21
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-णSatyanarayan Gangaram Pitroda “Invent a New India Using Knowledge” प0रा1 को छोड न’ 5 तरफJawaharlal Nehru “Step Out From the Old to the New” जान1 का अ+धकार, जी1 का अ+धकारMazdoor Kisan Shakti Sangathan “The Right to Information, The Right to Live” !ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह Bharthari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 5280 (1969): Fenitrothion, Technical [FAD 1: Pesticides and Pesticides Residue Analysis]

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Page 1: IS 5280 (1969): Fenitrothion, Technical

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 5280 (1969): Fenitrothion, Technical [FAD 1: Pesticidesand Pesticides Residue Analysis]

Page 2: IS 5280 (1969): Fenitrothion, Technical
Page 3: IS 5280 (1969): Fenitrothion, Technical
Page 4: IS 5280 (1969): Fenitrothion, Technical

Cr4

IS : 6280 • 1989( Rellfftrmed1117 )

Indian StandardSPECIFICATION FOR

FENITROTHION, TECHNICAL

( Second ReprintFEBRUARY 2(01)

UDC,632.951 [FENITRonDON)

oCopyright 1969

BUREAU OF INDIAN ST.4.NDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARO

NEW DELHI 110002

December 1969

Page 5: IS 5280 (1969): Fenitrothion, Technical

18,5280.1.

Indian StandardSPECIFICATION FOR

FENITROTHION, TECHNICAL

Pest Control Sectional Committee, AFCDC 6

CluJimtaftDa SARDA-Ii. SINGH

&/Wun:tingDirectorate of Plant Protection, Quarantine It Stor..~

(Ministry of Food, Agriculture, CommunityDevelopment It Co-operation)

Ministry of Health, Family Planning. Workl, Houainl&. Urban Development

Central Forensic Science Laboratory, Central Bureauof Investigationa, New Delhi

I. C. I. (India) Private Ltd, Calcutta

Tata Fison Industries Limited, Bombay

DR B. B. BHATIADR N. K. BA-au ( AllmiaU ) .

M.&J-GBN M. S. BoPARAI t Directorate General of Armed Foreet MedicalServices, Ministry of Defence

SUIU A.. W. COtlRT 11

Shaw Wallace &. Company Limited, CalcuttaSHRI H. C. 80)148111[8 .. 8 ( AlI,mat' )

DIRBCToa OJ' AuIUCUI.TURE Department of Agriculture, Government or uttarPradesh

Da P. L. CHATURVJtUI (.Alt,t'fIat, ) tDIRECTOR or S'rORAOX & INSPJlio- Directorate of Storage &. Inspection (MiDi.tr~ of

TION Food, Agriculture, Community Development &Co-operation) I

MIm6trsSRIU M. L. ADVANI

DR K. KALYAN (AltmW')DR K. DAGORI

DB H. L. BAMI

DEPUTY DIRECTOR ( STORA08TICOHNICAL) ( AltnlttJu)

DUVG8 CONTROLLER Indian Pharmacope-ia Committee (MinistrY ofHealth, Family Planning, Works, Houlinl atUrban Development )

SHRI G. D. GOKHALIC BombayChemicals Private Ltd, BombaySURI V. V. KETKAR (Altnnatl)

DR R. GONl~ALVEI\ National Organic Chemical IndUitri. Limited,Bombay

DR S. B. D. AOABWALA ( Allmrat, )DRK. C. GULATI Indian Agricultural Research Institute, New DelhiSHRI T. GKOROB JOHN Hindustan Insecticidet Limited, New Delhi

Da S. N. NAG ( Altnnall )DR LALLAN RAt Cyanatnid India Limited, Bombay

SRRI M. K. ZU1'8HI (Altmaatl)

( Conti,.,d Drr /NJI' 2 )

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARO

NEW DELHI 110002

Page 6: IS 5280 (1969): Fenitrothion, Technical

IS15280.1969

(Co"tin..,d from /JaI' 1 )

InstituteResearchRlprulnting

Central Food Technological( CSIR )J Mysore

SlIRJ S. L. PATEL

:It..- M. MUTBt1 ( AltmulU)SuRl I.. P. MATHUR Ministry of Defence ( DGI )

~HRI K. P. SINGH ( Allma4l, )Dn P. R. M1'.lITA Pesticid...s Association of India, New DelhiSIHU T. S. M~~IlTA Bharat Pulverising ~fills Private Limited, Bombay

SHRI S. Cn ATTJ:KJI (AlI,matl)SURf 1). N. N.~KJ{ATE Bayer (India) Ltd. Bombay

D1& D. V. KA9HELIICA'R (Altlf"PUltl)SHIll R. NARASIMUAN Directorate Gt·neraJ of T ...chnical Development

( Ministry of Industrial Development & CompanyAffairs )

Amf'rican Spring & Pressing Work.. Private Ltd,Bombay

M",.b"sSHIH S. K. MAJUMDAr

Sn ur L. M. PATltI. ( .Alt"natl )PLAN'.r PHOTleCTI0N OJ'J'IOB:B Department of Agriculture. Government of MY80reDRS. PI.I.ADHAN Indian Agricultural Research Institute, New Delhi

nIt RATTAN tAL ( Altmta,,)SURl P. llAMDAs Central Warehousing Corporation. Ne-w DelhiDR A. SARUP Pest Control Corporation, CalcuttaSHIU A. K. SENRVPTA National Malaria Eradication Programme, DelhiDR V rNOll R. SHAH Pest Control ( India) Pvt l.td, BombayDn H. I). SlUVA8TAVA Indian Veterinary Research Institute, Izatnapr

f)1t R P. CUAUDHURI (Allmlau)DIt L. R. SUIl Mini'try of Defence ( R & I> )

SHIU S. K. MITRA (Alllmall)DJt B. L. WATTAr.. National Institute of Communicable Difl@ases, DelhiDR HABJ BttAGWAN, Director General, lSI (Ex-officio Mmb,,)

Deputy Director ( Agri at Food)

Sen,t.,)SHltl E. N. SUND.lR

Deputy Director (Alri &t Food), lSI

Pesticides Subcommittee, AFCDC 6: 1

Con...On P. R. l\iXHT4 P~.tif:id8AJlociation of India, New Delhi

MnnbnlSUIU M. L. Anv ANI Tata Filon Industries Ltd, Bombay

DB K. KALYA.M (.4IImt4I')A01UCtJLTUDAL CHEttU8T AND Agricultural College tit Rest-arch Institute, ClimootQre

A.80CIATB: PI\O•••OR 0 .. SOILSOI.NCB

SHIU V. J. 04)[R. Central Revenue. Control Laboratory, New DelhiSUIll N. K. CUOWDBt1Bl (Altmaal,)

( Gmt."".d on /JOlt 15)

Page 7: IS 5280 (1969): Fenitrothion, Technical

IS 15280-1969

&/I"smlin,Central Forensic Science Laboratory, Central Bureau

of Investigations, New DelhiI. C. 1. ( India) Private Ltd, Calcutta

H industan Insecticides Limited, New Delhi

( Conlinwd from /'GI' 2 )

Mfmb"sDR H. L. BAJlJ

DB K. D. PAUA.P.IA

Chemistry Department, Dolhl University, DelhiBharat Pulverising 1\1111s Pvt Ltd, Bombay

( Altnnau)Ministry of Defence ( R&D)Directorate General of Technical Development

(Ministry of Industrial Development, InternalTrade & Company Affair.)

Directorate of Plant Protection, Quarantine &. Storage(Ministry of Food, Agriculture. CommunityDevelopment s. Co-operation )

Da R. S. RAIAGOPALA.N Agromore Limited, BangaloreDR V. SAJ)ASIVAN Bombay Municipal Corporation, BombayDB P. R. SARMA f~. l. I). - Parry Limited, Madras .DR VINOD R. SHAH Pest Control ( India) Private Ltd, Bombay ,SSK) R. D, SKROJ'.F Excel Industries Limited, Bombay :

SaRI K. K. CUBAY A ( .41lma1JU )DR B. L. WATTAI.. National Institute of Communicable Diseasea,~Delhi

8Hftl V. N. BHATNAQAR ( Altlrnal.)

DBB. B. BU&TIADB N. K. BA8U ( Altmaatl )

DR. S. L. CHOPRA Punjab Agricultural Univenity, LudhianaSiun M. S. DHATT National Malaria Eradication Programme, DelhiSURI G. D. GOKHALB Bombay Chemicals Private Ltd, Bombay

SURI V. V. KETJtAl\ ( AI'mud, )DRR. GONCALVU National Organic Chemical I ndustries Limited,

BombayDR S. lJ.. D. AOARWALA (Alttrnale)

DR K. C. GUI.A'l'! Indian Agricultural Research Institute, New DelhiDR H.•S. DEWAN ( Alllrnal, )

Snnt 1'. G~ onoa JOHN

Dn S. N. NAtJ (Alllrnatl;DR K. B. I•. MA'rHuRSURI T. S. MB:ll'rA

SUR! S. CflATTF.KJlSUIU D. P. l\~lT1tA

SURI R. NARA.8IMllAM

15

Page 8: IS 5280 (1969): Fenitrothion, Technical

AMEND\1ENT NO. 1 APRll~ 1989TO

IS : 5280 - 1969 SPECIFICATION FORFENITROTHION, TECHNICAL

( Page 4t clause 2.2, Table 1. Sf No. (v), col 2 and 3 ) - 'Substitute-27C'/27"'C' for '25°(' and '1·,310 - )"320'for '1"32'.

t Page 9 and II ) - Substuute '27)Ct for '2511(" wherever It occurs.

1

( AFCDC 6)

---- -----~---r--

Pnnred d' New IncJlJ l'II11IIUJ;. I'IC" "'lIUld I.d".

Page 9: IS 5280 (1969): Fenitrothion, Technical

IS.5280·1969

Indian StandardSPECIFICATION FOR

FENITROTHION, TECHNICAL

o. FOR E W 0 R D

0.1 This Indian Standard was adopted by the Indian Standards Institutionon 26 September 1969, after the draft finalized by the Pest Control SectionalCommittee had been approved by the Agricultural and Food ProductsDivision Council and the Chemical Division Council.

0.2 Fenitrothion, technical, is employed in the preparation of insecticidalformulations used for the control of pests of agricultural and public healthimportance, '

0.2.1 Fenitrothion is tlie common name accepted by the InternationalOrganization for Standardization for the pesticide chemical containingOO-dimethyl 0-( 3-methyl-4-nitrophenyl) phosphorothioate (sle Note) asits active ingredient. The empirical and structural forrnulee and themolecular weight of the compound are as indicated below:

277-24

Molecular H'eighiStructural FOr"'UIaEmpir;,al Formula

CHI°tP 0-\ ( N02

CHI 0 \IS CH)

NOTE - The other chemical name accerted by the International Organization forStandardization for this pesticide isdimethy 3-methyl.4-nltrophenyl phOlphorothionate.

0.3 Taking into consideration the views of producers, consumers. testingauthorities and technologists, the Sectional Committee responsible for thepreparation of this standard felt that it should be related to the manufactur­ing and trade practices followed in the country in this field.

0.4 This standard is one of a series of Indian Standards on pesticides andtheir formulations.

0.5 This standard contains clause! E-2.S and £.3.4 which can for an agree­ment between the purchaser and the vendor.

3

Page 10: IS 5280 (1969): Fenitrothion, Technical

11,,,.1_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- t960·. 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 of testfor fenitrothion, technical, employed in the preparation of insecticidalformulations.

2. REQ,UlREMENTS

2.1 Dnerlpdoa-The material shall be amber coloured, slightly oilyliquid, free from extraneous impurities or modifying agents and it shall beinsoluble in water.

2.2 The materlal shal! comply with the requirements given in Table 1.

TABLE 1 REQUIREMENTS fOR FENITROTHlON, TECHNICAL

SL CHARACTERISTIC REQUIREMENT METJlOU 0,. TaT,No. Rltl' '1'0,... ---_A_----.

Appendix IndianStandard

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

i) Ac:~iYf: iOlredieilt ( su 0.2.1 ), 95 Apercent by weight, Min

ii) Material insoluble in acetone. 05 Bpercent by weilht, MtJJt

iii) Moilture content, percent by 0·5 IS: 2362-weicht, Max 1963-

iv) Acidity .1 (RaSa.). pearcent o·~ Cbyweilht, M_

v) Specific ....vity at 25°C 1'32 D

.Method Cor the d~t...min.tion of water by the Karl Filcher method.

3. PACKING AND MARKING

3.1 P.~-The material shall be packed in mild steel containers linedwith phthalllc, phenolic or epoxy resins. For retail packs, galvanized tincontaIners lined with phthallic, phenolic or epoxy resins shall be used .

• Rulel for rounding off numerical valu8 ( ,evi,. ).

Page 11: IS 5280 (1969): Fenitrothion, Technical

IS .5280 ·1969

3.2 Marldal-The containers shall be leCW'ely closed and shall bearlegibly and indelibly the following information:

a) Name of the material;b) Name of the manufacturer;c) Date of manufacture;d) Batch number;e) Net weight of contents;f) Active ingredient content; andg) The minimum cautionary notice worded as under:

'HIGHLY POISONOUS. HANDLE WI'fH CARE. KEEPAWAY FROM FOODSTUFFS AND ANIMAL :FEEDS. DONOT TOUCH OR INHALE THE CONTENTS. WHILEHANDLING THE CONTENTS, USE RUBBER GLOVES ANDFACE MASK. USE OF EMPTY CONTAINERS DAN­GEROUS. IN C~E OF POISONING, CALL A PHYSICIAN.ATROPINE AN~-J..<?XYGEN ARE USEFUL IN 'rREATMENT.AVOID SKIN C~,.TACT.'

B.2.! The product may al80 be Rl.rked witb Standard mark.r

p.2.LI The use of the Stan'ard Mark is governed by tbe provisions of tbeBureau 01Indian Standards Act, 1986 and the Rules Ind Regulations m,dethereunder. The details of conditions under which the licence for the us~ ofStandard Mark may be granted to maauCactureas or producers may be obtaiileelfrom tbe Bureau of Indian SlIndards. ·

~ SAMPLING

4.1 The method of drawing representative samples of the material and thecriteria for conformity shall be as prescribed in Appendix E.

5. TESTS

5.1 "rests shall be carried out as prescribed in the appropriate appendicesgiven in col 4 and 5 of Table 1.

5.2 Q,aality ofa.....t. - Unless specified otherwise, pure chemicals anddistilled water (sle IS: 1070-1960·) shall be employed in tests.

NOTE - C Pure Chemicals t sball mean chemicals that do not contain impurities whichafrflCt the reeult. of analysd.

*Speclfication for water, distilled quality ( "vis,d ).

5

Page 12: IS 5280 (1969): Fenitrothion, Technical

IS: 5280·1969

APPENDIX A[ Table 1~ Item (i)]

DETERMINATION OF OO-DIMETHYLD-(3-METHYIA-NlTROPHENYL) PHOSPHOROTIDOATE

A-I. PRINCIPLE OF METHOD

A-1.1 The sample is dissolved in ether and the most likely impurity, 4-nitro­m-cresol. is extracted with mild alkali. The ether layer is treated withzinc and an acetic acid- hydrochloric acid mixture, and the amino groupsare ,titrated with standard sodium nitrite solution.

A-2. REAGENTS

A-2.1 Acetic AdcI.Hyclroeh1oric Acid Mixture - Mix 9 volumes ofglacial acetic acid with one volume of concentrated hydrochloric acid.

A.2.2 Staaclard SodIum Nitrite SoladoD-O') M, standardized againstaulphanilic acid. Dissolve 6·90 g of sodium nitrite in distilled water andmake up to one litre with distilled water. Standardize as follows:

. Weigh accurately 0·40·0·45 g of anhydrous sulphanilic acid(analytical grade) into a 400-mJ tall-form beaker. Add 80 m1 ofdistilled water) 10 ml of concentrated hydrochloric acid, SO ml ofglacial acetic acid and 5 g of sodium (or potassium) bromide. Coolthe mixture to 0°·10°0 by the addition of clean, shaved ice and stirmechanically. Titrate at O°·IO°C with the 0'1 M sodium nitrite asrapidly as the spot test permits. Near the end-point, add the sodiumnitrite in four-drop portions.

N 1· ro 1M d" ". ax5'774arma uy o· so tum nitrite = b

where

/I =- weight (in g) of sulphanilic acid used, and

II- volume (in ml) of 0'1 M sodium nitrite required.

"'-S.PROCBDUUA-3.1~.. af Free 4-Nitro-...cre8ol- Weigh accurately about1 I of the ample and transfer the same in a 200-ml separating funnelcontainilll 100 ml of ether. Extract the ether 101ULion four timeswith 20 ml portions of chilled 1 percent (w/v) sodium carbonate solutionand discard the aqueous layers. The t'..xtraction should be done as quicklyal possible to prevent decomposition of the active ingredient.

6

Page 13: IS 5280 (1969): Fenitrothion, Technical

ISa5280-19&t

A-3.2 Detenabaadoa 01 OO-Dlmetlayl 0-( 3-Metlayl-4--Nltropheayl )p......orotbloat. Ia Ether Layer - Transfer the ether layer quanti­tatively to a 400-ml beaker. using small portions of ether. Add 100 ml ofthe acetic acid-hydrochloric acid mixture and 10 g of iron-free zinc dust.Cover the beaker with a watch-glass and heat gently on a steam-bath untilmost of the ether has evaporated and the solution is colourless. Add 25 mlof concentrated hydrochloric acid and 75 ml of distilled water to completethe solution of the zinc dust. Cool, wash down the beaker and watch-glasswith distilled water, and add five grams of sodium (or potassium)bromide. Cool the mixture to 0°·10°0 by the addition of clean, shavedice and stir mechanically. Titrate at 0°·10°0 with the standardized 0'1 Msodium nitrite as rapidly as the spot test permits. Near the end-point, addthe sodium nitrite in four-drop portions.

A-,.3 Spot Tnt - Dip a glass rod into the solution to be tested and thentouch the rod quickly to a piece of potassium iodide/starch paper. Theend-point is reached when an intense blue-black colour appears immediate­ly and may be obtained repeatedly during a one-minute period withoutfurther addition of sodium aitrite.

A-t. CALCULATION

A-t.l OO-dimethy! 0-( g-mtthyl.4-nitrophenyl) 27-72 WNfpbosphorothioate content, percent by weight -=---­

w

whereW - volume (in ml) of 0'1 M sodium nitrite required;N = normality of 0'1 M sodium nitrite;

f = correction factor~ ; and

w -= weight (in g) of sample;

whereT = quantity (in ml) of 0-1 M sodium nitrite calculated for the

nitro-group determination of one gram of a mono-nitroreference material, and

.A .. quantity (in ml) of 0'1 M sodium nitrite used in thenitro-group determination of one gram of a recrystallized.mple of the same substance, following the method de..cribed above and ulioS the lame reagentl.

The correction factor f is intended to allow for errors due to impuritiesin the reagentl. as well al those inherent in the method itself or in itsapplication by • given laboratory. It. value shall lie within the range0-98 to 1-02.

7

Page 14: IS 5280 (1969): Fenitrothion, Technical

18 .5218.1969

APPENDIX B[ T abl« 1, Item (ii) ]

DETERMINATION OF MATERIAL INSOLUBLE IN ACETONE

B-1. REAGENT8-1.1 Aeetoae

B-2. PROCEDURE8-2.1 Weigh 10 g of the material into a clean and dry 25().ml Erlenmeyerflask fitted with a ground-glass joint. Add 150 ml of dry acetone andwarm under reflux until all soluble material is dissolved. Filter the solutionusing a tared Gooch or sintered glass crucible of porosity No.3, and washwell with more solvent. Dry at 110°C for 30 minutes) coolJ and weigh.

B-3. CALCULAnON8-3.1 Matter insoluble in acetone, 100w

percent by weight = ---wwhere

w := weight in g of the residue obtained after drying) andW == weight in g of the material taken for the test.

APPENDIX C[Table 1, Item (iv) ]

DETERMINATION OF AOIDITY

o-r, REAGENTS

0.1.1 AeetoDe(J.J.2 Methyl Red IacUcator SolutiOIl- aqueous, one percent (WIll).C.l.3 Staad.nI Sodlam Ryclrodcle SoladoD-O·02 N.(:.1.4 StuMlani HyVoehlorie Aeld-0402 N.

c..2.PROCEDVRE04.1 Weigh accurately about 10 g of the material and dissolve it in 25 mlof acetone. Solution may beeffected by gently warming if necessary, Add75 ml of water and titrate immediately with the standard sodium hydroxidesolution using methyl red as the indicator.

C4.2 Carry out a blank determination using 25 ml of acetone and 75 mlof water.

8

Page 15: IS 5280 (1969): Fenitrothion, Technical

ca CALCULAnONc.3.1 Acidity (as HI~O,), 4-9 (V - v) N

percent by weight == W

whereV .. volume in ml of the standard sodium hydroxide solution

required for the test with the material,v == volume in ml of the standard sodium hydroxide solution

required for the blank determination,N = normality of the standard sodium hydroxide solution, andW = weight in g of the material taken for the test.

C-3.1.1 In case the blank determination shows an alkaline reaction,neutralize it with the standard hydrochloric acid and calculate the acidityas follows:

Acidity (as HIS,?,). 4-9 (VoM +vN: )percent by weight = ~.

whereV = volume i1\ ml of the standard sodium hydroxide solution

required f~r the test with the material,Nl == normality of the standard sodium hydroxide solution,

v .. volume in ml of the standard hydrochloric acid required forthe blank determination, t

NI = normality of the standard hydrochloric acid, andJi' =- weight in g of the material taken for the test.

APPENDIX D[ T able I, Item (v) ]

DETERMINATION OF SPECIFIC GRAVITY

0.1. TERMINOLOGY1).1.1 For the purpose of this standard, the specific gravity of the materialshall be the ratio of the weight in air of a given volume of the materialat 2!)OC to that of an equal volume of water at the same temperature.

D-2. METHOD1).2.1 The specific gravity shall be determined with a specific gravitybottle - Castell Evans modification with ground-in stopper and ground-oncap (Stl Fig. 1) or with a pyknometer tube of the Perkin's type (ste Fig. 2).

9

Page 16: IS 5280 (1969): Fenitrothion, Technical

11.5280·1_

Flo. 1 SPECIFIC GRAvrrY BonLB (CAsTELL EVANS MODIFIOATIONwrrH GROUND-IN STOPPEll AND GROUND-ON CAP)

Flo. 2 PYKNOMETER TuBE (haKIN'S TYPa)

10

Page 17: IS 5280 (1969): Fenitrothion, Technical

IS 15280·1969

0-3.paOCEDURE0-3.1 Weigh the clean and dry specific gravity bottle or pyknometer of25-ml capacity. Fill the tared specific gravity bottle or pyknometer withfreshly boiled water and place it in a bath maintained at 25°:1: 1°C andallow sufficient time to attain the temperature of the bath. Then insert theground-in stopper which has also been brought to 25° :I: 1°0. Wipe theexcess liquid from the stopper and place the cap in position on it. Removethe specific gravity bottle or the pyknometer from the bath, bring to roomtemperature and weigh. Empty the specific gravity bottle or the pykno­meter, clean and dry it, and repeat the operation with the material at250 ::1: i-c.D-t. CALCULATION AND REPORT

D-f.l Specify the temperature of testing in the report.

D-t.2 The specific gravity is calculated by the following formula:

Specific gravity at 25°/25°C = i _~where ~F

C - weight in , of the specific gravity bottle or pyknometer filledwith the naterial at 25°0, I

A = weight in I' of the dry specific gravity bottle or pyknotieter.md t

B = weight in S of the specific gravity bottle or pyknometeriilledwith water at 25°C. ~

APPENDIX E(Clause 4.1 )

SAMPLING OF FENlTROTIDON, TECHNICAL

B-1. GENERAL PRECAUTIONS

£-1.0 In drawing, preparing, storing, and handling test samples, thefollowing precautions and directions shall beobserved.

B-l.1 Samples shall not be taken in an exposed place.

£.1.2 The sampling instrument shall be clean and dry when used.

11

Page 18: IS 5280 (1969): Fenitrothion, Technical

18.5280;,1969

&1.3 Proper precautions shall be taken while drawing samples .inee therna terial is poisonous.

£-1.4 Precautions shall be taken to protect the samples, the material beingsampled, the sampling instrument and the receptacles for samples fromadventitious contamination.

£.1.5 The samples shall be placed in suitable, clean, dry and air-tightsample receptacles.

&.1.6 The sample receptacles shall be ef such a size that they are almost,but not completely, filled by the sample.

1',.1.7 Each sample receptacle shall be sealed air-tight after filling andmarked with full details of sampling, the date of manufacture, name of themanufacturer and other particulars of the consignment.

£-1.8 Samples shall be stored in such a manner that the temperature ofthe material does not vary unduly from the normal temperature.

£-2. SCALE or SAMPLING

&2.1 Lot - All the containers in a single consignment of the materialdrawn from the same batch of manufacture shall constitute a lot. If aconsignment is declared or known to consist of different batches of manu­facture, the containers belonging to the same batch shall be groupedtogether and each such group .hall constitute a separate lot.

£-2.1.1 Samples shall be tested for each lot for ascertaining the con­Connity of the material to the requirements of this specification.

£.2.2 The number of containers to be selected from the lot shall depend onthe size of the lot and shall be in accordance wjth col 1 and 2 of Table 2.

TABLE 2 NUMBER OF CONTAINERS TO 88 SELECTEDPO. SAMPLING

( CJIJUIII &.2.2.E-2.3. B.S.1 .d £-3.3 )

LoT 81Z8

N(1)

3 to 1516 n 4041., 65

66 " 110<?ver 110

12

No. 01' CONTAIN!:" TOBZ SIC£BCr.D

II

(2)

s•57

10

Page 19: IS 5280 (1969): Fenitrothion, Technical

IS 15280 .1969

B-2.3 These containers shall be selected at random from the lot. Toensure the randomness of selection, a random number table as agreed tobetween the purchaser and the supplier, shall be used. In case such a tableis not available, the following procedure shall be adopted:

Starting from any container in the lot, count thern as 1,2,3, up to ,and 10 on, in one order, where r is equal to the integral part of thevalue of Nln; N being the total number of containers in the lot and nthe number of containers to be selected (see Table 2). Every rthcontainer thus counted shall be separated until the requisite numberof containers is obtained from the lot to give samples for test.

:&-3. TEST SAMPLES AND REFEREE SAMPLES

:&-3.1 Before drawing the test sample, mix thoroughly the contents of eachcontainer selected, by shaking or by any other suitable means so as to bringall portions into uniform distribution. Draw small portions of the materialfrom different parts of each container selected (Jee Table 2). The totalquantity of the material drawn from each container shall be not less than300 g.

£-3.2 Mix thoroughly all the material drawn from the same container. Asmall but equal quantity shall be taken from each selected container andshall be well mixed together so as to form a sample of not less than 250 g.This sample shall be divided into three equal composite test samples, onefor the purchaser, another for the supplier, and the third for the referee,

£.3.3 The remaining material drawn from a container (after the qJ,ntityneeded for the formation of the composite test samples has been takc~1.out)slid-a L~ divided iuto ihree e"lual pdttb. 'rl.l'&\. 1.J&J., ts shall be iu.r.ie atclytransferred separately to thoroughly dried sample receptacles whic arethen sealed air-tight, and labelled with all the particulars of sampling givenunder E-l.7. The material in each such sealed sample receptacle shallconstitute an individual test sample. These individual test samples shallbe separated into three identical sets of individual test samples in such away that each set has a sample representing each container selected (seeTable 2). One of these three sets shall be marked for the purchaser,another for the supplier and the third for the referee.

&-3.4 Referee Sample. - Referee samples shall consist of one of thecomposite test samples (Jet &.3.2) and a set of individual test samples(set :&-3.3) for this purpost', and shall bear the seals of the purchaser andthe supplier. These shall be kept at a place agreed to between the two.

E-4. TESTING OF SAMPLES

E-4.0 The number of tests mentioned in E-4.1 and E-4.2 shall be first con­ducted on the test samples marked for the purchaser. In contingencies,

l~

Page 20: IS 5280 (1969): Fenitrothion, Technical

11.'.-1969such as loss, spoilage, or spilling, of the purchaser's test samples or if thesupplier so desires, the test samples marked for the supplier may be tested.In case of a dispute, the referee test samples shall be tested and the testresults obtained on the referee lest samples shall be considered al final.

&-4.1 Tests for description (SII 2.1 ) and determination of active ingredientcontent shall be conducted on each of the individual test samples.

£-4.2 Tests for the determination of the remaining characteristics, namely,water content, acidityt material insoluble in acetone, and specific gravityshall be conducted on the composite test sample as prepared under :&.3.2.

£-5. CRITERIA FOR CONFORMITY

:B.S.1 A lot shall be declared as conforming to the specification, when:a) each of the individual test samples satisfies the requirement speci­

fied in 2.1;b) Each of the test results for active ingredient content satisfies the

requirements specified in Table 1. If, however, one or more of thetest results does not satisfy the specified requirement, the conformityof the lot shall be ascertained in accordance with £-5.1.1; and

c) the test results on the composite test sample satisfy the corres­ponding requirements given in Table 1.

£-5.1.1 In case one or more of the test results does not satisfy the require­ment for active ingredient content, the following procedure shall be adoptedfor conformity of the material in respect of this characteristic, The meanand the range of the corresponding test results shall be calculated as:

M (X) Sum of test resultsean ~ Number of test results

Range (R) == Difference between the highest and the lowest valuesobtained for the test results.

The appropriate expression as shown in col 5 of Table 3 shall be cal­culated. If the value of this expression satisfies the relevant condition a,given in col 5 of Table 3, the lot shall be declared to have satisfied therequirement for active ingredient content.

TABLE J CRITERION 'OR CONFORMITY

CUARAOTB.U8TIC

(1)

Active in8~jent

content, pe-rcentby weight

TS8T RuuLTa

(2)

14

(3)

Y

RANG. CR1TBRION I'ORCONI'ORMITY

(4) (5)

R (1"- 0·6 R) ;;. 95-0

Page 21: IS 5280 (1969): Fenitrothion, Technical

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