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है”ह”ह

IS 15163 (2002): Isoprothiolane, Technical [FAD 1:Pesticides and Pesticides Residue Analysis]

IS 15163:2002

$TRdhw’-=m-

3Tl$TiEim-a$r~,WA’i$l –Rilmz

Indian Standard

ISOPROTHIOLANE, TECHNICAL — SPECIFICATION

ICS 65,100.30

0 BIS 2002

BLJREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

(k’/(J/~Lfr2(102 Price Croup 2

I’csticidcs Sectional Cotnmittee. FAD I

FORI.WORD

I“l~isIndian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the PesticidesSectional Committee had been approved by the Food and Agriculture Division Council.

l~oprothiolane, technical is used in fungicidal formulations.

lsopmthiolane is the common name accepted by the International Organization for Standardization (I SO) for[)iisopropyl 1,3-dithiolan-2-yl idenemalonate.

I“hu empirical formula, structural formula and the molecular mass are as given below:

/.’/llpiri~al Formula Structural Formula

C,,111804S2

Molecular Ma,v,Y

290.39

0

In the preparation of this standard, due consideration has been given to the provisions of the [rrsecticiak.s ,4LI[.1968 and the Rules framed thereunder. However this standard is subject to the restrictions imposed under theAct and Rules, wherever applicable.

I’or the purpose of deciding whether a particular requirement of this standard is complied with, the final value,okrved or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2: 1960 ‘Rules for rounding off numerical values (revise@’, The number of significant places retained in therounded off value should be the same as that of the specified value in this standard.

IS 15163:2002

Indian Standard

1SOPROTHIOLANE, TECHNICAL — SPECIFICATION

1 SCOPE

This standard prescribes the requirements and methodsof sampling and test for isoprothiolane, technical.

2 REFERENCFjS

“I_hefollowing Indian Standards contain provisionswhich through reference in this text, constituteprovisions of this standard . At the time ofpublication, the editions indicated were valid. Allstandards are subject to revision, and parties toagreements based on this standard are encouragedto investigate the possibility of applying the mostrecent editions of the standards indicated below:

ILT,vo.

1070: 1992

6940:

1783(Part

glo(-)

982

) :1993

(Part 1) : 1988

10946: 1996

TitleReagent grade water (thirdrevision)Methods of test for pesticides andtheir formulations (first revision)Drums, large, fixed ends —Specification: Part 1 Grade Adrums (third revision)Requirements for packing ofpesticides: Part 1 Solid pesticides(second revision)Methods of sampling for technicalgrade pesticides ~rst revision)

3 REQUIREMENTS

3. I Description

“rhe lmaterial shall be in the form of crystallineflakes, off-white to yellowish in colour, free fromextraneous matter.

3.2 The material shall also comply with therequirements given in Table 1.

3.3 Iwo methods, namely, gas chromatographicmethod and high performance liquid chromato-graphic (HPLC) method have been prescribed forthe determination of isoprothiolane content.Ilowever, HPLC method is considered as refereemethod.

4 PACKING

The material shall be packed in mild steel drums[S(JL IS 1783 (Part 1)] containers provided with aLDPE liner of thickness not less than 0.062 mm.The general requirements as given in IS 8190(Part 1) shall also be followed.

Table 1 Requirements for Isoprothiolane,Technical

(Cfauses 3.2 and 7. 1)

SI Characteristic Requirement Method of Test, Ref toNo. ~

(3 No. ofthis Standard IS 6940

(1) (2) (3) (4) (5)i) lsoprothiolaoe 96.0 A and B —

eontent, percent bymass, A4in

ii) Acidity (as HzSO+), 1.00 — 11.3percent by mass,Max

iii) Material insoluble 0.10 — 9

in acetone, percentby mass, MUX

iv) Moistore content, 0.50 4

percent by mass,Max

5 MARKING

5.1 The containers shall bear legibly and indelibly thefollowing information in addition to any other

information as required under the Insecticide’s

Act, 1968 and Rules framed thereunder:

a)

b)

c)

d)

e)

8

g)h)

j)

Name of the material,

Name and address of the manufacturer,

Batch number,

Date of manufacture,

Date ofexpiry,

Net mass of contents,

Nominal isoprothiolane content, percent (m/m),

A cautionary notice as worded in theInsecticides Act, 1968 and Rules framedthereunder, and

Any other information required under theStandards of Weights and Measurcq(Packaged Commodities) Rules, 1977,

5.2 BIS Certification Marking

The product may also be marked with the StandarcfMark.

5.2.1 The use of the Standard Mark is governed b>the provisions of the Bureau of Indian Standards Act,

1986 and the Rules and Regulations made thereunder,The details of conditions under which the Iicence forthe use of the Standard Mark may be granted tomanufacturers or producers may be obtained from theBureau of Indian Standards.

IS 15163:2002

6 SAMPLING 7.2 Unless specified otherwise, pure chemicals and

Representative samples of the material shall be drawnreagent grade water (see IS 1070) shall be employedin tests.

according to IS 10946.NOTE — ‘Pure chemicals’ shall mean chemicals that

7 TESTS do not contain impurities which affect the results of

7. I I’ests shall be carried out by the methods referred analysis.

in COI 4 and 5 of Table 1.

ANNEX A

[Table 1, S1 No. (i)]

DETERMINATION OF lSOPROTHIOLANE CONTENT

A-1 GAS CHROMATOGRAPHY METHOD

A-1.1 Principle

For the determination of isoprothiolane content a gasliqLI id chromatographic method with internal standardtechnique has been specified.

A-2 APPARATUS

A-2.1 Gas Chromatography

A gas chromatography equipped with flame ionizationdetector and a printer-plotter-cum-integrator is usedft~r this determination. The suggested parameters areas follows, but can be changed provided standardi-zation is done:

C‘o[wnn : Glass, length 2 m, ID 5 mm,

packed with 5 percent SE-30on Chromosorb WHP(80-100 mesh).

Temperature : Column oven : 21O”CInjection port : 240°CDetector : 260°C

Cta.s F-low Rates : Nitrogen 30 ml/minHydrogen 30 ml/minAir 300 ml/min

A-2.2 Microlitre Syringe — 10pl capacity.

A-2.3 Standard Glassware

A-3 RETENTION TIME (GUIDE VALVES)

A-3.1 lsoprothiolane — 3.8 min.

A-3.2 Internal Standard -— 2.2 min.

A-3.3 Total Run Time — 5 min.

A-4 REAGENTS

A-4.1 Standard Isoprothiolane — of known purity.

A-4.2 Di-Butyl Phthalate — AR grade or equivalent.

A-4.3 Acetone — AR grade or equivalent.

A-5 PROCEDURE

A-5.1 Preparation of Internal Standard Solution

Weigh about 4.5g of di-butyl phthalate into a

250-ml volumetric flask and make up to volume withacetone.

A-5.2 Preparation of Standard IsoprothiolaneSolution

Weigh accurately about 0.08g of standard isoproth io-Iane into a 50-ml volumetric flask. Add 5 m I acetone

into a volumetric flask and shake well to dissolve. Add5 ml of IS internal standard solution (A-5.1) and makeup the volume with acetone.

A-5.3 Preparation of Sample Solution

Weigh accurately a quantity of sample equivalent to

about 0.08 g of isoprothiolane in a 50-ml volumetricflask. Add 5 ml acetone into the volumetric flask andshake well to dissolve. Add 5 ml of IS internal standardsolution (A-5.1) and make up the volume with acetone.

A-5.4 Estimation

Inject 1 WIstandard solution until the area quotient 01internal standard/reference standard of two successivechromatograms do not deviate from each other by morethan 2 percent.

Then use the following injection sequence:

. . . . . . . . . . . . CS, S, CS7S, CS3 ............

2

where

1S 15163:2002

where

(’ = Standard solution, and

s = Sample solution ( 1,2, . . . ... n).

From the chromalograms of the standard solution andsample solution, measure the peak areas of the activeingt-edient and the internal standard and calculate thepercentage of the active ingredient as given incalculations (A-6).

A-6 CALCULATION

Isoprothiolane content, M,x A,x[,——percent mlrn XP

A4, xA, x11

Ml = mass in g of standard isoprothiolane,

M2 = mass in g of sample isoprothiolane,

A, = area of isoprothiolane peak in thechromatograrn of standard solution,

A, = area of isoprothiolane peak in thechromatogram of sample solution,

I, = area of internal standard peak in thechromatogram of standard solution,

12 = area of internal standard peak in thechromatogram of sample solution, and

P = percent purity of standard isoproth iolane.

ANNEX B

[Table 1, S1 No. (i)]

DETERMINATION OF lSOPROTHIOLANE CONTENT

B-1 l{IGH PERFORMANCE LIQUIDCHROMATOGRAPHIC METHOD

B-1.1 Principle

Isoprotbiolane content is determined by using highperformance liquid chromatography (HPLC) using theitllernal standard technique.

B-2 APPARATUS

B-2.1 High Performance Liquid Chromatography

A high performance liquid chromatography equippedJ! ith ul[ra-violet ([JV) detector and a printer-plotter-

~1{)~~-integrator is used for this determination. Thesuggested operative parameters are as follows, but canbc changed, if necessary, provided standardization is

done:

( “(l[l{) )7/7

250’mm 1D4.6 mm’1$~1%: S.S. or equivalent

with Nu;leosil C18 (manu-facturing by Phenomenex).

,110/7ilc, ph(l.sc : Acetonitrile : Water(70 :30, v/v)

[’/(11{I’cltl’ : 1.0 ml/min

1/‘<[t’,’IJc’n,yfh 280 run

IIljc’cli(jtl l(~[utne : ~ microlirres

B-2.2 Microlitre Syringe — 50 PI

B-2.3 Standard Glassware

B-3 RETENTION TIME (GUIDE VALVES)

B-3.1 lsoprothiolane (a.i.) — 6.5 min

B-3.2 Acetophenone (Internal Standard) — 4,2 min

B-3.3 Total Run Time — 10 min

B-4 REAGENTS

B-4,1 Internal Standard, Acetophenone --- AR

grade or equivalent.

B-4.2 Acetonitrile — HPLC grade.

B-4.3 Water — HPLC grade.

B-4.4 Isoprothiolane Standard — of known put-it}

B-5 PROCEDURE

B-5. I Preparation oflnternal Standard Solution

Weigh about 5 g acetophenone into a 100 ml volumetricflask and make up the volume with acetonitrile.

B-5.2 Preparation of Standard Solution

Weigh accurately about 0.1 g of isoprothiolane

3

IS 15163:2002

standard into a 100 ml volumetric flask, add 5 mlinternal standard solution (B-5.l)and make up tovt~lumc with acetonitrile.

B-5.3 Preparation of Sample Solution

W’cigh accurately about 0.1 g of isoprothiolane into a100 ml volumetric flask, add 5 ml internal standards~~lution (B-5. I ) and then make up to the volume with

accto nitri le.

B-%-f Estimation

Inject standard solution until the area quotient ofinternal standard/reference standard of two successivechromatograms do not deviate from each oLher by moretil<}n2 percent.

[’hen use the following injection sequence:

,,,...C.....C’.Y..SICLY.S2CY..............

where

~.-- standard solution, and

,Y sample solulion (1, 2, . . . . n).

From the chromatograms of the standard solution, and

sample solution measure the peak areas of the activeingredient and the internal standard and calculate thepercentage of the active ingredient as given in B-6.

B-6 CALCULATION

[soprothiolane content, M,x A,x I, ..,.—percent, tnlm

— ‘Xt’M. x A, x [.

where

~, =

M, =

A, =

A, =

I, =

[2 =

P=

‘1,

mass in g of standard isoprothiolane.

mass in g of isoprothiolane sample,

area of isoprothiolane peak inchromatogram of standard solution,

area of isoprothiolane peak inchromatogram of sample solution,

area of internal standard peak inchromatogram of standard solution,

area of internal standard peak in

tile

tile

the

thechromatogram of sample solution, and

percent purity of isoprothiolane standard.

131S k (i ~,lat{ltory institution established under the Bureau of /ttdian Standards Act, 1986 to promoteh:irll](~nic~us development of the activities of standardization, marking and quality certification of goods,Ind at[cn dins toconnected matters in the country.

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im~~lcmcnting the standard, of necessary details, such as symbols and sizes, type or grade designations,

I’OL]II il-ic~ wlating to copyright be addressed to the Director (Publications), BIS.

l{c~icw of [ndian Standards

/! IIIcnd Incnts arc issued to standards as the need arises on the basis of comments. Standards are also reviewed

pet-it~dicall~: a standard along with amendments is reaffirmed when such review indicates that no changes areilccdtxi; if [he review indicates that changes are needed, it is taken up for revision. Users of Indian Standards~h~~llldascertain that they are in possession of the latest amendments or edition by referring to the Iatcst issue of

‘111S [’:~l:llo~!ae” and ‘Standards: Monthly Additions’.

lhli Itldian Standard has been developed from Doc : No. FAD 1 (logo).

Amendments Issued Since Publication

—Amend N(o, Date of Issue Text Affected

—

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