IS 7976 (1976): Phorate, TechnicalDisclosure to Promote the Right To Information
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IS 7976 (1976): Phorate, Technical [FAD 1: Pesticides and Pesticides Residue Analysis]
Gr3
-Indian Standard
,i) Copynght 1976
BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH / MAR MAR(;
NEW DB HI
Indian Standard SPECIFICATION FOR
ChaIrman
DR S R BAROOAH DR N K. Basu
RepreJentmg Directorate of Plant Protection, Quarantine &
Storage ( MInistry of Agriculture & Irngauon ), Fandabad
Mmistry of Defence ( R&D)
Central Forensic Science Laboratory, Central Bureau of Invesnganon, New Delbi
Pesticides Association of India, New Delhi The Alkali & Chemical Corporation of India Limited.
Calcutta
Pradesh) Lucknow
Indian Pharmacopoeia Committee (MlOlstry of Health and Family Plannmg ), New Dellu
DR T. V. RAGHURAMAN ( Alternate) DR O. S BINDRA Punjab Agrtcultural Umver-uty, Ludhrana
DR R. L. KALKA ( Alternate) SSRI P. CHAWLA National Organic Chemical Industries LImited.
Bombay SHRI K. D. AMRE (Alternat, I ) SHRl BHUPINDER SINOH ( Alternate II )
SHRI V. G DESHPANDE CIBA·Gelgy of India Limited, Bombay SHRI E A. ALMEIDA ( Alternate)
SHRI 0 P DHAMIJ" Export Inspection Council of India, New Delhi SHRtG. C. DE (AI"".I, )
DR M. S. DHATr DIRECTOR OF AGRICULTURE
DEPUTY D,RECTOR (PLANT
PROTECTION) (Altunate) DIRECTOR Gt.NERAL. ARM E D DIrectorate General of Armed Forces Medical
FORces MEDICAL SERVICES Services, Mmistrv of Defence, New Delhi MAJ-GEN DARYAO S,NOH (Alt"nal')
SHRI R S. DlWEDI Food Corporaton of India, New Delhi SHRI). P GUPTA ( Allmlal,)
DRVGS CoNTROLLER (INDIA)
( C••llIIUId •• /JOl' 2 )
BUREAU OF INDIAN STANDARDS
ThIS pubucation IS protected under the Indian Copyrtgtu Act (XIV of 1957) and reproduction In whole or 10 part by any means except With wntten permrssion ofthe pubhsber shall be deemed to be an mfrmgement of copyright under the said Act.
IS I "'6 • 1"6
( Cantinu••from pag. I )
Rtp,eun1mg
MemblYs
SHRI T~ GEORGE JOHN
DR S. N. NAG ( All.,.." J SHRI G D GOKHALE Bombay Chemicals Private Ltd, Bombay
SMRI V. V. KETKAR ( AllffM") SHRI PRITA... SINOH HOSHIARPURI Department of Agriculture, Government of Punjab,
Chandrgarh SHRt MUKHTIAR SINOH SRA (Altmuzu)
JOINT DIRECTOR OP AORICULTURE Department of Agriculture, Ocvemmenr of Kama- (DEVE.LOPMENT & ICP ) taka, Mvsore
D2PUTY DIRBCTOR 0. AGRICULTURE (PLANT PRO- mOTIoN) (AIUma")
DR KlSHAN SINOH
DR S. C SRIVASTAVA (Alttrnote) Smu S. K. MAJUMDAR Central Food Technological Research Institute
(CSIR J, Mysorc
Department or Agrrculture, Government of Andhra Pradesh, Hyderabad
Bharat PulverISing Mills Private Ltd, Bombay
Central Insecnctdes Board, Directorate of Plant Protection, Quarantme & Storage (MlOutry of Agriculture & Irrtganon " Farrdabad
DR S Y r A!'oD1T Bayer ( India) Limned, Bombay Snar D N NAKHATE (Alterna(t:)
SHRI M A PATI::.L Department of Agriculture, Government of Gujarat, Ahmadabad
Rallis India Limited. Bombay
SURI Y A PRADHAN
DR Z J KAPADIA ( AlJeTlJo/e ) DR F RAHMAN Tea Research Assocrauon, Calcutta
DR G. SATYANARAYANA ( Alternate) SHRI G. K. RAO MInistry of Defence (DGI ), New Delhi
DR A K SEN ( Alt""a', ) DR RATrAN LAL
SIIRI M Murau ( AlltrMIt) SHRI K. S. MEHTA
SURI S. CllATTERJl ( Alternnt, ) DR H. N MOHAN RAO Pest Control ( Indra ) Prrvarc Ltd, Bombay
StiRI MOIlAN S RAO ( Altt:rnalt: ) Dn A. L. MOOKlRJI!.E. Cyanamid India Limned, Bombay
SHRI J P PARIKH ( Al'"nal, ) D. S K MUKHER)EE
SURI M. V. GOPALA KRISHNA SARMA
SHRI P SUA,NKAIt RAO ( Alternate) DR G. C. SENGUPTA Department of Agnculrure, Government of Orissa,
Bhubaneswar SHRJJ. M SATPATHY (Altmlate)
Dit K D. SHARMA DIrectorate General of Technical Development, New Deihl
DR K. 5 SINOH Indian Veterinary Research Institute (leAR). Izatnagar
SHRJ S. C. SRIVASTAVA ( Alurnou)
(Conlin"".n pag. 3)
DR B. L. WATTAL
National Institute of Cornmurucable Diseases, Deihl Director General) lSI (Ex-offiCIO Memb,T)
Secretary
.Members DRN S. AGRAWAL
Department of food (Mimslry of Agnculture & Irrrganon }
National Organic Chemical Induames LUIUtcd J
Bombay
Central Forensic SCIence Laboratory, Central Bureau of Invesuganon, New Deihl
Pesticides ASSOCiation of India, New Delhi The Alkah & Chemical Oorporauon of India Limited,
Calcutta
DR S. R. BAROOAH
DR N. K. BASU
DR K KRISHNAMURTHY (Alttrnatt) SHIll E. A. ALMF.IDA CIBA·Geigy of India Limited, Bombay
DR R.]. KAMAT (AII,moI,) DR H. L BAMI
DR A. P DUTTA ( All".." ) SHRI P. CHAWLA
SHRI K. D. AMRE ( Alternate I ) SHRJ BHUPINDER SINGH (Alternate II)
Smu K. K. CHHAYA Excel Industnes Limited, Bombay SHRI P V. KANGO ( Alternate)
SHRI A. K. DAS Directorate General of Technical Development, New Delbi
DR K. D. SHARMA ( ,111m..', ) SHRl C DHARMA RAO Pesticides Tcsung Laboratory, Hyderabad DR 1\1. S DIIATT National Malarra Eradrca non Programme, Delhi SmH G D GOKHAIE Bombay Chemicals Pnv.ne Ltd, Bombay
:"'Iwu \ V KI,.Th.AR \ Auemau s DR J....ALYAN SIM.H U. P Institute of Agrrcultural Sciences, Kanpur SHRI K. S. MERfA Bharat Pulvensmg Mills Pnvate Lrd.Bornbav
SURI S CHATThRJl I, Alumate ) DR H N. MOHAN RAO Pest Control ( Indra ] Pnvate Ltd) Bombay
SHRI MOHAN S. RAO (Altem~te)
DR S. K. MUKHERJEE Agncultural Chemicals DIviSIOn, Indian Agricultural Research Insntute (ICAR )J New DelhI
DR R. S. DEWAN (AlteHlate J DR S. N l\'Ar. Hmdustan Insecticides Lrmrted, New Ddht
Smu A. N I'\ATARAJAN ( Alternate)
I ronlmuedon Pilt~ 4 )
(C"ntlnuedjTOm page 3)
Member; Represmlrng SHRI N. B. PATJ>.L Tata Chemicals Limited, Mnhapur
Slial D N. V. RAO ( Alternate ) SHill S L PER't1 Muustrv of Defence ( R&D) PLANT PROTECTION ADVISER TO Directorate of Plant Protection. Quarantine &
TH! GOVERNMENT OF INDIA Storage ( MinIStry of Agnculture & Irngahon), Farrdabad
DR V. LAKSHMIN>\RAYANA (Allernnk) SHRI Y. A. PRADHAN Rallis India Limited, Bombay
SHRI M. L ~IIAH ( Alternau y DIl V. S. RAMANATHAN Central Revenues Control Laboratory (Ministry of
Finance ). New Delhi SRal P P. MATRFW (Alt,mal' )
SRO' G K. RAO MLnl>try of Defence ( DGI ) DR A. K SEN (Alternate)
DR K. K. SAXENA Indahl Chemicals Limited, Bombay SKU S S. SHAH New Cherm Industries Prr ... ate LImited, Bombay
SHRI N A SHANBHAG (Alternate) SHRI P. P. SINGHAL Pesncides India, Udaipur
SHRI MOHOMED YUSUf (Alternate ) SHRI N. S. VENKETARAMAN Pesticides Testing Laboratory, Madura. Da B. L. WATTAL National Institute of Communicable Diseases, Delhi
SHR. V. N. BHATNAQAR (Alternate)
FEBRUARY 1985AMENDMENT NO.1 TO
( Page 6, Table I ):
a) Col 5 - Substitute ' 15 : 6940-1982' • fa' , IS· 6940-1973 ".
b) Foot-note untl: ' • ' mark - Substitute the fallawmg far the exisnng foot-note:
I 'Methods of test for pesticides and their formulations (first revlSZon). '
( Page 6, clause 3.1 ) - Substitute the following for the existing clause:
'3.1 Packing - The material shaJJ be packed as per requirement given in IS : 8190 ( Part II ).1980·,'
( Page 6 ) - Add the following foot-note'
(.ReqUlremcnts for packmg of pesticides. Part II Liquid pesncidee (first revuion).·
[ Page 7, clause 3.2(g) 1-- Delete.
( Page 7, clause 3.2.1 ) - Delete.
( Page 7, clause 4.1 and note) - Substitute the foliowing lor the eXIS­ ting matter:
'4.1 Representative samples of the material shall be drawn according to IS : 10946-1984".
( Page 7, clause 5.2, line 2) - Substitute 'IS: 1070-1977t' Jo, , IS : 1070.1960t '.
(Page 7,foot-notes with' • ' and' t' marks ) - Substitute the following for the existing foot-notes:
, .Methods for samplmg of t echnn-al grade pesncrdes. tSpeclficahon for water for !5eneral laboratory usc (jecond TfVBIOn ) ."
. (Page 10, clause A.2.3.1, equanon i - Substitute the following for the existing equation:
'A.2.3.1 Phorate content, percent by mass
_[6'510 X (VIF,) - ( V, F')}J ~ [1'302 :< {( V1F j ) - ( [',F,) 1J - ~ ~
(AFCDC 6) Prlnred a' New Indii Pnnrlng Press, KhurJa,. india
(FAD 1)
IS 7976 : 1976 SPECIFICATION FOR PHORATE, TECHNICAL
(Page 6, clause 2.2, Table I, SI No. 1, col 4) — Substitute 'Clause 3.3.1 of IS 9359 : 1995†' for 'A ' .
(Page 6, clause 2.2, Table 1) — Add the following footnote at the end:
'†Pesticide — Phorate eucapsulated — Specification (first revision).'
IS: 7976 .1976
PHORATE, TECHNICAL
O. FOREWORD
0.1 This Indian Standard was adopted by the Indian Standards Institution on 25 February 1976, after the draft finalized by the Pest Control Sectional Committee had been approved by the Agricultural and Food Products Division Council and the Chemical Division Council.
0.2 Phorate is an organophosphorus soil and svsternic insecticide used for protection against SUCking and chewing insects, mites and certain neuratodoes infestmg various crops.
0.3 Phorate is the accepted common name by the International Organiza­ tion for Srandardization (ISO) for O,O-diethyl S.[ (ethylthio )-methyl] phosphorodithioate. Its empirical and structural formulae and molecular weight is as given below:
Empirical Formula Structural Formula Molecular Weight
CzH.O<, /P.S.CHz.S.CzH,
260·4
0.4 In the preparation of this standard due consideration has been given to the provisions of the Insecticides Act, 1968 and the Rules framed there­ under. However, this standard is subject to the restrictions imposed under these, wherever applicable.
0.5 For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expres<­ ing the result of a test or analysis, shall be rounded off m accordance with IS : 2-1960.. The number of significant places retained in the rounded off value 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 of sampl­ ing and test for phorate, technical•
• Rules for rounding oft'numencal values (r,uiud).
5
15.7976.1976
2. REQ.UlREMENTS
2.1 Description - The material shall be yellow to amber coloured liquid, free from foreign matter and added modifying agents.
2.2 The material shall also comply with the requirements given in Table I.
TAliLE 1 REQUIREMENTS FOR PRORATE, TECHNICAL
4.1
9
11.3.2
Appendix CI No. of IS : 6940-1973·
(5)
CHARACTER,ISTIC
II) Material insoluble 10 acetone, 0'5 percent by mass, Max
ill) Moisrure content, percent by 0'5 mass, .l\1(g>
IV) Acidity ( as HzSO",), percent by 0'5 mass, Max
v) Specific gravity at 2YC, Mm 1'00
*Methods of tests for pesticides and their Iormulanons.
SL No.
3. PACKING AND MARKING
3.1 Packing - The material shall be packed in clean and dry mild steel containers which arc SUitably lacquered
3.2 Marking - The containers shall be securely closed and shall bear legibly and indelibly the folloWIng Information in addition to the informa­ tion as is necessary under the Insecticrdcs Act and Rules;
a) Name of the material,
b) Name of the manufacturer,
c) Date of manufacture,
6
g) The minimum cautionary notice worded as under:
HANDLE WITH CARE. KEEP OUT OF REACH OF CHILDREN AND WELL AWAY FROM FOODSTUFFS, ANIMAL FEEDS, AND THEIR CONTAINERS. AVOID SKIN CONTACT. WHILE HANDLING WEAR PROTECTIVE GLOVES AND CLEAN PROTECTIVE CLOTHING. IN CASE OF POISONING CALL PHYSICIAN SPECIFIC ANTI­ DOTES - ATROPINE AND PRALIDOXIME
3.2.1 In addinon to the above, the container shall also be marked with the symbol for danger of poisoning as specified in IS: 1260 ( Part I )-1973*.
3.2.2 Thc containers may also be marked with the lSI Certification Mark.
NOTE - The use or the lSI Certification Mark I~ governed by the provlStons of the Indian Standards Insutunon ( Cernficanon Mark... ) Act and the Rules and Regulauons made thereunder. The lSI Mark on products covered by an Indian Standard conveys tbe assurance that they have been produced to com pi}' with the requirements of that standard under a well-defined system of mspecuon, tc... nng and quality control which 15 devised and supervised by lSI and operated lJy the producer. lSI marked products arc also conunuouely checked by lSI for conformity to that standard as a further safeguard. Details of condmons under which a licence for the use of the IS] Ceruficauon Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution.
4. SAMPLING
4.1 Representative samples of the material shall be drawn according to the method prescribed in 'Indian Standard methods for sampling of pesti­ cide! and their formulations (und" preparatIon)'.
NOT.E - TJlJ such nme thrs standard IS published, the samples sbalJ be drawn as agreed to between the parties concerned
5. TESTS
5.1 Tests shall be carried out by the method. prescribed under col 4 and 5 of Table I.
5.2 Quality of Reagents - Unless specified otherwise, pure chemicals and distilled water ( see IS . 1070-1 960t ) shall be employed 10 tests
NOTE - • Pure chemicals' shall mean chemicals that do not contain ImpUfllle5 which affect the results of analysis
-PIctorial marking for handling and labelling of goods. Pact I Dangerous goods (fir" """011 ).
'tSpecificauon for water, drsulled quality (revued)
7
DETERMINATION OF PHORATE CONTENT
A~. PRINCIPLE
A~.I Phorate is hydrolysed in slightly aqueous acid in the presence of standard silver nitrate solution. The hydrolysis products consume two moles of silver The excess srlver is titrated with standard ammonium thiocyanate solution. A correction for the amount of standard silver nitrate solution consumed by impurities present before hydrolysis is applied. Total Sliver consumed grves a measure of the acuve ingredient content.
A." REAGENTS
A.I.I Acetooe
A,.t.2 Nitric: Acid - concentrated (Jee IS: 26-}-196B·).
A-I.3 Standard Silver Nitrate Solution - 0 I N, prepared by dissolvmg 17'5 g silver nitrate m I 000 ml of water, and standardized.
A-t.3.1 Standarduution of Standard Sliver NItrate Soluuon - PIpette or measure accurately, about 40 ml of silver nitrate solution, and add slowly, with contmuous surring, dilute hydrochlonc acid until preci­ prtation of the Sliver is complete. BOll the mixture cautiously for about 5 minutes; then, allow it to stand m the dark until the precipitate has settled and the supernatant Irquid has become clear. Transfer the preci­ pitate completely to a tared filtering crucible, and wash it WIth small poruons of water slightly acidified WIth mtnc acid Dry the precipitate at 110°C to constant mass. From the mass of the silver chlorrde obtained, calculate the normality of the srlver rutrate solution
A,.t.3.l.t Calculatwns
a) Normality of standard silver mtrate soluuon, N I = _mX 6'98 v
where m = mass m g of silver chloride, and v = volume in ml of silver rntrate solution consumed.
N b) Factor of normaluy, FI = 'OT
·Speclficanon or mULe acid (fint rIVinG" )
8
A-1.5 Ferric Nitrate Solation - 10 percent.
A-I.6 Standard Ammomnm Thiocyanate Solution - O' IN, prepared by dissolving 8 g of ammonium thiocyanate in I 000 ml of water, and -tandardized,
A-I.6.1 Standardizanon of AmmOnium Thiocyanate SolutIon-Measure accurately about 30 ml of standard silver nurate solution (A 1.3) into a glass.stoppered flask. Dilute with 50 ml of water, add 2 ml of nitric acid and 2 ml of ferric ammonium sulphate indicator and titrate with ammonium thiocyanate solution to the first appearance of a reddish-brown colour.
A-l.6.1.1 Calculations
where
o = volume in ml of SIlver nitrate solution, n = normality of standard silver nrtrate solution, and V =- volume in rnl of amrnoruurn thiocyanate solution
consumed.
A-I.7 Benzene
A-1.8 Standard Potassium Hydrazide Solution - 0'[ N, aqueous in 10 percent potassium nurate.
A-1.9 Congo Red Test Paper
.\-2. PROCEDURE
A-2.1 Weigh accurately a sample containmz ••bout 2'5 g of phorate into .. 250-ml volumetric flask. DIlute to the mark With acetone and mix.
A-2.1.1 Place 150 ml water, 5 drop, ot concentrated nitric ..cid and exactly 50 ml of standard silver nitrate solution into a 500-ml Erlenmeyer flask. Immerse in a water- bath rnaintamed at 50'C unnl a constant tempe­ rature is attained. PIpette 50 ml of diluted sample ( A-2.1 ) into the Erlen­ meyer flask. Swirl the flask while zddmg solution. Stopper and allow to remain in the 50'C water-bath for 15 minutes. Add 5 ml mtrobenzene, stopper tightly and shake vigorously for about I minute. Add I ml of ferne nitrate solution, shake for I minute and begin titrating with standard
9
II. '7976 - 1976
ammonium thiocyanate solution. As the end point is approached, the solution will assume a light salmon-pink colour. Stopper and shake vigoro­ usly, the salmon-pink colour will disappear. Add more standard ammonium thiocyanate solunon and shake again. Repeat this process until the colour is not completely discharged on shaking, but avoid adding of excess standard ammonium thiocyanate solution. When a little colour remains, remove this by the addition of a drop or two of standard silver nnrare solution. At this point, one addiuonal drop of standard ammonium thiocyanate solution should reproduce the faint salmon-pink colour, this indicates the end point.
"-2.2 Detel"DlinadOD or Imparities - Weigh accurately a quantity of sample containing 0'5 g of phoratc into a 250'ml separatory funnel contain­ ing 150 ml of benzene. Extract the benzene solution three times by shakmg each time with 50 ml of standard potassium hydroxide solution in 10 per· cent potassium nitrate, then once with 50 ml of water. Collect the aqueous layers in a 500'ml glass-stoppered Erlenmeyer flask. Neutralize the combi­ ned aqueous layers with nitric acid, using congo red paper. Add 5 drops of acid in excess, then add exactly 5 ml of standard silver nitrate solution. Add 5 ml of nitrobenzene and shake vigorously for about I minute, and continue titration as in A-2.1.
A-2.3 CalealatioD
A-2.3.1 Phorate content, percent by mass
_ [6'510 X ( V,F,) - (V,F2) J- [1'302 X (D,F,) - (DoFo)] M 1 i ....J.
where
I, _~ volume In m! ofstandard silver nitrate solution consumed,
FI = factor of normality of standard silver nitrate solution,
IT, = volume in ml of standard ammonium thiosulphate solu­ tion consumed,
F, = factor of normality of standard ammonium thiocyanate solution)
M, - mass in g 01 the material taken for the test (A-2.1), ", - volume in ml of standard silver nitrate solution eon­
sumed for determination of impurities (A-2.2), v. "" volume in ml of standard ammonium thiocyanate solu­
non consumed for determination of impurities (A-2.2). and
M l - mass in g of the material taken for determmation of impurities ( A-2.2 ).
10
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27 10 85
Text1: IS : 7976 - 1976 (Reaffirmed - 2012)