Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of 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.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 11995 (1987): Isoproturon, WP [FAD 1: Pesticides andPesticides Residue Analysis]

Gr3

IS : 11995 - 1987

Indian StandardSPECIFICATION FORISOPROTURON WP

(Firsf Reprint APRIL 19(6)

Dnc 632.954 ISOP

(0 (~()pyrig"l t 987

1.1 (] R .: A l1 0 ... I N D I A N S TAN n A R I) SMANAK BHAVAN, Q BAJIADUR SIIAII ZAFAR MARG

NEW I)EIJII 110002

October 1987

IS s 11995 • 1987

Indian StandardSPECIFICATION FORISOPROTURON WP

Pest Control Sectional Committee, AFCDC 6

Chairman

DR R. L. RAJAK

Repr6s,nl;ng

Directorate of Plant Protection, Quarantine &Storage (Ministry of Agriculture & RuralDevelopment ), Faridabad

Committee,

M,mb6TS

DR P. K. AGGARWAl. IDMA Laboratories, ChandigarhSHItI ACHJN'l' CHAUDHRY ( Alternau )

DR H. L. HAMI Pesticides Residue Analysis SectionalAFDC 56, BIS

On. B. HANEltJEP: 'rea Research Association, Jorhatn« G. S-"'.rYANARAYANA ( Alternat« I )Snnr S. C. DA8 ( Alternat« I I )

Dn. S. R. BAUOOAH

SBRI O. K. BllATNAOAR

Pesticides Formulators Association of India ( SS I ),Bombay

Agriculture Department, Government of UttarPradesh, Lucknow

SnRY RAM NARAIN SINGH ( All,rnale)SaRI N. S. BIlUHE Shriram Institute for Industrial Research, Delhi

SHRI R. K. BAKERJEE ( AllmuJl. )SURI D. CHATTERJEE Agriculture Department, Government of West

Bengal, CalcuttaAtul Products Limited, AtulSHaI M. V. DESAI

SaRI A. R. DESAI ( Allmaal,)SaRI G. D. GOKHALE Bombay Chemicals Private Limited, Bombay

SHRt P. M.JADHAV ( Alternate)SHRI B. K. VIJAYA GOPAL Agromore Limited, Bangalore

SURI S. K. RAMAN ( Alt,rnDtt )DR R. C. GUPTA Central Insecticides Laboratory, Directorate of Plant

Protect ion, Quarantine & Storage ( Ministry ofAgriculture & Rural Development ), Faridabad

SUR I S. K. GHOSH (Allernal, I )SSRI R. S. SHAnKA ( Altemat« II )

DB. S. S. GUPTE Bayer ( India) Limited, BombayDR R. N.JUKAB ( Alumat» )

DR V. N. IYER Coromandel Indag Products India (P) Limited,Madras

DB M. O. ALIAS ( Alurnat« )

( Contimud on pa"~ 2 )

(G) C.,-""h, 1987BUREAU OF INDIAN STANDARDS

This publication is protected under the I"Jitua Copyright Act (XIV of 1957 ) andreproductioD in whole or in part by any means except with written permission of thepublisher shall be deemed to be an infringement of copyright under the aa.id Act.

IS : 11995 • 1987

( ContinUld from paR' 1 )

C.S.A. University of Agriculture & Technology,Kanpur

National Institute of Occupational Health ( ICMR ),Ahmadabad

Department of Agriculture, Government ofKarnataka, Bangalore

Agriculture Department, Government of Punjab,Chandigarh

National Organic Chemical Industries Limited,Bombay

Central Food Technological Research Institute( CSIR ), Mysore

SURI M. P. SHAH ( Alternat« )Ds KENCUAIAH

DR S. K. KASRYAP

Memb,rs ReprlsenliRg

SURf N. L. KALRA National Institute of Communicable Diseases, DelhiSHRI G. C. JOSHI ( Alurnau i

DR R. L. KALHA Punjab Agricultural University, LudhianaDR R. P. CnA\VLA ( Alternate)

DR KALYAN SINGH

DRJ. S. VERMA ( Alel,rnale )SHRt S. K. r..1AJUMDAR

SURI J A8\V ANT SINGH KHOKHAR

Snru S. G. Knl811NAN

Ranis India Limited, Bombay

In personal capacity (296, SFS Gulmohar Enelaue,New Delhi 110049 )

National Malaria Eradication Programme, Delhi

SHRI N. MUTRU ( Alternate )SnRI B. P. S. MAN'N Pesticides Association of India, New Delhi

DR B. S. SUETTY ( Alternate I )S~RI T. V. JAOADISAN ( Alternat« II )

Snnr K. S. MEHTA Bharat Pulverising Mills Private Limited, BombaySunl S. Cj{.\TT~RJEE ( .Alt"nat, )

On. A. L. MOOKltRJEE Cynamid India Limited, BombayOn, A. P. SHINTRE (Allernal, )

DR S. K. MUKERJI

SHRI NAWAD SINOHCu KRISIIN A R AO ( Alternat« )

SURI Y. A. PRAJ>HANSun] M. L. SHAH ( AltertUlt,)

On. P. S. RAMANATHAN Gharda Chemicals Private Limited, ThaneDR A. M. M ALTE ( Alternal, I )SHRI D. G. UDA8 ( Alt"."atl II )

DB N. K. Roy Agricultural Chemicals Division, Indian Agricultu-ral Research Institute ( leAR ), New Delhi

Gujarat Insecticides Limited, AnkleshwarSHRI H. V. RUPARELDRJ. K. ASTlE ( Alternal,)

SURI P. K. RAO Mini'try of Defence ( DGI )SHRI P. N. AOARWAL ( Alt,rnat, )

SECRETARY ( CIB & RC ) Central Insecticides Cell, Directorate of Plant Pro-tection, Quarantine & Storage (Ministry ofAgriculture & Rural Development ), Faridabad

SHRt V. C. BUAROAVA ( ,AllmuJt' I )DR SHA:NTI SARUP ( Alumau II )

DRK. D. SHARMA Directorate General of Technical Development,New Delhi

SRRI N. R. NARAYANAN ( Altl1nat,)SURI V. C. SBAlfJlA Department of Agriculture, Government of

Rajasthan, jaipurDR K. N. SURIV.'a8TAVA Shaw Wallace Company Limited, Calcutta

SURI R. N. ROYCHOWDBUBY ( Alurnat« )

( ContinUla DIIpa"~ 12 )

2

AMENDMENT NO. 1 JULY 1994TO

IS 11995: 1987 SPECIFICATION FORISOPROTURON EC

(Page 5, Table 1 ):

a) Sf NiJ. (ii), col 2}) I

- Delete the words 'after accelerated storage'.b) SI No. (iii J co 2

( Page 5, Table 1, col 4, Heading) - Substitute 'Appendix of IS 12004 :1987' for 'Appendix of This Standard'.

( Page 6, clause 4.1 ) - Substitute the following for the existing:

'When freshly manufactured material in bulk quantity is offered for inspection,representative samples of the material sball be drawn and tested IS prescribed inIS 10627 : 1983 within 90 days of its manufacture. Wben tbe material is offeredfor inspection after 90 days of its manufacture, sampling shall be done 8S

prescribed in IS 10627 : 1983. However, the criteria for conformity of thematerial when tested, shall be the limits of tolerances, as applicable over tbedeclared nominal value and given under clause Z.4.1 of the standard. t

( Page 6, Appendix A ) - Delete,

(FAt> 1 )Reprograpby Unit, BIS.New Delhi, India

AMENDMENT NO. 2 MARCH 2002TO

IS 11995: 1987 SPECIFICATION FOR ISOPROTURON WP(AII,elld",elll No. I, Title] - Substitute 'Wp' for 'Ee·.

( FAD 1 )Reprography Unit. 81S. New Delhi, India

AMENDMENT NO. 3 MAY 2002TO

IS 11995: 1987 SPECIFICATION FOR ISOPROTURONWP

[ Page 4, clause 2.2 including Note] - Delete.

(FAD 1)Reprography Unit. BIS. NewDe~ India

IS I 11995 • 1987

Indian StandardSPECIFICATION FORISOPROTURON WP

o. FO RE W OR D

0.1 This Indian Standard was adopted by the Bureau of IndianStandards on 30 April 1987, after the draft finalized by the Pest ControlSectional Committee had been approved by the Agricultural and FoodProducts Division Council and the Chemical Division Council.

0.2 Isoproturon WP is used in the control of weeds in agriculturalcrops.

0.3 Isoproturon WP is generally manufactured .to contain 50 percent or75 percent ( mlm ) of isoproturon.

0.4 In the preparation of this standard, due consideration has beengiven to the provisions of the Insecticides Act, 1968 and the Rules framedthereunder. However, this standard is subject to the restrictions imposedunder the Act and Rules, wherever applicable.

0.5 For the purpose of deciding whether a particular requirement ofthis standard is complied with, the final value, observed or calculated,expressing the result of a test Or analysis, shall be rounded off inaccordance with IS: 2-1960·. The number of significant placesretained in the rounded off value should be the same as that of thespecified value in this standard.

1. SCOPE

1.1 This standard prescribes the requirements and the method. ofsampling and test for isoproturon WP.

2. REQ,UlREMENTS

2.1 De8criptioD - The material shall be in the form of a homogenouspowder, off-white in colour and shall wet readily on mixing with waterproviding a suspension suitable for use as a spray.

-RuIn (or roundiDI off Dum~rical values ( rlPis,d).

3

IS I 11995 • 1987

2.2 IdeDtity Test - Extract about 1 g of the sample in about 50 mlmethanol. Centrifuge for about 5 minutes. Decant the clear super­natant liquid into a beaker. Add 250 to 300 ml of water to precipitatethe isoproturon. Filter, wash thoroughly with water and dry at 100°C.Melting point of dry residue shall be between 154 and 156°C, and shallnot be depressed by the addition of pure isoproturon. Further, IRspectrum of the residue taken in potassium bromide should be superim­posable on the IR spectrum of the reference sample of isoproturonbetween 2·5 and 15 p.

NOTB- Identity test need Dot be carried out if isoproturon content is determinedby HPLC method ( $16 A-I ).

2.3 Isoproturon, technical employed in the formulation of this materialshall conform to IS : 12004-1987·.

Tolerance Limit, Percent

+ 10 I± ~ l of the nominal

I value+ 5 I

3 J50 and above

Above 9 and below 50

2.4 The material shall alia comply with the requirements given in Table 1.

2.4.1 Isoproturon Content - When determined by the method prescribedin Appendix A, the observed isoproturon content percent ( mlm) of anyof the sample shall not differ from the declared nominal value by morethan the tolerance limit given below:

Nominal Value, PercentUp to 9

2.4.1.1 The actual value of isoproturon content in the material shallbe calculated to the second decimal place and then rounded off to thefirst decimal place before applying the tolerances given in 2.4.1.

2.4.1.2 The average content of all the samples taken shall Dot beless than the declared nominal content.

3. PACKING AND MARKING

3.1 Pacldag - The material shall be packed according to the require­ment given in IS : 8190 (Part 1 )-19801".

3.2 Markl•• - The container shall bear legibly and indelibly thefollowing information and any other information- as is necessary underthe lruteticides Act, 1968 and Rules framed thereunder:

a) Name of the material;b) Name of the manufacturer or trade-mark;

.Specification for ilOproturon. technical.tJlequirementi for packiDl of pelticidea: Part I Solid pesticid.) (fir,' r,.triM ).

4

IS : 11915 • 1'87

c) Date of manufacture and date of expiry;d) Batch number;e) Isoproturon content, percent ( mlm );f) Net mass of the contents; and

g) Cautionary notice as worded in Insecticides Act, 1968 and Rulesframed thereunder.

TABLE 1 REQUIREMENTS FOR ISOPROTURON WP( Clause 2.4 )

SLNo.

CHARACTERISTIC REQUIREMENT ~{ETlIOD 0 .. TEST,

REF TOr----- --.A-- ~

Appendix CI No. ofof this IS : 6940-

Standard 1982*

] 1.1

(5)(4)

A

70'0 11.2

8~)'O 11.2

120 11.4-

0'10 11.5

0-20 11.3

(3)

Nominal value asdeclared on thecontainer ( see 2.4.1 )

98-0

(1) (2)

i) Isoproturon content, percentby mass

ii) Sievin~ requirement, materialpassmg through 75-micronIS Sieve, after acceleratedstorage, percent by mass,Min ( see Note 1 )

iii) Suspensihility , after accelera­ted storage ( see Note 2 ),percent by mass, Min:

a) (or 50 percent WP

b) for 75 percent WP

iv) Wettability, in seconds, Mtlx

v) Acidity ( as }-i,SO& L percentby mass, AJax

or

Alkalinity (as NaOH ), per­cent by mass, A1a...:

NOTE I - IS : 4tiO ( Part 1 ) -1985 "Specificat ion for test sieves: Part 1 Wire clothtest sieves (third revision ), BS Test Sieve 200, AST~1 'fest Sieve 200, Tyler TestSieve 200, have their aperture within the limits specified for the above IS '1 est sieveand rnay, therefore, be used as 75- micron IS si eve.

NOTE 2 - The rnaterial shall not be subjected to accelcrat ed storage t reat mont if:t has crossed half of irs shelf-life as ascertained from its date of manufacture andexpiry date given on the container.

-Methods of test for pesticides and their f~£'mulations (first revision ).

5

18 I 11995 • 1987

3.3 DIS Certification Marking

The product may also be marked with Standard Mark.

3 3 1 The use of the Standard Mark is governed by the provisions ofBu·re~u of Indian Standards Act, 1986 and tbe Rules and Regulations madethereunder. The details of conditions under which tbe licence for the US~ ofStandard Mark may be granted to manufacturers or producers may be obtainedfrom the Bureau of Indian Standards.

4. SAMPLING

4.1 Representative samples of the material shall be drawn as prescribedin IS : 10627-1983*.

5. TESTS

5.1 For suspensibility test, start .with O·5 percent of concentration afteraccelerated storage at 54 ± 1°C for 24 h as described in 11.2 of IS :6940-1982t. Transfer 25 ml portion of suspension and sediment in areaction flask. Wash the cylinder thrice with 100 ml of methanol.Proceed to determine active ingredient as described in Appendix A.

5.2 Q,uaJity of Reagents - Unless specified otherwise, pure chemicalsand distilled water ( see IS : 1070-1977: ) shall be employed in the tests.

NOTE - 'Pure chemicals' shall mean chemicals that do not contain impuritieswhich affect the result of analysis.

APPENDIX A[ Table 1, Item (i) ]

DETERMINATION OF ISOPROTURON CONTENT

A-8.GENERAL

A-O.I For the determination of isoproturon content, two methods,namely, HPI~C ( see A-I) and basic hydrolysis method (see A-2 ) havebeen prescribed. HPLC method will be the referee method in case ofdispute.

• Methods for sampling of pesticidal formulations.tMethods of test for pesticides and their formulations (first rlvisitm ).:Specification for water for general laboratory use ( s,cond r,vision ).

6

IS I 11995 - It87

A-I. HPLC METHOD

A-I.I Principle - A HPLC unit with a UV detector is used for thedetermination. Using a solution containing known amounts of thestandard isoproturon and the internal standard, the response factor,RF, for isoproturon in the internal standard is arrived at. A solutioncontaining the internal standard and active ingredient extracted quanti­tatively from a known mass of the sample (under test) is injected sub­sequently into the HPLC unit. The percentage of isoproturon in thesample is then computed by the standard relationship.

A-l.2 Apparata.

A-I.2.1 High performance liquid chromatograph equipped with aprinter-plotter-cum integrator and l.JV: detector. The suggestive HPLCoperating conditions are given below. However, these operating condi­tions are likely to change with change in the HPLC equipment employedand are allowed, provided standardization is done:

Column Silica 10 I-'m25 em X 4-6 rom ( S.S )

Solvent system 1) Cyclohexane 90 percent ( v/' )2) Isopropanol 10 percent ( fJjv )

Detector UV ( at 254 nm )Solvent flow rate 1·5 ml/rninChart speed 0·2 em/minSample size 10 ",1

A-l.2.2 Filtration Assembly - with G-4 sintered crucible.

A-l.3 Reagent.

A-1.3.1 Internal Standard - Acetanilide, AR or equivalent grade.

A-l.3.2 Cyclohexane - Spectroscopic grade.

A-l.3.3 Isopropanol - Spectroscopic grade_

A-l.3.4 Isoproturon - of known purity.

A-I.4 Preparation orStandard. and Calibration

A-l.4.1 Weigh accurately 0-25 g of acetanilide into a lOO-ml volumetricflask and make up to volume using the cyclohexane-isopropariol mixture( 90 : 10 v/l). This will give a solution containing 2-5 mg/ml of theinternal standard.

A-l.f.2 Weigh 0"5 g of standard isoproturon into a lOO-ml volumetricflask and. dissolve it in ]0 ml isopropanol. Make up to volume using

7

II I 11995 - 1987

the cyclohexane, This will give a stock solution containing 5 mg/mlof the standard isoproturon. Pipette out 5 ml of this standard solutioninto a 50-ml volumetric flask. Then pipette out 5 ml of the internalstandard solution into the same flask. Mix well. Make up to the markusing the solvent mixture. Call this Solution A.

A-l.5 Procedure

A-l.5.1 Weigh into a beaker with a glass rod, an amount of the testsample which will contain about O·5 g of the active ingredient. Addabout 10 ml of isopropanol and stir well for a few minutes. Warm thebeaker to facilitate dissolution of the active ingredient. Filter carefullythrough a G-4 crucible and collect the filtrate ill a conical flask. Washthe residue repeatedly with small quantities of cyclohexane, stirwell and add these fractions to the G-4 crucible. Finally transfer theresidue to the crucible and continue to wash with cyclohexane. Collectall the filtrate in the conical flask. Then quantitatively transfer it toa 100 ... nil volumetric flask and make up to volume with cyclohexane.Pipette out 5 ml of this final solution (containing the active ingredientextracted (rom the test sample) into a 50-ml volumetric flask.Pipette out 5 ml of internal standard solution ( see A-l.4.1 ) into the sameflask. Mix well and make up to the mark using the solvent mixture.Call this Solution B.

A-].5.2 Introduce 10 JAI of the Solution A and Solution B into theHPLC unit. From the integrator, print out and note down the peak areasof the isoproturon and acetanilide peaks in both the cases. Adjust theattenuation in such a way that the isoproturon and acetanilide peaksare obtained within the scale in both the cases. (This attenuation maychange from equipment to equipment ). Compute the percentage ofisoproturon content in the sample as given in A-l.6.

A-l.6 Calculation.

Isoproturon content,percent by mass

m1 X A2 X P X A3

A1 X "'2 X A4

where

m1 === mass of standard isoproturon in solution Ai

A2 = area of the isoproturon peak in solution B;P = percentage purity of standard Isoproturon;As ::.:'I area of internal standard peak in solution A;Ai = area of the standard isoproturon peak in solution A;m2 =: mass of the isoproturon sample taken for analysis; andAt :::I area of internal standard peak in solution B.

8

IS I 11995 - 1987

A-I.7 PrecisioD - Data obtained by this method indicate standarddeviation of 0·7 and 0'6 for isoproturon at 50 percent and 75 percentlevel in the test samples respectively.

A·2. BASIC HYDROLYSIS METHOD

A-2.1 Principle

A-2.1.1 Isoproturon in the sample is hydrolyzed using potassiumhydroxide in aqueous diethylene glycol ( I: 1 by volume ). DimethyJa­mine, the volatile product of hydrolysis, is distilled off and absorbed instandard hydrochloric acid. From the quantity of hydrochloric acidconsumed by dimethylamine, the percentage of isoproturon present inthe original sample is computed.

A-2.2 Appanta.

A-2.2.1 An all glass distillation assembly of suitable type. A suggestiveassembly is shown in Fig. 1. Minor changes in the suggestive assemblymay be made to improve its suitability.

A-2.3 ReaReDt.

A-2.3.1 Hydrochloric Acid Solution - 0·2 N.

A-2.3.2 Sodium Hydroxide Solution - 0'2 N.

A-2.3.3 Diethylene Glycol

A-2.3.4 Potassium HydrDxide Solution - 35 percent aqueous.

A-2.3.5 Silicon Defoamer

A-2.4 Procedure

A-2.4.1 Accurately weigh an amount of the sample which will containabout 1·0 g of the active ingredient and transfer it quantitatively to a cleandry 500-ml reaction flask of the hydrolysis-cum-distillation apparatus.Add 50 ml of diethylene glycol and one or two boiling chips. One ml ofsilicon defoamer may be added to check foaming. Attach the reactionflask to the other parts of the assembly as shown in Fig. I: 50 ml ofhydrochloric acid is taken in a beaker in which the delivery tube anddips as shown in Fig. I. Add 50 ml of 35 percent potassium hydroxidesolution to the flask through a dropping funnel. Close the stopcock ofthe dropping funnel as soon as the addition of alkali ia complete. Heatthe contents of the reaction flask to boiling. Continue the distillationup to about 2i hours. The distillation can be stopped when the contentsof the flask become orange brown in colour. The distillate will cease tobe alkaline by that time. This can further be confirmed using a multi­range pH paper to test the distillate. The pH of the distillate, as

9

IS I 11995 • 1181

300

1-

18/7 BALL- SOCKET

19 mm 00 VIGREAUXCOLUMN WRAPPED WITHASBESTOS TAPE

250ml GRADUATEDCVLINDER

GAS DISPERSIONTUBE. COARSEFRITlED GLASSV

35/20 BALL-SOCKET

ELECTRIC HEATING MANTLE J

220 WATTS,RHEOSTAT-CONTROLLED

All dimeDiioDi in millimetres.

Flo. 1 APPARATUs POR DETERMINATION OF IIOPROTURONCONTENT ( ALK.ALINE HYDIlOLYSIS MBTHOD )

10

IS I 11995 • 1987

indicated by the colour of the pH paper, must be 7. Take care todisconnect the inverted funnel from the lower end of the condenserbefore switching off the heating source. If this is not done, the distillatewill be sucked back into the distilling flask, when it starts cooling down,after the removal of the heating source. If however, arrangements canbe made to maintain a flow of nitrogen gas through the distillationassembly, then the back suction problem will not be experienced. Rinsethe funnel and the connecting tube with distilled water and add therinsings to the receiver beaker. Titrate the contents of the beaker with0·2 N sodium hydroxide solution using phenolphthalein as indicator.At the end point, the colourless solution will turn pink.

A-2.5 Calculations

Isoproturon content, [ ( Vl

X Nl

) - ( V2 X N 2 )] X 20'6percent by mass == - - -- .-M - -"-- -.

where

Vl === volume, in rnl, of standard hydrochloric acid used;N1 = normality of the hydrochloric acid used;V2 = volume, in ml, of sodium hydroxide required to

neutralize; the excess of acid when the sample isanalyzed;

N2 = normality of sodium hydroxide used for titration; andM =-: mass, in g, of the sample taken for the test.

11

18 I 11995 • 1987

( C.IiIIIIM ftom 1M" 2 )

MnnlJ"s lUpr,s.,UlISURJ}. L. SJPABIJIALAlfI CMA Laboratories, Bombay

SHRI A. H. KARA.OBI ( .Alima.'. )Da R. SOIlAN Sudarshan Chemical Industria Limited, Pun.

SKaIK.RATBI(A~u)Da R. V. Vmra:.A.TABATNAIl Regional Research Laboratory (CSIR ), Hyderabad

Da NAOABH118HAN RAO ( AlImuJI,)SBBI T. PuBNANANDAII, Director General, BIS ( Ex-ojiQo Mlm1Jn)

Director ( Agri &: Food )

Sur"Il':?SUBI LAJINDER SINOH

Joint Director ( Agri & Food ), BIS

12

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