IS 15229: Metolachlor Technical

10 Pages·2002·1.1 MB·English

by  Bureau of Indian Standards

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IS 15229 (2002): Metolachlor Technical [FAD 1: Pesticides
and Pesticides Residue Analysis]
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IS 15229:2002

Indian Standard
METOLACHLOR~C~Cfi’- SPECIFICATION
,.
ICS 65.100.20

,’
CI BIS2002
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Price Group 2
November 2002
I
Pesticides Sectional Committee, FAD 1
FOREWORD
This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Pesticides
Sectional Committee had been approved by the Food and Agriculture Division Council.
Metolachlor technical is employed in the preparation of herbicidal formulations for agricultural use.
Metolachlor is the accepted common name by the International Organization for Standardization 1S0) for
2-chloro-6-ethyl-N-(2 -methoxy-1-methylethyl) acet-o-toluidide.
The empirical and structural formula and the molecular mass of metolachlor are given below:
Empirical Formula Structural Formula Molecular Mass
C15H22CIN02 283.8
CH3 O
— CH2CI ,
>
\ / ‘~CH3
4-
‘CH20CH
‘C2H5
3
In the preparation of this standard due consideration has been given to the provisions
of Insecticide Act, 1968 and the Rules framed thereunder. However this standard is subjected to restrictions
imposed under the Act and Rules wherever applicable.
For the purpose of deciding whether aparticular requirement ofthis standard iscomplied with, the final value,
observed or calculated, expressin g the result of a test or analysis, shall be rounded off in accordance with

IS2: 1960‘Rules forrounding off n umerical values(revised)’. Thenumber ofsignificant places retained inthe

rounded off value should be the same asthat of the specified value inthis standard.
\’>
IS 15229:2002
Indian Standard
METOLACHLOR TECHNICAL — SPECIFICATION
1SCOPE information as required under the Insecticides Act,
1968 and Rules framed thereunder:
This standard prescribes the requirements, methods
of sampling and test for metolachlor technical. a) Name of the material;
b) Name and address of the manufacturer;
2 REFERENCES
c) Batch number;
The following Indian Standards contain provisions d) Date of manufacture;
which through reference in this text, constitute e) Dateof expiry;
provisions ofthis standard. Atthetimeofpublication, 8 Net mass of contents;
the editions indicated were valid. All standards are g) Nominal metolachlor content, percent(m/m);
subject to revision, and parties to agreements based and
on this standard are encouraged to investigate the h) A cautionary notice worded as in the
possibility of applying themost recent editions ofthe Insecticides Act, 1968 and Rules framed
standards indicated below: thereunder; and Standards of Weights. and
Measures (Packaged Commodities) Rule.Y,
1SNo. Title 1977.
1070:1992 Reagentgradewater(third revision)
Table 1Requirements for Metolachlor Technical
2552:1989 Steel drums (galvanized and
ungalvanized) (third revision) (Clause 3.2)
6940:1982 Methods of test for pesticides and
SI Characteristic Require- Method of
their formulations (first revision) No. ments Test, Refto
8190 Requirement for packing of pes-
~
(Part 2): 1988 ticides: Part 2 Liquid pesticides c1No.Of
ofthis IS6940
(second revision)
Standard
10946:1996 Method of sampling for technical
(1) (2) (3) (4) (5)
grade pesticides (/irst revision) i) Metolachlor con- 95.0 A — ------
tent, percent by
3 REQUIREMENT mass,J4in
ii) Moisture content 0.20 - 4
3.1 Description percent by mass, b
Max
The material shall be in the form of a liquid, light iii) Material insoluble 0.15 - 9
in acetone, percent
yellow to yellowish brown in colour, free from
bymass,M2ZX
extraneous impurities or added modi~ing agents. iv) Acidity as HzSO,, 0.50 - 11,3.2
percent by mass,
3.2 The material shall also comply with the Max
requirements given in Table 1.
3.3 Determination of Metolachlor Content
5.2 BIS Certification Marking
Either Annex A or Annex B shall be used. However,
The product may also be marked with the Standard
in case of dispute, Annex A shall be the referee
Mark.
method.
5.2.1 The use of the Standard Mark is governed by
4PACKING the provisions of the Bureau of Indian Standards
Act, 1986 and the Rules and Regulations made
Thematerial shallbepacked inmild steeldrums. Mild
thereunder. The details of conditions under which the
steel drums shall conform to IS2552. The packaging
Iicence for the use of the Standard Mark may be
shall also conform to the general requirements given
grantedtomanufacturers orproducers maybe obtained
in IS 8190 (Part 2 ). from the Bureau of Indian Standards.
5 MARKING 6 SAMPLING
5.1The containers shall bear legibly and indelibly the Representative samples ofthematerial shall bedrawn
following information in addition to any other according to IS 10946.

1
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IS 15229:2002 ;.,i;,1
q
7 TESTS 7.2 Quality of Reagents -
Unless specified otherwise, pure chemicals and
7.1 Tests shall be carried out by the methods referred
distilled water(seeIS 1070)shallbeemployed intests.
inCOI4 and 5 of Table 1.
NOTE— ‘Purechemicals’ shall meanchemicals that do not
containimpurities,whichaffecttheresultsofanalysis.
ANNEX A
[Table 1, Item (i) and Clause 3.3]
DETERMINATION OF METOLACHLOR CONTENT
A-1 PRINCIPLE A-4 PROCEDURE
Metolachlor content is determined by gas chromato- A-4.1 Preparation of Internal Standard Solution
graphy, using internal standard technique.
Weigh out accurately 1.8g of methyl palmitate into
a 250 ml volumetric flask. Dissolve in dichloro-
A-2APPARATUS
methane andmake upthe volume upto the mark with
A-2.1 Gaschromatography(GLC) isequipped withFID dichloromethane. Shake well to homogenize.
and iscoupled toaprinter-plotter-cum integrator. The
operative conditions suggestedbelow aretypicalwhich A-4.2 Preparation of Standard Solution
can be changed provided standardization isdone:
Weighoutaccurately 0.200gofmetolachlor reference
Column : Glass, length= 1.8m, I.D. = standardofknownpurity intoa25mlvolumetric flask.
2mm, packed with 3percent Add 20ml ofthe internal standard solution and make --...-
Silicon 0V-225 ongaschrom up the volume upto the mark with dichloromethane.
Q, 80-100 mesh. Shake well to homogenize.
iJ
Temperatures : Temperature oven – 150”C
for 8 m in. Temperature A-4.3 Preparation of Sample Solution

programmin g at 1O°C/minto Weigh outaccurate quantity ofasample equivalent to
170”C for 10min. 0.2 g of metolachlor into a 25 ml volumetric flask.
Injector : 230°C. Add 20 ml ofthe internal standard solution and make
up the volume upto the mark with dichloromethane.
Detector : 270”C.
Shake well to homogenize.
Carrier gas : Nitrogen :30 ml/min
Hydrogen : 30 ml/min A-4.4 Estimation
Air : 300 ml/min
A-4.4.1 Inject 1 ml of standard solution until the
internal standardlreference substance area quotients
A-2.2 Microlitre Syringe — 5/10 ml capacity.
oftwo successive chromatograms donot deviate from
A-2.3 Standard Glassware each other by more than 2 percent. Then use the
following injection sequence:
A-3 REAGENTS
.-cs,s,,CS2S2c, S3S3...
A-3.1Dichloromethane — AR grade or equivalent.
where
A-3.2 Internal Standard —Methyl palmitate —AR
C= standard solution, and
grade or equivalent.
S = sample solution (1,2, 3, ....n).
A-3.3 Metolachlor Reference Standard —of known
purity.

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IS 15229:2002 4
From the chromatograms of standard solution and where
sample solution measure the peak areas of internal &f, = mass in g of standard metolachlor in
standard and metolachlor peaks and compute the
standard solution,
percentage ofmetolachlor as given in A-5. &f, . mass ing ofthe sample taken for test,
A-4.4.2 Retention Time Guide Values A, = peak area of metolachlor in the chrolma-
togram of standard solution,
Methyl palpitate : 4.8min
A, = peak area of metolachlor in the chroma-
Metolachlor : 12.4min
togram of sample solution,
A-4.4.3 Total Run Time —20min. A, = peak areaof internal standard inthe chro-
matogram of standard solution,
A-5 CALCULATIONS
A4 = peak areaofinternal standard inthe chro-
Metolachlor content, = Mlx A~xAzx P matogram of sample solution, and
percent by mass P= percentage purityofmetolachlor reference
A4,xA4x A,
standard.
ANNEX B
(Clause 3.3)
DETERMINATION OF METOLACHLOR CONTENT
B-1 PRINCIPLE B-3.2 Internal Standard — Methyl Stearate — AR
grade or equivalent.
Metolachlor content is determined by gas chromato-
graphy, using internal standard technique. B-3.3Metolachlor Reference Standard —ofknown
purity.
B-2APPARATUS
B-4 PROCEDURE
B-2.1Gaschromatography(GLC) isequippedwithFID
and iscoupled toaprinter-plotter - cum integrator. The
B-4.1 Preparation of Internal Standard Solution
operativeconditions suggestedbelow aretypicalwhich
can be changed provided standardization isdone. Weigh out accurately 1.8g of methyl stearate into a
250mlvolumetric flask.Dissolve indichloromethane
Column : Glass/S.S., length = 1.8 m,
and make up the volume upto the mark with
I.D. = 2 mm, packed with
dichloromethane. Shake well to homogenize.
10percent OV-101 on gas
chrom Q, 80-100 mesh.
B-4.2 Preparation of Standard Solution
Temperatures : Column — 240”C.
Weigh out accurately 0.2 g of metolachlor reference
Injector — 270”C.
standardofknownpurity intoa25mlvolumetric flask.
Detector — 270°C.
Add 20ml ofthe internal standard solution and make
Carrier gas : Nitrogen :30 ml/min.
up the volume upto the mark with dichloromethane.
Hydrogen : 30 ml/min.
Shake well to homogenize.
Air 300 ml/min.
B-4.3 Preparation of Sample Solution
B-2.2 Microlitre Syringe — 5/1Oml capacity.
Weigh out accurately quantity of asample equivalent
B-2.3 Standard Glassware to 0.2 gofmetolachlor into a25 ml volumetric flask.
Add 20ml ofthe internal standard solution and make
B-3 REAGENTS
up the volume upto the mark with dichloromethane.
B-3.1Dichloromethane — AR grade or equivalent. Shake well to homogenize.

3
IS 15229:2002
B-4.4 Estimation B-4.4.3 Total Run Time — 10min.
B-4.4.1 inject 1pl ofreference standard solution until B-5 CALCULATIONS
the internal standard/reference substance area
quotients of two successive chromatograms do not Metolachlor content, A4.xA. x.z LxP
percent bymass = ‘ -
deviate from each other by more than 2percent.Then Mz XA4X-A,
use the following injection sequence.
where
c s,s,,cS2S*c, S3S3,- &f, . massingofstandardmetolachlor instand-
ard solution,
where
M, = mass ing of the sample taken for test, ..
C = Reference solution, and
A, = peak area of metolachlor in the chroma-
s = Test solution (1,2, 3, ....n),
togram of standard solution,
From the chromatograms of standard solution and A, = peak area of metolachlor in the chroma-
sample solution measure the peak areas of internal togram of sample solution,
standard and metolachlor peaks and compute the A, = peak area ofinternal standard inthe chro-
percentage of metolachlor as given in A-5. matogram of standard soIution,
B-4.4.2 Retention Time (Guide Values) A, = peak area ofinternal standard inthe chro-
matogram of sample solution, and
Metolachlor : 3.1 min.
P= percentagepurityofmetolachlor reference
Methyl stearate : 4.5 min. standard.
,.
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development of the activities of standardization,marking and quality certification of goods and attending to
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Amendments are issued to standards asthe need arises onthe basis ofcomments. Standards are also reviewed
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should ascertain that they areinpossession ofthe latest amendments oredition byreferring tothe latest issue of
‘BISCatalogue’ and’ Standards: Monthly Additions’.
This Indian Standard has been developed from Dot: No. FAD 1(1093).
Amendments Issued Since Publication
Amend No. Date ofIssue Text Affected
I,, 1
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