Analytical Chemistry Laboratory Report

Bretaña, Dupaya, Tan

I. Objectives
1. Determine the constant weight of the crucible and its exact weight.
2. Precipitate Barium Sulfate (BaSO4) from Barium Chloride (BaCl), water
and an unknown Sulfate sample.
3. Isolate the precipitate through ignition.
4. Filter out Chlorine compounds from the precipitate and test with a Silver
Nitrate (AgNO3) solution.
5. Determine the constant weight of the crucible with precipitate sample.
6. Determine the amount of Sulfur in a Soluble Sulfate Salt using gravimetric
analysis, specifically, the Precipitation Method.
7.
II. Outline of Procedure
III. Data and Results

Table 1. ​Masses of crucible without precipitate; and the mean, standard deviation and
relative standard deviation.
1st heating 2nd heating 3rd heating Mean std. dev %RSD
(g) (g) (g) (Standard (Relative
Deviation) Standard
Deviation)

Crucible 1 24.1470 24.1465 24.1469 24.1468 2.6458 x 10​-4 ± 0.0012%

~ ​0.0003

Crucible 2 27.1319 27.1321 27.1316 27.1319 2.5166 ​x 10​-4 ± 0.0011%

~ ​0.0003

Crucible 3 25.9991 25.9988 25.9993 25.9991 2.5166 ​x 10​-4 ± 0.0011%

 ~ ​0.0003

Table 2. ​Masses of crucible with precipitate

1st heating 2nd heating 3rd heating Mean std.dev %RSD

(g) (g) (g) (Standard (Relative
Deviation) Standard
Deviation)

Crucible 1 24.8055 24.8070 24.8080 24.8068 1.2583​x10​-4 ± 0.0052%

~ ​0.0013

Crucible 2 27.9991 28.0007 28.0012 28.0003 1.0970​x10​-4 ± 0.0039%

~ ​0.0011

Crucible 3 27.0520 - - 27.0520 - -

Table 3. ​Summary of the mass of crucible, mass of crucible with precipitate and mass of
the precipitate; and the mean, standard deviation, relative standard deviation and the
amount of percent sulfur.

Constant Constant Weight of Mean std.dev %RSD %Sulfur

weight of weight of the the (Standard (Relative
the crucible + precipitate; Deviation Standard
crucible; ​B precipitate; ​A (A-B) ) Deviation)

Crucible
1 24.1468 g 24.8068 g 0.6600 g 24.4768 0.4667 ± 1.9067% 16.64%

Crucible
2 27.1319 g 28.0003 g 0.8684 g 27.5661 0.6141 ± 2.2277% 21.90%
Crucible 25.9991 g 27.0520 g 1.0529 g 25.5256 0.7445 ± 2.9167% 26.55%
3

Mean 21.70%
(%Sulfur)

std.dev 4.9581
(Standard
Deviation)

%RSD 22.85%
(Relative
Standard
Deviation)

The determination of sulfur from the unknown soluble sulfur salt is done through
the formula,
32.06
(A− B) × 233.40
%S = wt sample
×100%

Solution:

Crucible 1
(24.8068 − 24.1468) × 32.06
%S = 0.5447
233.40
×100%
=16.64367499%

Crucible 2
(28.0003 − 27.1319) × 32.06
%S = 0.5447
233.40
×100%
=21.89904146%

Crucible 3
(27.0520 − 25.9991) × 32.06
%S = 0.5447
233.40
×100%
=26.55170515%

wherein the %S refers to the percent composition of Sulfur in the sample, A referring to
the constant weight achieved from the crucible + precipitate, which in this case is
24.8068g, 28.0003g and 27.0520g respectively, B referring to the constant weight
achieved from the crucible only, which is 24.1468g, 27.1319 and 25.9991g,
respectively, and wt sample referring to the weight of the sample soluble sulphate salt,
which in this case is 0.6600g, 0.8684g and 1.0529 g respectively. The numbers 32.06
and 233.40 refer to the molar masses of Sulfur (32.06 g/mol) and Barium Sulfate
(233.40 g/mol), respectively. The determination for the percent composition of Sulfur
requires determining the number of moles of Sulfur in the precipitate, which is Barium
Sulfate (BaSO4), importantly a known compound with a known molar mass, and from
there, determine the Sulfur content from the soluble Sulfur compound, an unknown
compound with an unidentifiable molar mass. In this sample, the crucible 1 had a %S of
16.64%, crucible 2 had a %S of 21.90% and crucible 3 had a %S of 26.55%.

Table 4.1 ​The amount %Sulfur of Group 3 and Group 6 and its mean, standard
deviation and relative standard deviation.

Group 3 (%S) Group 6 (%S)

Crucible 1 16.64% 17.58%

Crucible 2 21.90% 16.94%

Crucible 3 26.55% 15.85%

Mean 21.70% 16.79%

Standard deviation 4.9581 0.8747

Relative Standard Deviation 22.85% 5.21%

Set-ups Mean T-Value Decision on Difference

Computed Tabulated

Group 3 21.70
/1.6892/ +/- 2.776 Not Significant
Group 6 16.79

Table 4.2 ​Difference in the amount of Percent Sulfur between Group 3 and Group 6.

In comparing two means, these formula will be used,

Solution:
4.95812
F= 0.87472
= 32.13 =/ 1 (U nequal variances)
2 2
Sp = √ (3−1)(4.9581 ) +(3−1)(0.8747 )
3 + 3 −2
21.70−16.79
= 3.56≈4
t= = 1.6892
3.56 √ 13+ 13
t95 = 2.776
 2.776 > 1.6892​ (​ Therefore, there is no significant difference between two means.)

IV. Discussion

In this experiment, an unknown Sulfate sample was given and the composition of
Sulfur in the sample is to be determined. Precipitation method was used to remove
metal ions from compounds in the solution with Barium Chloride as precipitation agent.
The crucible was weighed thrice as a matter of preparation. Then the sample solution
was prepared by heating in the Bunsen burner, adding water, Hydrochloric acid, and the
Barium Chloride solution. The residual compound of Chlorine and the unknown ion was
then filtered out of the precipitate, leaving the Barium Sulfate, which is insoluble in
water. However, during the process in one of our three trials, a colloid precipitate was
formed instead of a crystalline precipitate. This process is termed peptization when the
coagulated particles are redispersed. This could have occurred probably because the
solution was not properly heated before adding the BaCl or the solution was not
properly stirred as instructed. The other two trials were successful though. Further
testing with the addition of Silver Nitrate was done because it helps in determining if all
of the Chlorine compound was filtered out. During filtration, the precipitates were
washed with hot water. The Barium Sulfate was then ignited to isolate it from the filter
paper. After precipitates were formed and weighed, the %S in the original sample can
then be calculated, giving a %S concentration of 16.64%, 21.90%, and 26.55% for the
three trials, respectively. Throughout the experiment, mistakes and uncertainties were
encountered, specifically during the constant weighing of the crucible; in the preparation
of the precipitate and on igniting the precipitate. Errors have been met during the
experiment affecting the outcome. These could have been avoided by carefully
following the instructions, by being constantly alert while in the laboratory, by integrating
the concepts on gravimetric analysis and precipitation methods while doing the
experiments, and always being mindful of the equipment and glass wares while on the
lab.
The masses of the crucible without the precipitate, their mean, standard
deviation, and relative standard deviation were shown in table 1. The mean mass of
crucible 1 was 24.1468g, while having a standard deviation of ​2.6458 x 10​-4​, and a
relative standard deviation of ​± 0.0012%. Crucible 2 had a mean mass of 27.1319g, a
standard deviation of 2.5166 ​x 10​-4​, and a % relative standard deviation of ​± 0.0011%.
Lastly, crucible 3 had a mean mass of 25.9991g, a standard deviation of 2.5166 ​x 10​-4
and a % relative standard deviation of ± 0.0011%. Crucible 2 and 3 have the same
standard deviation and % relative standard deviation.
In table 2, the masses of the crucible with precipitate, mean, standard deviation,
and relative standard deviation were shown. In crucible 1, it had a mean mass of
24.8068g, a standard deviation of 1.2583​x10​-4​, and a % relative standard deviation of ±
0.0052%. Crucible 2 had a mean mass of 28.0003g, a standard deviation of
1.0970​x10​-4​, and a % relative standard deviation of ± 0.0039%. However, in crucible 3, it
had a weight of 27.050g and it only underwent 1 trial. We have only weighed it once
because we did not have enough time since we had to perform it again due to the fact
that it turned out to be colloidal, thus, it only underwent heating and weighing once.
 Table 3 presented the summary of all of our data, the mean masses of the
crucible only (A), the mean masses of the crucible with precipitate (B), the weight of the
precipitates, the mean of (A) and (B), their standard deviation, their % relative standard
deviation, and the % Sulfur. Crucible 1 had mean masses of 24.1468g (A), 24.8068g
(B), the weight of its precipitate was 0.6600g, a standard deviation of 0.4667, a %
relative standard deviation of ± 1.9067%, and a % Sulfur of 16.64%. Crucible 2 had
mean masses of 27.1319g (A), 28.0003g (B), a precipitate that weighed 0.8684g, a
mean of 27.5661, a standard deviation of 0.6141, a % relative standard deviation of ±
2.2277%, and a 21.90% of sulfur. Lastly, crucible 3 had mean masses of 25.9991g (A),
and 27.0520g (B), a precipitate that weighed 1.0529g, a mean of 25.5256, a standard
deviation of 0.7445, a % relative standard deviation of ±2.9167%, and a 26.55% of
Sulfur.
Computing for the weight of the precipitate was subtracting the constant weight
of the crucible + precipitate (A) to the constant weight of the crucible (B). Computing for
the relative standard deviation was done by using the formula of standard deviation
mean
×100% .
32.06
(A−B)× 233.40
Computing for the % Sulfur was done by using the formula %S = wt sample
×100%

Table 4.1 presented the amount of % Sulfur of group 3 and group 6 and their
respective means, standard deviation, and relative standard deviation. In the 1st
crucible, group 3 had a %Sulfur of 16.64 while group 6 had a %Sulfur of 17.58. In the
second crucible, group 3 had a value of 21.90%, while group 6 got 16.94%. In the 3rd
crucible, group 3 had a %Sulfur of 26.55, while group 6 got a result of 15.85%. Group 3
had a mean of 21.70%, while group 6 had a mean 16.79%. The standard deviation for
group 3 was 4.9581, while group 6 had 0.8747. Lastly, the relative standard deviation
for group 3 was 22.85%, and group 6 had a relative standard deviation of 5.21%.
Table 4.2 showed the difference in the amount of percent Sulfur between group 3
and group 6. Having a mean of 21.70 and 16.79 respectively, the computed t-value was
/1.6892/ while the tabulated value of a 95% confidence interval was +/- 2.776. This
means that there is no significant difference between the two means since the
computed t-value was smaller than the tabulated t-value.

V. Conclusion

The experiment started with doing a constant weighing on the given crucibles.
The sample was heated and was added with water, Hydrochloric acid, and Barium
Chloride solution. After adding the following substances, the proponents then
proceeded with the filtering process. Because of the solubility of chlorine and unknown
ion residuals, both can be filtered easily. Barium sulfate will be left because it is
insoluble with water. Adding a drop of silver nitrate would allow the proponents to
determine if there is still chlorine present.
Igniting the Barium Sulfate will allow it to isolate from the filter paper. The
proponents can then identify the percent of the sulfur from the original sample. 16.64%
of Sulfur for trial 1, 21.90% of Sulfur for trial 2, and 26.55 % of Sulfur for trial 3 were
obtained.
The proponents encountered complications throughout the experiment. one out
of the three trials was still colloidal throughout the experiment and must be placed on
the hot plate again to not make it colloidal again. This hinders the proponents to
proceed to the next step since they have to do the previous step again. From this, the
proponents was not able to finish one out of three trials.
There were lessons gained from this experiment. The proponents have realized
that they must carefully follow the steps in order for them to avoid any complications
that may hinder them from achieving their goal. The proponents also realized that they
should always be mindful with their lab equipment so that they will not break any
equipment in their future laboratory activities. Teamwork was also present in doing this
experiment. Teamwork allowed the proponents to achieve their goal despite of
encountering a lot of challenges.