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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 11305 (1985): Thionyl Chloride [CHD 1: Inorganic

Chemicals]

“!ा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”
( Reaffirmed 2003 )
 15:11305-1985

Indian Standbrd
SPECIFICATION FOR
THIONYL CHLORIDE

Acids, Alkalis and Halides Sectional Committee, CDC 56

II

Chairman Representing
PROE M.M. TAQUI I<IIAIc Central Salt and Marine Chemicals Research
Institute ( CSIR ), Bhavnagar

Members
DR G. D. BHAT ( Alternate to
Prof M. M. Taqui Khen )
SHRI B. K. AN.~ND Punjab National Fertilizers and Chemicals Ltd,
Chandigarh
SHRI R. C. JAIN ( Alternate )
SHRI M. L. BHAMBANI National Test House, Calcutta
SKRI T. K. DUTTA ( Alternate )
SHRI R. C. BH.ITTACHARYB Directorate General of Technical Developmenr,
New Delhi
SHRI R. N. DAS Bengal Chemicals and Pharmaceuticals Ltd,
Calcutta
SHRI P. N. HALDAR ( Alternate )
SHRI M. V. DESAI Atul Products Ltd, Atul
DR J. M. TUREL ( Alternatr )
SHRI B. L, GUPTA Kothari Industrial Corporation Ltd, Madras
DR H. V. R. IEN~AX E. I. D.-Parry ( India ) Ltd, Madras
DR V. C. NAII~ ( Alternate )
SHRI N. V. KAMBLF: Saurashtra Chemicals, Porbandar
SHRI L. K. MALAVIYA ( Alternate )
SHRI V. B. KHANNA Directorate Genera! of Supplies and Disposals, New
Delhi
SHRI N. K. KANSAL ( Alternate )
SHRI MANMORAN SINGI~ Indian Paper Mills Association, Calcutta
SHRI N. K. GUPTA ( Alternate )
DR B. S. NAQ.~J~ Indian Dyestuff Industiies Ltd, Bombay
SHRI N. R. FADNIS ( Altcmatt )
DR V. N. NICAM Ministry of Defence ( DGI )
SH~I K. B. DUTTA ( Actcrnale )
DR ANIL PANDIT Deepak Nitrite Ltd, Vadodara
SHRI J. T. VORA ( Alternntc )
SHRI M. D. PATEL Gujarat State Fertilizers Co Ltd, Vadodara
SHRI R. N. CHOIZSHI ( Alternate )

( Continued cn page 2 )

@ Copyright 1986
INDIAN STANDARDS INSTITUTION
This publication is protected under the In&n Copyright Act ( XIV of 1957 1 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 : 11305 - 1985

( Continucdfrompagc 1 )

Mcmbrrs Rcpescntiq
SHRI G. C. DUY.TA ROY Shriram Foods & Fertiliser Industries, New Delhi
SRRI S. K. NANDA ( Alternate )
SHRI N. K. SACHAR Gujarat Alkalis & Chemicals Ltd, Vadodara
SRRI J. B. SRARMA ( Alternate )
SRRI V. S. SAXENA Ballarpur Industries Ltd, New Delhi
SHRI J. S. TALWAR ( Alternate )
DR N. SEN Indian Soap & Toiletries Makers’ Association,
Bombay-
DR N. N. SRARMA Tata Chemicals Ltd, Bombay
SRRI K. H. PAREKH ( Alternate)
SHRI S. X. SUBBAROYAN Hindustan Lever Ltd, Bombay
DR A. N. BRAT ( Alternate )
SHRI P. SUBRAMAN~AN Salt Commissioner, .Taipur
SRRI B. REVANNA ( Alternate )
DR M. S. VAIDYA The Dharamsi Morarji Chemical Co Ltd, Bombay
DR A. S. VAIDYANATHAN Standard Alkali ( Chemicals Division ), Bombay
SHRI T. P. VENKATRAMAH ( Alternate )
SHRI H. K. VENKATARAMAIAH Hindustan Organic Chemicals Ltd, Rasayani
DR K. M. VERMA Projects and Development India Ltd, Sindri
SERI-SATISH CH~NDER, Director General, IS1 ( Ex-ojicio Member )
Director ( Chem )
Secretary
SHRI M. BAKSHI GTJPTA
Deputy Director ( Chem ), ISI

Chlorine and its Inorganic Products Subcommittee, CDC 56 : 3

Convener
SHRI V. S. SAXENA Ballarpur Industries Ltd, New Delhi

Members
SHRI J. S. TALWAR ( Alternate to
Shri V. S. Saxena )
DR M. H. BHATT United Phosphorus Pvt Ltd, Bombay
SERI P. MITJIA ( Alternate)
SRRI R. C. BHATTACHARYA Directorate General of Technical Development,
New Delhi
SHRI R. C. SHARMA I\ Alternate
~~ J
SRRI S. N. BHATTACHARYA ‘Tata Chemicals Ltd, Bombay
SHRI D. N. V. RAO ( Alternate)
SERI L. N. CAOWDHARY Indian Paper Mills Association, Calcutta
SHRI M. V. DESAI Atul Products Ltd, Atul
DR J. M. TUREL ( Alternate )
SHRI S. C. GUDI~~ANI Gudimani Enterprises ( India ), New Delhi
SHRI 0. P. JEJANI Kahoria~chemicals and Industries Ltd, Calcutta
SHRI P. K. BANERJEE ( Alternate )
( Continued
onpap 17 )

2
 Indian
Standard
SPECIFICATION FOR
THIONYL CHLORIDE

0. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards
Institution on 29 August 1985, after the draft finalized by the Acids,
Alkalis and Halides Sectional Committee had been approved by the
Chemical Division Council.

0.2 Thionyl chloride finds wide use in dyestuff industries, pesticides,

and as surface active agent. Use of the chemical in vulcanizing rubber,
in wood hardening and in the extraction of gold from its ores is
gradually increasing.

0.3 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 accord-
ance with IS : 2-1960*. The number of significant places retained
in the rounded off value should be same as that of the specified value in
this standard.

1. SCOPE
1.1 This standard prescribes the requirements and methods of sampling
and test for thionyl chloride.

2. GRADES

2.1 There shall be two grades of the material, namely:

a) Technical, and
b) Pure.

3. REQUIREMENTS

3.1 Description - The material shall be in the form of -pale-yellow

liquid.

*Rules for rounding off numerical values ( revised ).

3
IS : 11305 - 1985

3.2 The material shall also comply with the requirements given in
Table 1 when tested in accordance with the methods prescribed in
Appendix A. Reference to the relevant clauses of Appendix A is given
co1 5 of the table.

TABLE 1 REQUIREMENTS FOR THIONYL CHLORIDE

SL CIIARACTERISTIC REQUIREMENT METHOD OF TEST,

No. r------h-----y REF TO CL No. IN
Technical Pure AKJENDIX A

(1) (2) (3) (4) (5)

i) Boiling range ( 95 percent 75 to 78°C 75 to 77w A-2

distillation by volume )
( 5 to 95 ml )
ii) Sulphur chloride ( as &Cl, 0.1 0.50 A-3
and SCl, ) percent by
mass, Max
iii) Iron ( as Fe ), ppm, Maw 20 10 A-4
iv) Sulphuryl chloride ( SOs 2.0 1.0 A-5
Cl8 ), percent by mass,
AJaax
v) Assay ( as SOCl, ) percent 98.0 98.5 A-6
by mass, Min
vi) Relative density at 30°C l-62 1.62 A-7
vii) Refractive index ( nzOD ) -_ 1’517 A-8
viii) Sulphur dioxide ( as SO, ), 0.20 0.20 A-9
percent by mass, Max

4. PACKING AND MARKING

4.1 Packing
4.1.1 The material shall be packed in cleari galvanized iron containers.
4.2 Marking - Each container shall bear legibly and indelibly the
following information:

4 Name and grade of the material;

b) Name of the manufacturer and,‘or his recognized trade-mark, if
any;
4 Net mass of the contents;
4 Date of manufacture;
4 Batch number; and
f) Warning - Corrosive or vesicant to skin, avoid contact with eyes,
skin and clothes.

4
 IS : 11305 - 19S5

4.2.1 The containers may aiso be marked with the ISI Certification
Mark.
NOSB - The use of the IS1 Certification Mark is governed by the provisions of the
Indian Standards Institution ( Certification Marks ) Act and the Rules and Regu-
lations made thereunder. The IS1 Mark on products covered by an Indian Standard
conveys the assurance that they have been produced to comply with the require-
ments of that standard under a well-defined system of inspection, testing and quality
control whichis devised and supervised by IS1 and operated by the producer. ISI
marked products are also continuously checked by IS1 for conformity to that
standard as a further safeguard. Details of conditions under which a licence for the
use of the IS1 Certification Mark may be granted to manufacturers or processors,
may be obtained from the Indian Standards Institution.

5. SAMPLING

5.1 The method of drawing representative samples of the material,

number of tests to be performed and the criteria for conformity of the
material to the requirements of this specification shall be as prescribed
in Appendix B.

APPENDIX A
3.2 )
(Clause
METHODS OF TEST FOR THIONYL CHLORIDE

A-l. QUALITY OF REAGENTS

A-l.1 Unless specified otherwise, pure chemicals and distilled water
( see IS : 1070-1977* ) shall be employed in tests.
NOTE - ‘ Pure chemicals’ shall mean chemicals that do not contain impurities
which affect the results of analysis.

A-2. BOILING RANGE

A-2.1 Apparatus
A-2.1.1 Round Bottom Flask - 200 ml.

A-2.1.2 Thermometer - 0 to 110°C.

A-2.1.3 Leibig Condenser, Band with Long Stem

A-2.1.4 Measuring Cylinder - loo-ml.

A-2.1.5 Glass Beads

*Specification for water for-general laboratory use ( scconl rev&en ).

c
IS : 11305 - 1985

A-2.2 Procedure - Take 100 ml sample in a 200-ml round bottomed

flask. Heat it to distil, then note down the temperature of very first
drop that is starting temperature. Then take a reading after 5 ml and
another after 95 ml keeping a rate of 120 to 125 drops/min,

A-2.3 Result
Boiling range = XC/5 ml to T”C/95 ml
where
X = temperature at 5 ml, and
Y = temperature at 95 ml.

A-3. SULPHUR CHLORIDE

A-3.0 Outline of the Method - It is necessary to remove both iron

and chloride before analysis. This is achieved by carrying out the
preliminary distillation of thionyl chloride after mixing it with
tetrachloroethane.
A-3.1 Reagents
A-3.1.1 Potassium Iodide Solution - 10 percent m/u.

A-3.1.2 Standard Bromate Bromide Solution - 0.1 N.

A-3.1.3 Standard Sodium Thiosulphate Solution - 0.1 N.

A-3.1.4 Concentrated Hydrochloric Acid - See IS : 265-1976*.

A-3.1.5 Tetrachloroethane - Boiling point 140°C.

A-3.1.6 Sulphur Powder

A-3.1.7 Iodine Solution - 0.1 N.
A-3.1.8 Methyl Orange Indicator Solution - 0.5 percent m/v.
A-3.1.9 Starch Indicator - 1 percent ( m/v ).

A-3.2 Procedure
A-3.2.1 Preliminary Distillation with Titrachloroethane - The material
80 ml is diluted to 100 ml with tetrachloroethane ( b. p. 147°C ) and
distilled at a pressure of 120 mm mercury in a ground glass joined
apparatus. To prevent loss of material during distillation the air leak is
kept as small as possible and an efficient dry cold ether reflux condenser
is attached to the receiver, the vacuum being applied at the top of
this condenser. Distillation is continued just to dryness ( preserve
the residue for iron estimation as in A-4.3 ), and the condenser
is drained for 10 minutes. The distillate is diluted to 100 ml. Exactly

*Specification for hydrochloric acid ( secondr&ion ).

6
 18:11305-1985

50 ml of this solution is removed and reserved for determination

( A-3.2.3 ) below. The remaining 50 ml is again diluted to 100 ml with
tetrachloroethane.
A-3.2.2 Hydrolysis and Titration with Bromate-Bromide Solution - Exactly
2 ml of the above solution ( constantly from a 2 ml pipette ) is hydro-
lysed with water ( 50 ml ) at 0°C by shaking vigorously for 2 minutes.
The hydrolisate is warmed to 50% and a vigorous stream of carbon
dioxide or nitrogen passed through for 10 minutes. The solution cooled
to room temperature and iodine solution ( about 0’1 N ) added dropwise
to the first yellow colour, subsequent slow fading being ignored. The
iodine oxidises any sulphur dioxide not removed by gassing. Concent-
rated hydrochloric acid ( 30 ml ) and methyl orange solution ( 2 drops )
are added and the solution is titrated with 0.1 N bromate-bromide
solution until the pink colour of the indicator fades ( tl ml ) potassium
iodide solution ( 10 ml ) is immediately added and the solution diluted
to 200 ml. The liberated iodine is back titrated with 0.1 N thiosul-
phate ), solution ( t2 ml ) volume of 0.1 N bromate-bromide used,
Tl =,(,!I - t2 ) ml.

A-3.2.3 The Sulphur Rejux - The second portion of the distillate

( diluted ) from A-3.2.1, 50 ml is very gently refluxed with 2 g sulphur
powder ( usually about 30 minutes ). The solution is cooled and diluted
to exactly 100 ml with tetrachloroethane. Exactly 2 ml of the diluted
solution is hydrolysed and examined as in A-3.2.2 above. Titrations
t3 ml of O-1 N bromate-bromide and tg ml of 0.1 N thiosulphate volume
of 0.1 N bromate-bromide used, XI;Z = ( tg - tp ) ml.

A-3.3 Calculation
Sulphur chloride ( as S2Cl2 ),
(7Tl--Tz)
pecrent by mass = 3.21
M
and
Sulphur chloride ( as SC12 ),
II 17.2 ( T2 - CT1 )
percent by mass
M
where
M = mass in g of the sample taken for the test.

A-4, DETERMINATION OF IRON

A-4.0 Outline-of the Method - Thioglycolic acid gives a red purple
colour with iron solution in alkaline medium.

A-4.1 Apparatus
A-4.1.1 .Nessler Cylinder - 50-ml-capacity ( see IS : 4161-1967* ).

*Specification for Neder cylinders.

7
IS : 11395 - 1985

A-4.2 Reagents

A-4.2.1 Thioglycolic Acid

A-4.2.2 Citric Acid Solution - 20 percent ( m/v ).

A-4.2.3 Dilute Ammonia Hydroxide Solution - 10 percent.

A-4.2.4 Standard Iron Solution - Dissolve O-702 g of ferrous ammonium
sulphate hexahydrate in 10 ml of dilute sulphuric acid ( 10 percent v/v).
Make the volume up to 1 000 ml. Take 10 ml of this solution and
dilute to 100 ml. One millilitre of this solution contains 0.01 mg of iron
( as Fe ).
A-4.3 Procedure - Add approximately 50 ml water and 10 ml
hydrochloric acid in ~bottom residue of the vacuum distillation flask from
determination of sulphur chloride ( A-3.2.1). Warm it, cool and make
500 ml. Take two 50-ml Nessler cylinders. In both the Nessler cylinders,
take 2 ml citric acid, 5 to 6 drqps thioglycolic acid, and 10 ml of
10 percent ammonium hydroxide solution. In one Nessler cylinder add
10 ml sample solution, red-purple coloured produced in alkaline medium.
Bring same colour intensity in Nessler cylinder by standard solution of
iron by drop-wise addition. Note the volume of standard solution
consumed.
A-4.4 Calculation

38.58 x R
Iron ( as Fe ), ppm =
V

where
R = volume in ml of standard iron solution consumed, and
v = volume in ml taken for the test.
A-4.5 Alternatively, the iron content can also be estimated by measuring
the transmittancy of the coloured complex at 530 nm with the help of
a spectrophotometer.

A-5. DETERMINATION OF SULPHURYL CHLORH)E

A-5.0 Outline of the Method - On hydrolysis sulphuryl chloride
gives hydrochloric acid and sulphuric acid. Sulphate is estimated
gravimetrically as barium sulphate.
A-5.1 Reagents

A-5.1.1 Concentrated Hydrochloric Acid - See IS : 265-1976*.

*Specification for hydrochloric acid ( second revision ).

8
 IS : 11395 w1985

A-5.1.2 Barrium Chloride - 10 percent ( m/v ).

A-5.2 Procedure - Weigh accurately about 15 g of sample in
stoppered weighing bottle. Transfer it into 500-ml beaker containing
ice-cold water under fuming hood. After reaction is over, add 20 ml
of hydrochloric acid. Boil for five minutes, cool to room temperature
and filter. Add 50 ml of 10 percent barium chloride solution. Digest
on water bath for half an hour.

Filter through Whatman No. 42 filter paper. Wash the precipitate

with hot water till free from chloride. Incinerate the filter paper on a
weighed silica crucible at 800°C. Cool and weigh as barium sulphate.
A-5.3 Calculation

Sulphuryl chloride ( as SO&12 ), = 57.84 Me

percent by mass iw,

where
M2 = mass in g of barium sulphate, and
Ml = mass in g of sample taken for the test.

A-6. ASSAY
A-6.0 Outline -of the Method - Thionyl chloride is hydrolised by
aqueous sodium hydroxide to give sodium sulphite. This is determined
by iodimetry.

A-6.1 Reagents

A-6.1.1 Sodium Hydroxide - 10 percent ( m/v).

A-6.1.2 Standard Sodium Thiosulphate - 0.1 N.

A-6.1.3 Standard Iodine Solution - 0.1 N.

A-6.1.4 Starch Solution - 1 percent ( m/v ).
A-6.1.5 Dilute Sulphuric Acid

A-6.2 Procedure - Weigh accurately about 0.8 to 1.0 g of sample in

weighing bottle ( 2-ml capacity ). Drop into stoppered glass flask contain-
ing cold ( below 5°C ) 50 ml sodium hydroxide. Keep it for 10 minutes
shake well. Again keep it for 10 to 15 minutes to come to room temp-
rature. Dilute it to 250 ml in volumetric flask. Pipette out 50 ml
solution into a 500 ml glass stoppered flask containing 50 ml iodine and
20 ml dilute sulphuric acid. Shake well and titrate it against 0’1 N
sodium thiosulphate solution using starch as indicator. Carry out the
blank.
9
IS :11305-1985

A-6.3 Calculation
Thionyl chloride ( as SOCIZ ), =( B–A)X.7VX59”5
percent by mass
M
where

B = volume required to titrate the blank,

A ===volume required to titrate the sample,
N = normality of sodium thiosulphate, and
M == mass of sample taken for test.

A-7. DETERMINATION OF RELATIVE DENSITY

A-7.1 Apparatus
A-7.1.1 Hydrometer
A-7.1.2 Thermometer

A-7.2 Procedure — Pour the material to be tested into the clean

hydrometer jar the diameter of which shall be at least 2“5 cm greater
than the diameter of the hydrometer used. Remove all air bubbles,
that might have formed in the liquid. Keep the jar in a vertical position
and in a water bath maintained at 30”C. When the sample in the jar
attains the temperature of the bath, that is 30°C, lower the hydrometer
gently into the material. When it has settled, depress it to about two scale
divisions into the liquid. Keep the unimmersed portion of the stem dry,
as any unnecessary liquid on the stem wiII change the effective weight
of the instrument and affect the reading obtained. Allow the hydro-
meter to become stationery. Remove all air bubbles that might have
formed during lowering of the hydrometer. Read the point on the
hydrometer scale, to which the sample rises, with the eye placed at the
principal surface of the material. This reading gives the relative
density of the material under test.

A-8. REFRACTIVE INDEX

A-8.O Outline of the Method — The principal of the instrument is
the observation of the critical angle for total reflection between glass
of high refractive index and substance to be examined.

A-8.1 Apparatus
A-8.1.1 Abbe Refractometer

A-8.2 Procedure — To determine the refractive index of a liquid at

20°C, circulate water at 20°C from a thermostat jacket through two
prisms until the temperature on the thermometer has remained steady

10
 IS:11305 -1985

for at least 10 minutes. Separate the prism jacket by opening the clamp
and move the index arm if necessary until the face of the prism is
horizontal. Wipe the water with a paper tissue. Place a drop or two
of the liquid on the ground glass prism face and then clamp it to the
upper polished prism. Focus the cross-wire of the telescope by rotating
the eyepiece and then adjust the mirror SO as to give good illumination
from suitably placed frosted electric lamp. By means of the rack and
pinion controlling the arm at the side of apparatus, turn the prism box
until the field of view becomes partly light and partly dark. When
white light is used, the edge of light band will show a coloured fringe.
By means of milled screw at the base of telescope, rotate the dispersion
compensator until the coloured fringe disappears and the light band is
bounded by a sharp edge coincides with the intersection of the cross-
wires in the telescope and read off directly refractive index for the
D-Sodium line on the divided arc by means of the magnifying lens.
Immediately the determination has been completed, wipe off the in-
organic liquid with a paper tissue and clean the prism surface with a
tissue soaked in acetone.

A-9. DETERMINATION OF SULPHUR DIOXIDE

A-9.0 Outline of the Method - In the hot state, the thionyl chloride
is blasted with nitrogen. Sulphur dioxide, a little quantity of thionyl
chloride and eventually the sulphur chloride present are expelled and
they enter a gas washing bottle.

A-9.1 Reagents
A-9.1.1 Jfitrogen Gas - Pure.
A-9.1.2 Standard Sodium Hydroxide Solution - 1 N.

A-9.1.3 Methyl Orange Indicator

A-9.1.4 Dilute flitric Acid - 20 percent ( v/v ).
A-9.1.5 Dilute Hydrogen Peroxide - 3 percent ( v/v ).

A-9.1.6 Dilute Sodium Bicarbonate Solution - 10 percent ( v/v ).

A-9.1.7 Potassium Chromate Indicator

A-9.1.8 Standard Siloer Nitrate Solution - 0’1 N.

A-9.1.9 Standard Iodine Solution - 0.1 N.

A-9.2 Apparatus

A-9.2.1 Three-Necked Flask - As shown in Fig. 1.

A-9.2.2 Glass Wash Bottles - 250-ml.

11
18:11305-1985

CONOENSOR

500ml,
FLASK

FIG. 1 APPARATUSFOR THE DETERMINATIONOF SULPH~JR DIOXIDE

A-9.3 Produre - About 50 ml of the sample is placed in three-necked

flask with a gas inlet pipe, The nitrogen gas blasted out passes through
the intensive cooler, functioning as a reflux cooler, into two serially fitted
glass bottles for gas washing; each containing 100 ml of 1 N sodium
hydroxide solution ( soda lye ). These bottles are cooled with water.
The flask containing thiony~l chloride is heated till ~obtaining weak reflux.
The sulphur dioxide is then blasted out with a weak stream of nitrogen
from the round flask into the receiver ( absorption bulb ).
A-9.3.1 The blasting continues for about 30 minutes, as a result the
absorption solution in the first wash bottle has to neutralize directly. In
order to check an over acidification few drops of methyl orange can be
added into second wash bottle. Subsequently, both the bottles trans-
ferred and washed in a 500-ml measuring flask, and dilute up to the mark
with water.
Additional sulphur dioxide due to decomposition of thionyI
chloride must be calculated with separate hydrochloric acid estimation.
The total value of sulphur dioxide is then corrected with the share from
the thionyl chloride.

12
 IS : 11305- 1985

A-9.4 Calculation
A-9.4.1 Hydrochloric Acid Esfimation - The solution ( 50 ml ) to be
analysed is measured out from the measuring flask with a burette into a
conical flask and the sulphur dioxide is oxidised with about 10 ml of
3 percent hydrogen peroxide and then make slightly acidic with dilute
nitric ~acid.
After the solution is neutralized with sodium bicarbonate, 12 drops
of potassium chromate indicator are added and the solution is titrated
against 0.1 N silver nitrate solution. The indicator is added before the
titration.

In case of consumption of (a’ ml of 0.1 N silver nitrate solution,

till a sudden change takes place the following relation is true:

‘a’ ml of 0.1 N silver nitrate x 0.036 47 = ( g ) hydrochloric

acid. or, ( g ) hydrochloric acid x 0.877 5 = ( g ) sulphur dioxide
from thionyl chloride = A ( say ).

A-9.4.2 Sulphur Dioxide Estimation - In a conical flask, about 100 ml

of water is poured and to it, 20 ml of 0.1 N iodine solution is added
from the burette and the solution is acidified with about 5 ml of sulphuric
acid diluted in a ratio of 1:3.

The sample solution to be analyzed is filled in a burette and the

pre-treated iodine solution is titrated till its decolouration. 20 ml of 0.1 N
iodine solution corresponds to 64 mg of sulphur dioxide with a consump-
tion of ‘a’ ml of the sample solution.

500 x 0.006 4
= ( g ) sulphur dioxide total
a
( in 500 ml solution ) = B ( say )

Sulphur dioxide ( as SO2 ),

= (A-B) x 100
percent by mass
M

where

M = mass in g of the sample taken for test.

13
IS : 11305 - 1985

APPENDIX B
( Czaust?5.~13
SAMPLING OF THIONYL CHLORIDE

B-l. SCALE OF SAMPLING

B-l.1 Lot - All the containers in a single consignment of the material

of the same grade and drawn from a single batch of manufacture shall
constitute a lot. If the consignment is found to consist of different
batches of packing, the containers belonging to the same batch shall be
grouped together and each such group shall constitute a separate lot.

B-l.2 For ascertaining the conformity of the material in the lot to the
requirements of the specification, samples shall be tested separately from
each lot. The number of containers to be selected at random from the
lot shall depend upon the size of the lot and shall be in accordance with
Table 2.

TABLE 2 NUMBER OF CONTAINERS TO BE SELECTED

No.0~ CONTAINERS SAMPLE SIZE

IN A LOT

(Jv) (n)

(1) (2)

up to 50 4

51 ” 100 5
101 ” 300 7

301 ” 1 000 10

1001 and above 15

B-1.2.1 In order to ensure randomness of selection, random number

tables shall be used. For guidance and use of the random number
tables reference may be made to IS : 4905-1968*. In case these tables
are not available, the following procedure is recommended for use:

Starting from any one container, count them as 1, 2 , . . . . . . . . . . . . . . f->

where Y is the integral part of N/n ( N and n being the lot size and
sample size respectively ). %very rth container thus counted shall be
withdrawn to constitute the sample.

*Methods for random sampling.

14
 IS : 11305 - 1985

B-2. PREPARATION OF TEST SAMPLES

B-2.1 From each of the containers selected according to B-1.2.1, a

representative portion of the material, sufficient to make triplicate
determination for all the requirements given in 3, shall be drawn.
B-2.2 Out of these portions a small but approximately equal quantity of
material shall be taken and thoroughly mixed to form a composite
sample, sufficient to carry out triplicate determination for all the
characteristics tested on the composite sample. The composite sample
shall be divided into three equal parts, one for the purchaser, another
for the supplier and the third to be used as referee sample.
B-2.3 The remaining portions of the material from each container shall
be divided into three equal parts each forming an individual sample,
one set of individual samples shall be marked for the purchaser, another
for the supplier and the third to be used-as a referee sample.
B-2.4 All the individual and composite samples shall be transferred to
separate containers. These containers shall be sealed air-tight and
labelled with full indentification particulars.

B-2.5 The referee sample consisting of a composite sample and a set of

individual samples shall bear the seals of both the purchaser and the
supplier. They shall be kept at a place agreed to between the purchaser
and the supplier to be used in case of any dispute between the two.

B-3. NUMBER OF TESTS

B-3.1 Tests for the determination of sulphuryl chloride -and assay

( Table 1 ) of the material shall be conducted on each of the individual
test samples and the test results shall be recorded separately for different
test samples.
B-3.2 Tests for the determination of all other characteristics given in
Table 1 shall be carried out on the composite test sample.

B-4. CRITERIA FOR CONFORMITY

B-4.1 From the results recorded according to B-3.1, the mean ( a ) and
range ( R ) of test results for any characteristic shall be computed as
follows:
Sum of test results 1, 2 ,... . .fz
Mean(X) =
Number of test results, n
Range ( R ) = difference between the maximum and minimum of
the test results.

15
IS : 11305- 1985

B-4.2 In the case of samples of size 10 or more, every 5 test results

shall
be grouped together and the range of each group shall be determined.
Average range ( R ) shall then be computed from the group ranges as
given below:
Sum of group ranges
Average range( R 1= Number of groups

B-4.3 The lot shall be declared as conforming to the requirements of the

specification for different characteristics if the corresponding criteria for
conformity given below are complied:

Characteristics Criteria for Conformi@

a) Suphuryl chloride ( a + 0*6R* ) shall be less than or

equal to the relevant limit prescribed
in Table 1.

b) Assay ( x - 0.6R* ) shall be greater than or

equal to the relevant limit prescribed
in Table 1.

c) Other characteristics Tests results on the composite test

sample shall meet the corresponding
requirement given in Table 1.

*When the sample size is 10 or more, an average range ( z ) ( see B-4.2 ) shall be
used in place of range ( R ).

16
 IS : 11305 1985
l

( Continued from page 2 )

Members Refirescntinp
SRRI M. P. MISTRY Excel Industries Ltd, Bombay
SHRI D. B. MEHTA ( Alternate)
SXRI l3. M. NAII~ Indian Dyestuff Industries Ltd, Bombay
SHRI D. P. PATEL ( Alternate)
SHRI K. M. SHAH The Millowners’ Association, Bombay
SHRI V. D. SHAR~~A Shriram Foods & Fertiliser Industries, New Delhi
SHRI P. K. BATERJEE ( Alternate )
SHRI M. R. SOMAYAJI The Mettur Chemical & Industrial Corporation Ltd,
Mettur Dam
SHRI D. SESHASAYEE ( Alternatc )
SHRI S. P. SRXVASTAVA Gujarat Alkalis & Chemicals Ltd, Vadodara
SHRI N. K. SACHAR ( Alternate )
DR A. S. VAIDYANATHAN Standard Alkali, Chemicals Division, Bombay
SHRI T. P. VENRATRAMAN ( Alternate )

17
INTERNATIONAL SYSTEM OF UNITS ( SI UNITS j
Base units
QUANTITY UNIT SYMROL

Length metre m
Mass kilogram kg
Time second 9
Electric current ampere A
Thermodynamic kelvin K
temperature
Luminous intensity candela cd
Amount of substance mole mol

Supplementary Units

QUANTITY UNIT SYhlBOL

Plane angle radian rad

Solid angle steradian sr

Derived Units

QUANTITY UNIT SYMBOL DZXINITION

Force newton N 1 N = 1 kg.m/s”

Energy joule J 1 J = 1 N.m
Power watt W 1 w = lJ/s
Flux weber Wb 1 Wb = 1 V.s
Flux density tesla T 1 T = 1 Wb/ms
Frequency hertz Hz 1 Hz = 1 c/s (s-3
Electric conductance S 1 S = 1 A/V
Electromotive force volt V 1 V = 1 W/A
Pressure, stress Pascal Pa 1 Pa = IN/m'
 AMENDMENT NO. 1 MARCH 1995

fS 11305 : 1985 SPE&ATION FOR THIONYL

CHLORIDE
[Page 4, Tubie 1, SZNo. (ii), co1 3 ] -Substitute ‘0.5’fir ‘0.1’.
[Page 4, Table 1, SENo. (ii), cot 4 J - Substitute ‘0.1' far ‘0.50’.

(CMDOO2)
ReprographyUnit, MS, New Delhi, India