BRITISH STANDARD
BS 3900-B4:
1986
ISO 6503:1984
[Total lead]
Methods of test for paints
Part B4: Determination
of total lead in paints
and similar materials —
[ISO title: Paints and varnishes —
Determination of total lead — Flame
atomic absorption spectrometric
method]
It is recommended that this Part be read in conjunction with the general
information in the Introduction to BS 3900, issued separately.
UDC 667.612:[543.06:546.815]
BS 3900-B4:1986
This British Standard, having
been prepared under the
direction of the Pigments, Paints
and Varnishes Standards
Committee, was published
under the authority of the Board
of BSI and comes
into effect on
31 January 1986
© BSI 04-1999
First published July 1967
First revision January 1986
The committees responsible for
this British Standard are shown
in BS 3900: Introduction.
The following BSI references
relate to the work on this
standard:
Committee reference PVC/10
Draft for comment 79/55200 DC
ISBN 0580 14804 1
Amendments issued since publication
Amd. No.
Date of issue
Comments
BS 3900-B4:1986
Contents
National foreword
1
Scope and field of application
2
References
3
Principle
4
Dry ashing method
5
Wet oxidation method
6
Determination
7
Expression of results
8
Test report
Table 1
Table 2
Table 3
Publications referred to
© BSI 04-1999
Page
ii
1
1
1
1
3
4
5
6
3
4
5
Inside back cover
i
BS 3900-B4:1986
National foreword
This revision of this Part of BS 3900 has been prepared under the direction of the
Pigments, Paints and Varnishes Standards Committee. It is identical with
ISO 6503:1984 “Paints and varnishes — Determination of total lead — Flame
atomic absorption spectrometric method” published by the International
Organization for Standardization (ISO). This Part of BS 3900 supersedes
BS 3900-B4:1967, which is withdrawn.
This revision of this Part of BS 3900 has been prepared principally to replace
method 1 of the previous edition by a method using modern procedures, which are
more rapid and have improved precision. Method 2 of the 1967 edition has not
been included, although the Technical Committee is considering an alternative
method to this which, if approved, will be introduced in due course.
BS 3900-B4 is not appropriate for determining the “soluble” lead content of
paints. For this purpose, reference should be made to the method described in
BS 3900-B3 “Determination of “soluble” lead in the solid matter in liquid paints:
method for use in conjunction with The Control of Lead at Work
Regulations, 1980 (S.I. 1980 No. 1248)”.
It has been assumed in the drafting of this standard that it will be used and
applied by those who are appropriately qualified and experienced.
Terminology and conventions. The text of the international standard has
been approved as suitable for publication as a British Standard without
deviation. Some terminology and certain conventions are not identical with those
used in British Standards; attention is drawn especially to the following.
The comma has been used as a decimal marker. In British Standards it is current
practice to use a full point on the baseline as the decimal marker.
Wherever the words “International Standard” appear, referring to this standard
they should be read as “British Standard” and wherever the identification
“ISO 6503” appears, it should be read as “BS 3900-B4”.
In British Standards, it is current practice to use the symbol “L” for litre (and its
submultiples) rather than “I”, and to use the spelling “sulphur”, etc., instead of
“sulfur”, etc.
Cross-references
International standard
Corresponding British Standard
ISO 1042:1983
BS 1792:1982 Specification for one-mark volumetric
flasks
(Identical)
BS 3900 Methods of test for paints
ISO 1512:1974
Part A1:1970 Sampling
(Technically equivalent)
ISO 1513:1980
Part A2:1983 Examination and preparation of samples
for testing
(Identical)
ISO 5725:1981
BS 5497 Precision of test methods
Part 1:1979 Guide for the determination of repeatibility
and reproducibility for a standard test method
(Technically equivalent)
The Technical Committee has reviewed the provisions of ISO 385/1 which has
now been published as a partial revision of ISO/R 385:1964, and has decided that
they are acceptable for use in conjunction with this standard. A related British
Standard to ISO 385/1:1984 is BS 846:1985 “Specification for burettes”.
ii
© BSI 04-1999
BS 3900-B4:1986
There are no British Standards corresponding to ISO 3696, currently at draft
stage, or ISO 3856/1. The Technical Committee has reviewed the requirements
for the water of grade 3 purity, proposed for inclusion in ISO 3696. As these are
compatible with the requirements of BS 3978:1966 “Water for laboratory use”,
the Technical Committee has decided that water complying with BS 3978 is
acceptable for use as required in 4.2 and 5.2. It is expected that ISO 3856/1 which
is only referred to in clause 1 for information will be implemented in group B of
BS 3900.
Additional information. With reference to 4.5.1, the full procedure requires
both the addition of liquid paraffin, as described in 4.5.2 paragraph 3, and the
extraction described in 4.5.4.2.
The single test results referred to in 7.2.1 and 7.2.2 are mean values obtained
in 7.1 for the two test portions (see 4.5.2 or 5.5.1).
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 6, 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.
© BSI 04-1999
iii
iv
blank
BS 3900-B4:1986
1 Scope and field of application
4.2 Reagents
This International Standard describes a flame
atomic absorption spectrometric method for the
determination of total lead in paints and related
products.
The method is applicable to products having
total lead contents in the range of about 0,01
to 2 % (m/m).
During the analysis, use only reagents of recognized
analytical grade and only water of at least grade 3
purity according to ISO 3696.
4.2.1 Sodium carbonate, anhydrous.
4.2.2 Magnesium carbonate.
4.2.3 Sulfur.
4.2.4 Liquid paraffin.
4.2.5 Sodium sulfide, 10 g/l solution.
4.2.6 Hydrochloric acid, approximately 180 g/l.
Add 450 ml of concentrated hydrochloric
acid [36 % (m/m), A approximately 1,18 g/ml] to an
approximately equal amount of water and dilute
to 1 000 ml.
4.2.7 Hydrochloric acid, approximately 18 g/l.
Add 100 ml of the hydrochloric acid (4.2.6) to water
and dilute to 1 000 ml.
4.2.8 Nitric acid, approximately 315 g/l.
Add 1 volume of concentrated nitric acid
[about 65 % (m/m), A approximately 1,40 g/ml]
to 2 volumes of water.
4.2.9 Lead, standard stock solution containing 1 g of
Pb per litre.
Either
a) transfer the contents of an ampoule of
standard lead solution containing exactly 1 g of
Pb into a 1 000 ml one-mark volumetric
flask containing some water and 30 ml of the
nitric acid (4.2.8), dilute to the mark with water
and mix well;
or
b) weigh, to the nearest 1 mg, 1,598 g of lead
nitrate [Pb(NO3)2] (previously dried
for 2 h at 105 °C), dissolve in water in a 1 000 ml
one-mark volumetric flask, add 30 ml of the
nitric acid (4.2.8), dilute to the mark with water
and mix well.
1 ml of this standard stock solution contains 1 mg of
Pb.
4.2.10 Lead, standard solution containing 100 mg of
Pb per litre.
Prepare this solution on the day of use.
Pipette 10 ml of the standard stock solution (4.2.9)
into a 100 ml one-mark volumetric flask, dilute to
the mark with the hydrochloric acid (4.2.7) and mix
well.
1 ml of this standard solution contains 100 4g of
Pb.
NOTE This method may also be applicable to products with a
total lead content of more than 2 % (m/m), but it should only be
used when the precision does not exceed the appropriate values
given in 7.2.
Two methods are given for the treatment of the test
portion; the dry ashing method (clause 4) should be
used as the referee method in cases of dispute.
For the determination of lead in the test solution,
the dithizone spectrophotometric method specified
in ISO 3856/1 may be used as an alternative
method.
2 References
ISO 385/1, Laboratory glassware — Burettes —
Part 1: General requirements1).
ISO 1042, Laboratory glassware — One-mark
volumetric flasks.
ISO 1512, Paints and varnishes — Sampling.
ISO 1513, Paints and varnishes — Examination
and preparation of samples for testing.
ISO 3696, Water for laboratory use —
Specifications2).
ISO 3856/1, Paints and varnishes — Determination
of “soluble” metal content — Part 1: Determination
of lead content — Flame atomic absorption
spectrometric method and dithizone
spectrophotometric method.
ISO 5725, Precision of test methods —
Determination of repeatability and reproducibility
by inter-laboratory tests.
3 Principle
Decomposition of a test portion by either the dry
ashing method (clause 4) or the wet oxidation
method (clause 5), and determination of the lead by
flame atomic absorption spectrometry.
4 Dry ashing method
4.1 Principle
Evaporation of a test portion to dryness and ashing
at 475 °C to remove all organic matter. Extraction of
any lead in the residue with hydrochloric acid.
1)
At present at the stage of draft. (Partial revision of ISO/R 385:1964.)
2)
At present at the stage of draft.
© BSI 04-1999
1
BS 3900-B4:1986
4.3 Apparatus
Ordinary laboratory apparatus and
4.3.1 Crucibles, silica, preferably new.
4.3.2 Muffle furnace, capable of being maintained
at 475 ± 25 °C.
4.3.3 Hotplate, with energy regulation control.
4.4 Sampling
Take a representative sample of the product to be
tested by the method described in ISO 1512.
Examine and prepare the sample for testing as
described in ISO 1513.
4.5 Procedure
4.5.1 Preliminary tests
If the composition of the product to be tested is not
known, carry out qualitative tests for the presence
of cellulose nitrate and antimony. If the results of
these tests do not confirm the absence of cellulose
nitrate and antimony, carry out the full procedure.
4.5.2 Test portion
Carry out the procedure in duplicate.
Mix the sample thoroughly and immediately
transfer about 5 g into a weighed silica
crucible (4.3.1). Weigh the test portion to the
nearest 10 mg.
If the product contains cellulose nitrate (see 4.5.1),
mix about 2 g of the liquid paraffin (4.2.4) with the
test portion in the crucible.
4.5.3 Ashing
Place the crucible and its contents on the
hotplate (4.3.3) in a fume cupboard. Gradually
increase the temperature of the hotplate to remove
all volatile solvents.
Spread 2 g of the magnesium carbonate (4.2.2) over
the contents of the crucible and, over a period
of 10 min, progressively introduce the crucible into
the muffle furnace (4.3.2) at approximately 350 °C.
Raise the temperature of the furnace to 475 ± 25 °C
over a further period of 60 min and maintain at this
temperature until ashing is complete. Ensure that
an adequate supply of air for oxidation is available.
Do not allow the material in the crucible to ignite at
any stage.
4.5.4 Extraction
4.5.4.1 If the material does not contain antimony
(see 4.5.1), proceed as follows.
Allow the crucible and ash (see 4.5.3) to cool.
Transfer the crucible and ash to a 250 ml beaker,
add 100 ml of the hydrochloric acid (4.2.6) and,
using the hotplate (4.3.3), boil gently for 15 min.
Then allow to digest for a further 15 min.
While still hot, filter by decantation through a
fine-texture filter paper3), into a 250 ml beaker.
Wash the paper and residue with hot water,
collecting the washings in the beaker. Cool the
beaker and transfer the filtrate and washings to
a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
4.5.4.2 If the material contains antimony
(see 4.5.1), proceed as follows.
Grind the ash (see 4.5.3) to a fine powder, replace it
in the same crucible and mix it with
approximately 10 g of a mixture of equal parts of the
sodium carbonate (4.2.1) and the sulfur (4.2.3).
Cover the crucible and heat it over a moderate flame
until there is no odour of sulfur dioxide; this should
take 1 to 2 h.
Cool the crucible and digest the contents with a
small quantity of hot water until the melt is
completely broken up. Filter, transferring all the
residue to a filter paper with the sodium sulfide
solution (4.2.5) and wash the residue with the
sodium sulfide solution. Reject the filtrate.
Transfer the filter paper and residue to a 250 ml
beaker. Add 15 ml of the nitric acid (4.2.8) and,
using the hotplate (4.3.3), boil gently for 15 min.
Add 100 ml of the hydrochloric acid (4.2.6) and
allow to digest for 30 min. While still hot, filter
through a fine-texture filter paper into a 250 ml
beaker. Wash the paper and residue with hot water,
collecting the washings in the beaker. Cool the
beaker and transfer the filtrate and washings to
a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
4.5.5 Preparation of test solutions
From each extract solution (4.5.4) take an aliquot
portion, of size determined by the expected lead
content in the sample, in accordance with Table 1.
3) The
following filter papers have been found to be suitable:
Whatman Nos. 42 and 44
Schleicher and Schüll Nos. 589/3 and 589/6.
2
© BSI 04-1999
BS 3900-B4:1986
Table 1
Expected lead content
Aliquot portion
% (m/m)
ml
less than 0,4
0,4 to 1
1 to 2
25
10
5
NOTE If the lead content is higher than 2 % (m/m), a suitable
aliquot portion should be taken.
Place the aliquot portion in a 100 ml one-mark
volumetric flask and, if a 5 ml or 10 ml aliquot
portion is taken, add 10 ml of the
hydrochloric acid (4.2.6). Dilute to the mark with
water and mix well.
4.5.6 Preparation of reagent blank
Repeat the procedures described in 4.5.3, 4.5.4.1
or 4.5.4.2 and 4.5.5, but omitting the test portion.
5 Wet oxidation method
5.1 Principle
Wet oxidation of a test portion with a mixture of
sulfuric acid and hydrogen peroxide in a beaker
(method A) or with a mixture of sulfuric acid and
nitric acid in a Kjeldahl flask (method B) to remove
all organic matter. Heating to remove the excess
sulfuric acid, and extraction of any lead (in the form
of lead sulfate) in the residue with EDTA and
ammonia solution.
NOTE The presence of antimony or cellulose nitrate in a
sample does not cause interference with this method.
5.2 Reagents
During the analysis, use only reagents of recognized
analytical grade and only water of at least grade 3
purity according to ISO 3696.
5.2.1 Sulfuric acid, about 96 % (m/m),
A approximately 1,84 g/ml.
5.2.2 Hydrogen peroxide,
approximately 30 % (m/m), or, with the appropriate
additional safety precautions,
approximately 50 % (m/m) solution.
5.2.3 Nitric acid, about 65 % (m/m), A
approximately 1,40 g/ml.
5.2.4 Nitric acid, approximately 315 g/l.
Add 1 volume of the nitric acid (5.2.3) to 2 volumes
of water.
5.2.5 Ammonia solution, approximately 85 g NH3/l
solution.
Dilute 380 ml of concentrated ammonia
solution [25 % (m/m)] to 1 000 ml with water.
5.2.6 EDTA (Ethylenediaminetetraacetic acid,
disodium salt), 37 g/l solution.
5.2.7 Lead, standard stock solution containing 1 g of
Pb per litre.
© BSI 04-1999
Either
a) tranfer the contents of an ampoule of standard
lead solution containing exactly 1 g of Pb into
a 1 000 ml one-mark volumetric flask containing
some water and 30 ml of the nitric acid (5.2.4),
dilute to the mark with water and mix well;
or
b) weigh to the nearest 1 mg, 1,598 g of lead
nitrate [Pb(NO3)2] (previously dried
for 2 h at 105 °C), dissolve in water in a 1 000 ml
one-mark volumetric flask, add 30 ml of the
nitric acid (5.2.4), dilute to the mark with water
and mix well.
1 ml of this standard stock solution contains 1 mg of
Pb.
5.2.8 Lead, standard solution containing 100 mg of
Pb per litre.
Prepare this solution on the day of use.
Pipette 10 ml of the standard stock solution (5.2.7)
into a 100 ml one-mark volumetric flask, add 10 ml
of the nitric acid (5.2.4), dilute to the mark with
water and mix well.
1 ml of this standard solution contains 100 4g of Pb.
5.3 Apparatus
Ordinary laboratory apparatus and
5.3.1 Hotplate, with energy regulation control.
5.4 Sampling
Take a representative sample of the product to be
tested by the method described in ISO 1512.
Examine and prepare the sample for testing as
described in ISO 1513.
5.5 Procedure
5.5.1 Test portion
Carry out the procedure in duplicate.
Mix the sample thoroughly and immediately
transfer about 0,5 g into a 400 ml beaker
(method A) or into a 250 ml Kjeldahl flask
(method B). Weigh the test portion to the
nearest 1 mg.
5.5.2 Decomposition
5.5.2.1 Method A
Place the beaker and its contents on the
hotplate (5.3.1) in a fume cupboard and heat gently
to remove all volatile solvents. Add about 5 ml of the
sulfuric acid (5.2.1), cover the beaker with a watch
glass and heat for about 15 min at a higher
temperature to decompose and carbonize the
organic substances. Continue heating until white
fumes are evolved.
3
BS 3900-B4:1986
Take the beaker from the hotplate and allow to cool
for about 10 min. Add slowly, from a 5 ml pipette,
four 5 ml portions of the hydrogen peroxide
solution (5.2.2), allowing the reaction to subside
after each addition (see WARNING).
WARNING — Because of the danger from
spattering, the beaker should be kept covered
between additions of hydrogen peroxide
solution.
Heat again for about 10 min and allow to cool
for 5 min. Then add two further 5 ml portions of the
hydrogen peroxide solution, heat for 5 min and
allow to cool for 5 min. Finally add one further 5 ml
portion of the hydrogen peroxide solution. Heat
again to decompose the remaining hydrogen
peroxide. Remove the watch glass and carefully
rinse the underside with water, collecting the
rinsings in the beaker. Heat the beaker until
copious white fumes are evolved and the solution
has evaporated almost to dryness. Remove the
beaker from the hotplate and allow to cool.
5.5.2.2 Method B
Heat gently the Kjeldahl flask and its contents with
a Bunsen burner to remove all volatile solvents. Add
about 5 ml of the sulfuric acid (5.2.1) and heat for
about 10 min to decompose and carbonize the
organic substances. Allow to cool for about 10 min.
Add slowly, from a 5 ml pipette, four 5 ml portions
of the nitric acid (5.2.3), allowing the reaction to
subside after each addition.
Heat again for about 10 min and allow to cool
for 5 min. Then add two further 5 ml portions of the
nitric acid, heat for 5 min and allow to cool
for 5 min. Finally add one further 5 ml portion of
the nitric acid. Heat again to decompose all the
nitric acid and until copious white fumes are evolved
and the solution has evaporated almost to dryness.
Allow to cool. If charring occurs during this final
stage, carefully add further portions of the
nitric acid and repeat the heating, fuming and
cooling procedure.
5.5.3 Extraction
Add to the beaker (method A) or the Kjeldahl flask
(method B), 50 ml of the EDTA
solution (5.2.6), 10 ml of the ammonia
solution (5.2.5) and 50 ml of water. Boil gently for
about 15 min, cool and, if necessary, filter by
decantation through a medium texture filter paper
into a 250 ml one-mark volumetric flask, washing
the paper and the residue with water. Dilute to the
mark with water and mix well.
4
5.5.4 Preparation of test solutions
From each extract solution (5.5.3) take an aliquot
portion, of size determined by the expected lead
content in the sample, in accordance with Table 2.
Table 2
Expected lead content
Aliquot portion
% (m/m)
ml
less than 0,5
0,5 to 1
1 to 2
100 (undiluted)
75
50
NOTE If the lead content is more than 2 % (m/m), a suitable
aliquot portion should be taken.
Place the aliquot portion in a 100 ml one-mark
volumetric flask, dilute to the mark with water and
mix well.
5.5.5 Preparation of reagent blank
Repeat the procedures described in 5.5.2.1
(method A) or 5.5.2.2 (method B), 5.5.3 and 5.5.4,
but omitting the test portion.
6 Determination
6.1 Principle
Aspiration of the test solution into an acetylene/air
flame. Measurement of the absorption of
the selected spectral line emitted by a lead
hollow-cathode lamp or lead discharge lamp in the
region of 283,3 nm.
6.2 Reagents and materials
During the analysis, use only reagents of recognized
analytical grade and only distilled water or water or
equivalent purity.
6.2.1 Acetylene, commercial grade, in a steel
cylinder.
6.2.2 Compressed air.
6.3 Apparatus
Ordinary laboratory apparatus and
6.3.1 Flame atomic absorption spectrometer,
suitable for measurements at a wavelength
of 283,3 nm and fitted with a burner fed with
acetylene and air.
6.3.2 Lead hollow-cathode lamp or lead discharge
lamp.
6.3.3 Burette, of capacity 50 ml, complying with the
requirements of ISO 385/1.
6.3.4 One-mark volumetric flasks, of
capacity 100 ml, complying with the requirements
of ISO 1042.
© BSI 04-1999
BS 3900-B4:1986
6.4 Procedure
6.4.1.3 Calibration graph
6.4.1 Preparation of the calibration graph
Plot a graph having the masses, in micrograms, of
Pb contained in 1 ml of the standard matching
solutions as abscissae and the corresponding values
of the absorbances, reduced by the reading for the
blank matching solution as ordinates.
Either prepare a calibration graph as described
below or use a method of instrumental calibration of
at least equivalent accuracy and precision.
6.4.1.1 Preparation of the standard matching
solutions
Prepare these solutions on the day of use.
Into a series of six 100 ml one-mark volumetric
flasks (6.3.4), introduce from the burette (6.3.3),
respectively, the volumes of the standard lead
solution (4.2.10 or 5.2.8) shown in Table 3.
Add 10 ml of the hydrochloric acid (4.2.6) to each,
dilute to the mark with water and mix well.
Table 3
Standard
matching
solution No.
Volume of the
standard lead
solution (4.2.10
or 5.2.8 as
appropriate)
Corresponding
concentration of
Pb in the
standard
matching solution
ml
4g/ml
0
0
0
1
2
2
2
5
5
3
10
10
4
20
20
5
30
30
a
a Blank
matching solution.
6.4.2 Determination
6.4.2.1 Measure first the absorbance of the blank
test solution (4.5.6 or 5.5.5) in the
spectrometer (6.3.1) after having adjusted it as
described in 6.4.1.2. Then measure the absorbance
of each test solution (4.5.5 or 5.5.4) three times and,
afterwards, that of the blank test solution again.
Finally, redetermine the absorbance of standard
matching solution No. 4 (see Table 3) in order to
verify that the response of the apparatus has not
changed. If the absorbance of a test solution is
higher than that of the standard matching solution
with the highest lead concentration, dilute the test
solution appropriately (dilution factor F) with a
known volume of water.
6.4.2.2 If the readings obtained for a test solution
differ by more than 2 % or by more than 1 % of their
mean, repeat the procedures described in 6.4.2.1.
6.4.2.3 From the absorbance, corrected for the
reagent blank, determine the concentration, c, of
lead in each test solution using the calibration
graph. If a direct reading instrument is used, record
the lead concentration registered by the instrument.
7 Expression of results
6.4.1.2 Spectrometric measurements
7.1 Calculation
Install the lead spectral source (6.3.2) in the
spectrometer (6.3.1) and optimize the conditions for
the determination of lead. Adjust the instrument in
accordance with the manufacturer’s instructions
and adjust the monochromator to the region
of 283,3 nm in order to obtain the maximum
absorbance.
Adjust the flow of the acetylene (6.2.1) and of the
air (6.2.2) according to the characteristics of the
aspirator-burner, and ignite the flame. Set the scale
expansion, if fitted, so that the standard matching
solution No. 5 (see Table 3) gives almost a full scale
deflection.
Aspirate into the flame each of the standard
matching solutions (see 6.4.1.1) in ascending order
of concentration, and repeat with the standard
matching solution No. 4 to verify that the
instrument has achieved stability. Aspirate water
through the burner between each measurement,
taking care to keep the rate of aspiration uniform.
Calculate the lead content of the paint, using the
equation
© BSI 04-1999
,5 ´ c ´ F
a = 2
----------------------------m´V
where
a
is the total lead content of the paint,
expressed as a percentage by mass;
c
is the lead concentration, in micrograms per
millilitre, of the test solution, obtained from
the calibration graph;
F
is the dilution factor referred to in 6.4.2.1;
m
is the mass, in grams, of the test
portion (4.5.2 or 5.5.1);
V
is the volume, in millilitres, of the aliquot
portion of the extract taken in 4.5.5 or 5.5.4.
Calculate the mean of the two results.
5
BS 3900-B4:1986
7.2 Precision
NOTE The following values are based on the calculating
procedure described in ISO 5725, using the experimental data
available. They are subject to revision as further experience of
the procedure is obtained.
7.2.1 Repeatability (r)
The value below which the absolute difference
between two single test results on identical
material, obtained within a short interval of time by
one operator in one laboratory using the same
equipment and the standardized test method, may
be expected to lie with a 95 % probability is
5 % relative to the mean value for the dry
ashing procedure described in 4.5.4.1;
10 % relative to the mean value for the dry
ashing procedure with antimony extraction
described in 4.5.4.2;
5 % relative to the mean value for the wet
oxidation procedure described in 5.5.2.1
(see the note 2 to 7.2.2).
7.2.2 Reproducibility (R)
The value below which the absolute difference
between two single test results on identical
material, obtained by operators in different
laboratories using the standardized test method,
may be expected to lie with a 95 % probability is
15 % relative to the mean value for the dry
ashing procedure described in 4.5.4.1;
30 % relative to the mean value for the dry
ashing procedure with antimony extraction
described in 4.5.4.2;
6
15 % relative to the mean value for the wet
oxidation procedure described in 5.5.2.1
(see notes).
NOTE 1 The precision data presented for the wet oxidation
procedure described in 5.5.2.1 (Method A) are based on a single
paint sample.
NOTE 2 No data are available for the wet oxidation procedure
described in 5.5.2.2 (Method B).
8 Test report
The test report shall contain at least the following
information:
a) the type and identification of the product
tested;
b) a reference to this International Standard
(ISO 6503);
c) the method used for the extraction of lead from
the product under test (dry ashing or wet
oxidation method) and, if the wet oxidation
method was used, record the de-composition
procedure used; method A or method B);
d) any preliminary treatment carried out in
accordance with 4.5.2;
e) the result of the test;
f) any deviation, by agreement or otherwise, from
the procedure specified;
g) the date of the test.
© BSI 04-1999
BS 3900-B4:1986
Publications referred to
See national foreword.
© BSI 04-1999
BS 3900-B4:
1986
ISO 6503:1984
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