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IS 15443 (2004): Imidacloprid Technical [FAD 1: Pesticides

and Pesticides Residue Analysis]

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IS 15443:2004

Indian Standard
IMIDACLOPRID

TECHNICAL SPECIFICATION

Ics

65.100.10

0 BIS 2004

BUREAU
MANAK

OF

INDIAN

STANDARDS

BHAVAN, 9 BAHADUR SHAH

NEW DELHI 110002

ZAFAR

MARG

Price Group 2

/kf(//l/l 2004

,.

>.,-

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 Division
coLlncil.
Imidacloprid

twhni~al,

is employed

in the preparation

Imidacloprid is the accepted common

I-((khlor[~-3-pyridinyl)
metbyl-4,5-dihy
E//lpiri[ (// Forlnulo

CgH,,CINfO,

of insecticidal

formulations.

name by the International

Organization
dro-N-nitro- 1-H-imidazole-2-amine.
Str[lc~uml Fornudu

for Standardization

Moleculur

5?

NH

(1S0) for

Muss

255.6

No

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 the
RLIICS 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 01a test or analysis, shall be rounded off in accordance with IS 2: 1960 Rules for
rounding 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
]egib]y and indelibly the following information in addition
to any other information
as is necessary under the
Insecticide Act, 1968 and Rules framed thereunder:

1 SCOPE
This standard prescribes the requirements and the methods
of sampling and test for imidacloprid technical.

a) Name of the material;

b) Name and address of the manufacturer;

2 REFERENCES

c) Batch number;
The following standards contain provisions which through
reference in this text, constitute provisions of this standard.
At the time of publication, the editions indicated were
valid. All standards are subject to revision and parties to

d) Date of manufacture;
e) Date of expiry;
f) Net mass of contents;
g) Nominal
(m/m);

agreements based on this standard are encouraged to

investigate 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

imidacloprid

technical

content, percent

h) 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

Title
Reagent
grade water (third
flevision)
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 technical
grtlde pesticides (jirst revision)

required
j) Any other information
Standards of Weights and Measures
Commodities) Rules, 1977.
5.2 BIS Certification
The product
Mark.

under the
(Packaged

Marking

may also be marked

with the Standard

5.2.1 The use of the Standard Mark is governed by the

provisions of the Bureau of Indian Sturtdards Act, 1986
and the Rules and Regulations made thereunder. The
details of conditions under which the licence for the use
of the Standard Mark may be granted to manufacturers
or producers may be obtained from the Bureau of Indian
Standards.

3 REQUIREMENTS
3.1 Description
The material shall be in the ~orm of cream to off white
coloured powder. It shall be devoid of hard aggregates
and free from extraneous impurities or added modifying
agents,

6 SAMPLING
Representative sample of the material shall be drawn as
prescribed in IS 10946.

3.2 The ma[erial shall also comply with the requirements

given in Table 1.

7 TESTS
4 PACKING
7.1 Tests shall be carried out by the methods as referred
in COI4 and 5 of Table 1.

h4aterial shall be packed in polyethylene bags closed

sui[ably and further inserted in[o fibreboard drums (we
IS 7601) with a ring clwnp/clip acting as a tampcrproof
device. The containers
shall also comply with the
requirements given in IS 8190 (Part 1).

7.2 Quality of Reagents

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

5 MARKING

NOTE Pure chemicals

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

shall mean chemicals

that do not

contain irnpulities which affect the resLdts of analysis.

.. ..

IS 15443:2004
Table 1 Requirements for Imidacloprid
(Clause 3.2)
S1 N().

Cb:lractcristics

Ii)

iii)

Requirement

Method of Test, Ref to

(2)

(3)

Annex Of
this Standard
(4)

Il]lid:lcloprid con[ent,
pwcellt by Il]ass. Miff

94.0

(1)
i)

Technical

Mois[uw content,
by 111;+SS.
M{/.r

percent

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

9
c1 No. Of
[S 6940
(5)

1.0

0.5

11.3

0.5

11.3

4.1

olAlkalinity (as NaOH),

})CICIM

by !llasS. Mflr

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

OF IMIDACLOPRID

A-1 PRINCIPLE

A-3 REAGENTS

A-1.l Itnidacloprid
content is determined
by high
performance liquid chromatography
(HPLC) equipped
with UV-VIS detector using internal standard tcchoique.

A-3.1 Acetonitrile

A.~. I The high performance

liquid

Standard

Acenaphthene

AR grade or

chromatograpb

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

a printer-plotter-c utn-integrator. The operative conditions
saggcsted below arc typical, which can be changed
provided the standardization is done:

Dctcclor
Solvent system
Solvent flow rate
Temperature
Snmplc size

: 150 mm x 3.9 mm, SS, packed

with Novapak C 18
: UV (278 nm)
: Acetonitrile : Water (80 :20 vh)
: l.0 mlhnin
: Ambient
: 20 pl

A-2.2 Micro Syringe

5/25 }d.

Column

A-3.2 Water HPLC grade or equivalent.

A-3.3 Internal
equivalent.

A-2 APPARATUS

HPLC grade or equivalent.

A-2.3 Glassware Volumetric flask 100 ml; pipettle

10 ml. 20 ml; fmicrosyringe 20 ml.

A-3.4 Reference
Purity

Imidacloprid

Standard

of Known

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 and
allow to attain the room temperature.
NOTE Dissolution of acetonitrile in water is cndotbermic.
Hence allow the mixing to start at ambient temperature ml
continue till it attains room temperature.

A-4.2 Preparation
Weigh out accurately

-.

of Internal Standard Solution

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 with
intermittent
shaking to dissolve the acenaphthene
completely. Make up the volume upto the mark with the
solvent mixture. Shake well to homogenize the solution.

A-4.3 Preparation

From the chromatograms of standard solution and sample

solution measure the peak areas of internal standard and
imidacloprid
peaks and compute the percentage of
imidacloprid as given in A-6.
NOTE Use guard column with packing material corasil
Type II normal phase (sitica get polar) and change the guard

of the Standard Solution

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

Weigh out accurately about 0.1 g of imidacloprid standard

of known purity into a 100 ml volumetric tlask. Add to it
about 40 ml of solvent mixture (see A-4.1). Keep the
solution for 30 min with intermittent shaking for complete
dissolution. Make up the volume upto the mark with the
solvent mixture (say Solution A).

A-4.5.2

!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).

Retention Times (Guide Values)

Internal standard (Acenaphthene)

6.55 min

Imidacloprid

2.87 min

20.0 min

lOtal

run time

A-6

CALCULATION

Imidacloprid

content, percent by mass = ~

x ~

x q

x P

ff12

Pipette out 20 ml of the solution B into a third 100 ml

volumetric 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

Al = area of imidacloprid
solution;

of the Sample Solution

Weigh OLI[ accurately about the sample containing about

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

in the standard

A, = area of imidacloprid
solution;

peak

As = area of acenaphthene
solution;

peak in the standard

A, = area of acenaphthene
solution;

A-4.5 Estimation

peak

peak

in the sample

in the sample

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

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.

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

P = percentage

,- ..+,,.. .

purity of the standard imidacloprid.

Bureau of Indian Standards

BIS is a statutory institution established
under the Bureau
harmonious development
of the activities of standardization,
and attending to connected matters in the country.

of Zndian Standards Act, 1986 to promote

marking and quality certification
of goods

Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced in any form
without the prior permission
in writing of BIS. This does not preclude the free use, in the course of
implementing
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
periodically; a standard along with amendments is reaffirmed when
needed; if the review indicates that changes are needed, it is taken
should ascertain that they are in possession of the latest amendments
BIS Catalogue and Standards: Monthly Additions.
This Indian Standard has been developed

from Doc : No.

Amendments
Amend No.

of comments. Standards are also reviewed

such review indicates that no changes are
up for revision. Users of Indian Standards
or edition by referring to the latest issue of

FAD 1 (1345).

Issued Since Publication

Text Affected

Date of Issue

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