Methods For Estimation of Preservatives in Treated Timber and in Treating Solutions

IS 2753 (Part 2) : 1991
(Reaffirmed 2000)
Edition 2.1
(1993-11)
Indian Standard
METHODS FOR ESTIMATION OF

PRESERVATIVES IN TREATED TIMBER
AND IN TREATING SOLUTIONS
PART 2 DETERMINATION OF COPPER (IN COPPER ORGANIC
PRESERVATIVE SALT) AND PENTACHLOROPHENOL
( First Revision )
(Incorporating Amendment No. 1)
UDC 674.048 : 543
BIS 2002
BUREAU
OF INDIAN
STANDARDS
MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002
Price Group 2
Timber Sectional Committee, CED 9
FOREWORD
This Indian Standard (Part 2) (First Revision) was adopted by the Bureau of Indian Standards,
after the draft finalized by the Timber Sectional Committee had been approved by the Civil
Engineering Division Council.
IS 401 : 1982 Code of practice for preservation of timber ( third revision ) covers details of
preservatives, methods of preservative treatment of timber, etc. This standard (Parts 1 and 2)
details the methods of detection and estimation of the preservatives in such treated timber and
treating solutions. While Part 1 covers determination of copper, arsenic, chromium, zinc, boron,
creosote and fuel oil, Part 2 of this standard covers the determination of copper (in copper organic
preservative salts) and pentachlorophenol.
This standard (Part 2) was first published in 1968. Among other things, it then provided for
determination for copper in copper naphthenate only. In this revision the procedure for
determination of copper has been extended to other copper organic preservative salts. Further, the
formulae for calculation of percentage of pentachlorophenol in treating solution and treated timber
have been modified.
This edition 2.1 incorporates Amendment No. 1 (November 1993). Side bar indicates modification
of the text as the result of incorporation of the amendment.
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 2753 (Part 2) : 1991
Indian Standard
METHODS FOR ESTIMATION OF

PRESERVATIVES IN TREATED TIMBER
AND IN TREATING SOLUTIONS
PART 2 DETERMINATION OF COPPER (IN COPPER ORGANIC
PRESERVATIVE SALT) AND PENTACHLOROPHENOL
( First Revision )
1 SCOPE
3.2.4 Nitric Acid, Concentrated
1.1 This standard (Part 2) lays down methods

for the quantitative estimation of the following
in treated timber and in treating solutions:
3.2.5 Sulphuric Acid, Concentrated

3.2.6 Potassium Iodide Solution 20 percent.
Dissolve 20 g of potassium iodide in water and
dilute to 100 ml.
a) Copper in copper organic preservative salt

solution and in timber treated with copper
organic salt, and
b) Pentachlorophenol in pentachlorophenol
solution in oil and in timber treated with
pentachlorophenol.
3.2.7 Sodium Thiocyanate Solution 20

percent. Dissolve 20 g sodium thiocyanate in
water and dilute to 100 ml.
3.3 Procedure
3.3.1 In Treating Solution
1.2 These methods are intended for the

chemical analysis of oils containing the
required preservative and wood treated with
the same preservative.
Take a known mass of filtered treating solution

in a porcelain dish and evaporate the solvent
over an electric hot plate under hood. Heat the
dish strongly with a burner till all the organic
matter is destroyed. Cool it for 5 minutes. Add
2 ml of sulphuric acid and 3 ml of nitric acid.
Cover with a watch glass and heat gently until
the sample is dissolved. Transfer the solution
from the dish into a 300 ml Erlenmeyer flask
using dilute nitric acid. Heat the flask until
fumes of sulphur trioxide appear and a
colourless or light green solution remains. Cool
and wash down the sides with 5 ml water and
repeat heating till fuming. Cool and add 20 ml
of water. Wash down the sides of flask with
water, boil for one minute, cool and neutralize
cautiously with concentrated ammonium
hydroxide until a permanent precipitate just
forms. Add concentrated sulphuric acid drop by
drop until the precipitate just dissolves. Boil
down to a volume of 30 ml, cool to below 20C
and dilute to 125 ml.
2 QUALITY OF REAGENTS
Unless specified otherwise, pure chemicals and
distilled water [ see IS 1070 : 1977 Specification
for water for general laboratory use ( second
revision ) ] shall be employed in the tests.
3 QUANTITATIVE
ESTIMATION
OF
COPPER
IN
COPPER
ORGANIC
PRESERVATIVE SALT AND IN TIMBER
TREATED WITH COPPER ORGANIC
PRESERVATIVE SALT
3.1 The sample in dilute or concentrated
filtered solution should contain approximately
0.02 g of copper.
3.2 Reagents
3.2.1 Ammonium Hydroxide, Concentrated
3.2.2 Sodium
Thiosulphate
Solution
Dissolve 2.482 1 g of sodium thiosulphate in
water and make up to one litre.
Add 10 ml of 20 percent potassium iodide

solution and 5 ml of 20 percent sodium
thiocyanate solution and mix thoroughly by
rotating the flask. Titrate with sodium
thiosulphate solution, adding 2 ml starch
solution just before the brownish colour of the
iodine disappears. Stop the titration when no
blue colour remains.
3.2.3 Starch Solution 1 g soluble starch is

made to paste in 5 ml of water. Add 50 ml water
and boil for one minute with stirring, cool and
add one drop chloroform. Use always a freshly
prepared solution of starch.
IS 2753 (Part 2) : 1991

4.2.4 Concentrated Nitric Acid vol 1.42,
chloride free.
3.3.1.1 Calculation
0.063 5
-----------------------------Percentage of copper = V
M
where
V = volume, in ml, of sodium thiosulphate
consumed; and
M = mass, in g, of sample taken for the test.
4.2.5 Standard Silver Nitrate Solution 0.1 N.

Dissolve 16.989 g of silver nitrate in water and
make up the volume to one litre in volumetric
flask.
4.2.6 Ferric Ammonium Sulphate ( Indicator )
Dissolve 10 g of ferric ammonium sulphate in
10 ml of concentrated nitric acid and dilute to
100 ml with water.
3.3.2 In Treated Timber

Determine the density, in kilograms per cubic
metre, of the wood sample. Grind the sample to
sawdust or cut into small pieces with a knife or
use increment borings1. Weigh accurately into
a tared porcelain crucible about 10 g of the
sample. Char the material slowly over a
Bunsen burner. When the sample is charred
heat strongly until all organic matter is
destroyed, cool the ash for 5 minutes add 2 ml
of sulphuric acid and 3 ml of nitric acid, cover
with a watch glass and heat gently until the
sample is dissolved. Transfer the solution in
300-ml Erlenmeyer flask using nitric acid and
proceed as in 3.3.1.
4.2.7 Ammonium Thiocyanate Solution

0.1 N. Dissolve 7.51 g of ammonium
thiocyanate in water and dilute to one litre.
Standardize it against 0.1 N silver nitrate
solution.
4.3 Procedure
4.3.1 In Treating Solution
Take 10 g of the lime nitrate mixture in a
100-ml iron crucible. Drop from a weighed
dropping bottle approximately 0.5-1 g of the
pentachlorophenol solution on the lime nitrate
mixture in such a manner so as to give even
distribution. Re-weigh the crucible with
reagents and samples and obtain the sample
mass. Cover the sample with an additional 20 g
of lime nitrate mixture and tap the crucible
gently. Heat the crucible on a Bunsen burner at
850C to 900C for 20 minutes. Sample should
be free of unburnt carbon, if necessary increase
the combustion time for 5-10 minutes. Cool the
crucible and empty its contents in a 400-ml
beaker by gently tapping the crucible. Place a
cover glass on beaker and rapidly pour 70 ml of
water on the contents of the beaker. Scrub the
crucible with water and stirring rod equipped
with a rubber policeman to loosen any
remaining residue and add it to the beaker
containing the sample. If desired 2 percent
nitric acid may be used to wash the crucible.
The volume of the solution of the beaker should
not be more than 100 ml. Place the beaker in
cold water and neutralize the lime with
concentrated nitric acid with constant stirring.
When the ignition mixture is dissolved, the
solution should be acid to congo red paper (blue
colour), if not add nitric acid dropwise until the
solution is acidic. Not more than 2 or 3 ml
excess of acid should be present.
Add 15 ml of standard 0.1 N silver nitrate
solution from a burette, cover and gently boil
for several minutes to coagulate the silver
chloride precipitate formed. Cool and filter
through Whatman No. 41 filter paper in a clean
400-ml beaker. Wash the beaker and the
precipitate thoroughly with water till the wash
water does not give any turbidity with
ammonium thiocyanate. The volume should not
exceed 200-250 ml after washing. Add 5 ml of
3.3.2.1 Calculations
Kilograms of copper
V 0.063 5 M 1
per m3 of wood
= ------------------------------ ---------100
M
where
V = volume, in ml, of sodium thiosulphate
consumed;
M1 = mass, in kg, of one m3 of wood; and
M = mass, in g, of the sample taken for the
test.
4 QUANTITATIVE ESTIMATION OF
PENTACHLOROPHENOL IN
PENTACHLOROPHENOL SOLUTION IN
OIL AND IN TIMBER TREATED WITH
PENTACHLOROPHENOL
4.1 The method is suitable for analysis of one to
ten percent pentachlorophenol in oils and up to
two percent pentachlorophenol in wood with
the limitation of not more than 2 g of organic
material.
4.2 Reagents
4.2.1 Calcium Hydroxide Powder having
chloride content less than 0.005 percent.
4.2.2 Potassium Nitrate Powder having
chloride content less than 0.002 percent, and
fineness of 425 micron.
4.2.3 Lime Nitrate Mixture Mix 9 parts of
calcium hydroxide with 1 part powdered
potassium nitrate.
1
One increment boring 2 cm long and 0.475 cm in
diameter has a volume of 0.354 6 cm2.
IS 2753 (Part 2) : 1991

indicator (4.2.6) and back titrate excess silver
nitrate with standard ammonium thiocyanate
(4.2.7) from a 25-ml burette to a pink end point
that lasts at least 5 minutes. Run a blank on all
reagents and untreated oil, if possible the oil
should be free from chlorides.
4.3.1.1 Calculations
Pentachlorophenol, percent by mass
( A B ) 0.532 7
= --------------------------------------------C
stir gently to ensure complete contact of the

lime nitrate mixture with wood and heat the
crucible on a Bunsen burner till all the organic
matter is destroyed. Then proceed as given
in 4.3.1.
4.3.2.1 Calculation
The calculations for treated wood will be made
on volume basis (since the moisture content of
the wood is often in doubt).
Volume basis kilogram pentachlorophenol per
( A B ) 5.327
cubic metre of wood = --------------------------------------D
where
A = (ml silver nitrate for sample) (ml
ammonium thiocyanate for sample)
(ammonium thiocyanate factor);
B = (ml silver nitrate for blank) (ml
ammonium thiocyanate for blank)
(ammonium thiocyanate factor); and
C = mass of sample, in g, taken for the test.
where
A = (ml silver nitrate for sample) (ml
ammonium thiocyanate for sample)
(ammonium thiocyanate factor);
B = (ml silver nitrate for blank) (ml
ammonium thiocyanate for blank)
(ammonium thiocyanate factor); and
4.3.2 In Wood Treated with Pentachlorophenol

Take 10 g of lime nitrate mixture in a 100-ml
iron crucible, then add 5-10 increment borings1,
D = volume of sample, in cm3.
1
One increment boring 2 cm long and 0.475 cm in
diameter has a volume of 0.354 6 cm3.
Standard Mark
The use of the Standard Mark is governed by the provisions of the Bureau of Indian
Standards Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on
products covered by an Indian Standard conveys the assurance that they have been produced
to comply with the requirements of that standard under a well defined system of inspection,
testing and quality control which is devised and supervised by BIS and operated by the
producer. Standard marked products are also continuously checked by BIS for conformity to
that standard as a further safeguard. Details of conditions under which a licence for the use of
the Standard Mark may be granted to manufacturers or producers may be obtained from the
Bureau of Indian Standards.
Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods and
attending to connected matters in the country.
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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 Catalogue and Standards : Monthly Additions.
This Indian Standard has been developed from Doc : No. CED 9 (4595).
Amendments Issued Since Publication
Amend No.
Date of Issue
Amd. No. 1
November 1993
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IS 2753 (Part 2) : 1991