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EXPERIMENT NO.

Determination of Sulfate from a Soluble Sample by


Gravimetry
Santillan, H.S.Y.1
1

Chemistry Department, College of Science, Adamson University, Ermita, Manila 1000


Philippines
Keywords: Gravimetry, Sulfate, Precipitating Agent
1.0 Introduction
2.0 Gravimetry is one of the oldest
analytical methods used to determine an
analyte by its change in mass. There are
four types of Gravimetry methods:
electrogravimetry, volatilization, particulate
and precipitation Gravimetry (Harvey, David,
2000). In this experiment, precipitation
Gravimetry was used. The analysis can be
accurately done if the ion to be analyzed is
completely precipitated; the precipitate must
be a pure compound and can be easily
filtered. The reaction below shows the
balanced chemical reaction that will occur to
obtain all of the precipitate needed.
3.0

2+=BaSO 4 ( s)
2+Ba
4.0
SO 4
5.0 Equation 1: Precipitation Reaction of
BaSO4

6.0
7.0 A precipitating agent plays an
important role in this experiment because
the determination of the substance is
dependent on the mass of the sample. The
objective of this experiment is to determine
the %SO3 by Gravimetry and also to
familiarize students with the Gravimetry
method of analysis.
8.0
9.0 Experimental
10.0
The reagents used
were sulfate sample, BaCl2, 6M HCl
and 0.1M AgNO3 solution. The
materials used were porcelain

crucible, A; foil-covered wire gauze,


rubber policeman, Whatman no. 42,
and desiccator.
11.0
12.0
A. Constant Weighing of Crucibles
13.0 Two porcelain crucibles were
heated for 15 minutes and were placed to Al
foil-covered wire gauze for 5 minutes. The
crucibles were put into a beaker with watch
glass for another 5 minutes and then placed
to a desiccator for 20 minutes. Using an
analytical balance, the crucibles were
weighed. The procedure was repeated until
a 0.3 mg difference is obtained.
14.0
B. %SO3 Determination
15.0 A sulfate sample was given
by the professor. Two samples were
weighed at approximately 0.5 to 0.7 g with a
0.1 mg difference. The samples were
transferred to a 1000-mL beaker each. The
sulfate sample was dissolved to 200 mL
distilled water with 4-mL 6M HCl. A 1.3g of
BaCl2 was dissolved in 100 mL distilled
water. The BaCl2 solution and sulfate
sample solution were heated at nearly
boiling. While hot, the entire BaCl2 solution
was added to the hot sulfate solution while
stirring. The glass rod was washed with
distilled water and the washings were added
to the final mixture. The mixture was
digested and left to stand overnight.
16.0 The mixture was filtered
using Whatman no. 42. All the precipitate
should be transferred to the filter paper
using a rubber policeman. The beaker was
washed with hot distilled water and the

washing was tested with 0.1M AgNO3


solution. If clouding formation occurred,
wash again and test the washing. If not, the
filter paper was lifted from the funnel and
folded until it fits the constant weighed
crucible. The crucible was heated with a
small flame. When the filter paper is already
dry, the flame was increased to char the
filter paper. If the filter paper catches fire,
smother the flame with the lid. The product
was ignited by heating it with full flame for
15 minutes. The crucible was cooled and
placed in an Al foil-covered wire gauze for 5
minutes then placed inside a beaker with
watch glass. After 5 minutes, place in a
desiccator for 20 minutes then weighed.
The procedure was repeated until 0.3 mg
difference was obtained. The %SO 3, mean,
standard deviation and %RSD was
computed.
17.0
18.0 Results and Discussion
A. Constant Weighing of Crucibles
19.0 Constant weighing is very
important for this experiment because the
result will be highly independent on the
mass so a lot of heating is required to
vaporize any impurities left on the crucible.
Also, a porcelain crucible was used
because it can withstand a great amount of
heat up to 1150C. Carbon soot may form
due
to
incomplete
combustion
of
hydrocarbons and can be removed by
directing it on the flame. The picture below
shows the correct position in heating a
crucible.
20.0
21.0
22.0
23.0
24.0
25.0
26.0
27.0
28.0
29.0

30.0 Source:
http://www.csudh.edu/oliver/demos/heatcru
c/coolside.jpg
31.0 The hot crucible is placed on
Al foil-covered wire gauze to avoid melting
of the paint and was placed again inside a
beaker with watch glass to prevent
absorption of impurities. Before putting into
the desiccator, the porcelain crucible should
not be too hot because it will vacuum the air
inside and will cause difficulty in opening the
desiccator. After 20 minutes, the crucible
was weighed in an analytical balance. The
balance should be wiped first and press the
tare button to ensure the accuracy of the
mass.
32.0
33.0
Table 1: Constant Weight of
Crucible
34.0
35.0 Cru 36.0 Cr
cible A
ucible B
37.0 Mass of 38.0 20. 39.0 21.
Trial 1
5254 g
5222 g
40.0 Mass of 41.0 20. 42.0 21.
Trial 2
5254 g
5221 g
43.0 Mass of 44.0 20. 45.0 21.
Trial 3
5257 g
5223 g
46.0 Constant
47.0 20. 48.0 21.
Weight
5257 g
5223 g
49.0 Table 1 shows the masses of
the crucible before achieving its constant
weight.
50.0
B. %SO3 Determination
51.0 A 0.5212 g and 0.5236 g of
the sample were weighed and dissolved to
distilled water with 6M HCl. The HCl will
help lower the ph of the solution which will
increase the solubility of the sulfate sample
and will inhibit the formation of BaCO3
precipitate to yield more BaSO 4 precipitate.
A 200 mL of BaCl2 solution was prepared for
each of the sample, this serves as the
precipitating agent. The hot BaCl2 solution
was added to the hot sulfate sample
solution because the solubility increases as
the temperature increases. The BaCl2
solution was added in excess to favor the
formation of the BaSO4 crystalline
precipitate. Stirring is very important to

completely dissolve the entire sulfate


sample and to thoroughly mix the solution
for a better formation of precipitate. The
washings of the glass rod should be added
to the mixture because some of the sulfate
is attached to it. The mixture was left
overnight for the precipitate to fully settle at
the bottom.
52.0 Filter paper is more preferred
than sintered glass filter because a higher
chance of error might occur when the
precipitate adheres on the surface of the
glass. Whatman no. 42 is used as a filter
paper because of its porosity and is very
suitable for hot barium sulfate. Whatman no.
42 is known for its being ashless because it
is made from cultured pulp and linters
(http://www.chimica.unipd.it/,
2014).
A
rubber policeman was used to scrape all the
remaining precipitate left on the beaker. A
glass rod was used to give path for the
solution and prevent it from spilling. The
picture below shows the correct way of
filtering.
53.0
54.0
55.0
56.0
57.0
58.0
59.0
60.0
61.0
62.0
63.0
64.0 Source:
http://www.csudh.edu/oliver/demos/gravsulf/
hhgrvslf.htm
65.0
The washings were tested
with AgNO3 to test for the presence of
chloride ions. The filter paper was carefully
lifted from the funnel to avoid the precipitate
from falling. The filter paper should be
properly fitted in the crucible to avoid the fire
from directly heating the filter paper. The
crucible was heated with a small flame to
dry the precipitate first and remove any
excess solvent. The flame should be
smothered to prevent carbon from reducing
sulfate ion to sulphide ion which will form
carbon
monoxide

(http://ww2.chemistry.gatech.edu/,
n.d.).
Ignition is when a substance undergoes
complete combustion and chemical change.
Ignition is more preferred because it is
faster and more efficient than drying. The
ignition is already done if the product looks
like shown in the picture below.
66.0
67.0
68.0
69.0
70.0
71.0
72.0
73.0
74.0
75.0
76.0
77.0 Source:
http://www.csudh.edu/oliver/demos/gravsulf/
hhgrvslf.htm
78.0
79.0 The product formed was Barium
sulphide from the Barium sulfate heated in a
filter paper. This reaction below occurred.
80.0
81.0

BaSO 4 (s)+ 4 C (s) BaS(s)+ 4 CO(g)


82.0
83.0
84.0
85.0

Equation 2: Reaction during ignition

Table 2: %SO3 Determination


86.0 Trial
87.0 Trial
1
2
88.0 Weig 89.0 0.521 90.0 0.523
ht of Sample 2 g
6g
91.0 Weig 92.0 0.663 93.0 0.694
ht
after 1 g
2g
ignition
94.0 %SO 95.0 43.64 96.0 45.48
%
%
3
97.0 Table 2 shows the mass of the
sulfate recovered after the ignition and the
%SO3 in the sulfate sample given the
professor.
98.0
99.0 Conclusion
100.0 The percentage of SO3 was
successfully determined through gravimetric
analysis. In trial 1, the %SO 3 recovered was

43.64% while in trial 2, 45.48% was


recovered. The mean of the two
percentages is 44.56% and its standard
deviation is 1.301%. The relative standard
deviation is 2.920 %.
101.0
102.0 References
No Author (n.d.) Chapter XV:
Gravimetric
Methods,
Website:
http://www.ecs.umass.edu/cee/reckhow/
courses/572/572bk15/572BK15.html
Harvey,
David
(n.d.)Analytical
Chemistry 2.0, Chapter 8, pg. 355
No Author (n.d.) Experiment Two
103.0
Gravimetric Determination of
Sulfate
in
Seawater,
Website:
http://ww2.chemistry.gatech.edu/class/2
115/bottomley/expt2.PDF
Harvey, David (2000) Modern Analytical
Chemistry,
Mc-Graw
Hill,
North
America, pg. 234
No Author (2014) Filter Papers and
Membranes, pg. 4
104.0

105.0
106.0 Sample Calculation
107.0

0.6631 g BaSO 4

1 mol BaSO 4

233.3906 g BaSO 4

108.0

1 mol SO 3
80.0642 g SO 3

=0.2275 g SO 3
1 mol BaSO 4
1 mol SO 3

109.0

0.2275 g SO3
100 =43.64 SO 3
0.5212 g SO 3

110.0

111.0
112.0 Mean %SO3
113.0

43.64 SO 3 +45.48 SO 3
=44.56 SO 3
2

114.0 Standard Dev. 1.301 % SO3


115.0 %RSD
116.0

1.301
100 =2.920
44.56

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