is 4344 (1978): endosulfan, technicalisi 4344. 1978 indian standard' specification for...
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IS 4344 (1978): Endosulfan, Technical [FAD 1: Pesticidesand Pesticides Residue Analysis]
Indian StandardSPECIFICATION FOR
ENDOSULFAN, TECHNICAL
( First Revision)
Third Reprint MAY 1993
UDC 632.951 END
IS I 43... • 1978( Reaffirmed 2002
Gr 3
@ Copyright J~78
BUREAU OP INDIAN STANDARDSMANAK BRAVAN. 9 BAHADUR SHAH ZAPAR MAllO
NEW DELHI 110002
MQY 1978
IS I 4344 • 191i
Indian StandardSPECIFICATION FOR
ENDOSULFAN, TECHNICAL
( First Revision)
Pest Control Sectional Committee, AFCDC 6
CluJirmtJnDR S. N. BANBRJltE
Re/W'u"tin,Directorate of Plant Prcteerion, Quarantine at
Storage (Mini.try of Agriculture & Irrigation ), Faridabad
( CQntinwtlOil tap 2 )
Department of Alriculture, Government of UttarPradesh, Lucknow
DnUTY DlBJ:OTOB ( PLAlfTPBOTEC'l ION ) .( Allmtllt, )
MnnlHrsDB N. S. AOARWAL
Pesticides lusociation of India, New DelhiCentral Forensic Science Laboratory, Central
Bureau of Investigation, New DelhiPesticides Formulators Association of India
( s. s. I. ), BombayAlkali" Chemical Corporation of India Limited,
CalcuttaDB T. V. RAOHURAMAN ( Altmtdl,)
DR A. K. BHATNAOAB. Hindustan Insecticides Limited, New DelhiS RBI C. C. ABBAHAM ( Alt"nal,)
SKBt V. G. D••HPANDB Ciba-Ge;gy of India Limited, BombaySRBI E. A. ALarBIDA. ( Altmuu, )
SSBI O. P. D1LUU1~ Export Inspection Council of India, New Delhi8111\1 P. K. CBA'rTB:anm ( AltmuJll )
DB M. S. DIUTT National Malaria Eradication Programme, DelhiDIBBeTo. CBlIfEBAL A R II B D Directorate General of Armed Forces Medical
FOReBa MEDICAL SIDRVICE8 Services ( Ministry of Defence )J New Delhia.....·ADIII.,u, M. S. M'ALBOTRA
( ~lt"""'" )DIRECTOR 0 .. AOBJCULTU.K
DB S. R. BABOOAH
DR N. K. BA8U
Department of Food (Ministry of ABriculture&t Irrigation ), New Delhi
DB K. KSI8HlfAMUBTHY ( AI/I1Mt, )DB P. !'I. AOARWAL Ministry of Defence ( R&D)
DR N. P. RA.o ( Alltrraal, )SHBI H. S. BA.HLDB H. L. BA.llI
<i) ~.,,,, 1978BUREAU OF INDIAN STANDARDS
This publication is protected under the I,.d•• eo"n,'" Ad (XIV of 1957) andreproduction in whole or in part by any meana except with written permislion of thepubliJber shall be deemed to be an in(riDlemeat of copyript unclei' the said Act.
IS J 4344 • 1978
( C(",li,wedjrom """ I )
AlnnHrsDu "f:~ CONTrtOI.I.En ( INDIA)
R,p"s,ntangIndian Pharmacopoeia Committee ( !\fini~try of
Health & Family Welfare ). Now De lhi
Indian Institute of Sugarc.ane Research ( ICAH. ),Lucknow
SHIll M. RAVIKI\NT ( Alt,rnQt~)
SHIU G. D. GOKHAl....; Bomhay Chern ica ls Private Limited, BombaySHIH V. V. KP;'CXAR ( AI'n-natl)
JOIN'l' DUtl':t'1.'OH OF AORICUI.TURE Department of Agriculture, Government( DEvELop~n:NT & ICP) Karnataka, M ysore
DJl:PUTY DIRECTOlt OF AORICULTUHJ<:( PLANT PIH1'rJi:CTtoN ) ( Alttr1l/J{e )
nit R. L. KALltA Punjab Agricultural University J Lud h ianar». R. P. CU.-\\VT.A (Altn-nale)
DM. KJ9HAN Srxn n
of
DR S. C. S1tlVABTAVA ( A.ltnnau )5MBJ S. G. KRISHNAN National Organic Chemical Industries Limited,
Bombay
( CSIR),Laboratory
Bhara t Pulverising Mills Private Limited,Bom ba v
Central Food Technological Research Institute( CSI R ), Mysore
Cyanamid India Limited, Bombay
Agricuf t-rral Chemicals Division, Indian Agricultural Research Institute ( ICAR ), New Dt:'Jhi
DR K. D. SHAMMA
DI~ K. S. SISON
Ccnt . al Inscct icidcs Hoard, Drrr-c torntr- of PlantProtection, Quarantine & Storage ( Ministryof .\griculture & Irrigation ). Faridabad
I)H S. Y. P"NIJJT Bayer ( India) Limited, BombaySH fU D. ;'\l. NAAHATE ( Alternate )
DII T. N. PAH'rHA8.AltATHY Regional ResearchHyderabad
Depar t ment of .'\griculture, Govcrnrnvrn ofGujarat ... \hmadabad
Su nr Y, A. PNADHAN Rail is India Limited, BombayDR Z. .J. KAP.-\DIA ( Alternate ) . .
Dn F, R_\lt~I.-\N Tea Research Association, CalcuttaUn G. SA"l'Y.\SARAY.\N.\ ( Alternate ;
StUll G. K. R.-\o Mi'nisrr v of Defence ( DGI )DR A. K. SJ.l:S ( Alternate )
SHill K. R. lXAl(AY.\NA" RAO Food Corporation of India, New DelhiS)IT K. K. M. BH.'VN-\.NI ( Altemate )
DR RATTAN LAL Entomology Divisioni
Indian Agricultural Re..searc h Institute ( C ...\R), !\ew Delhi
Directorate General of Technical Development,New Delhi
Indian Veterinary Research Institute (leAR),Izatnagar
SUItI S. CHAT'rl4:nJI ( Alternate )])lL A. L. ~100I\:J';IlJEJ~
SHUI]. P. PAnlKH (.llle,nall)Un S. K. ~hTJ\EnJF.l';
SHJlI M. MtJTHU (AltnNJI.)SHU 1 K. S. l\rJ.:HTA
I) h N. K. Rov ( (fl ternate )1) II K. D. P.\ H ~\ Ie rA
Sffl:l 1\1. .\. P.\TEL
DR J. S. \,'t:R~fA ( Alternate)SMJU S. K. MAJUMDAR
S.tflCl S. C. SRl\·.-\ST.AX.\ ( Alternat« )( Coralirru,d Dn /Jtll' 8 )
2
SHKIT.PURNANANDAM,Deputy Director ( Agri & Food)
IS I 4344 • 1978
( COIII;""ufrom /Ja" 2 )
MmllNTs Rf.P'tj~"li',g
SaBI K, VENKA'r,\CliJ\L,\~1 Dcpar t.ncnt of ,\grlC\1lture. Cov('rnnlf>lll ofArulhra Pradesh, Hyclcrabud
SHRI K. SATYANARANA RAO ( Alt~'1UJ16 )SHill N. S. VENXATARAliAN Depur t mrnt of AgricuJtltrf', (~ovl('rnJllenl of
'rami! NaduDR P. R. VENKATESWAllAN Union Carbide India Li mitcd , New Dr-Ih i
Dn K. N. SUJUVA8T.\.VA ( Altmuzl,)SHIU N. G. WAGLE • Pest Control ( India) Private Li rn it cd , Bornbay
SURI M. R. BAJIJCAR ( AlternGt, )Da B. L. WATTAL National Iusritutc of Cornrnu nicable Diseases,
DelhiDirector G('ncra 1, BIS ( E\-njficio Mnnb" J
&c,darySHill LAJINDER SINon
Assistant Director ( Agri & f'ood J, DIS
Pesticides Subcommittee, AFCDC 6: 1
ConlJtnn
DR K. D. PAlfARIA Central Insectic ides Hoa rcl , !Jirl'('lori.l" flI" Pl~&nt
Protection. Qlarantint: & SlfJr;lgl' ( ~'lini,·
try of Agricu lrur« & lrrig;u lUll ). I;a.ridiJbad
DR. N. K. BA8U
Mmrbns
Os N. S. AOARWAL lJepartment of Food ( Miniatr y uf .\griC:ll1ture &Irrigation L New DC!lhi
DR K. KKISH.NAMUll'l'HY ( AllnJUlu )SH.RI E. A. ALMEIDA Ciba.G~igy of India Limited, IJolllh;\)Da H. L. BAMI Central Forensic Sc ience Laboraturv, Central
Bureau of Investigation, New Ilf;1tliAlkali &. Chemical Corpcrarion of India Limited,
CalcuttaOa A. P. DUTTA ( AltlNUJt, )
Da A. K. BHATM,AOAR Hindustan Insccricjdcs Lirni ted , :\cw Dc lh iSa.Rl C. C. AUR.A.HAM ( Alllt'NlU )
Da N. F. DE8A.l Sandoz ( India) Limited, ThanaD. P. S. PHADE. ( Allmlll'. )
D. M. S. DIUT'l' National Malaria Eradication Programme, DelhiSHJlI G. D. GoKHALE Bombay Chemicals Private Limited, Bombay
SHal V. V. KBTKAD. (AIUmilI')Da KALY.6..k SDftlH U. P. Institute of Agricultural Scienccs , KanpurSa·al 1<.. S. MIIHTA Bharat Pulverising Mills Private Limjtcd ,
BombaySaRI S. CBATTEBJ I ( AltlF",," J
( ClJ1IJUlUld onpa" !J )
8
IS 1 4:444 • 1978
(G'o,,'inucd)'0111 ~lgt 1 )
MemberJS .. ,.., J.. S. M IfnI"~:
J )1: S. J". ~I' 1'lu·;n.n:I':
R,pr'~mlir&J
Agromore Limited, BangaloreAgricultural Chemicals Division, Indian Agri·
cultural Research Institute (leAR), NewDelhi
(CSIR ),Laboratory
Centra] Revenue. Control Laboratory (Ministryof Finance), New Delhi
S II It I (~. )) 11.\ IC\I\ R.-\o Pesticides Testing Laboratory. HyderabadSUlCI D. X. V. R ..\O ' 'rata Chemicals Limited, Mithapur
SIInl C. NI'~";"K,,\N"'JI_\~ (Al',.-,nfJle)Du K. K. S.\:\: ":N \ Inuofil Chemicals Limited, Bombay
SUI" (;. N.\'.".\H.\.f.\N ( Allum",)s ...:, .\. (:, S'tt,Ol"'" Excel Industries Limited, Bombay
S It It I P. V. K \ Nun ( .)lI,·"lIlllj )S'itH K. S,' N It.\ It.,)l Hiudustan Petrol cum Corporation Limited,
Bomba)'
nit N. K. Roy ( All,rnat,)l)u S. Y. PANfH'r Bayer (India) Lim itod, Bombay
S 111\1 J). N. NAKllA'rE ( AlterMI, )Du '1'. N. PAU.'I'IL'~,\HATJl y R~gional Research
HyderabadP',.\~"· l'uo"'~t'''''I)N ADV]s}<~n 'J'f) Directorate of Plant Protection, Quarantine It
"'IU: (;OV1~ltNJ\-"';N'" of INDIA Storage (Ministry of Agriculture at Irrigation ), Faridabad
n« V. J..J\KHU1\()NAItAYAl-iA ( AltnTuJt,)Sill:' Y. A. PU.\IHIAN Rallis India Limited, Bombay
S" HI ~l. L, SU,\U ( Alternat« )1)1: v, S, ){,\ l'f" N ,\'I'Jl1\1(
S n n r u, R ..\JMJ\SI ( Alternate )~"lCt 1\;, S. \'·':}l;).;;O\'I'A1LAMAf'l,
Du U. J.. '''',\'rT,\ f.
Pest ir idvs 'Test in~ Laboratory, Kovilpntt iNationnf I n!titlt tc of ConJmun;cabJff Diseases,
Delhi
9
IS I 4344. 1978
Indian Standard'
SPECIFICATION FORENDOSlJLFAN, TECHNICAL
( First Revision)
o. FOREWORD
0.1 This Indian Standard (First Revision) was adopted by the IndianStandards Institution on 15 February 1978, after the draft finalize d by thePest Control Sectional Committee had been approved by the Agriculturaland Food Products Division Council and the Chemical Division Council.0.2 Endosulfan is a non-systemic and stomach insecticide and is effectiveagainst. agricultural and household insectsjpests,0.3 This standard was first publ ished in 1967. Subsequently AmendmentNo. 1 was issued, In the first revision the packaging, sampling and.cautionary notice requirements had be en modified. Opportunity has beentaken to refer IS: 6940 ... 1973· to bring uniformity in testing procedure{or the various requirernents given in the standard.0.4 EndosuJfan is the accepted common name by the International Organization for Standardization (ISO) for the insecticidal chemical 6, 7,8. 9, 10, lO-hexachloro-l, 5, Sa, 6, 9. 9a-hexahydro-6, 9..methane..2, 4,3-benzo [e]-di<1xathiepin 3-oxide. The empirical anti structural formulaeand the molecular mass of endosulfan are as indicated below:Empirical Formula Siruct""al Formula Mol(c"lar Mass
. CI H
/c,1a-c I C-CH2-o,
C.H.CI.OaS II CCla I 5=0 406-95
Cl-C,!/,-CHZ-o/Ct.. .
0.5 In the preparation of this standard, due consideration has been givento the provisions vof the Insecticides Act, 1968 and the Rules frame dthereunder. However. this standard is subject to the rertrictions imposedunder these, wherever applicable,
• Methodl of telts for pesticides and their formulations.
3
IS I 4344 - 1978
0.6 For the purpose of deciding whether a particular requirement of thisstandard i~ complied with. the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in"accordance withIS: 2·1960·. The number of significant places retained in the rounded offvalue should be the same as that of the specified value in this standard.
1. SCOPE
1.1 This standard prescribes the requirements and the methods ofsampling and test for cndosulfan, technical.
2. REQ,UIREMENTS
2.1 DHcripdoD -- Endosulfan, technical shall be in the form of light todark brown solid and shall be free from foreign matter or added modifyingagent(s) .
2.2 The material shall also comply with the requirements given inTable 1.
TABLE 1 REQUIREMENTS FOR ENDOSULFAN, TECHNICAL
s., <':' •.\ItAC1'Jr.UISTll' RY.QUIU. ..;MKNT MY-TUOD 0.· TP:8T) n.t;1" TONo. r----- ..---..A-.-----~
Appendix of Cl No. ofThis Standard IS: 6940... 1973·
( 1) (2) (3) (4) (5)
i) Act ivo inl{redient content) 90 Apercent by mas-s, Min
ii) Moisture content, percent 0·1 4-by mass, AfGX
iii) Material insoluble in ace- 1·0 9tone. percent by mass,4\1"
iv ) Acidity ( as "2S0. ). per- 0·1 11.3cent by 'Has" It-IG:\:
·M("thod~ ortests for pesticides and thrir for mulat ions.
3. PACKING AND MARKING
3.1 Paeld•• - The material shall be packed according to IS: 8190 .( Part I )-1976t.
·Rult'A for rounding off numerical values ( recised },tRequir("lnent, for p"ckin~ orpPlticid~.: Part I Solid pesticides.
4
IS.OH.lt71
3.2 Marilla. - The container shall bear legibly and indelibly the following inrormJ.tion and any other information as is necessary under theInsecticides Act and Rules:
a) Name of the material;b) Name of the manufacturer;c) Batch number;d) Dat~ of manufacture;e) Active ingredient content, percent ( mlm );C) Net mass of contents; andg) The minimum cautionary notice worded as in the Insecticides
Act and Rules.
3.2.1 When packed in bags, the pictorial marking for • USE NOHOOKS. DO NOT PUNCTURE' as contained in IS : 1260 ( Part II )1973* shall be stencilled on the bags.
3.2.2 Each container may also be marked with the Standard Mark
NOTS - The use of the Standard Mark is lavernecl by the proviuou of theBureau of IndiaD Sraadards Act, 1986 and the Rules aDd RelulatioDs nwlo thereunder. The Staadard Mark on products covered by aD IDdiaD StaDdard CODveysthe assurance that they bave been produced to comply with the requirements of -thatstandard under a well defined sYltem or inspection. tettin. and quaBty coatrolwhich .. deviloct and luperviled by DIS and operated by the producer. StaDdarclmarked products are also continuously checked by DIS IQr conformity to thatltaaclard as a further safeauard. Details or conditioal under which • JlceDce forthe use of tho Standard Mark may be aranted to manuractuten or producers ma,be obtained from the Bureau of Indian Standa.rdl.
f.8AMPUNGf.l Representative samples of the material shall be drawn as prescribedin C Indian Standard methods for sampling of pesticides and their formula..tions (untili' P"PIl,Qlioll ).
NOTE - Till such time the Itandard under preparation fa published, the ..atterthall be .. agreed co between the concerned parde•.
5. TESTS5.1 Tests shall be carried out by the appropriate methods referred to incol 4 and 5 of Table I.5.2 Q,aaUty 01 Re••eat. - Unless specified otherwise, pure chemicalsand distilled water (I" IS: l070-1977t) shall be employed in the tests.
NOTE - C Pure chemica" t .hall mean chemicals that do not contain impuritieswhich a8'ect the results of analYlb.
·Pictorial marklng for h'lndUng and labellinl of good.: Part 11 General good.(first r,rtisioft).
fSpecification for water for general laboratory use ( ueotUJ ,,,,;,n.,, ).
IS I 4344 • 1978
APPENDIX A[Table I, SI No. (i) ]
DETERMINATION OF THE ACTIVE INGREDIENT
A-I. PRINCIPLE OF THE METHOD
A-I.I The principle, in determination of the active ingredient of endosulfan, namely, 6, 7, 8, 9, 10, lO-hexachloro-l J 5, 5a, 6, 9, 9a-hexahydro-6,9-methano-2, 4. 3-benzo [ ~ ]-dioxathiepin 3';oxide, is based on hydrolysisof endosuJfan with methanolic sodium hydroxide and estimating thesodium sulphite ( Na,SOa) so formed iodornetrically,
A-2. REAGENTS
A-2.1 M.thaDol
A-2.2 SocIi1llD Hydroxide - pellets.
A-2.3 Phellolphtbaleia ladie.tor SolutioD - one percent (m/v) inrectified spirit.
A-2.4 Staaclard Sulphuric Acid - 5 N.
A-2.5 Staadard Iodine SolutioD '- 0·1 N.
A-2.6 StaDdarcl SocHam Thio8.lphate Solutio. - 0·1 N.
A-2.7 Starch SolutioD -0'2 percent, freshly prepared.
A-3.PROCEDUREA-3.1 Weigh accurately about 0·5 g of the material and transfer it to a250-ml flask. Add 100 ml of methanol by a pipette. Introduce about1·5 g of sodium hydroxide pellets (about 15 pellets). Connect the flaskto a reflux condenser and boil the contents at least for 2 hours. Shake theflask occasionally. Wash down the condenser with 20 ml of methanoland 50 mJ of distilled water. Add one drop of the phenolphthaleinindicator solution. Neutralize with standard sulphuric acid. Add a fewdrops of dilute sodium hydroxide to restore the indicator colour and toprevent any loss of sulphur dioxide.
A-3.2 For accurate determination of the sulphite, it is essential to add thesodium sulphite to an excess of acidified standard iodine solution and backtitrate the excess of iodine with standard sodium thiosulphate solution.
A-3.3 Take 40 ml of standard iodine solution in' a SOO-ml glass stopperedflask from a burette. Add 10-15 ml of the standard sulphuric acid to makesufficiently acidic and shake it slowly (set Note). 'Vhile agitating, add
6
IS I 4344 • 1~18
the aliquot containing sulphite solution... Rinse the flask well with smallportions of distilled water until all the sulphite has been transferred (thewashing procedure should be continued until there is insufficient sulphitein the flask to bleach a small drop of iodine). The final volume in theiodine flask should be about 225 to 250 ml.
NOTJI: - This process will have to be conducted in an evacuated flalk.
A-3.4 Back titrate the excess iodine; with the standard sodium thiosulphitesolution, using starch solution as indicator and titrate until the blue colourdisappears.
A-3.5 Carry out a blank determination by titrating 40 ml of the standardiodine solution to which "175 ml of water acidified with the same amountof standard sulphuric acid that has been added in the sample with standardsodium thiosulphate solution.
A-3.6 The difference in the volume of sodium thiosulphate solution indicates the iodine equivalent consumed by endosulfan.
A-4. CALCULAnON..&. ..4. 1 A' · di b V x 2·0353-". ctive mgre lent, percent y mass = kf
whereJ/ =-= volume of 0·1 N iodine solution as used in the test, andJ1 == mass in g of the sample taken for the test.
7
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