BS 544 (1969)
BS 544 (1969)
BS 544 (1969)
, CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
British Standard
Specification for
BRITISH STANDARD
Co-operating organizations
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
© BSI 08-1999
Amendments issued since publication
First published April 1934
First revision February 1939
Second revision February 1969
Amd. No. Date of issue Comments
Contents
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
Page
Co-operating organizations Inside front cover
Foreword ii
1 Scope 1
2 Sampling 1
3 Text deleted 1
4 Composition 1
5 Paintability 1
6 Workability 1
7 Consistency 2
8 Skins and coarse particles 2
9 Keeping qualities and storage stability 2
10 Marking 2
Appendix A Methods for sampling 3
Appendix B Specification for whiting 3
Appendix C Method for the determination of oil content, whiting
content and the unsaponifiable matter on the extracted oil 4
Appendix D Method for the determination of paintability 6
Appendix E Method for the determination of consistency 6
Appendix F Method for the determination of skins and coarse particles 7
Figure 1a — Auger 8
Figure 1b — Tube for sampling 9
Figure 2 — Penetration device and penetrometer 10
© BSI 08-1999 i
BS 544:1969
Foreword
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
pages 1 to 10, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.
ii © BSI 08-1999
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
1 Scope
This British Standard specifies the requirements and composition of linseed oil putty for use in glazing
wooden frames as recommended in BS 62621).
NOTE The paintability test in this standard only covers the compatibility of putties with priming paints complying with BS 53582).
The use of other types of paint with putties should be agreed between the specifier and the manufacturer.
2 Sampling
For the purpose of examination under Clauses 4, 5, 6 and 8 of this specification samples shall be drawn,
and prepared by one of the methods described in Appendix A. Only original unopened containers shall be
sampled.
NOTE The number of containers sampled should be by agreement between the purchaser and the vendor. As a guide it is suggested
n
that the number of containers sampled should be ---- where n is the number of containers in each separate batch.
2
3 Text deleted
4 Composition
The material shall consist of a homogeneous paste composed of the following.
Raw linseed oil complying with BS 243, 632a or Not less than 10.0 % by mass as
refined linseed oil complying with BS 242a determined within 3 months from
the date of manufacture by the
method given in Appendix C
Additives taken as the unsaponifiable matter Not more than 2.5 % by mass of
determined by the method given in Appendix C the extracted oil
Water Not more than 0.5 % by mass as
determined by the method
described in BS 3900-B1b
Filler (as specified in Appendix B) Remainder as determined by the
method given in Appendix C
a
BS 242, BS 243, BS 259, BS 632, “Specifications for linseed oil”.
b
BS 3900, “Methods of test for paints” — Part B1: “Determination of water by the Dean and Stark method”.
5 Paintability
When tested according to the method described in Appendix D, the condition of the material shall be such
that:
1) It is capable of being painted after drying for a 48 hours period with white priming paint complying
with BS 53582) without any lifting or disturbance of its surface.
2) The coat of white priming paint applied as in 1) shall dry in 24 hours and not show any discoloration,
wrinkling, grittiness or other defect.
NOTE Some timber preservatives, particularly those containing wax or silicones and some water thinnable wood primers are found
to give adhesion and drying problems when used with putties under certain conditions. The manufacturers’ advice should be sought
where these types of preservative or primer are used.
6 Workability
The material shall work readily and smoothly in the hand and under a knife when used in glazing.
1)
BS 6262, “Code of practice for glazing for buildings”.
2)
BS 5358, “Specification for low-lead solvent-thinned priming paint for woodwork”.
© BSI 08-1999 1
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
7 Consistency
The consistency of the material shall be agreed between the purchaser and the vendor. Where the container
is of an appropriate size, the method of determining consistency as described in Appendix E shall be used
and the consistency of the material shall be such that the depth of penetration is within ± 20 % of the figure
agreed between purchaser and vendor.
NOTE The consistency is specified as the depth of penetration in a certain time with a stated load. The requirements of most
glaziers will be met by materials which are stiffer than those where the penetration is 300 mm, 25 s, 2 500 g and softer
than 200 mm, 15 s, 4 000 g where the weight is the superimposed load. A method of determining consistency is given in Appendix E.
10 Marking
Each container in which the material is packed shall be clearly and indelibly marked with the following
information:
a) name of identification mark of the supplier or manufacturer;
b) number and date of this British Standard;
c) batch number, manufacturing date and shelf life;
d) storage temperature range and conditions relevant to the stated expiry date.
3)
BS 410, “Specification for test sieves”.
2 © BSI 08-1999
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
2) Calcium carbonate content. When tested as described in clause 15 of BS 17954):1976 the material shall
have a calcium carbonate content of not less than 94 %.
3) pH value of aqueous suspension. When tested as described in clause 13 or BS 17954):1976 the pH value
of the aqueous suspension of the material shall be in the range 8 to 10.
4) Matter volatile at 105 °C. When tested as described in clause 10 of BS 17954):1976 the percentage loss
in mass of the material as delivered shall be not greater than 0.25 %.
© BSI 08-1999 3
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
Appendix C Method for the determination of oil content, whiting content and
the unsaponifiable matter on the extracted oil
NOTE Full laboratory precautions should be taken when using diethyl ether.
C.1 Apparatus
The following apparatus is required:
1) Centrifuge.
2) Centrifuge tube, 100 ml capacity.
3) Flask, 500 ml, flat-bottomed, fitted with a B24 cone complying with BS 5725).
4) Condenser, glass, complying with BS 59226) and fitted with a B24 cone complying with BS 572.
5) Separating funnel (2), 250 ml, complying with BS 20217).
C.2 Reagents
The reagents used shall be of recognized analytical reagent quality. Distilled water or water otherwise
prepared of equal purity shall be used throughout.
1) Potassium hydroxide. 0.5N solution in 95 % (v/v) ethanol8). The strength should be approximately but
not less than 0.5N and its colour not darker than pale yellow. Dissolve 35–40 g of potassium hydroxide
pellets in 20 ml of water and mix the solution with 1 000 ml of 95 % (v/v) ethanol. Allow the solution to
stand for several hours, preferably overnight, then decant or filter off the clear supernatant liquid. Keep
the clarified solution in a dark place.
2) Diethyl ether.
3) Acetone.
4) Potassium hydroxide, approximately 0.5N aqueous solution.
5) Sodium hydroxide, 0.1N solution in ethanol8). Dissolve 5–6 g of sodium hydroxide pellets in 10 ml of
water and mix the solution with 1 000 ml of 95 % (v/v) ethanol. Allow the solution to stand for several
hours, preferably overnight, then decant or filter off the clear supernatant liquid. Keep the filtered
solution in a dark place.
6) Hydrochloric acid, d = 1.18.
7) Ethanol8), 95 % (v/v).
8) Phenolphthalein indicator, 1.0 % solution in 95 % (v/v) ethanol8).
C.3 Procedure
C.3.1 Determination of oil content. Weigh to the nearest 0.1 g, about 18 g of the material into a previously
tared centrifuge tube. Add 15 ml of the diethyl ether, mix thoroughly with a stirring rod; wash the stirring
rod with diethyl ether to make a total volume of 75 ml. Place the centrifuge tube in the centrifuge and whirl
at a moderate rate until all the pigment is well settled. Decant the supernatant liquid into the tared flask.
Repeat the extraction three times more using a similar amount of diethyl ether for each extraction. Decant
the supernatant liquid into the flask after each extraction. When the extraction procedure is complete, fit
the flask with a condenser and distil off the diethyl ether on a steam-bath. Carry out this process in a
fume-cupboard. When distillation is complete continue heating the open flask, occasionally passing in a
stream of air from a rubber blowing ball until only a trace of solvent remains.
Then place the flask in a ventilated oven at 80 °C for 1 hour, cool in a desiccator and weigh. Reheat at 80 °C
for a further half hour, cool and reweigh. Continue with this procedure until the difference between two
successive weighings is not more than 1 mg.
Calculate the percentage of oil in the material.
5)
BS 572, “Interchangeable conical ground glass joints”.
6) BS 5922, “Specification for glass condensers for laboratory use”.
7) BS 2021, “Specification for separating and dropping funnels for laboratory use”.
8) Ethanol may be replaced by 66 OP industrial methylated spirit complying with BS 3591, “Industrial methylated spirits”.
It should be noted that the use of industrial methylated spirit is governed by the Methylated Spirits Regulations, 1983
(S.I. 1983/252).
4 © BSI 08-1999
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
C.3.2 Determination of whiting content. Dry the residue in the centrifuge tube by placing the tube and
residue on a steam-bath and heating until no smell of diethyl ether can be detected. Then transfer the tube
and its contents to a ventilated oven and heat at 105 °C for 1 hour. Cool in a desiccator and weigh. Reheat
at 105 °C for a further half hour, cool and reweigh. Continue heating at 105 °C until the difference between
two successive weighings is not more than 1 mg. Calculate the percentage of whiting in the material.
C.3.3 Determination of unsaponifiable matter on extracted oil
Weigh to the nearest milligramme, 2.0 – 2.5 g of the extracted oil into a 250 ml flask or use the flask and
oil from C.3.1, and add 25 ml of the alcoholic potassium hydroxide solution. Attach the flask to a reflux
condenser and heat on a boiling water bath for 1 hour, swirling at frequent intervals to ensure complete
saponification.
Remove the flask from the bath, detach the condenser and transfer the contents of the flask to a 250 ml
separating funnel. Wash the flask with 50 ml of water and add the washings to the solution in the funnel.
Then wash the flask with 50 ml of diethyl ether and add this cautiously to the solution in the funnel.
Stopper the funnel, invert and ventilate by opening the tap, close the tap, shake vigorously, ventilate and
then allow the funnel to stand until the two layers of liquid separate and clarify. Run off the aqueous
alcoholic layer into the flask used for the saponification.
Pour the ethereal layer from the top of the funnel into a second 250 ml separating funnel containing 20 ml
of water. Extract the aqueous alcoholic soap solution twice more, each time with 50 ml of diethyl ether in
the same manner and combine the three extracts in the second funnel. If the extracts contain solid
suspended matter, pass them through a small, dry, fat-free filter into the second separating funnel,
washing the filter subsequently with warm diethyl ether and adding to the main diethyl ether extract.
Rotate the extracts gently in the second funnel, without violent shaking, with the 20 ml of water and, after
allowing to separate, run off the water.
If the presence of metallic soap in the extracted oil is known or suspected, the second separating funnel
should be empty instead of containing 20 ml of water.
In this case add 5 drops of hydrochloric acid d = 1.18, and shake vigorously. Wash the combined extracts
successively with two quantities of 20 ml of water, employing vigorous shaking on each occasion.
After one or other of these preliminary treatments, wash the ethereal solution twice with 20 ml of water,
shaking vigorously on each occasion. Then successively wash with 20 ml of the 0.5N aqueous potassium
hydroxide solution, 20 ml of water, 20 ml of the 0.5N aqueous potassium hydroxide solution, 20 ml of water
and again with 20 ml of the 0.5N aqueous potassium hydroxide solution, and at least twice more with 20 ml
of water. Continue washing with water until the wash water no longer turns pink on addition of
phenolphthalein indicator.
Transfer the ethereal solution to a previously tared flask and evaporate to small bulk. Add 2–3 ml of
acetone and completely remove the solvent from the flask, for example by means of a gentle current of air,
the flask being almost entirely immersed, held obliquely and rotated in a boiling-water bath. Dry the flask
and contents to constant weight9) at a temperature not exceeding 80 °C.
Dissolve the contents in 10 ml of freshly boiled and neutralized 95 % ethanol and titrate with the 0.1N
alcoholic sodium hydroxide solution, using phenolphthalein indicator.
The titration should not exceed 0.1 ml. If it does, reject the test and repeat the determination from the
beginning.
If there is any reason to suspect the incomplete separation of saponifiable matter, subject the weighed
residue to re-saponification, re-extraction and washing, under the conditions specified in the method. If, by
the treatment, the amount of unsaponifiable matter differs from that first obtained in the first
determination, within the limits of manipulative error10) reject the test and repeat the determination from
the beginning.
100W
Calculation. Unsaponifiable matter, per cent by weight = ------------------1
W
where W1 = weight of unsaponifiable residue (g)
and W = weight of extracted oil (g).
9) Incertain unusual cases, the unsaponifiable matter appears to give a continuous loss during drying, owing to the presence of
some matter difficult to volatilize, as, for example, residual solvent fractions. In such instances transfer the washed ethereal
extract to a flask containing about 2 g of neutral oil, such as ground nut oil, previously brought to constant weight at 80 °C, and
then proceed as in an ordinary determination. Under these conditions the neutral oil serves to minimize any loss.
10) The limits of experimental error in terms of weight will naturally vary with the amount of unsaponifiable matter in the
sample.
© BSI 08-1999 5
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
Appendix E Method for the determination of consistency (50 kg (1 cwt) kegs only)
E.1 Principle
The results obtained by submitting the putty to the penetration test will enable an assessment to be made
of the property usually referred to as the consistency of the putty.
The penetration is the distance in millimetres which a loaded 38 mm (1½ in) ball mounted on a shaft
penetrates vertically into the keg of putty under standard conditions of loading, time and temperature.
E.2 Apparatus
The following apparatus is required:
1) Penetration device. A polished shaft of rust resisting steel 635 mm (25 in) long and 8 mm (5/16 in)
diameter terminating at one end in a 38 mm (1½ in) diameter monel metal ball and at the other in a
circular plate of aluminium alloy approximately 150 mm (6 in) in diameter and
approximately 5 mm (3/16 in) thick on which weights can be placed (see Figure 2), the weights
being adjustable to give superimposed loading of 2 500 g to 4 000 g in steps of 500 g.
2) Penetrometer. A penetrometer apparatus which will allow the penetration device to move without
appreciable friction and which is fitted with a device capable of indicating the depth of penetration
in mm. The sides of the guide should be vertical. A suitable hole is provided in the baseboard through
which the surface of the putty may be observed when lowering the ball (see Figure 2 for a suitable
apparatus).
3) Constant temperature enclosure. An enclosure capable of accommodating 1 cwt kegs of putty and
regulated at a temperature of 20 ± 1 °C unless otherwise agreed.
4) Timing device. An audible seconds counter is recommended.
E.3 Preparation of specimen
Immediately prior to carrying out the determination, place the keg of unopened putty in the constant
temperature enclosure13) for one week or until the putty has attained the agreed test temperature.
11)
BS 5358, Specification for low-lead solvent-thinned priming paint for woodwork.
12)
BS 3900, “Methods of test for paints”, Part C2, “Surface-drying test (ballotini method)”.
13)
For convenience in routine testing a correction for temperature can be determined by the manufacturer for his particular
formulation. Where a constant temperature enclosure is not available, the putty can be allowed to cool from a higher temperature
until the temperature indicated by a thermometer midway between the side of the keg and its centre, inserted to a depth of six inches
reaches the test temperature.
Usually only one keg out of a mixer load need be tested and the contents of that keg should be incorporated in a subsequent batch
6 © BSI 08-1999
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
E.4 Procedure
Examine the penetrometer and establish that the penetration device falls freely.
Then after removing the lid from the keg and the paper from the surface of putty, place the penetrometer
with the base board resting on the rim of the keg with the penetrometer device raised above the putty
surface. Load the device by placing weights on the top plate and lower slowly until the ball just makes
contact with the surface of the putty. Note the scale reading. Release the penetration device, read and
record the depth of penetration in the specified time, using the specified superimposed load. Make four
determinations, each midway between the centre and the side of the keg and equally spaced around the
keg. Clean the ball between each determination.
NOTE When withdrawing the penetration device care must be taken not to introduce oil or putty into the bearings of the guide.
If the difference between any individual reading and the mean is greater than 50 mm the test should be
repeated with a fresh keg.
E.5 Reporting
Record the values of the superimposed load, time and penetration depths. Average the penetration depth
figures obtained and report whether the average falls within 20 % of the specified penetration depth figure.
14)
BS 410, “Specification for test sieves”.
15)
BS 245, “Specification for mineral solvents (white spirit and related hydrocarbon solvents) for paints and other purposes”.
© BSI 08-1999 7
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003
© BSI 08-1999 8
Figure 1a — Auger
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003
9 © BSI 08-1999
BS 544:1969
Licensed Copy: Technical Information Services Dept ., CNL Technical Information Services, 29 August 2003, Uncontrolled Copy, (c) BSI
10
BS 544:1969
© BSI 08-1999
BS 544:1969
British Standards
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© BSI 08-1999
BS 544:1969
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