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 BRITISH STANDARD BS 812-118:
1988

Testing aggregates —
Part 118: Methods for determination of
sulphate content
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UDC [625.07+691.22]:[620.1+543.217.6:546.226]
 BS 812-118:1988

Committees responsible for this

British Standard

The preparation of this British Standard was entrusted by the Cement

Gypsum, Aggregates and Quarry Products Standards Committee (CAB/-) to
Technical Committee CAB/2, upon which the following bodies were
represented:

Aggregate Concrete Block Association

Association of Consulting Engineers
Association of Consulting Scientists
Association of Lightweight Aggregate Manufacturers
Brick Development Association
British Aggregate Construction Materials Industries
British Ceramic Research Ltd.
British Civil Engineering Test Equipment Manufacturers’ Association
British Geological Sciences
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British Precast Concrete Federation Ltd.

British Ready Mixed Concrete Association
British Steel Industry
Building Employers’ Confederation
Calcium Silicate Brick Association Limited
Cement and Concrete Association
Cement Makers’ Federation
Chartered Institute of Building
Concrete Society
County Surveyors’ Society
Department of the Environment (Building Research Establishment)
Department of the Environment (Property Services Agency)
Department of Transport (Highways)
Department of Transport (Transport and Road Research Laboratory)
Electricity Supply Industry in England and Wales
Federation of Civil Engineering Contractors
Institute of Concrete Technology
Institution of Civil Engineers
Institution of Highways and Transportation
Institution of Structural Engineers
Institution of Water and Environmental Management (IWEM)
Mortar Producers’ Association Limited
This British Standard, having Sand and Gravel Association Limited
been prepared under the Society of Chemical Industry
direction of the Cement Gypsum,
Aggregates and Quarry Products
Standards Committee, was
published under the authority
of the Board of BSI and comes Amendments issued since publication
into effect on
31 August 1988
Amd. no. Date of issue Comments
© BSI 01-1999

The following BSI references

relate to the work on this
standard:
Committee reference CAB/2
Draft for comment 84/14036 DC

ISBN 0 580 16534 5

 BS 812-118:1988

Contents

Page
Committees responsible Inside front cover
Foreword ii
1 Scope 1
2 Definitions 1
3 Principle 1
4 Sampling 1
5 Determination of the sulphate content of a 2 : 1
water/aggregate extract 1
6 Determination of the total sulphate content by
acid extraction 5
7 Precision 7
8 Test report 7
Appendix A Semi-quantitative test for the presence of
sulphate ions 8
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Appendix B Details of experiments for determining precision of tests

for water-soluble sulphate and total sulphate contents of aggregates 8
Figure 1 — Ion-exchange column for water-soluble sulphates 3
Table 1 — Minimum mass of preliminary sub-sample for
water-soluble sulphate method 4
Table 2 — Minimum mass of preliminary sub-sample for
total sulphate content method 6
Table 3 — Precision data, water-soluble sulphate determination 9
Table 4 — Precision data, total sulphate determination 9
Table 5 — Results excluded from calculation of precision data
in Table 3 10
Table 6 — Results excluded from calculation of precision data
in Table 4 10
Publications referred to Inside back cover

© BSI 01-1999 i
 BS 812-118:1988

Foreword
This Part of BS 812 has been prepared under the direction of the Cement,
Gypsum, Aggregates and Quarry Products Standards Committee. In the revision
of BS 812-2:1975, BS 812-3:1975 and BS 812-4:1976 each test, or collection of
related tests, is being revised separately and is being issued as a separate Part or
Section of BS 812.
This Part of BS 812 contains methods for determination of total sulphate content
and water-soluble sulphate content of aggregates, neither of which was
previously included in BS 812, but are included now because of the problems that
may arise if aggregates containing high concentrations of sulphates are used in
concrete or placed close to concrete structures.
It is intended that other British Standards should call up BS 812 test methods as
the basis of compliance. Nevertheless it is not intended that aggregates should be
subjected regularly to all the listed tests. Specifications in other standards,
should call up only relevant test methods.
Advice on the use of simpler qualitative tests is given for a preliminary sorting of
aggregates to see whether more precise and expensive testing is justified.
Reference should be made to BS 812-101 for general guidance on testing
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aggregates, precision of test methods and variance arising from sampling errors.
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 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 01-1999
 BS 812-118:1988

1 Scope 3.2 Method for total sulphate content

This Part of BS 812 describes two methods for The sulphates are extracted from a crushed sample
determining the sulphate content of aggregates. of aggregate by dilute hydrochloric acid. Barium
chloride solution is added to the extract. The
The first method determines the water-soluble
precipitate of barium sulphate is collected, dried
sulphate content of aggregates, which applies to
and weighed and the total sulphate content is
natural and synthetic aggregates to be used as
calculated.
drainage materials or for fill or hard core,
e.g. unbound roadbases or sub-bases or foundations.
4 Sampling
The second method determines the total sulphate
content of aggregates, which applies to aggregates The sample to be used for the test (the laboratory
used in concrete and cement bound materials. sample) shall be taken in accordance with the
procedure described in clause 5 of BS 812-102:1984.
NOTE 1 The second method for the determination of total
sulphate by acid extraction is specified as it is impractical to Ensure that the sample is representative of the
produce a method for the determinatin of total water-soluble moisture content as well as the solids by preventing
sulphate because of low water solubility of calcium sulphate. For
practical purposes for aggregates in concrete the total sulphate loss of moisture, except through evaporation,
content determined by this method is taken to be the same as the throughout the sampling procedure and at any
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total water-soluble sulphate content. subsequent stage up to the point of test.

NOTE 2 In Appendix A two procedures for
NOTE This is necessary because where the aggregate to be
a semi-quantitative test are described. It is strongly
tested carries surface water the sulphates will normally be
recommended that one of these is used as a preliminary check
dissolved, at least partly, in both this and the absorbed water and
before resorting to the test described in the main text, which may
hence the sulphate content will be affected by migration of water
be needed for compliance with a specification.
through the bulk materials.
NOTE 3 The titles of the publications referred to in this
standard are listed on the inside back cover.
5 Determination of the sulphate
2 Definitions content of a 2 : 1 water/aggregate
For the purposes of this Part of BS 812, the
extract
definitions given in BS 812-101 and BS 812-102 NOTE Calcium sulphate is relatively harmless because of its
apply. limited solubility and the extraction conditions have been chosen
so that aggregates containing only calcium sulphate are
classified as falling in class 1 of Table 6.1 in BS 8110-1:1985.
3 Principle 5.1 Apparatus
3.1 Method for water-soluble sulphates 5.1.1 Apparatus for preparation of test portion and
An aggregate sample is extracted with twice its own extraction of the sulphate (see 5.4 and 5.5.1)
mass of distilled or demineralized water to remove 5.1.1.1 Well ventilated oven, capable of being
water-soluble sulphate ions. The water-soluble controlled to maintain a temperature of 105 ± 5 °C.
sulphate content is determined by either an
5.1.1.2 Balance, capable of weighing up to 5 kg
ion-exchange method or a gravimetric method in
accurate to 5 g. The balance shall be regularly
one of the following ways.
calibrated as specified in BS 5781-1.
a) Some of the extract is transferred to an
5.1.1.3 Test sieve, 20 mm square hole perforated
ion-exchange column and the eluate is titrated
with standardized sodium hydroxide solution. plate complying with BS 410.
b) Some of the extract is treated with diluted 5.1.1.4 Pestle and mortar, or suitable mechanical
crusher.
hydrochloric acid. Barium chloride solution is
added and the precipitate is collected, dried and NOTE This is not required for aggregate all passing the 20 mm
sieve.
weighed.
5.1.1.5 Two plastics or metal bottles, wide-mouthed,
The ion-exchange method measures the presence of screw-capped. The bottles shall be 5 L capacity
sulphate ions. When other anions (see note) are when testing coarse aggregates or 2 L when testing
present this method is precluded. The gravimetric fine aggregate.
method is applicable when aggregates containing
sulphides (i.e. slags) are being analysed. 5.1.1.6 Mechanical shakers or rollers, to take the
extraction bottles (5.1.1.5).
NOTE Anions of strong acids, e.g. chlorides, nitrates and
phosphates, interfere with the ion-exchange method and are
apparently measured as sulphate. However, when chloride is the
only other ion present, and it has been quantitatively
determined, the ion-exchange method described can be used
provided the result is corrected as shown in 5.6.2.

© BSI 01-1999 1
 BS 812-118:1988

5.1.1.7 Two filter funnels, of approximately 100 mm 5.2.2.5 Sodium hydroxide solution
diameter with medium grade1) filter papers of a (c(NaOH) = approximately 0.1 mol/L), made by
diameter appropriate to the size of the funnel. dissolving 2 g of sodium hydroxide in 500 mL of
5.1.1.8 Beakers. water. Determine the exact concentration (in mol/L)
by titration against potassium hydrogen phthalate
5.1.2 Apparatus for the ion-exchange method
or with a standardized acid solution, and keep the
(see 5.3 and 5.5.2.1)
solution in an airtight plastics container (5.1.4.1).
5.1.2.1 Pipette, 50 mL size, grade B in accordance
5.2.2.6 Indicator, giving a distinct colour change in
with BS 1797.
the pH range 4 to 5.
5.1.2.2 An ion-exchange column and reservoir. NOTE Screened methyl orange is suitable.
NOTE A typical design is shown in Figure 1.
5.2.2.7 Silver nitrate solution, made by
5.1.2.3 Conical flasks, 500 mL capacity. At least two dissolving 0.5 g of silver nitrate in 100 mL of water.
are required. Store the solution in an amber-coloured glass
5.1.2.4 Graduated measuring cylinder, reagent bottle (5.1.4.2).
capacity 100 mL, grade B in accordance with 5.3 Preparation of the ion-exchange column
BS 1797.
NOTE This procedure is not required if the ion-exchange
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5.1.2.5 Burette, 50 mL size, grade B in accordance column method is not used (see 3.1).
with BS 1797. 5.3.1 Empty a quantity of cation-exchange
5.1.2.6 Beakers. resin (5.2.2.1), sufficient to half-fill the
5.1.3 Apparatus for the gravimetric method column (5.1.2.2), into a beaker (5.1.2.6) and stir
(see 5.5.2.2) with water. Empty this suspension of resin in water
into the column so that when the resin has settled,
5.1.3.1 Pipette, 50 mL size, grade B in accordance
there is approximately 20 mm depth of water above
with BS 1797.
the resin when the surplus water has drained away.
5.1.3.2 Apparatus as listed in 6.1.2.1 to 6.1.2.10. Maintain this depth of water above the resin at all
5.1.4 Apparatus for preparation of reagents times as it is important that the resin is not allowed
(see 5.2.2) to dry out.
5.1.4.1 Plastics container, airtight. 5.3.2 Activate the cation-exchange resin by leaching
5.1.4.2 Amber-coloured glass reagent bottle. with 100 mL of the hydrochloric acid
solution (5.2.2.2) followed by washing with distilled
5.2 Reagents water. Place the acid in the reservoir and leave the
5.2.1 General. Reagents of recognized analytical apparatus until the acid has passed through the
quality and only distilled water or water of column. Rinse and fill the reservoir with distilled
equivalent quality shall be used. water and leave the water to percolate through until
NOTE 1 Where accurately standardized solutions are required the liquid coming from the column gives no turbidity
it may be more convenient to obtain them already standardized when tested with about 1 mL of silver nitrate
to be used in accordance with the manufacturer’s instructions. solution (5.2.2.7) acidified with about five drops of
NOTE 2 If the ion-exchange column method is not used, the
reagents described in 5.2.2.1 to 5.2.2.7 are not required.
nitric acid (5.2.2.4).
5.2.2 Reagents 5.3.3 Regenerate the cation-exchange resin in the
manner described in 5.3.2 after it has been used for
5.2.2.1 Cation-exchange resin, strongly acid2).
four consecutive determinations.
5.2.2.2 Hydrochloric acid solution
(c(HCl) = approximately 4 mol/L), made by
diluting 360 mL concentrated hydrochloric acid
(relative density 1.18) to 1 L with water.
5.2.2.3 Hydrochloric acid solution, made by
diluting 200 mL concentrated hydrochloric acid
(relative density 1.18) to 1 L with water.
5.2.2.4 Nitric acid (c(HNO3) =
approximately 1 mol/L), made by diluting 15 mL of
concentrated nitric acid (relative density 1.42)
to 100 mL with water.

1)
Whatman No. 40 have been found suitable.
2)
A suitable material is Zerolit 225 or Amberlite 1R-120.

2 © BSI 01-1999
Licensed Copy: KEO International, KEO International, 25 March 2004, Uncontrolled Copy, (c) BSI

© BSI 01-1999
Figure 1 — Ion-exchange column for water-soluble sulphates

3
BS 812-118:1988
 BS 812-118:1988

5.4 Preparation of test portion 5.5.2 Determination of the sulphate in the

5.4.1 Dry the laboratory sample at a temperature extracts
of 105 ± 5 °C to remove surface water so that the 5.5.2.1 Ion-exchange method. With a
sample is free flowing. pipette (5.1.2.1) transfer 50 mL of filtered extract to
5.4.2 Reduce the laboratory sample by the the top of the ion-exchange column and allow to
procedures described in clause 6 of BS 812-102:1984 drain through the resin.
to an amount not less than the mass given Rinse the resin with two 75 mL increments of
in Table 1 appropriate to the nominal size of the distilled water collecting all the solution and
aggregate. washings in a conical flask (5.1.2.3) placed under
Table 1 — Minimum mass of preliminary the outlet of the column.
sub-sample for water-soluble sulphate method Add three to five drops of the indicator (5.2.2.6) to
Nominal maximum size of Minimum mass of the contents of the conical flask and titrate to the
aggregate sub-sample colour change with the standardized sodium
mm kg hydroxide solution (5.2.2.5).
63 50 Replace the flask under the outlet of the column and
50 35 pass a further 75 mL of distilled water through the
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40 15 resin. If the indicator colour changes to show that

28 or less 5 more acid has been washed from the resin, titrate
again to neutrality.
5.4.3 Sieve the sub-sample through a 20 mm
sieve (5.1.1.3) and crush any oversize aggregate to Record the total volume of standardized sodium
pass the sieve avoiding excessive grinding. hydroxide solution used (v1).
Combine, mix thoroughly and by suitable sample Repeat with another 50 mL aliquot of the filtrate
reduction techniques produce two test portions each and record the volume of standardized sodium
of about 2 kg mass for coarse aggregate or two test hydroxide solution used (v2).
portions each of about 500 g mass for sand. Dry the Take the mean value of v1 and v2 (V).
test portions by heating at a temperature
If the values of v1 and v2 differ by more than 0.5 mL
of 105 ± 5 °C to achieve a dry mass which is
repeat the procedure.
constant to within 0.1 %.
Repeat the complete procedure with a second test
5.5 Analytical procedure
portion.
5.5.1 Preparation of extracts 5.5.2.2 Gravimetric method. Transfer 50 mL of
5.5.1.1 For coarse aggregates use the two plastics or filtered extract to a 500 mL beaker, dilute to 300 mL
metal bottles of 5 L capacity and for fine aggregate with distilled or demineralized water, add 10 mL of
use the two bottles of 2 L capacity (5.1.1.5). Weigh hydrochloric acid solution (5.2.2.3) and carry out the
each bottle and record its mass to the nearest 5 g. procedure described in 6.4.2 to 6.4.9.
5.5.1.2 Transfer the test portions obtained as NOTE When aggregates containing sulphide are being
described in 5.4 to the bottles, weigh bottle and analysed see the note to 6.4.2.
contents and record their mass to the nearest 5 g. Repeat the procedure with a second test portion.
Calculate the mass of aggregate in each bottle by 5.6 Calculation and expression of results
difference.
5.6.1 If no other anions are present, calculate the
5.5.1.3 Add to each bottle a mass of distilled or concentration of sulphate ions, (as SO3 in g/L),
demineralized water equal to twice the mass of the present in the extracts, from the equation:
test portion. Fasten the water-tight bottle closures
and mix the contents by shaking or rolling concentration of SO3 = 0.8mV
continuously for a minimum of 24 h. where
NOTE If mechanical agitation equipment is not used and the V is the volume of sodium hydroxide solution
sample and water are merely allowed to remain in contact with (in mL);
occasional shaking there is a possibility (particularly if the source
of sulphate is, for example, large crystals of gypsum) that the m is the concentration of sodium hydroxide
sulphate which could theoretically dissolve will not all be solution (in mol/L).
extracted in 24 h.
5.5.1.4 Filter the extracts through dry,
medium-grade filter papers (5.1.1.7) until
at least 100 mL of clear filtrates have been collected
in clean dry beakers (5.1.1.8).

4 © BSI 01-1999
 BS 812-118:1988

5.6.2 If chlorides are the only other ions present, 6.1.2.4 Fume cupboard.
calculate the concentration of sulphate ions, 6.1.2.5 Two filter funnels, of approximately 100 mm
(as SO3 in g/L), present in the extracts from the diameter with medium grade3) and fine grade4)
equation: filter papers of a diameter appropriate to the size of
concentration of SO3 = 0.8mV – 5.64 C the funnels.
where 6.1.2.6 Dropping pipette, capacity 10 mL.
C is the chloride ion content as a percentage by 6.1.2.7 Sintered silica filtering crucibles, porosity
mass of dry aggregate. grade 4, approximately 35 mm in diameter
and 40 mm in height.
5.6.3 When the gravimetric method has been used, NOTE These are not required if filtration through
calculate the sulphate concentration of sulphate 4)
fine grade filter papers is preferred.
ions, (as SO3 in g/L), present in the extracts from the 6.1.2.8 Ignition crucibles, approximately 35 mm in
equation: diameter and 40 mm in height and capable of
concentration of SO3 = 6.86m2 maintaining a constant mass when heated
where to 800 °C.
m2 is the mass of precipitate obtained in 6.4.9 NOTE These crucibles are not required if the filtering
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(in g). crucibles (6.1.2.7) are used. Porcelain, silica or platinum are
suitable materials for ignition crucibles.
5.6.4 Express the mean sulphate contents of 6.1.2.9 A suitable means of igniting the precipitate,
the 2 : 1 extracts to the nearest 0.1 g/L. If the preferably an electric muffle furnace capable of
individual results differ by more than 0.1 g/L and r1, reaching and maintaining 800 °C.
(calculated from B.5) repeat the test starting with 6.1.2.10 Dessicator.
new analytical test portions (see 5.4). 6.1.3 Apparatus for preparation of reagents
NOTE With aggregates containing discrete crystals of gypsum (see 6.2.2)
it may be difficult to obtain close agreement between individual
test portions. 6.1.3.1 Amber-coloured glass reagent bottle.
6.2 Reagents
6 Determination of the total sulphate
content by acid extraction 6.2.1 General. Reagents of recognized analytical
quality and only distilled water or water of
6.1 Apparatus equivalent quality shall be used.
6.1.1 Apparatus for preparation of test portion 6.2.2 Reagents
(see 6.3) 6.2.2.1 Barium chloride, 5 % solution, made by
6.1.1.1 Well ventilated oven, capable of being dissolving 50 g of barium chloride in 1 L of water,
controlled to maintain a temperature of 105 ± 5 °C. and filtered before use if necessary.
6.1.1.2 Balance, capable of weighing up to 5 kg 6.2.2.2 Dilute hydrochloric acid, made by
accurate to 5 g. The balance shall be regularly diluting 100 mL of concentrated hydrochloric acid
calibrated as specified in BS 5781-1. (relative density 1.18) to 1 L with water.
6.1.1.3 Test sieves, 20 mm, 5 mm, 1 mm and 150 µm 6.2.2.3 Silver nitrate solution, made by
complying with BS 410. dissolving 0.5 g of silver nitrate in 100 mL of water.
6.1.1.4 Pestle and mortar, or suitable mechanical Store the solution in an amber-coloured glass
crusher. reagent bottle (6.1.3.1).
6.1.2 Apparatus for analysis of test portion 6.3 Preparation of test portion
6.1.2.1 Balance, capable of weighing up to 100 g 6.3.1 Dry the laboratory sample at a temperature
accurate to 0.001 g. The balance shall be regularly of 105 ± 5 °C to remove surface water so that the
calibrated as specified in BS 5781-1. sample is free flowing.
6.1.2.2 Beakers, capacity 250 mL and 500 mL. 6.3.2 Reduce the laboratory sample by the
6.1.2.3 Electric hot-plate, capable of being controlled procedures described in clause 6 of BS 812-102:1984
to boil the contents of beakers without causing to an amount not less than the mass given in
undue overheating. Table 2 appropriate to the nominal maximum size of
aggregate.

3)
Whatman No. 40 is suitable, but fine filter paper, e.g. Whatman No. 42 may be necessary if the filtrate is not completely clear.
4)
Whatman No. 42 is suitable.

© BSI 01-1999 5
 BS 812-118:1988

Table 2 — Minimum mass of preliminary 6.4.2 Heat to boiling and simmer gently for 15 min
sub-sample for total sulphate content method in a fume cupboard (6.1.2.4). Filter through a
Nominal maximum size of Minimum mass of medium filter paper (6.1.2.5). Ensure that the
aggregate sub-sample filtrate is clear. If not, refilter with a fine filter
mm kg paper. Wash thoroughly with hot distilled water.
63 50 Collect the filtrate and washings in a 500 mL beaker
50 35 (6.1.2.2) and dilute to 300 mL with distilled water.
40 15 NOTE When analysing extracts for water soluble sulphate
28 5 (see 5.5.2.2) filtration will not normally be necessary unless the
aggregate contains sulphides (e.g. slags). When such aggregates
20 2 are being tested, stand the solution in a warm place for 30 min
14 1 after simmering. If a white precipitate develops, filter through a
10 0.5 medium filter paper and wash thoroughly with hot distilled
5 or less 0.2 water and continue as described in 6.4.3.
6.4.3 Boil and add 10 mL barium chloride
6.3.3 Sieve the sub-sample through a 20 mm solution (6.2.2.1) dropwise with constant stirring.
sieve (6.1.1.3) and crush any oversize aggregate to Continue boiling until the precipitate is properly
pass the sieve. Combine, mix thoroughly and where formed and then let the solution stand at just below
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the mass of the sub-sample exceeds 2 kg reduce the boiling point for at least 30 min then leave to cool
sub-sample to 2 kg. Dry the sub-sample by heating for 24 h or overnight.
at a temperature of 105 ± 5 °C to achieve a constant 6.4.4 Transfer the precipitate of barium sulphate
mass to within 0.1 %. Crush all the aggregate to with extreme care to a previously ignited and
pass a 5 mm sieve, mix and reduce to not less weighed sintered silica filter crucible (6.1.2.7) using
than 200 g. Crush all the aggregate to pass a 1 mm suction. Alternatively transfer the precipitate with
sieve and produce a sample of approximately 100 g extreme care to a suitable filter paper in the glass
and grind all this to pass a 150 µm sieve. This is the funnel and filter.
test portion. Carry out all sampling reduction by the
method described in clause 6 of BS 812-102:1984. 6.4.5 In either case wash the precipitate several
times with hot distilled water until the washings are
NOTE With suitable mechanical grinding equipment it is
possible to by-pass some of these stages. For example, a free from chloride as indicated by an absence of
jaw-crusher could be used to crush all the sub-sample to turbidity when a drop is tested with the solution of
pass 5 mm without the preliminary sieving and crushing at silver nitrate (6.2.2.3). If a sintered silica filter
the 20 mm size. Similarly the 200 g sub-sample portion passing
the 5 mm sieve could be crushed to pass 150 µm, by-passing
crucible is used remove it from the filter flask and
the 1 mm size operation, in, for example, a disc mill. The dry at 105 ± 5 °C for approximately 30 min and
intention is to produce a test portion which is fully representative gradually raise the temperature to 800 °C either in
of the laboratory sample. an electric muffle furnace or by other suitable
6.4 Analytical procedure means (6.1.2.9) until no further loss in mass
6.4.1 Weigh accurately to the nearest 0.001 g occurs; 15 min at 800 °C should suffice.
about 3 g of the test portion (prepared as described 6.4.6 Cool the crucible in a desiccator (6.1.2.10) and
in 6.3) and record the mass (m1). Place it in weigh to the nearest 0.001 g, and calculate the mass
a 250 mL beaker (6.1.2.2), add 100 mL of the diluted of the precipitate (m2) from the increase in mass of
hydrochloric acid (6.2.2.2) and stir. Repeat with a the crucible.
second duplicate 3 g of the test portion, and follow 6.4.7 If the precipitate is filtered through a filter
the procedure for both. paper, transfer the filter paper and precipitate to a
NOTE 1 Aggregates containing significant amounts of previously ignited and weighed crucible (6.1.2.8).
carbonates will froth at this stage. In these cases add the acid
slowly while continuously stirring. 6.4.8 If an electric muffle furnace is used, place the
NOTE 2 Aggregates containing sulphide will release H2S on crucible and contents in it at room temperature and
acidification and this will be noticeable by its smell. In these gradually raise the temperature to 800 °C. If a
cases there is a danger that this procedure will overestimate the bunsen or other burner is used, first dry the filter
sulphate content because of sulphide oxidation.
paper and precipitate slowly over a small flame
If the aggregates contain sulphide, place 100 mL of taking care to char the filter paper slowly rather
the diluted hydrochloric acid in a 250 mL beaker than to allow it to inflame, otherwise some of the
and heat to boiling point. Remove from the source of precipitate may be lost, and gradually raise the
heat and, while stirring the acid solution, sprinkle temperature to red heat.
the weighed analytical portion of about 3 g mass on
NOTE Ignition for about 15 min should be sufficient in all
to the acid. cases.

6 © BSI 01-1999
 BS 812-118:1988

6.4.9 Calculate the mass of the precipitate obtained 8 Test report

(m2) from the increase in mass (to the
The test report shall affirm that the sulphate
nearest 0.001 g) of the crucible.
content was determined in accordance with this
6.5 Calculation and expression of results Part of BS 812 and state whether or not a certificate
6.5.1 Calculate the total sulphate content, as a of sampling is available. If available, a copy of the
percentage by mass of the dry aggregate, from the certificate of sampling shall be provided. The test
equation: report shall include the following information:
m ×34.3 a) sample identification;
2
percentage of SO3 = -----------------------
-
m1 b) the sulphate content in g/L of a 2 : 1
water/aggregate extract expressed in g/L; and/or
6.5.2 Express the mean total sulphate content of the
two test portions to the nearest 0.01 % (as SO3) of c) the total sulphate content expressed as a
the dry mass of aggregate. Repeat the test starting percentage by mass of the dry aggregate.
with new 3 g analytical portions if the individual
results differ by more than 0.05 % (SO3).
Licensed Copy: KEO International, KEO International, 25 March 2004, Uncontrolled Copy, (c) BSI

7 Precision
7.1 A precision experiment was carried out on five
aggregates by 10 laboratories. Details of the
experiment and the precision data are given
in Appendix B.
7.2 The uses of the precision data are described
in clause 5 of BS 812-101:1984.

© BSI 01-1999 7
 BS 812-118:1988

Appendix A Semi-quantitative test for NOTE The barium chloride test is very sensitive and an
observable turbidity will eventually form (after
the presence of sulphate ions approximately 1 min), even when the SO3 content of the
aggregate is only 0.004 %. It is also necessary to ensure that the
A.1 Apparatus and reagents water used for testing does not contain sufficient
A.1.1 Apparatus for method 1 or method 2 sulphates (< 20 mg/L) to give a positive result.
(see A.2.2)
Appendix B Details of experiments for
A.1.1.1 Plastics bucket, capacity 10 L.
determining precision of tests for
A.1.1.2 Beaker or plastics drinking cup.
water-soluble sulphate and total
A.1.2 Additional apparatus for method 2 sulphate contents of aggregates
A.1.2.1 Filter paper, medium grade5).
B.1 The precision data given in Table 3 and Table 4
A.1.2.2 Beaker, capacity 500 mL. were determined from an experiment conducted
A.1.2.3 Test tube. in 1984/5 involving 10 laboratories. The experiment
A.1.3 Reagent for method 1 was designed, and the data analysed following the
principles set out in BS 5497-1:1979.
A.1.3.1 Sulphate test strips6).
B.2 The materials used were approximately 200 kg
A.1.4 Reagents for method 2
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lots. With each material, twenty 5 kg to 10 kg

A.1.4.1 Hydrochloric acid solution, made by laboratory samples were prepared and two sent to
diluting 200 mL of concentrated hydrochloric acid each laboratory. The laboratories divided each
(relative density 1.18) to 1 L with water. laboratory sample into four test portions: one was
A.1.4.2 Barium chloride 5 % solution, made by used for the chloride determination described in BS
dissolving 50 g of barium chloride in 1 L of water, 812-117, one for the water-soluble sulphate
and filtered before use, if necessary. determination and two for the total sulphate
A.1.4.3 Measuring cylinder. determination described in this Part of BS 812.
A.1.4.4 Stop watch. B.3 The tests for outliers given in BS 5497-1:1979
were applied to the data. A summary of the results
A.2 Procedure
shown to be outliers by these tests is given in
A.2.1 Place approximately 5 kg of coarse aggregate Table 5 and Table 6.
or 1 kg of sand in the bucket (A.1.1.1) and add an
B.4 Because of the small quantities of the
equivalent mass of water of low sulphate content. aggregates obtained for this experiment, the
Agitate the contents intermittently for 7 h and then estimates of VS measure only that variability which
pour some solution into a beaker or plastics
arises when dividing 100 kg to 200 kg of material
drinking cup (A.1.1.2).
into 5 kg to 10 kg laboratory samples. Likewise the
A.2.2 Carry out one of the following procedures. contribution of sample reduction variability to the
Method 1. Allow any solids to settle and briefly dip estimates of Vr1 consists only of the variability
the sulphate test strip (A.1.3.1) into the clear which arises when dividing 5 kg to 10 kg laboratory
supernatant liquid. After 2 min observe the samples into two test portions. In practice one might
colouration of the three test zones. If none of the test expect VS and perhaps Vr1 to be larger than found in
zones has changed from red to yellow the sulphate this experiment.
in the aggregate can be taken to be less than 0.02 %. B.5 The precision data from Table 3 (water-soluble
Method 2. Filter the solution through a medium sulphate) for four of the materials (limestone, shale,
grade filter paper (A.1.2.1) until gravel and sand) fit the following relationships:
approximately 50 mL solution has been collected. r1 = 0.02 + 0.05 x
Measure 50 mL into a 500 mL beaker (A.1.2.2), R1 = R2 = 0.06 + 0.11 x
add 150 mL water and stir thoroughly. Pour some of
the diluted solution into a test tube (A.1.2.3) so that These may be used to interpolate values of r1, R1
it is half filled, add 5 mL hydrochloric acid (A.1.4.1) and R2 for levels of sulphate ion ( x g/L) between
and 5 to 10 drops barium chloride solution (A.1.4.2) those which appear in Table 3. The blastfurnace
and mix. If there is no turbidity or it has not formed slag gave a higher value of R1 and R2 that that
within 5 s, assume that the aggregate contains less predicted by the relationship. This is attributed to
than 0.02 % sulphate as SO3. the presence of sulphides: this difficulty is overcome
by following the procedure described in the note
to 6.4.2.

5)
Whatman No. 40 has been found suitable.
6)
Merck quant test strips have been found suitable.

8 © BSI 01-1999
 BS 812-118:1988

B.6 The precision data from Table 4 (total sulphate) R2 = 0.05 + 0.58 x
fit the following relationships: These may be used to interpolate values of r1, R1
r1 = 0.03 + 0.01 x and R2 for levels of sulphate ion ( x %) between those
R1 = 0.06 + 0.49 x which appear in Table 4.
Table 3 — Precision data, water-soluble sulphate determination
Aggregate Sulphate ion g/L

n x r1 R1 R2 Vr VL VS
1

14 mm light grey limestone (D) 9 0.01 0.01 0.03 0.003 0.003 0.010 0.003
14 mm sea-dredged gravel and
sand (B) 9 0.14 0.04 0.05 0.06 0.015 0.012 0.004
5 mm medium grey limestone
crushed sand/shell mixture (E) 9 0.17 0.03 0.13 0.13 0.011 0.045 0.000
14 mm blastfurnace slag (A) 8 1.31 0.10 0.60 0.62 0.035 0.210 0.065
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28 mm colliery shale (C) 8 2.13 0.12 0.29 0.29 0.041 0.095 0.000
NOTE n is the number of laboratories whose results were included in the calculation of the precision data. Definitions of x , r1,
R1, R2, Vr1, VL and VS are given in 5.2 of BS 812-101:1984.

Table 4 — Precision data, total sulphate determination

Aggregate Sulphate ion %

n x r1 R1 R2 Vr VL VS
1

14 mm light grey limestone (D) 9 0.02 0.02 0.06 0.06 0.008 0.018 0.006
14 mm sea-dredged gravel and sand (B) 9 0.08 0.05 0.18 0.18 0.017 0.062 0.000
5 mm medium grey limestone crushed
sand/shell mixture (E) 9 0.28 0.03 0.14 0.14 0.012 0.049 0.014
14 mm blastfurnace slag (A) 9 0.52 0.04 0.28 0.30 0.015 0.100 0.034
28 mm colliery shale (C) 9 0.80 0.04 0.50 0.57 0.015 0.177 0.098
NOTE n is the number of laboratories whose results were included in the calculation of the precision data. Definitions of x , r1, R1,
R2, Vr1, VL and VS are given in 5.2 of BS 812-101:1984.

© BSI 01-1999 9
 BS 812-118:1988

Table 5 — Results excluded from calculation of precision data in Table 3

Laboratory Aggregate Laboratory average Between-sample range Between-test-portion range
Laboratory Laboratory
sample 1 sample 2
L2 C Outlier
L3 A Also excluded
L3 B Outlier
L3 C Outlier
L3 D Also excluded
L3 E Outlier
L4 E Outlier
L7 D Outlier
L9 A Outlier (spoiled samples)

Table 6 — Results excluded from calculation of precision data in Table 4

Laboratory Aggregate Laboratory average Between-sample Between-test-portion range
range
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Laboratory Laboratory
sample 1 sample 2
L1 A Outlier
L3 A Outlier
L3 B Also excluded
L3 C Also excluded
L3 D Outlier
L3 E Outlier
L10 C Outlier

10 © BSI 01-1999
 BS 812-118:1988

Publications referred to

BS 410, Specification for test sieves.

BS 812, Testing aggregates.
BS 812-2, Methods for determination of physical properties7).
BS 812-3, Methods for determination of mechanical properties7).
BS 812-4, Methods for determination of chemical properties7).
BS 812-101, Guide to sampling and testing aggregates.
BS 812-102, Methods for sampling.
BS 812-117, Method for determination of water-soluble chloride salts.
BS 1797, Tables for use in the calibration of volumetric glassware.
BS 5497, Precision of test methods.
BS 5497-1, Guide for the determination of repeatability and reproducibility for a standard test method by
interlaboratory tests.
BS 5781, Measurement and calibration systems.
BS 5781-1, Specification for system requirements.
Licensed Copy: KEO International, KEO International, 25 March 2004, Uncontrolled Copy, (c) BSI

BS 8110, Structural use of concrete.

BS 8110-1, Code of practice for design and construction.

7) Referred to in the foreword only. Under revision.

© BSI 01-1999
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