Determination of Sulfur in a Soluble Sulfate Salt

Objectives:
 To be able to apply the concept of constant weighing and be able to get the constant weight
of the crucible within 3 trials and record its data.
 Digest the precipitate concisely without showing signs of cloudiness
 Determine the amount and percentage of Sulfur in the unknown soluble sulfate salt using
gravimetry analysis
 The experimenters will be able to learn to use the techniques of gravimetry analysis.
 Furthermore, the experimenters would be able to learn the dynamics of precipitation,
nucleation, peptization, filtration, ignition, and calculations in gravimetry,

Outline of procedures:

Constant weighing with the crucible + precipitate

Precipitation:

x SO4 (aq) + HCl (aq) + H2O BaCl2

Heat Separately

Digestion: x SO4 (aq) + HCl (aq) + H2O + BaCl2

Crystallization

Filtration

Wash 3 times
With hot water
BaSO4 discard HCl (aq) + H2O

Igniting the precipitate using Supernatant + AgNO3

The muffle furnace (wash again until no longer cloudy)
 Data and Results

CONSTANT WEIGHING OF CRUCIBLES

1st 2nd 3rd Standard

Crucible attempt attempt attempt Mean Deviation %RSD
1 25.2311 25.2307 25.2318 25.2312 0.000556776 0.002207
2 25.2000 25.2096 25.2100 25.1720 0.065817931 0.261473
3 25.1781 25.1785 25.1786 25.1784 0.000264575 0.001051

CONSTANT WEIGHING OF CRUCIBLES + PRECIPITATE

Crucible + 1st 2nd 3rd Standard

Precipitate attempt attempt attempt Mean Deviation %RSD
1 26.6297 26.6295 26.6292 26.62947 0.000251661 0.000945
2 26.1555 26.1551 26.1553 26.1553 0.0002 0.000765
3 26.3858 26.3854 26.3856 26.3856 0.0002 0.000758

Weight of the sample :

Sulfur in Crucible 1 0.5381

Sulfur in Crucible 2 0.5477
Sulfur in Crucible 3 0.5747

PERCENT SULFUR

(26.6295−25.2312) 𝑥 32.06/233.40
%S = 0.5381
𝑥 100 = 35.6202% Outlier
 (26.1553−25.1720) 𝑥 32.06/233.40
%S = 0.5477
𝑥 100 = 24.6607%

(26.3856−25.1784) 𝑥 32.06/233.40
%S = 𝑥 100 = 28.8536%
0.5747

Since Crucible 1 is an outlier, we must do a separate test for it (Q – test). Resulting to only
two sets of %Sulfur to gets its mean, standard deviation, and % RSD.

Mean 26.7572
Standard Deviation 2.9648
%RSD 11.0805 %

T TEST FOR TWO MEANS

𝑋1 =26.7572

𝑋2 = 24.6285

𝑆1 =2.9648

𝑆2 = 1.0373

(2−1)(8.79003904)+(2−1)(1.07599129)
sp = √
2+2−2

sp = 2.2210

26.7572−24.6285
t= 1 1
2.2210√ +
2 2

t = 0.9584
Q – test:

𝑞𝑢𝑒𝑠𝑡𝑖𝑜𝑛𝑎𝑏𝑙𝑒 𝑣𝑎𝑙𝑢𝑒 − 𝑛𝑒𝑎𝑟𝑒𝑠𝑡 𝑣𝑎𝑙𝑢𝑒

𝑄𝑒𝑥𝑝 =
𝑙𝑎𝑟𝑔𝑒𝑠𝑡 𝑣𝑎𝑙𝑢𝑒 − 𝑠𝑚𝑎𝑙𝑙𝑒𝑠𝑡 𝑣𝑎𝑙𝑢𝑒

0.356202−0.246607
= 0.356202−0.288536

= 1.62

𝑄exp

Discussion
We were tasked to determine the percent of Sulfate in the solution, to do so, we first needed to
use the precipitation process wherein it removes the metal ions from the compounds in a solution. With
this the Barium Chloride will be the precipitation agent because of the Barium ions ability to combine with
sulfur ions thus becoming Barium Sulfate. First, we needed to get the crucible’s constant weight by heating
it and then weighing it on the analytical balance. Next we prepare the sample by adding the H20,
Hydrochloric Acid and then Barium Chloride solution and then heat it. However, several errors were
encountered due to the presence of impure substances in the precipitate. The lingering compound of
Chlorine and the obscure particles, due to its solubility it can simply be filtered through the filter paper,
leaving just Barium Sulfate, which is insoluble with water. Further testing through the expansion of Silver
Nitrate can help in deciding whether most of the Chlorine compound was sifted through. The Barium
Sulfate was then touched off to separate it from the channel paper. In the wake of gauging this precipitate,
the %S in the first example would then be able to be determined, giving 35.62%, 24.66% and 28.85%
fixation, based from the data you can see that we have an outlier which is 35.62%, this is due to the errors
that were made in conducting the experiment. With the outlier, we must do a separate test which is the
Q - test. Having a Q – test result of 1.62, which is greater than the value of 0.941, therefore it is rejected.
All through the test, blunders and vulnerabilities were perhaps experienced, explicitly around the
consistent weighing of the crucible, during the planning of the precipitation and on igniting the
precipitate. There were numerous exercises mastered during the experiment, especially around following
legitimate technique, continually acting naturally mindful while in the laboratory, incorporating the ideas
on gravimetric analysis and precipitation strategies while doing the trials, and continually being aware of
the glassware and equipment while inside the lab.

Conclusion
 In order to successfully determine the percentage of sulfur in a soluble sulfate salt, there should
be a few processes that is needed to be done first. Before the precipitation analysis, the constant weight
of the three crucibles must be determined first. Once the constant weight of the crucibles is obtained
comes the precipitation of Barium Sulfate. Digestion comes next followed by filtering and washing of the
precipitate. The last step is the ignition to get the purity of the precipitate. Once the pure Barium Sulfate
(BaSO4) from each attempt are obtained, the percentage of Sulfur in each crucible can now be obtained.
Each BaSO4 yielded 35.6202%, 24.6607%, and 28.8536% of Sulfur consecutively. After getting the
percentage of Sulfur, a mean of 29.1775, a standard deviation of 5.5299, and %RSD of 18.6119 was
acquired from all the sample. To determine the difference between the mean of the three samples, t-
test was used which produced a 0.3122 result. The result shows that there is no significance difference
between the two means. The experimenters encountered several difficulties throughout the process
such as when handling chemical compounds like silver nitrate and breaking of the porcelain crucible.
Despite the difficulties, the experimenters were still able to successfully execute the appropriate step.
The experimenters also able to learn to use the techniques of gravimetry analysis. The experimenters
took precautions in order to avoid the accidents. Throughout the process, the experimenters were
able to learn the dynamics of precipitation, nucleation, peptization, filtration, ignition, and
calculations in gravimetry, executing each step effectively.