BS812:Partll8:1988

WC f626.07 + [email protected] : [020.1 + 642.217.6 : 64&m]

British Standard
Testing aggregates
Part 118. Methods for determination of
sulphate content

Essais des granulats

Partie 118. Mbthodes de dosage des sulfates

Priifung von Zuschlagstoffen

Teil 118. Verfahren zur Bestimmung des Sulfatgehalts
BS812 ; PartllB: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 : Part 2 :
1975, Part 3 : 1975 and Part 4 : 1976 each test, or collec-
tion 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. Neverthe-
less 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 : Part 101 for general
guidance on testing aggregates, precision of test methods
and variance arising from sampling errors.
Compliance with a British Standard does not of itself
confer immunity from legal obligations.
 BS812:Part118:1988

Contents

Page
Foreword Inside front cover
Committees responsible Back cover

Mathocb
1 -w!
2 Definitions
3 Principle
4 Sampling
5 Determination of the sulphate content of
a 2: 1 water/aggregate extract
6 Determination of the total sulphate content
by acid extraction
7 Precision
8 Test repon

Appendices
A Semi-quantitative test for the presence of
sulphate ions 9
B Details of experiments for determining precision
of tests for water-soluble sulphate and total
sulphate contents of aggregates 9

Tables
1 Minimum mass of preliminary sub-sample for
water-soluble sulphate method 5
2 Minimum mass of preliminary sub-sample for
total sulphate content method 6
3 Precision data, water-soluble sulphate
determination 10
4 Precision data, total sulphate determination 10
5 Results excluded from calculation of precision
data in table 3 11
6 Results excluded from calculation of precision
data in table 4 11

Figure
1 Ion-exchange column for water-soluble sulphates 4
8S812:Part118:1988

Methods

1 Scope 3.2 Method for total sulphate content

The sulphates are extracted from a crushed sample of
This Part of BS 812 describes two methods for aggregate by dilute hydrochloric acid. Barium chloride
determining the sulphate content of aggregates. solution is added to the extract. The precipitate of barium
The first method determines the water-soluble sulphate sulphate is collected, dried and weighed and the total
content of aggregates, which applies to natural and synthetic sulphate content is calculated.
aggregates to be used as 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 used in concrete The sample to be used for the test (the laboratory sample)
and cement bound materials. shall be taken in accordance with the procedure described
in clause 5 of BS 812 : Part 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 moisture
produce a method for the determinatin of total water-soluble content as well as the solids by preventing loss of moisture,
sulphate because of low water solubility of calcium sulphate.
except through evaporation, throughout the sampling
For practical purposes for aggregates in concrete the total sulphate
content determined by this method is taken to be the same as the procedure and at any subsequent stage up to the point
total water-soluble sulphate content. of test.
NOTE 2. In appendix A two procedures for a semi-quantitative test NOTE. This is necessary because where the aggregate to be tested
are described. It is stronglv recommended that one of these is used carries surface water the sulphates will normally be dissolved,
as a preliminary check before resorting to the test described in the at least partly, in both this and the absorbed water and hence the
main text, which may be needed for compliance with a specification. sulphate content will ba affected by migration of water 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 content of

2 Definitions a 2:l water/aggregate extract
For the purposes of this Part of 8S 812, the definitions NOTE. Calcium sulphate is relatively harmless because of its limited
given in BS 812 : Part 101 and Part 102 apply. 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 : Part 1 : 1985.

3 Principle 5.1 Apparatus

3.1 Method for water-soluble sulphates 5.1.1 Apparatus for preparation of test portion and
extraction of the sulphate (see 5.4 and 5.5.1)
An aggregate sample is extracted with twice its own mass
of distilled or demineralized water to remove water-soluble 5.1.1.1 Well ventilated oven, capable of being controlled
sulphate ions. The water-soluble sulphate content is to maintain a temperature of 105 f 5 ‘C.
determined by either an ion-exchange method or a gravi-
5.1.1.2 Balance, capable of weighing up to 5 kg accurate
metric method in one of the following ways.
to 5 g. The balance shall be regularly calibrated as specified
(a) Some of the extract is transferred to an ion-exchange in BS 5781 : Part 1.
column and the eluate is titrated with standardized
sodium hydroxide solution. 5.1.1.3 Test sieve, 20 mm square hole perforated plate
complying with BS 410.
(b) Some of the extract is treated with diluted hydro-
chloric acid. Barium chloride solution is added and the 5.1.1.4 Pestle and mortar, or suitable mechanical crusher.
precipitate is collected, dried and weighed. NOTE. This is not required for aggregate all passing the 20 mm sieve.
The ion-exchange method measures the presence of 5.1.1.5 Two plastics or metal bottles, wide-mouthed,
sulphate ions. When other anions (see note) are present this
screw-capped. The bottles shall be 5 L capacity when
method is precluded. The gravimetric method is applicable
testing coarse aggregates or 2 L when testing fine aggregate.
when aggregates containing sulphides (i.e. slags) are being
analysed. 5.1.1.6 Mechanical shakers or rollers, to take the extrac-
NOTE. Anions of strong acids, e.g. chlorides, nitrates and phos- tion bottles (5.1.1.5).
phates, interfere with the ion-exchange method and are apparently
measured as sulphate. However, when chloride is the only other ion 5.1 .1.7 Two filter funnels, of approximately 100 mm
present, and ;t has been quantitatively determined, the ion-exchange diameter with medium grade” filter papers of a diameter
method described can be used provided the result is corrected as appropriate to the size of the funnel.
shown in 5.62.

‘Whatman No. 40 have been found suitable.

2
 BS812:Part118:1988

5.1.1.8 Beakers. 5.2.2.4 Nitric acid (c(HNOs) = approximately 1 mol/L),

made by diluting 15 mL of concentrated nitric acid
51.2 Apparatus for the ion-exchange method (see 5.3
(relative density 1.42) to 100 mL with water.
and 5.5.2.1)
5.2.2.5 Sodium hydroxide solution (c(NaOH) = approxi-
5.1.2.1 Pipette, 50 mL size, grade B in accordance
mately 0.1 mol/L), made by dissolving 2 g of sodium
with BS 1797.
hydroxide in 500 mL of water. Determine the exact
5.1.2.2 An ion-exchang8 column and reuwvoir. concentration (in mol/L) by titration against potassium
NOTE. A typical design is shown in figure 1. hydrogen phthalate or with a standardized acid solution,
and keep the solution in an airtight plastics container
5.1.23 Conical flasks, 500 mL capacity. At least two
(5.1.4.1).
are required.
5.2.2.6 Indicator, giving a distinct colour change in the
5. I .2.4 Graduated measuring cylinder, capacity 100 m L,
pH range 4 to 5.
grade B in accordance with BS 1797.
NOTE. Screened methyl orange is suitable.
5.1.2.5 Burette, 50 mL size, grade B in accordance
6.2.2.7 Silver nitrate solution, made by dissolving 0.5 g
with BS 1797.
of silver nitrate in 100 mL of water. Store the solution in
5.1.2.6 Beakers. an amber-coloured glass reagent bottle (5.1.4.2).
5.1.3 Apparatus for the gravimetric method (see 5.5.2.2) 5.3 Preparation of the ion-exchange column
5.1.3.1 Pipette, 50 mL size, grade B in accordance with NOTE. This procedure is not required if the ion-exchange column
BS 1797. method is not used (see 3.1).

5.1.3.2 Apparatus as listed in 6.1.2.1 to 6.1.2.10. 5.3.1 Empty a quantity of cation-exchange resin (5.2.2.1))
sufficient to half-fill the column (5.122). into a
5.1.4 Apparatus for preparation of reagents (see 5.2.2) beaker (5.1.2.6) and stir with water. Empty this suspension
of resin in water into the column so that when the resin
5.1.4.1 Plastics container, airtight. has settled, there is approximately 20 mm depth of water
5.1.4.2 Amber-coloured glass reagent bottle. above the resin when the surplus water has drained away.
Maintain this depth of water above the resin at all times
5.2 Reagents as it is important that the resin is not allowed to dry out.

5.2.1 Gen8m/. Reagents of recognized analytical quality 5.32 Activate the cationexchange resin by leaching with
and only distilled water or water of equivalent quality shall 100 mL of the hydrochloric acid solution (5.2.2.2)
be used. followed by washing with distilled water. Place the acid
NOTE 1. Where accurately standardired solutions are required it in the reservoir and leave the apparatus until the acid has
may be more convenient to obtain them already standerdized to passed through the column, Rinse and fill the reservoir
be used in accordance with the manufacturer’s instructions. with distilled water and leave the water to percolate
NOTE 2. If the ion-exchange column method is not used, through until the liquid coming from the column gives no
the reagents described in 5.2.2.1 to 5.2.2.7 are not required. turbidity when tested with about I mL of silver nitrate
5.2.2 /?8ag8ntS solution (5.2.2.7) acidified with about five drops of nitric
acid (5.2.2.4).
5.2.2.1 Cationexchange resin, strongly acid*.
5.3.3 Regenerate the cation-exchange resin in the manner
5.2.2.2 Hydrochloric acid solution (c(HCI) = approxi- described in 5.32 after it has been used for four consecu-
mately 4 mol/L), made by diluting 390 mL concentrated tive determinations.
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.

‘A suitable material is Zerolit 225 or Amberlite lR-120.

3
BS812:Part118:1988

19126 socket
( not required
constant head
not used 1

Cation-exchange
resin

Glass wool pad

Rubber bung -
bored to take
glass tube

(a) ion-exchange column

24 129 stopper

--El

Glass tube fused to

Round bottomed
side of flask to
flask 500 mL
provide stability
capacity

-3 i.d.

19126 cone

Ib) Constant head device for use with ion-exchange column

All dimensions are in millimetres.

Figure 1. Ion-exchange column for water-soluble sulphates

4
 BS812:Part118:1988

5.4 Preparation of test portion 5.5.2 Determination of the sulphate in the extracts
54.1 Dry the laboratory sample at a temperature 5.5.2.1 /on-exchange method. With a pipette (5.1.2.1)
of 105 2 5 “C to remove surface water so that the sample transfer 50 mL of filtered extract to the top of the
is free flowing. ion-exchange column and allow to drain through the
resin.
5.4.2 Reduce the laboratory sample by the procedures
described in clause 6 of BS 812 : Part 102 : 1984 to an Rinse the resin with two 75 mL increments of distilled
amount not less than the mass given in table 1 appropriate water collecting all the solution and washings in a conical
to the nominal size of the aggregate. flask (5.1.2.3) placed under the outlet of the column.
Add three to five drops of the indicator (5.2.2.6) to the
contents of the conical flask and titrate to the colour
Table 1. Minimum mass of preliminary sub-sample change with the standardized sodium hydroxide
for water-soluble sulphate method solution (5.2.2.5).
Replace the flask under the outlet of the column and pass
Nominal maximum size Minimum ma= of
of xggrogxte sub-sxmplo a further 75 mL of distilled water through the resin. If the
indicator colour changes to show that more acid has been
mm washed from the resin, titrate again to neutrality.
kg
63 50 Record the total volume of standardized sodium hydroxide
50 35 solution used (vl I.
40 15 Repeat with another 50 mL aliquot of the filtrate and
28 or less 5 record the volume of standardized sodium hydroxide
solution used (v2 1.
Take the mean value of v1 and vz (VI.
5.4.3 Sieve the sub-sample through a 20 mm sieve (5.1.1.3)
and crush any oversize aggregate to pass the sieve avoiding If the values of v1 and ~2 differ by more than 0.5 mL
excessive grinding. Combine, mix thoroughly and by suitable repeat the procedure.
sample reduction techniques produce two test portions Repeat the complete procedure with a second test portion.
each of about 2 kg mass for coarse aggregate or two test
portions each of about 500 g mass for sand. Dry the test 5.5.2.2 Gravimetric method. Transfer 50 mL of filtered
portions by heating at a temperature of 105 + 5 ‘C to extract to a 500 mL beaker, dilute to 300 mL with distilled
achieve a dry mass which is constant to within 0.1 %. or demineralized water, add 10 mL of hydrochloric acid
solution (5.2.2.3) and carry out the procedure described in
5.5 Analytical procedure 6.4.2 to 6.4.8.
NOTE. When aggregates containing sulphide are being analysed
5.5.1 Preparation of extracts see the note to 6.43.

5.5.1.1 For coarse aggregates use the two plastics or metal Repeat the procedure with a second test portion.
bottles of 5 L capacity and for fine aggregate use the two
bottles of 2 L capacity (5.1.1.5). Weigh each bottle and 5.8 Calculation and expression of results
record its mass to the nearest 5 g. 5.6.1 If no other anions are present, calculate the
5.5.1.2 Transfer the test portions obtained as described concentration of sulphate ions, (as SOa in g/L), present
in 5.4 to the bottles, weigh bottle and contents and record in the extracts, from the equation:
their mass to the nearest 5 g. Calculate the mass of concentration of SOa = 0.8m V
aggregate in each bottle by difference. where
5.5.1.3 Add to each bottle a mass of distilled or V is the volume of sodium hydroxide solution (in mL);
demineralized water equal to twice the mass of the test m is the concentration of sodium hydroxide solution
portion. Fasten the water-tight bottle closures and mix the (in mol/L).
contents by shaking or rolling continuously for a minimum
of 24 h. 5.6.2 If chlorides are the only other ions present, calculate
NOTE. If mechanical agitation equipment is not used and the the concentration of sulphate ions, (as SOB in g/L), present
sample and water are merelv allowed to remain in contact with in the extracts from the equation:
occasional shaking there is a possibility (particularly if the source
concentration of SOa = 0.8m V - 5.64C
of sulphate is, for example, large crystals of gypsum) that the
sulphate which could theoretically dissolve will not all be extracted where
in 24 h.
C is the chloride ion content as a percentage by mass
5.5.1.4 Filter the extracts through dry, medium-grade of dry aggregate.
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).

5
BS812:Part118:1988

5.6.3 When the gravimetric method has been used, 6.1.2.8 Ignition crucibles, approximately 35 mm in
calculate the sulphate concentration of sulphate ions, diameter and 40 mm in height and capable of maintaining
(as SOa in g/L), present in the extracts from the equation: a constant mass when heated to 800 ‘C.
NOTE. These crucibles are not required if the filtering crucibles
concentration of SOS = 6.86m,
(6.1.2.7) are used. Porcelain. silica or platinum are suitable
where materials for ignition crucibles.
m2 is the mass of precipitate obtained in 6.4.9 (in 9). 8.1.2.9 A suitable means of igniting the pnrcipitate,
5.6.4 Express the mean sulphate contents of the 2: 1 preferably an electric muffle furnace capable of reaching
extracts to the nearest 0.1 g/L. If the individual results and maintaining 800 ‘C.
differ by more than 0.1 g/L and rl , (calculated from B.5) 6.1.2.10 Dessicator.
repeat the test starting with new analytical test portions
(see 5.4). . 8.1.3 Apparatus for preparation of magents (see 8.2.2)
NOTE. With aggregates containing discrete crystals of gypsum it
6.1.3.1 Ambercoloured glass megent bottle.
may be difficult to obtam close agreement between individual
test portions.
6.2 Reagents
8.2.1 Genera/. Reagents of recognized analytical quality
6 Determination of the total sulphate and only distilled water or water of equivalent quality
content by acid extraction shall be used.
6.2.2 Reagents
6.1 Apparatus
6.2.2.1 Barium chloride, 5 % solution, made by dissolving
6.1.1 Apparatus for preparation of test portion (see 6.3) 50 g of barium chloride in 1 L of water, and filtered before
6.1.1.1 Well ventilated oven, capable of being controlled use if necessary.
to maintain a temperature of 105 + 5 ‘C. 6.2.2.2 Dilute hydrochloric acid, made by diluting 100 mL
6.1.1.2 Balance, capable of weighing up to 5 kg accurate of concentrated hydrochloric acid (relative density 1.18)
to 5 g. The balance shall be regularly calibrated as specified to 1 L with water.
in BS 5781 : Part 1. 6.2.2.3 Silver nitrate solution, made by dissolving 0.5 g
6.1.1.3 Test sieves, 20 mm, 5 mm, 1 mm and 150 pm of silver nitrate in 100 mL of water. Store the solution
complying with BS 410. in an amber-coloured glass reagent bottle (8.1.3.1).

6.1 .1.4 Pestle and mortar, or suitable mechanical crusher. 8.3 Preparation of test portion
6.1.2 Apparatus for analysis of test portion 6.3.1 Dry the laboratory sample at a temperature
of 105 + 5 ‘C to remove surface water so that the sample
6.1.2.1 Balance, capable of weighing up to 100 g accurate
is free flowing.
to 0.001 g. The balance shall be regularly calibrated as
specified in 8s 5781 : Part 1. 6.3.2 Reduce the laboratory sample by the procedures
described in clause 6 of BS 812 : Pat-t 102 : 1984 to an
6.1.2.2 Beakers, capacity 250 mL and 500 mL.
amount not less than the mass given in table 2 appropriate
6.1.2.3 Electric hot-plate, capable of being controlled to to the nominal maximum size of aggregate.
boil the contents of beakers without causing undue
overheating. Table 2. Minimum mass of preliminary sub-sample
for total sulphate contint method
6.1.2.4 Fume cupboard.
6.1.2.5 Two filter funnels, of approximately 100 mm Nominal maximum sire Minimum maa of
diameter with medium grade’ and fine gradet filter papers of aggragato rub-mm&
of a diameter appropriate to the size of the funnels.
mm kg
6.1.2.6 Dropping pipette, capacity 10 m L.
63 50
6.1.2.7 Sintered silica filtering crucibles, porosity grade 4, 50 35
approximately 35 mm in diameter and 40 mm in height. 40 15
NOTE. These are not required if filtration through fine gradet 28 5
filter papers is preferred.
20 2
14 1
10 0.5
5 or less 0.2

*Whatman No. 40 is suitable, but fine filter paper, e.g. Whatman NO. 42 may be necessary if the filtrate is not completely clear.
tWhatman No. 42 is suitable.

6
 BS812:Part118:1988

6.3.3 Sieve the sub-sample through a 20 mm sieve (6.1.1.3) 6.4.3 Boil and add 10 mL barium chloride solution
and crush any oversize aggregate to pass the sieve. Combine, (6.2.2.1) dropwise with constant stirring. Continue boiling
mix thoroughly and where the mass of the sub-sample until the precipitate is properly formed and then let the
exceeds 2 kg raduca the sub-sample to 2 kg. Dry the sub- solution stand at just below boiling point for at least
sample by heating at a temperature of 105 f 5 ‘C to 30 min then leave to cool for 24 h or overnight.
achieve a constant mass to within 0.1 %. Crush all the
aggregate to pass a 5 mm sieve, mix and reduce to not less 6.4.4 Transfer the precipitate of barium sulphate with
than 200 g. Crush all the aggregate to pass a 1 mm sieve extreme care to a previously ignited and weighed sintered
and produce a sample of approximately 100 g and grind all silica filter crucible (6.1.2.7) using suction. Alternatively
this to pass a 150 pm sieve. This is the test portion. Carry
transfer the precipitate with extreme care to a suitable
out all sampling reduction by the method described in filter paper in the glass funnel and filter.
clause 6 of BS 812 : Part 102 : 1984. 6.4.5 In either case wash the precipitate several times with
NOTE. With suitable mechanical grinding equipment it is possible hot distilled water until the washings are free from chloride
to by-pass some of these stages. For example, a jaw-crusher could as indicated by an absence of turbidity when a drop is
bs use0 to crush all the sub-sample to pass 5 mm without the tested with the solution of silver nitrate (6.2.2.3). If a
preliminary sieving and crushing at the 20 mm size. Similarly the
200 g sub-sample portion passing the 5 mm sieve could be crushed sintered silica filter crucible is used remove it from the
to pass 150 urn, by-passing the 1 mm size operation, in, for example, filter flask and dry at 105 f 5 ‘C for approximately 30 min
a disc mill. The intention is to produce a test portion which is and gradually raise the temperature to 800 “C either in an
fully representative of the laboratory sample. electric muffle furnace or by other suitable means (6.1.2.9)
until no further loss in mass occurs; 15 min at 800 ‘C
0.4 Anrlytial procedure should suffice.
6.4.1 Weigh accurately to the nearest 0.001 g about 3 g 6.4.6 Cool the crucible in a desiccator (6.1.2.10) and
of the test portion (prepared as described in 6.3) and weigh to the nearest 0.001 g, and calculate the mass of the
record the mass (m, 1. Place it in a 250 mL beaker (6.1.221, precipitate (m2 ) from the increase in mass of the crucible.
add 100 mL of the diluted hydrochloric acid (6.2.2.2)
and stir. Repeat with a second duplicate 3 g of the test 6.4.7 If the precipitate is filtered through a filter paper,
portion, and follow the procedure for both. transfer the filter paper and precipitate to a previously
NOTE 1. Aggregates containing significant amounts of carbonates ignited and weighed crucible (6.1.2.8).
will froth at this stage. In these cases add the acid slowly while
v:* continuously stirring.
6.4.8 If an electric muffle furnace is used, place the
crucible and contents in it at room temperature and
NOTE 2. Aggregates containing sulphide wit1 release HIS on
acidification and this will be noticeable by its smell. In these cases gradually raise the temperature to 800 “C. If a bunsen
there is a danger that this procedure will overestimate the sulphate or other burner is used, first dry the filter paper and
content &cause of sulphide oxidation. precipitate slowly over a small flame taking care to char
If the aggregates contain sulphide, place 100 mL of the the filter paper slowly rather than to allow it to inflame,
diluted hydrochloric acid in a 250 mL beaker and heat otherwise some of the precipitate may be lost, and
to boiling point. Remove from the source of heat and, gradually raise the temperature to red heat.
while stirring the acid solution, sprinkle the weighed NOTE. Ignition for about 15 min should be sufficient in all cases.
analytical portion of about 3 g mass on to the acid.
6.4.9 Calculate the mass of the precipitate obtained (m2 1
6.4.2 Heat to boiling and simmer gently for 15 min in a from the increase in mass (to the nearest 0.001 g) of the
fume cupboard (6.1.2.43. Filter through a medium filter crucible.
paper (6.125). Ensure that the filtrate is clear. If not,
refilter with a fine filter paper. Wash thoroughly with hot 6.5 Calculation and expression of results
distilled water. Collect the filtrate and washings in a
6.5.1 Calculate the total sulphate content, as a percentage
500 mL beaker (6.122) and dilute to 300 mL with
by mass of the dry aggregate, from the equation:
distilled water.
NOTE. When analysing extracts for water soluble sulphate m2 x 34.3
(see 5.6.2.2) filtration will not normally k necessary unless the percentage of SOs =
ml
aggregate contains sulphides (e.g. slagsL When such aggregates
are being tested, stand the solution in a warm place for 30 min 6.5.2 Express the mean total sulphate content of the two
after simmering. If a white precipitate develops, filter through
a medium filter paper and wash thoroughly with hot distilled
test portions to the nearest 0.01 % (as SOs) of the dry
water and continue as described in 8.4.3. mass of aggregate. Repeat the test starting with new 3 g
analytical portions if the individual results differ by more
than 0.05 % (SOs 1.
8S812: Part118:1988

7 Precision 8 Test report

7.1 A precision experiment was carried out on five The test report shall affirm that the sulphate conten? was
aggregates by 10 laboratories. Details of the experiment determined in accordance with this Part of 8s 812 and state
and the precision data are given in appendix 8. whether or not a certificate of sampling is available.
If available, a copy of the certificate of sampling shall be
7.2 The uses of the precision data are described in clause 5 provided. The test report shall include the following
of 8S812 : Part 101 : 1984. information:
(a) sample identification;
(b) the sulphate content in g/L of a 2: 1 water/aggregate
extract expressed in g/L; and/or
(c) the total sulphate content expressed as a percentage
by mass of the dry aggregate.

8
 BS812:Part118:1988

Appendices

Appendix A. Semi-quantitative test for the mix. If there is no turbidity or it has not formed within 5 s,
assume that the aggregate contains less than 0.02 % sulphate
presence of sulphate ions as SOB.
NOTE. The barium chloride test is very sensitive and an observable
A.1 Apparatus and reagents turbidity will eventually form (after approximately 1 mini, even
when the SO3 content of the aggregate is only 0.004 %. It IS also
necessary to ensure that the water used for testing does not contain
A.l.l Apparatus for mathod 1 or mathod 2 (see A.2.2) sufficient sulphates I< 20 mg/L) to give a positive result.

A.l.l .l Plastics bucker, capacity 10 L.

A.1 .1.2 Beaker or plastics drinking cup.
Appendix B. Details of experiments for
A.1.2 Additional apparatus for mathod 2 determining precision of tests for
water-soluble sulphate and total sulphate
A.1.2.1 Filterpaper, medium grade*.
contents of aggregates
A.1.2.2 Beaker, capacity 500 mL.
A-1.2.3 Test tube. B.l The precision data given in tables 3 and 4 were
determined from an experiment conducted in 1984/5
involving 10 laboratories. The experiment was designed,
A.1.3 Reagant for method 1
and the data analysed following the principles set out
A.1.3.1 Sulphate rest strips+. in 8s 5497 : Part 1 : 1979.
B.2 The materials used were approximately 200 kg lots.
A.1.4 Reagants for mathod 2
With each material, twenty 5 kg to 10 kg laboratory samples
A.1.4.1 Hydrochloric acid solution, made by diluting were prepared and two sent to each laboratory.
200 mL of concentrated hydrochloric acid (relative The laboratories divided each laboratory sample into four
density 1.18) to 1 L with water. test portions: one was used for the chloride determination
A.1.4.2 Barium chloride 5 % solution. made by dissolving described in 8s 812 : Part 117, one for the water-soluble
sulphate determination and two for the total sulphate
50 g of barium chloride in 1 L of water, and filtered before
determination described in this Part of 8s 812.
use, if necessary.
6.3 The tests for outliers given in BS 5497 : Part 1 : 1979
A.l.4.3 Measuring cylinder.
were applied to the data. A summary of the results shown
A.l.4.4 Srop watch. to be outliers by these tests is given in tables 5 and 6.
8.4 Because of the small quantities of the aggregates
obtained for this experiment, the estimates of Vs measure
A2 Procedure only that variability which arises when dividing 100 kg to
200 kg of material into 5 kg to 10 kg laboratory samples.
A.2.1 Place approximately 5 kg of coarse aggregate or 1 kg Likewise the contribution of sample reduction variability
of sand in the bucket (A.l.l.l) and add an equivalent mass to the estimates of Vr, consists only of the variability
of water of low sulphate content. Agitate the contents which arises when dividing 5 kg to 10 kg laboratory samples
intermittently for 7 h and then pour some solution into a into two test portions. In practice one might expect V,
beaker or plastics drinking cup (A.1.1.2). and perhaps Vr, to be larger than found in this
experiment.
A.2.2 Carry out one of the following procedures.
Method 1. Allow any solids to settle and briefly dip the 8.5 The precision data from table 3 (water-soluble
sulphate test strip (A.1.3.1) into the clear supernatant sulphate) for four of the materials (limestone, shale,
liquid. After 2 min observe the colouration of the three gravel and sand) fit the following relationships:
test zones. If none of the test zones has changed from rl = 0.02 + 0.05 X
red to yellow the sulphate in the aggregate can be taken RI = R2 = 0.06 + 0.11 3T
to be less than 0.02 %.
These may be used to interpolate values of rl , RI and R2
Method 2. Filter the solution through a medium grade
for levels of sulphate ion ( 2 g/L) between those which
filter paper (A.1.2.1) until approximately 50 mL solution
appear in table 3. The blastfurnace slag gave a higher value
has been collected. Measure 50 mL into a 500 mL
of RI and R, that that predicted by the relationship.
beaker (A.1 -2.21, add 150 m L water and stir thoroughly.
This is attributed to the presence of sulphides: this diffi-
Pour some of the diluted solution into a test tube (A.1 2.3)
culty is overcome by following the procedure described
so that it is half filled, add 5 mL hydrochloric acid (A.1.4.1) in the nOte to 6 4 2
. . .
and 5 to 10 drops barium chloride solution (A.1.4.2) and

*Whatman No. 40 has been found suitable.

thlerck quant test strips have been found suitable.

9
BS 812 : Part 118 : 1988

8.6 The precision data from table 4 (total sulphate) fit R2 = 0.05 + 0.58 ST
thefollowing relationships: These may be used to interpolate values of rl , RI and R1
fl = 0.03 + 0.012 for levels of sulphate ion (i7 %) between those which
R, = 0.06 + 0.49F appear in table 4.

Table 3. Precision data, water-soluble sulphate determinaticn

TSulphate ion g/L
11
RI ‘72 h, lk dvs
14 mm light grey limestone (D) 0.01 0.03 0.03 0.003 0.010 0.003
14 mm sea-dredged gravel and sand (8) 0.04 0.05 0.06 0.015 0.012 0.004
5 mm medium grey limestone crushed +
sand/shell mixture (E) 0.13 0.13 0.011 0.045 0.000
14 mm blastfumace slag (A) 0.60 0.62 0.035 0.210 0.065
, P, y iery shale (Cl 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 z, fl,
‘,, VL and V5 are given in 5.2 of BS 912 : Part 101 : 1984.

Table 4. Precision data, total sulphate determination

j A-to I Sulphato ion %

n x rl Rl R2 Y/V,,
14 mm light grey limestone (D) 0.02 0.02 0.06 0.06 0.008
14 mm sea-dredged gravel and sand (B) 0.08 0.05 0.18 0.18 0.017
5 mm medium grey limestone crushed
sand/shell mixture (E) 0.28 0.03 0.14 0.14 0.012
14 mm blastfurnace slag (A) 0.52 0.04 0.28 0.30 0.015
28 mm colliery shale (C) 0.80 0.04 0.50 0.57 0.015

NOTE. n IS the number of laboratories whose results were included in the calculation of the precision data. Definitions of 5 rl,
RI. R2, VI,, VL and Vs ace given in 5.2 of 5s 812 : Part 101 : 1984.

10
Trblr 5. Raults rxduded from calculation of pmision data in tabh 3

Laboratory Aggngste Lab0m-w - Batvmn-umplr bm-tat-portion rm

m
Labontory L a b o r a t o r y
umplo 1 sampI 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)

Tabk 6. Results rxdti from calculation of pm&ion data in table 4

Botwoon-rrmph
nngr
Laboratory
samplo 1
I
Batwaon-tat-portion ranga

Laboratory
lamplo 2
I

Ll A Outlier
L3 A Outlier
L3 B Also excluded
L3 C Also excluded
L3
L3
LlO
D
E
C
Outlier
Outlier
I
Outlier

11
Publications refarred to
BS 410 Specification for test sieves
8sai2 Testing aggregetes
*Part 2 Methods for determination of physical properties
*Part 3 Mathods for determination of mechaniil properties
‘Part 4 Methods for determination of chamical properties
Part 101 Guide to sampling and testing aggregetes
Part 102 Methods for sampling
Part 117 Method for determination of water-soluble chloride salts
BS 1797 Tables for use in the calibration of volumetric glassware
ES 5497 Precision of test methods
Part 1 Guide for the determination of repeatability and mproducibility for a standard test method by interlaboratory tests
es 5781 Measurement and calibration systems
Part 1 Specifkation for system requirements
BS 8110 Structuml use of concmte
Part 1 Coda of practice for design and construction

*Referred to in the foreword only. Under revision.

 BS812:Part118:1988
This British Standard, having been prepared under the direction of implementing the standard, of necessary details such as symbols and
the Cement Gypsum, Aggregates end Quarry Products Standards size, tvpe or grade designetlons. Enquirres should be addressed to
Committaa, was published under the authority of the Board of BSI the Publications Manager, BSI, Linford Wood, Milton Kevnes
end comes into effect on 31 August 18BB. MK14 6LE. The number for telephone enquiries is 0908 220022
end for telex 825777.
Q British Standards Institution, 1988
Contrect requirements. A 8rmsh Standard does not purport ro
ISBN 0 580 16534 5
Include all the necessary provmons of a contract Users of Brrtlsh
The followlng BSI references relate to the work on this standard: Standards are responsrble for their correct applrcatcon.
CommIttee reference CA812 Draft for comment 84114036 DC

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Committees responsible for this British Standard

The preparation of this British Standard was entrusted by the Cement Makers’ Federation
Cement Gypsum, Aggregates and Duarry Products Standards Chartered Institute of Building
Committee (CA8/-) to Technical Committee CAB/Z, upon which Concrete Society
the following bodies were represented: County Surveyors’ Society
Aggregate Concrete Block Association Department of the Environment (Building Research Estebhshment)
Association of Consulting Engineers Department of the Environment (Property Services Agencv)
Association of Consulting Scientists Department of Transport (Highwavs)
Association of Lightweight Aggregate Manufacturers Department of Transport (Transport and Road Research
Brick Development Association Laboratory)
British Aggregate Construction Materiels Industries Electricity Supply Industry in England and Wales
British Ceramic Research Ltd. Federation of Civil Engineering Contractors
British Civil Engineering Test Equipment Manufacturers’ Institute of Concrete Technology
Association Institution of Civil Engineers
British Geological Sciences Institution of Highways and Transportation
British Precast Concrete Federation Ltd. Institution of Structural Engineers
British Readv Mixed Concrete Association Institution of Water end Environmental Management (IWEM)
British Steel industry Mortar Producers’ Association Limited
Building Employers’ Confederation Send and Gravel Association Limited
Calcium Silicate Brick Association Limited Society of Chemical Industry
Cement and Concrete Association

Amendments issued since publication

Amd. No. Date of issue Text affected ic

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