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है”ह”ह

IS 2142 (1992): Bromine, technical [CHD 1: InorganicChemicals]

IS 2142:1992

*, a+ixi - m ( $mT @MJT )

Indian Standard

BROMINE, TECHNICAL - SPECIFICATION

( Second Revision )

UDC 661’46

@ BIS 1992

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

January 1992 Price Group 2

Acids, Alkalies and Halides Sectional Committee, CHD 02

.—

FOP. EWORD

This Irdian Standard ( Second Revision ) was adopted by the Bureau of Indian Standards, afterthe draft finalized by the Acids, Alkalies and Halides Sectional Committee had been approved bythe Chemical Division Council.

Bromine is used in the manufacture of ethylene dibromide for antiknock fluids and bromidesalts. It is also used in shrinkage-proof wool, as an intermediate for fumigants, as fire extinguisherfluid and military poison gas.

This standard was originally published in 1962 and subsequently revised in 1974 incorporatingrequirements for iodine content and sulphates alongwith their methods of test. In this revision,requirements for bromine and chlorine content have been modified keeping in line with theavailable manufacturing practices in the country. Also, the method of test for chlorine has beensuitably modified. The requirement for relative density has been deleted.

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. roundedoff in accordance with IS 2: 1960 ‘Rules for rounding off numerical values (revised)’. Thenumber of significant places retained in the rounded off value should be the same as that of thespecified value in this standard.

IS 2142 : 1992

Indian StandardBROMINE, TECHNICAL - SPECIFICATION

1 SCOPE

This standard prescribes requirements andmethods of sampling and test for bromine:technical.

2 REFERENCES

The Indian Standards listed below are necessaryadjuncts to this standard.

IS No. Title

264 : 19761070 : 1977

Nitric acid ( second revision )Water for general laboratoryuse ( second revision )

1260 Pictorial markings for handl-( Part 1 > : 1973 ing and labelling of goods:

Part 1 Dangerous goods(first revision )

4905 : 1968 Methods for random sampl-ing

5296 : 1979 Chloroform, pure and tech-nical (&St revision )

.3 REQUIREMENTS

3.1 Description

The material shall be in the form of reddish-brown fuming liquid.

-3.2 The material shall also comply with therequirements given in Table 1 when testedaccording to the methods given in Annex A.Reference to the relevant clauses of Annex A isgiven in co1 4 of the table.

4 PACKING AND MARKING

4.1 Packing

The material shall be packed in glass bottleswith lead caps or ground glass stoppered bottlessealed with an inert material. The bottles shallthen be packed in expanded mica, diatomaceous

‘silica or other inert absorbents. For largerpackings, homogeneously lead-lined mild steel

Table 1 Requirements forBromine, Technical

( Clause 3.2 )

SI Characteristic RequirementNo.

(0 (2) (3)i) Bromine, percent 98.5

by mass, Minii) Chlorine ( as Cl, ) 0.5

percent by mass,Max

iii) Non-volatile 0.05matter. percent bymass, Max

iv) Iodine ( as I ), per- O-05cent by mass, Max

Method of Test( Ref to Cl No.

in Annex A )(4)A-2

A-3

A-4

A-5

v) Sulphates ( as SO& ), 0.015 A-6percent by mass, Max

drums or monel metal drums conforming to+hp . . ..lP" mnAa hx. the. rrr\.,,at"m~ntLUG lL&lclJ Luaukd "J Cur u""v'llllurllL of In&i3

and in force shall be used.

4.2 Marking

The containers shall be securely closed and mar-ked with the following information :

. _I 1 . .a) Name ot tne materiai;b) Indication of the source of manufacture;c) Net mass; andd) Batch number or lot number in code or

otherwise.

4.2.1 The containers shall prominently displaythe words CORROSIVE HANDLE WITHCARE, and the appropriate caution label [seeIS 1260 ( Part 1 ) : 1973 1.

5 SAMPLING AND CRITERIA FORCONFORMITY

Representative samples of the material shall bedrawn and judged for conformity to the require-ments of this specification in accordance withthe procedure prescribed in Annex B.

IS 2142:1992

ANNEX A( C’iause 3.2 and Table 1 )

ANALYSIS OF BROMINE, TECHNICAL

A-1 QUALITY OF REAGENTS

A-ii ‘Cniess specified otherwise, pure &cmidS

- and distilled weter ( xee 1S 1070 : 1977 ) shall beemployed in tests.

NOTE — *pure chtimicaIs’ shal] mean chemicalsIkal do not cc,n:ain impurities which 2Kect th~results of analysis.

A-2 DETERMINATION OF BROMINE

A-2.1 ‘Method A ( Referee Method )

A-2.1.1 Reagents

A-2.1 .1.1 POIUYSiU.rniodide

A-2.1.1.2 Standard sodium thiosu{phate solution— 0’1 N. The solution shall be standardizedbefore use.

A-2.1.1.3 Starch indicator solution

Triturate 5 g of starch and 0“01 g of mercuriciodide with 30 ml of cold water and slowly pourit with stirring into one litre of boiling”w-ater.Boil for 3 mlrtutes. Allow the solution to cooland decant off the supernatant clear liquid.

A-2.1.2 Procedure

Dissolve about 10 g of potassium iodide in 30 mlof water and transfer the solution to a cleanlLO-ml volumetric flask. Weigh the flaskac~~~~ate]~. .~dd &QIJ~ fj”~ ~! of the mats.islU.,A. WA .$+.

to the flask, stopper immediately and weighagain. Di;ute the contents of the flask to 100ml acd mix well. Pipette out 25 ml of the solu-tion f~om the flask into a conical flask andtitrate with standard sodium thiosttjphate solu-tion using freshly prepared starch indicatorsolution. -

A-2.1.3 C’alczilation

Bromine, percent by

whereJ/ = Vol,lme in-. ”....,

mas~_ 31’97 VN—M

~.], of S?w?dd sdtixthiosulphate solution used in thetitration:

~ = no~malitJ’ of the standard sodiumth]osulphate solution; and

M = mass in g of the material taken for thetest.

A-2.1.3. 1 In the value cf bromine percentage asobtained in A-2.1.3, make a correction for thecbiorine present by subtracting the percentageresult for chlorine obtained in A-3.3 multipliedby 2.~5<

A-2.2 Method B ( Routine Method)

T~~e‘ur~mirl~~on[ent is Caicuiated by su-btractingthe sum of impurities from 100.

Bromine content, percent by mass =100–(XI +X2+X3+X*)

where

Xl = chlorine content, percent by mass ( $eeA-3,3 );

.%’z= rmrr-volatile matierj permit by mass( see A-4.2);

Xa = i~d~~ ~content, percent by mass ( see-.;

X4 = sulphates, percent by mass ( see A-6.3 )

NOTE —The limits of impurities for iodine andsulphates shall be taken at the maximum permissi-ble IeveIs, for example, iodine as 0.05 percent bymass arid Sttfp!tates as 0.015 p~i~~ill ‘uy-mass.

A-3 DETERMINATION OF CHLORINE

A-3.1 Reagents

A-3.1 1 Zinc Filings

A-3.1.2 Concentrated Nitric Acid — conformingto 1S 264:1976.

A-3.1.3 Standard Silver Nftrate So/tition —O.1 N.

A-3.1.4 Nitrobenzene

A-3.1.5 Stcndard Ammonium ThiocyancteSolution –O”l N.

A-3.1.6 Ferric Alum Indicator — saturatedSOltiiiOrs.

A-3.2 Procedure

Add 50 ml of water to a 250-ml volumetric flaskfitted with a stopper and weigh ( Ml ). To thisadd about 3 ml of liquid bromine and weighagain ( Mz ). The difference between Mz and Mlgives the exact amourit ( M ) of the materialtaken for the test. .Adrj about o’s g ofzi~~ dustand shake thoroughly for 10 minutes. Heat theflask on a steam-bath to remove the excess ofbromine. Dissolve the residue in 75 ml of waterand 25 ml of concentrated nitric acid. Heattiie ic~~lij~g soiution to boiiing on a water bathfor 5 minutes. Pass a gentle strrarn of air for 20minutes through a tapered in-let tube extendingto the bottom of the flask to completely removebromine. Allow the flask to cool and add 2Qml of standard silver nitrate solution. To thisadd 10 drops of nitrobenzene and shakevigorously for one minute. Titrate the excess

~

IS 2142:1992

si}ver nitrate with standard sodium thiocyanatesoiution using ferric aium indicator, shakingwell between successive additions of the titrant.Carry out a blank determination using the samequantities of all the reagents.

A-3.3 Calculation

Chlorine ( as Cl ), 3“546 ( VI—V, ) Nperter-. t by mass =

Mwhere

VI = volume, in m], of standard ammoniumthiocyanate solution used in theblank determination;

V2= volume, in ml, of standard amoniumthiocyanate solution used in testwith the material;

M = mass in g of the material taken for thetest.

A-4 DETERMINATION OF NON-VOLATILE MATTER

A-5.3 Procedure

Shake 1 ml of the material with 50 ml of waterand 3 g of zinc dust until all the bromine isdecolonized. Filter the contents into a Nesslercylinder. Add to the filtrate 1 ml of ferricchloride solution, 5 ml of chloroform andshake well. In another Nessler cylinder,take 1 ml of standard potassium iodidesohstion and to this add 50 ml of water, I ml offerric cidoride soi~tio~, 5 ~i Gf ch!orofor,m andshake thoroughly. Compare the colour of thecylinders.

A-5.3.1 The material shafl be taken as not hav-ing exceeded the limit prescribed in Table 1 ifthe intensity of pink or violet colour of thechloroform layer in the first cylinder is notdeeper than that of the colour of the chloroformlayer in the second cylinder. This e~iaur intefi-sity corresponds to 0’05 percent iodine in thesample.

A-6 TEST FOR SULPHATES

A-6.1 Apparatus

A-4.1 ProcedureA-6,1.1 Ness[er Cylinders – 50 ml capacity.

Transfer exactly 5 ml of the material to aA-6.2 Reagents

weighed silica dish. Volatilize the mattrial on a A-6.2. 1 Dilute Ammonium Hydroxide Solution —stezm-bath und?r hood and dry the dish for onehour at 105 * 5°C. Cool in a desiccator and

10 percent ( P/v ).

weigh again.

A.4, ~ cal~u]ation

N~~n-volatile m-after,i 00 ‘x M

percent by mass = ~ ~ ~

whereM = mass in g of the residue;

V = volume in ml of the material takenfor the test: and

D = relative density of the material.

A-5 TEST FOR IODINE

A-5.1 Apparatus

A-5.1.1 .~e~sler C.v//nders — 50 ml capacity.

A-5.2 Reagents

A-5.2.1 Zinc Dust

.4-!5.2.2 Ferric Chloride Solution — 10 percent(n:v).

Dissolve 10”0 g of ferric chioride in 100 ml ofw~tfr and filter.

A-6.2.2 Dilute Hydrochloric Actd — 1 N.

A-6.2.3 Barium Chloride Solution — A proxim-ately 10 percent m~v.

A-6.2.4 Standard SuIphate Solution

Dissolve 0.1814 g of potassium sulphate inwater and make up the voIums to 1 000 ml. Onemillilitre of the solution contains 0’1 mg ofsulphate ( as S01 ),

A-6.3 Procedure

Take l‘3 ml of the material in a 100-ml porce-lain evaporating dish with 30 ml of water. Addslowly 15 ml of dilute ammonium hydroxidesoluton and evaporate to dryness. Dissolv~ thewhite residue obtai]:ed in 80 ml of dilutehydrochloric acid. Take 40 ml of this solutionin a Ncssler cyli]:der and add 1 m! of bariumchloride solution; mix well and allow to standfor 1 hour. S;mil~r!y, in another Nessler cylinder,take 3 mi of standard srdphate solution, 40 mlof dilute hydrochloric acid and 1 ml of bariumchloride solution; mix and set aside for 1 hour.

A-5,2.3 Chloroform — see IS 5296: 1979. A-6.3.1 The materiai shall be taken as not hJv-

A.5.~.4 Standard pota~siujn Iodide So[utiofling exceeded the limit prescribed in Table 1 ifthe turb;dity produced with the material is not

Dissolv: 0“202 S g of pot:: ssium iodide in water greater th~n that produced with the stard~rdand diiute to ]00 ml in a voiumetrtic flask. One sample. This standard turbidity correspondsmillililre of this solution is equivalent to to 0’015 percent sulphate content in the0“001 55 g of icdine. material.

3

IS 2142:1992

ANNEX B(C/ause 5)

SAMPLING OF BROMINE, TECHNICAL

B-1 GENERAL REQUIREMENTS OFSAMPLING

B-1.1 In drawing samples, the followingpre~allti~il~ an d directions ~ha!l be observed.

B-1.2 Precautions shall be taken to protect thesamples, the material being sampled, the sampl-ing instrument and the containers for samplesfrom adventitious contamination.

B-1.3 Samples shall be placed in suitable, cleanand dry containers on which the material has noaction.

B-1.4 Sample containers shall be of such a sizethat they are almost completely filled with thesample.

B-1.5 Each sample container shaii be sealed air-tight after filling and marked with full details ofsampling and the date of sampling.

B-2 SCALE OF SAMPLING

B-2.1 Lot

AH containers in a single consignment of themate+ai drawn from a single hatch of manufac-ture shall constitute a lot. If a consignment isdeclared or known to consist of different batchesof manufacture, the containers belonging tothe same batch shall b: grouped together andeach such group shaii constitute a separate lot.

B-2.1.1 Samples shall be tested for each lot forascertaining the conformity of the material tothe requirements of the specification.

B-2.2 The number of containers ( n ) to beselected for sampling from the lot shall dependon the size of the lot ( N ) and shall bs inaccordance with Table 2.

B-2.3 These containers shall be selected at ran-dom from the lot and in order to ensure therandomness of sampling, rardom ssimplingproc~dures as given in 1S 4905 : 1968 may befollowed.

Table 2 Number of Containersto be Drawn for Sampling

( Clause B-22 )

Lot Size

(N)

(1)up to 1s16 ,, 2526 100 .

101 ;: 300301 ,, 500501 800801 ;: 1000

Number of Containersto be Selected

(n)(2)234568

10

It-3 TEST SAMPLES AND REFEREESAMPLE

B-3.1 Preparation of Test Samples

Take out not less than 50 ml of the material fromeach container selected for sampling, the totaivolume of the rnaterial collected from all thecontainers being not less than 500 ml. Thiscompcsite sample shall be divided into threeequal parts not less than 100 ml each, and eachpart shall be transferred to a clean dry amberglass bottle. The bottles shall be sealed air-tightand labelled with all the particulars of sampling.

B-3.2 One set of test samples shall be sent tothe purchaser and one to the supplier. Thethird set bearing the seal of the purchaser andthe supplier shall constitute the referee sample,to be used in case of dispute.

B-4 TEST

B-4.1 Tests for all the characteristics given inTable 1 shall be conducted on the compositesampie.

B-5 CRITERIA FOR CONFORMITY

B-5.1 The lot shall be declared as conformingto the specification if the test restdts on thecomposite sample meet the requirements givenin Table i.

4

Standard Msrg

The use of the Standard Mark is governed by the provisions of the Bureau of IndianSlarrdards A et, 19L?6and the Rules and Regulations made thereunder, The Standard Mark onproducts covered by an Indian Standard conveys the assurance that they have been producedto comply with the requirements of that standard under a well defined system of inspection,testing and quality control which is devised and supervised by BIS and operated by the pro-ducer. Standard marked products are also continuously checked by BIS for conformity tothat standard as a further safeguard. Details of conditions under which a Iicence for the useof the Standard Mark may be granted to manufacturers or producers may be obtained fromthe Bureau of Indian Standards.

.—

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BIS is a statutory institution established under the Bureau oflndian Standar& Act, /986 to promotoharmonious development of the activities of standardization , marking and quality Certification ofgoods and attending to corinected matters in the country.

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BIS has the copyright of ail its publications. No part of these publications may be reprochwed inany form without the prior permission in writing of BIS. This does not preclude the free Use: inthe course of implementing the standard, of necessary details, such as symbols and sizes, type orgrade designations. Enquiries relating to copyright be addressed to the Director ( Publication ), BIS.

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Indian Standards are reviewed periodically and revised, when neeessary and amendments, If any,are issued from time to time, Users of Indian Standar& should ascertain that they are in

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O.-....,...*”

to BIS giving the following reference :

DOC :No. CHD 02 ( 0016)

Amendments Issued Since Pablicatlort

.—

Amend No. Date of Issue Text Affected

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