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है”ह”ह

IS 2962 (1964): Methods of Sampling and Test for Kattha[FAD 8: Food Additives]

IS t 2962- 1964

( Reafftrmed 1998

Gr 3

Indian StandardMETHODS OF SAMPLING AND

TEST FOR KATTHAFourth Reprint MARCH 1998

( Incorporatin. AmMtdmf"nt No. I )

e Copyright 1979D IJ REA U 0 FIN D I A N S TAN DAR D SMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARO

NEW DELHI 110002January J96S

xxxx2009

1I.2M2-IIM

Indian StandardMETHODS OF SAMPLING AND

TEST FOR KATTHA

KAITHA, Vqetable Tan. and Allied Products SectionalCommittee, CDC S6

CMnIa~".I 8. N. SAft.'

.."...,."Ministry or Delence (R • D )

AI"SIIIlI C. S. AuK The IncUu Wood Produca Co Ltd, Dareill)-SR.' Aa.n•• CHA.....A." The National Tannery Co., Ltd., CalcuttaOft S. K. BARAI' Ceatral Leather Research IDititute ( CSIR). Madr..

n. R. S....aAMoAli ( AI",.,.)Oa D. GaOl. Central~ Laboratory, CalcuttaSHill R. K. D.OOPrA The Britith India CorPoradoD Ltd (Cooper Allen

8ranch&r~DR A. ItAMKAII Munki~ doll of DelhiSII_' NAMD K.811011 The QWalMw Forelt ProcIucIi Lad.,ShlvpwlSHIU J. P. PAUL I..lab Private Ltd • Bomba,

OR S. M. K.u1 ( AIImMU)S••I P. S. IlAMAOIIAJmRAlI IndiaD_.c:oaumttee, New DeIhla..llA.lWAlfIV. Director ot Health SenIceI. ChaadiprbDR P. R. SulKA onandN.turaI 0.CorDIa"" Deli,. DuD

DR. M. It. lJrDu ( AI",." )Da R. S. S..y"ftAYA ow.e- otHealda ServiceI, LucbowD" Y. K. SU.""••AIIW:All Central CoaunIttee for rood StaDdarcII. New DeUaiS.... I VAlArrLAL HAaJDA8 Shri Laxml a..icaI a IndUltria Private Ltd.,

Bombay; aIChemIc:aIa and AUIed ProcIuetI BapariPromot.IoD Councu. Calcutta

5... A. KA......A" RAG ( AI-..)n. 8A~At., DlrectGr. lSI (~ AI.... )~ Diredor ( Qan)

t· '

,.,.""

DR O. M. SAXIIIIAAIIItcaDt DireeIor (a.a ). lSI

S••I N. R. h ....A8AJfa.~ ,Alllltaal DIrector ( CbaD), 181

(~.,.,,2)

B II REA U 0 F ) N D I A N S TAN DAR D SMANAKBHAVAN, 9 BAHADUR SHAH ZAFAR MARO

NBW DELHI 110002

1S.2ICi2-11M

(C""'.,I/r-~ I )KA7THA Subcommittee, CDC 36 : I

e.-wDa A. K.unf.ur

AI...,S..I C. S. ALA. The Indian Wood Produett Co Ltd J hreW'ISOl BalllAlI DAD M"~A Kattba DeaIert'~dOD, DeIhl

5KIU GI.DRA.. LAL ( AI,.".." )SUN KB1...A aoJ-AL LA80'r1 Bhartl7a Ka'tba VyavuaJk Scv. San_b.K~rS••I Soa.. CaA.DIU. WB&n U. P. Kauha MaDufacturen' AlIOCialaon, Najibabad

SOIIblt1PmrDRA KUllA.RU1)JU.u ( dl,.".." )

2

.. ;

CONTENTS

O. FOREWORDJ. Scor-e2. SAMPI.INO3. Ql'ALITY OF R2AGP:NTS4. PREPARED SAMPLE5. TEST FOR 51'ARCH6. Loss ON DRYINO7. CATECHIN8. COLD WATER EXTRACTIVES •••9. MATTER INSOLUBLE IN RECTlFIBD SPOUT

10. WATER INSOLUOr.E SOUDS AT 37°:1:2°011. BoiLING WATER INSOLUBLE SOLIDS •••12. TOTAL ASH13. ASII INIOLl'BLE IN HYDROCHLORIC ACID

.,

IS I 2962-1964

PAOE

455777889

1010II1112

IS I 2962 .1964

Indian StandardMETHODS OF SAMPLING AND

TEST FOR KATTHA

o. 'F 0 R E W 0 R D0.1 Thia Indian Standard was adopted by the Indian StandardsInstitution on 23 October 1964, after the draft finalized by the KATTHA.Vegetable Tans and Allied Products Sectional Committee had beenapproved by the Chemical Division Council.

0.2 KATTHA is obtained by crystallization from the extract of theheartwood .of ACadd etlJ«. Willd fame Legurninose called KHIJIR inHindi. The manufacture of KATTHA is carried out in India on bethsmall and large scale. "ATTHA js one of the principal ingredientsused in the preparation of PAN (betel leaves) for chewing purposes;in combination with lime, it gives the characteristic red colourationon chewing. KATTHA is regarded as an astringent; cooling and digestive;useful in relaxed conditions of the throat, mouth and gums; and also'in cough and diarrhoea. Externally, it is employed as an astringentand as a cooling application to ulcers. boils and eruptions on theskin. KATTHA. also enters into a number of ..I,"n',d;c and Unanimedicinal preparations. .

0.3 Accepted methods for analysis of KATTH.4 are not available inliterature. The Sectional Committee responsible for the preparationof this standard, therefore, referred to whatever varying. or even conflict-ing, paper. had been published on the subject; in that connection, thepublication tA note on the analysis of cutch and the preparation of purecatechin' [ lniiQN Forester MIIMirS, Vol It Part It ( 1908) 1by Puran Singhwas found valuable. The Committee has formulated these methods of teston the basis of the 'accumulated experience of various Public Analystsin this country as well as actual analyses made by a group of collaboratinglaboratories, namely, The Public Analyst, Delhi; The Public Analyst.Uttar Pradesh; The Public Analyst, Punjab; Italab Private Ltd.,Bombay; The Indian Wood Products Co. Ltd., Bareilly; and The GwaliorForest Products Ltd., Shivpuri. The co-operation received is gratefullyacknowJedged.

0:.3.1 In this standard. catechin determination (s" 7 ) is carried out byextraction with • mixed organic solvent. The Committee consideredit desirable to .preseribe a melting point teit for the purity of theisolated catechin but found that adequate, data are not available. TheCommittee hal initiated steps for the collection of this information.

18,2162.1_

0.4 For ~t1de size, Indian Standard -Sieves conforming to IS: 460-1962·are prescribed. Where IS Sieve. are not available, other equivalentstandard sieves a. judged by aperture size may be tiled.

0.5 In reportins the result or a telt or analyaia made in accordancewith this ltand8rd. if the final value, observed or calculated, i. to berounded off. it shall be done in accordance with IS: 2- 196Ot.

1. SCOPE

1.1 This atandard lay. down the method, or sampling and test forKATTH_4.

2. SAMPLING

2.1 OeDerat Requlre•••t. of Sampllas

2.1.0 In d~winJ' preparing, storin, and handlinglample•• the followinlprecautions and direction. shall beobserved.

2.1.1 Samples shall not be taken in a place espoled to dampnell and ininsanitary conditions.

2.1.2 Precaution. shall be taken to protect the ma~1 beibS aampled,-the samples, the sampling instrument and the containen for samples fromadventitious contamination. particularly from ablorption of wate'r. .

2.1.3 The .mpl~ .h.II be placed in suitable, clean. dry and air-tightgl... or other suitable containen on which &be material has no action.

2.1.4 .FAI&ch .mpJe container .hall be ...Ied air-tilht with • suitableItopper after filIiDi. and marked with lUll particulan of the material andthe date of aampJing. .

2.1.5 Samples .han be stored in a cool and dry place.

2.2 Scal. olSampllaa

2.2.1 lAl-The material offered Ibr inspection at oae time lhall consti-tute a loL

2.2.1.1 Samples shall be tested fo.r each lor tor ucertaininr conbmityof the material to the requirements of the relevant materiallpeciftcation.

2.2.2 The number (,,) of packages to bechosen rrom • lot shall dependon the number of packages in the Jot (X) and ah.U bein accordance withTable 1.

~clfiQtioa for teat IiewI ( ........... ).tRuJttI tor round"'. oIrnumerical YUUIt (~ ).

~

IS a2962-1964

TABU: I NUMBER or PACKAGES TO DI SELECTED FOR SAMPLINGia•• 2.2.2)

Xo. or PACX40a So. 0 .. PAMCAOXSIN ~JfX JDr TO B'& CHO.P;~

A- ~(1) (2)

S to 15 S16 .. 40 4-41 It 65 ~()#i " 110 7Over 110 10

2.2.3 These packages shall be chosen at random from the lor. To en-sure the randomness or selection, a random number table as agreed tobetween the purchaser and the supplier shan be used. In case such atable Is not available. the following procedure shall be adopted:

Arrange all the packagea in the lot in a systematic manner andstarting from any package. count them as 1J 2, 3, etc up to ,and 10 on, where' is equal to the integral part of the value of XI".Every rth container thus counted shall be separated until the requisitenumber of packages is obtained to give the samples for test.

2.3 Preparadoa of Samplea

2.3.1 Draw representative portions of the material from different partsof each ~.ge selected for sampHng, 10 as to obtain not Jess than 200 gof material, In cue the proportion of fines in the material so taken outdoe' not exceed 1 percent by weight, the material shall be crushed topowder form and processed further as under 2.3.3. 2.3.4 and 2.3.5. Fortbis purpose, fines shall constitute the portion or the material passingthrough 2-00-mm IS Sieve (SI' IS: 460·1962·).

2.3.2 In cqe the proportion of fines .. obtained under 2.3.1 exceedsI percent by weight, the entire contents of the package shall be taken outand pasted through 2·00-mm IS Sieve. The lumps and fines so separatedshall then be weighed and their proportion determined.

2.3.2.1 The lumps after weighing shan be quartered so as to obtainnot leu than 200 g of material and the latter shall be crushed to passthrough 2-()()..mm IS Sieve. The fine. after weighing shall also beseparately quartered 10 as to obtain not leu than 100 g of material.

2.3.2.2 Proportionate weights of Jumps and fines •• determinedunder 2.3.2 .hall be taken from the portioDl obtained under 2.3.2.1 andthoroughly mixed together to obtain a total orabout 200 g of material.

-5pecifi.-.tinn ror test aievea (SJaet 1ftIIIcI).

6

IS ,2962·1964

2.3.3 ComptJsiti SD1Ifpll- Out of the material obtained under 2.3.1or 2.3.2.2. as the case may be, a small but equal quantity shall betaken fromeach selected package and .hall be well mixed up together so u to form acomposite sample of not leu than 150 g (or the lot. This composite sampleshall be divided into three equal parts, one for the purchaser, another forthe supplier and the third for the referee.

2.3.4 Individual Sampltl- The remaining portion of the material fromeach package (af~er the lman quantity needed for the formation of com-posite sample has been taken out) shall be divided into three equal parll,each part weighing not leu than 50 g. These ~rtl .hall be transferredimmediately- to thoroughly dried bottles, closed With air-tight glass-stoppersand labelled with all the particulars of sampJins_ The material in eachsuch closed bottle shall constitute an individual sample. These individualsamples shall be separated into three identical sets in such a way that eachset has an individual sample representing each of the packages selected.One of these sets shall be marked for the purchaser, another for the supplierand the third for the referee.

2.3.5 Rt/trt, Sonlplls- Referee samples Ihall consist of l\ compositesample and a set of individual samples marked for this purpose and shanbear the seals of the purchaser and the sufplier. These shall be kept at aplace agreed to between the two and .hal be used in case of a dispute.

3. Q.UALITY OF REAGENTS

3.1 Unless specified otherwise, pure chemicals 'and distilled water( se« IS: 1070 • 1960- ) shall be used in testa.

NM'I': - •Pure chemicals' mall mean chemical. that do not contain impurities whichaff~t the ~\\h, 0( analysis.

4. PREPARED SAMPLE

4.1 Grind the sample in a porcelain mortar and pestle Or other suitableRrinder 10 that it completely panes through 425-micron IS Sieve(St, IS : 460. 1962t )_ ThlS shall be the /JU/HU,d sampU and man be usedfor tests.

5. TEST FOR STARCH

5.0 Outline or the Method -A IOlution or the material is tested withiodine.

5.1 Rea.eat

5.1.1 lodi. Solutio" - DiIIolve 2-6 g of iodine and 3 g of potassiumiodide in a sufficient quantity of water to obtain 100 ml.

~peciftcadon few water, distilled qualitY ("'). ($iQce rm.d).tspedflcation ror tete sieves (SIDce rnIIecl ).

7

IS, 2962 -1964

5.2 Procedure - Boil about 1 g of the pr'!Jar,d Sll11Ipl, with 10 ml of waterfor about 1 minute; allow to cool and add a few drops of iodine solution.

5.2.1 The material shall be considered to be free from starch if no distinctblue colour is developed.

6. LOSS ON DRYING

6.1 Procedure- Weigh accurately about 2 g of the p"/JGrtd lamp/' in atared weighing bottle or petri dish and dry in an oven at 980 to 100°C for3 to 4 hours, Repeat heatin~, cooling and weighing till constant weight(conltant to ± 2 mg) is obtained.6.2 CalealatioD

Loss on drying, ~r· 100 ( WI - H'.)cent by weIght :::: IVI

whereWI s= weight in g of the p"partd sampl« taken for the test, andWI := weight in g after drying.

7. CATECHIN

7.0 OutUDe orthe Method- The catechin is extracted out by refluxingwith a mixture of carbon disulphide and ethyl ether; the extract. isevaporated to dryness and weighed.

7.0.1 The catechin content sjgnifi~ the efficiency of separation of(crystallized out) KATTHA from the mother liquor in the manufacturingprocess.

7.1 ReapDt.

7.1.1 M,t/r.11 Altolaol-conforming to 18:517·1954·.

7.1.2 Solvntl Mixtu,,- prepared by mixing carbon disulphide (confor-ming to IS: 717 • 1955t) with ethyl ether (conforming to IS: 336 - 1964: )in the ratio I : 4.

7.2 Procedure - 'Veigh accurately about 1 g of the P"/JD"d sampk in a)OO-ml conical Oaak and shake with 20 ml of methyl alcohol to form aslurry. Evaporate the methyl alcohol on a water-bath. Add)OO ml ofthe solvent mixture and reflux, using a water condenser. on a water-bathfor halfan hour. Cool the mixture, allow to settle and filter by decantationthrough a filter paper (Whatman No. 11 or equivalent) into a beaker.Repeat the process of extraction twice, each time using fresh 100 ml of the

*Speciftcation (or methanol (methyl alcohol). (Since rm.ed).tSpecificadon (or C'arbon dilulphideL.technical. (Since reviled ).:Spet"ification for ether ( rtri#J). (zstnce reQ~ ).

8

IS .2962 • 1964

solvent mixture. \\'ash the residue after the last extraction with 20 ml ofthe solvent mixture and combine the filtrates and washings in the beaker.Evaporate the combined liquid to about 20 ml and then transfer quantita-tively, using small volumes of the solvent mixture for washing the beaker,into a weighed dish. Continue .evaporarion ,j;' the solvent at room tem-perature and then dry the dish with the residue in an oven at 50°..l. 2QCto constant weight (constant to ± 2 mg). --

Non; - In case of difficulty in filtering after rcAuxing due to high volatility of the~)v~nt mixture, suitable: arrangcmcnll shaU he made to keep the temperature of tirecontents in the funnel low.

7.3 C.lcul.rioDCatechin, percent by weight

( on dry bosis)

whereWI r:= weight in g of the residue,It', = weight in g of the p,tparld sampl« taken for the test, andM e: percent lou on drying as determined in 6.

8. COLD WATER EXTRACTIVES

8.0 Outline or the Method -1'he sample is kept for about 72 hours withwater at about 3°C. The filtrate is evaporated and the residue weighed.

8.0.1 Cold water extractives indicate the amount of cutch present inJi:1TTHA.8.1 RftlleDt

8.1.1 TollJInt

8.2 ProeeduJ;e - \-Veigh accurately about 1 g of the prepartd sampl« andmix thoroughly in a conical flask with 100 ml of water at about 3t'C.Add 1 ml of toluene as a preservative to the flask and keep in therefrigerator at about 3°C for 72 hours. Shake the flask occasionallyduring this period. Filter the supernatant liquid through a filter paper(\\'hatman No.1 t or. equivalent) under vacuum. Stir the residue with afurther quantity of water at about 3°C and filter until no more colour isextracted from the residue. Combine the filtrate and the washings andtransfer to a tared porcelain dish. Evaporate the water at 95° ± 2°C.Dry the residue at 98 0 to 100°C to constant weight (constant to ± 2 mg ),8.3 CalculadoD

Cold water extractives, percentby weight ( till thy basis)

whereJ1~1 .. weight in g of the residue,11', =: weight in g of the prtpar,d slimp" taken for the test, andM == percent loss on drying as determined in 6.

9

IS : 2962 -19M

9. MATTER INSOLUBLE IN REcrIFlED SPIRrr9.0 OutUa.- 0',· the Method - The sample ia treated with rectified spiritat 37°C for 24 hours, the residue is dried and weighed.9.1 R.a.eat

9.1.1 R"tified Spirit- conforming to IS: 323 • 1959·.9.2 Procedure - Weigh accurately about J g of the pr,pa"d sample andmacerate with 100 ml of rectified spirit. Shake frequently for 6 hours andthen allow to stand for J8 hours at 37° ± 2°C. Filter the supernatantliquid on a filter paper (Whatman No. II or equivalent) and wash theresidue free of soluble matter with rectified spirit maintained at 370 ± 2°C.Washing of the residue shall be continued till the filtrate leaves no residueon evaporation. Dry the residue with the filter paper in a tared weighingbottle at 98° to 100°C for 3 to 4 hours, cool in a desiccator and weigh,using a filter paper similarly treated as counterpoise. Repeat heating,cooling and weighing until constant weight (constant to ± 2 mg) isobtained.

Non _. Filtration may be dune with a sintered glaa crucible ( G No... ) or a Goochcrucible witlaubatnt bed u an .Jtemaaiwo.

9.3 Calculatloa

Matter insoluble in rectified spirit, 10000 JiJ1percent by weight (on dry 6asis) = fV~rlO(f-::"M)

wher~

J1'l .. weight in g of the residue,

WI - weight in g of the pr'fHl"t/'.fampl, taken for the test, and

M - percent lOA on drying al determined in 6.

10. WATER INSOLUBLE SOLIDS AT 37° ± 2°C10.1 Procedure - Weigh accurately about I g of the trt/Jarld sampl, in aconical Ruk and add 100 ml of water maintained at 37 ± 2°C to it. Shakethe flask f~ent'l for about 6 houri and then allow it to stand for18 hours at 37 ± 2 C. Filter the supernatant solution through a filler paper(Whatman No. JI or equivalent) under vacuum and wash the residuewith water (at 37· ± 2QC) until washings are colourlee. Dry the residuewith the filter paper at 98° to 100°0 in a weighing bottle to constantweight (conltant to ± 2 mg ), using a filter paper similarly treated a.counterpoise.

Nan - Filtraticxl may bedooe with • siatered .... crucible ( G No. 4 ) 01'. Goochaucible with Mbc8toI bed MIA a1terDatift.

~pedficadOD fOr reed6ed Iplrit ( mUM).

10

IS 12962 -1964

10.2 OalcaladoaWater insoluble solidi at 37°± 2°C, 10000 W

pereen t by weight {01l dry basis) =- AtWI (100 - )

whereJY1 = weight in g of the residue,J1.'I = weigh t in g of the prepar,d sampl« taken for the test, andM ~ percent loss on drying as determined in 6.

11. BOILING WATER INSOLUBLE SOUDS

10000 JY1

11.1 Procedure- Weigh accurately about 1 g of the prepared sample andreflux with 100 in} of water. for one hour. Filter the supernatant liquidthrough a filter paper (Whatman No. 11 or equivalent) under vacuum,using a hot water jacket funnel. Wash the residue with boiling wateruntil washings are colourless. Dry the residue with the filter paper in aweighing bottle at 98° to lOO~C to constant weight (constant to ± 2 mg),using a filter paper similarly treated as counterpoise.

Non - Filtration may be done with a sintered gla. crucible (G No... ) or a Gooc1lcroci ble with asbestos bed u an alternative.

11.2 CalcalatioaBoiling water insoluble solid_, percent

by weighr (011 dry basis)

whereWI =: weight in g of the residue,J-Y. :Dr weight in g of the prlJHmd sllmpl, taken for the test, andM -= percent loa on drying as determined in 6.

12. TOTAL AsH

12.1 Procedare-Weigh accurately about 2 g of the ""parld sdmpl, in atared platinum or silica dish and incinerate at dull red heat in a mufflefurnace or over a Bunsen flame till no carbonaceous particles are visible.Allow it to cool and weigh. Repeat heating, cooling and weighing tillconstant weight ( constant to ± 2 mg) it obtained. Preserve the ub fortest in 13.

12.2 Calcalado.Total uh,-percent by weight 10 000 W

(011 t/r;1 buiI) - W.{lOO-inwhere

WI - weight in I or the aah obtained,W. - weight in I ofthe~l...pU taken for the test, andM - percent lou on clryiDg as determined in 6.

II

IS s2962 • It&t

13. ASH INSOLUBLE IN HYDROCHLORIC ACID

13.1 R.apat

13.1.1 Dil"" H.1droeAlorie .Acid- J : 2-5( 010).

13.2 Procedure-To the dish containing the preserved ..h (12.1), add25 ml of dilute hydrochloric acid. Cover the dish with a watch-glass andboil the contents carefully for 5 minutes. Cool the solution and filterthrough a filter paper (Whatman No. 11 or equivalent). Wash the resi-due with hot water until the filtrate is neutral to litmus. Transfer thefilter paper along with the residue to the dish and incinerate completely.Cool the basin and weigh, Repeat heating. cooling and weighing tillconstant weight (coostant to ± 2 mg) js obtained ..13.3 CalCUlatiOD

Ash insoluble in hydrochloric acid, 10000 Wpercent by weight' (on dt.1 basis);:= It

W. ( 100- )

whereWl = weight in g of the ash insoluble in hydrochloric acid,WI :::z weifht in g of the prt/Nlrltl stlmpk taken for the test in

12. ,and -."M =- percent loss on drying al determined in 6.

"1'

12

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