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 10369 (1982): Ethion, Technical [FAD 1: Pesticides andPesticides Residue Analysis]

15 t t036t .. 1911( Reaffirmed 2004 )

[ndlan StandardSPECIFICATION FOR ETI-IION. rELHNt(~.r\L

• ('""",. 1'JN*~

t " D I \ N , r .., N DA I D.I tN S TI r tJ r io ~

~",,,,NJfa.K RH ..,\tAN. ~ aMtAOa;a .AH lAFAa ,.tAR~)

"I!~'Datu tl000J

IS: IOJt»9· 1981

Indian StandardSPECIFICATION FOR ETHION, TECHNICAL

Pe,t Control Sectional Committee. AFCDC 6

Chalrmall

DR K. D. PAHARIA

R.p,.,.",''''Directorate or Plant Protection, Quarantino -'

Slorale (Ministry of Aariculture ). Faridabad

M~mb."

Da H. L. BAM' Central Forenlic Science Laboratory ( CeDtralBureau of loveltilation ), New Delhi

Da B. BANIRJIB Tea Researcb Association, CalcuttaDR G. SATYANARAYANA ( I4lt,rnal. )

DR N. K. BAIU Tbe Alkali a. Chemical Corporation or IndiaLimited, Calcutta

SHRJ S. R. NIN. ( Alt.,,,al. )Da A. K. BHATNAOAR Hindultan IDsecticides Limited, New Delhi

SMRI C. C. ABRAHAM ( Aiternill. )CHII' CHIMIIT Central Revenues Control Laboratory (Ministry

01 Plnaoce ), New DelhiSHal S. KRIIHNAMURTHY ( Alt,rntll. )

CHIB' PLANT PROTECTION a'PlelR Department or Agriculture, Government ofMabarasbtra, Bomba,

CHEMIST INCIIAROI, INIICfICIDIITIITINO LABORATORY ( Alt.,nll'. )

SHaJ V. O. DIIHPANDI Ciba-OeilY of India Limited, BombaySRRI B. A. ALMEIDA ( Alt.rnal_ )

SHRIOM P. DHAMIJA Export Inspection Council of India, New DeIhlSHRI P. P. RANOA RAO ( ,flt~'''tll. )

Da M. S. DHATr National Malaria Eradication Prolramme, DelhiDJRICTOR OINIRAL Directorate Oeneral Armed Force. Medical Services

( Ministry of Defence ). New DelhiDJRBerGR 0' AORICULTURI Department or Alriculture, Government or Uttar

Pradesb, LuckoowDEPUTY DI1tICfOR (PLANT

PROTlCfION ) l All.'''.'.)SRR. V. Do.AI.AJ Plutlc ContaiDen Sectional Committee. MCPD 1J.

lSIDRUGS CONTROLLIR Indian Pharmacopoeia Committee (Ministry of

Healtb and Pamily Welfare ). New DelhiSRRI M. RAVIKANT ( Alt.rnat.)

( COII,In••011 pap 2 )

o CDPJlrl,,,, 1983INDIAN STANDARDS INSTITUTION

This publication i. protected under tho INlklll Cop,rl,la, Act ( XIV of 1957 ) aDdreproduction in whole or in part by any means except with written permiuioD ofthe publilber shall be deemed to be an inrrin,emeat of coPyrilbt under the laid Ace.

IS : 10369· 1981

( Conl,"u~d from pUle I )

DR KRISHAN SINOH

Entomology Division, Indian AlricuJtural ResearchInstitute ( leAR ), New Delhi

DR Il. L. KALRA Punjab Agrtcultural University, LudbianaDR R. P. CHAWLA ( A/lerna'. )

DR KALYAN SINGII Chander Sekhar Azad University or Agriculture"Technology, Kanpur

Indian Institute of SUlare_ne Research (leAR).Lucknow

AI~nnb~rs R,pr.,.n,ln,SHRI o. D. GOKHALB Bombay Chemicals Private Limited, Bombay

SHRI V. V. KETKAR ( Alternat« )SaRI D. K. JAIN Punjab United Pesticides and Chemicals Ltd,

ChandigarhJOINT DIRECTOR OF AORICULTVRE. Department of Aariculture. Government or

( DRVELOPM£NT & ICP ) Karnataka, MYlareDEPUTY D IRE C TOR 0'

AORICULTURB (PLANTPROTECTION ) ( Alternate )

DR M. G. JOTWANI

DR S. C. SRIVASTAVA ( Allernate)DR K. KRISHNAMURTHY Ministry of Alriculture (Department of Food),

New DelhiSHRI O. N. BHARDWAJ ( Alternate )

SHRI S. G. KRISHNAN National Ora_nie Chemical Industries Limited.Bombay

DR J. S. VERMA ( Alternate )DR. V. LAKSHMINARAYANA Directorate or Plant Protection, Quarantine "

Storale (MinIstry of Alrlculturo). FaridabadSRRI V. C. BHAROAVA ( Altemat« )

SHRI S. K. LUTHRA Directorate General of Technical Development,New Deihl

SHRI S. C. DAJAI ( AII~rnQt. )DR J. C. MAJUMDAR BASP India Limited, New Delhi

OR B. P. CHANDRASEItHAR ( Aiternat« )SHRI S. K. MAJUMDAR Central Food Technological Research Institute

( CSIR). MysoreSHRI M. MUTHU ( Alternat« )

SHRI O. N. M~HROIRA Ministry of Defence ( R&D)SHRI M. O. CHATtERJEB ( Alternate )

SRRI K. S. MEHTA Bharat PulveriliDI Mills Private Ltd, BombaySHRI S. CHATTERJ. ( Alt.rnate )

SRRI L. S. MIRLB Alromore Limited. BanaaloreSHRI S. K. RAMAN ( Alternat« )

8aRI J. M. MODI Pesticides Formulators Association of India( 8.5.1. ), Bombay

DR S. R. BAROOAH ( A.11.rnal. )DR A. L. MOOKBRJEB Cyanamid India Limited. Bombay

SRRI J. P. PARIKH ( Alt.rlUll. )DR S. K. MUKERJIB Alricultural Chemicall Division. Indian Agricultural

R.esearcb lastitute ( leAR ), New DelhiDa N. K. Roy ( Alt.rnllt. )

SRRI K. R. NARAYANA RAO Food CorporatioD of India, New DelhiSH1\IMATl K. K. M. BHAVNANI ( Alterna'e )

( Co"'l".~dGil Ptll- 10 )

2

AMENDMENT NO. 1 JANUARY 2007TO

IS 10369: 1982 SPECIFICATION FOR ETHION,TECHNICAL

(Page 4, clause 3.1) -- Substitute 'The material shall be packed as per•requirements given in IS 8190 (Part 2) : 1988 ' for 'The material shall be-,

packed as per requirements given in IS : 8190 (Part II) - 1980 as applicable topacking of malathion, technical.'

•(Page 4, footnote marked) - Substitute 'Requirements for packing ofpesticides: Part 2 Liquid pesticides ( second revision)' for the existing.

(Page 5, clause 4.1) -- Substitute 'Representative samples of the materialshall be drawn as prescribedin IS 10946 : 1996t' for 'Representative samplesofthe material shall be drawn as prescribed in 'Indian Standard methods forsamplingof pesticidesand their formulations' (under preparation).

(Page S. clause 4.1, Note) - Delete Note and its contents.

(Page S) - Insert the following footnote at the endof page:

•tMethod. of samplins for technical Fade pesticide•.•

(FAD 1)

Reproaraphy Unit. BIS. New Delhi. Indi.

MolecularMass

384-S

IS : 10369 • 1981

Indian StandardSPECIFICATION FOR ETHION, TECHNICAL

o. FO R E W 0 R D

0.1 This Indian Standard was adopted by the Indian Standards Institutionon 10 November 1982, 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 Ethion, technical is employed in the preparation of number of insecti­cidal and acaricidal formulations.

0.3 Btbion is the accepted common name. by the International Orga­nization for Standardization (ISO) for ss-methylene non o-tetraethyldie phosphorodithioate). The empirical and structural formulae and themolecular mass of ethion arc as given below:

Empirical Structural FormulaFormula

CZHsO <OC2 HI>p-s-cH2-S- Pc 2 H,O II II 0 C2 He

5 S

0.4 In the preparation of this standard, due consideration bas been givento the provisions of the Insecttctdes Act, 1968, and the Rules framedthereunder. However, this standard is subject to tho restrictions imposeeunder these, wherever applicable.

0.5 For the purpose of deciding whether a particular requirement of thisstandard is 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 methods of samplingand test for ethioD. technical.

• Rulea for rounding off Dumorical valuCl ("v;"d).

3

IS : J0369• 1982

2. REQUIREMENTS

2.1 Description -- The material shall be an amber liquid, free fromextraneous impurities or added modifying agents.

2.1 The material shall also comply whith the requirements specified inTable 1.

TABLE I REQUIREMENTS FOR ETHION, TECHNICAL

SL CHAR.ACTBRISTIC REQUIREMENT NaTHOD 0. TIST, RIP TONo. t .A.. \

Appendix CI No. of IS:6940·1982-

(1) (2) (3) (4) (5)

i) Bthion content, percent by 92-0 Amass. Min

ii) Acidity ( as A,SO. ), percent 0-30 11'3by mass, Max

iii) Moisture content, percent by 0-20 4mass. Max

.Methods or testsCor pesticides and their formulations ( ji", ,.villon ).

3. PACKING AND MARK.ING

3.1 Paeking - The material shall be packed as per requirements given inIS : 8190 ( Part 11 ).. 1980· as applicable to packing of malathion technical.

3.2 Markial - The containers shall bear legibly and indelibly thefollowing information in addition to any other information as is necessaryunder the Insecticides Act and Rules framed thoreunder:

a) Name of the material;

b) Name of the manufacturer;c) Date of manufacture;d) Batch number;

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

g) A cautionary notice as worded in Insecticides Act and Rules.

-Requirements for packiDIof pesticidel, Part II Liquid pesticides (jir" ,.vl.rlo,,).

4

IS : 10369· 1981

3.2.1 Bach container may also be marked with the lSI CertificationMark.

NOTi - The use of the lSI Certiftcation Mark is lovorned by the provisioDi 01tb, Indiaa Standard, Inltitution (Certiftcation Mark.) Act and tbe Rules andRe,ulationl made thereunder. The lSI Mart on products covered by an IndianStandard convey. the ..surance that they have been produced to comply withtbe requirements of that standard under a well-derined system or inspection. testinland quality control which is devised and supervised by lSI and operated by theproducer. lSI marked product. are also continuously checked by lSI for conrormityCO that standard as a further safe,ulrd. Details of conditions under which.licence (or the use of the lSI Certiftcation Mark may be granted to manufacturers orproceuorl, may be obtained from tbe Indian Standarda Inatitution.

4. SAMPLING

4.1 Representative samples of the material shall: be drawn as prescribed in'Indian Standard methods for sampling of pesticides and their formulations'( unde preparation).

NOTa - Till luch time the standard under preparation is published, the samplesshall be drawn as aareed to between the parties concerned.

5. TESTS

5.1 Tests shall be carried out by appropriate methods referred to in col 4and S of Table 1.

5.% Quality of RelleDtl - Unless specified otherwise, pure chemicals anddistilled water ( see IS : 1070-1977· ) shall be employed in the tests.

NOTE - 'Pure chemicala' Ihall mean chemical. that do Dot cODtain impuritieswhicb affect the result. of analysis.

APPENDIX A

[Table 1, Item (i)l

DETERMINATION OF ETMON CONTENT

A-G. GENERAL

A-O.I For the determination of ethion content. two metbods namelyinfra-red spectrophotometric method (ste A-I) and column chromato­graphy followed by phosphate determination as quinoline phosphomolyb­date t se« A-2) have been specified. Either of tho two methods may beused (or the determination of ethion content but infra-red speetophoto­metric method shall be the referee method.

·SpodflcatioD Cor wator Cor loaorallaboratory use ( I,co"dr"i,lon ).

5

IS: 10369· 1981

A·l. INFRA·RED SPECTROPHOTOMETRIC METHOD

A-I.I Metbod- The method consists or dissolving etbion in tetrachloro­ethylene. spectroscopic grade; scanning the solution in the wave lengthregion of 9-5-10·5". ( lOSO·9S0 em-I) in an infra-red spectrophotometerand measuring the characteristic absorption peak at 9-88" ( 1012 cm- t )

through the base point at 10-151£ (985 cm- 1 )_

NOT! - Since compounds witb ethoxy Iroups attached to phosphorus exhibitstrong absorption band between 1030 and 1010 cm- 1 and the absorption bandis attributed to P-O(C) vibration in the molecule. a wide raDSo spectrum foridentification of individual peaks may be taken.

A-l.1 Apparatas

A-I.J.t Infra-Red Spectrophotometer - Capable of recording in thoregion of 2000 to 400 em-I. The slit width, gain, response time andscanning speed should be so adjusted as to produce a satisfactory signal tonoise ratio and an adequate resolution. For the determination of ethioncontent by this method following parameters have been observed to besuitable:

Slit programme

Gain

Attenuator speed

Scan time

Suppression

Scale

Source current

1000

4

1100

100 em-t/min

S

IX

0-3 A

A..t.2.% Absorption Cells - sealed absorption cells with sodium chlorideor potassium bromide windows having an internal light path 0-1 mm.

A-l.1.3 Hypodermic Glass Syringe - 1-0 or 2'O-ml capacity. fitted withan 1-25 rom ( 18 gauge) slip on type needle.

A-l.1.4 Volumetric Flask, - capacity 2S·ml, Ilass stoppered.

A-l.3 Reagents

A-I.3.1 Bthion - of known (plus 99 percent) purity.

A-l.3.Z Tetrachloroethylene - spectroscopic grade.

A-l.4 Procedure

A-I.4.t Preparation 0/ calibration graph

6

IS ~ 10369 • 1981

A-l.4.1.1 Weigh accurately into separate 2S-ml volumetric flasksSO, 75. 100, 125 and 150 mg of pure ethion, Dissolve in tetrachloroethy­lene and dilute to the mark after mixing thoroughly.

A-l.4.t.2 Fill the absorption cell with each of the five standardsolutions of ethion (see A-l.4.1.1 ) in turn, starting with the dilute standardsolution, by means of hypodermic syringe. Make three scans of each ofthese solutions in the wavelength region 9'5-10'5#-, ( 1050 to 950 cm- t ).

A-l.4.1.3 For each of the scans of the standard solutions, measurethe absorbance at 1012 cm- t and the base point optical absorbance at985 cot-i. The difference between the maximum absorbance at 1012 em"!and the base point optical absorbance at 985 em"! gives absorbance dueto ethion,

A-l.4.1.4 Average the absorbance of the three scans of each of thestandard solution (see A-l.4.1.1) and plot a graph, taking absorbance asordinate against concentration as abscissa, for the five calibration solutions.

A-l.4.1 Estimation of Bthion Content

A-l.4.1.1 Weigh accurately a quantity of the sample containing100-150 mg of ethion in a 2S-ml volumetric flask and proceed as givenin A-l.4.I.l to A-l.4.1.3.

A-I.! CalculatloD

Ethion content, percent by mass = M X 100M 1

where

M = mass, in mg, of ethion as calculated from the calibrationcurve.

M1 = mass, in mgt of sample taken for test.

A·2. COLUMN CHROMATOGRAPHY/GRAVIMETRIC METHOD

A-1.1 Metbod - Ethion is separated from impurities by column chromato­graphy and an aliquot of purified etbion made to volume is decomposedwith a mixture of sulphuric acid and nitric acid. The phosphate thusobtained is precipitated as quinoline pbosphomolybdate and is estimatedgravimetrically.

A-2.2 Apparatus

A-Z.l.1 Chromatographic Column - about 40 ems in length and having20 mm internal diameter, with a fritted glass disc (G 3) at the bottomthat supports the absorbant and a burette tap. The top shall have a B 19joint fused.

7

IS : 10369 - 198Z

A-2.2.1 Sintered Glass Crucible - porosity 0-4, 30-ml capacity.

A-l.3 Reagents

A-l.3.1 Silica Gel- Chromatographic grade (60·120 mesh ). dried for4 bours at 110°C.

A-2.3.1 Ether-Hexane Mixture - 10 percent ether in hexane ( ,I, ).A-2.3.3 Sulphuric Acid-s- analytical reagent grade.

A-2.3.4 Nitric Acid - analytical reagent grade.

A-Z.3.S Citric Molybdate Solution - prepared as given in A-2.3.5.1and A-2.3.5.1.

A-Z.3.5.1 Weigh 54 g of molybdic anhydride (MoO.) in a SOO·mlbeaker. Add 200 ml of distilled water and 11 g of sodium hydroxidepellets. Heat the beaker until molybdic anhydride dissolves.

A-1.3.5.1 Dissolve 60 g of citric acid crystals in 250 ml of water in aone litre beaker and add 140 ml of hydrochloric acid (relative density 1-16).To this solution. add solution prepared in A-l.3.5.1 with stirring. Filterand dilute to one litre. This solution may be green or blue in colour. AddO·S to 1 percent solution of potassium bromide until green colourdisappears. Keep solution in a dark place in a well stoppered bottle ofpolyethylene.

A-1.3.6 Quinoline Solution - dilute 60 ml of concentrated hydrochloricacid with 300-400 ml water in a beaker and heat to 70 to 80°C. Slowlyadd 50 ml of pure quinoline stirring all the while when quinoline dissolves.Cool the solution, dilute with distilled water and filter into a one litrevolumetric flask and make up the volume with water. Keep solution in apolyethylene bottle.

A-2.4 Procedure

A-2.4.1 Weigh about 22-5 g of silica gel at room temperature into a2S0-ml beaker and make a slurry with hexane. Mix the slurry with aglass rod and transfer to the column by keeping the stop-cock open andwithout allowing the gel to dry during the operation by using more hexane.Gently tap the column to drive out any air bubbles entrapped. Applynitrogen pressure 0·7 Kg/em' ( 10 Ibs) on the column for compactionof the gel. Do not allow the liquid level to drop below the top of thesilica gel column. Layer about 2 ems of washed sand on the top of thecolumn to prevent disturbing the silica gel while charging the solvent orsample.

A-2.4.1 Accurately weigh a sample containing 0·5 g of ethion technicalin a 2S-ml beaker and dissolve in about 2-3 ml of hexane. When the liquidlevel is about 1 rom above the silica gel. pour the solution of ethion

8

IS : 10369 • 1981

carefully along the sides of the column. Rinse the beaker and the columnwith three times 2 ml of hexane. Again, do not aJlow the liquid level to fallbelow the top of the silica gel column.

A-2.4.3 Elute with 250 ml of 10 percent ether in hexane at a rate ofS ml/min. Discard the first SO ml fraction and collect the next ISO mlfraction in a cylinder. Transfer this fraction into a 2So-ml volumetricflask quantitatively using hexane and make up to the mark.

A-2.4.4 Pipette out 2' ml aliquot (see A-2.4.3) into a dry KjeJdahlflask of lOO-ml capacity. Evaporate the solvent on a water bath. Cool theflask and add carefully 4-5 rot of concentrated sulphuric acid and 1-S mlconcentrated nitric acid. Heat on a low flame till dense fumes appear. Letit cool and repeat the operation. Add 1 ml nitric acid and continue heatingtill the solution becomes perfectly clear and almost colourless.

A-2.4.5 Transfer the contents quantitatively, on cooling, into a SOO-mlbeaker with water to a volume of about 2S·30 mI. Boil for S minutes anddilute with water to about ISO mi. Add 25 ml of citric molybdate solutionand boil for 3 minutes. Immediately add 12-' ml of quinoline solutionfrom a burette. The quinoline solution should be added dropwise and thecontents of the beaker must be stirred continuously so that the precipitateobtained can be easily filtered. Let the beaker stand for 5 minutes stirringfor 5·10 seconds each time and then cool it to room temperature.

A-1.4.6 Filter by suction through a 04 sintered glass crucible. Washprecipitate four times by decantation and then wash with plenty ordistilled water. Dry the precipitate at 110°C for 2 hours.

A-2.4.7 Weigh the precipitate as quinoline phospbomolybdate(C,H, N )3HIP04 .12 MoO•.

A-1.! CalculatioD

Ethion content, percent by mass

384·S m 250== 2x 31 x 0'01399 X M x 25 X 100

86-76 x m=-- M

where

m :::I mass, in I, of the precipitate obtained; and

M = mass, in g. of the sample taken for test.

NOTI - 0-01399 is tho cODvenioD factor for quinoline phOlphomolybdate tophosphorus as P-

9

IS : 10369 • 1981

( Continued from PQI~ 2 )

8HR) R. G. JADEJA ( Alternate )DR S. Y. PANDIT Bayer ( India) Limited, Bomba)'

S'''RI c. o. DHARNB ( Alternat« )DR P. S. PHADKB Sandoz ( India) Limited, Thane

SHRI A. V. NATU ( A/',rnal. )SHRI S. M. PRADHAN Metal Container. Sectional Committee. MCPD 12,

lSISHRI Y. A. PRADHAN Rallis India Limited. Bombay

DR Z. J. KAPADIA ( Alt,rnat,)SHRI D. N. V. RAO Tata Chemicals Limited, Mithapur

SMR. C. NBliLKANTAN ( Alternat« )REPRESENTATIVI Pesticides Association of India, New DeIhlSBCRETARY Central Insecticides Board, Directorate of Plant

Proteetron, Quarantine &. Storlie (Ministryof Alriculturc ), Faridabad

M~mblrl Rtpr"entl",SHRII. NARSAREDDY Departmentor Agriculture, Government or Andhra

Pradesh, HyderabadSHR) C. DHARMA RAO ( Alternat« )

SHRIO. NATARAJAN Indoftl Chemicals Limited, BombayDR V. N. NIGAM Ministry of Defence ( 001 )

SHRI P. N. AOARWAL ( Alternate )SHRI M. M. PADALIA Department of Agriculture, Government or

Oujarat, Ahmadabad

DR R. C. GUPTA ( Atterna: )SHRI A. C. SHROFP Excel Industries Limited. Bombay

SHRt P. V. KANOO ( Allernat. )DR K. S. SINOR Indian Veterinary Research Institute (ICAR),

Izatn81arSMRI S. C. SRIVASTAVA ( Alternat« )

SHRI N. S. VENKATARAMAN Department of Alriculture, Government of TamilNadu. Madras

DR R. V. VENICATARATNAM Reaional Research Laboratory (CSIR), HyderabadDR NAOABUSHAN RAO ( Alternat« )

DR R. R. VENKATESWARAN Union Carbide ( India) Limited, New DelhiDil K. N SHRIVASTAVA ( Alternate)

SRR. E. R. VICCAJ8B Paper and Flexible PackaaiDI Sectional Committee,MCPD 14, lSI

SHRI N. O. WAOLB Pest Control (India) Private Limited, BombaySHRI M. R. BAJIKAR ( Altemat« ) ..

DR B. L. WAlTAL National Institute of Communicable Diseases, DelhiSRRI G. C. JOSHI ( Allernat~ )

SHRI T. PURNANANDAM. Director General, lSI (Ex-officio M~mb~,)Director ( A,rJ &, Food )

SecretarY

SHRI M. L. KUMAR

Deputy Director (Asri" Food), lSI

10