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IS 15600 (2005): Cymoxanil , Technical [FAD 1: Pesticidesand Pesticides Residue Analysis]

IS 15600:2005

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Indian Standard

CYMOXANIL, TECHNICAL — SPECIFICATION

ICS 65.100.30

. . ..

0 BIS 2005

BUREAU O-F INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

November 2005 Price Group 2

..

Pest icicles and Pesticides -Residue Analysis Sectional Committee, FAD I

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Pesticidesand Pesticides Residue Analysis Sectional Committee had been approved by the Food and Agriculture DivisionCouncil.

Cymoxanil, technical is employed in the preparation of fungicidal formulations for agricultural use.

Cymoxanil is the accepted common name by the International Organization for Standardization ( 1S0 ) for~-cyano-N-[ ( ethylamino ) carbonyl ]-2-( methoxyimino ) acetamide.

The empirical and structural formulae and the molecular mass of cymoxanil are given below.

Empirical Formula Structural Formula Molecular Mass

C7H10N403 HI 198.18

N=C-C-C-NH-C-NH-CHZCH3

IINOCH3

In preparation of this standard, due consideration has been given to the provisions of the Insecticides A c(,1968 and the Rules framed thereunder. However, this standard is subject to the restrictions imposed under theInsecticides Act, 1968 and Rules, wherever applicable.

For the purpose of deciding whether a particular requirement of this standard is complied with the finalvalue, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordancewith 1S2: 1960 ‘Rules for rounding off numerical values ( revised)’. The number of significant places retainedin the rounded off value should be the same.as that of the specified value in this standard.

IS 15600:2005

Indian Standard

CYMOXANIL, TECHNICAL — SPECIFICATION

1 SCOPE

This standard prescribes the requirements andthe methods of sampling and test for cymoxanil,technical.

2 REFERENCES

The following standards contain provisions which

through reference in this text, corrstitute provisionsof this standard. At the time of publication, theeditions indicated were valid. All standards aresubject to revision and parties to agreements basedon this standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below:

IS No.

1070:1992

6940:1982

8190(Part I ):”1988

10946:1996

Tit[e

Reagent grade water ( thirdrevision )

Methods of test for pesticides andtheir formulations (jht revision)

Requirements for packing ofpesticides: Part 1 Solid pesticides( second revtiion )

Methods of sampling for technicalgrade pest icicles (first revision )

3 REQUIREMENTS

3.1 Description

The material shall be in the form of peach colouredhomogeneous powder, free tlom extraneous impuritiesand hard lumps.

3.2 The material shall also comply with requirementsgiven in Table 1.

4 PACKING

The product shall be packed” in multi-layered bagof capacity 20 kg with suitable leak proof andpilfer proof closure system. The container shallalso conform to the general requirements as given .inISt3190(Part 1).

5 MARKING

5.1 The containers shall bear legibly and indeliblythe folIowing information in addition to theinformation as is necessary under the InsecticidesAct, 1968 and Rules framed thereunder:

a)

b)

c)

d)

e)

f)

13)

h)

.0

Name of the material;

Name and address of the manufacturer;

Batch number;

Date of manufacture;

Date ofexpiry;

Net mass of contents;

Nominal cymoxanil content, percent (m/m);

Cautionary notice as worded in InsecticidesAct, 1968 and Rules framed thereunder; and

Any other information required under IheStandards of Weights ‘and Measures(Packaged Commodities) Rules,.1 977.

5.2 BXSCertification Marking

The product may also be marked with the StandardMark.

5.2.1 The use of the Standard Mark is governed bythe provisions of the Bureau of Indian StandardsAct, 1986 and the Rules and Regulations madethereunder. The details of conditions under which

Table 1 Requirements for Cymoxanil, Technical

( Clause 3.2)

S1 No. Characteristic Requirement Method of Test, Ref to

Annex of Clause No. ofthis Standard IS 6940

(1) (2) (3) (4) (5)

i) Cymoxanil content, percent by mass, &fin 96.0 A —

ii) Material insoluble in acetone, percent by mass, Mm 0.1 — 9

iii) Moisture content, percent by mass, Mox 0.2 — 4.2

iv) Acidity ( as H2S04 ), percent by mass, Max 0.2 — 11.3.2

1

Is 15600:2005

the -Iicence for the use of the Standard Mark maybegranted to manufacturers or producers may beobtainedfiom the Bureau of Indian Standards.

6 SAMPLING

Representative samples of the material shall be drawnas prescribed in IS 10946.

7 TESTS

7.1 Tests shalj be carried out by the methods referred

to in COI4 and 5 of Table 1.

7.2 Quality of Reagents

Unless specified otherwise, pure chemicals andreagent grade water (see IS 1070) shall be employedin tests.

NOTE — ‘Pure chemicals’ shall mean chemicals thatdo not contain impurities, which affect the results ofanalysis.

ANNEX A

( Table 1 )

DETERMINATION OF CYMOXANIL CONTENT

A-1 PRINCIPLE

Cymoxanil content is determined by highperformance liquid chromatography ( HPLC ) usinginternal standard technique.

.A-2 APPARATUS

A-2.1 High Performance Liquid Chramatograph,equipped with a constant flow pump, -constanttemperature column compartment, sample injectorcapabje of injecting 25 pl aliquots, a 254 m wavelengthultraviolet detector.artd a recorder ( digital integratoror other data handjing device ) is used for thisdetermination. The suggested operative parametersare as follows, but can be changed if necessary,provided standardization is done:

Column

Temperature

Mobile phase

Flow rate

Injection vojume :

Detector :

Reverse phase C8, C 18 orequivalent pre-packed column,4.6x 250mm

Ambient

Acetonitrile : Water ( 2“5 :75,v/v ), pH of water= 2.8 adjustedwith 85 percent phosphoric acid

( H~pOq)

1.5ml/min

20 pl

Ultraviolet detector ( 254 nm )

A-2.2 Analytical Balance

A-2.3 Microlitre Syringe — 25 pl.

A-2.4 -FilteringApparatus for Sample and StandardSolutions

A-2.5 Ultrasonic Bath

A-2.+ Standard Glassware

A-3 REAGENTS

A-3.1 Acetonitrile, HPLC grade.

A-3.2 HPLC Grade Water

A-3.3 Acetanilide, ( internal standard ] of known

purity.

A-3.4 Cymoxanil, analytical standard of knownpurity.

A-3.5 Ortho Phosphoric Acid, HPLC grade,85 percent.

A-4 PROCEDURE

A-4.1 Preparation of Mobile Phase

Adjust the pH of water to 2.8 with ortho phosphoricacid. Add 1 500 ml of the pH 2.8 adjusted water to500 ml of acetonitrile in a flask , mix thoroughly.Filter the mixture using the fikering apparatus.

A-4.2 Preparation of Internal Standard

Weigh accurately 400 mg of acetanilide into a100ml volumetric flask. Makeup to volume with HPLCgrade acetonitrile and ultrasonicate for 5 min.

A-4.3 Preparation of Standard Solution

Weigh accurately 35 mg of cymoxanil analyticalstandard of known purity and add it into a 25 mlvolumetric flask. Pipette 5 ml ofacetanilide internalstandard solution into the volumetric flask. Makeup to volume with acetonitrile and mix. Dissolve

ultrasonically for 5 min and filter the standardsolution through 0.45 pm filter.

2

A-4.4 Preparation of Sample Solution

Weigh accurately 35 mg of cymoxanil,-technical andadd it into a 25-ml volumetric flask. Pipette 5 ml ofinternal standard solution in the flask. Make up tovolume with acetonitrile, mix and ultrasonicate for5 min. Filter the solution through the 0.45 pm filter.

A-4.5 Estimation

A-4.5.1 Equilibrate the column with the mobilephase for 45 min before injecting the standard/sample.After the column has equilibrated and a stablebaseline is obtained, inject. in duplicate, 20 p] eachof standard and sample solution.

A-4.5.2 Retention Time

Cymoxanil : 13.Omin

Acetanilide ( Internal standard ) : 8.4 min

Total run time : 15.Omin

A-4.5.3 From the chromatograms of the standardsolution and sample solution measure the peak areasof the active ingredient and the internal standard andcalculate the percentage of the active ingredient as

IS 15600:2005

given in the Calculation ( see A-5).

A-5 CALCULATION

MI XA3XAZXPCymoxanil content, percent m/m = M ~ A x ~

24i

where

M, =

~2 .

A, =

P=

mass of cymoxanil in standard solution,in g;

mass of the sample taken for test, in g;

peak area of cymoxanil in the chromatogramof standard solution;

peak area of-standard cymoxanil in thechromatogram of sample solution;

peak area of internal standard,acetanilide, in the chromatogram ofstandard solution;

peak area of internal standard, acetanilide,in the chromatogram of sample solution;and

percentage purity ofcymoxanil in analyticalstandard.

.

3

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This Indian Standard has been developed from Doc : No. FAD 1( 1534).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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