1840 - Specification Benzene
1840 - Specification Benzene
1840 - Specification Benzene
( Reaffirmed 1997 )
( Reaffirmed 2004 )
Indian Standard
SPECIFICATION
BENZENE,
FOR
REAGENT
GRADE
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
DK V. RANGANATIIAN
Members
DR U. P. BASU
DR S. P. BH_~TT.~~IIA~~Y.~
((r
BUREAU
OF
INDIAN
STANDARDS
IS :1840-1961
Secrefary
Extra
DR G. M. SAXENA
.\ssistant
Director
( Chem
), ISI
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.
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
range
by
Sulphur
percent
by weight,
Max
compounds
viii)
Water,
percent
ix)
Acidity
or alkalinity
x)
Refractive
index
0.00
To pass the text
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
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.
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
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
All the
containers
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
SAMPLES
AND REFEREE
SAMPLE
FOR
ACCEPTANCE
shall
IS : 1840 - 1961
APPENDIX
( Clause 3.2 )
OF SPECIFIC GRAVITY
DETERMINATION
B-2.1 Apparatus
B-2.1.1 S#ecijc Gravity Bottle -
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-_~-
DE&MINATION
bottle
bottle,
bottle
OF CRYSTALLIZING
IL*.-
- 1961
STIRRER.
!MMERSlON
,-INNER
3 TO 3.5 $
MARK
i-
GLASS LOOP 18 $
OVER ALL
LOADING MATERIAL
MITER
GLASS TEST TUBE
!_
100
0 -
2.
APPARATUS
FOR
IS s 1840 - l%l
B-3.1.4
Thermometer -
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.
and graduations
as
11
IStlW-1961
INT MA ISmm tl
SS O~emm TO IQ mm
FIG. 3
IN1DIA
4mmtD.S
DISTILLATIONFLASK
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
SO
range.
that the heat source can
13
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.
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
OF WATER
+ 3CsH:N = 2CsH:N.Hl
+ CaHjNSGa
Apparatus
Stirrer -
,Microammeter
Reagents
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
where
w=
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
B-10.1.2
B-10.1.3
0.02 N.
0.02 N.
The requirements
if:
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.
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
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Telegrams : Manaksanstha
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Central
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Offices:
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17
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