IS 534: Benzene

2007·2.9 MB·English

by  Bureau of Indian Standards

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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.
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“The Right to Information, The Right to Live” “Step Out From the Old to the New”
IS 534 (2007): Benzene [PCD 3: Petroleum, Lubricants and
their Related Products]
“!ान $ एक न’ भारत का +नम-ण”
Satyanarayan Gangaram Pitroda
““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee””
“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै”
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”

IS 534:2007

Indian Standard
BENZENE — SPECIFICATION
(Fourth Revision )
ICS 71.080.15

0 BIS 2007
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

November 2007 Price Group 11
Petroleum, Lubricants and Their Related Products Sectional Committee, PCD 3
FOREWORD
This Indian Standard (Fourth Revision) was adopted by the Bureau of Indian Standards, after the draft finalized
by the Petroleum, Lubricants and Their Related Products Sectional Committee had been approved by the Petroleum,
Coal and Related Products Division Council.
Benzene isderived by suitable fractionation and refining by washing with acid or hydrorefining of crude benzole
recovered from the gas produced during carbonization of coal in coke ovens and retorts or recovered as by-
product in petroleum refining or petrochemical operations.
Earlier benzene was essentially acoal base product being made available as by-product from coke ovens of steel
plants. The requirements and methods of test were also stipulated on the basis of the publications by National
Benzole and Allied Products Association (NBA) and the Standardization ofTar Products Test Committee (STPTC),
UK inorder to suit the prevailing quality of the product. However, cognizance was taken of the fact that consequent
upon exploration of oil fields in the recent past specially the Bombay High, substantial quantities of indigenous
crude was being made available, which has completely changed the scenario. On a quantum basis there is a
distinct shift in production of various aromatic hydrocarbons from coal base to petroleum base as a result of
which benzene is currently being made available in abundance. The Committee, therefore, decided to update the
standard in accordance with the latest developments in the field, both in production and usage and in the light of
the experience gained in the past.
This standard was first published in 1955. In view of the growing demand for benzene for organic synthesis it
was considered necessary to include the material for this end use also. It was also felt that pure and ordinary
grades of the material should be brought under acomposite standard on the subject. The standard was, therefore,
revised in 1965 amalgamating with IS 535: 1955 ‘Specification for benzene, pure, nitration grade’. In the second
revision, the method of test for total sulphur was replaced by Raney nickel method, as the latter was found more
convenient and reliable. Various changes covered under Amendment No. 1 issued in March 1973 were also
incorporttted in the third revision.
In the third revision in 1992, keeping in view various end uses and the source of crude base, benzene was
classified into three types. In view of stringent quality of benzene required for the manufacture of caprolactam,

it was decided to incorporate additional requirement of aliphatic and aromatic impurities and bromine index.

In the present revision, Type C has been deleted in order to align with the International practices. Additional
requirements like purity of benzene by GC method including percent of toluene, non-aromatic hydrocarbons 1,4
dioxane, carbon disulphide, N-formylmorphine as nitrogen, residue on evaporation and n-heptane have been
included, in addition to making the requirements of other characteristics more stringent. Requirements like copper
corrosion and neutrality have been deleted.
‘IS 1840:1961 Benzene, reagent grade’ has been withdrawn, as itwas observed by the technical committee, that
this standard would cover the requirements of reagent grade benzene.
In the formulation ofthis standard, considerable assistance has been drawn from the following standards published
by International Organization for Standardization (1S0) and American Society for Testing and Materials, USA:
ASTM D 835:1995 Standard specification for refined benzene — 485 (withdrawn)
ASTM D 848:1997 Standard test method for acid wash color of industrial aromatic hydrocarbons
ASTM D 850:1999 Standard test method fordistillation ofindustrial aromatic hydrocarbons and related
materials
ASTM D 852:1997 Standard test method for solidification point of benzene
ASTM D 853:1997 Standard test method for hydrogen sulfide and sulfur dioxide content (qualitative)
of industrial aromatic hydrocarbons
(Continued on third cover)
IS 534:2007
Indian Standard
BENZENE — SPECIFICATION
(Fourth Revision )
1SCOPE 5REQUIREMENTS
This standard prescribes the requirements and the 5.1 Description
methods of sampling and tests for benzene.
The material shall be a clear liquid, free of sediments
and haze when observed at 18° to 26”C.
2REFERENCES
5.2 The material shall comply with the requirements
The following standards contain provisions which,
as given in Table 1.
through reference in the text, constitute provisions of
this standard. At the time of publication, the editions
6PACKING, MARKING AND STORAGE
indicated were valid. Allstandards are subject torevision,
and parties to agreements based on this standard are 6.1 Packing and Storage
encouraged toinvestigate the possibility ofapplying the
6.1.1 The material shall be packed asagreed tobetween
most recent editions of the standards indicated below:
the purchaser and the supplier.
ISNo. Title
6.1.2 All the containers in which the material ispacked
82:1973 Method of sampling and test for
shall be dry, clean, and free from substances soluble
thinners and solvents for paints @-st
in benzene and leak proof.
revision)
1070:1992 Reagent grade water (third revision) 6.1.3 The containers shall be securely closed, protected
1260 (Part 1): Pictorial marking for handling and from light, and shall be stored in acool place.
1973 labelling of goods: Part 1Dangerous
6.1.4 The containers for storage and transport of the
goods (ftrst revision)
material, since classified as flammable and dangerous
1446:2002 Classification of dangerous goods
goods, shall, in addition comply with the requirements
(secortd revision)
of the latest issue of Red Tariff and the requirements
4644:1968 Code of safety for benzene, toluene
as laid down from time to time by the Chief Controller
and xylene
of Explosives, Government of India, for packing,
4905:1968 Methods for random sampling
storage and transit of flammable liquids and the Board
5165:1969 Interchangeable conical ground-
ofTrade Regulations asapplicable thereon for transport
glass joints
by steamers.
3 TERMINOLOGY 6.1.5 Necessary safeguards against the risk arising from
the storage and handling oflarge volumes offlammable
For the purpose of this standard, the definitions given
liquids (see IS 1446) shall be provided and all due
in IS 82 and the following shall apply.
precautions shall be taken [see IS 1260 (Part 1)] at all
3.1 Bromine Index — The number of milligrams of times to prevent accidents by fire or explosion.
bromine consumed by 100 g of sample under given
6.1.6 Except when they are opened for the purpose of
conditions.
cleaning and rendering them free from benzene vapour,
3.2 Solidification Point — An empirical constant all empty tanks or other containers shall be kept
defined as the temperature at which the liquid phase securely closed unless they have been thoroughly
of a substance is in approximate equilibrium with a cleaned and freed from benzene vapour.
relatively small portion of the solid phase.
6.2 Marking
4TYPES
6.2.1 Each container shall be securely closed and
There shall be two types of material, namely: marked legibly and indelibly with the following
information:
a) Type A — Suitable for manufacture of
caprolactam; and a) Name and type of the material,
b) Type B — Suitable for manufacture of b) Indication of the source of manufacture,
other products
c) Net mass of the material in the container,

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IS 534:2007
d) Batch number or code number, and carefully (see IS 4644). Exposure of benzene in
e) Date of manufacture. atmosphere should be monitored regularly. Persons
exposed to benzene shall be periodically checked
6.2.2 Each container shall have the caution label
according to State Factory Rules and Local State
‘FLAMMABLE’ together with the corresponding
Regulations.
symbol for labelling of dangerous goods as given in
IS 1260 (Part 1). 8SAMPLING
6.2.3 BIS Certification Marking Representative samples of the material shall be
The containers may also be marked with the BIS prepared as prescribed in Annex M.
Certification Mark.
9TEST METHODS
6.2.3.1 The use of the Standard Mark is governed by
9.1 Tests shall be conducted according to the methods
the provisions ofBureau ofIndian Standards Act, 1986
referred to in CO15 of Table 1.
and the Rules and Regulations made thereunder. The
details of conditions under which the licence for the
9.2 Quality of Reagents
use of the Standard Mark may be granted to
manufacturers or producers may be obtained from the Unless otherwise specified, pure chemicals and
Bureau of Indian Standards. distilled water (see IS 1070) shall be employed in
tests.
7 HANDLING
NOTE— ‘Purechemicals’shallmeanchemicalsthatdonot
Benzene ishighly toxic and therefore itshall be handled containimpurities,whichaffecttheresultsofanalysis.
Table 1Requirements for Benzene
(Clauses 5.2,9.1 and M-6.1. 1)
S1 Characteristic Requirement Methods ofTest,
A
No. < -1 ReftoAnnex
TypeA TypeB
(1) (2) (3) (4) (5)
O Benzene,percentbymass,Min 99.90 99.80 A
ii) Colour,Pt-Coscale,Max 10 10 B
iii) Relativedensity,15.56/15.56°C 0.8820to0.8860 0.8820 to0.8860 c
or
Density20”C,ml 0.8780to0.8820 0.8780 to0.8820 c

iv) Sulphur,mg/kg,Ma 1 Asagreedtobetweenthe D
purchaserandthesupplier
v) Distillationrangeincludingthetemperature80.1‘C 1.0 1.0 E
at101.3kPa(760mmHg)pressure,“C,Max
vi) Non-aromatichydrocarbons,percentbymass,Mux 0.10 0.10 A
vii) Toluene,percentbymass,Max 0.01 0.05 A
viii) Bromineindex,Max 10 20 F
ix) Solidificationpoint,anhydrousbasis,“C,Min 5.45 5.35 G
x) Thiophene,mgikg,Max 0.6 1 H
xi) Acidwashcolour,Max Passwith1 Passwith1 J
xii) N-formylmorphineasnitrogen Asagreedtobetweenthe Asagreedtobetweenthe K
purchaserandthesupplier purchaserandthesupplier
xiii) 1,4Dioxane do — A
xiv) Carbondisulphide do Asagreedtobetweenthe L
purchaserandthesupplier
xv) Residueonevaporation,mg/100ml,Max do do Clause8of
IS82
xvi) n-heutane,higheraliphaticandacycliccom~ounds do do A
(cycjohexane-andm&hylhexane):mgikg,~az
NOTE—IfpuritybyGCmethod[S1No.(i)]iscarriedout,distillationtestandsolidificationpointtestareoptional.
IS 534:2007
ANNEX A
[Table 1, S1No. (i), (vi), (vii), (xiii) and (xvi)]
DETERMINATION OF PURITY OF BENZENE BY GC
A-1 OUTLINE OF THE METHOD Table 2 fipical Instrumental Parameters
A-1.l A known amount of an internal standard is (Clauses A-3. 1andA-5. 1)
added tothe specimen. A small volume of this mixture
S1 Characteristic Requirement
is injected into agas chromatography equipped with a
No.
flame ionization detector (FID) and a capillary
(1) (2) (3)
column.
O Detector Flameionization
A-1.2 The peak area of each impurity and the internal ii) Column: Fusedsilica
a) Length,m 50
standard is measured by an electronic integrator. The
b) Insidediameter,mm 0.32
concentration of each impurity is calculated from the
c) Stationaryphase Crosslinked
ratio of the peak area of the internal standard versus polyethyleneglycol
the peak area of the impurity. Purity is calculated by d) Filmthickness,~m 0.25
iii) Temperatures:
subtracting the sum of the impurities found from
a) Injector,“C 200
100,00 mass, percent. Results are reported in mass,
b) Detector,“C 250
percent. c) Column,“C 70isothermal
iv) Carriergas Helium
A-2 INTERFERENCES v) Linearvelocity,crds 22
vi) Splitratio 200:1
A-2.1 Benzene is typically resolved from naturally vii) Samplesize,@ 0.5
occurring components with boiling points less than viii) Recorder Electronicintegrationrequired
138”C. Naturally occurring components include non-
aromatic hydrocarbons, toluene, C8 aromatics and 1, A-4.2 High Purity Benzene, 99.99 percent by mass,
4-dioxane. An adequate separation ofknown impurities minimum, prepared by multiple step recrystallization
from benzene should be evaluated for the column of commercially available benzene of not less than 99
selected. percent purity.
A-2.2 The internal standard chosen shall be sufficiently
A-4.3 Internal Standard, rz-Nonane, (nC,J with a
resolved from any impurity and the benzene peak.
purity of 99 percent by mass, minimum is
recommended. Other compounds may be acceptable
A-3 APPARATUS
provided they can be obtained in high purity and meet
A-3.1 Gas Chromatograph — Any c hromatography the requirements of A-2.2.
having aflame ionization detector that can be operated
A-4.4 Pure compounds for calibration should include
at the conditions given in Table 2 may be used. The
toluene, benzene, ethyl benzene, cyclohexane and 1,4-
system should have sufficient sensitivity to obtain a
dioxane of apurity not less than 99 percent. Ifthe purity
minimum peak height response for a 0.000 5 mass,
of the calibration compounds is less than 99 percent,
percent impurity twice the height of the signal
the concentration and identification of impurities must
background noise.
be known so that the composition of the final weighed
A-3.2 Electronic Integrator — Computer based blends can be adjusted for the presence of the
capable of handling internal standard calculations and impurities.
peak grouping is recommended.
A-5 PREPARATION OF APPARATUS
A-3.3 Column — Fused silica capillary column with
crosslinked polyethylene glycol stationary phase is A-5.1 Follow manufacturer’s instructions for
recommended. Alternate stationary phases may beused mounting the column into the chromatography and
if they produce at least the same aromatic separation adjusting the instrument to the conditions described
and elute Cgnon-aromatic impurities before benzene. inTable 2.Allow sufficient time for the equipment to
reach equilibrium.
A-3.4 Microsyringes, 10 and 100 !-dcapacity.
A-4 REAGENTS AND MATERIALS A-6 CALIBRATION
A-4.1 Carrier Gas, chromatographic grade helium is A-6.1 Prepare a synthetic mixture of high purity
recommended. benzene and representative impurities by direct

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IS 534:2007
weighing. Weigh each impurity tothenearest O.l mg. where
Table 3 contains a typical calibration blend. RRFi = impurity, i;
Cyclohexane is used for the non-aromatic portion and
A, = peak area of internal standard;
ethyl benzene for the C8aromatic portion.
Ai = peak area of impurity, i;
Ci = percent by mass, impurity, i, from A-6.2;
Table 3‘&pical Calibration Blend, G
and
S1No. Compound Weight, Percent c,, = concentration of internal standard, percent
(1) (2) (3) by mass from A-6.3.
i) Benzaie 99.0000
ii) Toluene 0.0500 A-7 PROCEDURE
iii) Cyclohexane 0,0500
iv) Elhylbenzene 0.0500 A-7.1 Into a 50-ml volumetric flask, add 50 U1of nCg
\) 1,4Dioxane 0.0200 internal standard and dilute to the mark with specimen.
Mix well.
A-6.2 Using the exact mass for each impurity, calculate
A-7.2 Inject 0.5 INof mixture into the chromatography.
the percent by mass, concentration of the calibration
blend. A-7.3 Integrate the area under all peaks except for
A-6.3 Into a50-ml volumetric flask, add 50 ml of nCg benzene. Sum the non-aromatic fraction up to nCg for
reporting asasingle component (see Fig. 1for atypical
to49.95 mlof the calibration blend and mix well. Using
adensity of 0.874 g/ml for the calibration blend and a chromatogram).
density of 0.718 g/ml for the nCg, the resulting nCg
A-8 CALCULATION
concentration will be 0.0825 percent by mass.
A-8.1 Calculate the amounts of each individual
A-6.4 Inject 0.5 L1of the blend with internal standard
impurity as required. Sum the areas of all the non-
into the chromatography and integrate the area under
aromatic peaks.
each peak, excluding benzene.
A-6.5 Calculate the relative response factors (RRF) as A-8.2 Calculate the mass, percent concentration ofeach
follows: impurity as follows:
RRFi = (A,)(Ci)/(CJ(Ai) Ci= (Ai)(RRFi)(CJ(AJ
A-8.3 Calculate the benzene purity as follows:
RI Benzene, percent by mass= 100.00- Ci
za) I where
ccN % $ac) Ci = total concentration of all impurities, percent
L’ by mass.
-1
I I I
l“’’I’’’’ 1’’’’ 1’’’’ 1’’’’ 1’’’’ 1’’’’ 1’’’’ 1’’”1
0.0 1.2 2.4 3.6 4.8 6.0 7.2 8.4 9.6 10.8 12.0
MINUTES
FIG. 1TYPICALCIIROMATOGRAM

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IS 534:2007
ANNEX B
[Table 1, S1No. (ii)]
DETERMINATION OF COLOUR (PLATINUM-COBALT SCALE)
B-1 OUTLINE OF THE METHOD B-5 PREPARATION OF STANDARD
CALORIMETRIC SOLUTIONS
Vkual comparison of the colour of asample with that of
colour standard, and expression of the result in terms of B-5.1 Standard Calorimetric Solution, 500 Hazen
Hazen (platinum-cobalt) colour units. For routine control Units — Dissolve 2.00 g of the cobalt chloride
purposes aninstrument such asacomparator, calorimeter (see B-3.1), and the equivalent of 1.00 g of platinum,
or spectrophotometer may be used, provided that it has that iseither 2.10 gofthe chloroplatinic acid (see B-3.3),
first been established that the results so obtained are or 2.49 g of the potassium chloroplatinate (see B-3.4),
identical with those obtained by visual comparison. in water in a2000-ml one-mark volumetric flask, add
200 ml of the hydrochloric acid solution (see B-3.2),
B-2 DEFINITION dilute tothe mark and mix. This solution has acolour of
500 Hazen colour units.
B-2.1 Hazen Colour Unit — The colour of asolution
containing 1 mg of platinum per litre in the form of B-5.2 Standard Hazen Matching Solution (Diluted
chloroplatinic acid, in the presence of 2 mg of cobalt Solution) — Into two series often 500-ml and fourteen
(II) chloride hexahydrate per litre. 250-ml one-mark volumetric flasks, place the volumes
of standard calorimetric solution (see B-5.1) shown in
B-3 CHEMICALS
Table 4, dilute to the mark and mix.
B-3.1 Cobalt (II) Chloride Hexahydrate
B-5.3 Storage
(COC12.6H20)
Store these solutions (see B-5.1 and B-5.2) in the dark
B-3.2 Hydrochloric Acid — approximately 1.19 g/
in stoppered glass bottles. Under these conditions the
ml. About 38 percent (mlnz) solution, or approximately
colour standard solution (see B-5.1) isstable for atleast
12N solution.
one year. The standard Hazen matching solution
B-3.3 ChloroplatinicAcid — Dissolve 1.00gplatinum (see B-5.2), although stable for atleast one month shall
in a sufficient quantity of aqua regia in a glass or preferably be prepared fresh.
porcelain dish by heating on aboiling water bath. When
the metal has dissolved, evaporate the solution to B-6 PROCEDURE
dryness. Add 4 ml of the hydrochloric acid solution
B-6.1 First check visually that the sample has colour
(B-3.2) and again evaporate to dryness. Repeat this
characteristics close to those of the standard Hazen
operation twice more. In this way 2.10 g of
matching solution (see B-5.2). If not, follow the
chloroplatinic acid (HqPtCIJ are obtained.
instructions given in B-7.2.
or
B-6.2 Pour into one of the calorimetric tubes
B-3.4 Potassium Chloroplatinate (KzPtCIJ (see B-4.1) aquantity of the sample sufficient to fill it
to the graduation mark. Similarly pour the standard
B-4 APPARATUS
Hazen matching solution (see B-5.2) which appears
B-4.1 Two Calorimetric ‘Ihbes, flat based ifpossible, tohave asimilar colour into the other tube tothe mark.
with agraduation mark atleast 100 mm above the base
B-6.3 Compare the colour of the sample with that of
and matched especially with respect to colour of glass
the standard, by looking down the tubes from top to
and height of graduation mark above the base. Suitable
bottom against a white background strongly
tubes are available commercially as 50 id or 100 ml
illuminated by daylight or by an electric ‘daylight’
Nessler cylinders.
lamp, taking care to avoid any side illumination.
For the measurement of low colorations (less than 50
B-6.4 Repeat, if necessary, with other standard Hazen
Hazen units), the height of the graduation mark above
matching solutions until the closest match is obtained.
the base must be greater than for the measurement of
deeper colours and must be sufficient that, on looking NOTES
through this greater depth of liquid, aclear distinction 1Instrumentsareavailablewhichpermitvisualcomparisonof
a liquid of a givendepth, with a movingtinted glass disc
between the standard Hazen matching solution can be
corresponding to the different standard Hazen matching
observed. solutions.Theuseof suchinstruments,whosestandardsare

5