DETERMINING SO 42- , Cl - CONTENT AND pH IN SOILS:

COLORIMETRIC METHOD

DETERMINING SO42METHOD

Cl- CONTENT AND pH IN SOILS COLORIMETRIC

1.0 SCOPE
This method determines the soluble sulfate (SO42-) and chloride (Cl-) content and pH of soil
by using turbidimetric techniques.
The values given in parentheses (if provided) are not standard and may not be exact
mathematical conversions. Use each system of units separately. Combining values from the
two systems may result in nonconformance with the standard.
2.0 DEFINITIONS
Turbidimetric Technique - The process of measuring the cloudiness of a liquid and
translating it into concentration. A reagent (sulfate, chloride and pH test tablet) is combined
with a sample, which causes cloudiness or turbidity in the sample.
Colorimetry Theory

The theory behind colorimetry hinges on Beers law:

A = abc = log (Io/I1)
Where,
A = absorbance
a = absorptivity of the sample
b = optical path length
c = concentration
Io = intensity of light entering solution
I1 = intensity of light emerging from solution
There is a linear relationship between absorbance and concentration of a solution if
the optical path length and wavelength of radiation remain constant. By measuring the
ratio I1/Io absorbance can be measured, therefore concentration can be calculated.
Beers law usually holds at low concentrations, but deviations are common at
concentrations above 200 ppm.
PPM - Parts per million; measure of concentration.
Filtrate - (Soil/water) material that has passed through a filter.
3.0 APPARATUS

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DETERMINING SO 42- , Cl - CONTENT AND pH IN SOILS:

COLORIMETRIC METHOD

a) Colorimeter and the following accessories:

b)

10 mL glass sample vial

Sulfate test tablets

Chloride test tablets

pH test tablets

White plastic rod.

9 V battery.

c) Auger sampler.
d) Core sampler.
e) Balance, minimum capacity of 3500 g.
f) Mortar and pestle.
g) Crusher.
h) Oven, capable of maintaining a temperature of 60 5C (140 9F).
i)

Beakers (glass or plastic), 250 mL.

j)

Beakers (glass or plastic), 600 mL.

k) Graduated cylinder (glass or plastic), 10 mL.

l)

Graduated cylinder (glass or plastic), 100 mL.

m) Wide-mouth round high-density poly ethylene (HDPE) bottles, 8 oz. (250 mL).
n) Wide-mouth round HDPE bottles, 16 oz. (500 mL).
o) Funnel (glass or plastic), 80 mm diameter with short wide stems.
p) Filter paper (fine porosity), 15 cm diameter.
q) 2 mL disposable pipettes.
r) Wash bottle, 16 oz. (500 mL), for distilled or deionized water.
s) Desiccator.
t)

Latex gloves.

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DETERMINING SO 42- , Cl - CONTENT AND pH IN SOILS:

COLORIMETRIC METHOD

u) Tweezers.
v) Pans, brush, and spatula.
w) Sample splitter.
x) Sieves, U.S. Standard No. 4 (4.75 mm) and No. 40 (425

m).

y) Distilled or deionized water.

4.0 PROCEDURES
The following procedure describes preparing soil samples for determining sulfate content in the
field.
4.1 Preparing Sample:
4.1.1

Sample soil within the depth of proposed stabilization with a hand auger at the
sampling frequency required by the guide schedule.

4.1.2

Obtain a 300 g representative sample.

4.1.3

Air-dry the sample to constant weight.

4.1.4

Pulverize the 300 g to pass the No. 40 (425 m) sieve.

4.1.5

Split the sample and obtain 10 g of representative sample. Do replicates for more
accuracy. This means split the material to obtain three samples of 20 g each and
run on each sample the colorimetric test.

4.1.6

Weigh 10 g to the nearest 0.1 g.

4.1.7

Place the 10 g soil sample in an 8 oz. (250 mL) HDPE bottle.

4.1.8

Add 200 mL of distilled or deionized water. This provides an initial dilution ratio of
1:20.

4.1.9

Vigorously shake the bottle of soil/water solution by hand for 1 min. Wait for 12 hr.

4.1.10 After a minimum of 12 hr. has elapsed, place one filter paper along the inside of the
funnel and place the funnel into an 8 oz. (250 mL) beaker to capture the filtrate.
4.1.11 Shake the bottle of soil/water solution again for 1 min. and pour the solution into the
funnel. Allow all the solution to filter and drain into the beaker.
4.2 Measuring Sulfate (SO4--)Content:
4.2.1

Fill a clean vial with 10 ml of the water sample, close tightly with the cap.

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DETERMINING SO 42- , Cl - CONTENT AND pH IN SOILS:

COLORIMETRIC METHOD

4.2.2

Place the vial in the sample chamber

4.2.3

Press ZERO key.

4.2.4

Remove the vial from the sample chamber.

4.2.5

Add one SULFATE T tablet straight from the foil to the water sample and crush the
tablet using a clean stirring rod.

4.2.6

Close the vial tightly with the cap and swirl several times until the tablet is dissolved.

4.2.7

Place the vial in the sample chamber

4.2.8

Press TEST key.

4.2.9

The result is shown in the display in mg/l Sulfate.

4.3 Measuring Chloride (Cl-)Content:

4.3.1

Fill a clean vial with 10 ml of the water sample, close tightly with the cap.

4.3.2

Place the vial in the sample chamber.

4.3.3

Press ZERO key.

4.3.4

Remove the vial from the sample chamber.

4.3.5

Add one CHLORIDE T1 tablet straight from the foil to the water sample, crush the
tablet using a clean stirring rod and dissolve the tablet.

4.3.6

Add one CHLORIDE T2 tablet straight from the foil to the same water sample and
crush the tablet using a clean stirring rod.

4.3.7

Close the vial tightly with the cap and swirl gently several times until the tablet is
dissolved

4.3.8

Place the vial in the sample chamber.

4.3.9

Press TEST key.

4.3.10 Wait for a reaction period of 2 minutes.

4.3.11 After the reaction period is finished the measurement starts automatically.
4.3.12 The result is shown in the display in mg/l Chloride.
4.4 Measuring pH Value:
4.4.1

Fill a clean vial (24 mm ) with 10 ml of the water sample, close tightly with the cap.

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DETERMINING SO 42- , Cl - CONTENT AND pH IN SOILS:

COLORIMETRIC METHOD

4.4.2

Place the vial in the sample chamber.

4.4.3

Press ZERO key.

4.4.4

Remove the vial from the sample chamber.

4.4.5

Add one PHENOL RED METER tablet straight from the foil to the water sample and
crush the tablet using a clean stirring rod.

4.4.6

Close the vial tightly with the cap and swirl several times until the tablet is dissolved.

4.4.7

Place the vial in the sample chamber.

4.4.8

Press TEST key.

4.4.9

The result is shown in the display as pH-value.

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