is 5279 (1969): dicofol emulsifiable concentrates · is : 5279-1969specification for dicofol...
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“Step Out From the Old to the New”
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“The Right to Information, The Right to Live”
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है”ह”ह
IS 5279 (1969): Dicofol Emulsifiable Concentrates [FAD 1:Pesticides and Pesticides Residue Analysis]
IS : 5279., 1969(Aeaffirmed 2002)
Indian StandardSPECIFICATION FOR
DICOFOL EMULSIFIABLE CONCENTRATESSecond Reprint OCTOBER 2007( IncludrngAmendment No.; J 2 & ~ )
UDC 632951 [DICOFOLJ
C Copyright 1969
BUREAU OF INDIAN STANDARDSMANAK BH.,AVAN, 9 BAHADUR SHAH ZAFAR MARG
, NEW DELHI 110002
Gr4 December 1969
18.5279.1_
Indian StandardSPECIFICATION FOR
DICOFOL EMULSIFIABLE CONCENTRATES
Pest Control Sectional Committee, AFCDC 6
ClulimumDR SARUAR SINOR
RtJwI3""i,.,Dil"f'Ctorateof Plant Protection, Quarantine & Stor.
(Ministry or Food, Agriculture, CommunityDevelopment It Co-operatioa )
Tata Fiaan Jndu.tries Limited, Bombay
Dinetorate General of Armed 'orca Medical. Services, Ministry of ner..nee (
SaRI A. W. CoCKY Shaw Wallace Ie Company Limited, CalcuttaSRR) H. C. SOMA••aHAR ( Allnnal, )
DlR.croa or AOlllCVL'l't1RJC Department of Alriculture. C,ovemment 01 tltarPradeah i
DR P. L CHATVBVZDf ( AllmttJl, ) IDIRECTOR or STORAGE at 11(8.£0- DirHtorate or StOFale cl Inspection (Minilt~ of
TION .'ood, ......icultW'e. Community Developme aCo-operation )
DDun D.aBcroa ( SToRAO. fTxcUKICAL) ( AI,.,.." ) l
naua. CONTBOu..1IR Indian Phannaco~i. Committee (MiDiittY 01Health, Family PJanninlt Works. HOUlint •UrbanDevelopmeat)
SRR.G. D. GO_HAL. Bombay Chemicals Private Ltd, BombaySHRI V. V. K"'''Aa ( AI,.".." )
DR R. GOlCCALntI National Organic Ch.mical Industries Limited.Bombay
DR S. B. D. AOA.WALA (AI"""')DR K. C. GULA'rJ Indian Al"icultura1 Research Institute, NewDellaiSURI T. GaoRG. Jo.. Hjndustan lnaecticidee Llnlited, New Deihl
D. S. N. NAG ( AI",." )D. !.Au",. RAJ Cyanamid ladia Limited, Bombay
SIlRI M. K. ZVTlHl ( AI"".." )
DaH. L. BAlli
M-'n,SHIU ){. L. Auv AWl
DRK.. K"LYAH (AI,."",)Da K. BAGOS! Maniltry or Health, Family Plaoninlt Woru. HoUliIll
; a. Urban DevelopmentIi Central Forensic Science Laboratory, Central 8111'••Ie or InveatiKalionl, New Delhi
DR B. B. BHATIA r I. C. I. (Jndia) PrIvate Ltd. CalcuuaDa N. K. BAIV ( .4lItruu )
MA.J-GBM M. S. BorAKAI
(c.IiMtM .. ,." 2)
It1REAU or INDIAN STANDARDSMANAK IlHAVAN. 'BAHADUa SHAH ZAFAR MARO
NEW DEUtIJ101m
IS ,5279..1969
Releareh Inatitute/bJlrultJIUaI
Central Food Technolosical( CSIR ), Myeore
SHRI S. L. PATEL
( Conti"",d from POI' I )
Mmcb"sSURI S. K. M4-JUIIDAR
SJlHl 1... l\1. PATEL ( tfltnnat#)PLANT PnOTEC'1'JON OFFICER Department of Agrkulture, Government of MYlOreDB S, PaADHAN Indian Agricultural Research Institute, New Delhi
DRRATTAN tAL ( All"",," )SHIll P. ItAKDAR (A,ntral Wart'houaing Corporation, New DelhiDIl A. SAlttJP Peat Control Corporation, CalcuttaSllRI A. K. SJ~NOtJPTA National Malaria Eradication Programme, DelhiDn VINon R. SUA1. Pest Control ( India) Pvt Ltd, BombayIJIl H. D, SIU\,ARTAVA Indian Veterinary Research Institule, Izatnalar
lJn R. P. (;HAvnHURl (AlurnQu)Dn I... R. Suo l\finistry of Defence (R " D)
SHJU S. K. AfJ'r.IA (AI/maalt)Dn B. L. WA'l'TAI. National Institute of Conununicable Diseases. DelhiOil Hvm IlHAG\VAN, Director General, lSI ( Ex-oJlitio MmaHr)
1)eputy ) lir('(.lor ( Agri & Food)
SKRI M. MITTllt1 ( A11mt4U )Stun L. P. MA'l'HVn Ministry of Defe-nee ( DGI )
Saar K. P. StNOJl (Allman/I)On P. R. MEHTA PMtiddtt. As~ociarion of rndia. New DelhiSHIU T. S. M1(llTA 8laarat Pulverising ~{ills Pvt Ltd, Bombay
Sli RI S. (~JI t\TT~ltJ I (Alter"ak)811ftr D. N. NAkliATE Bayer ( India) Ltd, Bombay
DIt D. V. KA8UKI.IEAR ( Iilt,rIlDII)SUBI R. NARASIMHAN Directorate General of Technical Development
( Miniatry of Industrial Development, atCompanyAffairs)
Anlerican Spring & Pressing "'orks Private Ltd,Bombay
S«r"aryS.tRI E. N. SlH(f).,n
{)eputy Director (Aari &. Food), lSI
Pesticides Subcommittee, AFCDC 6: I
c.....Oft P. R. MKHTA PHticidei Auociation of India, New Delhi
M...,SaRI M. L. AnVANI Tata Fiaon Indultries Limited, Bombay
DR ~. KALW AN ( .~II'''Ult' )AGRICULTURAL CHatl"" ANO Alricultural College &: Research Institute, Coimbatore
ASSOCIATE PRO...oa OW SOILS~I1bfCB
Sanr V. J. RAK.. Central Revenues Control LaboratorYt New DelhiSH&JN.X.C.OWDRVBt(A~)
2
AMENDMENT NO. 1 AUGUST 1972TO
IS : 5279-1969 SPECIFICATION FORDICOFOL EMULSIFIABLE CONCENTRATES
Alteratioll
( PtJ" 4, ,Inrls, 2.3.1 ) - Substitute the follow ing tor U,c existingclause:
, 2.3.1 D"n/ol Content - When determined by the method prosenbed III
vppendrx r:,lhrol~rrvcddicorolcontent, perl tint h\ weight, of anv ot thesamples shall not drllet Iiom the nouuual "due by more than thE' tolerancehmus mduated below:
SIND. Nominat V4111c Pr runt Joleranc: J l1111t Peru 171
i) up (0 10 f- lO- ') of the nominal value
It) Above 10·clnd up to SO ± 5 It
iii) Abov« 50· + 5 JJ- 3tA
2.3.1.1 1 he di tual V,l(Ut' of the t('( hnu al material In the tnrmtldtton~h(tll 1)(' l all ulated to the c,Plond dPl tnldl place dnd then rounded otlt to thvIust decimal pl'll (.I betore etppl) Ing the tolt' f cl n l e "t e1\ en 'lbo\ tJ" t
;t
(.uux 0 r
AMENDMENT NO.2 JULY. 1976TO
IS: 5279-1969 SPECIFICATION FORDICOFOL EMULSIFIABLE CONCENTRATES
Alteration
::I: 5
Tolerance LmutPercent of the nommal value
-+ '05Upto9
t
10 and below sO:
( Pagt 4, clause 2.3.1 (a.. also Amendment No. J)] -Substitute thefollowina for the existing clause:
'2.3.1 DieD/til Content-- When determined by the method prescribed inAppendix C, the observed dicofol content, percent mass/mass of any of thesamples shall not differ from the declared nominal value by more than thetolerance limits indicated below:
Nominal Valu$Percent
+- S3SO and above i
i~
2.3.1.1 The actual value of dicofol content shall be caJcuJat~ to thesecond decimal place and then rounded ofT to the first decimal p'af beforeapplying the tolerances as stipulated In 2.3.1.• t
.)4
(AFCDC 6)
Printed at S,mco Prant.ng Press. Deihl
AMENDMENT NO. 3 MAY 1994TO
IS 5279: 1969 SPECIFICATION FOR DICOFOIJEMULSIFIABLE CONCENTR~TES
t Pag« 5, clau..e 4.1 ) - Substitute the following for the existing:
'When treshly manufactured matenal in bulk quantity i~ otlcred lor inspection,representative samples of the matcnal shall he drawIt and tested as prescribed inIS 10627 : 19R3 within 90 days of it", manufacture, When the material i~ offeredfor invpcction ;tft("r 90 days of 11\ manufacture, 4\alnphn~ vhall hl' done a,prrvcribed in IS 10617 : 19S3. HCl\Vl'VCr, the criteria for conformity of themateriaI \\ hen tested. ~ball he tbe Illuit~ of tolerances, as apphcable over thedeclared nominal value and given under clause 2.3.1 of the standard:
(FAD 1)Printed at Simco Prlnteng Press, Deihl
11,5279.1_
Indian StandardSPECIFICATION FOR
DICOFOL EMULSIFIABLE CONCENTRATES
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 Pelt ControlSectional Committee had been approved by the Agricultural and FoodProducts Division Council and the Chemical Division Council.
'\
0.2 The emulsifiable ~oni('ntrates formulations of dicofol are used in thecontrol of acarine pests ofptgricultural importance.
"~0.3 Taking into consideration the views of producers, consumers, te,stingauthorities and technologists, the Sectional Committee responsible fot thepreparation of this stancl8.rd felt that it should be related to the raanufacturing and trade practices followed in the country in this field. !O.t This standard is one of a series of Indian Standards on pestirid~ andtheir formulations. ,
i0.5 This standard contains clauses £-3.3 and E-4.4 which call for an Itgree-ment between the purchaser and the vendor.
0.6 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 ac-cordance 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 Thil standard prescribes the requirements and the methods of test fordicofo! emulsifiable concentrates used in the control of acarine pests ofagricultural Importance.
*Ruleslnr roundiftl off numerical valun (".11 ).
lI.sm.l.2. ItEQ,VIRIMENTS
2.1 The material shall consist of dicofol. tecJmical. cliuolvecl iD IUitableIOlveDt. together with· emullifyiDI asent( a) and, when necessary,atabilizer(. ).
2.1.1 Dicorol, technical, employed in the manufacture of the material,ahall conform to IS: 5278.1969·•
2.2 1'IIyUcaI-The material shall comply with the physical requirementsal described in 2.2.1 to 2.2.~
2.2.1 DlstriJllitnt-The material abaIl be in the form of • clear ableliquid free from extraneoUI matter.
2.2.2 CoI4 T,,, - No turbidity or separation or aoIicI or both or oilymatter sha)J occur when the material i...ijectecl to the coW test at lere. AIprescribed in Appendix A.
Non-lithe cold lilt ....... to l- carriecI out at lower .... Ire. It ............... by .... parcJIMer.
u.s FItuIt p,;", (AM) - WheD determiDed by the method P:20 el18:1448 (Part 1)-J96Ot. the fIuh pOint 01 the matwial ahaIl be .bove24·~oC.
2.2.4 E.Lri... S,.IIiI.-.The creaminr or the lICIimeDtatioD, if a"~shall DOt in either c:&Ie exceed 2-0 mI at tbe ~ or bottom 01 100 mIcylinder. _heR tested by ODe or the methods prelCnbecl in Appeadix IS.
U m..-a The material aWl comply with the chemical requirementa liven in 2.&1 aDd2.1.2.
2.1.1 J?i«lol c.,.".,-When d....ined by the IDeIhocI~in Appendix C, the oa..wd dicolol coatent. percent by weiaM, 01., orthe aampJea aIIII IIGt difter&om tbe noaaiaaI value by more t1uUa .5 ,.ceat 01 the Iatt.-.
I.U Ariiifl- .4/""-WIaeD~ by the 1D~~esa;will~ D, alae~~. if~. calculated • ~aulpbwic acid(~,)or .au.uaky. if .,....... IOdiuIR hydroxicfe (NaOH), .-u DeBel .ore daD 8-1 perc:.t by weiPLIe ~4GKING AND1MB...
1.1 PM!,! ,-The IIIaCtriaI IhaII he packed ia Mild ateel COD""lined with1MW pIleaolic .IUM .,.y pheaoJic CIt aDOCIiIIcI .........~ ,. tcIaaIcaI (..,,,,.).t et tor"" itt~PutI
•
11.5271.1_
3.1.1 The packing sball allO conform to Tariff Rule••1 in force fromtime to time for packing of good. falling in the category of materials ofhigh flash point.
3.2 MarJdaa-The containen lball be securely closed and .hall 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 volume of contents; and
f) Nominal technical dicofol content, percent by weight, and minimumcautionary noti~ worded as under:
•KEEP AWAY fROM FOODSTUFFS AND ANIMAL FEEDS.DESTROY EMfTI' CONTAINERS. •
3.2.1 The product rna} plliiO be marked with Standard Mark.
1 :
3.2.2 The use of the Standard Mark is governed by the provisions of the ~ureauof I"dian Standard~ Act, '986 and the Rules and Regulations made ther~nderThe details of conditions under which the licence for the use of Standar MarkIna) be granted to manufactures or producers may be obtained from the ureauof Indian Standards, ~
4. SAMPLING
4.1 Representative samples of the material shall be drawn al prescribed inAppendix E.
5. TESTS
5.1 Testl shall be carried out by the appropriate methods referred toin 2.2.2, 2.2.3, 2.2.t, 2.3.1 and 2.3.2.
5.2 (laaIlty .1 Rea,eat. - Unless specified otherwise, pure chemicalsand distilled water (see IS: 1070.1960·) shan beemployed in tests.
NOD - 'Pure chemicals' shall man chemicals that do Dot contain impurities whichaffect the Multi of analysil.
·Specification for water, distilled quality (,IfIiI,d).
5
IS I 5279-1969
APPENDIX A( Clause 2.2.2 )
COLD TEST
A-I. PROCEDURE
A-I.I Take 50 ml of the material in a l00-ml transparent glass containerand close it with a cork or stopper fitted with the thermometer. <Jool thematerial to 100e (se, Note) by placing the container in the water mainrained at go to lOne. When the temperature of the material in thecon taincr reaches IO~C, add to it a small seeding crystal of dicofol withminimum opening of the stopper within the shortest possible duration oftime. Gently stir the material in the container at intervals for one hourmaintaining the temperature of. the material at 10°C. At the end of onehour J examine the material for any turbidity or separated solid or oilymatter or both.
NO'l'E - In casE' the purchaser Ipecified tbat the telt il required to be carried out at0°0, the material in a c.ontainer ahall be cooled to O°Cby placiD, the container in abath of crushed ice and the telt carried out at oec iDitead of 10°0.
APPENDIX B(Clause 2.2.4 )
DETERMINATION OF EMULSION STABD..ITY
B-1. METHODS
8-1.1 Two methods are prescribed for the determination of emulsionstability of the material. The method to be employed shall depend uponthe manufacturer'. instructions for the preparation of the diluted emulsionfrom the material. Method 1 shall be employed in the case of a materialwhich is required to be added to standard hard water Cor the preparationof the diluted emulsion, while Method 2 shall be employed in the case ofa material to which standard hard water should be added to prepare thediluted emulsion.
B-2. METHOD 1
11-2.1 Appua..e11-2.1.1 Btdtr- 250 ml rapaC'ityJ with an internal diam.tft' of 6-0 to
6'5 em and marked at 100 ml,
6
15.5279.1969
8-2.1.2 Moh, TyfJI Pi/JIII,
B-2.1.3 GldSs Rod-4 to 6 mm in diameter and of a convenient length.
8-2.1.4 G,aduaua Cylindn- 100 ml capacity and graduated at eachmillilitre from 2 to 100 ml.
B-2.2 Realeat
8-2.2.1 Standard Hard Ii'ater - Dissolve 2-740 g of calcium carbonateand 0-276 g of magnesium oxide in the minimum of dilute hydrochloricacid (approximately 2N). Expel the excess acid by evaporation to dryness on a water-bath and dissolve the residue in a small quantity of water.Transfer this solu tion quan titatively to a lOO-ml graduated flask, make upthe volume with water and mix. Pipette 10 ml of this solution into a onelitre graduated flask, make up the volume with water and mix.
NOTE- Standard hard Wa«t'f is defined al 'water' which provides a hardnEls or 342parts per million, calculated ~a calcium carbonate and bas the following compositiom
Calcium chloride, anttdroul 0·304 IMagnesium chloride, 'exahydrate 0-139gDistilled water ~ To make 1 000 ml
8-2.3 Procedure - Pour ts to 80 rnl of standard hard water at a temperature of 30°:J: 1°C into th~ beaker. By means of the Mohr type pipptte,add 5 ml of the concentrate to the standard hard water contained iff thebeaker. The material should be added to the standard hard water a therate of 25 to 30 rnl per minute, with the pointed end of the pipette 2· eminside the beaker and aDowing the material to pour directly int thestandard hard water and not along the sides of the beaker. The con ntsof the beaker should be stirred vigorously with a glass rod durin theaddition. Add more water to bring the volume of the diluted ernulsidn tothe lOQ-ml mark with continued stirring and transfer immediately to theclean and dry graduated cylinder. Keep the cylinder with its contents at atemperature of 30t> :i-: 1°C in a thermostatically controlled bath for half anhour. After the half hour, note the volume of the creamed matter at thetop and the sediment at the bottom, if any.
B-2.4 Report-- Report the total volume in millilitres of the creamedmatter at the top and the sediment at the bottorn in the cylinder,
8-,. METHOD 2
N.l Proeedan-Place 5 ml of the concentrate in the beaker. Addsufficient standard hard water at a temperature of 30°:: tOe into thedropping funnel and add it to the material contained in the beaker at therate of 15to 20 ml per minute. During the addition, continuously stir thecontents of the beaker with the glass rod. Stop the addition of thestandard hard water just when the volume of diluted emulsion in the
7
IS1527'.196'
beaker reaches 190 mi. Transfer the diluted emulsion immediately to theclean and dry graduated cylinder. Keep the cylinder with it. contents ata temperature of 300 d: 1°0 in a thermostatically controlled bath for halfan hour. After the half hour J note the volume of the creamed matter at thetop and the sediment at the bottom, if any.
8-3.2 Report - Report the total volume in millllitres of the creamedmatter at the top and the sediment at the bottom in the cylinder.
APPENDIX C(Clawe 2.3.1 )
DETERMINATION OF DICOFOL CONTENT
0.1. REAGENTS
0-1.1 Eth,1 Alcohol - 95 percent.
0.1.2 EthaaoUe Pota.ll.. Hy..xlcle-O·5 N.
<:-1.3 Coae_taW Nitric Acld ....analytical reagent grade conformingto 18:264·1968·.
e-l.f Ferric AI1IID IacUcator- Dissolve 350 g of ferric ammoniumsulphate crystals in 700 ml distilled water, heating gentlyJ if necessary,Add 50 ml of eoncentrated nitric acid, dilute to 1 litre with distilledwater and mix thoroughly.
c.J.5 Nltrobe..eae
e.I.6 Sta.eI.rd 811y. Nitrate SoladOD - 0'1 N.
0-1.7 Staaclarcl Ammoal•• TIalocy...te Sol.doa-O'I N.
C.IJI PIa..olpJatlaaleia I_tea- IoI.tlOII-Diaolve 0-5 g of phenolphthalein powder in 100ml of95 percent ethyl alcohol.
C.2.PROCED1JIlB
e-2.1 Weigh accurately sufficient quantity of the material containing 0·51of the technical material in an erlenmeyer flask. Add 50 ml of the standardethaoolie potassium hydroxidesolution to the sample. Place the flask on ahot.plate and connect the neck of the flask to a water-cooled condenser..using S to 4 drops of 95 percent ethyl alcoholas a seal. Boil the solution
'Speciflcation tor nitric acid (,m-J).
8
IS : 52'79-1969
under gentle reflux for 90 minutes. At the end of this time, stop heatingand allow the flask to cool slightly, rinse the condenser with 25 ml of95 percent ethyl alcohol. Disconnect the flask and rinse the tip of thecondenser with 95 percent ethyl alcohol, adding the rinsings to the flask.
C-2.2 Drain the liquid contents of the flask into a 4OO-ml beaker, add50 ml of 95 percent ethyl alcohol to the flask. Swirl the flask, and againdrain the liquid contents into the 4OO-ml beaker. Add approximately100 ml of distilled water to the flask, swirl, and add the contents of theflask to tllP 400 ml beaker by stirring. Rinse the flask with small portionsof distilled water and add the rinsings to the 40Q-ml beaker by stirring.Continue rinsing the fta\k until there is a total volume of approximately300 ml in the beaker,
0.2.3 Place the beaker on a steam-bath until all of the alcohol has beenevaporated. Cool the btaker in a water-bath and add 2 to 3 drops ofstandard phenolphthalein indicator solution and sufficient 1 : 1 nitric acidto turn the indicator coleurless, Add an additional )0 ml of 1:) nitricacid and 50 rnl of the sta'dard silver nitrate solution. Thoroughly mix thecontents of the beaker. ~dd 5 ml elf ferric alum indicator solution, 5 mlofnitrobenzene to the bealfr, stir vigorously, and titrate the eXCflSS silvernitrate with the standar' ammonium thiocyanate solution with vigorousstirring, until the app~ararc~ is of a faint hut permanent pink end-poipt.
C-3. CALCULATION !e-3.1 Active ingredient, percent content = f
(11£1 AgNoa for sample -nll AgNo3 for blank) N 12-g-1t------~- ~ -- X X ') t;weight of sample (grams ) , 1
NOTB - Run a blank determination through all .t~p. uC the procedure Ul$ng allreagent. except the material to be analyzed. '
APPENDIX D(Clause 2.3.2)
DETERMINATION OF ACIDITY OR ALKALINITY
0.1. Q,UALITATIVE TEST
1).1.1 Proeeclve- Take about 0'5 ml of the material in a test-tube andmix with about one millilitre of water. Test the mixture for acidity oralkalinity with a litmus paper. Determine, as the case may bet the acidity(s" 0.2) or the alkalinity (SIt D.').
9
••527'.1_
1).2. DETERMINATION OP ACIDITY
1).2.1 a..pat.
1).2.1.1 M,'h.11 R,d Indicator Solution-prepared by dissolving 0 15 g ofthe indicator in 500 ml of water.
0.2.1.2 Standard Sodium HJt/roxitll 80Iutio,,-0·02 N.
D-2.1.3 Standard Hydrochloric Acid- 0'02 N.
1).2.2 Proeedare- Weigh accurately about 10 g of the material into adry conical flask and dilute with 100 ml of water. Titrate the contents ofthe flask immediately with the standard sodium hydroxide solution usingmethyl red as the indicator. Alternatively, the end-point may be determined pontentiometricaUy.
D-2.2.1 Carry out a blank determination on 100 mlofwater.
0.2.3 CalealatioD
Acidity (as HISO,), 4-9 (V - v) Npercent by weight == W
whereV == volume in ml of the standard sodium hydroxide solution
required for the test,v == volume in ml of the standard sodium hydroxide solution
required for the blank determination,N == normality of the standard sodium hydroxide solution, andH' = weight in g of material taken for the test.
0.2.3.1 In case the blank determination shows alkaline reaction, neutralize with the standard hydrochloric acid and calculate the acidity asfollows:
Acidity (as H.s~,), 4'9 (V.N + vX )percent by weight == ~'
wheteV == volume in m1 of the standard sodium hydroxide solution
required for the test,N, .. normality of the standard sodium hydroxide solution,
v _ volume in ml of the .tandard hydrochloric acid required forthe blank determination,
N. :II normality or the standard hydrochloric acid, andW == weight in g of the material taken for tbe test.
10
IS I 5279-1969
D-3. DETERMINATION OF ALKALINITY
1).3.1 R.,eats
0-3.1.1 M,thyl R,d Indicator Solution -prepared by dissolving 0-15 g ofthe indicator in 500 ml of water.
0.3.1.2 Standa,d Hydrochloric Acid- 0'02 N.
0.3.1.3 Standard Sodium Hydroxide Solution-O·02 N.
0-3.2 Pro~eclure-Wf'igh accurately about 10 g of the material into adry conical flask and dilute with 100 ml of water. Titrate the contents ofthe flask immediately with the standard hydrochloric acid, using methylred as the indicator. Alternatively, the end-point may be determinedpotentiometrically.
D·:J.2.1 Carry out a blank determinatlon with 100 ml of water.
D-3.3 Calcula\ioll
Alkalinity~as (~aOH), 4'0 (V -LJ) Npercentlby weight == ------~.--
~ . ~
~
acid required,requ}rI'd
ft·1
whereV = volume in 011 of the standard hydrochloric
for the resr,v = volume in ml of the standard hydrochloric acid
for the blank determination,}I =- normality of the standard hydrochloric acid, and
Ji' == weight in g of the material taken for the test.
0.3.3.1 In case the blank determination shows an acid reaction,neutralize with the standard sodium hydroxide solution and calculate thealkalinity a8 follows:
Alkalinity (as N~OH), 4-0 (V}{t + vN: )percent by weight = IV •
whereV c= volume in ml of the standard hydrochloric acid for the test.
Xl - normality of the standard hydrochloric acid,u =volume in m) of the standard sodium hydroxide solution
required for the blank determination,
N. = normality of the standard sodium hydroxide solution. andf1" == weight in g of the material taken for the test.
11
APPENDIX E( Clawe 4.1 )
SAMPLING or DlcorOL EMULSIFIABLE CONCENTBATU
"1. GENERAL PRECAU110NS
£.1.0 In drawing, preparing, storing and handlinl test _mples, thefoflowing precautions and directions shall be observed.
E-l.1 Samples .hall not be taken in an exposed place.
8-1.2 The sampling insteumen; shall be of glass or of a metal on whichthe material has no action and shall be clean and dry when used"
£-1.3 Proper precautions shall be taken while drawing samples since thematerial is highly poisonous.
8-1.. Precautions shall be taken to protect the samples, the material beingsampled, the sampling instruments and the containers for samples fromadventitious contamination.
£-1.5 The samples shall be placed in leak-proof lOO-ml aluminiumcontainers of a minimum purity of 99 'percent.
£.1.6 The sample containers shall be of such a size that they are almost,but not completely-filled by the sample.
B-l.1 Each sample container shall be fitted with an inner stopper, whichshall be sealed in the neck of the container by means of a suitable sealingcomposition. The container shall then be securely closed by screw caplined with tin foil. The containers shall then be marked with full detailsof sampling, the date of manufacture, name of the manufacturer and otherparticulars or the con.ignment.
£.1.8 Samples shall be stored in such a manner that the temperature of thematerial does not vary unduly from the normal temperature.
£.1.9 Samples shall beprotected from Jight.
£.2. SAMPLING INSTRUMENTB-2.1 s.mpHaa T.IIe- It shall be made of thick glass or of a metalonwhich the material baa no action, and shall be of 20 to 40 mm diameterand 400 to 800 mm in length (," Fig. 1). Tbe upper and lower endsare conical and of 5 to 10 mm diameter at the narrow ends. Handling itfacilitated by two rings at the upper end. For taking a sample, the tube isfirst closed at the top with. the thumb or a .topper and lowered until thedesired depth il reached. It is then opened for a ahort time to admit thematerial and finally closed and withdrawn.
12
Ii
18:5219·1_
....., ,..... TO10 D"..........- ..~
20 TO .0 D'A
8•e0->o•
-H-.TO 10 DIA
All dilMlllica ill .Wimetta
'IG. 1 SAllPLIKO TunN.I.I For small containers. a .maller IUDpIins tube or suitable dimen
..... maybe used.
a-s. 1CAL! or MMPUNG&&1 !At - All the containen in a aiDlle ~ipment of the materialdrawn &om the same batch or manufacture ahall CODllitute a lot. If.eoDsipment ia declared or knowD to CODsist or different betches or manufactaie, the containers beJouliftl to the _e batch shall be sroupecltopth. and each such group shall constitute. teparate lot.
B-S.I.I Samples .hall be tested foreacla lot forucertain.illl the conformityof the material to the requirement. or thi. specification.a.&2 Tbe number (JI) of containers to becholen fromthe lot thaD d.ndOR the size of the lot (.~) and shall be in accordance with col I and 2ofT.hle I.
13
IS .527••1969
£-3.3 These containers shall be chosen at random from the lot and in orderto ensure the randomness of selection, some random number table asagreed to between the purchaser and the vendor, shall be used. In casesuch a table is not available, the following procedure shall be adopted:
Starting from any container in the lot, count them as 1, 2, 3.... ,up to " in a systematic manner, where' is equal to the integral part ofthe value of Nln, N being the total number of containers in the lot andn the number of containers to be chosen (st' Table 1). Every rthcontainer thus counted shall be separated until the requisite number ofcontainers is obtained from the lot to give the samples for test.
TABLE 1 NUMBER. 01' CONTAINERS TO BE CHOSEN POR SAMPLING( Claus,s E..3.2 and E-3.3)
LOT SIZE
AI'(I)
3 to 1516 ., 4041 u 6566 " 110Over 110
No. OJ' CONTAINRas'1'0 BE enu8EN
n(2)3451
10
E·4. TEST SAMPLES AND REFEREE SAMPLESE-f.l Before drawing the test samples, mix thoroughly the contents of eachcontainer selected by shaking or stirrin~ by suitable means, or by rolling.so as to bring all portions into uniform distribution. Draw by inserting thesampling instrument through the bung-hole or any other convenientopening, small portions of the material from different parts of each selectedcontainer. The total quantity of the material drawn from each containershall benot less than 350 ml,
1£·...2 Mix thoroughlyall the material drawn from the same container. Asmall but equal quantity shall betaken from the each selectedcontai.nerandshall be well mixed topther 80 al to form a sampleof not Jess than 450 ml.Thi. sample shall be divided into three equal composite test samples.onefor the purchaser, another For the vendor and thethird for the referee. .
w.s The remaining material drawn from a container (after the quantityneeded for formation of the composite teat sample bas been taken out) shallbe divided into three equal partl. These parts shall be immediately tranlferred separately to thoroughly dried bottles which are then sealed air-tishtwith 8to~rl and labelled with all the particulars of sampli", givenunder ~1.7. The material in each such sealed bottle .hall constitute anIl\dividual teat sample. These individual test samples ahaD be separated
14
IS: 5279.1969
into three identical sets of individual test samples in such a way that eachset has a sample representing each selected container. One of these threesets shall be marked for the purchaser, another for the vendor and thethird for the referee.&-4•• Releree Sample. - Referee samples shall consist of the compositetest sample (see E-4.2) and a set of individual tE'st samples (Sft E-4.3)marked for this purpose and shall bear the seals of the purchaser and thevendor. These shall be kept at a place agreed to between the two.
E·5. TESTING OF SAMPLES£-5.0 The number of tests mentioned in E-5.1 and E-S.2 shall he firstconducted on the test samples mar ked for the purchaser. In the romingencies, 8\1<..h as IOSSt spoilage and spilling, of the purchaser's test samplesor if the vendor so desires, the test sample's marked for the vendor may betested. In case of a dispute, the referee test samples shall be tested andthe test results obtained On the referee test samples shall be consideredas final.E-5.1 Tests for the determination of dicofol content and emulsion stabilityshall be conducted on eac' of the individual samples i see E-f.3 ).£.5.2 Tests for the deter~inatjon of the remaining characteristics, namelycold test, flash point, and .acidity or alkalinity shall be conducted 01) thecomposite test samples (sef EA.2). ;
&.6. CRITERIA FOR CONFORMITY J"E-6.1 A lot shall be declared as conforming to this specification wher
a) each of the test results for emulsion stability and dicofol co~tentsatisfies the corresponding requirements specified in 2.2.4 and t-3.1.
b) the test results on the composite test sample for cold test, ~ashpoint, and acidity or alkalinity, satisfy the corresponding requirements given in 2.
£.6.1.1 In case one or more of thE' test results do not satisfy the requirements for dieofol content and emulsion stability, the following procedureshall be adopted for determining the conformity of the material in respectof these characteristics, The mean and range of the corresponding testresults shall be calculated as:
- Sum of the test r~sults
Mean (X) == Number of test results
Range (R) =Difference between the highest and the lowest valueobtained for the test results.
The appropriate expression as shown in col 6 of Table 2 shall becalculated. If the values of these expressions satisfy the relevant conditionas given in col 6 of Table 2 the lot shall be declared to have satisfied therequirements for dicofol content and emulsion stability.
15
(~/"/MI'2).......,Da H. L. BAlli
II.S27t·1961
T..... 2 CIUTDIA POR CONIOUIITY(a.. 1-6.11)
SL CHABAOTDlmca "'TRavvre MIld !lA.G. CBlft&I01f "_No. I, 2, .•....•• eo.'OBlllft
(I) (2) (3) (4) (5) (6)
1) Dicofol content ~ R, ~ :I: 0-6 R1 aballlie within ttie nomi.naI value :1:5 % orthe nominal value
Ii) Emulaion ItabUit, X, R. .f; +&6 a. <2-0
.",...,CeDtral ForeIWe Science Labontary. OeDlra1 BuNMI
01InVeltiptionl. New DelhiD. B.B.B."'rIA I. C. I. ( lpdia ) Private Ltd. CaIcu...
Da N. K. 8••u ( ....._)DRS. L. CHOPRA Punjab Aarieultural UllivenJty.L~~~SM81 M. S. DIiAn National Malaria Endicalioa~. DelhiSa.1 G. D. GO.HAUI Bombay Chemicals Private Ltd. lOmba,
S••I V. V. Kas•• ( .AI"".", )D. 1t.. GO.CALYM NatioDal Olpnic Chemical IncNatri. Limhecl.
Ion.ba,J)a S. I. D. Ao••WALA (A""')
Da K. C. GUL.~I Indian Alricultural ReseArCh IMtitute. New DelhiDa •• S. DllwA. (.AlIIntatI)
SOl T. O...".~.. HilaclUitu IDleCticWea Limited. NewDeIWDB S. N. NAG (MIItwII)
D. K." 1... "AbU. a.emiatry DlpartllleDt, Delhi UDiv",. DelhiSa.1 T. S. M.ftA _at Pulv...... Milia Private Limited, Bo...,
ilia. L 0.•.,...,1 (.."".,,).... D. P. MrtN MiIUIcryatOCJ1l a: D}baa It. NA.AaI.... DirectOrate 0( Techftlal ~t
( Miniltry of JacI.&rW DeveIopmeaI a Canapeay.wain)
Da &. D. r••AldA DirecIerale 01Plat ProsecdoR, (bIINDClM a. s.....~at Pood,~..... e.-ueky•• Co-otwauoa )
D. It. I. 'kAlA......... ~ itecI~Da v. S"DA8l.... ....., M.nicij;l CerP:ntioa, ....,Da PI' k. SARIIA L I. D.. - Parry Limited. ,.....D" V.lIODk. aa'8 .. ContlOl { India ) Private Ltd. 10m.,Ilnll R. D.S.... ... JDCbaItnes LiIaiIed, "ba,
a..1K..It. euAT.(~)Oa 8. L WA"'r. Nationallaadtute oleo.tamuaicaWe~ Dellai
.... V.N. BR..b"'A1' ( ...".",)
16
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