Effective: September 1, 2000

Revised: January 26, 2011

Florida Method of Test

for
Sulfate in Soil and Water
Designation: FM 5-553

1. SCOPE

1.1 This method covers the determination of sulfate in soil and water using
either a sulfate reagent system for field analysis or standard laboratory
method as found in the Standard Methods for the Examination of Water
and Wastewater, Section 4500- SO42-.

2. APPARATUS

2.1 Sulfate reagent system - Sulfate, Pocket Colorimeter II Test Kit, 2 to 70

mg/L as sold by Hach Company, or equivalent, may be used for sulfate
determinations. Alternatively, the apparatus referred to in Section 4500-
SO42- of the Standard Methods for the Examination of Water and
Wastewater may be used for laboratory tests.

3. REAGENTS

3.1 Barium chloride (BaCl2) and distilled water are required for the above field
test kit. Reagents used in sulfate determinations using a laboratory
method depend on the method chosen.

4. SAMPLES

4.1 Soil Sampling: Every effort should be made to obtain a soil sample which
is representative of the bulk material. Use clean tools for gathering
samples. Excessive moisture should be avoided by sampling from an
area, which has been allowed to gravity drain for a short time. If the soil
sample has excess free moisture, place approximately 2.2 pounds (1 kg)
of the soil on top of a suitable sieve and cover with plastic. Allow the
sample to drain for one hour. This step may be performed in the lab prior
to testing.

If the soil sample is obtained from a heap, which has been sitting for a
long time, take the sample from a depth below the weathered surface
where the moisture content appears to have stabilized. Avoid taking the

FM 5-553 1
 Effective: September 1, 2000
Revised: January 26, 2011

sample from near a weathered soil surface. If sampling from ground level,
remove top 12 to eliminate vegetation and debris before sampling. The
soil sample may be taken from underneath standing water, but excess
water should not be included with the sample. Soil samples should be
placed in plastic or plastic-lined bags. Squeeze the bag down snugly
around the sample and seal tightly to minimize contact with air.

4.2 Water Sampling: Water samples should be obtained from the main
channel of rivers and streams. Sampling from other bodies of water, such
as, lakes or ponds should be obtained from areas conducive to the
capture of representative samples. Care should be observed not to
sample from stagnant or pooled water, unless a structure will be placed in
such an area. Sample the water just below the surface to alleviate
introduction of floating debris, i.e. leaves, sticks, foam or trash. Fill the
sample container to the top to eliminate introducing air into the sample
and tightly seal the lid. The sample container shall be at least 1 quart (1
L) in size, clean and be either glass or plastic with an air tight lid. When
possible, submerge the sample container below the surface of the water to
completely fill and secure lid underwater.

4.3 Transporting the samples: Maintain test samples in a cool dark area after
sampling and during transport to the test facility.

4.4 Storing Samples: If samples need to be stored, this period shall not
exceed seven (7) days and must be maintained at or below 39 o F (4o C).
Care should be taken to prevent freezing of the samples.

5. SAMPLE PREPARATION

5.1 Preparation of Soil:

A. Loose Granular Soils: Dry sample to constant mass by spreading

in a thin layer on paper or by placing in an oven at 110 C (230 F)
for approximately four hours or until constant mass is achieved.
Sieve through a No. 10 mesh sieve. Split the sample per ASTM C
702-98 to obtain approximately 400 grams.

B. Muck and Soils with Clay: Dry sample to constant mass by

spreading in a thin layer on paper or by placing in an oven at 110 C
(230 F) for approximately four hours or until constant mass is
achieved. Using a rawhide mallet or other suitable device pulverize
the sample and sieve through a No. 10 mesh sieve. Split the
sample per ASTM C 702-98 to obtain approximately 400 grams.

FM 5-553 2
 Effective: September 1, 2000
Revised: January 26, 2011

5.2 Place 100 grams of dried soil in a 500 ml Erlenmeyer flask. Add 300 ml
distilled/de-ionized water, stopper, and shake vigorously for 20 seconds.
Let stand for one hour and repeat agitation. Let stand for a minimum of 12
hours.

Filter the water layer through a Whatman No. 41 filter paper. When nearly
all the water has been filtered, swirl the flask and empty the soil into the
filter paper and continue to filter until the liquid stops dripping.

Some soil solutions will remain cloudy due to the suspension of fine
particles. This will interfere with the sulfate determination. If the filtrate is
to be used for additional tests, divide in half using a second clean
container. Add a few drops (three to five) of hydrochloric acid (HCl) to the
container used for the sulfate determination, and let stand for
approximately one hour. The remaining half of the sample may be used
for other tests, not tolerant to the addition of acid.

5.3 Preparation of Water: Allow test sample to reach room temperature.

6. PROCEDURE

6.1 Test for sulfates by referring to the method detailed in the manufacturers
operation manual for the sulfate test kit or in the Standard Methods for the
Examination of Water and Wastewater for laboratory tests.

Results for soil samples must be multiplied by 3 to account for the mixing
ratio used (100 grams of soil to 300 ml water).

Dilution of the test sample will be necessary if the sulfate concentration is

greater than the maximum limit of the testing apparatus. In most cases, a
dilution of 100 times (1ml:99ml) using distilled/de-ionized water will be
sufficient. Remember to correct for dilution by multiplying the result by the
dilution factor, in this case 100.

Notes:
1. Rinse the measuring tube and/or mixing bottle with un-reacted sample before testing.
2. Rinse the glassware with distilled/de-ionized water after each test to limit the amount of
chemical residue accumulation.

FM 5-553 3