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ISBN 978-0-626-30922-0
SANS 5850-2:2008
Edition 1.3

Any reference to SABS SM 850-2 is deemed

to be a reference to this standard
(Government Notice No. 1373 of 8 November 2002)

SOUTH AFRICAN NATIONAL STANDARD

Sulfates content of fines in aggregates Amdt 1

Part 2: Acid-soluble sulfates in fines in

aggregates

Published by SABS Standards Division

1 Dr Lategan Road Groenkloof Private Bag X191 Pretoria 0001
Tel: +27 12 428 7911 Fax: +27 12 344 1568
www.sabs.co.za
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SANS 5850-2:2008
Edition 1.3

Table of changes
Change No. Date Scope
Amdt 1 1998 Amended to change the number, the title of this standard and to
change the reference of first revision to the first edition.
Amdt 2 2002 Amended to update normative references.
Amdt 3 2008 Amended to change the designation of SABS standards to SANS
standards, and to update referenced standards.

Foreword
This South African standard was approved by National Committee SABS/TC 081/SC 01, Construction
materials, products and test methods – Cement, lime and concrete, in accordance with procedures of
the SABS Standards Division, in compliance with annex 3 of the WTO/TBT agreement.

This document was published in August 2008. This document supersedes SABS SM 850-2:2002
(edition 1.2).

A vertical line in margin shows where the text has been technically modified by amendment No. 3.

Reaffirmed and reprinted in August 2014.

This document will be reviewed every five years
and be reaffirmed, amended, revised or withdrawn.

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SANS 5850-2:2008
Edition 1.3

Sulfates content of fines in aggregates Amdt 1

Part 2:
Acid-soluble sulfates in fines in aggregates

1 Scope and field of application

This part of SANS 5850 specifies a method for determining the acid-soluble sulfates content of fines in
aggregates.

NOTE Acid-soluble sulfates can be detrimental to roads, to stabilized foundations for paved areas and to
concrete.

2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of
this part of SANS 5850. All standards are subject to revision and, since any reference to a standard is
deemed to be a reference to the latest edition of that standard, parties to agreements based on this part
of SANS 5850 are encouraged to take steps to ensure the use of the most recent editions of the
standards indicated below. Information on currently valid national and international standards can be
obtained from the SABS Standards Division.

BS 3978, Specification for water for laboratory use. Amdt 3

ISO 3696, Water for analytical laboratory use – Specification and test methods. Amdt 3

SANS 3310-1/ISO 3310-1, Test sieves – Technical requirements and testing – Part 1: Test sieves of
metal wire cloth. Amdt 2

SANS 3310-2/ISO 3310-2, Test sieves – Technical requirements and testing – Part 2: Test sieves of
perforated metal plate. Amdt 2

SANS 197, Preparation of test samples of aggregates.

3 Reagents
Use only water that complies with the requirements of ISO 3696 and reagents of analytical reagent
grade or (when analytical reagent grade is unobtainable) of the purest grade available. Use only
glassware made of borosilicate glass. Store all calibration solutions in polyethylene containers that have
been rinsed with 50 % nitric acid solution prior to use. Amdt 3

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3.1 Hydrochloric acid

Hydrochloric acid, concentrated, analytical reagent of relative density 1,16.

3.2 Dilute hydrochloric acid

Concentrated hydrochloric acid (see 3.1) diluted with water in the volumetric proportions 1:1, 1:9 and
1:99.

3.3 Cation exchange resin

A suitable cation exchange resin in strong acidic form and of particle size 150 ȝm to 300 ȝm.

3.4 Barium chloride solution

10 g of barium chloride dihydrate (BaCl2.2H2O) dissolved in water and diluted to 100 mL.

4 Apparatus
4.1 Test sieves, of nominal aperture sizes 4 750 ȝm, 1 700 ȝm, 425 ȝm, and 125 ȝm and that comply
with the requirements of SANS 3310-1 or SANS 3310-2. Amdt 2

4.2 Mortar and rubber-covered pestle.

4.3 Stirring device, that consists of combined magnetic stirrer and hot-plate with
polytetrafluoroethylene-covered magnetic stirring bars of suitable size.

4.4 Witt filter apparatus, fitted with a Buchner funnel of diameter approximately 90 mm.

4.5 Evaporation dish, of capacity approximately 100 mL.

4.6 Platinum crucible, ignited and tared.

4.7 Cation exchange column, that consists of a glass column, of length 400 mm and of internal
diameter 15 mm, one end of which is provided with a stopcock and the other end with a reservoir of
capacity 200 mL.

The cation exchange column is prepared as follows:

a) Place 25 mL of the cation exchange resin in a 100 mL beaker, cover the resin with water, and allow
to soak for 16 h.

b) Insert a glass-wool plug in the glass column, approximately 10 mm above the stopcock. Decant the
water in which the resin was soaked, and wash the resin into the column by means of a jet of water
from a wash bottle. Ensure that the height of the column of resin, measured from the top of the glass-
wool plug, is approximately 200 mm. Drain excess water from the column until the water level is
approximately 10 mm above the top of the resin.

c) Put 100 mL of the 1:1 dilute hydrochloric acid into the reservoir and allow it to run through the column
at a rate of approximately 15 mL/min. If the acid emerging from the stopcock is not colourless, wash
with further consecutive 50 mL aliquots of the 1:1 dilute hydrochloric acid until the eluate is
colourless.

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SANS 5850-2:2008
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d) Allow the acid to drain from the column until it just covers the resin. Put 200 mL of water into the
reservoir and allow it to drain through the resin until the water level is approximately 10 mm above the
top of the resin.

e) After every two tests, re-activate the resin in the column by following the procedures in (c) and (d)
above.

5 Preparation of test specimen

5.1 From the test sample (see SANS 197), take a mass estimated to contain approximately 400 g of
material that passed the 425 ȝm sieve, dry it to constant mass at a temperature not exceeding 80 °C,
allow it to cool, and sieve it on the 4 750 ȝm and 1 700 ȝm sieves. Break up any aggregation of smaller
particles (taking care not to reduce the size of individual grains) by placing the portion that passed the
4 750 ȝm sieve and was retained on the 1 700 ȝm sieve in the mortar, and rubbing it with the rubber-
covered pestle.

5.2 Once more sieve this portion on the 1 700 ȝm sieve, add the material that passed the sieve to the
quantity that passed the same sieve in 5.1, and sieve the mixture on the 425 ȝm sieve. Place the portion
retained on the 425 ȝm sieve in the mortar, rub as in 5.1, and again sieve thoroughly on the 425 ȝm
sieve. Combine the fines (i.e. all the material that has passed the 425 ȝm sieve) and mix well.

5.3 Obtain a portion of mass approximately 100 g of the fines prepared as in 5.2, by means of a sample
splitter, or by coning and quartering. So grind this portion that the entire mass passes a 125 ȝm sieve.
Dry the material to constant mass at a temperature not exceeding 80 °C, and cool to room temperature
in a desiccator.

6 Procedure
6.1 Weigh out, to the nearest 0,001 g, approximately 10 g of the test specimen (mass a) into a 400 mL
beaker and add 200 mL of the 1:9 dilute hydrochloric acid. Place a magnetic stirring bar in the beaker,
cover with a cover glass and place the beaker, with contents, on the stirring device. So adjust the speed
of the stirrer that all the material remains in suspension, and so adjust the heat that the contents of the
beaker are just maintained at boiling point.

6.2 After boiling (with stirring) for 15 min, place the beaker on a warm water bath and, by allowing the
beaker to stand undisturbed for 30 min, allow the undissolved material to settle to the bottom of the
beaker.

6.3 Place a dry 600 mL beaker in the Witt filter apparatus and place a double layer of glass fibre filter
paper of fine texture1) on the Buchner funnel, and wet the paper with a few drops of the aqueous extract
(see 6.1).

6.4 Using low vacuum and ensuring that none of the sediment in the beaker is disturbed, filter
approximately 150 mL of the supernatant extract, stir the contents of the beaker until all the sediment is
in suspension and rapidly transfer it onto the filter paper. Rinse the beaker three times with successive
small quantities of the 1: 9 warm dilute hydrochloric acid, adding the washings to the Buchner funnel
after each rinse and ensuring that the filter paper is at no stage allowed to become dry.

6.5 Add approximately 0,5 g of dry filter paper pulp to the filtrate, stir until all the filter paper has
disintegrated and again filter through the same glass fibre filter paper. Wash the beaker and filter paper
thoroughly with the 1: 99 dilute hydrochloric acid. Boil the filtrate until its volume has been reduced to
approximately 50 mL and transfer it quantitatively to the evaporation dish, using the 1: 99 dilute

1)
Whatman GF/C or equivalent.

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Edition 1.3

hydrochloric acid to wash out the beaker. Evaporate the contents of the evaporation dish on a water
bath until dry, then transfer the dish to an oven maintained at a temperature of 105 °C to 110 °C and
allow to dry for 30 min.

6.6 Add 1 mL of concentrated hydrochloric acid to the contents of the evaporation dish, allow the dish
to stand for 5 min, and then add 50 mL of warm water. Place the dish on a water bath, add
approximately 0,2 g of dry filter paper pulp, stir until a homogeneous suspension is obtained, and heat
for 15 min. Filter the contents of the dish through a fine-textured filter paper2) into a 250 mL beaker.
Wash the dish and filter paper with small volumes of warm water until the filtrate has a volume of
100 mL and then allow it to cool to room temperature.

6.7 Transfer the filtrate quantitatively (with water) to the reservoir of the cation exchange column and
allow it to drain through the column of resin at a rate of about 15 mL/min into a 500 mL beaker. Finally
wash the column with four consecutive 50 mL aliquots of water, adding the washings to the beaker that
contains the acid eluate.

6.8 Add 1 mL of concentrated hydrochloric acid to the contents of the beaker, heat to boiling point, and
then add (one drop at a time and stirring the contents of the beaker continuously) 10 mL of barium
chloride solution. Boil for 2 min, place in a water bath for 2 h and then allow to cool for 16 h.

6.9 Filter the contents of the beaker through a fine-textured filter paper3), transferring the precipitate
quantitatively to the filter paper by means of a jet of warm water from a wash bottle. Then wash the filter
paper and the precipitate with consecutive small volumes of warm water until the filtrate is free from
chlorides.

NOTE The presence of chlorides can be detected by putting a drop of silver nitrate solution (50 g/L) in
approximately 10 mL of the filtrate. If chlorides are present, a milky suspension will be formed.

6.10 Place the filter paper and the precipitate in the ignited and tared platinum crucible, char the paper
slowly (without flaming), then increase the temperature and maintain it at just under 600 °C until all
carbon has burnt off.

6.11 Ignite the crucible at a temperature of 800 °C to 900 °C for 30 min, cool to room temperature in a
desiccator, and determine, to the nearest 0,001 g, the mass of the residue (barium sulfate, mass b).

6.12 Carry out a blank determination by following the procedures described in 6.1 to 6.11, using the
same quantities of reagents but omitting the 10 g of test specimen (mass c).

7 Expression and reporting of results

7.1 Calculate, to the nearest 0,1 %, the acid-soluble sulfates content (expressed as SO3), S,
percentage by mass, of the fines (material that passed the 425 ȝm sieve) as follows:

( b - c ) × 34,3
S=
a

2)
Whatman No. 42 or equivalent.
3)
See footnote (2).

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where

a is the mass of the test specimen taken, in grams;

b is the mass of barium sulfate found, in grams; and

c is the mass of the residue found in the blank determination, in grams.

7.2 Report the mass percentage acid-soluble sulfates (expressed as SO3) to the nearest 0,1 %.

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