IS 15616: Alphacypermethrin, Technical

2006·1.1 MB·English

by  Bureau of Indian Standards

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IS 15616 (2006): Alphacypermethrin, Technical [FAD 1:
Pesticides and Pesticides Residue Analysis]
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IS 15616:2006

Indian Standard
ALPHACYPERMETHRIN, TECHNICAL —
SPECIFICATION
ICS65.100.10
. .

(3 BIS 2006
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

January 2006
Price Group 2
l
Pesticides and Pesticides Residue Analysis Sectional Committee, FAD 1
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Pesticides
and Pesticides Residue Analysis Sectional Committee hadbeen approved bythe Food and Agriculture Division
Council.
Alphacypermethrin, technical, is an insecticide employed inthe preparation of insecticidal formulations for the
control of agricultural insect pests.
Alphacyperrnethrin isthe common name accepted byInternational Organization for Standardization (1S0) fora
recemate comprising two isomers Rand Sofrx-cyano-(3-phenoxyphenyl) methyl (1R)-cis-3-(2-2 dichlorovinyl)-
2-2-dimethyl-cyclopropane carboxylate.
The empirical formula, structural formula andthe molecular massof alphacypermethrin are indicated below:
Empirical Formula Structural Formula Molecular Mass
CZ2H,9C12N0, 416.32
H3C CH3
cl
cl FA’~*&oD
H CN
Inpreparation of this standard, due consideration has been given to theprovisions ofthe Insecticide{ Act,, 1968
andtheRulesframedthereunder. However,thisstandard issubjecttotherestrictions imposedundertheInsecticides
Act and Rules, wherever applicable.
For the purpose of deciding whether a particular requirement of this standard is complied with the final value,
observed or calculated, expres sing the result of a test or analysis, shall be rounded off in accordance with
IS 2:1960 ‘Rules for rounding of f numerical values (revise~’. The number ofsignificant places retained inthe
rounded off value should be the same asthat ofthe specified value inthis standard.
AMENDMENT NO. 1 OCTOBER 2010
TO
IS 15616 : 2006 ALPHACYPERMETHRIN, TECHNICAL —
SPECIFICATION
(Foreword, para 3) — Add the following at the end of the para:
'The cis-2 isomer of Cypermethrin is called Alphacypermethrin.'
[Page 3, Annex A, clause A-2.4.6(b)] — Substitute '9.0 min' for '8.0
min'.
[Page 4, Annex B, clause B-1.4.3(a)] — Delete '[(1R cis)R + (1 Scis)S]'.
[Page 4, Annex B, clause B-1.4.3(b)] — Add the following after cis-2
isomer:
' [(1R cis)S + (IS cis)R]'.

(FAD 1)
Reprography Unit, BIS, New Delhi, India
IS 15616:2006
Indian Standard
ALPHACYPERMETHRIN, TECHNICAL —
SPECIFICATION
1 SCOPE 4 PACKING
This standard prescribes therequirements andmethods The material shall be packed according to the
of sampIing and test for alphacypermethrin technical. requirements given inIS 8190 (Part 1).
2 REFERENCES 5 MARKING
The following standards contain provisions which 5.1 Thecontainers shallbear legibly and indelibly the
through reference inthis text, constitute provisions of followinginformation andotheradditional information,
this standard. At the time of publication, the editions as is required under the Insecticides Act, 1968, and
indicated were valid. All standards are subject to Rules framed thereunder:
revision and parties to agreements based on this
a) Nameofthe material;
standard are encouraged to investigate the possibility
of applying the most recent editions of the standards b) Nameand address ofthe manufacturer;
indicated below: c) Batch numbeL
1SNo. Title d) Date ofmanufacture;
1070:1992 Reagent grade water (third revision) e) Date ofexpiry;
6940:1982 Methods of test for pesticides and 9 Net mass of contents;
their formulations @st revision) g) Nominal alphacypermethrin content, percent
8190 Requirements for packaging of (m/m);
(Part 1): 1988 pesticides: Part 1 Solid pesticides h) A cautionary notice as worded in the
(second revision) Insecticides Act, 1968 and Rule_sframed
10946:1996 Methods of sampling for technical thereunder; and
grade pesticides (.fht revision) j) Any other information required under the
Standards of Weights and Measures
3 REQUIREMENTS
(Packaging Commodities) Rules, 1977.
3.1 Description

5.2 BIS Certification Marking
The material shall be inthe form of off-white to light
brown coloured, free flowing yowder. It shall be free The product may also be marked with the Standard
from extraneous matter. Mark.
3.2 The material shall comply with the requirements 5.2.1 The use of the Standard Mark is governed by
specified inTable 1. the provisions ofthe Bureau tflndian Standards Act,
Table 1Requirements for Alphacypermethrin, Technical
(Clauses 3.2 and 7.1)
sl Characteristic Requirement Method ofTest, Refto
No. / A \
Annexofthis Clauseof
Standard 1S6940
(1) (2) (3) (4) (5)
O Alphacypermethrin content,percentbynmss,A4irr 957 A —
ii) (1Rcis)Rand(1Scis)Sisomers,percentbymass,Mm 3.5 B .
iii) Transisomer,percentbymass,IUux 0.5 B —
iv) Alkalinity (asNaOH),percentbymass,Mm 0.25 . 11.3
v) Moisturecontent,percentbymass,Max 0.25 — 4s

1
IS 15616:2006
1986and the Rules and Regulations made thereunder. 7 TESTS
The details of the conditions under which the licence
7.1 Testsshall becarried out bythe methods referred
for the use of the Standard Mark may be granted to
to inCO14and 5ofTable 1.
manufacturers orproducers maybe obtained from the
Bureau of Indian Standards. 7.2 QuaIity of Reagextts
Unlessspecified otherwise,purechemicals andreagent
6 SAMPLING
grade water (see IS 1070) shallbe employed intest.
Representative samples ofthematerial shallbedrawn, NOTE — ‘Pure chemicals’ shall mean chemical that do not
asprescribed in IS 10946. contain impurities whichaffecttheresultsofanalysis.
ANNEX A
[Table 1, fi’1No. (i)]
DETERMINATION OF ALPHACYPERMETHRIN CONTENT
A-1 GENERAL A-2.3 Reagents
Alphacypermethrin content isdetermined bytheHPLC A-2.3. 1 Internal Standard — Benzyl benzoate.
method (see A-2). This will be the routine as well as
A-2.3.2 Alphacypermethrin Reference Standard— of
referee method.
known purity.
A-2 HPLC METHOD
A-2.3.3 Di-isopropyl Ether — HPI,CISpectroscopic
A-2.1 Principle grade.
AHPLC unitwith aUV detector isused forthis assay. A-2.3.4 n-Pentane — HPLC/Spectroscopic grade.
Usingsolutions containing known amountsofstandard
a[phacypermethrin and internal standard, theresponse A-2.3.5 Toluene — AR grade.
factor (RF), for alphacypermethrin and internal
A-2.4 Procedure
standard is arrived at. A solution containing known
mass of the technical sample and internal standard is A-2.4.1 Preparation ofInternal Standard Solution
injected subsequently. The percentage of
Weighaccurately about 2.0 gof internal standard (IS)
alphacypermethrin inthe sample isthen computed by
intoa 100mlstandard volumetric flask and add about
standard relationship.
20 ml oftoluene to dissolve the contents. Make up to

A-2.2 Apparatus volumeusingtohtene. Shakewelltohomogenize. This
willgive a20mg/ml solution of internal standard.
A-2.2. 1 High Performance Liquid Chromatography —
Equipped with a printer plotter-cum-integrator or A-2.4.2 Preparation of Working Standard So[ution
computer and UV detector, and preferably with
Weighaccurately about 100mg ofalphacypermethrin
chromatographic software. The suggested parameters
reference standard, in duplicate, into two 100 ml
aregiven below, andtheseoperating conditions caa be
standardvolumetric flasks.Pipette out 10mlofinternal
varied, provided standardization isdone.
standard solution into each flask. Ultrasonicate for
Column : Stainless steel, 250 mm x about5mintodissolvethecontents.Dilute withmobile
4.6 mmid., packedwithsilica phase to themark and mix well to homogenize. Label
of 5~m particle size these solutions asCAand CB respectively.
Detector : UV (1 =280 nm)
A-2.4.3 Preparation of Sample Solution
Mobile phase : 3.0percent (v/v)Di-isopropyl
ether inn-pentane. Weigh accurately 100mg of the technical sample (or
Flow rate : 1.5ml/min. EC sample containing an equivalent amount of
alphacypermethrin) in duplicate, into two 100 ml
Sample size : 20 pl
standardvolumetric flasks.Pipette out 10mlofinternal
Temperature : Ambient (25 +2°C).
standard solution into each flask. Make up to volume
A-2.2.2 Glassware — Standard volumetric flasks of withmobile phase andmixwell. Label these solutions
100ml capacity. Bulbpipettes of 10ml capacity. as SAand SBrespectively.

2
IS 15616:2006
A-2.4.4 Estimation
RF (standard
Area of standard peak (Al)
Introduce 20 pl of the working standard solutions CA
solution)
and CB and the sample solutions SA and SB into the = Area ofinternal standard peak (A,)
HPLC unit in the indicated sequence. From the
Alphacypermethrin,
integrator/computer print out,notedownthepeakareas RF(sample solution) #4, xp
percentagebymass=
ofalphacypermethrin andinternalstandardineachcase. RF (standard solution) A42
A-2.4.5 Injection Sequence
where
CA1, SA1, SA2, CB1, CA2, SB1, SB2, CB2.
M, = mass of alphacypermethrin reference
Calculate the response factor (RF) for the pair of
standard insolution CA/CB, inmg;
calibrationsolutions,whichbracketthesamplesolutions,
&f, . mass of alphacypermethrin in sample
for example, use CA1 and CB1for SA1and SA2,etc.
.Injecttwoorthreetimesuntilresponsefactor(RF)agrees solutions SA/SB, inmg;
within one percent. A, = peakareaofalphacypermethrin instandard
solutions CA/CB;
Calculate the alphacypermethrin content as indicated
under A-2.5. Az = peakareaofalphacypermethrin insolutions
SA/SB;
A-2.4.6 Elution Order
A, = peak area ofinternal standard insolutions
a) Internal standard =5.0 min CA/CB;
b) Alphacyperrnethrin s 8.0 min A, = peak area of internal standard insolutions
SA/SB; and
A-2.5 Calculation
P= percent purity of alphacypermethrin
RF (sample Area of sample peak (~)
reference standard.
solution) = Area of internal standard peak (A,)
ANNEX B
[Table 1, S1No. (ii) and (iii)]
DETERMINATION OF ISOMER CONTENT IN ALPHACYPERMETHRIN (TECHNICAL)

BY THE HPLC METHOD

B-1 HPLC METHOD Detector : UV (k =280 nm)
Mobile phase : 3.0 percent (v/v)Di-isopropyl
B-1.1 Principle
ether inn-pentane
AFIPLCunitwithanUVdetector isusedforthisassay.
Flow rate : 1.5ml/min
A solution containing known mass of the technical
Sample size : 20.pl
sampleisinjected.Thepercentageofalphacypermethrin
isomers in a sample is then computed by the area B-1.2.2 Glassware — Standard volumetric flask of
normalization method. 100ml capacity.
B-1.2 Apparatus B-1.3 Reagents
B-1.2. 1 High Performance Liquid Chromatography — B-1.3.1 Di-isopropyl Ether — HPLC/Spectroscopic
Equipped with a printer plotter-cum--integrator/ grade.
computer and UV detector, and preferably with
B-1.3.2 n-pentane — HPLC/Spectroscopic grade.
chromatographic sofiware. The suggested parameters
aregivenbelow, andthese operating conditions canbe B-1.3.3 Toluene — AR grade.
varied, provided standardization isdone:
B-1.4 Procedure
Column : Stainless steel, 250 mm x
B-1.4.1 Preparation ofSample Solution
4.6 mminnerdiameter, packed

withsilicaof5pm particle size Weighaccurately 100mg of sample in duplicate into
3
IS 15616:2006
two 100ml standard volumetric flasks. Dissolve the B-1.4.3 Elution Order
sample and make up the volume using mobile phase, a) cis-1isomer[(1Rcis)R+(1Scis)S] ~ 8.0 min
and mix well.
b) cis-2 isomer s 9:0 min
. B-1.4.2 Determination c) trans-1isomer s 10.5min
d) trans-2 isomer z 12.0min
Introduce 20 @of sample solution intotheHPLC unit.
Fromintegrator/computer printout,notedownthepeak NOTE— Downthepeakareaandcalculatethepercentageof
eachisomerasindicated below.
area percent ofalphacypermethrin isomers. Themajor
peak inthe chromatogram represents the cis-2 isomer. B-1.5 Calculation
Thepeak immediately preceding this isofcis-1isomer
Alphacypermethrin isomer content, Percentage
and the peaks after the major peak represents trans
of isomer = Area of individual isomer peak ~~O.
isomers.
Total areaofallisomer peaks