Abstract:

To determine the amount of sulfate in a unknown sample by gravimetric

analysis.

Introduction :
Gravimetric analysis is a technique through which the amount of an analyte
(the ion being analyzed) can be determined through the measurement of mass.
Gravimetric analyses depend on comparing the masses of two compounds
containing the analyte [1].
Gravimetric analysis includes several steps such as;
1- Preparation.
2- Precipitation.
3- Digestion, which is a process where the precipitate is re-dissolved and
precipitated out of a cleaner environment (solution) [2].
4- Filtration, which is a process of separating suspended solid matter from a
liquid, by causing the latter to pass through the pores of some substance
[3].
5- Washing.
6- Drying / ignition.
7- Weighing
Sulfate is routinely determined by precipitating it with barium chloride to
form insoluble barium sulfate. The Barium Sulfate particles precipitating
initially are too small to filter and wash properly so they are digested to form
larger crystals, which can be handled more easily. This process produces
extremely insoluble crystals according to the following equation [4]:
Na2SO4(aq) +BaCl2(aq)  BaSO4(s)+ 2NaCl(aq)
 Materials :
- Dried Na2SO4.
- 0.2 M BaCl2.
- 0.1 M AgNO3.
- Filter paper (ashless).
- Two 600 mL beaker.
- Concentrated HCl.
- Concentrated HNO3.
- Dropper.
- 100 mL beaker.
- Watch glass.
- Glass rod.

Results and calculations :

Trial 1 Trial 2 Trial 3

Mass of unknown Sample 0.3297 0.4065 0.4952
Na2SO4(g)
Molar Mass of Na2SO4 (g/mol) 142
Mass of crucible &Lid (empty)(g) 49.8037 53.4245 53.2009
Mass of product 50.2902 54.0378 53.8084
[BaSO4]&crucible (g)
Mass of BaSO4 (g) 0.4865 0.6133 0.6075
Molar mass of BaSO4(g/mol) 233.38
Moles of BaSO4 (mol) 2.084 x 10-3 2.627x 10-3 2.603x 10-3
Moles of SO4 -2 (mol) 2.084 x 10-3 2.627x 10-3 2.603x 10-3
Molar mass of SO4 -2 (g/mol) 96.06
Mass of SO4 -2 (g) 0.2001 0.2523 0.2500
Experimental% of SO4 -2 60.69% 62.06% 50.48%
Theoretical% of SO4 -2 67.64%
Error% 10.27% 8.24% 25.36%

Mean 0.2341 Standard deviation 0.029

Variance 5.8x 10-4 Range 0.2523-0.2001
Relative Standard 12.387 Coefficient of 0.12387
deviation variation
Discussion :
A certain amount (from 0.3 to 0.5 g) of the sample was weighed into 600 ml
beaker. The sample was diluted with 150 ml of distilled water, then 2.0 ml of
concentrated HCL was added in the beaker and the mixture was heated nearly
to the boiling point. Then, 50.0 ml of water was added to 15.0 ml of 0.2 M of
BaCl2 in a smaller beaker and heated nearly to the boiling point. This mixture
was then added to mixture in the bigger beaker and let it sitter slowly and
effectively after some time the precipitate was allowed to settle down. Later,
few drops of BaCl2 was added for complete precipitation test. When the
precipitating was completed, the beaker was covered with the watch glass
and digested below the boiling point for 30 minutes. The supernatant was
decanted through ash less filter paper. The precipitate in the beaker was
washed by warm water and then decanted after the precipitate settled. The
filter paper was washed with warm water for transferring the precipitate to it.
Later, two drops of concentrated nitric acid (HNO3) was added for complete
filtration test, an empty porcelain crucible(with its lid) was weighed. When the
filtrating was completed, the filter paper was folded completely around the
precipitate and put into the crucible which was later heated in a furnace.
We diluted the sample and let the mixture have an effective stirring so we
can keep the concentration (Q) low and we let the mixture heat to increase
solubility (S).
For filtration, ashless paper was used. Ash less paper is composed of a volatile
material, and therefore, it will not affect our mass reading when we ignite our
precipitated product.
The experiment’s accuracy can be improved by doing more iterations of
washing the precipitated product.

References:
[1] "Wired Chemist," www.wiredchemist.com Accessed December 20, 2017.

[2] "Ion chem," ion.chem.usu.edu Accessed December 20, 2017.

[3] "Lenntech," www.lenntech.com Accessed December 20, 2017.

[4] Chemistry 310 Lab Manual. Bahrain: University of Bahrain, 2017.