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Report on the Gravimetric Analysis of Sulfate in Trisethylenediaminecobalt(III) Chloride

Sulfate Trihydrate.

March 8, 2009
Jordan Hughey
Union University
This report details the procedure and analyzes the results of the Gravimetric
Analysis of Sulfate lab. The entire procedure for this gravimetric analysis is given
including all required figures. Results are also given and analyzed. The experimental
results gave a higher percentage of sulfate in the cobalt complex than the absolute value
(calculated from formula weights). The lab presents relatively precise data, but there must
be changes in the method to improve accuracy.

This is experiment is to determine the relative amount of sulfate in our final
precipitate from lab 1, Synthesis of Trisethylenediaminecobalt(III) Chloride Sulfate
Trihydrate, as opposed to the absolute amount simply calculated by formula weights. The
gravimetric analysis method has been used for a very long time because of its accuracy1
and ease of procedure (the only major instrumentation is an analytical balance). However,
in today’s fast paced industry gravimetric analysis isn’t often used because of its time
consumption. We use gravimetric analysis because of its ease of completion.

In this gravimetric analysis the main chemicals we will use are resin made by
Dowex, barium chloride dihydrate from Fisher Science, trisethylenediaminecobalt(III)
chloride sulfate trihydrate (Co(en)3ClSO4*3H2O)that was prepared in a previous lab, and
silver nitrate prepared by Union University. The procedure is fairly simple to follow, but
very time consuming due to the many heatings.
To begin, dry three crucible for a half hour, cool for a half hour, and weigh. Repeat this
until consecutive weights agree within 0.3mg (Table 1). Next weigh out .5-.7g of
Co(en)3ClSO4*3H2O (Table 2). Dissolve this in a minimum amount of water and keep
track of the amount of water used for dissolution. You must also setup a cation exchange
using a buret, a small amount of glass wool, and about 10mL of resin. Take the glass
wool, form it into a plug and the place it into the buret. Then make a slurry with
deionized (DI) water and pour into the buret. Rinse down any resin on the sides of the
buret with DI water. Be sure the water has at least drained down to the level of the resin.
Now that the cation exchange is setup, add the Co(en)3ClSO4*3H2O solution to the buret
using a pipette. Place a flask beneath the buret and open the stopcock. This packs the
cobalt solution onto the resin and allows the sulfate ion and DI water to wash through to
the flask below. Rinse through with a total of 100mL of DI water (include the amount
used to make the Co(en)3ClSO4*3H2O solution in the 100mL). The drained liquid
contains sulfate ion.
For the next step, find the amount of barium chloride dihydrate (with 10% excess) needed
to precipitate a maximal amount of sulfate ion (Figure 1). Take this amount and dissolve
it in 200mL of water. Take this solution and the sulfate ion solution and heat. While hot,
pour the barium chloride into the sulfate ion and mix for 2-3 minutes. Allow to stand for
15 minutes. Check for completion by adding a few drops of barium chloride solution to
the barium/sulfate solution. If the solution gets cloudy not all sulfate has precipitated and
more barium chloride should be added until precipitation is complete.
Next, filter the solution with gravity filtration. A white precipitate should be caught in the
filter paper. Rinse the precipitate with DI water. Test for chloride ions by adding a few
drops of silver nitrate directly to the washings. If the washings turn cloudy, continue to
rinse till all chloride ion has washed through.
Finally, the filter and precipitate must be ashed to purify. To do this, place the filter paper
with precipitate into one of the previously dried crucibles. Burn/heat the crucible and
contents over a Bunsen burner setup and char off all filter paper. After 30 minutes of
heating, remove the flame for a moment, cool for 30 minutes in the desiccator, and
weigh. Continue this heat, cool, and weigh process until the crucible and contents have
achieved a constant weight (±3mg)(Table 3). Remember crucibles are hygroscopic, so
they should kept in the desiccator for a maximal amount of time and weighing should be
done rapidly.

This table shows the weights of the crucibles after the first and second firings. Only two
firings were done because after the first two firings the weights were within ±0.3mg.
Table 1:
Weights of Crucibles
Crucible: Initial Weight (g) Final Weight (g)
A 10.1325 10.1325
B 11.9689 11.9690
C 11.2265 11.2266

This table shows the weights of the samples used in the experimental procedure.
Table 2:
Sample Weights
Sample A (g) Sample B (g) Sample C (g)
.5000 .5203 .5965

This was the process used to find the amount barium chloride needed to precipitate all
sulfate (with 10% excess):
Figure 1:
10% Excess BaCl2
(.6g Co(en)3ClSO4*3H2O)/(424.1g/mol) = (xg BaCl2*2H2O)/(244.268g/mol)
(.00141g/mol)(244.268g/mol) = (xg BaCl2*2H2O)
= .346g BaCl22H2O
(.346g BaCl22H2O)(1.1) = .380g BaCl22H2O

This table shows the final two weights of the all three crucible with the final filtered
Table 3:
Weights of Crucible with Precipitate After Ashing and Heatings (g)
Sample and Crucible A Sample and Crucible B Sample and Crucible C
Weight 1 10.4264 12.2706 11.5696
Weight 2 10.4261 12.2708 11.5699

With calculations we found that the average mass percent of Sulfate in the complex to be
23.90(±.2587). This value however does not agree with the accepted value for mass
percent sulfate in the complex at the 95% confidence level (figure 2).

Figure 2:
T-test for Equivalence
Calculated Percent: 23.90% Accepted Percent: 22.65%
±t=(x(avg)-μ)(Sqrt(N)/s) Table value for ±t at the 95% confidence
±t=(23.90-22.65)(Sqrt(3)/.2587) level:
±t=8.369 ±t=4.303

Although the experiment was carefully carried out with great attention to detail,
the results obtained are not in agreement with the accepted results. The t-test showed that
the percentages found experimentally are not equivalent to the accepted values. No trials
were found to be significant outliers; therefore, none could be eliminated. We can be
fairly certain that all of our lab equipment is well calibrated. Therefore the only other
determinate error possible is an error in method. It is important to notice that the
experimental percentage is higher than the accepted. It seems most likely that most of the
error came when washing the filtered precipitate. Any chloride ions that precipitated out
and were not washed off would add to the mass. Thereby giving a higher percentage. The
only way to improve this method would be to more carefully wash the precipitate, adding
even more time to the experiment.
Works Cited:

1. Henrickson, C. The Gravimetric Determination of Sulfate.

[www.wku.edu/~charles.henrickson/sulfate.pdf.] (3/8/2009)

2. Johnston, R. Gravimetric Analysis of Sulfate in Trisethylenediaminecobalt(III)

Chloride Sulfate Trihydrate. Union University, Jackson, 2009, pg. 25-26.