IS : 1840 - 1961

( Reaffirmed 1997 )
( Reaffirmed 2004 )

Indian Standard
SPECIFICATION
BENZENE,

FOR

REAGENT

GRADE

Third Reprint APRIL 1999

( Incorporating Amendments No. 1 and 2)

UDC

BUREAU
MANAK

Gr 5

OF
BHAVAN,

547.532

Copyright

INDIAN

: 54-4

1972

STANDARDS

9 BAHADUR
SHAH
NEW DELHI
110002

ZAFAR

MARG

August

1961

IS :1840-1961

Indian Standard
SPECIFICATION FOR
BENZENE, REAGENT GRADE
Fine Chemicals

( Organic

and Inorganic

) Sectional

Committee,

CDC 4

Representing

Chairmun

Ministry of Defence (R & D)

DK V. RANGANATIIAN
Members

Bengal Immunity Co Ltd, Calcutta

Development
Wing ( Ministry of Commerce
Industry )

DR U. P. BASU
DR S. P. BH_~TT.~~IIA~~Y.~

((r

SHEI S. L. MEHXA ( Alternate )

SHRI S. K. kk)RKAR

Directorate General of Health Scrviccs ( Ministry

of Health )
SHRI P. S. RAJIA~~AN~RAN ( Alternate)
Kesar Sugar Works Ltd, Bombay
SHRI M. B. DESAI
SRRI N. G. M.4DAN ( Alternate )
University of Bombay, Bombay
DR N. F. DESAI
Amar Dye-Chcm Ltd, Bombay
SHRI S. v. Dgs.41
SHRI J. H. DOS~I ( illterttale )
National Chemical Laboratory (CSIR), Poona
DR J. GUPTA
DR SUK~ DO ( Alternate )
Bengal Chemical & Pharmaceutical
Works Ltd,
SHRI AMIYA KUIVIARLAHIRI
-Calcutta
SHRI MANINDRA CIIAN~RA UAI~SIXI( Alternate )
Indian
Chemicnl
Manufacturers
Associalion,
SHRI B. MAITRA
Calcutta
SHRI M. ROHATGI ( Alfernate )
Sarabhai Chemicals, Baroda
DR S. L. MUKEERJEE
SHRI B. SRINIVASAN ( Alternate )
British Drug Houses (India) Private Ltd. Bombay
DR S. K. MUNSHI
SHRI P. S. STROSS ( Alfernate )
Central Drug Research Institute (CSIR), Lucknow
DR NITYA NAND
Government Test House, Calcutta
REPRESENTATIVE
SHRI K. L. BANEI~JEE ( Alternate )
Directorate General of Supplies & Disposals (MinisSHRI P. B. SAKKAR
try of Works, Housing & Supply )
Atul Products Ltd, Parnera
SHRI B. V. SHAH
SHRI S. M. Mxw~a ( Alternate )
( Continued onpage 2 )

BUREAU

OF

INDIAN

STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

IS :1840-1961

Secrefary
Extra

DR G. M. SAXENA
.\ssistant
Director
( Chem

), ISI

Iancl 1Lr Benzene and Toluene ( Reagent Grades ), CDC 4 : P 1

Sindri

Fertilizers

& Chemicals

Ltd,

Sindri

Sarabhai
Merck Private Ltd, Baroda
Central Drug Research
Institute
(CSIR),

Lucknow

IS : 1840 - 1961

Indian Standard
SPECIFICATION FOR
BENZENE, REAGENT GRADE
0.

FOREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institution
on 15 May 1961, after the draft finalized by the Fine Chemicals ( Organic
and Inorganic ) Sectional Committee had been approved by the Chemical
Division Council.
0.2 Wherever a reference to any Indian Standard appears in this specitication, it shall be taken as a reference to the latest version of the standard.
0.3 In reporting the result 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 wzith IS : Z-1960 Rules for Rounding
OR Numerical Values ( Revised ) .
0.4 This standard is intended chiefly to cover the technical provisions
relating to benzene, reagent grade, and it does not include all the necessary
provisions of a contract.
1. SCOPE
1.1 This standard prescribes the requirements and the methods of sampling
5
and test for benzene, reagent grade.
2. SAMPLING
2.1 Representative
in Appendix A.

samples of the material

shall be drawn as prescribed

3. REQmMENTS
3.1 Description-The
material shall be clear, colourless liquid, with a
characteristic
odour, insoluble in water but completely miscible with
absolute alcohol or ether. It shall be free from suspended matter.
3.2 The material shall also comply with the requirements given in Table I
when tested according to the methods prescribed in Appendix B. Reference
to the relevant clauses of Appendix B is given in co1 4 of the table.
4. PACKING AND MARKING
4.1 Packing - Subject to the provisions of the Red Tariff No. 18 of 1960
issued by the Indian Railway Conference Association with any additions
3

IS : 1840- 1961
~.U-YLLliYL_~-I-~_Lii~il~.-___
TABLE

I REQUIREMENTS

1-.L.r&__f.__>.
L-_ . --Y_I_Y__LI

FOR BENZENE,

REAGENT

GKADE

( Cl0fW 3. )
8F,1,

lll~c)rrrr~ls\ll:s~r

hAR.~CTERIS~IC

~fl~:TllOT~

No.

( l<KV

OF ?lCST
70 CL

(IV .\III:NUI.\
(1
i)

Specific

gravity

Crystallizing

iii)

Distillation

iv)

Residue on evaporation,
weight, lMax

VI
vi)
vii)

0+371 10 O-1:7,1

at 2inC/2ioC

ii)

point

Not less than

range

by

Sulphur

percent

by weight,

Max

compounds

viii)

Water,

percent

ix)

Acidity

or alkalinity

x)

Refractive

index

0.00
To pass the text

Acid wash colour

Thiophene,

5YC:

The difference
bctwccn
the temprraturc(rLmning
points) at which 1 and 91;
percent
of the volunn
taken
has been collccted, shall
not
exceed
0.6C. This rang!: sh;tll
include the tcmprraturr.
of 8O*lY~
percent

Mm

by weight,

a&,

1% j

(.I )

(3)

(1

so.

II-2
b-3
R-4

R-5
b-6

O*OOO25

13-7

To pass 111~test

B-8

0.05

n-n

To pass the test

IL.10

1,495 to 1.497

n-11

and alterations made thereafter, the material shall be packed in ambercoloured glass or other suitable containers compatible with the properties
of the material. The containers shall be securely closecl. \Vhile sealing, the
following precautions shall be observed.
4.1.1 Rubber stoppers or composition corks shall not brused for closing
the containers.
4.1.2 Each container
shall be protected by cover of a suitable
impervious material over the stopper to keep away moisture and dust from
the mouth of the bottle and to protect it while being handled.
4.1.3 Sealing wax or other plastic material, if used, shall be applied in
such a way that it does not contaminate the material when the containers
are opened.
4.2 MarkingThe containers shall be marked with the following information:
Manufacturers name and recognized trade-mark, if any;
Name and grade of the material in the container;
Weight of the material in the container;
Complete analytical data for the characteristics given in Table
4

I;

IS : 1840 - 1961
e) R/lonth and year of manufacture;
f ) Batch number, in code or otherwise,
to enable
facture to be traced back from records; and
g) The words Highly Inflammable.

the lot of manu-

4.2.1 The product may also be tnarked with Standard mark.

4.2.2 The use of the Standard Mark is governed by the provisions
of the
Bureau of Indian Standards Act, 1986 and the Rules and Regulations
made
thereunder.
The details of conditions under which the liccnce for the use of
Standard Mark may be granted to manufacturers or producers nray be obtained
from the Bureau of Indian Standards.

APPENDIX
( Clause 2.1 )
SAMPLING
A-l.

GENERAL

REQUIREMENTS

A-1.0 In drawing,
following precautions
A-l.1
A-l.2

OF BENZENE,

REAGENT

GRADE

OF SAMPLING

preparing,
storing and handling
and directions shall be observed.

test

samples,

the

Samples shall not be taken in an exposed place.

The sampling instrument
shall be clean and dry when used.

A-l.3 Precautions
shall be taken to protect the samples, the material being
sampled,
the sampling
instrument
and the containers
for samples from
adventitious
contamination.
A-l.4 To draw a representative
sample, the contents of each container
selected for sampling shall be mixed as thoroughly
as possible by suitable
means.
A-l.5 The samples shall be placed in clean, dry,%ir-tight
suitable containers
on which the material has no action.
A-l.6 The sample containers
shall be of such a size that
completely
filled by the sample.

glass or other
they

are almost

A-l.7 Each sample container

shall be sealed air-tight with a stopper after
filling, and marked with full details of sampling,
the date of sampling and
the month and year of manufacture.
A-l.8 In addition,
the precautions
A-2. SCALE OF SAMPLING
A-2.1 Lot -

All the

containers

given in 4.1.1 to 4.1.3 shall be observed.

in a single
5

consignment

of the material

IS : 1840- 1961
drawn from a single batch of manufacture shall constitute a lot.
If a
consignment is declared to consist of different batches of manufacture,
the batches shall be marked separately and the groups of containers in each
batch shall constitute separate lots.
A-2.2 For ascertaining conformity of the material in a lot to the requirements of this specification, samples shall be tested for each lot separately.
The number of containers ( n ) to be selected at random from the lot shall
depend on the size of the lot ( N) and shall be in accordance with Table II.
TABLE II NUMBER
LOT

OF CONTAINERS

TO BE SELECTED
No. OF CONTAINERS TO
BE SELECTED

SIZE

.N
(1)
lto

(:I
All containers

5 ,, 100

More

than

At least
10 percent,
with a minimum
of
4 containers
100

At least 5 percent,
with a minimum
of
10 containers

A-2.2.1 In order to ensure randomness of selection,

the following
procedure shall be adopted.
Arrange all the containers in the lot in a
systematic manner and, starting from any container, count them as 1, 2,
3 ,.........,
etc, up to Y, where Y is the integral part of N/n. Every rth
container thus counted shall be withdrawn to constitute the sample.
A-3. TEST

SAMPLES

AND REFEREE

SAMPLE

A-3.1 Procedure for Preparation

-To
prepare a test sample, draw with
an appropriate sampling instrument, small portions of the material from
each container selected for sampling ( see A-2.2 ) and freshly opened. Keep
separately the material drawn out from different containers.
Mix equal
portions of this material from different containers and obtain a composite
sample of not more than 1 500 ml. Divide the composite sample into three
test samples, each test sample being not less than 300 ml. Transfer them
immediately to suitable containers.
One test sample shall be sent to the
purchaser and one to the vendor. The third test sample, bearing the seals
of the purchaser and the vendor, shall constitute the referee sample, to be
used in case of a dispute between the purchaser and the vendor.
A-4. CRITERION

FOR

ACCEPTANCE

A-4.1 The test samples, representative of each lot in a consignment,

satisfy all the requirements given in 3.
6

shall

IS : 1840 - 1961

APPENDIX
( Clause 3.2 )

ANALYSIS OF BENZENE, REAGENT GRADE

B-l. QUALITY OF REAGENTS
B-l.1 Unless specified otherwise, pure chemicals and distilled water [SCG
IS : 1070.1960 Specification for Water, Distilled Quality ( Revised ) ] shall
be employed in tests.
NOTE- ( Pure chemicals shall mean chemicals that do not contain impurities
which affect the results of analysis.
B-2.

OF SPECIFIC GRAVITY

DETERMINATION

B-2.1 Apparatus
B-2.1.1 S#ecijc Gravity Bottle -

25 ml nominal capacity, as shown in

1. The bottle shall be provided with a cap.
B-2.1.2 Water-Bath - maintained at 27.0 rf: 0.5%.
~2.1.3 Thermometer - any convenient thermometer of a suitable range
with O-1 or 02C sub-divisions.

Fig.

0
0

FIG. 1

SPECIFIC GRAVITYBOTTLE

IS : 1840 - 1961
B-2.2 Procedure -Clean
and dry the bottle along with the cap and
weigh accurately
to the nearest milligram.
Hold the bottle in a slightly
inclined position and pour distilled water in such a manner
as to prevent
the entrapment
of air bubbles.
Fill the bottle up to the lower part of the
ground-glass
neck.
Insert the stopper without the cap taking care that no
air bubbles are trapped in the neck and that the small excess of the water
Immerse the bottle vertiis expelled through the capillary of the stopper.
cally in the water-bath
up to not more than 5 mm from the top of the
stopper.
Keep the bottle immersed
in the water at 27.0 f 0.5% and
hold at that temperature
for 30 minutes.
Carefully
remove any water,
which has exuded from the capillary
opening with a piece of filter paper.
Remove the bottle from the bath, replace the cap and wipe completely
dry.
Cool at the room temperature
and weigh accurately
to the nearest
milligram.
Pour out the water and dry the bottle.
Using the material
under test, proceed exactly in the same manner as in the case of water
and weigh the bottle with material.
NOTE -In
case the room temperature is higher than 27C, cool the material to
27C or below prior to filling. . The specific gravity bottle also shall be cooled to a
temperature
lower than 27C immediately
after removal from the bath and weighed
quickly before the bottle attains temperature of 27%.

B-2.3 Calculation
Specific

gravity

where
A = weight

A-B
at 27/27C = c-_~-

in g of the specific gravity

B = weight in g of the specific gravity

c
weight in g of the specific gravity
B-3,

DE&MINATION

bottle
bottle,
bottle

OF CRYSTALLIZING

with the material,

and
with water.
POINT

B-3.1 Apparatur - The crystallizing

point
apparatus
of the shape,
dimensions
and tolerances
given in Fig. 2, consists of the following.
B-3.1.1 Outer Glass Test-Tube - serves as an air-jacket and is weighted
with lead shot or similar loading material.
It is provided
with a cork
through which the inner tube is held in position.
B-3.1.2 Inner Glass Test-Tube -fitted
with a cork which carries a stirrer
in the form of a loop of glass with a glass stem and the thermometer
placed
centrally within the tube and the glass loop. The bottom of the bulb of the
thermometer
shall be about 10 mm from the bottom of the inner tube.
The cork is so fixed that the immersion
mark on the thermometer
is in
level with the top of the cork.
B-3.1,3 Cooling Bath - 1 000.ml glass beaker, about 150 mm in height.
The level of the cooling liquid in the bath shall be at least as high as the
level of the sample in the inner tube.

IL*.-

- 1961

STIRRER.

!MMERSlON

,-INNER

3 TO 3.5 $

MARK

GLASS TEST TUBE

i-

GLASS LOOP 18 $
OVER ALL

LOADING MATERIAL

MITER
GLASS TEST TUBE

!_

100

0 -

f 5 percent tolerance on dimensions except

where otherwise *stated. AH diemeter dimensions are external.
FIG.

2.

APPARATUS

FOR

I~TERMINATION OF CRYSTALLIZING POINT

IS s 1840 - l%l
B-3.1.4

Thermometer -

with the following dimensions and characteristics:

Range
Graduation at each
Immersion
Overall length, MUX
Length of main scale, Min
3ulb length
Distance from bottom of bulb to
bottom of main scale, Min
Error, MUX
Limit of accuracy
B-3.2

- 2Q5C to +205C
0.1%
100 mm
405 mm
280 mm
10 to 15 mm
30 mm
0*3C
0*05C

Procedure

B-3.2.1 Remove the inner tube of the apparatus from its jacket and
introduce a representative
portion of about 20 g of the material for test.
Carry out a preliminary rapid cooling of the liquid to determine the
approximate crystallizing point. Partially immerse the tube in a bath at
about 5C above the crystallizing point, until all but the last traces of
crystals are melted. Replace the inner tube in its jacket, and assemble the
apparatus as shown in Fig. 2, with the cooling bath between 6 to 8C
below the expected crystallizing point. Take thermometer readings at halfminute intervals, with continuous and gentle stirring; this operation being
so conducted that seed crystal is present as the temperature of the sample
The crystallizing point
falls to that at which crystallization commences.
corresponds to the first five consecutive readings during which the temperature remains constant within O*lC.
B-3.2.2 The crystallizing point of a sample which tends to crystallize
with some lack of constancy of temperature
during the crystallization
period of the material should be determined by removing the test-tube
from its jacket at intervals of 2C, quickly but without disturbing the
contents, and replacing in the jacket. This operation should not take more
than three seconds. The crystallizing point should be taken as the temperature at which the bulb of the thermometer ceases to be visible.
B-3.2.3 If supercooling takes place, the constant temperature
should
be observed immediately after temperature-rise.
A temperature-rise
of
1C should be regarded as the maximum allowable.
B-39.4
If a constant temperature is not obtained over the first five
readings after the rise in temperature,
six readings should be taken commencing with the point at which the maximum temperature
is first
attained.
The readings should be plotted on graph paper against time

10

IS : 1840 - 1961
intervals and a straight line drawn to lie evenly between the first and
second and between the fifth and sixth of the six points just mentioned.
This line should be produced backwards until it intersects the portion of
The point of intersection should, in
the curve before the temperature-rise.
this case, be reported as the crystallizing point.
B-4. DISTILLATION RANGE

R-4.1 Apparatus
R-4.1.1 Distillation Flask - of the shape and dimensions shown in Fig. 3.
B-4.1.2 Thermometer - with immersion of 100 mm. The dimensions and
particulars of the thermometer are given below:
65 to 90C
Range
O*lC
Graduation at each
0.5 and 1C
Longer lines at each
Fully figured at each
2C
400 mm
Overall length, Max
215 mm
Length of main scale, Min
12 mm
.Bulb length, Max
f0*4C
Error, Max
25 mm
Distance from bottom of bulb to top of
contraction chamber, Max
The thermometer shall be SO fitted that the bottom of the capillary is in
level with the lower edge of the side tube joint.
B-4.1.3 Liebig Condenser -made
of good quality resistant glass, with a
wall thickness of 1.0 to l-5 mm and conforming to the shape and dimensions
given in Fig. 4.
R-4.1.4 Crow Receiver shown in Fig. 5.

lOO-ml, with dimensions

and graduations

as

B-4.1.5 Rectangular Draught Screen-made

of 0*710-mm ( or 22 gauge)
metal sheet, with the dimensions shown in Fig. 6 and open at the top and
bottom. It shall comply with the following requirements:
a) In each of the two narrow sides of the draught screen, there shall be
two circular holes, each of 25 mm diamet.er, and in each of the
four sides of the draught screen, there shall be three holes with their
centres 25 mm above the base of the draught screen. These holes
shall occupy the position as shown in Fig. 6. The diameter of each of
the holes centrally situated in the longer sides shall be 25 mm and
of the remaining ten holes shall be 12.5 mm. At the middle of each
of the wider sides, a vertical slot with the dimensions shown in
Fig. 6 shall be cut downward from the top of the screen.

11

IStlW-1961

INT MA ISmm tl
SS O~emm TO IQ mm

FIG. 3

IN1DIA

4mmtD.S

DISTILLATIONFLASK

b) A sheet of hard asbestos, 6 mm in thickness, and having a centif

circular hole 100 mm in diameter shall be supported horizontally rn
the screen and shall fit closely to the sides of the screen to ensure
that hot gases from the source of heat do not come in contact with
the sides or neck of the flask. The supports for this asbestos sheet
may conveniently consist of triangular pieces of metal sheet firmly
fixed to the screen at its four corners.

12

IS: 1840-1961

INT

FIG.
4

DIA Mmm

+I

/ t
EXT DIA 35

mm

sstim%5

+3

-L_._.

LIEBIG CONDEMER

In one of the

narrow sides of the screen, a door shall be provided

cl
having the dimensions
and position as shown in Fig. 6. In each of
the narrow sides of the screen, a mica window shall be placed centrally, with the bottom of the window on a level with the top of the
asbestos sheet. The dimensions
and position
of the windows are
shown in Fig. 6.
4 In addition to the asbestos sheet referred to above, an asbestos
This
asbestos
board
board,
150 mm square,
is required.
shall he 6 mm in thickness and shall have a central hole 30 mm
in diameter.
This shall be placed on the asbestos sheet as described
in B-4.1.5(b).
B-4.1.6 Bunsen Burner - giving an entirely non-smoky flame and provided
with an adjustable
screw clip with the help of which the flame may be
lowered or raised according to requirements.
B-4.2 Procedure -Assemble the apparatus
as shown in Fig. 7. Measure
100 ml of the material at laboratory
temperature
into the crow receiver
and transfer to the distillation
flask, the contents of the crow receiver being
allowed to drain for 15 seconds into the flask. Add a fragment of porous
pot or other suitable inert material
to prevent
bumping.
Connect the
condenser to the distillation
flask so that the distance
from the upper end
of the jacket to the neck of the flask shall be 180 to 250 mm. Insert the
thermometer
and pass an adequate
supply of cooling water through the
condenser.
To receive the distillate?
use the crow receiver in which the
sample was measured,
without rinsmg or drying. Heat the flask slowly,
especially after ebullition
has begun,
in such a way that between the start
of heating and the emergence
of the first drop of distillate,
an interval of
time not less than 5 minutes nor more than 10 minutes is taken. Place the
receiver so that. the condensate
flows down its side. Adjust heating
to give
a rate of distillation
of 4 to 5 ml per minute. Continue the distillation and

take the readings of volume in t!le specified temperature

Nom -

It is desirable to run a preliminary distillation

SO

range.
that the heat source can

be regulated to supply heat to distil the liquid at the specified rate.

be cleaned after preliminary distillation.

13

The flask should

IS:1840-1961

T--

1
I

I
I

1 ml

, AT 20% I

250mm+to

,P.
._

I--

70mmf 5 I
FIG. 5 CROW

14

RmXVER

r-2SOm*S

---

rm
lt-'"""

IOOmm

===f

E -=-A=

=A==-_-_-_

FIG. 6

DRAUGHT SCREEN

B-4.3 Corrections of Thermometer Reading tions shall be applied before starting distillation.

The following correc-

B-4.3.1 Error of Scale - In all thermometer readings,

tions as indicated on the certificate of the instrument.

make the correc-

B-4.3.2 Correction for Baremetr_ PTCSSUW-I~ the barometric prwre

prevailing during the determinatron is 760 mm, no correction is necessary
and the thermometer scale as corrected under B-4.3.1 may be wed as such.
If the prevailing barometric pressure deviates from 760 mm, the spaSed
temperature shall be corrected with the correction factor given in Table III
and used on the thermometer scale as corrected under B-4.3.1. Add the
correction if the barometric pressure is lower thah 760 mm and subtract if
it is higher than 760 mm.

IS : 1840 - 1961

,-DISTILLATION

FLAW

RETORT STAND

IEBIG CONDENSE1

FIG. 7 ASSEMBLY
OF APPARATUS FORDETERMINATION OF DBTILLATION RANGE
B-5. DETERMINATION
OF RESIDUE ON EVAPORATION
B-5.1 Procedure - Evaporate 50 ml of the material, accurately weighed,
to dryness in a weighed platinum or silica dish, about 75 mm in diameter
and 20 mm deep, on a water-bath.
Dry the residue in an oven at a
temperature of 100 f 2C for one hour. Cool in a desiccator and weigh.
Express the weight of the residue as percentage of the weight of the
material taken for the test
B-6. T&T FOR ACID WASH COLOUR
B-6.1 Apparatus
B-6.1.1 Stoppered Test-lubes - approximately
100 x 13 mm.
B-6.2 Reagents
B-6.2.1 Sulphuric Acid - 95 percent ( w/w ).
B-6.2.2 Standard Potassium Dichromate Solution - D,issolve O-2 g of potassium dichromate in 1 000 ml of a mixture of equal volumes of sulphuric
acid (98 percent w/w) and water.
R-6.3 Procedure - Take 5 ml of the material in a stoppered test-tube and
place it in a water-bath maintained at 20.0 f 0*5C. Add 5 ml of sulphuric
acid to it. Shake vigorpusly for 2 minutes and allow to stand in the watabath at 20~0-&0*5C for 10 minutes. Compare the colour produced in the
acid layer with that of standard potassium diclwomate solution taken in a
similar t ule.
16

IS : 1840 - 1961
TABLE

III CORRECTION
OF THERMOMETER
BAROMETRIC
PRESSURE
( Chtsc

READING

Ib+.3.2 )

PIm~!suI~l?

~0JtllIV110?I
?I1 1:IfVOMliJl:l:

(1)

nun of

FOR

FOR

b:.\

I)ISt:

(3

Hg

720
725
730

+ 1.8
+ 1.6
+1.3

735
740
745

+I1
+W!l
+0-i

750
755
560

$2
Nil

7G5
770
775

-0~2
-0.4
-0.7

780

-09

B-6.3.1 The material shall be taken to have paqsed the test if the colou~
produced
in the test with the material
is not deeper thnn th;lt of the
standard potassium dichromate
solution.
B-7. TEST

FOR

THIOPHENE

B-7.1 Reagent
B-7.1 .I Isatitz Reagent - Dissolve 6 mg of ferric sulphate in 8 ml of water
and add cautiously 50 ml of sulphuric acid. To this solution add 6 mg of
isatin and stir until dissolved. The colour of this reagent should be pale
yellow; if it is orange or red, the reagent shall be discarded.
B-7.2 Procedure - Shake 1 ml of the material with .5 ml of isatin reagent
for 5 minutes and leave to stand for 15 minutes.
B-7.2.1 The material shall be taken as not having exceeded the limit
prescribed in Table I if no blue colour is produced in the lower layer.
B-8. TEST

FOR SULPHUR

COMPOUNDS

B-8.1 Reagents
B-8.1.1 Absolute Alcohol - conforming
to *IS : 321-1952 Specification for
Ethyl Alcohol ( .4bsolute Alcohol ).
B-8.1.2 Potassium Plumbite Solution- prepared by dissolving
0.8 g of lead
acetate,
1.7 g of potassium
citrate and 25 g of potassium hydroxide
in
water sufficient to make 50 ml.
Since revised.

17

IS: 1840- 1961

B-8.2 Procedure - Take 10 ml of the material in a conical flask and add
Gently
1 ml of absolute alcohol and 3 ml of potassium plumbite solution.
boil the mixture under a reflux condenser for 15 minutes, agitating the
contents of the flask several times and then set aside for 5 minutes.
B-8.2.1 The material shall be taken to have satisfied the requirements
of the test if the aqueous layer remains colourless and/or no separation of
black residue takes place.
B-9. DETERMINATION

OF WATER

B-9.0 Method -The

method ( Karl Fischer method) is based on the
reaction between iodine and sulphur dioxide in the presence of water.
Methanol and pyridine, besides acting as solvent and buffer, also partake
in the reaction as expressed in the following equations:
H,O + l,+Soa

+ 3CsH:N = 2CsH:N.Hl

+ CaHjNSGa

CGH,NSO~ + CHaOH = CsHjN.HSGICHa

B-9.1

Apparatus

B-9.1.1 ?ilration FIask -with

a capacity of 60 to 75 ml, fitted with a
rubber stopper with accommodation for the burette tip, a vent tube
provided with a desiccant, and two platinum electrodes.
B-9.1.2

Stirrer -

magnetic or propeller type.

B-9.1.3 Potentiometer - of resistance 2 000 ohms. Two bright platinum

electrodes which are externally polarized by means of a 1.5~volt dry cell
shall be connected through the potentiometer.
B-9.1.4
B-9.2

,Microammeter

Reagents

~-9.2.1 Preparation of the Fisher Reagent

Solution A - Add 125 g of iodine to a mixture of 650 ml of
methanol and 200 ml of pyridine contained in a flask, and
immediately close the flask tightly.
ii) Solution B - Pass dry sulphur dioxide into 100 ml of pyridine
contained in a 250-ml graduated cylinder and cooled in an icebath, until the volume reaches 200 ml.

i)

iii) Slowly add solution B to the cooled solution A, stopper immediately and shake well until the iodine is dissolved. Transfer the
solution to an automatic pipette protected from absorption of
moisture by a drying agent, and allow to stand for 24 hours
before standardizing. The reagent deteriorates continuously and
it should be standardized within one hour before use.

18

IS : 1840- 1961
B-9.2.2 Standard Water Solution - Measure exactly 2 ml of water into a
thoroughly dry I-litre volumetric flask, dilute to volume with methanol.
Retain sufficient quantity of the same methanol for a blank determination.
Keep the solution in tightly closed containers.
B-9.3

Procedure

.
B-9.3.1 Determination of End Point in Kur2 Ftsher Titration - In many
cases, the end point can be detected visually.by the change from a light
brownish yehow to an amber colour. But when the end point is not cIearly
defined, the electrometric method for determining the end point is adopted.
The potentiometer is adjusted so that when a small excess ( 0.02 ml) of the
reagent is present, a current of 50 to 150 microamperes is recorded. The
solution is continuously and efficiently stirred. At the beginning of the
titration, a current of only a few microamperes will flow. After each addition of reagent the pointer of the microammeter is deflected but rapidly
returns to the original position. At the end point, a deflection is obtained
which endures for a longer period.
B-9.3.2 Standardization of the Fischer Reagent - Pipette exactly 10 ml of
methanol into a dry titration flask and titrate with the Fischer reagent to
the end point. Then pipette exactly 10 ml of standard water solution into
the flask and titrate to the end point.
B-9.3.3 Titration of the Material - Transfer 25 ml of methanol to the
titration Rask and titrate to the end point with the Fischer reagent. Donot
record the volume consumed. Quickly transfer to the titrated liquid an
accurately measured quantity of the material containing IO to 50 mg of
water, stir vigorously and titrate to end point?*
B-9.4

Calculation

Water, percent by weight =

0.1 x W ( vs--2.5 v,)

(Vs-V,)
SA

where

w=

weight in mg of water contained in 10 ml of standard water

solution,
Vs = total volume in ml of the reagent used in titration in B-9.3.3,

I, = volume in ml of the reagent used .in titration of methanol in

B-9.3.2,
V, = total volume in ml of the reagent used in titration in B-9.3.2,
S = specific gravity of the material, and
A = volume in ml of the material taken for test in B-9.3.3.
19

IS : 1840 - 1961
B-10. TEST FOR ACIDITY OR ALKALINITY
B-10.1 Reagents
B-10.1.1 Methyl Red Indicator - Dissolve
[ conforming
to IS : 323-1959 Specification

01 g in 100 ml OS rectified spirit

for rectified spirit ( Revised)].

B-10.1.2

Standard Sodium Hydroxide Solution -

B-10.1.3

Standard Hydrochloric Acid -

0.02 N.

0.02 N.

B-10.2 Procedure - Shake 20 ml of the material

with 10 ml of carbon
dioxide-free
water in a separating
funnel. Draw off the aqueous layer and
add to it one drop of methyl red indicator.
B-10.3

The requirements

of the test shall be satisfied

if:

a) the red colour produced

is changed to yellow by the addition
not more than 01 ml of standard sodium hydroxide solcition;

of

or
b) the yellow colour produced is changed to red by the addition
not more than 0-l ml of standard hydrochloric
acid.
B-11. DETERMINATION

OF REFRACTIVE

of

INDEX

B-11.1 Apparatus
B-11.1.1 Refractometer for circulating
a current of
prisms. The reading of the
the refractometer
adjusted,

Abbe refractometer
with ancillary
apparatus
water through the water jacket surrounding
the
refractometer
shall be checked periodically
and
if necessary.

B-l 1.2 Procedure

B-11.2.1 Circulate
water at above or below 27C through
until a steady temperature
of 27C is recorded.

the apparatus

B-11.2.2 Place a few drops of the sample between the two prisms so that
the liquid is distributed
over the entire space between them. Set the mirror
on the instrument
so that the field is properly illuminated
by a source of
white light, preferably
daylight,
and rotate the double prism gently until
a border line is clearly visible within the field of the telescope.
Adjust the
position of the mirror until the brightest
illumination
is obtained.
If the
instrument
is provided
with colour correction,
rotate the correcting
disc
until the border line shows no chromatic fringe.
Adjust the border line
upon the point of intersection
of the cross wires in the telescope,
and read
off the refractive index directly from the scale by means of the magnifier.
20

BUREAU

OF INDIAN STANDARDS

Headquarters.
Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002
Telephones: 323 0131,323 3375,323 9402
Fax : 91 11 3234062,91
11 3239399, 91 11 3239382
Telegrams : Manaksanstha
(Common to all Offices)
Central Laboratory :
Telephone
Plot No. 20/9, Site IV, Sahibabad Industrial Area, Sahibabad 201010
Regional
Central

8-77 00 32

Offices:

: Manak Bhavan, 9 Bahadur Shah Zafar Marg, NEW DELHI 110002

*Eastern

: 1I1 4 CIT Scheme VII M, V.I.P. Road, Maniktola, CALCUTTA 700054

Northern : SC0 335-336, Sector 34-A, CHANDIGARH

160022

32376

17

337 86 62
60 38 43

: C.I.T. Campus, IV Cross Road, CHENNAI 600113

23523 15
tWestern : Manakalaya, E9, Behind Mar01 Telephone Exchange, Andheri (East), 832 92 95

Southern

MUMBAI 400093
Branch Offices::
Pushpak, Nurmohamed Shaikh Marg, Khanpur, AHMEDABAD
SPeenya Industrial Area, 1 st Stage, Bangalore-Tumkur
BANGALORE 560058

5501348

380001

Road,

839 49 55

Gangotri Complex, 5th Floor, Bhadbhada Road, T.T. Nagar, BHOPAL 462003

55 40 21

Plot No. 62-63, Unit VI, Ganga Nagar, BHUBANESHWAR

40 36 27

Kalaikathir Buildings, 670 Avinashi Road, COIMBATORE

Plot No. 43, Sector 16 A, Mathura Road, FARIDABAD
Savitri Complex, 116 G.T. Road, GHAZIABAD

751001

21 01 41

641037

8-28 88 01

121001

201001

8-71 1996

53/5 Ward No.29, R.G. Barua Road, 5th By-lane, GUWAHATI

541137

781003

5-8-56C, L.N. Gupta Marg, Nampatly Station Road, HYDERABAD

500001

21 68 76

117/418 B, Sarvodaya Nagar, KANPUR 208005

Seth Bhawan, 2nd floor,
LUCKNOW 226001

Behind

Leela

201083
37 29 25

E-52, Chitaranjan Marg, C- Scheme, JAIPUR 302001

Cinema,

Naval

Kishore

Road,

238923

NIT Building, Second Floor, Gokulpat Market, NAGPUR 440010

52 51 71

Patliputra Industrial Estate, PATNA 800013

26 23 05

Institution of Engineers (India) Building 1332 Shivaji Nagar, PUNE 411005

32 36 35

T.C. No. 14/l 421, Univerjity P. 0. Pafayam, THIRUVANANTHAPURAM

621 17

695034

*Sales Office is at 5 Chowringhee Approach, P.O. Princep Street,

CALCUTTA 700072

27 1085

tSales Cffice is at Novelty Chambers, Grant Road, MUMBAI 400007

309 65 28

*Sates Cffice is at F Block, Unity Building, Narashimaraja Square,

BANGALORE 560002

222 39 71

Reprography Unit, BIS, New Delhi, India