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Disclosure to Promote the Right To Information


Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”


Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 8701 (1996): Temephos, Technical [FAD 1: Pesticides and


Pesticides Residue Analysis]

“!ान $ एक न' भारत का +नम-ण”


Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”


है”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
IS 8701 : 1996
( Reaffirmed 2001 )

Indian Standard
TEMEPHOS, TECHNICAL - SPECIFICATION

( First -Revision )

ICS 65.100

Q BIS 1996

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARC3
NEW DELHI 110002

Price Group 2
November 1996
Pesticides Sectional Committee, FAD 1

FOREWORD

This Indian Standard ( First Revision ) 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.

Temephos is the accepted common name by the International Organization for Standardization (ISO) for
the 0, 0,0’, O’-tetramethyl 0, 0’ -thiodi-p-phenylene bis (phosphorothioate). The empirical and structural
formulae and the molecular mass of temephos are indicated below:
Empirical Formula Structural Formula Molecular Mass

Cd2006P2S3 466.5

Temephos, technical is employed in the preparation of pesticides formulations. The product has been
registered for production and use in the country under the provisions of Insecticides Act, 1968 and the
Rules framed thereunder. In the preparation of this standard, due consideration has, therefore, been given
to the provisions-of the Act and the Rules framed thereunder as well as Standards of Weights and Measures
(Packaged Commodities) Rules, 1977. However, this standard is subject to therestrictions imposed under
these, wherever applicable.
This standard was first published in 1978. This standard has been revised to incorporate:
a) HPLC method for determination of temephos content in addition to spectrophotometric method,
b) Amendment No. 1, and
c) update referred standards.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final
value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance
with IS 2-: 1960 ‘Rules for rounding off numerical values ( revised )‘. The number of significant ’ places
retained in the rounded off value should be the same as that of the specified value in this standard.
IS 8701 : 1996

Indian Standard
TEMEPHOS, TECHNICAL - SPECIFICATION
( First Revision )

1 SCOPE finally closed with HDPE screw caps. It shall


also conform to general requirements given in IS
1.1 This standard prescribes the requirements and fhe 8190 (Part2) : 1988.
methods of sampling and test for temephos, technical.
5 MARKING
2 REFERENCES
5.1 The containers shall be marked legibly and
The following Indian Standards contain provisions indelibly with the following information:
which, through reference in this text, constitute
provision ofthis standard. At the time of publication, a) Name of the material;
the editions indicated were valid. All standards are b) Name of the manufacturer;
subject to revision and parties to agreements based cl Batch number;
on this standard are encouraged to investigate the
4 Date of manufacture;
possibility of applying the most recent editions of
the standards indicated below: e) Date of expiry;
4 Nominal temephos content, percent ( m/m ),
IS No. Title as registered under the provisions of
6940 : J982 Methods of test for pesticides Insecticides Act, 1968 and the Rules
and their formulations ( first framed thereunder;
revision ) g) Net volume in litres; and
-8190 Requirements for packing of h) Any other information required under
the Insecticides Act, 1968 and the Rules
( Part 2 ) : 1988 pesticides : Part 2 Liquid
framed thereunder and Standards of
pesticides ( second revision )
Weights and Measures ( Packaged
10946: 1996 Method of sampling for Commodities) Rules, 1977.
technical grade pesticides ( first 5.2 BIS Certification Marking
revision )
The product may also be marked with~the Standard
3 REQUIREMENTS Mark.
3.1 Description 5.2.1 The use of the Standard mark is governed by
the provisions of Bureau of Indian Standards Act,
Temephos, technical shall be in the form of pale yellow
1986, and the Rules and Regulations made thereunder.
to brown viscous liquid, free from extraneous
The details of conditions under which the licence
impurities or added modifying agents.
for the use of Standard Mark may be granted to
3.2 The material shall also comply with the manufacturers or producers may be obtained from
requirements specified in Table 1. the Bureau of Indian Standards.

4 PACKING 6 SAMPLING

The material shall be packed in HDPE containers. The 6.1 Representative samples of the material shall be
containers shall be heat sealed with HDPE plugs and drawn as prescribed in IS 10946 : 1996.

1
IS 8701 : 1996
Table 1 Requimments for Temepbos, Technical
( Clause 3.2 )

SI Characteristic Requirement Methods of Test, Rcf to


No. Annex Cl No. of
IS 6940 : 1982
(1) (2) (3) (4) (5)
Temcphos content, percent by mass (m/m). Min 90 A -
9
ii) Moisture conten& percent by mass (m/ml Mar 0.2 4.1

iii) Material insoluble in acetone, percent by mass 0.5 - 9


(m/m), Max

iv) $diy, (as&SO,). pcrccnt by mass 0.3 113.2


m, ax

ANNEX A
[Table 1, Item(i)]
DETERMINATION OF TEMEPIIOS CONTENT

A-O Either of the two methods, namely, HPLC method Mobile phase : n-Hexane : ethyl acetate
(A-l) or Spectrophotometric method (A-2) shall be ( 95 : 5 v/v)
used for determination of temephos content but HPLC
Detector : UV,274nm
method shall be the referee method.
Solvent flow rate : 1.0 ml/min
A-l HIGH PERFORMANCE LIQUID
CIIROMATOGRAPHN=METFIOD Chart speed : 0.25cmimin

A-l.1 Principle Sample size : 10/I!


HPLC unit, equipped with a UV detector , is used for A-1.2.2 Volumetric Flask - 50-m! and 250-m!
estimation of temephos content. A solution containing capacity.
known amounts of the reference standard and internal
is injected into the HPLC unit. Subsequently temephos A-1.2.3 Pipettes (Graduated) - 5-m! and 10-m!
sample is injected and the percentage of temephos capacity.
in the sample is then computed by the standard
relationship. A-1.2.4 Analytical Balance

A-l.2 Apparatus A-1.2.5 Microlitre Syringe - 10 pl capacity


A-1.2.1 High Performance Liquid Chromatograph A-l.3 Reagents
A High Performance Liquid Chromatograph equipped A-1.3.1 Internal Standard - p-nitrophenyl-p-
with a printer- plotter-cum-integrator and UV detector. nitrobenzoate.
The suggestive HPLC operating conditions~are given
below, which can be changed provided standardization A-1.3.2 n-Hexane - HPLC grade.
is done.
A-1.3.3 Ethyl Acetate - HPLC grade.
C&ulUl : Spherical silica, 150 mm
length X 4.6 mm, I. Dstainless A-1.3.4 Refeerence Standard Temephos - of known
steel, 5 pm puirty.

L
IS 8701 : 1996

A-l.4 Preparation of the Standard and Sample A-2 SPECTROPHOTOMETRIC METHOD


Solutions
A-2,1 Principle
A-1.4.1 Preparation of Internal Standard Solution
The sample is dissolved in ethyl acetate and hexane
Weigh 0.12 14 g ofp-nitrophenylp-nitrobenzoate into and chromatographed on silica gel to remove
50-ml volumetric flask and make up the volume to interfering substances. The chromatographed solution
the mark with mobile phase n-Hexane : Ethyl acetate is evaporated to dryness, the residue taken np in
( 95 : 5 v/v ). methanol, and the ultraviolet absorbance of the
methanol solution is compared with a temephos
A-1.4.2 Preparafion of Reference Standard
standard treated in the same way.
Solution
A-2.2 Apparatus
Weigh 0.033 3 g of reference standard temephos of
known purity in 50-ml volumetric flask. Add 5 ml A-2.2.1 Chromatographic Column
internal standard solution ~( see A-1.4.1 ) and
Glass, with a removable fine-porosity fiitted glass plate,
make up the volume to the mark with mobile phase
n-Hexane : Ethyl acetate ( 95 : 5 v/v ). a~teflon stopcock, lOO-ml capacity and 19 mm inside
diameter.
A-1.4.3 Preparation of Sample Solution
A-2.2.2 Funnels - long stemmed, 75-mm diameter.
Weigh a quantity of sample equivalent to contain
0.033 3 g of temephos into 50-ml volumetric flask and A-2.2.3 Round-Bottom Flask - 1 ODO-mlcapacity.
proceed as described in A-1.4.2. A-2.2.4 Spectrophotometer - capable of measuring
A-1.5 Procedure
absorbance in the ultraviolet region.

Inject 10 pl of the reference standard solution into A-3 REAGENTS


the high performance liquid chromatograph (HPLC) A-3.1 Hexane
followed by the sample solution with the help of
microlitre syringe. Measure the peak areas of standard A-3.2 Methanol
and sample solution. Compute the percentage of the
A-3.3 Ethyl Acetate
temephos content in the sample.
A-3.4 Silica Gel - particle size ranging between
A-1.6 Calculation
0.05 mm and 0.20 mm.
Temephos content,
M, xA,xA, NOTE - Different batches of silica gel sometimes show
percent bv mass = XD anomalous chromatographic properties. The absorbance
A,xM,xA, ’ of a standard passed through the column should be at
least 94 percent of the value measured directly. If lower
where values are observed, the batch should be discarded or
its evaluation properties determined and the volumes of

V mass of Reference standard solvents used for chromatographic changed accordingly.


temephos,
A-3.5 Reference Standard Temephos -of known
A, peak area 01 temephos in the sample purity.
solution,
A4PROCEDURE
A, peak arca of internal standard in the
Reference standard solution, A-4.1 Prepare a column for each of the samples to
peak area of temephos in the be assayed, plus one for the reference standard. Fill
A,
Reference standard solution, the lOO-ml glass chromatographic column with
hexane. Weigh 20 f 0.1 g of silica gel and slowly
M, mass of the temephos sample taken
add to the column. Stopper and shake well. Allow the
for the test,
silica gel to settle. Rinse down the column with hexane
A, peak area of internal standard in the to remove any silica gel adhering to the column wall.
sample solution, and Drain excess solvent through until the liquid is 2 to
percentage purity of Reference 3 mm above silica gel.
standard tcmephos.
A-4.2 Weigh accurately about 0.150 g of the sample

3
IS 8701 : 1996

into a 50-ml volumetric flask. Dissolve in 2 ml of ethyl A-4.4 Weigh accurately~o. 150 g of reference standard
acetate, dilute to volume with hexane and mix well. in a 50-ml volumetric flask, add 2 ml of ethyl acetate
Transfer a 15-ml aliquot to the prepared column. Wash to disslove, dilute to volume with hexane. Transfer~a
down the side of the column three times with 5-ml 15-ml aliquot to the prepared column and proceed as
portions of 4 percent ethyl acetate in hexane and described above.
continue to add until a total of 250 ml of the wash
A-4.5 Calculation
solution has passed through the column. Discard the
wash. Temephos content,
A-4.3 Place a 1 OOO-mlround-bottomed flask below A samule
. It!fXD .
X-
percent by mass =
the column and eluate the temephos by passing A standard m
through 500 ml of lo-percent ethyl acetate in hexane. where
Place the flask containing the eluate on a rotary film
A sample = absorbance of the sample at 274
evaporator, and evaporate to dryness under vacuum
using a water bath at 50°C. Remove the flask from r-m%
the evaporator and add by pipette 100 ml of methanol. A standard = absorbance of the standard at 274
Stopper the flask and shake well. Transfer a 5 ml aliquot nm;
of this solution to a lOO-ml volumetric flask. Dilute M = mass, in mg, of reference standard
to volume with methanol and mix well. Measure the taken to prepare standard solution;
absorbance at 274 nm in a 1 cm quartz cell using
methanol in the reference cell. P = percent purity of the reference
standard; and
m = mass, in mg, of the sample taken
for test.

4
Bureau of Indian Standards

BIS is a~statutory institution established under the Bureau oflndian Standards Act, 1986to promote harmonious
development of the activities of standardization, marking and quality certification of goods and 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 form without
the prior permission in writing af 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 of comments. Standards are also reviewed
periodically; a standard along with amendments is reaffirmed when such review indicates that no changes are
needed; if the review indicates that changes are needed, it is taken up-for revision. Users of Indian Standards
should ascertain that they are in possession of the latest amendments or edition by referring to the latest issue
of ‘BIS Handbook’ and ‘Standards : Monthly Additions’.

This Indian Standard has been developed from Dot : No. FAD 1 ( 375 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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