Experiment #1:

Determination of Sulfur in a
Soluble Sulfate Salt
Materials:
 4 pieces of porcelain crucible and cover (must be
constant weighed at 1000 to 1200 °C)
 Dessicator (wide-mouth glass jar with air-tight cap)

Reagents:
 150 mL - 5% BaCl2 solution (precipitatant)
 100 mL - 0.1 M AgNO3
 100 mL concentrated HCl
 Constant weighing the crucibles:
(using the Bunsen burner)

 Clean the porcelain crucible and cover.

 Label the bottom the crucible with a pencil. Write your
initials and the crucible number.
 Place the crucible and its cover in an upright position
on the clay triangle.
 Ignite the crucible using a strong blue flame from a
Bunsen burner. The heating temperature would be
1,100 to 1,200 oC.
 Heat the crucible for 10 minutes.
Heating the crucible
 Cool down the crucible for at least two minutes. Transfer
the crucible and cover inside the dessicator and let it cool
down for at least 20 minutes.
 Weigh the crucible (do not include the cover) in an
analytical balance.
 Record the weight and repeat the procedure until the
difference in weight is at least ± 0.0005 grams for three
weight trials.
 Take the average of the three trials as the weight of the
crucible.
Cool the crucible inside the dessicator for
at least 20 minutes
Effect of temperature on
weighing data. Absolute error in
weight as a function of time
after the object was removed
from a 110 °C drying oven.
A: porcelain filtering crucible.
B: weighing bottle containing
about 7.5 grams of KCl.
 Precipitation of Barium sulfate:

 Ground the sample using a mortar and pestle. Be

careful not to spill the sample.
 Store the ground sample in a dessicator.
 Weigh out accurately about 0.5 to 0.8 g of the dried
sample. (Four trials must be performed in the
experiment)
 Dissolve each sample in about 200 ml of distilled water
and 1 ml of concentrated HCl.
 Heat both the sample solution and the solution of
barium chloride nearly to boiling.
Digestion of the precipitate
 Pour the 25 ml hot barium chloride solution quickly but
carefully into the hot sample solution and stir vigorously.
 Allow the precipitate to settle and test the supernatant
liquid for completeness of precipitation by adding a few
more drops of the barium chloride solution.
 After precipitation is complete, cover the beaker with a
watch glass and allow the precipitate to digest for 1 to 2
hours keeping the solution hot (80 to 90 °C) over a low
heat setting.
 Cool down the solution, cover the beaker with a shrink-
wrap and keep it in the locker for next meeting. (This will
further enhance the crystallization of the precipitate.)
 Filtering and washing the precipitate:

 Collect the precipitate on an ashless filter paper.

 Wash the precipitate with hot water three times and
test the last few drops of the filtrate for the presence
of chlorides. To do this place 1 mL of the filtrate in a
test tube and add 1 drop of 0.1 M AgNO3, a cloudy
solution would indicate that chlorides are still present
with the precipitate, repeat this procedure again.
Folding the filter paper
Folding the filter paper
The filtration set-up
Transferring and washing precipitates
Placing the precipitate in the crucible
Placing the precipitate in the crucible
Placing the precipitate in the crucible
 Igniting the precipitate (using the muffle
furnace)

 Your instructor will demonstrate

how to turn-on the furnace and
how to set the temperature
program for the ignition of the
precipitate.
 Place crucible containing the
precipitate inside the furnace. It
should be slightly opened as to
allow air to reach inside the
crucible. Ney 3-550A Venturi Air
Furnace
Furnace temperature program

Stage Temperature Hold time (hour)

Drying 110 °C 0:30
Charring 550 °C 1:00
Ignition 800 °C 1:00
 Constant weighing of the crucible

 On next meeting, collect your crucible from the

furnace, be careful not to spill the residue inside.
 The precipitate should be white and ash-like material.
 Constant weigh the crucible by heating it under the
blue flame of the bunsen burner for 10 minutes.
 Igniting the precipitate (using the bunsen
burner)
 Place the crucible on the clay triangle in an upright
position. Place its cover with a slight opening to allow the
exit of gases.
 Dry the precipitate slowly over a low flame for about 15
minutes. [Drying]
 Reposition the cover to completely close the crucible.
Increase the heat a little bit and char the paper carefully. A
stream of white smoke will slowly emit out of the crucible.
[Charring]
 Caution: If the smoke becomes black decrease the heating,
otherwise the paper will catch fire which may reduce BaSO4 to BaS.
 Igniting the precipitate (using the bunsen
burner)
 Gradually increase the heat until no more
white smoke comes out of the crucible.
 After charring, the crucible should be
uncovered and in a slanted position for
free access of air to prevent reduction of
barium sulfate to barium sulfide. Heating
should be increased to its maximum.
[Ignition]
 Ignition should be continued until no
more black particles are found in the
crucible.
 Constant weighing of the crucible

 The precipitate should be white and ash-like material.

 Constant weigh the crucible by heating it under the
blue flame of the bunsen burner for 10 minutes.
 Calculation:

 Calculate for % sulfur in the sample:

 A = average weight (of three trials) of crucible and

precipitate (in grams)
 B = average weight (of three trials) of crucible (in grams)
 Calculate the average % sulfur for four trials.
 Calculate the standard deviation and RSD (relative
standard deviation).
 Calculate the confidence interval at 95% Confidence
Level.