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“Invent a New India Using Knowledge”

है”ह”ह

IS 15443 (2004): Imidacloprid Technical [FAD 1: Pesticidesand Pesticides Residue Analysis]

IS 15443:2004

Indian Standard

IMIDACLOPRID TECHNICAL — SPECIFICATION

Ics 65.100.10

0 BIS 2004

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

/kf(//’l/l 2004”

,. >.,-

Price Group 2

Pesllci&s and Pesticide Residue Analysis Sectional Committee, FAD 1

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft firmlized by the Pesticides and

Ptsti~ide Residue Analysis Sectional Committee had been approved by the Agricultural and Food Products DivisioncoLlncil.

Imidacloprid twhni~al, is employed in the preparation of insecticidal formulations.

Imidacloprid is the accepted common name by the International Organization for StandardizationI-((khlor[~-3-pyridinyl) metbyl-4,5-dihy dro-N-nitro- 1-H-imidazole-2-amine.

E//lpiri[ ’(// Forlnulo

CgH,,CINfO,

#

Str[lc~uml Fornudu Moleculur Muss

5?N NH255.6

‘\ No2

(1S0) for

In (IK preparation ol this standard, due consideration has been given to the provisions of the Insecticides Act, 1968. .and the Rules framed thmcunder. However, this standard is subjected to the restrictions imposed under the Act and theRLIICS wherever applicable.

F(N [hc purpose olckiding whether a particular requirement of this standard is complied with the final value, observed

or calculated. expressing the result 01’a test or analysis, shall be rounded off in accordance with IS 2: 1960 ‘Rules forrounding oft’numerical values (revised)’. The number of significant places retained in the rounded off value should be

he same as [hat oi’ the specified value in this standard.

,., ,,.

IS 15443:2004

Indian Standard

IMIDACLOPRID TECHNICAL — SPECIFICATION

1 SCOPE

This standard prescribes the requirements and the methods

of’sampling and test for imidacloprid technical.

2 REFERENCES

The following standards contain provisions which through

reference in this text, constitute provisions of this standard.At the time of publication, the editions indicated werevalid. All standards are subject to revision and parties to

agreements based on this standard are encouraged toinvestigate the possibility of app[ying the most recent

editions of the standards indicated below:

1S No.

1070:1992

6940:1982

7601 :1983

8190 (Part 1) :1988

10946: 1996

3 REQUIREMENTS

3.1 Description

Title

Reagent grade water (thirdflevision)

Methods of test for pesticides and

(heir formulations (jir.st revision)Fibreboard drums for general

purposes (first revision)Requirements for packing of

pesticides : Part I Solid pesticides(second t-evisio]l)

Methods of sampling for technicalgrtlde pesticides (jirst revision)

The material shall be in the ~orm of cream to off white

coloured powder. It shall be devoid of hard aggregatesand free from extraneous impurities or added modifyingagents,

3.2 The ma[erial shall also comply with the requirements

given in Table 1.

4 PACKING

h4aterial shall be packed in polyethylene bags closedsui[ably and further inserted in[o fibreboard drums (weIS 7601) with a ring clwnp/clip acting as a tampcrproof

device. The containers shall also comply with therequirements given in IS 8190 (Part 1).

5 MARKING

S. 1 Tbc contaiimrs shall be securely closed and shall bear

]egib]y and indelibly the following information in addition

to any other information as is necessary under theInsecticide Act, 1968 and Rules framed thereunder:

a) Name of the material;

b) Name and address of the manufacturer;

c) Batch number;

d) Date of manufacture;

e) Date of expiry;

f) Net mass of contents;

g) Nominal imidacloprid technical content, percent

h)

j)

(m/m);

A cautionary notice worded as in the Insecticides

Act, 1968 and Rules framed thereunder; and

Standards of Weights and Measures (Packaged

Commodities) Rules, 1977; and

Any other information required under theStandards of Weights and Measures (Packaged

Commodities) Rules, 1977.

5.2 BIS Certification Marking

The product may also be markedMark.

with the Standard

5.2.1 The use of the Standard Mark is governed by the

provisions of the Bureau of Indian Sturtdards Act, 1986and the Rules and Regulations made thereunder. The

details of conditions under which the licence for the useof the Standard Mark may be granted to manufacturersor producers may be obtained from the Bureau of IndianStandards.

6 SAMPLING

Representative sample of the material shall be drawn as

prescribed in IS 10946.

7 TESTS

7.1 Tests shall be carried out by the methods as referred

in COI4 and 5 of Table 1.

7.2 Quality of Reagents

Unless specified otherwise, pure chemicals and distilledwater (see IS 1070) shall be employed in the tests.

NOTE — ‘Pure chemicals’ shall mean chemicals that do not

contain irnpulities which affect the resLdts of analysis.

1

.. ..

IS 15443:2004

Table 1 Requirements for Imidacloprid Technical

(Clause 3.2)

S1 N(). Cb:lractcristics Requirement Method of Test, Ref to

9Annex Of c1 No. Of

this Standard [S 6940(1) (2) (3) (4) (5)

i) Il]lid:lcloprid con[ent, 94.0 A —pwcellt by Il]ass. Miff

Ii) Mois[uw content, percent 1.0 — 4.1by 111;+SS.M{/.r

iii) A~idily (m H,SO,). 0.5 — 11.3percent by I;Iass, Jlmi

ol-

Alkalinity (as NaOH), 0.5 . 11.3

})CI’CIM by !llasS. Mflr,

1

ANNEX A[Table 1, S1No. (i)]

DETERMINATION OF IMIDACLOPRID

A-1 PRINCIPLE

A-1.l Itnidacloprid content is determined by high

performance liquid chromatography (HPLC) equippedwith UV-VIS detector using internal standard tcchoique.

A-2 APPARATUS

A.~. I The high performance liquid chromatograpb

(HPLC) equipped with UV-VIS detector and coupled to

a printer-plotter-c utn-integrator. The operative conditionssaggcsted below arc typical, which can be changed

provided the standardization is done:

Column : 150 mm x 3.9 mm, SS, packedwith Novapak – C 18

Dctcclor : UV (278 nm)

Solvent system : Acetonitrile : Water (80 :20 vh)

Solvent flow rate : l.0 mlhnin

Temperature : Ambient

Snmplc size : 20 pl

A-2.2 Micro Syringe — 5/25 }d.

A-2.3 Glassware — Volumetric flask 100 ml; pipettle10 ml. 20 ml; fmicrosyringe 20 ml.

A-3 REAGENTS

A-3.1 Acetonitrile — HPLC grade or equivalent.

A-3.2 W’ater — HPLC grade or equivalent.

A-3.3 Internal Standard — Acenaphthene AR grade or

equivalent.

A-3.4 Reference Imidacloprid Standard of Known

Purity

A-4 PROCEDURE

A-4.1 Preparation of the Mobile Phase

Mix acetonitrile and water in the proportion of 80:20

(v/v) and pass through membrane filter under vacuum.Homogenize the mixture using a magnetic stirrer andallow to attain the room temperature.

NOTE — Dissolution of acetonitrile in water is cndotbermic.Hence allow the mixing to start at ambient temperature mlcontinue till it attains room temperature.

A-4.2 Preparation of Internal Standard Solution

Weigh out accurately about 0.03 g of acenaphthene into

-.

IS 15443:2004

a 100 ml volumetric flask. Add to it about 40 ml of the

solvent mixture (see A-4.1). Keep it for 30 min withintermittent shaking to dissolve the acenaphthene

completely. Make up the volume upto the mark with thesolvent mixture. Shake well to homogenize the solution.

A-4.3 Preparation of the Standard Solution

Weigh out accurately about 0.1 g of imidacloprid standard

of known purity into a 100 ml volumetric tlask. Add to itabout 40 ml of solvent mixture (see A-4.1). Keep thesolution for 30 min with intermittent shaking for completedissolution. Make up the volume upto the mark with the

solvent mixture (say Solution A).

!’ipette out 10 ml of the solution A into an another 100 ml

volumetric flask. Make up the volume upto the mark with

the solvent mixture and homogenize (say Solution B).

Pipette out 20 ml of the solution B into a third 100 mlvolumetric flask. Add to it 20 ml of internal standard

solution (see A-4.2) and make up the volume with the

solvent mixture (see A-4.1). Shake well to homogenize(say Solution C).

A-4.4 Preparation of the Sample Solution

Weigh OLI[ accurately about the sample containing about

O.I g of imidacloprid into a 100 ml volumetric flask andproceed as in A-4.3.

A-4.5 Estimation

A-4.5.1 Itlject 20 p] of the reference standard solution(,ree A-4.3) followed by the sample solution (see A-4.4)

in[o the HPLC.

From the chromatograms of standard solution and samplesolution measure the peak areas of internal standard andimidacloprid peaks and compute the percentage ofimidacloprid as given in A-6.

NOTE — Use guard column with packing material corasilType II normal phase (sitica get polar) and change the guard

column after 20 injections or when the peak shape gets distufied.

A-4.5.2 Retention Times (Guide Values)

Internal standard (Acenaphthene) — 6.55 min

Imidacloprid — 2.87 min

l’Otal run time — 20.0 min

A-6 CALCULATION

Imidacloprid content, percent by mass = ~ x ~ x q x P

ff12

Al = area of imidacloprid peak in the standard

solution;

A, = area of imidacloprid peak in the samplesolution;

As = area of acenaphthene peak in the standard

solution;

A, = area of acenaphthene peak in the sample

solution;

m] = mass, in g, of the standard;

m, = mass, in g, of the sample; and

P = percentage purity of the standard imidacloprid.

3

,- ..+,,.. .

Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Zndian Standards Act, 1986 to promoteharmonious development of the activities of standardization, marking and quality certification of goodsand attending to connected matters in the country.

Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any formwithout the prior permission in writing of BIS. This does not preclude the free use, in the course ofimplementing the standard, of necessary details, such as symbols and sizes, type or grade designations.

Enquiries relating to copyright be addressed to the Director (Publications), BIS.

Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewed

periodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. FAD 1 (1345).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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