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 12004 (1987): Isoproturon Technical [FAD 1: Pesticidesand Pesticides Residue Analysis]

REAFFIRMED

--.~

Gr 3

Indian StandardSPECIFICATION FOR

ISOPROTURON TECHNICAL

FiJlt Reprint AUGUST 1997

( l.corporaliDI AlDeDdmeDI No.1)

UDe 632.954 ISO

C Copyri,ht 1997

BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARO

NEW DBLHI 110002

18 I 1200f • 1987

Indian StandardSPECIFICATION FOR

ISOPROTURON TECHNICAL

Pest Control Sectional Committee, AFCDC 6

CluJi,.."DB R. L. RA.J~J[

RIp",,,,,i,,,Directorate of Plant Protection, (tuaraatiae at

Storale (Ministry of Alriculture It RuralDevelopment ), 'aridabad

SURl O. K. BRATlfAOAR

S8RI S. K. GHOSH ("41',,ntll, I )SRRI R. S. SHARMA ( J41t,rnal, II )

D. S. S. GonE Bayer ( India) Limited, BombayDR R. N.Jt7K.lB ( A11""Qlt )

DR V. N. IYEI\ Coromandel Indag Products India (P) Limited.MadraJi

SURI M. V. D!:"8AISaRI A. R. DESAI ( A11,mal, )

SaRI G. D. GOJCHAL'. Bombay Chemicals Private Limited, Bomba)'8MBJ P. M.JADHAV ( AI'ma.',)

SBRJ B. K. VIJAYA GOPAL Agromore Limited, BangaloreSURI S. K. R~HAN ( Al"rntll, )

DB R. C. GVltTA Central Insecticides Laboratory••Directorate ofPJan&Protection, Qparantine & Storage ( Ministry ofAgriculture & Rural Development ). Faridabad

Pesticides Formulators AlSociation of India ( 58I ),Bombay

Agriculture Department, Govemmtnt of UttarPradesh, Lucknow

SaRI RAM NABAIH S)NOH ( ~ll"ntl" )SUBI N. S. BIBD1B Shriram Institute for Industrial Research, Delbi

SRRJ R. K. BAlORJEB ( Al'""al, )SHBI D. CHAT'lBRJEE Agriculture Department, Government of West

Bengal, CalcuttaAtul Products Limited, Atul

M,.71b",DB P. K. AOGA'RW.4L IDMA Laboratorie., Chandilarh

SSRI ACIIIN·r CHAUDHRY ( AII"u" )DBH. L. BAllI Pesticides Residue Analysis Stctional. Committee"

AFDC56. DISDR B. BANBRJER "rea Research AsaociatioD, Jorhat

DB G. SATYANARAY£NA ( All,""", I )SR81 S. C. DAB ( Allmlal, II )

Da S. R. BAKOOAH

DR M. O. ALlAH ( Alt""tll, )

( C,,,,inuld on /HJ" 2 )

@ C••yri,1I1 1988

BUREAU OF INDIAN SrANDARDS

This publication is protecteel under the l"diG" C.pyriRlat .4e' (XIV of 1957 ) andreproductioD in whole or in part by any means excepr with wriuen permission of thepublisher shall be deemed to be an infrinlement oC copyright under the said Act.

IS : 12004 • 1987

( c:.,.,inrud/r,,,. ,." 1 )

MIttIHr, &1"'1"".'SRal N. L. KALKA NatioDlllustitute of Communicable Diseas~I, Delhi

SRR1 G. C. JOSBI ( Alt"".', )DBR. L. KALKA. Punjab Agricultural University, Ludhiana

Da R. P. CHAWLA ( AI",,",,,)DR KALYAK 8150B C. S. A. Univenity of Agriculture &, Technology,

KanpurDB S. K. KA8BYAP National Institute of Occupational Health ( leMR ),

Abmadabad

Central Food Technological Research Imtitute( CSIR ), MYlore

Department of Agriculture. Government ofKamataka, Bang.lore

Alriculture Department. Government of Punjab,Chandilarh

National Organic Chemical Industries Limited,Bombay

DB]. S. VBRMA ( ~I'",.." )SBRI S. K. MAJUMDAR

SimI H. V. R.UJtARBLDB J. K. ASTlE ( ~1'''1IG1' )

S..I P. K. RAO Ministry or Defence ( DGI )SRBI P. N. AOARWAL ( All",..',)

S.OBBTARY ( CIS &. RC ) Central IDiecticidea Cell, Directorate of PI.at Pro-tection, Quarantine at Starale (Miniatry orAgriculture at Rural Development ), r.rid_bad

SIUtI V. C. BHARGAVA ( AI,,,,,.,, I )DR SSA.TI SAaup ( J.lt""." II )

DR K. D. SBARII~ Directorate General of Technical Developmeat,New Delhi

SHKI N. R. NARAYANAN (AI"".",,)SRBI V• C. SHARMA Department of Ap-iculture. Government of

R.ajasthan, JaiRurDB K. N. SBRIV.4ITAVA Shaw Wallace Company Limited, Calcutta

SS.I R. N. ROY-OROWDRURY ( AI,,,,,,,,, )

SHRt M. P. SHAH ( All"." )DR KZlfOBAIAB

5B.1JASWANT SmaB KRO)[B~B

SBBI S. G. KRISHNAN

SBBI N. MtTTRU ( Al'",",I, )SDBI B. P. S. MANN Pesticide. Association of India, New Delhi

DB B. S. SHICTTY ( AI,,,,..,, I )SRBI T. V.JAGADIIA!f (All""'" II )

SBBI K. S. MBBTA Dharat Pulverising Mills Private Limited, BombaySHltl S. CHATTBBJI:B ( AI'muJI,)

Da A. L. MOOXBRJBE Oynamid India Limited, BombayDB A. P. SSIN'l'RB (AI,,,,,,,,,)

DB S. K. MUKBRJI I" /JIrs.ul ltJ/J4tity, Prof or Eminence ( Retd ) IARI,New Delhi

SBBI NAWAB SINOR National Malaria Eradication Prop-amme, DelhiOR KRISHNA RAO ( Alt"".,,)

SR81 Y. A. PRADBAK Ralli.lndia Limited, BombaySERI M. L. SRAB ( AI,,,,,.,,)

DB P. S. RAIiAlfATKAN Gharda Chemicals Private Limited, ThaneDB A. M. MALTB ( AI'''tUJI, I )SRIlI D. G. UDAl ( AII,,,.." II )

Da N. K. Roy Agricultural Chemicals DivilioD. Indian Apicul-tura1 Research IDititute ( leAR ), New D.lhi

Gujarat Insecticidd Limited, Ankleshwar

( C".,illU14 .. ,." 12 )

2

AMENDMENT NO. 2 MAY 2002TO

IS 12004 : 1987 SPECIFICATION FOR ISOpaOTURONTECHNICAL

( FAD I ) RepropaphyUnit. 81S, New Delhi. IDdiI

IS : 12004· 1987

Indian StandardSPECIFICATION FOR

ISOPROTURON TECHNICAL

o. FO RE W OR D

0.1 This Indian Standard was adopted by the Bureau of IndianStandards on 28 May 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.

Mol'eultlr MfJ,J1

206'29Structural Formula

0.2 Isoproturon, technical is used for making formulations meant for weeccontrol in agricultural crops.

0.3 Iscproturen is the accepted common name by the InternationalOrganisation for Standardization ( ISO) for N, N-dimethy)-N-4-isopropyl­phenyl urea. The empirical and structural formulae, and molecularmasl are as given below:

Empirical FormulaCllH l l NIO

I.f In the preparation of this standard, due consideration has been givento the provisions of the Insleticidu Act, 1968, and Rules framed there­under. 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" in accor­dance with IS : 2-1960*. The number of significant places retained inthe rounded otT value should be the same as that of the specified valuein this standard.

eRul•• for roundiq otT numerical values ( "lIi,,4 ).

3

IS I 12004· 1987

I. SCOPE

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

2. REQ,UIREMENTS

2.1 De.crlptloa - The material shall be in the form of white togreyish white or yellowish crystalline powder free from extraneous impu­rities or hard lumps,

2.2 Ide.tlty Te.t - Extract about I g of the sample in about 50 m1methanol. Centrifuge for about 5 minutes. Decant the dear superna­tent 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 154·156°C and shall notbe depressed by the addition of pure isoproturon, Further IR spectrumof the residue taken in potassium bromide should be superimposable onthe IR spectrum or the reference sample of isoproturon between 2-5and 15,,-

NOTB - Identity test need not be carried out if isoproturon eonteat i. dettrmiDedby UV spectrophotometric method ( st, A·l ) Or HPLC method (", A-2 ).

2.3 The material shall also comply with the requirements specified inTable 1.

TABLE 1 REQUIREMENTS FOR ISOPROTURON TECHNICAL

SL CHARACTERISTIC REQUJBEIIEJi'l' METHOD 01' TEST,No_ RBI' TO

r--......_._~-_._~Appendix CI No. ofof this IS : 6940-Standard 1982-

(I) (2) (3) (4) (5)

i) IlOproturon content, percent by 95-0 AmalS, Mill

ii) Water content, percent by mau, 0·5Ma

iii) Melting point, °0 152-1~8 6

iv) Acidity ( as H.80.), percent by 0-1 II-Small, MtUI.r

v) Alkalinity (AI NaOH), percent 0-4 11-3by mau, M••

-Methods of test for pesticides and their Cormulations (firs' "nsiD1I ).

4

II I 12004 • 1187

3. PACKING AND MARKING

3.1 Packial - The material shall be packed according to therequirements given in IS : 8190 ( Part 1 )-1980·.

3.2 MarkiDI - The container shall bear legibly and indelibly thefollowing information and any other information as is necessary under the1""cticitUs Act and Rules:

a) Name of the material;b) Name of the manufacturer or trade-mark;c) Batch number;d) Date of manufacture;

e) Isoproturon content, percent ( mlm );f) Net mass of the contents; and

I) The cautionary notice as worded in the InsI&ti'idts Ad and Rules.

3.2.1 The container may also be marked with the Standard Mark.

Non: - The use of the Standard Mark is governed by the provisions of the Bureauor Indian Standards Act 1986 and the Rules and RelUlations made thereunder. TheStandard Mark on products covered by an Indian Standard conveys the .aurancethat they have been produced to comply with the requirements of that Itandardblader a weI' defined system or inspection, testins and quality control which i. devisedand supervised by DIS aad operated by the producer. Standard marked produetlare .)10 eontIDuOU8I~ cheeked by BIS tor conformity to that standard as • Curther..Ceguard. Details of conditions under which a licence for the we of the StandardMark may be Jrtanted to manutacturer. or producers may be obtained from theBureau of Indian Standards.

4. SAMPLING

4.1 Representative lampIes of material shall be drawn as prescribed in18 : l0946-1984t.

5. TESTS

5.1 Telts shall be carried out al referred to in col 4 and 5 of Table 1.

5.2 (lallllt, or a_leat. - Unless specified otherwise. pure chemicalsand distilled water ( ", IS : 1070-1977: ) shall be employed in rests,

No.,. - 'Pure chemical.' shall mean chemicals that do Dot contain impuritieswhich a«eet the resultsot analysis.

-R.equirements Cor packing of pesticides: Part I Solid pesticide. (firs' ""ilion ).tMethod••raamplinl for technicalsrade pesticides.$8pecificatioD for water for seneral laboratory use ( II,ond ",is;'. ).

IS I 12004 • 1987

APPENDIX A[ Table 1, Item (i) ]

DETERMINATION OF ISOPROTURON CONTENTS

A-I.GENERAL

A-O.l For the determination of Isoproturon content, three methodsnamely. UV spectrophotometric method (see A·l), HI'LC method( se« A-2) and basic hydrolysis method ( sel A-3 ) havt been specified.UV spectrophotometric method and HPLC method shall be the refereemethod in case of dispute.

A-I. UV SPECTROPHOTOMETRIC METHOD

A-I.I PriDciple - The absorbance of a methanolic solution of technicalmateria) is measured against the solvent at 242 nm, The isoproturoncontent of the sample is then computed .making use of the absorbancevalue of a solution of standard isoproturon.

: A-l.2 Apparatu8

A-l.2.1 Ultraviolet Speclrophotometl'

A-l.2.2 -Q,uar/~ Cetl» - Matched pair with path length equal to 1'000 em.

A-I.2.3 Volum,tric Flasks - 250-ml, 200-ml and lOO-ml capacity.

A-l.2.4 Pipettes - 10-ml and S-ml capacity ( graduated ).

1..-1.3 RealeDt.

A-l.3.1 Methanol - Spectroscopic grade.

NOTE - The absorbance ( '-000 em cell) of methanol should not. in any case,exceed 0'150 at 240 om. The spectral absorbance curve should be smooth throughoutthe 210·300 nm range and should not show any extraneous impurity peaks.

A-I.t Procedure

1..-1.4.1 Weigh out accurately about 150 mg of the standard isoproturonmaterial into a dry 250-ml flask, dissolve and dilute to volume withmethanol. Pipette out 10 ml of this solution into a IOO-mt flask anddilute to volume with methanol. Pipette out 10 ml of this solution intoa third flask of lOO-ml capacity and dilute to volume. This final solutionis taken for absorbance measurement. Weigh out accurately about150 mg of the isoproturon, technical sample to be analyzed, into a dry250-ml flask and proceed exactly as suggested above for the standardpreparation.

A-l.4.2 SptttrophOlorn,tric D,'"mi"(Jlion - Measure the absorbance ofthe standard as well as sample solutions described under A-I.4.1 at 242 omusing the 1-000 em cuvette and methanol as blank.

6

IS I 120M • 1987

A-l.5 Calculatio.e

m1 X As x PIsoproturon content, percent by mass - ---~----

Al X m2

whereml :.:.: mass in mg of the standard taken,As == absorbance of the sample,P = percentage purity of standard isoproturon,Al -= absorbance of the standard isoproturon, andma =-= mass in mg of the sample taken.

A·2. HPLC METHOD

A-2.1 Prlaeiple - A HPLC unit with a UV detector is used for tltisassay. Using a solution containing known amounts of the standardisoproturon sample and the internal standard, the response factor, RF,for isoproturon in the internal approach is arrived at. A solution con­taining a known mass of the isoproturon sample and internal standard isinjected subsequently into the HPLC unit. The percentage of isoprortu­ron in the sample is then computed by the standard relationship.

A-2.2 Apparata.

A-2.2.1 High performance liquid chromatograph equipped with aprinter-plotter-cem-integrator and UV Detector. The suggestive HPLCoperating conditions are given below. However, these operating condi­tions are likely to change with change in HPLC equipment employedand are allowed provided standardization is done:

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

Solvent system a) Cyclohexane 90 percent ( vlv )b) Isopropanol 10 percent ( vlv )

Detector UV ( at 254 nm )Solvent flow rate 1-5 mJ/minChart speed 0-2 em/minSample size 10 1£1

.&-2.2.2 Volum,"ie Flask - 50-ml and lOO-ml capacity.

A-2.2.3 Pip,tteJ ( gradullted) - 2-ml, 5-ml and lO·ml capacity.

A-2.3 Realeat.

A-2.3.1 Internal Standard - acetanilide, A.R. or equivalent grade.

A-2.3.2 CJcloMxa", -- spectroscopic grade.7

II I 120M at 1987

A-2.3.3 lsoproptmol- spectroscopic grade.

A-2.3.4 ]soproluroft - of know~ purity.

A·2.~ Prep.ratlo. 01 t.e St••da..d aad SaIDpie Solutio••

A-2.4.1 Weigh out accurately 0'25 g of acetanilide into a IOO-mlvolumetric flask and make up to volume using the cyclohexane-isopro­panol mixture ( 90 : 10, vlv). This will give a solution containing 2·5 mgtml of the internal standard.

A·2.f.2 Weigh out 0-5 g of standard isoproturon into a IOO-mlvolumetric flask and dissolve it in '25 ml isopropanol. Make up to volumeusing the cyclohexane. This will give a stock solution containing 5 mglml of the standard isoproturon, Pipette out 5 ml of this standardsolution into a 50-ml volumetric flask. Then pipette out 5 ml of theinternal standard solution into the same flask. Mix well. Make up tothe mark uljng the solvent mixture. Call this, solution A. Weigh out0-5 g of the lsoproturon sample and proceed exactly as in the case of thestandard sample. Call this, solution B.

A-2.5 Proceclure

A-2.5.1 Introduce 10 "I of the ,olution A and solution B into the HPLCunit. From the integrator print out and note down the peak areas ofthe isoproturon and acetanilide peaks in both the cases. Adjust the·attenuation in such a way that the isoproturon and acetanilide peaks areobtained within the scale in both the cases, (This attenuation maychange from equipment to equipment). Compute the percentage oriloproturon content in the sample as indicated in A-2.6,

A-2.6 Calealatlo••

"'1 X A2 X P X AaIsoproturon content, percent by mass - At X m, X A.

where

ml = mals of standard insoproturon in solution Aj

AI = area of isoproturon peak in solulion B;P = percentage purity of standard Isoproturon;

Aa == area of internal standard peak in solution A.Al = area of standard isoproturon peak in solution Ajrnl = mass of the iscproruron sample in s·DlutiDn B;At - area of internal standard peak in solution B.

t

A-2.7 Precl.loD - Data obtained by this method indicate a standarddeviation of 0·5 tor Isoproturon at 96 percent level.

8

IS I 120M • 1917

A-3. BASIC HYDROLYSIS METHOD

A-3.1 PrlDelple - Isoproturon is hydrolysed using potassium hydroxidein aqueous diethylene glycol ( 1 : 1 by volume). Dimethylamine, thevolatile product of hydrolysis, is distilled off and absorbed in standardhydrochloric acid. From the quantity of acid consumed by dimethy­lamine, the percentage of isoproturon present in the original sample ilcomputed,

A·3.2 Apparat••

A-3.2.1 An all glass disstillation assembly of a suitable type. Asuggestive assembly is shown in Fig. 1.

A-3.3 RealeatsA-3.3.1 Hydrochloric Acid Solution - 0'2 N.A-S.S.2 Sodium H,droxitU S.lution - 0-2 N.A-3.:J.3 Potassium H,droxid, Solution - 35 percent aqueous.

A-3.3.t Di,thylt,,' GLJcolA-I.3.5 Silieon Difoamer

A-3.4 ProcedureA-3.4.1 Accurately weigh 1'0 ± 0'1 g of the lsoproturon, technical

sample and transfer it quantitatively to a clean dry reaction flask of thehydrolysis-cum-distillation apparatus. Add 50-ml of diethylene glycoland one or two boiling chips. One ml of silicon defoamer may be addedto check foaming. Attach the reaction flask to the other parts of theassembly as shown in Fig. 1. 50 ml of hydrochloric acid is taken in abeaker in which the delivery tube end dips as shown in Fig. 1. Add50 ml of potassium hydroxide solution to the flask through a droppingfunnel. Close the stop-cock of the dropping funnel as soon 81 theaddition of alkali i. complete. Heat the contents of the reaction flask toboiling. Continue the distillation up to about 21 hours. The distillationcan be stopped when the contents of the flask become orange brown incolour. The distillate will cease to be alkaline by that time. This canfurther be confirmed using a multi-range pH paper to test the distillate.The pH of the distillate, as indicated by the colour of the pH paper,must be 7. Take care to disconnect the delivery tube from the lowerend of the condenser before switching off the heating source. If this isnot done, the distillate will be sucked back into the distilling flaask, whenit Itarta cooling dOWD, after the removal of the heating source. If, how­ever, arrangements can be made to maintain a flow or nitrogen gasthrough the distillation assembly, then the back suction problem will notbe experienced. Rinse the connecting tube with distilled water and addthe rinsings to the receiver beaker. Titrate the contents of the beakerwith 0-2 N sodium hydroxide solution using phenolphthalein as indicator.At the end point. colourless solution will turn pink.

9

ELECTRIC HEATING MANTLE,220 WATTS, RHEOSTAT-CONTROLLED

GAS DISPERSIONTU8E,COARSEFRllTED GLAS

35120 BALL-SOCKET

19mm 00 VIGREAUXCOLUMN WRAPPED WITHASBESTOS TAPE

300

All dimensions in millimetre••

Flo. 1 ApPARATU. 'OR DBTBRYINATJON OP I,oPROTURONCONTBNT ( ALKAUNB HYDROLYSIS MBTiJOD)

10

IS I 120M • 1117

.4.5 Calealatlo••

IlOproturoD content,percent by mass ==

where

Yl = volume in ml of hydrochloric acid originaUy taken inthe receiver beaker,

NI =- normality of the hydrochloric acid,VI = volume in ml of sodium hydroxide consumed in the

titration,NI == normality of sodium hydroxide, andM = ma.1 in g of the sample taken Cor analysil.

11

( c:.u..d" .. ,.,. 2 )

M"g", Ill"" • .,SBBIJ. L. SI.ABIIIALAKJ CMA Laboratorie., Bombay

5BBI A. H. KABABOBI ( ~lImI", )Da R. SoM.ur Sudanban Chemical Industries Limited, PUDe

S"I K. RATBI (AI""..,,)D. R. V. V"K~TA.A'rKAli Re,iooal R...reb Laboratory ( CSIR ), Hyder.bad

Da NAQA.BUIJI~ a.o (All"".,,)S..I T. h ••AKAIIDAM, DirftCtor GeneraJ, BIS (&-oliN M",*,)

Director ( AFi It Food )s",,~

SBBI LA.TDfD" SUIOKJOIDt Director ( Asri It Food ), HIS

BUREAU OF INDIAN STANDARDS

323 7817 .337••803843

236 23 1&832 92 85

T~ams : ManakMnetta(Common to III ottIce.)

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