METHOD A22T

TENTATIVE METHOD FOR THE QUANTITATIVE DETERMINATION OF

ACID-SOLUBLE SULPHATES IN SOILS AND AGGREGATES BY MEANS OF
A NEPHELOMETER

1 SCOPE capable of pulverizing the sample

This method describes a
procedure whereby all the acid- 2.6
soluble salts in a soil or
aggregate are dissolved in
hydrochloric acid. Barium 2.7
chloride is added to the solution
and the turbidity of the
precipitate is measured by means 2.8
of a nephelometer. From a
standard curve, which is obtained
by plotting nephelometer
readings against known
concentrations of sulphate ions 2.9
producing the turbidity, the
percentage of acid-soluble 2.10
sulphates in soils or aggregates is
determined. 2.11
to pass the 0,425 mm sieve.
A balance to weigh up to 100 g,
accurate to 0,001 g.
A balance to weigh up to 10 kg,
accurate to 1 g.
A drying oven, thermostatically
controlled and capable of
maintaining a temperature of 80
ºC ± 5 ºC.
A mechanical flask shaker.
A vacuum pump.
Buchner funnels.

2 APPARATUS 2.12 250 and 1 000 ml volumetric

flasks.
2.1 A photoelectric nephelometer
consisting of a head and a 2.13 Vacuum filter flasks.
galvanometer such as the
Unigalvo Type 200, EEL, 2.14 Filter paper (Whatman No. 40 0r
complete with special test tubes. 41 or similar).

2.2 A riffler with 25,0 mm openings. 2.15 Filter aid (such as Celite).

2.3 The following sieves 2.16 1, 2, 3, 5, 10, 20, 25, 50 and 100
(recommended diameter 200 ml pipettes (at least Class B,
mm): 19,0 mm, 13,2mm, 2,36 accurate at 20 ºC).
mm and 0,425 mm.
2.17 A measuring spoon.
2.4 A suitable laboratory crusher.
Reagents
2.5 A suitable mechanical pulverisr,
Standard Test Methods – Method A22T 1
TMH1 - 1986
2.18 Hydrochloric acid, concentrated than 20 %
(CP) retained on
the 19,0 mm
2.19 Glycerol (CP). sieve
2,5 kg
2.20 Ethyl alcohol absolute (CP). Medium
graded: Less
2.21 Barium chloride (AR). than 20 % 250 g
retained on
2.22 Potassium sulphate (AR) the 19,0 mm
sieve and not
2.23 Activated charcoal powder (CP). more than 80
% passing
3 METHOD the 2,36 mm
sieve
3.1 Preparation of test sample
Finely
If the sample contains + 13,2 mm graded: More
aggregate, crush it to pass the than 80 %
13,2 mm sieve. Mix thoroughly passing the
and quarter out by means of a 2,36 mm
riffler a representative sample of sieve
approximate mass according to
the table belo. keep the loss of Carefully remove all organic
fines and dust to an absolute matter from the laboratory
minimum. sample. Pulverize the sample to
pass a 0,425 mm sieve and mix it
Type of Approximate thoroughly. Dry the material to
material mass of constant mass at a temperature of
laboratory not more than 80 ºC. Weigh out
sample approximately 1,5 or 10 g of the
Coarsely pulverized sample accurately to
graded: More 6 kg the nearest 0,001 g and transfer it
to a 1 000 ml volumetric flask.

3.2 Dissolving test sample distilled water, then allow it to

Add approximately 5 ml of
concentrated hydrochloric acid to
the sample in the 1 000 ml
volumetric flask. Add 200 ml of
distilled water. Shake the
suspension for two hours ± 1
minute using the flask shaker.
Fill the flask up to the mark with
stand for at least two hours,
preferably overnight.
3.3 Filtering of test sample
Filter the suspension into a filter
flask using a medium vacuum. In
order to obtain a clear filtrate use
a Whatman No. 40 or 41 or

Standard Test Methods – Method A22T 2

TMH1 - 1986
 similar filter paper, placing a
layer of filter aid and a further
layer of wetted charcoal on top
of it.
2.1 Testing of filtrate
By means of a pipette, transfer
50 ml of the filtrate to a 250 ml
volumetric flask. Add 150 ml of
distilled water. Add 5 ml of
glycerol-ethyl alcohol (1:4) and
approximately 2 g of barium
chloride crystals have been
dissolved. Fill the flask up to the
mark with distilled water. Shake
again. Transfer a sample into the
nephelometer test tube and take
the readings on the nephelometer
according to the manufacturer’s
instructions. The reading must be
taken five minutes after the
barium chloride has been added.
No readings should be taken after
ten miuntes.
The corresponding number of
milligram of SO4²- may be be
read off from a standard graph
(see 5.1).
Readings below 20 and above 80
on the nephelometer scale are
inaccurate; they can be avoided
by taking respectively less or
more soil for the preparation of
the soil suspension, or by using
respectively less or more than 50
ml of the filtrate for a reading.
4 CALCULATIONS
The sulphate content is expressed
as a percentage of the mass of the
dry soil taken, and is calculated
to the nearest 0,01 as follows:
Standard Test Methods – Method A22T
TMH1 - 1986
A = B  D  100
C E 1
where
A = mg SO4², expressed as a
percentage of the dry soil taken
B = mass of SO4² (mg) as read
off from the standard graph (see
5.1)
C = mass of dry soil taken (mg)
D = volume of soil suspension
(see 3.2)
E = volume of filtrate
transferred to a 250 ml
volumetric flask (see 3.4)
To correct the results as a
percentage of CaSO4 or
CaSO4.2H2O of the dry soil,
multiply A by 1,4172 or 1,7924
respectively (see 5.2).
5 NOTES
5.1 Preparation of the standard
calibration graph (a new
calibration graph should be
prepared if the potassium
sulphate solution is more than
five months old or barium
chloride from a different
production lot is being used):
Dry the potassium sulphate at
180 ºC for at least two hours and
allow it to cool off in a
desiccator.
Weigh off accurately 1,8141 g of
3
 the dried potassium sulphate and
wash it into a 1 000 ml
volumetric flask. Fill the flsk up
to the mark with distilled water.
The mass of potassium sulphate
used is calculated as follows:
Molecular mass of K2SO4 =
174,268
Ionic mass of SO4²-
96,064
= 1,8141 g of K2SO4
The concentration of this
solution, called the standard
stock solution, is 1 000 mg
SO4²-/l. Using a pipette, transfer
from this solution 100 ml into
another 1 000 ml volumetric
flask and fill it up to the mark
with distilled water. 1 ml of this
solution (called the standard
working solution) contains 0,2
mg of SO4²-, 5 ml contains 1,0
mg of SO4²-, and so on.
Using a pipette, transfer at least
12 increasing volumes of the
standard working solution into
250 ml volumetric flasks as
explained in the above examples-
covering the range of SO4²-
solutions to be tested.
Draw a graph on ordinary graph
paper of nepelometer readings
against SO4² concentrations in
mg/l (see Fig. A22T/1).
Standard Test Methods – Method A22T
TMH1 - 1986
Add to each of the samples 5 ml
of a 5 percent by volume
hydrochloric acid solution, 5 ml
of a 1:4 mixture of glycerol and
ethyl alcohol, and approximately
2 g of barium chloride. Shake the
flasks, using a flask shaker, until
the barium chloride has been
dissolved. Fill the flsks up to the
mark with distilled water and
shake them again. Transfer a
sample of each concentration into
a nephelometer test tube and take
the nephelometer readings
according to the manufacturer’s
instructions. The readings must
be taken within ten minutes of
adding the barium chloride.
5.2.1 The factors for calculating the
percentage of CaSO4 or
CaSO4.2H2O are calculated as
follows:
For CaSO4:
Mol. mass of CaSO4 = 136,142
= 1,4172
Ionic mass of SO4 96,064
For CaSO4.2H20:
Mol. mass of CaSO4.2H2O =
172,176 = 1,7924
Ionic mass of SO4
96,064
4
Standard Test Methods – Method A22T 5
TMH1 - 1986