Analytical Chemistry 2 2012

Experiment 2

Determination of Sulfate (as %SO3) in a Soluble Sample

The sulfate content in a soluble sample can be found by precipitation of the slightly
soluble BaSO4 according to the reaction: .

This analysis illustrates procedures used for precipitating and washing an almost
insoluble precipitate of very small crystals. The precipitate adsorbs many substances
strongly but is not peptized by being washed with water. The method described in
this experiment can also be used in the analysis of other sulfur-containing
compounds by first converting S to SO42-.

Procedure

A. Constant Weighing of the Crucibles

a. Bring two porcelain crucibles to constant weight by heating to redness for
15 min over a burner (not including the cover; follow instructor’s demo of
the setup)
b. Cool the crucibles briefly on clean Al foil-covered wire gauze at room
temperature for ~ 5 min and into the desiccator for 25 minutes.
c. Weigh each crucible accurately on an analytical balance. Repeat
procedure a and b until successive weighings agree within ± 0.3 mg. Be
sure that all oxidizable substances on the entire surface of each crucible
have been burned off.
B. %SO3 Determination
a. Dry the soluble sulfate sample at 100⁰C for 1-2 hours, and cool in
desiccators. Weigh out 0.5 – 0.7 g (± 0.1 mg) duplicate samples. Transfer
to 800-mL beakers. Dissolve each in 200 mL of dist. H2O + 4 mL of 6M
HCl.
b. Precipitant is prepared by dissolving 1.3 g BaCl2 · H2O in 100 mL water.
Filter if solution is not perfectly clear.
c. Heat the BaCl2 solution nearly to boiling, and then add the entire amount
to the HOT sulfate sample solution while stirring vigorously. Wash stirring
rod with distilled water and include washings in your final mixture.

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 Analytical Chemistry 2 2012
d. Digest by letting stand for 1-2 hours. Overnight standing is acceptable.
Filter through an ashless filter paper of fine porosity (Whatman no. 42).
Slowly pour the supernatant liquid through the filter paper,
e. Transfer all precipitate to the filter paper avoiding any loses during the
filtration procedure. One may use a rubber policeman to scrape remaining
precipitate in the beaker. Wash the precipitate in the beaker 3X with hot
water before transferring to the filter paper. Test the washings with 0.1 M
AgNO3 solution. Cloudiness indicates presence of chloride ions; therefore
there is a need to wash more the precipitate. Carefully lift the paper out of
the funnel, fold it as demonstrated by your instructor and transfer it onto
the constant weighed crucible.
f. Dry the crucible cautiously with a small flame, as instructed by your
instructor. The flame should be directed at the top of the container, and
the lid should be off. Avoid spattering. After drying, CHAR the filter paper
by increasing the flame temperature. The crucible should have free
access to air. The lid should be kept handy to smother the filter paper in
case it catches fire. Any soot left in the crucible and the lid should be
removed by directing these to the flame. Use tongs to manipulate crucible.
Finally, ignite the product for 15 minutes with the full heat of the burner.
g. Cool the crucible, briefly in air and then in a desiccator for 30 min. weigh
the crucible, re-ignite, and bring to constant weight (±0.3 mg) with
repeated heatings.
h. Calculate the %SO3 in the sample, the average, sd, and % rsd.

Porcelain Crucible

Clay Triangle

Figure 1: How to position the crucible

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 Analytical Chemistry 2 2012

Guide Questions

[1] What type of precipitate is BaSO4?

[2] Why is a filter paper preferred over a sintered glass filter?
[3] What made an ashless filter paper ashless?
[4] Why is a porcelain crucible used in this procedure?
[5] Why do we need to precipitate from a hot solution?
[6] Why is the precipitating agent added all at once?
[7] What is the purpose of adding 6M HCl in the sample solution?
[8] Why do we need to test the washings with AgNO3?
[9] What is ignition?
[10] What is the product after the precipitate was ignited?
[11] What are the advantages of performing ignition?
[12] Cite the sources of errors for this experiment and how to circumvent these
problems.

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 Analytical Chemistry 2 2012

Sample Data Sheet (You may devise your own on your logbook. Make sure that it
presents your data in a CLEAN, LEGIBLE, COMPLETE, and TRUTHFUL manner).

A. Constant Weighing of Crucibles

Crucible A Crucible B
Mass of Trial 1
Mass of Trial 2
Mass of Trial 3
Mass of Trial 4
Mass of Trial 5

Mass of Trial 6

B. Analysis of Sample

Trial 1 Trial 2

Wt. of Sample (g)

Wt. after ignition
(g)
%SO3

Mean %SO3

SD

%RSD

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