon dioxide percentage by the

following formula:

Weight of carbon dioxide absorbed x 1OO

Carbon dioxide, percent = __
Weight of sample (W)

14. DETERMINATION OF WATER OF CRYSTALLIZATION

14.1 Apparatus

14.1.1 Tared Porcelain Crmible

14.1.2 Electric Furnace - 925” f 25°C.
14.1.3 Desiccator
14.1.4 Chemical Balance
14.2 Procedure - Ignite in a tared porcelain crucible, the sample which
has been dried to constant weight, by placing the crucible and contents
in an electric furnace maintained at 925” + 25°C and continue the ignition
for one hour. Cool in an oven at 110°C and then in a desiccator.
Then reweigh to nearest O*OOl g.
14.3 Czilcdations - Determine the water of crystallization percentage
by the following formula:
Water of crystalli- = Loss on ignition, percent (see 14.2) - Carbon
zation, percent dioxide, percent (see 13.5)

19
IS: 5328 - 1969

(Continued from page 2)

Panel- for Amphibole Variety of Indigenous Asbestos, BDC 2: 3: 1
Convener Rcprcscntirtg

SHRI R. K. Srxria Indian Bureau of Mines, Ministry of Petroleum &

Chemicals and Mines & Metals

Members
DR N. C. BASAK Central Fuel Research Institute (CSIR), Jealgora
SWRI N. RISWAS Directorate General of Technical Development
SHRI .A. K. CHATIERJEE Central Building Research Institute (CSIR),
Roorkee -
SHRI S. KRISHNASWAMY In personal capacity (21, Lakshmi Colony, North
Crescent Road, Thyagavaja Nagar, Madras 17)
SHRI PUSALAL MANSINGHKA PusalPl Mansinahka Pvt Ltd. Bhilwara
SHRI V. R. KATaRaJaN Rohtas Industr&s Ltd, Dalmianagar
SHRI RABINDER SIN& National Buildings Organization, New Delhi
SHRI K. V. RA?.IASESHAN Shree Digvijay Cement Co Ltd, Ahmedabad
SWRI S: K. SWAMI Asbestos Cement Ltd, Bombay
SHRI R. THIAGARAJAN Geological Survey of India, Calcutta
SHRI N. VENKATA&AN Hindustan Ferodo ‘Ltd. Bombay
SHRI H. C. VERMA Associated Instrument Manufacturers (India) Pvt
Ltd. New Delhi
DR I. D. VERMA Hyderabad Asbestos Cement Products Ltd,
Hyderabad
DR H. C. VISVESVARAYA Cement Research Institute of India, New Delhi

20
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