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है”ह”ह

IS 15837 (2009): Anhydrous Diboron Trioxide [CHD 30:Nuclear Materials]

IS 15837 : 2009

'J-TTW"lJ 1fT;:rC/J

~I~~'!f ~ ~~ICfffI~'5 - ~

Indian Standard

ANHYDROUS DIBORON TRIOXIDE - SPECIFICATION

ICS 27. 120.1O;7 1.060J) I

© S IS 2009

B UREA U OF I NDIAN STANDARDSMANA K BH AVAN, 9 BA HA DUR SHA H ZA FAR MA RG

NEW DELHI 110002

lil ly 2009 Price G ro up 3

Nuc lear Matcri uls Sectional Co mmiuc e. CliO 30\ ..- r: ~ : :

f'( lREWORIJ

Th i-, Indian Standard was adopted by the Bu reau o f Indian Standards. a fter the draft finali zed by the N ucl earMatcrinl s Se ct ion al Cornmiucc had been approved by the C he m ica l Divi s io n Co unci l.

Boron co mpo unds arc used for controlling the rate of nuclea r reactions in the nu clear react ors and thus play

a \~r")' crucial role in reactor control. The material mu st therefore meet criteria like isotopi c compositi on,

impuriry conte n t.

There i~ no ISO Standard on the subject . Thi s sta ndard is formul ated based on the ind igen ous manufacturer s 'd ata/pract ice-, pre valent in the field in Indi a .

The compoxit ion o f the Committee respons ible fo r formul ati on of th is sta nd a rd is g iven in Anne x G .

For the purpose of deciding whether a particular requirement of this sta nda rd is complied with, the finalvalue obxcrvcd or ca lc ulated, expressing the result o f a test o r analysi s , sha ll be rounded o ff in accordancewith IS 2 : Jl)()() ' Ru les fo r round ing o ff numeri cal values (revised s> . The number o f s ig nifica n t pl aces

reta ined in the rounded off value sho uld be the sa me as th at of th e spec ified valu e in th is s tand ard .

IS 15837 : 2009

Indian Standard

ANHYDROUS DIBORON TRIOXIDE - SPECIFICATION

1 SCOPE 3 TERMINOLOGY

This standard prescribes the requirements and themethods of tests for Diboron Trioxide (13 :0,) used innuclear reactors,

For the purpose of this standard. the followingdefin itions shall apply.

2 REFERENCES

The standards listed below contain provis ions whichthrough reference in this text . constitute provisions ofthis standa rd. At the time of publication. the editionsindicated were valid . All standards are subject torevi sions and parties to agreements based on thisstandard arc encouraged to inve stigate the possibilityof applying the most recent editions of the standards

indicated below.

3.1 Nuclear Reactor - A de vice in which a selfsustaining nuclear fixs ion cha in reaction can hemaintained and controlled (fi ~sion reactor) .

3.2 Reactor Contrnl - The intentional variationsof the reaction rate in a nuclear reactor obtained byadjustment 01 reactivity to achieve or maintain adesired state of operation.

~ REQUIREMENTS

IS No. Tille 4.1 Description

The material sha ll he in the form of fine free flowingdry white powder, fre e from od our. dirt , foreignmatter and visible impurities .

~.2.1 The material shall conform to the isotopiccontent of natural boron that is lOB shall be19.9 ± 0.3 atom percent and II B shall be 80.I ± 0.3atom percent when tested in accordance with methodgiven in Annex A.

4.2.2 The material shall also conform to therequirements prescribed in Table I when tested inaccordance with methods referred in col 5 ofTable I.

and

Methods of sampling chemical andchemica l products :General requ irement sprecautions (first revision )

Sampling equipment. Se ction I For ~.2 Chemical RequirementssolidsMethod for atomic absorptionspectrophotometric determinationof sodium and potassiumMethod for determination ofmanganese by atomic absorptionspectrophotometryMethod of determination ofmagnesium by atomic absorptionspectrophotometryDetermination of iron by atomicabsorption spectrophotometry -Test method

Table 1 Requirements for Dlboron Trioxide

(Pan I) : ::!005

8883

(Pan 2/Sec I ) :!97X10614 : 1983

12046 : 1987

12491 1988

13320 : 1992

51 No. Characteristic Requirement Method or Test. Rer to

( I ) (3)

IS No.

(4)

Annex

(5)

i)

ii)

iii)

iv )

v)

vi)

vii)

viii)

ix)

Diboron Trioxide (as B,O,) percent by mass. Min

Chloride (as CI) percent by mass. Mux

Sodium (as No) percent by mass. Max

Iron (as Fe) percent by mass. Max

Calcium (as Cal percent by mass, Max

Magnesium (as Mg) percent by mass. Max

Heavy metals (as Pb) percent by mass . Max

Cobalt (as CO) percent by mass. Max

Manganese (as Mn) percent by mass. Max

99

0 .002

0 .003

0 ,005

0 .002

0.005

0 .002

0 .0005

0 .0006

IS 10614

IS 13320

IS 12491

IS 12046

B

C

D

E

F

IS 15837 : 2009

5 PACKING AND MARKIN(;

5.1 PackinK

Unless othe rwise agreed to between ihe purchaserand the supplier. the powder shall be packed insuitable containers such as HOPE bottles and sealedunder moisture proof condit ions .

5.2 MarkinK

5.2.1 The containers shall be securely closed andbear legibly and inde libly the following particulars:

a) Name of the material.

b) Minimum assay and maximum impurityconcentration.

c) Gross and net mass.

d) Date of manufacture and batch number. and

c) Naiuc of the manufacturer and his recognisedtrade-mark . if any .

5.2.2 IUS Cerrificution Marking

The product may also be marked with the StandardMark.

5.2.2.1 The usc of the Standard Mark is governedby the prov isions of Bureau of Indian Standards Act.19Xo and the Rule s and Regulations madethereunder. The details of conditions under whichthe licence for the use of the Standard Mark may be

granted to manufacturers or producers Illay beobtained from the Bureau of Indian Standards.

6 SAMPLING AND CRITERIA FORCONFORl\llTY

6.1 The sumples shall be collected according 10 themethod prescribed in IS XXX 3 (Part I ) and with thehelp of the equipment prescribed in IS XX X3 (Part 21Sec I).

6.2 Criteria for Conformity

6.2.1 Sampl ing plans to meet acceptance criteri aand inspection and measurement procedures thatdescribe the method of compliance with thisstandard shall be established by the seller andsubmitted to the buyer for approval.

6.2.2 Each sample taken shall be sufficient toperform the following in the event they are necessaryor desired by the buyer:

a) Quality verification tests by the seller.

b) Acceptance tests by the buyer,

c) Referee tests in the event these becomenecessary. and

d) Retention of archive samples by the seller.

6.3 Archive samples shall be retained by the sellerfor a period of time specified by the buyer anddelivered to the buyer upon request.

ANNEX A(Clause 4.2.1)

THERMAL IONIZATION MASS SPECTROMETRIC METHOD FOR TilEDETERMINATION OF THE ISOTOPIC CONTENT OF nORON

A-I APPARATUS

A-1.1 Thermal Ionization Mas..s Spectrometer

:\ -2 REAGENTS

A-2.1 Demlncralized Water

A-2.2 Sodium Carbonate

A-3 PROCEDURE

A-3.1 Dissolve 3.23 rug of B~O; in boron-freedemineralized water. Warm if necessary. Dilute to getit concentration of I ppm of boron. Two ml of thissolution (containing about 2 Ilg of B) is treated witha known amount of sodium carbonate to maintainatom ratio of B: Na equal to I : I . The treated sample

2

is evaporated under infra-red lamp to get sodiumtetraborate. The residue is redissolved indemineralized water and concentrated into a tinydrop. Using a capillary this drop is carefully loadedon a degassed rhenium/tantalum filament. Pass aboutO.IlA current through the filament to dry the sampleon the filament. Then momentarily increase thefilament current to about 1.6A to dull red heat. Theloaded filament is taken into the ion source of thethermal ionization mass spectrometer.

:\-3.2 After the pressure in the mass spectrometerbecomes less than 10'" rnb, the filament is electricallyheated slowly to about 0 .8 to 1.2A (700'C - 900 'C) .Thermal ionization of the sample results in theformation of Na.,BO,· ions and after optimising thefocusing and other analysis parameters, the Na,BO,­molecular ion s at m/z 88 and 89 corresponding t"o

IS 15837 : 2009

R ::: measured ato m rat io of J!lB/ I I B

lOB" and ! I B" are mass unalys ed by the magnetic'ana lyse r of the mass spect ro met e r, Th e ion inte ns itiesare mea sure d by a s uitable detec tor (Faraduy Cup orelec tro n mulriplier o r Dal y scintilluti ou detect or ).The rati o of the ion inte nsities g iv e-, the atom ratioof '''B/I 'B. From th is iso to pic compos iti on can becalc ula ted .

at percent of

at per cent of

III B ::: ---B.- x llJ()I+R

"13::: _1_ x (00I+R

A·4 CALCULATION

IlI BR=­li B

B-1 REAGENTS

:\'OTE - \\\' 11 Ira ll1l'l! pc r so un c l all' I l ' LlU I Il..' J It \( 111.1"

'Pl"\,: lll lJllL' lri ..: an .I IY ~ I' . ~' a " J I...c ru ninauon duriu!! 1111:1,.' uu rvc ..If an ;l!y"l . \ . i f ;111) shou ld 1,1." ;1 ~"' l' (I :J i ll t" d :tII J

app ro pfl J h." ,,:urrCI,:ltoli I";.h.:h )r ... d l.."'h,' r m llh.'J h~ '1II .1I ~ "I "

•.\olop h.: re rerc ncc m;l1l'r ia b. .

ANNEX B

lTable I, Sl No. (i) ITEST FOR PURITY OF 8 0: .\

8-2 PROCEDURE

B-1.1 Mannitol or Sorbitol - Neutral. The reagentshall satisfy the test given in B-1.1.1.

B-I.1.1 Five g of mann itol/sorb itol d issol ved in50 ml of carbondioxide free wat er shall require forneutral ization not more than 0.3 ml o f 0.02 Nsod ium hydroxide so lutio n using phenolphthaleinas ind icator .

8-1.2 Standard Sodium Hydroxide Solution - I N.

8-1.3 Phenolphthalein Indicator Solution

Dissolve 0.1 g of the phenolphthal ein in 60 ml ofrect ified spirit and dilute with water to 100 ml.

Weigh accurately about 2 g of the dri ed mat eri al anddissol ve it in abou t 120 ml of water by slight heatingif required . Add abo ut 15 g of mannitol or sorbi toland 0.4 1111 of phenolphthalein . Titrate with standa rdsodi um hydroxide so lution to a disti nct pink colou r.

8-3 CALCULATION

3AIlI x V8 ;01' percent by mass ::: M

where

\' ::: volume in ml of standard sodiumhydroxide solution used in the titr ation ,in ml, and

M = mass of the dried material taken fo r thetest , in g.

ANNEX C[Table 1, SI No. (ii)]

SPECTROPHOTOMETRIC DETERMINATION OF CHLORIDE IN DIBORON TRIOXIDE

C-I PRINCIPLE

A known weight of the sa mple is heated to I 100"Cin a current to s team. The hydrogen chloride formedis collec ted in the condensate, and the chloride isdetermined by spectro pho tometry after the addi tionof mercuric thiocyanate and ferric alum.

C-2 REAGENTS

C-2.I Double Distilled Water - Freshly distilledwater is used through out the experiment.

C-2.2 Ferric Alum Solution, 12 percent - Dissolve120 g of ferric alum sail in 430 ml of bo iling water.

3

Add with stirring 500 ml of hot nitric ac id . Gentlyheat the solution until complete di sso lut ion . Makethe solution to I 000 ml.

C-2.3 Mercuric Thiocyanate Solution, .. percent- Dissolve 4 g of recrystallized mercuric th iocyanatein 100 ml of ethyl alcohol.

C-3 PROCEDURE

A known weight of the sample in powder form is takenin a sili ca reacti on tub e and is heated to I lOOT . Aconstant current of steam is passed ove r the sa mplefor an hour at I 10<J'C. On pyrohydrolys is . hydrogen

IS ISlD7 : 2009

chloride is Io rmed which is then co llec ted a lon g withthe condensed stea m in a co llec tion tube . About S()­l)() III I o f the condensate is collected. This i, then

concentrated to about 20 1111. About 2 1111 each of ferr ic

a lum and mercuric thiocyanate arc added and the to ta lvo lume is made uptu 25 ni l. The solut ion is a llo we dto stand for 20 min and then ab sorbance is mea suredat -txo nm against a reagent blank,

Cons truc t a calibration pl ot between the kn owna mount of chlo ride a nd the absorbance by tak in g a

se ries o f s ta nda rd sa m ples containing kn o wnco nce ntra tion o f c h lori d e in th e ra ng e I to

100 ppmw. The con centration of c h lo ride ca n then

be read from the c al ib rati on pl ot .

1>-1 API'ARATl}S

I>-LI Platinum Dish

1>-2 REACENTS

1)-2.1 Methanol

D-2.2 Hydruchloric Add

D-2..1 Sulphuric Add

1)-2.~ Ammonia Solution

ANNEX DITahle I. Sl No. (v ) J

TEST FOR CALCIUM

dish . Add 5 drops of hydrochloric acid and evaporateto dryness . To the residue add 25 rnl of methanol and5 drops of hydrochloric acid and again evaporate todryness . Moi st th e residue with sulphuri c ac id andignite . Di ssol ve the residue in 50 ml o f water. add10 ml of anunonia -uuuuoniuru chl orid e bu ffersolution. 25 ml uf s tro ng ammon ia sol ut io n an d5 drops of sod iu m su lph ide solut ion . Tit rat e wit h

EDTA so lu tio n lbing meth yl th ym o l blue asind icator urui I the blue solution become co lou rlessor grey.

1>-2.5 Ammonia-Ammonium Chloride HufrerSolution

1>-2.6 Sodium Sulphide Solution

1>-2.7 F.DTA (lUll 1\1)

D-2.8 Meth)"1 Thymol Blue Indicator Solution

D-.' I)ROCEDURE

Weigh accura te ly about 5 g of the powdered sa mpleand dissolve it in 25 1111 of methanol in a platinum

The amount o f calcium present is calcu lated by th eform ul a as g ive n be low:

A xBCa. per ce n t by mass =-- x 0.1

1'-1

where

A vo lu me o f EDT A requ ired for titrati on . in011 ;

/J mass o f Ca equ ivalent 10 I ml of EDTAsolution, in mg: a nd

.\I = ma ss o f sa m ple taken for the test. in g .

E-I AI'PARATl'S

ANNEX ElTable I, 51 No.(viil]

TEST FOR HEAVY METALS

E-2.3 Standard Lead Solution

E-l.l Nessler Cylinders - 50 1111 cap acity a nd:\e s~krilcr.

E-1 REAG ENTS

E-2.1 Dilute Hydrochloric Acid - Approximatel yIN,

E-2.2 Hydrogen Sulphide Solution - Saturateda nd freshly prepared .

Di ssol ve 0 .1831 g of lead acetate [Pb(C~HP~)2"3HPl

in 100 ml of water a nd clear any cloudiness th a t

might appear w ith a few drops o f ac e tic ac id. D ilutethe so lu ti on to I 00 0 ml . Take 100 ml o f th is

solution and make it upto I 000 rnl . One m1 of thi sso lution co nta ins 0.01 mg of lead (as Pb).

E -3 PJ{OCEDU{E

Dissnl w I .()O() g of B:O , in 25 ml " I Ihll

deminerulizcd water, aJd n.S 1111 of d ihlled

hyd rochl oric ac id, he at to liO'C, transkr 10 a !':t'ssla

cy linder a nd add III 1111 o f hyd rogen sul ph id e

<ol uuon . M ake up the xolu tion tu 5011I1. Carry out :1

IS ISHJ7 : 21111'1

clln ll,,1 I,'s l IIs ing 2 111 1Ill' s l:m ,brd k :lol ~, "u lilln ;," d

th e ,a 111 " <j 1l ;lIlllly "I' rt'a ~t:III.' III lhe '/l In,' Illliil

\ o lun «, "f lh ,' re:I<.:l in ll m ixture . ( "lIll p:lre Ih,' ,'" In lll

III the s,\ IUli' 1I 1 ~ :illl'l l u m in . Inl l'n ~ll y II I the (Ilh 'u rp r\l, lu( l'd In Ihc' tt' sl so lu tio n shall he c u hc r l' '1u:d \I I

k" :" , 'd lllp;I, n J 1(\ I kll in th e cou u ol I" sl <oluuon .

:\~:\EX F17;")lt' I. SI.\'o. ( \ i l i) 1

()ETI':J{'11;\:\T10~ OF COBALT I!': I>lBOI{()~ TRIOXIDE

BY ATO:\lIC . \ B SO J{ PTlO~ SPECTI{():\lETRY

F-I PRINCIPLE

-\ kno wn amount of B .O I.' dl , ,, )1\ ,'d III

de ru iucru lizc d water, Th « ,:al l(\nl,' i mp uri uc :lnc!

bo ro n arc xcp nrutcd l' mplo ) in g a st ro ng ;lcid cali"n

exchange resi n. Cohal l hl'lJ u p 1111 Ih\' col umn is

eluted ill d ilute HCl . c'onl'\'lllr;Il,'d an d introducedin to acet yl ene-ai r /I ;II I1C' a nd the in tvuvi ty of l i ne al

2-W.7 111 11 (t llTes po nding t" c'ohail is meas ured .

1"-2 :\ 1'1':\ RYITS

F-2 .1 .-\ to m k Ahxurptiun Spectrometer

F-J I{EA(;r~NTS

F-3.1 A Strong Cation Exchange Rcsin (1-1 - Form)

1"-3.2 Double Distilled Watcr

F-4 PROCEDURE

W~i gh o ut a kn own a m o u nt o f 8,0, ( 100 mg ) and

d issolv e in demineral ized water. Wa rm if necess ary.

Se t u p a strong aci d c a tio n exchange re sin(A mber ti tc IR -l~() or cqu ivulent) 8-10('01 long and

5

o.S 10 I em d i.une tc r an d co nd itio n \\ nh d ilutc 11<'1.Tra ux tc r Ihe di ' Sllhed mel: Oil 10 the cu hunn ;lIl d

\\ ;I, h the t'I \IUlIlIl w ith di xti llcd wate r. Horou dUl es

dm\ n . W:I,h the colu mn with m iniu unn IWo bed

vol ume s. Re ject the w ;ls h in g s . Wash lll e CO I U IIl II

with abou t I() ml of 3 M lI el a nd c o llec t thewashi np ill a fresh via l. It s ho u ld he m ent ion ed th at

the vol umes o f elu ant » give n abov e is oulv

ind ica tiv e a nd il may he ne ce ssary to opri misc theelution Sll'pS during the ion e xchange se para tio n

p ro cedure . Evaporat e th e wash ings c o lle c ted an dd issol ve in d is till ed wa ter ,

Setup the at omi c a bsorp rio n s pe c trome te r sys te m.

Introduce the soluti on in to the a ir -acetyl e ne fla me

and m e asure th e in te ns ity o f a bsorp ti on sig na l a t

240 .711111.

Prepare a se ri e s of so lu tio ns conta inin g known

amounts of cobalt in I to Ino I-tg/ml range . Cunstruc i

a calibration pl ot by a na ly s ing a ll the s ta nda rd

solutions . Pl ot the intensity agai n!> t the a mount o f

cobalt presen t in the standard solution . The amount

of cobalt in sa mp le so lut io n can he read from the

calibration pl ot . This ca n then he converted intoconcentration ,

IS 15M37 2009

ANNEX G(Foreword)

CO:\'tMITfEE COMPOSITION

Nuclear Mater ials Sec tio nal Com mittee , CHD 30

Bh ahna Atom ic Rcs eurcl. Centre (Radioc hemistry &

Isot o pe Group ), Mumbai

Atu nuc Energy Regul atory Board , Murnb ui

Bhu bha A to mic Research Centr e ( Env i ro nmen t Division).

Mumhai

Hharut Heav y Elc ctricals Limi ted. Hyd cru bad

£I "ard of Rad iat ion ..nd Isotope Tech nolo gy (BRIT ).

Ne", De lhi

Defen ce L abora tory , Jodhpu r

Dep artment of Atomic Energy. Nu clear Fuel Complex .

HyderabadIndian Rare Earths LId. Mum bai

Indira Gandhi Ce ntre lor Ar onu c Research . Ka lpakkam

Mad ras A to mic Powe r Sta tion . Kalpakkam

~li l1lS lry of Defe nce (ln vtitute of Nuclear Medicine and

Allied Sciences) . DelhiMinht r} of Defence (DGQA), Pun e

Minis try o f Environment and Fores ts. New Delhi

Nuclcur Power Corporation Ind ia Ltd. Tarapur Atomic

Power Stati on. Mumbai

Nuclear Power Corpora tion of India Ltd. Mumba i

Rajasth an Atomi c Pow er Station, Raja sthan

Sah a institu te of Nucl ea r Phys ics. Ko lka ta

Shr irnm Institut e of Industr ial Research . De lhi

Ta ta Inst itute of Fund ament a l Resea rch . Mu mbaiTat a Memorial Ce ntre. Mu mbai

Uranium Corporat ion of India Ltd. Jharkhand

Vikram Sarahhai Space Research Ce ntre. Th iruvan anth apuramBIS Directora te Ge nera l

DR V. VU' VGOP." . (Cha irma n ;DR K. L. R.·\M.\ Kt:S1 ·\ R (AIIU 'Ila lc)

SHR ' S . P. A('ARWALDR (SM") G. G. Pxxnn:

SURI K. NATARAlAN

DR N. C. GOOMER

SIIRt S. G. VAIJ"PVRKA RDR PRADEEP NARAYAN (Alternate s

DR R. N . MI!RTH Y

SHRI Y. BALAlI RAO (A l temate)

SIlR' V. K. VERMASURI A . K. DAS (Alt crnates

REI'IlLSENfATIVE

DR K. S. KRISH" ,\ RAQ• DR RAV! KASHYAP

DR A" UPAM MO~D,\L iA lternatei

SHRI KUKP!LLAISllRI P. G. DATE (Alte rna te;

DR S. MAUDGALDR Y. P. KAKAR (A lterna te)

SIlRI U. RAMAMURTIlY

SIIRI S. BIlATTACIl·\ RJEE iAlternatei

SIlR I H. D. SHARMA

SIIRI R. Y. SINGH (A l le male)

SIlR' P. K. PALS HRI S. L. SAI NI (A lfemme)

PilOF SUDEU BHATTACHARYA

PROF SUSANTA LAHIR! (A llemale)

DR A. K. VERMA

SHill SANJAY RAJPUT (A IICOWle)

PROF H. C. JAIN

RfI'llESENrATIVE

SHRI S. SIDDIC"UEREPRE-,r.'TATI VE

DR U. C. SRIVASTAVA. Scientist ' F" & Head (C HD)[Represent ing Director Gener al (Ex- officioll

Member Secr etaryDR KANCHAN ANA:<D

Scient ist T (C HD). SI S

6

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Th ix Indi an Standard has been dev eloped from Doc No.: CHD 30 (14 29) .

Amendments Iss ued Since Publication

Amend No.

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