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IS 14626 (1999): Method for Determination of Total Bromide

Residues in Grains and Food Commodities Fumigated with
Methyl Bromide [FAD 1: Pesticides and Pesticides Residue
Analysis]

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 IS 14626 : 1999
( Reaffirmed 2004 )
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METHOD FOR DETERMINATION OF TOTAL

BROMIDE RESIDUES IN GRAINS AND FOOD
COMMODITIES FUMIGATED WITH METHYL
BROMIDE

ICS 65.100 ; 67.040

0 BIS 1999

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
*
NEW DELHI 110002

January 1999 Price Group 1

Pesticides Residue Analysis Sectional Committee, FAD 34

FOREWORD

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

Methyl bromide IS used as a fumigant either as such or in admixture with other material for control of pests of
stored grains/food commodities, such as fresh fruits and vegetables, stored products like flour, dry fruits, etc.
Frequent and increased use of methyl bromide often result in harmful effects due to its toxic nature. Careful
assessment of residues is, therefore, an important step in safeguarding human health and in the establishment of
sound regulatory policy.

This standard will enable the health authorities andothers engaged in the field to follow a uniform test procedure
for estimation of total bromide in grains/food commodities fumigated with methyl bromide.

In preparation of this standard due consideration has been given to the limits of total bromide residues which
have been laid down under the provisions of Prevention of Food Adulteration Act, 1954 and Rules framed
thereunder. The specified test methods are sensitive to the prescribed levels of residue.

In reporting the result of a test or analysis made in accordance with this standard, if the final value, observed or
calculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 Rules for rounding off numerical
values (revised).
 IS 14626 : 1999

Indian Standard

METHOD FOR DETERMINATION OF TOTAL

BROMIDE RESIDUES IN GRAINS AND FOOD
COMMODITIES FUMIGATED WITH METHYL
BROMIDE
1 SCOPE IS No. Title

This standard prescribes the method for determination 1 iiii (part ) Methods of sampling for the deter-
mination of pesticides residue : Part
of total bromide residues in grains and food
1 Agricultural and food com-
commodities fumigated with methyl bromide.
modities
2 REFERENCE 3 TESTS
Tests shall be carried out in accordance with the
The following Indian Standard contains provisions
method given in Annex A.
which through reference in this text, constitutes
provision of this standard. At the time of publication, 4 SAMPLING
the editions indicated was valid. Representative samples for the purpose of estimation
of total bromide residues shall be drawn in accordance
with IS 11380 (Part 1).

ANNEX A
(Clause 3)
DETERMINATION OF TOTAL BROMIDE RESIDUE

A-l TITRATION METHOD Complete combustion of the organic matter can be

A-l.1 Procedure
A sample of 5-10 g is treated in a 100 ml nickel
crucible with 40 ml of alcoholic KOH (2.5 g in 100 ml
of rectified spirit, that is 95 percent alcohol), allowed
to stand for an hour and evaporated to dryness on a
steam bath. It is then dried for a short time at 110C
and is covered with 10 g of NaOH pellets. The
crucible is left for an hour or two on a hot plate until
the bubbling or smoking diminishes, after which it is
placed in a muffle furnace at 6OOC. Fusion should be
carried without excessive burning or foaming. If the
charge becomes ignited the crucible should be
removed from the muffle until the flame is
extinguished. It is then returned to the muffle and this
process is repeated until the volatile gases have been
removed. Sodium peroxide is added to the melt a few
mg at a time to complete the oxidation of the remaining
carbon or organic matter. The peroxide shall be added
cautiously while the crucible is removed from the
furnance, bromide is lost if the charge burns with a
flare when too much peroxide is added.
effected best by returning any organic matter that has
raised above the NaOH to the bottom of the crucible,
when it mixes with the melt and is easily destroyed by
addition of peroxide. This is accomplished by
carefully rotating the hot crucible to wash down the
organic matter and adding 0.5 g more of peroxide. If
no burning or bubbling takes place, the oxidation is
complete. A few carbon particles which may remain
after final addition of peroxide do not affect the
accuracy of the results.
The crucible is rotated to allow the melt to solidify on
the sides and cooled, the contents are dissolved in
75 ml of water. Solution of the sodium compounds is
hastened by placing the crucible on a hot plate for
several minutes. The solution is transferred to a
400 ml beaker and partially neutralized with about
50 ml of 6 N HCl. The solution is boiled to destroy
peroxides and to reduce the volume to loo-125 ml.
Nickel hydroxides and other insoluble hydroxides are
removed by filtering through a Whatman No. 2 filter
paper collecting the filtrate and washings in 8 500 ml
wide mouth erlenmeyer flask.

1
P

IS 14626 : 1999

A-l.2 Extraction A-1.2.1 Standardization of Thiosulphate

The filtrate is made slightly acid with 6N HCl, then O.OlN stabilised with 1 g of Na2C03 per litre,
neutralised with NaOH solution, adjusting to the standardized against 0.01 N KI03 using 75 ml water,
colour change of methyl red. The volume at this point 10 ml 6N H2S04 and 0.5 g pure KI.
should be approximately 150 ml.
A-l.3 Calculation
About 2 g of sodium acid phosphate NaH2 Po4.H20
and 5 ml of hypochlorite (1N sodium or potassium Total bromide, mg/kg = ( - @ N 133*2
M x 0.01
hypochlorite in 0.1 N NaOH or KOH) solution are
added and the mix heated to boiling. After a minute where
or so 5 ml of sodium formate solution (50 g/100 ml) S = volume of thiosulphate used for sample,
are introduced and boiling is continued for 2 minutes.
B = volume of thiosulphate used for blank,
The sample is cooled and treated with a few drops of
1 percent sodium molybdate solution, 0.5 g pure N = normality of thiosulphate, and
potassium iodide and 25 ml of 6 N sulphuric acid. M = mass of sample in grams taken for the
Titration should be done immediately with standard test.
0.01 N Na2S203, starch indicator added just before the NOTE-To obtain bromide as methyl bromide use factor 158.3
end point. A blank titration is also carried out, using for detection up to 1 ppm.
all reagents.
Bureau of Indian Standards

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Enquiries relating to copyright be addressed to the Director (Publication), 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 34 ( 378 ).

Amendments Issued Since Publication

Amend No. Date of Issue .. Text Affected

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