is 5549 (1970): warfarin bait concentrates · is : 5549 - 1970 indian standard specification for...
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है”ह”ह
IS 5549 (1970): Warfarin Bait Concentrates [FAD 1:Pesticides and Pesticides Residue Analysis]
0 .. 3
18 : 5549 • 1111
Indian StandardSPECIFICATION FOR
WARFARIN BAIT CONCENTRATES
First Reprint DECEMBER 1990(Incorporating Amendments No, 1,2 and 3)
una 632'958'31
-
@ CoJ1.1righl 1990
BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR. SHAH ZAPAll MAR.G
NEW DELHI 110002
August 1970
IS : 5549 - 1970
Indian StandardSPECIFICATION FOR
WARFARIN BAIT CONCENTRATES
Pest Control Sectional Committee, AFCDC 6
C/ulirmanDR K. D. PA,JLo\lUA
R,prmntin,Directorate of Plant Protection, Q!larantinr &
Storage (Ministry of Food, Agric111ture~
Community Development & Co-operation)
M1f1I6"sSHRI M. L. ADVANI
DB K. KALYAN ( .tf.llernal')DR. K. BAOClJI
DR H. L. HAMI
DR B. n, DJlATIADB N. K. BASO (.AlI,nat,)
MU-GlllN M. S. BOPARAI
DIRlllOTOR 01' AORICUI,TUBJl:
Tata Fison Industries Ltd, Bombay
Minsitry of Health, l~amily Planning, Works,Housing &. Urban Developemcnt
Central Forensic Scienc « Laboratory. CentralBureau of Investigations, Now Dr lhi
I.G.I. ( India) Private Ltd, Calcutta
Directorate General of Armed Forces MedicalServices, Milli'lry of Defence
Department of Agriculture, Government of UttarPradesh
Indian Pharmacopoeia Committee, Ministry ofHealth, Family Planning, Works Homing &Urban Development
Bombay Chemical Private Ltd, Bombay
SHat M. MUTBU (AlttrR/JI,)
DR P. L. Cn....TuRvEDl ( Alt"nate)DIREOTOR OF STORAGE ANlJ Dirctorate of Storage & Inspection (Mini'ltry of
INSPEOTION Food, Agriculture, Community Deve lopruent& Co-operat ion)
DEPUTY DIBEc'I'on (STOB.AQ1~
TSIJRNlOAL) (Alllrttall)Dntms CONTROJ,LER
S'H)\.l G. D. GO'KHALE
SaRI V. V. KE'l'K:AR (AltITnale)DR R. GONOALVES Nat ioI)3.I Organic Chemical Industei..s Limited,
, BombaySBRI H. J. D,AD.... OU ...N,1] (Alt6rnaJ, )
n. K. C. GULA'l'I Indian Agricultural Research Institute, New DelhiSaRI T. GBOROEJOHN Hindustan Insecticides Limited, New Delhi
DR S. N. NAG ( AII,rna', )DR LULAN RAI Cyanamid India Limited, Bombay
SRl\l M. K. ZUTSBI ( Jllttrnal. )SHRl S. K. MUUMDAB. Central Food Tvchnological Research Institute
( CSIR ), Mysore
( ContiJnt4d tin (HII' 2 )
BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI lJOOO2
18 ~ 55_· 1"0
R,pm,ntinlMinistry of Defence ( DOl )
Department of Agriculture, Government of MysoreIndian Agricultural Research Institute, New Delhi
Secretar;]SURI E. N. SUNDAR
Deputy Director ( Agri & Food ), 151
SHRI S. L. PATEL
SHIU L. M. PATEL (Alterna',)PLANT PBOTEOTION Oll'll'IOl!:R
DR S. PRADHANDR RATTAN LAT. (Alternal')
SURI P. RAMDA8 Central Warehousing Corporation, New Dl·)hiOn A. SABUP P(~Bt Control Corporation, CalcutraDa VUl'OD R. SHAll Pest Control ( India) Pvt Ltd, BombayDB L. R. SflAUMA. Shaw Wallace & Company Limited, Calcutta
SORI N. R. jAYARUNDAR (Alt"nau)Da K. S. SIN'(Hf Indian Veterinary Research Inatirute, Izarnagar
01\ R. P. CKAUDHURI ( AllmUJI' )DR L. R. SUD Ministry of Defence ( R&D)DR B. L. WATTAL National Institute of Communicable Diseases,
Dl'1biDa HAnI BIIAGWAN, Director General, lSI (Ex.officio Memb,,)
Deputy Director ( Agri & Food)
( C,ntinu,dJrMlt ~a" 1)
M"nb,r,SaRI L. P. MATBUli
SaRI K. P. SumB ( Al,,,ntd,)DB P. R. ME}{TA Pesticides AllociatioD of India, New Delhi5HftI T. S. M.sBT.A. Bharar Pu)verilin, Mil), Private Ltd, Bombay
SHKJ S. CUATTI!lBJI ( AIt"nat, )SHRI D. N. NAJOIATB Bayer (India) Ltd, Bombay
On. D. V. KASHELIKAR ( Alt",UJI,)SHKI R. NAR.lSJMB~N ~f"ctoraC6 C~aeral of 'l'eihoi<:lll Development
(Ministry of Industrial Development &Company Affain)
American S~ring & Pressing Work. Private Ltd,Bombay
Pesticides Subcommittee, AFCDC 6 : I
Pesticides ASiodation of India, New Delhi
DR B. a BHATUDR~. K. BA8u ( Al'"nIJH )
DR S. L. CnoPRA Punjab Agricultural Uaiversity, LudhiaaaSaRI M. S. DUAT'J;' National Malaria Eradication Programme, DelhiSIlR! O. D. OOXBALE Bombay Ohemicals Private Ltd, Bombay
SHRI V. V. KETKAR (AltUMt,)
DR P. R. MBHTAMmabm
SRI\! M. L. AnvANI Tara Fison Industries Limited, BombayDi~ K. KUYAN (Alemlal,) •
AORIOULTURAL CHEMIST AN)) Agricultural College & Research Institute,A8S00IAT1~ PROJrKssoR 01' SOIL Coimbaw..SOI:C:Ilt().
SHKI V.J. BA.H:a. Central Revenues Control Laboratory, New DelhiSURI N. K. CUOWDHURI ( Altertlat, )
DR H. L. Bun Central ForeDlic Science Laboratory, tAntralBureau of Inveatigation•• New Delbi
I.C.1. ( India) Private Ltd, Calcutta
( C.rJlimud '11 ,." 12)
2
IS z 5549 • 1970
( C,nlinu,dlrlm pal' 2 )
Mnn6ers011. R. R. GONC.\L'VES
R'prlJ,nfin,National Organic Chemical Industries Limited,
Bombay
Ministry of Dpfl'nce ( R Be D)Narional I nstitu te of Communicable Diseases.
Dclbi
Central Plant Protection Training Inetiture,Hyderabad
ChE'mlltry Department, Delhi University, DelhiBharat Pulver ising Mills Private Ltd, Bombay
Hindustan Insecticides Limited. New Delhi
Directorate General of Technical Development(Minsitry of Industrial Development &Company Affairs)
Directorate of Plant Protection Quarantine &Storage (Ministry of Food, Agriculture,Community Development & Co-operation)
Agromore Limited, BangaloreBombay Municipal Corporation, BombayE. I. D.-Patry Limited, MadrasPelt Control ( India) Pvt Ltd, BombayExcel Induatries Limited, Bombay
DR K. D. PADARJ"
SSBI H. J. DADACnANJI ( Alternate)DR K. C. GULATI Indian A~ticulturaJResearch IDititute, New Delhi
DB R. S. DEWAN ( Alt"nate)SURI T. GJtOROZjoHN
DR S. N. NAG ( Alt".nat, )SHRI V. LAKSHIlrt:INAItAYANA
DB R. S. RAJAOUPA.LANDB V. SA.DABIVA.N
Da P. R. SAltMA
DB VINOD R. SHARSaBI R. D. REROFF
SaRI K. K. CHH"Y A ( Altmwle )DI\ L. R. SunDR n. L. WATT \L
DB K. n. L MATHURSURI T. S. MEHTA
SURI S. ClIA'l"rEun ( Alternat&)SHRI R. NARASIMHAN
SHaI V. N. UBA.'l'N A(UR ( Alternate)
12
AMENDMENT NO. 4 MAY 1994TO
IS 5549: 1970 SPECIFICATION FOR WARFARINBAIT CONCENTRATES
( Page 5, clause 4.1 ) - Substitute the following for 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 : 1983 within 90 days of its manufacture. When (be material is offeredfor inspection after 90 days of its manufacture, sampling shall be done asprescribed in IS 10627 : 1983. However, the criteria for confonnity of thematerial whentested, shall be the limits of tolerances, as applicable over thedeclared nominal value and given under clause 2.2.1 of the standard'.
(FAD 1)Reprography Unit. BIS. New Delhi. India
lOO(W-w)=
W
AMENDMENT NO.5 AUGUST 2008TO
IS 5549: 1970 SPECIFICATION FOR WARFARINBAIT CONCENTRATES
(Page 6. clause A-3.t) - Substitute the following for the existing text:
'Material passing through 53~micron
IS Sieve, percent by weight
where
w ::;:; weight in g of the material retained on the test sieve, andW = weight in g of the material taken for the test.
_ (Page II. Table 2, col 5) - Substitute' XI - 0.6 RI ~ 95 percent' for, X(-06. Rl~ 95 percent'.
(FAD 1)
Reprography Unit. BlS, New Deihl, India
II c 5541 • 19'"
Indian StandardSPECIFICATION FOR
WARFARIN BAIt CONCENTRAtES
o. FOREWORD
0.1 This Indian Standard was adopted by the Indian StandardsInstitution on 27 February 1970, after the draft finalized by the PestControl Sectional Committee had been approved by the Agriculturaland Food Products Division Council and the Chemical Division Council.
0.2 Warfarin bait concentrates are used in formulating rodent baits forthe control of rodent pests in homes, fields and warehouses.
0.3 Taking into consideration the views of producers, consumers, testingauthorities and technologists, the Sectional Committee responsible forthe preparation of this standard felt that it should be related to themanufacturing and trade practices followed in the country in this field.
0.4 This standard is one of a series of Indian Standards on pesticidesand their formulations.
0.5 This standard contains clauses 3.1, C-2.3 and C-3.4 which call foran agreement between the purchaser and the vendor.
0.6 For the purpo~e 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 inaccordance with IS : 2-1960*. The number of significant places retainedin the rounded off value should be the same as that of the specifiedvalue in this standard.
I. SCOPE
1.1 This standard prescribes the requirements and the methods of testfor warfarin bait concentrates used in the preparation of rodent baits.
2. REQUIREMENTS
2.1 Phy.lcal- The material shall conform to the following physicalrequirements.
·Rulell for rounding off numerical values ( WJis,d).
3
IS : 5549-1970
2.1.1 Description - The material shall consist of technical warfarincompounded with talc or other suitable diluent, and shall be in theform of uniformly blended free-flowing powder, free from lumps andextraneous impurities which may limit its suitability for baiting rodentsor impair its effectiveness. The technical warfarin used in the manufacture of the concentrates shall conform to IS : 5552-1970*.
2.1.2 Sieving Requirement - When tested by the method prescribed inAppendix A, not less than 95 percent by dry weight of the initialamount taken for the test, shall pass through 75-micron IS Sieve ( seeIS : 460-1962t).
2.2 Cbemical- The material shall comply with the following chemicalrequirement.
2.2.1 Warfarin Conten! - When determined by the method prescribedin Appendix B, the observed warfarin content, percent by weight, ofany of the samples shall not differ from the nominal value by more thanthe tolerance limits indicated below:
Sl No.
i)
Nominal Value. Percent
Up to 10
Tolerance Limit, Percent
+ l~ of the nominal value
ii)
iii)
Above 10 and up to 50
Above 50
± 5
+ 53
"
2.2.1.1 The actual value of the technical material in the formulationshall be calculated to the second decimal place and then rounded offto the first decimal place before applying the tolerances given above.
3. PACKING AND MARKING
3.1 Packing -The material shall be packed in clean and dry air-tightcontainers made of galvanized steel sheet. tinplate, steel, glass, plastic orcardboard and polyethylene as agreed to between the purchaser andthe manufacturer.
3.2 Marking - The containers shall be securely closed and sealed airtight after filling them with the material, and shall bear legibly andindelibly the following information:
a) Common name of the material;b) Name of the manufacturer;
·Specification for warfarin technical.tSpedfication for test sieves ( ,mIld).
4
IS : 5549-1970
c) Date of manufacture;
d) Batch Dumber;
e) Net weight of the contents;
f) Warfarin, technical, percent content by weight;
g) The word 'POISON- in distinct, bold capital letters, in red; and
h) The minimum cautionary notice worded as under:
'HAZARDOUS. KEEP THE MATERIAL AND BAITSCONTAINING THE MATERIAL AWAY FROMCHILDREN, DOMESTIC ANIMALS, FOODSTUFFS,ANIMAL FEEDS. DO NOT USE THE EMPTY CONTAINERFOR STORAGE OF FOODSTUFFS OR FEEDS.
ANTIDOTE: MASSIVE DOSES OF VITAMIN K AND IF'FOUND NECESSARY BLOOD MAY BE TRANSFUSED'.
3.2.1 The containers may also be marked with the CertificationMark.
NOTB - The use of the Standard Mark is governed by the provisions of theBureau of Indian Standards Act and the Rules and Regulations made thereunder.The Standard Mark on products covered by an Indian Standard conveys theassurance that they have been produced to comply with the requirements of thatstandard under a well-defined system of inspection, testing and quality controlwhich is devised and supervised by BIS and operated by the producer. Standardmarked products are also continuously checked by HIS for conformity to thatstandard 'as a further safeguard. Details of conditions under which a licence for theuse of the Standard Mark may b,' granted to manufacturers or processors, may beobtained from the Bureau of Indian Standards.
4. SAMPLING
4.1 The method of drawing eepresent ative samples of the material andthe criteria for conformity shall be as prescribed in Appendix C.
5. TESTS
5.1 Tests shall be carried out by the appropriate methods referred toin 2.1.2 and 2.2.1.
5.2 Q.uaUty of Reagents - Unless specified otherwise, pure chemicalsand distilled water (se, IS : 1070-1960·) shall be employed in tests.
NOTE - 'Pure chemicals' shall mean chemicals that do not contain impuritieswhich affect the results of analysis.
·Specification for water. ~istilled quality ( revised).
5
IS : 5549-1970
APPENDIX A
( Clause 2.1.2)
TEST FOR SIEVING REQ,UI1lJ!:MENT
A-t. APPARATUS
A-I.t Test Sieve - 75-micron IS Sieve ( see IS : 460-1962* ), preparedfor test by removing any film, grease or other water-repellent materialand then drying.
A"2. METHOD
A-2.1 Weigh accurately 100 g of the material and transfer it to the testsieve. Cover the sieve and screen the material in a suitable sievevibrator for 10 minutes. Two small square rubber cubes are introducedalong with the material on the sieve to facilitate the breaking up of anysoft lumps of the caked material. After 10 minutes, stop the machineand brush the residue on the sieve into a tared weighing dish. Weighthe dish and determine tho weight of the residue.
A-3.CALCULATION
A-3.1 Material passing through 53-micronIS Sieve, percent by weight c:: 100 ( 1 - w)
W
where
w = weight in g of the material retained on the test sieve, and
W = weight in g of the material taken for the test.
APPENDIX B
( Clause 2.2.1 )
DETERMINATION OF ACTIVE INGREDIENT CONTENT
B-1.. APPARATUS
B-l.1 Spectrophotometer - Beckman, model DU, or equivalentinstruments with l·cm quartz cells,
·Specification for teat sieves (,tDis,d).
6
IS 15549·1970
B-2. REAGENTS
B-2.1 Refereace Sola.doD - Prepare by pipetting 2 ml of ethylenedichloride into a glass stoppered cylinder, adding 10 ml of one percentsodium hydroxide solution with a pipette, and shaking for one minute.The sodium hydroxide layer is decanted into a centrifuge tube andcentrifuging until it becomes clear,
8-3. PROCDURE
B-3.1 weigh accurately about 600 mg of the sample into a 125-ml glassstoppered flask, add 50 ml of ethylene dichloride with a pipette, placethe flask on a shaking machine and shake for at least 10 minutes.Transfer the contents to a centrifuge tube, stopper and centrifuge athigh speed for 5 minutes or until clear. Pipette 2 ml of ethylenedichloride extract into a glass stoppered cylinder, add 10 ml of onepercent sodium hydroxide solution with a pipette, and shake by handfor 1 minute. Decant the sodium hydroxide layer into a centrifuge tubeand centrifuge until clear. Pipette a sufficient amount (about 3 ml )of the alkali layer into l-cm quartz cell and, with the spectrophotometerset at maximum sensitivity determine its absorption (sel Note) at308 nm ( nanometre) against the reference solution.
NO'1'E - For routine testing it is necessary to have a standard curve down andcompared with the test sample.
B-4. CALCULATION
B-4.1 Molecular weight of warfarin = 308·3
Molar extinction coefficient = 1"42 X 10'
E X 308·3 X lOx 50 X 100I' 42 X 10000 x 1 000 X 2 X W
Ex 0'54W=
[ Molar extinction coefficient shall be determined with pure 3~
( alpha-phenyl-beta-acetylethyl )-4·hydroxycoumarin; the value givenhere is an example only. ]
3-( alpha-phenyl-beta-acetyl-ethyl )-4-hydroxycoumarin,percent content (warfarin) =
where
E z= absorption of the final solution at 308 nm, and
W -= weight in g of the sample.,
IS I 5549-1970
APPENDIX C
(Clause 4.1 )
SAMPLING OF WARFARIN BAIT CONCENTRATES
o-r, GENERAL PRECAUTIONS
C-l.0 In drawing, preparing, storing and handling test samples, thefollowing precautions and directions shall be observed.
0-1.1 Samples shall not be taken in an exposed place.
C-1.2 The sampling instrument shall be clean and dry when used.
0-1.3 Proper precautions shall be taken while drawing samples since thematerial is poisonous.
C-I.4 Precautions shall be taken to protect the samples, the materialbeing sampled, the sampling instrument and the receptacles for samplesfrom adventitious contamination.
0-1.5 The samples shall be placed in suitable, clean, dry, and air-tightsample receptacles. The samples shall be protected from light.
C-l.6 The sample receptacles shall be of such a size that they arealmost, but not completely, filled by the sample.
C-l.7 Each sample receptacles 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.
0-1.8 Samples shall be stored in such a manner that the temperature ofthe materia] does not vary unduly from the normal temperature.
C-2. SCALE OF SAMPLING
C-2.1 Lot - All the containers in single consignment of the materialdrawn from the same batch of manufacture shall constitute a lot. Ifaconsignment is declared or 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.
C-2.1.1 Samples shall be tested for each lot for ascertaining theconformity of the material to the requirements of this specification.
8
IS : 5549-1970
C-2.2 The number of containers to be chosen from the lot shall dependon the size of the lot and shall be in accordance with col I and 2 ofTable 1.
TABLE 1 NUMBER OP CONTAINERS TO BE CHOSEN FOR SAMPLING
LOT SIZE
N
(1)
3 to 15]6 to 4041 to 6566 to 110Over 1]0
No. OJ' CONTAINERS'1'0 BE CHOSEN
n
(2)
3457
10
0-2.3 These containers shall be chosen at random from the lot. Inorder to ensure the randommess of selection, some random numbertable, as agreed to between the purchaser and the vendor, shall be used.In case such a table is not available, the following procedure shall beadopted:
Starting from any container in the lot, count them as 1, 2,3, .....etc, up to r in a systematic manner where' is equal to the integralpart of the value of Nln, }I being the total number of containers inthe lot and n the number of containers to be chosen (see Table 1 ).Every rth container thus counted shall be separated until therequisite number of containers is obtained from the lot to givesamples for test.
0 ..3. TEST SAMPLES J\~D REFEREE SAMPLES
C-3.1 Before drawing the test sample, mix thoroughly the contents ofeach container selected, by shaking or by any other suitable means soas to bring all portions into uniform distribution. Draw small portionsof the material from different parts of each container selected (seeTable I). The total quantity of the material drawn from eachcontainer shall be not less than 750 g.
C-3.2 Mix thoroughly all the material drawn from the same container.A small but equal quantity shall be taken from each selected containerand shall be well mixed together so as to form a sample of not less than100 g. This sample shall be divided into three equal composite testsamples, one for the purchaser, another for the vendor, and the thirdfor the referee.
9
IS ; 5549-1970
C-:t3 The remaining material drawn from a container (after thequantity needed for formation of the composite test samples has beentaken out) shan be divided into three equal parts. These parts shallbe immediately transferred separately to thoroughly dried samplereceptacles which are then sealed air-tight, and labelled with all theparticulars of sampling given under C-l.7. The material in each suchsealed sample receptacle shall constitute an individual test sample.These individual test samples shall be separated into three identical setsof individual test samples in such a way that each set has a samplerepresenting each container selected (see Table I). One of these threesets shall be marked for the purchaser, another for the vendor, and thethird for the referee.
(:-3.4 Referee Samples - Referee samples shall consist of one of thecomposite test samples (see C-3.2) and a set of individual test samples(Sfl C-3.3) marked for this purpose and shall bear the seals of thepurchaser and the vendor. These shall be kept at a place agreed tobetween the two.
C-4. TESTING OF SAMPLES
C-4.0 The number at' tests mentioned in C-4.1 and C-4.2 shall be firstconducted on the test samples marked for the purchaser. In thecontingencies, such as loss, spoilage, spilling, etc, of the purchaser's testsamples or if the vendor so desires, the test samples marked for thevendor may be tested. In case of a dispute, the referee test samplesshall be tested and the test results obtained on the referee test samplesshall be considered as final.
C-4.1 Tests for the determination of warfarin content shall beconducted on each of the individual test samples ( C-3.3 1.
C-4.2 Tests for the determination of the remaining characteristic,namely, the sieving requirement, material passing through 53-micronIS Sieve, shall be conducted on the composite test sample as preparedunder 0-3.2.
0-5. CRITERIA OF CONFORMITY
0-5.1 A lot shall be declared as confer ming to the specification, when:
a) each of the test results for warfarin content satisfies therequirement specified in 2.2.1. If, however, one or more ofthe test results do not satisfy the specified requirement, theconformity of the lot shall be ascertained in accordancewith 0-5.1.1; and
10
IS I 5549 - 1970
b) the test results on the composite sample for sieving requirement,material passing through IS Sieve 75, satisfy the correspondingrequirement given in 2.1.2.
C-5.1.1 In case one or more of the test results do not satisfy therequirement for warfarin content, the following procedure shall beadopted for determining conformity of the material in respect of thischaracteristic.
The mean and the range of the corresponding test results shall becalculated as:
Mean (X ) = The sum of the test results1 Number of test results
Range (Rl) = The difference between the highest and the lowestvalue obtained for the test results.
The appropriate expression as shown in col 5 of Table 2 shall becalculated. If the value of this expression satisfies the relevant conditiongiven in col 5 of Table 2, the lot shall be declared to have satisfied therequirement for ~arfarin content.
TABLE 2 CRITERION FOR CONFORMITY
CllAll.A(JTElRlSTlC
(1)
Warfarin content.percent by weight
TEST RlCSUVl'S MIDAN RANOH CRITERION '"ORCONI'ORMITY
(2) (3) (4) (5)
1,2,3, .···'1 --:\'1 R1 Xl -06·Rt ;;' 95 percentof the value as declaredon the container
",Y;'+O"6RI '< 105percentof the value as declaredon the container
11
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