UDC 667’612 f 643’812 (First Reprint SEPTEMBER 1993) IS : 101 ( Part P/Set 1 ) - 1988

Indian Standard ( Reaffirmed 1996 )

METHODS OF SAMPLING AND TEST FOR PAINTS,

1. scope - Prescribes the Dean and Stark method for the determination of water content in paints
This method shall be used if the percentage of water content is more than 0’5 percent.

2. Principle - The material is refluxed with organic solvent which is immiscible with water. Thr
Carrier liquid distils into a graduated receiver carrying water with it which then separates to form tht
lower layer, the excess carrier liquid overflowing from the trap and returning to the still.

3. Apparatus

3.1 The Dean and Stark apparatus used for determination of water content has the following essential
features.

3.1 .l Flask - 600 ml capacity, as shown in Fig. 1, and made of. hard resistance glass, Nell annealed
and as free as possible from striae and similar defects. Alternatively, a metal flask may be used.

CONDENSER

FLASK

FIG. 1 DEAN AND STARK ASSEMBLY (WITH lo-ml RECEIVER )

3.1.2 Condenser - Made of hard resistance glass, well annealed and as free as possible from striae
,nd similar defects, with shape and dimensions as shown in Fig. 2.

Adopted 30 March 1988 Q February 1989, BIS Or 2

T O/A 30 ?r 2

L b/A ME TE.. OF
HOLES ABOUT 06
SPRAY TuaL

All dimensions in millimetres.

FIG. 2 CONDENSER AND SPRAY TUBE ( DEAN AND STARK APPARATUS 1

3.1.3 Spray tube - made of glass, sealed at one end, having four small holes equidistantly placed
around the wall near the closed end of the tube, with the shape and dimensions as shown in Fig. 2.

3.1.4 Two-millilitre receiver - made of hard resistance glass, well annealed and as free as possible
from striae and similar defects, provided with ground glass joints, and of shape and dimensions as
given in Fig. 3. It consists essentially of the upper chamber together with the tube and ground joint
leading to the flask and the graduated tube, When a metal flask is used, care shall be taken to
provide an air-tight connection between the flask and the receiver. The graduated portion shall have a
capacity of 2 ml at 20°C when filled to the highest graduation mark. The scale shall cover the range
of 0.1-2 ml and shall be divided into intervals each of 0.05 ml. The graduation marks corresponding to
0’5 ml, 1’0 ml, 1’5 ml and 2.0 ml shall be numbered. The numbered graduation marks shall be carried
completely round the tube. The graduation marks corresponding to 0.15 ml, 0’25ml, 0’35 ml and so on up
to and including 1’95 ml, shall be carried half way round the tube. The remaining graduation marks shall
be intermediate in length and shall project equally at each end beyond the shortest graduation marks.
The error at any point on the scale shall not exceed f0’03 ml and the difference between the errors at
any two points shall not exceed 0’03 ml.

3.1.5 Graduated cylinder - 100 ml capacity.

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 IS:101 (Part2/Secl )-IS88

All dimensions in millimetres.

FIG. 3 Z-ml RECEIVER

3.2 Procedure - Weigh 100 g of the material in the flask, add 100 ml of dry toluene ( see IS : 1839-
1961 Toluene, reagent grade ) and 1 ml of dry ethyl acetate [see IS : 229-1972 Ethyl acetate (second
revision ) ] or amyl acetate (see IS : 231-1957 Amy1 acetate ) and thoroughly mix the contents of the
flask. Pour toluene solvent into the receiver up to the level of the side tube. Attach the flask to the
Dean and Stark condensing and collecting system and heat the flask at such a rate that the condensate
falls from the end of the condenser at a rate of two-five drops per second. Continue the distillation
until condensed water is no longer visible in any part of the apparatus except at the bottom
of the graduated tube and until the volume of water collected remains constant. Remove the
persistent ring of condensed water in the condenser tube, if any, by increasing the rate of distillation
by a few drops per second. Wash droplets of water which adhere to the lower end of the condenser
tube into the receiver with toluene solvent, using the spray tube.

3.3 Note the quantity of water in the receiver in ml and also the temperature at which the sample was
measured. Assuming the density as 1’000 g/ml for the water collected in the receiver, calculate the
percentage of water (by mass) in the material.

EXPLANATORY NOTE

This standard is one of a series of Indian Standards dealing with methods of sampling and tests
for paints, varnishes and related products. This standard supersedes 14 of fS : 101-1964 ‘Methods
of test for ready mixed paints and enamels ( second revision )‘.

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Reprography Unit, BE, New Delhi, India