Experiment No.

2
Chem 28.1-4
Quantitative Inorganic Analysis Laboratory
Department of Chemistry
College of Arts and Sciences
University of the Philippines Visayas

Gravimetric
Determination of SO3 in
a Soluble Sulfate

Amilbahar, Seannekate V.

Lerona, Paul Gabriel E.

31 October 2014

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GRAVIMETRIC DETERMINATION OF SO3 IN A SOLUBLE
SULFATE
Amilbahar, S.V., Lerona, P.G.E.

ABSTRACT

This experiment mainly aims to determine the % SO 3 w/w in an unknown sulfate salt sample

using gravimetric analysis, specifically the precipitation analysis. The sample solution was

precipitated as barium sulfate, BaSO4, using BaCl2 as a precipitating agent. The obtained

precipitated was purified by a series of processes, to wit, digestion, filtration, ignition and drying.

After drying, assuming a pure substance, the dried BaSO 4 was weighed and analysed. The mass

of SO3 was calculated by multiplying the mass of BaSO 4 to the predetermined gravimetric factor

(0.3430). The obtained percentage SO3 is 25.27% which is close to the actual percentage

25.39%.

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INTRODUCTION

Gravimetric analysis is a quantitative method for accurately determining the amount of a

substance by means of selective precipitation of the substance from an aqueous solution (SMC,

n.d.). In precipitation gravimetry, the analyte is separated from the solution by converting it to a

sparingly soluble precipitate and is then filtered and converted to a known compound of known

composition by suitable heat treatment that can be weighed.

This experiment aims to determine the amount and the percentage of SO 3 in the unknown

sulfate salt using gravimetric analysis. By performing the experiment, the experimenters will be

able to learn the techniques of gravimetry and the science of accuracy. Furthermore, the

experimenters will also be able to learn the dynamics of precipitation, particle growth and

nucleation, coprecipitation, peptization, filtration, ignition, and stoichiometric calculations in

gravimetry.

Given the specific mass of the sample provided by the lab instructor, the experiment is

expected to yield close result to the actual percentage of SO3 in the sample which is 25.39% w/w.

To abide with the purpose of this experiment and with its specified expectancy, Barium

chloride is used as the precipitating agent to produce barium sulfate. It is done in accordance

with the following chemical formula

2−¿→ BaS O4 (S) ¿
2+¿+S O 4( aq) ¿
Ba(aq)

This experiment is only limited to the determination of SO3 from a soluble sulfate salt.

Only three replicates will be done. This will be conducted at the Chemistry Laboratory,

Department of Chemistry, University of the Philippines Visayas, Miag-ao Campus, Miag-ao,

Iloilo.

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MATERIALS AND METHODS

Preparing the Crucibles

The thoroughly clean and labeled crucibles

were heated to redness at maximum temparature over

the Tirill burner for 15 minutes. After heating to

redness, the crucibles were cooled in a clean place for

two minutes, then were transferred in a desiccator for

30 minutes. The crucibles were then weighed.

Figure 1 Preparing the crucibles
Repetition of heating and cooling were done until the

constant weights per crucible were achieved. Figure 1 shows the setup for the heating of

crucibles.

Preparation of Sample

The sample was dried in an oven for two hours at 110.5°C and cooled in a

desiccator for 30 minutes. Then, the sample was divided into three subsamples by

weighing 0.5709 g., 0.5341 g., 0.5448g., of the sample, repectively, using the analytical

balance (Model: Shimadzu).The weighed subsamples were dissolved in 225 mL distilled

water with 1 mL HCl in it.

Precipitation

The sample solution was boiled along with the

BaCl2 solution. Both solutions were heated to boiling

and the BaCl2 solution was poured into the sample in

a slow manner to encourage particle growth. The

settling of precipitate was allowed and the completion

Figure 2.0 Precipitation of BaSO4
(www.fphoto.photoshelter.com)

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 of precipitation was tested using BaCl2 and the supernatant liquid. Then, the solution was

steam bathed for 30 minutes. Figure 2 shows the dramtization of the precipitation of

BaSO4.

Filtration and Washing the Precipitate

Using Whatman Filter Paper No.42, the

solution was filtered and its supernatant liquid

was decanted and discarded. Any precipitat es

from the beaker were removed using a stream of

water from the was bottle and rinsed into the

filter paper. The rinsing was continued until

chloride is absent from the test portion of the

washings. Figure 3 shows an example of

Figure 3 Filtration Setup (ww.csudh.edu)
filtration setup.

Ignition and Weighing of the Precipitate

The filtered precipitate was transferred to

the prepared crucible. The precipitate was dried

and ignited over the Tirill burner until the filter

paper charred and the precipitate became wh ite.

The dried precipitate was cooled for two minutes

in a separate place an d then transferred into the

dessicator for 30 minutes. Subsequently, after

cooling, the crucibles and its contents were

Figure 4 Ignition and Drying (ww.csudh.edu)

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weighed. The whole ignition process were repeated until the constant weights were

achieved. Figure 4 shows the iginition and drying setup.

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RESULTS

This section includes all the findings in this experiment. The data were organized in

tabular form. It has been found that the sample containing a soluble sulfate salt contains 25.27%

SO3 that is very close to 25.39%, as in the actual value. This experiment led the experimenters to

different aspects of gravimentry. Skills in weighing, liquid transferring and precipation were

being tested, which is being reflected in the results for precision and accuracy.

Table 1 Percent SO3 in the Sample

Trials Masscruc+prec MassCrucible MassBaSO4 Masssample MassSO3 % SO3

1 26.872 26.4662 0.4058 0.5709 0.1392 24.38
2 21.5274 21.1533 0.3741 0.5341 0.1283 24.03
3 24.9151 24.48 0.4351 0.5448 0.1492 27.39

Table 1 shows the gathered data for the gravimetric analysis of the sample. It has been

found that the sample contains almost 25% SO 3 w/w and its relative variability for the three

replicates is determined to be 73.25 parts per thousand which is usually considered as good for

repeatability and routine measurements (Hibbert, 2006). In order to solve for the %SO3, the

weight of the precipitate is obtained from the subtraction of the constant mass of the crucible to

the mass of the crucible + precipitate. The mass of precipitate, BaSO 4, is then subjected to

gravimetric calculations involving the use of the gravimetric factor. Moreover, as shown in

Appendix, constant weights for the three crucibles are obtained through repeated heating until

the recorded weights agree to the ±0.0003g range.

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DISCUSSION

Given the raw data from the Lab Instructor, the sample should contain 25.39% SO3 w/w.

With such aforementioned claim, the experiment supported it after obtaining 25.27% SO 3.

Moreover, the precision of the methods performed is described in its relative error which -0.49%

that is very small. Furthermore, just between the replicates, there is 73.25 ppt which is still good.

Using the gravimetric analysis, the percent SO3 is determined from the mass of the

precipitate, BaSO4, multiplied to its gravimetric factor. Moreover, in all precipitation analysis,

the precipitate that will be weighed is a pure substance of definitely known composition.

However, several errors, both systematic and random, were encountered throughout the

experiment. The major source of error in gravimetric analysis is the presence of impurities in the

precipitate. It is difficult to prevent other ions from coming down with the precipitate. Such

dragging down of normally soluble ions with an insoluble substance is coprecipitation. Foreign

ions were incorporated in the crystal lattice, either adsorbed in the surface, or occluded within

the crystal structure. Barium sulfate, as in this experiment, has great selective coprecipitation

tendencies (Hamilton, 1971). Thus, in filtration, the precipitate was washed with water.

However, peptization, a process in which the coagulated particles are redispersed, could have

happened and washing with a dilute electrolyte solution was not observed.

Barium sulfate normally precipitates as very small crystalline particles, and ideal

precipitates should have bigger particle size. Digestion, or Ostwald Ripening, is a process in

which a precipitate is heated in the solution from which it was formed and allowed to stand in

contact with the solution (Skoog et al., 2014). In this experiment, barium sulfate undergone

digestion where its particles increased in size by favoring particle growth than nucleation,

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became easier to filter, and the particles decreased in surface area and the amount of its adsorbed

impurities (Pierce et al., 1958).

Impurities may be gone after digestion, but water molecules may be adhering loosely in

the crystal structure. So before weighing, to ensure the purity of the precipitate, the excess wash

liquid was removed by drying and ignition. The precipitate folded together within the ashless

filter paper was ignited in the crucible. However, by ignition, the precipitate may decompose by

driving off volatile oxides, from which, BaSO 4, at high temperature decomposes to BaO and

SO3. So, with this idea, the temperature is carefully controlled. Extra care were taken to prevent

possible reduction of BaSO4 by carbon from the paper, BaSO 4 +4 C → BaS+ 4 CO.

However, the relative error noted is negative, which implies that there is a loss of

precipitate during the purification process. This could be either due to an accidental tearing of the

filter paper because of the experimenter’s mishandling of the filtration setup; or the

aforementioned phenomena (e.g. peptization, smaller particle size that might be from insufficient

digestion, etc.). With respect to the errors that may be arising or may have arose in the

experiment regarding the purity of BaSO4, and other potential errors in the precipitation method,

still, such analysis gave a very accurate result.

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CONCLUSION

In this precipitation analysis, the unknown salt containing sulfate was precipitated using

BaCl2. The resulting precipitate, BaSO4, undergone: digestion, for favouring particle growth and

filterability; and, filtration and ignition, for the purity of the precipitate. After obtaining and

weighing a pure BaSO4, the mass of the SO3 was determined by multiplying the mass of the

precipitate to its gravimetric factor (0.3430). The experiment showed that the sample contains

25.27% SO3 which is close to the actual value determined by the Lab Instructor that is 25.39%.

The yielded relative error was -0.49% and the error between the replicates is 73.25 ppt. Errors

that caused the loss of precipitate (e.g., coprecipitation, peptization, smaller sizes of particles,

etc.) will be avoided and countered; and the skills will be improved for the next experiments. The

dynamics of precipitation has been elucidated and were comprehended by the experimenters.

The skills of accurate weighing, transferring of liquids, precipitating, filtrating and getting the

constant were learned and mastered by the experimenters, which is reflecting the precision and

accuracy of results. Filtration of the precipitate may have been taking the time but experimenters

were able to learn new and maneuvering techniques to speed up the entire filtration by constant

washing and stirring. The utilization and application of the skills that were learned and mastered

are looked forward by the group into the next few experiments.

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CONTRIBUTION OF PARTNERS

Each of us did our best for the success of this experiment. Seannekate, my lab partner was able to

contribute effectively in proper handling of the instrument and other necessary calculations for

the data. It was a job well done for her.

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REFERENCES

Books

Hamilton, L.F., Simpson, S.G., Quantitative Chemical Analysis, 12th ed.; MacMillan Publishing

Co., Inc.: New York, 1971; pp 320-330.

Hibbert, D.B., et al., Data Analysis for Chemistry : An Introductory Guide for Students and

Laboratory Scientists; Oxford University Press, Inc.: New York, 2006; p. 43.

Pierce, W.C., et al., Quantitative Analysis,4th ed.; John Wiley & Sons, Inc.: New York, 1958; pp

337-344.

Skoog, D.A., West, D.M., et al., Fundamentals of Analytical Chemistry, 9th ed. ; Cengage

Learning Asia Pte Ltd., 2014.

Portable Document Formats/Websites

Santa Monica College. Chemistry 11. Gravimetric Analysis. [Online] n.d.

http://www.smc.edu/projects/28/chemistry_11_experiments/gravimetric_analysis_procedure

.pdf (Retrieved last October 31, 2014)

Photos.

Ftphoto, Fundamental Photographs-Precipitation: Barium Sulfate. From http://fphoto.photoshel

ter.com/image/I0000.yLVq6Q5oak. (Retrieved last October 31, 2014).

Seely, O., CSUDH, Gravimetric Sulfate Determination, Helpful Hints. From:

http://www.csudh.edu/oliver/demos/gravsulf/hhgrvslf.htm. (Retrieved last October 31,

2014).

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APPENDIX A- Table

Table 2 Constant Weights for the Crucible

Crucible No. W1 W2 W3 W4 CWg

1 26.4606 26.4661 26.4645 26.4662 26.4662

2 21.1531 21.1546 21.1534 --- 21.1533

3 24.4788 24.48 24.48 --- 24.48

Table 3 Constant Weights for the Precipitate

Crucible
W1 W2 W3 W4 Masscruc+prec Massempty cruc Massprec
No.

1 26.8279 26.872 26.872 --- 26.872 26.4662 0.4058

2 21.5278 21.5274 21.5273 --- 21.5274 21.1532 0.3741

3 24.9141 24.9156 24.9149 24.9152 24.9151 24.48 0.4351

Calculation of True Value of %SO3 from the Unknown Salt

Mass Na2SO4 0.7513

Mass Sample 1.66787
MW Na2SO4 142.05
MW SO3 80.07
0.42350
Mass SO3 8
0.25392 25.3921
2 8
MW S O3
Mass S O3 =Mass N a2 S O4 ×
MW N a2 S O4
80.07 g SO❑3
¿ 0.7513 g N a2 S O4 × =0.42351 g S O3
142.05 g N a2 S O4

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 0.42351 g S O 3
%S O 3 = ×100 %=25.3 9 %
1. 66787 g sample

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