Lab: 15

Title: Gravimetric Analysis

Aim: To determine the percentage of sulphate in an unknown sulphate salt.

Apparatus:

o 250mL beaker

o 50mL measuring cylinder

o 25mL measuring cylinder

o Teat dropper

o Electronic balance

o Stirring rod

o Spatula

o Crucible with cover

o Small funnel

o Filter paper

o Bunsen burner

o Clay triangle

o Tripod stand

Materials:

o A- unknown sample

o B- 6M hydrochloric acid

o C- 0.15M barium chloride

Procedure:
1. The mass of a clean, dry 250mL beaker was measured to the nearest 0.01g using an

electronic balance. Between 0.35g and 0.40g of the unknown sample was added to the

250mL beaker and the mass of the beaker plus the sample to the nearest 0.01g was

recorded.

2. 50mL of distilled water was added to the sample in the beaker. 20 drops of 6M HCL

was then added to the beaker. The contents of the beaker were stirred until the sample

was entirely dissolved. The stirring rod was left in the beaker.

3. 25mL of 0.15M BaCl2 solution was measured in a graduated cylinder. The graduated

cylinder was cleaned and washed with distilled water but was not dried.

4. The solution containing the sample in the 250mL beaker was heated until it was

nearly boiling. The burner was turned off and small portions of BaCl2 was slowly

poured in small portions into the 250mL beaker containing the sample. This step took

three minutes. The contents of beaker were stirred as the BaCl2 solution was added.

The formation of a BaSO4 precipitate was observed. Remains of precipitate on the

stirring rod was washed into the solution with small amounts of distilled water and the

precipitate was allowed to settle in the beaker for 20 minutes.

5. While the precipitate settled the crucible was prepared by heating on the hottest part

of the Bunsen burner flame for about 2 minutes. After the crucible was cooled to

room temperature the mass of the crucible and cover to the nearest 0.01g was

recorded with the use of an electronic balance.

6. A piece of filter paper was prepared by folding it into quarters. The folded paper was

opened into a cone. It was placed into a funnel and it was wet with distilled water so

that it adhered to the funnel. A 500mL conical flask was placed under the funnel to

collect the filtrate.

7. After 20 minutes the mixture containing the BaSO4 precipitate was slowly poured

down into the filter paper while being stirred with a stirring rod. Caution was taken so

that the level of liquid in the filter funnel was never more than three-fourths of the

way to the top of the filter paper. When the transfer was completed the wash bottle

was used to rinse the residual precipitate from the beaker and the stirring rod into the

funnel.

8. After all the liquid was drained from the funnel the top edges of the filter paper was

pressed carefully together and the filter paper was folded into a compact package that

fit into the crucible. Little force was used to avoid tearing the filter paper. The folded

filter paper was placed into the crucible.

9. The crucible was supported with the clay triangle on the tripod stand. The crucible

was gently heated without the cover to remove the water. After several minutes when

the paper was dried, the crucible was heated vigorously and the filter paper burst into

flames. The filter paper was smothered with the crucible cover and the amount of heat

was lessened. it was heated moderately until the paper turned black.

10. Once the filter paper turned black the crucible was heated vigorously with the cover

off in the hottest part of the Bunsen burner. The bottom of the crucible was red hot.

The charred filter paper was gradually combusted and converted into CO2 gas. When

the filter paper was entirely combusted the while BaSO4 remained in the crucible. The

crucible was heated vigorously until there was no charred remaining in the filter

paper.

11. The crucible was cooled. When the crucible cooled to room temperature the mass of

the crucible, the cover and its contents, were recorded to the nearest 0.01g on the

electronic balance.
Results:

TABLE SHOWING RESULTS OF GRAVIMETRIC ANALYSIS

Mass/g
Mass of clean dry beaker 122.27
Mass of unknown sample + beaker 122.64
Mass of unknown sample 0.37
Mass of crucible + cover 78.85
Mass of crucible + cover + BaSO4 79.23

Calculations:

Mass of BaSO4 = 79.23 – 78.85

= 0.38g

Moles of BaSO4 produced = mass  molar mass

= 0.38  233

= 1.631  10-3mols

Mass of SO4 in BaSO4 = mass  molar mass

= 1.631  10-3  96

= 0.157g

Mass of SO4 in BaSO4 = Mass of SO4 in unknown sample

Mass of SO4 in unknown sample = 0.157g

% of SO4 in unknown sample = mass of SO4  mass of unknown sample  100

= 0.157  0.37  100

= 42.432%
Discussion:

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

substance by selective precipitation of the substance from an aqueous solution. The

precipitate is separated from the aqueous solution via filtration. The filtrate is then weighed.

The aim of this experiment was to determine the percentage of sulphate in an unknown

sulphate salt. This was done by gravimetric analysis. In the experiment, 0.37g of the

unknown salt was dissolved in water after which an excess of barium chloride was added to.

As a result, there was a precipitation of a sulphate namely, barium sulphate which was

collected weighed and dried. The mass recorded when weighed was used to determine the

number of moles of barium sulphate precipitate (1.631  10-3mols) which was equal to the

number of moles of sulphate in the original sample of the unknown. The number of moles of

barium sulphate precipitate (was equal to the number of moles of the sulphate in original

sample of the unknown because it was assumed that the reaction went to completion since

barium chloride added was added in excess. This was used to calculate the percentage by

mass of the original sample of the unknown which was calculated to be 42.432%.

Conclusion:

By adding excess barium chloride to an unknown sulphate salt, a precipitate, barium

sulphate, was formed which was dried and weighed. The mass of this weighed precipitate

was used to calculate the moles and the mass of sulphate in the unknown sample. The

percentage by mas was calculated which is 42.32%.

Sources of error:

1. Failure to combust all of the filter paper to form CO2 would’ve resulted in an

inaccurate measurement.