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  • Disclosure to Promote the Right To Information

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    इंटरनेट मानक

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    “Step Out From the Old to the New”

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    “Knowledge is such a treasure which cannot be stolen”

    “Invent a New India Using Knowledge”

    है”ह”ह

    IS 4324 (1967): Endosulfan Water Dispersible PowderConcentrates [FAD 1: Pesticides and Pesticides ResidueAnalysis]

  • IS : 4324 - 1967( Reaffirmed 2007 )

    Indian StandardSPECIFICATION 1~~OR ENDOStJLI~AN

    WArER fJISPERSIBLE P()WDER CONCENTRATES

    Tlllrd Repnnt FEBRUARY 2008

    ( Incorporating Amendment No~ 1 to ~ and IncludingAmendment No,", " & 5 )

    UDe 612 95 Endosulfan

    (() Copynght 1987

    BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

    NEW DELHI 110002

    Gr5 January )968

  • IS : 43%4 • 1'67

    Indian StandardSPECIFICATION FOR ENDOSULFAN

    WATER DISPERSIBLE POWDER CONCENTRATES

    Pest Control Sectional Committee, AFCDC 6

    Chairman

    DR SAIlDAIl SINOH

    Repre,enting

    Directorate of Plant Protection} Quarantine &Storage (Ministry of Food, Agriculture,Community Development & Co-operation)

    Central Food TechnoJo,ical Research IDltitute( CSIR), Mysore

    SHIll M. MurHU ( Alternate)

    SHal T. OBORGI JOHNDR. S. N. NAG ( Altlrnal,)

    SHIU S. K. MAJUMDaR.

    SHIll S. K. BORKAIl

    Directorate General of Armed Forces MedicalServices ( Ministry of Defence)

    Indian Pharmacopoeia Committee ( Miaistry orHealth & Family PJanning )

    DRP. N. CHATTERJEE Forest Research Institute &: Colleges, DebraDunSHRI A. W. COURT Shaw Wallace & Company Limited, Calcutta

    SUIlI H. C. SoMAIBKHAIt ( Alternate)DJllECTOR. 0' AOIlICULTURE Department of Aariculture. Government of

    Uttar PradeshDR P. L. CHATURV£DI ( Alternar« )

    DIRECTOR 0' RESEARCH, CSNTRAL Coffee Board, BanlaloreCOP'!I! RESEARCH INSTITtrrE,BALBHONNUR.

    SHRt S. C. GHOSB Ministry of Defence ( 001 )SHRI O. D. OOKHALI Bombay Chemicals Private Ltd, Bombay

    SaRI V. V. KETKAR (A/lernale )DR R. GONCALVES National Or.aDic Chemical Industries Ltd.

    BombayDil s. B. D. AOAIlWALA ( Alttrllal. )

    Oil K.C. GULATI Indian Aaricultural Research Institute, NewDelhi

    Hindustan Insecticides Limited, New Delhi

    Member,

    SHill M. L. ADVANI Tata Piaon Industries Limited, BombaySHIU G. J. MEDLEY ( Alternate)

    DR. P. N. AOARWAL Ministry of Defence ( R cl D )DR H. L. BAMI Central Drugs Laboratory, CalcuttaDRB. B. BHATIA I.C.I. ( India) Private Limited, Calcutta

    DR N. K. BASU ( Altemat« )MAJ-GBN M. S. BOPARAI

    ( Contlnu,d 011 INIII 2 )

    BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAPAR MARO

    NEW DBUB 110002

  • IS : 4314• 1967

    ( Continued from page 1 ),.,embers Representing

    D1l P R. MEHTA Pesticides Associauon of India, New DelhiSHRI T. S. MEHTA Bharat Pulverising Mills Prtvate Ltd, Bombay

    SHRI S. CHAlTERJI ( Alternate )DRK K MITRA Tea Board, Calcutta

    SHRI K N CHOWDHURY ( Alternate)SHRl R. NARASIMHAN Diectorate General of Technical Development

    ( MInistry of Industry & Supply)SHill S L. PATEL American Spring &: Pressmg Works Private Ltd.

    BombaySHRI L M. PATBL ( Alternate)

    DR S. V. PINOALE DIrectorate of Storage & Inspection (Mlnlc;(ryof Food, Agriculture, Community Develop-ment & Co-operation )

    Pest Control Corporation, Calcutta

    ( AariDR. HARI BHAGWAN,

    Deputy DirectorFood'

    DEPUTY DIRECTOR ( STORAGETECHNICAL ( Alternate )

    PLANT PROTfCTION OFfICER. Department of Agriculture. Government ofMysore

    Indian Agricultural Research Instrtute, NewDelhI

    DR 1 M PURl Cyanamid India Limited. BombayDR LALLAN RAt ( Alt.,,,QI. )

    DR A. SAllUPSHJU A. S. GOEL ( Alternate)

    DR H 0 SRIVASTAVA Indian Vetennary Research Institute. JzatnagarDR R. P. CHAUDHURI (Alternate)

    SHRI M K SUBRA RAO Bayer ( India) Limited. BombayDR V. K SUBRAHMANYAM Ministry of Health & Family PlanningSHIU P. M. THOMAS Central Warehousing Corporation, New Delhi

    SHRI P R AMOAS (AllerllQt,)Da B. L. WATTAL National Institute of Communicable Diseases,

    DeIhlDirector General, lSI (Ex-officIo Member)

    DR. S. PItADHAN

    SecretarySHKI E. N. SUNDAR

    Deputy Director ( Agn & Food ), lSI

    Pesticides Subcommittee, AFCDC 6 : 1

    ConvenerDR P. R. MEHTA Pesticides ASloclation of India, New Delhi

    Memberl

    SHill M. L ADVANI Tata Pilon Industries Limited, BombaySHRI G. J. MEDLEY ( AIII,,,ale )

    DR H L. BAMI Central DruS' Laboratory, CalcuttaDIl B. B. BHATIA r.c.r. ( India) Private Limited, CalcuttaDR. S. L. CHOPR.A Punjab A.ricutural Univer$ity. Ludbiana

    ( ContlnlWd onpall 18 )

    2

  • IS : ~324 - 1967

    ( Conllnll~d from pal' 2 )

    Memb,rJ R,prtJt'ntl",SHill G. D. GOkHAlE Bombay ChemicalsPrivate Ltd, Bombay

    SHRI V. V. KETKAR ( AJte'1IQtl )DR R. GONCALVFS National Organic Chemical industries Ltd.

    BombayDR S. B. D. AOARWAlA (Alll'fnalt)

    DR K. C. GULATI Indian AariculturaJ Research Institute, NewDelhi

    Hindustan Insectides Limited, New Delhi

    SHIll S. L. PERTIREPRESENTATIVIREPRESENTATIVEDR P. R. SARMASHal C. C. SHROFFDR B. L. WATTAL

    DR R. S. DEWAN ( Alternate )SHRI T. GEORGE JOHN

    DR S. N. NAG ( Altemat« )SHal T. S. MEHTA Bharat Pulverisiol Mills Private Ltd. Bombay

    SHRI S. CHATTERJI ( Alternate )DIl K. D. PAHAIUA Directorate of Plant Protection, Quarantine"

    Storlie (Ministry of Food, AaricuJture,Community Development & Co-operation)

    Ministry of Defence ( R &; D )Alricultural Department, Government of MadrasChemistry Department, Delhi University. DelhiE.I.D. - Parry Limited. MadrasExcel Industries Ltd t BombayNational In.thule of Communicable Dil.ases.

    Delhi

    18

  • AMENDMENT NO.4 ocrOBER 1988TO

    IS I 4324 • 1967 SPECIFICATION 'ORENDOSULFAN WATER DISPERSIBLE POWDER

    CONCENTRATES

    (Page 4, Table 1) - Add the following note at the end of theTable:

    , NOT. - The material shall not be subjected to accelerated .torage treatmentif it bu crossed balr of itt ahelf life a, ascertained from itl date of manufacture anddate or expiry declared 00 the container.'

    (AFCDC 6)

    Pnntcd lit Power Pnnte: '. Nc\' Deihl

  • AMENDMENT NO.5 MAY 1994TO

    IS 4324: 1967 SPECIFICATION FOR ENDOSULFANWATER DISPERSIBLE POWDER CONCENTRATES

    ( Pa~e 4 Table t ):

    a) 51 No. (ii), (,01" }-) - Delete the words 'after accelerated storctgt.".

    h) SI No. (iii), col _

    ( Paue 51 clause 4.1 ) - Substitute the following tor the existing:

    'When freshly manufactured material in bulk quantity is offered for inspection,representative samples of the material shall be drawn and tested as prescribed inIS 10627 : ItJ83 within 40 days of its manufacture. When the material i'\ offeredfor inspection after YO days of its manufacture. sampling shall he done asprescribed in IS ]On:!7 : 1983. However, the criteria tor conformity of thematerial \\ hen tested, shall be the limits of tolerances, as applicable over thedeclared nominal value and given under clause 2.2.1 of the standard.'

    ( FAD 1 )

    Punted at Power Printers. N~\\ Delhi

  • IS : 4324 - 1967

    Indian StandardSPECIFICATION FOR ENDOSULFAN

    WATER DISPERSIBLE POWDER CONCENTRATES

    o. FORE WORD0.1 This Indian Standard was adopted by the Indian Standards Insti-tution on 31 October 1967J 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 Endosulfan water dispersible powder concentrates containing vary-ing percentages of endosulfan, technical, are largely used in the controlof pests of agricultural importance.

    0.3 Taking into consideration the views of producers, consumers,testing authorities and technologists, the Sectional Committee respon-sible for the preparation of this standard felt that it should be relatedto the manufacturing and trade practices followed in the country in thisfield.

    0.4 This standard is one of a series of Indian Standards on pesticidesand their formulations.

    0.5 This standard contains clauses 3.1, E..2.3 and E-3.4 which can foran agreement between the purchaser and the vendor.

    0.6 For the purpose of deciding whether a particular requirement ofthis standard is complied with, the final value, observed or calculated,expressing the result of a test or analysis, shall be rounded off in accor-dance with IS: 2-1960*. The number of significant places retained inthe rounded off value should be the same as that of the specified valuein this standard.

    1. SCOPE1.1 This standard prescribes the requirements and the methods of testfor endosulfan water dispersible powder concentrates containing varyingpercentages of endosulfan, technical.

    NOTE - Endosulfan is the accepted common name for this pesticide by theInternational Oraanization for Standardization, ISO.

    -Rules for roundina off numerical values ( revised).

    3

  • IS : 4324- 1967

    B

    c

    D

    1-0

    so

    (3)Nominal value as

    declared OD thecontainer withappropriate tol·erance ( lee2.2.1 )

    97

    SLNo.(1) (2)i) EndosuJfan content, percent by

    weilbt .

    ii) Slevina requirement. materialpalsing through 7S·micronIS Sieve-, after acceleratedstorase, percent by weight.Min

    iii) Suspensibility after acceleratedstoraae, percent by weilht.Min

    iv) Acidity ( as HCL ). percent byweiaht, Max

    ORAlkalinity (as Nal CO. ),

    percent by weilht. MQ~ .·See IS : 460-1962 • Specification for test sieves ( ,ev/ltd) '. BS Sieve 200,

    ASTM Sieve 200 and Tyler Sieve 100 have their apert urea within the limits speci.fied for the above IS Telt Sieveaad. tberefore, may be used in place of 7'·microDIS Sieve.

    :2. REQUIREMENTS2.1 Description - The material shall be in the form of powder and shallwet readily on mixing with water providing a suspension suitable foruse as a spray.

    2.t.l Endosulfan, technical, employed in the manufacture of thematerial, shall conform to IS : 4344-1967*.2.2 The material shall comply with the requirements given in Table 1.

    TABLE 1 REQUIREMENTS FOR ENDOSULFAN WATERDISPERSrBLE POWDER CONCENTRATES

    CHARACTERISTIC REQUIREMENT METHOD OF TEST( REF TO ApPENDIX)

    (4)A

    -2.1.1 Endosulfan Content- Whendetermined by the method prescribedin Appendix A, the observed endoeulfan content. percent by mass, ofany of the samples shall not differ from the declared nominal value bymore than the tolerance limit. indicated below:

    Nominal Valu« Tolerance LimitPercent

    Up to 910and below SOSO and above

    + 10S

    ± S+ ~

    3

    percent of thenominal value

    ·Speciftcatlon for eDdOlulfaD, t.cbnioal.4

  • IS : 4324- 1967

    2.2.1.1 The actual value of endosulfan content shall be calculatedto the second decimal place and then rounded off to the first decimalplace before applying the tolerances as stipulated in 2.2.1,

    3. PACKING AND MARKING

    3.1 Packlna - The material shall be packed in clean and dry containersmade of tinplate, fibreboard or cardboard, with polyethylene liner asagreed to between the purchaser and the vendor.

    3.2 Mlrklng - The containers shall be securely closed and shall bearlegibly and indelibly the following .informaticn:

    a) Name of the material;

    b) Name of the manufacturer;

    c) Date of manufacture;

    d) Batch number;

    e) Net weight of the contents;f) Nominal content of endosulfan, technical, percent by weight;

    and '

    g) The minimum cautionary notice worded as under:6 KEEP WELL AWAY FROM FOODSTUFFS. EMPTY

    FOODSTUFF CONTAINERS AND ANIMAL FEEDS.DESTROY EMPTY CONTAINERS. '

    3.2.1 The product may also be marked with Standard Mark.

    3.2.2 The liseof the Standard Mark is governed by the provisions of the Bureauof Indian Standards Act, 1986 and the Rules and Regulations made thereunder.The detai Is of conditions under which the licence for the use of Standard Mark:may be granted to manufactures or producers may be obtained from the Bureauof Indian Standards.

    4. SAMPLING

    4.1 The method of drawing representative samples of the material andthe criteria for conformity ahall be al prescribed in Appendix E.

    5

  • IS : 4324 • 1967

    5.T£STS

    5.1 Tests shall be carried out as prescribed in the appropriate appendicesgiven in col 4 of Table 1.

    S.2 Quality of ReageDts - Unless specified otherwise, pure chemicalsand distilled water ( see IS : 1070-1960· ) shall be employed in tests.

    NOTE - • Pure chemical, t shall mean chemicals that do Dot contain impuri-ties which a"tel the results of any)ysis.

    APPENDIX A

    [ Table 1, Item (i) ]

    DETERMINATION OF ENDOSULFAN,TECHNICAL CONTENT

    A-I. PRINCIPLE OF THE METHOD

    A-l.1 The principle in determination of endosulfan is based on hydro-lysis of endosulfan with methanolic sodium hydroxide and estimatingas sodium sulphite ( NatSOI ) formed iodimetrically.

    A·2. REAGENTS

    A-2.l M,tbaaol

    A-2.2 Socllum Hydroxide - pelleta.

    A-2.3 Pbe.olplatbalela ladle.tor Solation - ono perceat ('It'/v) inrectified spirit ( conform in. to IS : 323-19S9t ).

    A-2.4 St••elarel Sulpharlc Acid - S N.

    A-2.5 Studard lodlD' SolutloD - O· J N.

    A-2.6 Sta.ard Socii•• TlIlOI8lpllate 8oIlltl•• - 0'1 N.

    A-2.7 Stucla SoIDtI.. - 0-2 percent, freshly prepared.

    A-3. PROCEDUREA-3.1 Wei,b accurately a quantity of the material containing aboutO'S 8 ot IDdolulfan. technical, aDd transfer it to • 250-ml flask. Add100 ml of methanol by a pipette. Introduce about 1'5 I of sodiumhydroxide peUet. (about 15 pellett J. Connect the flask to a reflux

    ·SpecllcatJOD for wlter, distilledquality ( ",'"d).tSpoc18cIUOII tor r.cUaed Ipirft ( ,,.,/,,d).

    6

  • IS : 4324 - 1967

    condenser and boil the contents at least for two hours. Shake theflask occasionally, Wash down the condenser with 20 ml of methanoland 50 ml of distilled water. Add one drop of the phenolphthaleinindicator solution. Neutralize with standard sulphuric acid. Add afew drops of dilute sodium hydroxide solution to restore the indicatorcolour and to prevent any loss of sulphur dioxide.

    A-3.2 For accurate determimtion of the sulphite, it is essential to addthe sodium sulphite to an excess of acidified standard iodine solutionand back titrate the excess of iodine with standard sodium thiosulphatesolution.

    A· 3.3 Take 40 ml of standard iodine solution in a SOO-ml glass stopper-ed iodine flask from a burette. Add I ml of the standard sulphuricacid and shake it slowly. While agitating, add the sulphite solution.Rinse the flask well with small portions of distilled water until all thesulphite has been transferred. (The washing procedure should becontinued until there is insufficient sulphite in the flask to bleach a smalldrop of iodine.) The final volume in the iodine flask should be bet-ween 225 to 250 mi.

    A-3.4 Back titrate the excess iodine with the standard sodium tbiosul-phate solution using starch solution as indicatorand titrate until theblue colour diappears.

    A-3.5 Carry out a blank determination by titrating 40 ml of the staD-dard iodine solution with 175 ml of water acidified by 1 ml of standardsulphuric acid ( S N ) witb standard sodium thiosulphate solution.

    A-3.6 The difference in the volumes of sodium thiosulphate solutioe inthe titrations in A-3.4 and A-3.S indicates the iodine equivalent con-sumed by endosulfan.

    A-.t. CALCULATIONv x 2'035

    A-4.1 Endosulfan content, percent by weight == W

    where

    Y == volume! '1 ml of 0'1 N iodine solution consumed by.cndosulfan ( A-3.6 ), and

    W - weiaht in 8 of the material taken for the test ( A-3.1 ).

    7

  • IS : 4324- 1967

    APPENDIX B

    [Table 1, Item (ii) ]

    TEST FOR SIEVING REQUIREMENT AFTERACCELERATED STORAGE

    B-1. APPARATUS

    B-1.! Beaker - of capacity 2S0 ml and internal diameter 6'0 to 6'Sem.

    B-l.2 Pres.ure Assembly - a piston or disc, loosely fitting the beakerand so formed or weighed as to exert an even pressure of 2S s/eml ,

    8-J.3 Test Sieve - 7S-micron IS Sieve, prepared for the test byremoving any film, arease or other water-repellent material and thenby dryiD8.

    B-l.4 Rabber Hose - of an internal diameter of about 10mm.

    B-2. PROCEDURE

    ~2.1 Accelerated Storl.e - Weigh 20'0 ± O'S g of the material andgently place it in the beaker. Gently level the surface of the materialin the beaker with the help of a paper strip, camel hair brush or afeather. Place the pressure assembly over the surface of the materialin the beaker and then place the beaker with the pressure assemblyin an oven at S3° to SSoC for 24 hours. Take out the beaker fromthe oven, remove the pressure assembly and allow the material in thebeaker to come down naturally to room temperature in a closedcontainer for a period of 3 hours.

    1-2.2 51.,IDI- At the completion or 3 hours of cooliD" weiah accu-rately 10'0 ± 0'5 I of the treated material (B-2.1) into a wide-mouthbottle (provided with a cork or rubber stopper) containing 100ml oftap water. Stopper the bottle and shake it to mix the contents and makea uniform slurry. Transfer the slurry to the test sieve and wash anyresidue in the bottle on to the sieve usin, small quantities of tap water.Wash the slurry OD the sieve with an oleUlatina. moderately viJorou.'pray of tap water iuuilll out of the rubber hose at the rate of 4 to ,litre. perminute. Continue wI.biDI for 10 minute, or until DO moresoJjd particle, of the material pa.. throulb the lieve. TranlCer tberelidue retained OD tbe lieve to I tared Gooch crucible. dry to constaat\\ei,bt, in tbe oven at I temperature Dot uceediDI SSoC, cool andweiah. Find the weiaht or tbe dry residue.

    8

  • 0'304 0 I0'13901

    to make 1 000 ml

    IS : 4324 • 1961

    B-3. CALCULATION

    8-3.1 Material passin~ through 75-micron IS Sieve, = 100 ( 1 - ~w)percent by weightwhere

    w = weight of the dry residue, andW = weight of the treated material taken for preparing

    the slurry.

    APPENDIX C

    [ lable 1, Item (iii) ]DETERMINATION OF SUSPENSIBILITY AFTER

    ACCELERATED STORAGEc-i, APPARATUSC-l.1 Beaker - of capacity 250 ml and internal diameter 6'0 to 6'S em.

    C-l.% Pressure Assembly - a piston or disc, loosely fitting the beakerand so formed or weighed as to exert an even pressure of 25 gJeml .

    C-l.3 Graduated Cylinder - of capacity 250 ml, with a ground glassstopper. The distance between 0 and 250 ml marks shall be21'0 ± O'S em.C-l.4 Gllss Tube - about 40 em long, of an internal diameter of about5 mm, drawn at one end to an opening of 2 to 3 mm diameter, .withthe other end connected to a vacuum pump.

    C-2. REAGENT

    C-2.1 Standard Hard Water - Dissolve 2'7400 g of calcium carbonateand 0·2760 g of magnesium oxide in a minimum of dilute hydrochloricacid ( 2 N ), Expel the excess acid by evaporation to dryness on awater-bath and dissolve the residue in a small quantity of water.Transfer this solution quantitatively to a lOO-ml volumetric flask, makeup the volume with water and mix. Pipette 10 ml of this solution intoa one-litre volumetric flask, make up the volume with water and mix.

    NOT! - Standard hard water is defined as' water '. whicb provides a bard..ness of 342 parta per million. calculated as calcium carbonate and has the follow..ina composition:

    Calcium chloride. anhydrousMaanesium chloride hexahydrateDistilled water

    9

  • IS : 4324- 1967

    C-3. PROCEDURE

    C-3.t Accelerated Storage - Weigh accurately 20'0 ± 0'5 g of thematerial and gently place it in the beaker. Gently level the surface ofthe material in the beaker with the help of a paper strip, a camel hairbrush or a feather. Place the pressure assembly over the surface of thematerial in the beaker and then place the beaker with the pressureassembly in an oven at 53° to 55°C for 24 hours. Take out the beakerfrom the oven, remove the pressure assembly and allow the material inthe beaker to come down naturally to room temperature in a closedcontainer for a period of 3 hours, taking care to avoid unnecessaryexposure of the sample to atmospheric humidity.C-3.2 Suspensibility Test - At the completion of 3 bours of cooling,weigh accurately Into a lOO-ml beaker, a quantity of the treatedmaterial which could form 250 ml of a suspension of 0·25 percent ofendosulfan. Add to it 30 ml of standard hard water at 30

    n ± 1°C, workthe mass into a uniform slurry and allow it to stand for 15 minutes at30° ± 1°C. Transfer the slurry to the graduated cylinder. Wash anyresidue in the beaker with small quantities of standard hard water at30° ± 1"C. Transfer the washings to the cylinder. Fill the cylinder tothe 2S0-ml mark with standard hard water at 30° ± 1°C. Close thecylinder with the stopper and invert it sharply through 30 completecycles within one minute, thermally insulating the cylinder from thehands to maintain the temperature of the contents at 30° ± 1°C duringthe operation. Allow the cylinder to stand at rest for 30 minutes in awater-bath maintained at 30° ± 1°C. (The bench on which the cylin-der is placed should be protected from vibrations. ) At the end of the~etthng period ( 30 minutes ), dip the nozzle of the glass tube ~ C-l.4 )l~to the supernatant liquid contained in the cylinder and wlthdr~wDIne-tenths ( 225 ml ) of the suspension, within 10 to 15 seconds, uSingthe vacuum pump. During its withdrawal the suspension should bedisturbed as little as possible, which could be achieved by maintainingthe no~zIe of the glass tube just below the sinking top level of thesuspension.

    C-3.3 Determine the endosulfan content of the sediment and the sus-pension r~mainiDg in the graduated cylinder by the methods prescribedID Appendix A.

    NOTE - Should excessive ftocculation occur durin. the test accompanied .bythe appearance of transparent liquid, tbe material sball be deemed unsatis-factory.

    C-4. CALCULATION

    C-4.1 Weight of endosulfan in suspension, expressedas percentage of the endosulfan contentin the treated material taken for the test

    10

    lOOO(W-w)9W

  • IS : 4324 • 1967

    whereW = weight in g of endosulfan present in the treated

    material taken for the preparation of thesuspension, and

    w = weight in g of endosulfan found in the sedimentand the suspension remaining in the graduatedcylinder ( C-3.3 ).

    C-5. INTERPRETATION

    C-5.1 If, by carrying out one test on a sample, the test result showsthat a minimum of 50 percent by weight of endosulfan is in suspension30 minutes after agitating, the sample should be treated as having metthe requirement without further testing.

    C-5.2 If, by carrying out one test on a sample, the test result showsthat the quantity of endosulfan in suspension 30 minutes after agitatingvaries between 45 and 50 percent by weight. the test should be repeat-ed three limes and if the average of the three test results is 50 percentor more, the sample should be treated as having met the requirement;but if the average is leIS than 50 percent, the sample should be treatedas having failed to meet the requirement.

    C-S.3 If, by carrying out one test on a sample, the test result shows thatthe quantity of endosulfan in suspension 30 minutes after agitating isless than 45 percent by weight, the sample should be treated as havingfailed to meet the requirement-

    APPENDIX D[ Table 1, Item (iv) ]

    DETERMINATION OF ACIDITY OR ALKALINITY

    o-r, QUALITATIVE TESTD-l.l Procedure - Take about 0·5 ml of the material in a test tube andmix it with about one millilitre of water. Test the mixture for acidityalkalinity with a litmus paper. Determine the accidity or the alkalinityby the following method.

    0.1. DETERMINATION OF ACIDITY0.2.1 Rea.ent. - The following reagents are required.

    D-1.1.1 Methyl Red Indicator Solution - aqueous, one percent ( wlv },

    D-2.1.2 Standard Sodium Hydroxide Solution - approximately 0·02 N.

    11

  • IS : 4324 • 1967

    0.2.2 Procedure

    D-2.Z.1 Weigh accurately about 10g of the material into a dry conicalflask, and dilute it with 100 ml of water. Titrate the contents of theflask immediately with standard sodium hydroxide solution usingmethyl red as indicator.

    »,,2.2.1 Carry out a blank determination on 100 ml of water.

    D-2.3 CalculatloD

    Acidi ( ) . 4°9 ( V - v ) NCJ ity as H.SO. ,percent by weight = W

    whereV = volume in ml of standard sodium hydroxide solution

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

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

    »,,2.3.1 In case the blank shows alkaline reaction, neutralize withstandard hydrochloric acid (approx 0'02 N), and calculate acidity asfollows:

    A idl ( S) · h 4·9 (VN, +vN,)

    Cl tty as HI 0, ,percent by well t = Wwhere

    V == volume in ml of standard solution hydroxide solutionrequired for the test with the material, .

    NI = normality of standard hydroxide solution,.. == volume in ml of standard hydrochloric acid required for

    the blank determination.N. = normality of standard hydrochloric acid, andW == weight in g of the material taken for the test.

    1)..3. DETERMINATIONOF ALKALINITY0.3.1 Real.at - The following reagents are required.

    0.3.1.1 Phenolphrhal,ln Indicator Solution - one percent (wlv), inrectified spirit ( conforminl to IS : 323-1959· ).

    D.3.1.2 StQndard Hydrochloric Acid ... approximately0'02 N•

    •Splcl8caUoD lor reetiBed IPlrit ( ""I,d ).12

  • )S : 4324 • 1967

    D-3.2 Procedure

    D-3.2.1 Weigh accurately about 10 g of the material into dry conicalflask and dilute it with 100 ml of water. Titrate the contents of the flaskimmediately with standard hydrochloric acid using phenolphthalein asindicator.

    D-3.2.2 Carry out a blank determination on 100 ml of water.D-3.3 Calculation

    .. ( ) bv wei h 4"O(V-v)NAlkalinity as NaOH ,percent y weig t = W

    whereV = volume in ml of standard hydrochloric acid required for

    the test with the material,v :;-:: volume in ml of standard hydrochloric acid required for

    the blank determination,N = normality of standard hydrochloric acid, andW == weight iO g of the material taken for the test.

    D·3.3.1 In Case the blank shows acid reaction, neutralize with standardsodium hydroxide solution ( approx 0·02 N ), and calculate alkalinity asfollows:

    Alkalinity (as NaOH ). percent by weight = 4'0 ( VNW:+- vNt )where

    V = volume in ml of standard hydrochloric acid required forthe test with the material,

    N: = normality of standard hydrochloric acid,v = normality in ml of standard sodium hydroxide solution

    required for the blank determination,N2 = normality of standard sodium hydroxide solution, andW = weight in g of the material taken for the test.

    APPENDIX E( Clause 4.1 )

    SAMPLING OF ENDOSULFAN WATER DISPERSIBLEPOWDER CONCENTRATES

    e-r, GENERAL PRECAUTIONS£-1.0 In drawing, preparing, storing and handling test samples, thefollowing precautions and directions shall be observed.E-l.1 Samples shall not be taken in an exposed place.[-1.2 The sampling instrument shall be clean and dry when used.

    ]3

  • IS : 4324 • 1961

    E-I.3 Proper precautions shall be taken while drawing samples sincethe material is toxic.

    E-l.4 Precautions shall be taken to protect the sample, the materialbeing sampled, the sampling instruments and the receptacles for samplesfrom adventitious contamination.

    E-l.S To draw a representative sample, the contents of each containerselected for sampling shall be mixed as thoroughly as possible by shak-ing or by any other suitable means so as to bring all portions intouniform distribution.

    E-l.6 The samples shall be placed in suitable, clean, dry and air-tightsample receptacles.

    E-l.7 The sample receptacles shall be of such a size tllat they arealmost, but not completely, filled by the sample.

    E-l.8 Each sample receptacle shall be sealed air-tight after filling andmarked with full details of sampling. the date of manufacture, name ofthe manufacturer and other particulars of the consignment.

    E-l.9 Samples shall be stored in such a manner that the temperatureof the material does not vary unduly from the normal temperature.

    E-l.10 Samples shall be protected from light.

    E-2. SCALE OF SAMPLING

    E-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 is known to consist of different batches ofmanufacture, the containers belonging to the same batch shall begrouped together and each such group shall constitute a separate lot.

    E-2.1.1 Samples shall be tested separately for each lot for ascertain-ing the conformity of the material to the requirements of the speci-fication.

    E-1.1 The number (n) of containers to be selected from the Jot shalldepend on the size of the lot and shall be in accordance with col l and2 of 'Table 2.E-2.3 These containers shall be selected at random from the lot. Toensure the randomness of selection, a random number table as agreedto between the purchaser and the supplier shall be used. In case sucha table is not available, the following procedure shall be used:

    Starting from any container, count all the containers as 1, 2,3, , up to r and so on, in one order, where r is equal to the

    14

  • IS : 4324 • 1967

    integral part of N/n, N being the number of containers in the lotand n the number of containers to be selected ( Table 2). Everyrth container thus counted shall be withdrawn until the requisitenumber of containers is obtained from the lot to give samples fortest.

    TABLE 2 NUMBER OF CONTAINERS TO BE SELECTEDFOR SAMPLING

    ( Clauses E-2.2 and E-2.3 )

    No. OF CONTAINeRSIN THE LOT

    (N)(1)

    3 to 1516 .. 4041 " 6566 " 110Over 110

    No. OF CONTAINERS TOBe SELEC1ED

    (n)(2)

    3457

    10

    E-3. TEST SAMPLES AND REFEREE SAMPLES

    E-3.1 Before drawing the test sample thoroughly mix the contents ofeach container selected by shaking or by any other suitable means.Draw small portions of the material from different parts of each con-tainer selected (Table 2). The total quantity of the material drawnfrom each container shall be not less than 300 g.

    E-3.2 Mix thoroughly all portions of the material drawn from the samecontainer. Out of these portions, a small but equal quantity shall betaken for each selected container and shall be well mixed together soas to form a composite sample of not less than 60 g. This compositesample shall be divided into three equal parts, one for the purchaser,another for the supplier and the third for the referee.

    E-3.3 The remaining portions of the the material from each container(after a small quantity needed for the formation of the compositesample has 'been taken out) shall be divided into three equal parts.These parts shall be immediately transfer red to thoroughly driedsample receptacles which are then sealed air-tight. and labelled withall the particulars of sampling given under E-l.8. 1 he material ineach such sealed sample receptacle shall constitute a test sample,These individual samples shall be separated into three identical setsof test samples in such a way that each set has a sample representingeach container selected (Table 2). One of these three sets shall be

    15

  • IS : 4324• 1967

    marked for the purchaser, another for the supplier and the third forthe referee.

    E-3.4 Referee Samples - Referee samples shall consist of the compositesample (E-3.2) and a set of individual t~st samples ( E-3.3 ) markedfor the purpose and shall bear the seals of the purchaser and thesupplier. These shall be kept at a place agreed to between the two.

    E-4. NUMBER OF TESTS

    1:-4.1 Tests for description ( 2.1 ) and the determination of endosulfancontent and suspensibiliry shall be conducted on each of the individualsamples ( E-3.3 ) separately.

    E-4.2 Tests for the determination of the remaining characteristics,namely, sieving requirement and acidity shall be conducted on thecomposite sample ( E-3.2 ).

    E-5. CRI'I~ERIA FOR CONFORMITY

    E-5.1 A lot sh~lI be declared as conforming to all the requirements ofthis specification, when:

    a) each of the sample tested for description satisfies the require-ment given in 2.1;

    b) each of the test results for endosulfan content and suspensibi-lity satisfies the corresponding requirement specified inTable 1. If, however, one or more of the test results do notsatisfy the specified requirements, the conformity of the lotshall be ascertained in accordance with E-5.1.1; and

    c) the results of the tests on the composite sample (E-4.2)satisfy the relevant requirements given in Table 1.

    E-S.1.1 In case one or more of the test results do not satisfy therequirements for endosulfan content and suspensibility, the follow...ing procedure shall be adopted for determining conformity of thematerial in respect of these characteristics. The mean and the rangeof the corresponding test results shall be calculated as:

    M ( X) = The sum of the test resultsean Number of test results

    Range ( R ) == The difference between the highest andthe lowest values obtained for the testresults.

    The appropriate expressions as shown in col 6 of Table 3 shall becalculated. If the values of these expressions satisfy the relevant

    16

  • IS : 4324 - 1967

    candition as givenin col 6 of Table 3, the lot shall be declared to havesatisfied the requirements for endosulfan content and suspensibility.

    Ii) SUlp.nsibility

    Can E.RION FORCONFORMITY

    (6)

    ( A'l::!:O 6 R1 )shall lie withinthe nominalvalue ±S per-cent of thenominal value.

    ( .f,-O 6 R, )~jO

    (4)

    ~1

    TABLE 3 CRITERIA f'OR CONFORMITY( Clause E-S.1.1 )

    CHARACTERISTICS TESTS RESULn AVERAGE RANGE1,2.3•...... n

    (3)

    SLNo.tl) (2)I) Bndcsulfan content

    17

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    Text1: (Reaffirmed - 2012)