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Activity 7
Gravimetric Determination of Sulfur as Barium Sulfate

I. Introduction:

A sample containing an alkali sulfate is dried, weighed and dissolved in dilute HCl. Barium chloride solution
is added in excess to precipitate barium sulfate, and the precipitate is digested in the hot solution. The
precipitate is filtered through a paper filter which is then ignited and completely ashed. From the weight of
the sample and weight of the precipitate, the percentage of sulfate in the sample is calculated. The
precipitation reaction is the following:

Ba2+(aq)+SO2−4(aq)→BaSO4(s)(1)(1)Ba2+(aq)+SO42−(aq)→BaSO4(s)

Variations in the acidity, temperature, manner of addition of the precipitant and time of digestion markedly
affect the filterability of the barium sulfate precipitate and the extent to which various foreign ions are
coprecipitated. Foreign anions such as nitrate, chlorate and chloride are coprecipitated as their barium salts,
and the ignited precipitate contains the salt or oxide as an additive impurity. The coprecipitation of chloride
can be decreased by slow addition of the precipitant. Since nitrate and chlorate interfere even at low
concentrations, they should be removed from the solution before precipitation.

Foreign cations such as ferric iron, calcium and, to a lesser extent, the alkali metals are coprecipitated as the
sulfates. These are substitutional impurities, and the magnitude of the error depends upon the differences
between the weight of the foreign sulfate or oxide and the weight of an equivalent amount of barium sulfate.

II. Objectives
 To be able to compute for the amount of Sulfur as %SO3

III. Materials
 Concentrated Hydrochloric Acid (6mL)  Cover glass
 0.05 M BaCl2  Analytical balance
 M AgNo3 (3 drops)  Weighing bottle
 Concentrated HNO3 (6 drops)  Beaker (499/600 mL)
 Crucible  Funnel
 Beaker  Filter paper
 Glass hooks

IV. Procedure:

Job 1: Preparation of Crucible

1. Remove dirt in crucible with Hydrochloric acid, wash with detergent solution and rinse well with
distilled water.
2. Dry the crucible in an oven at 110 C using a beaker, glass hooks and a cover glass for 1 hour.
3. Cool for 15-30 minutes in desiccator.
4. Weigh using the analytical balance.
5. Do 2 and 3 until constant weight of crucible is attained

Job 2: Preparation of 0.05 M BaCl2 solution.

1. Compute for the amount of BaCl2 (weight) using the equation.
𝑤𝑒𝑖𝑔ℎ𝑡 𝑥 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑊𝑒𝑖𝑔ℎ𝑡
M= 𝑣𝑜𝑙 (𝐿)
Weight BaCl2 = 2 H2O
= 0.05(0.100) (244.27)
= 1.22 grams
2. Weigh the computed amount of BaCl2 x H2O
3. Dissolve in distilled water
4. Dilute to 100 mL volumetric flask
5. Transfer to reagent bottle, label the bottle and set aside.

Job 3: Treatment of Sample

1. Using a marked weighing bottle, dry the sulfate containing sample in an oven at 110 C for at least 1
hour. Cool in a desiccator.
2. Weigh accurately 0.4-0.6 gram sample of unknown and put in a clean, 600 mL beaker.
3. Dissolve sample in 200-mL distilled water and 2 mL of concentrated hydrochloric acid and heat to near
boiling
4. In another beaker heat 100-mL of 0.05 M BaCl2 to near boiling and add it once with vigorous stirring to
the hot sample solution. Leave the stirring rod in the beaker.
5. With a clean watch glass, cover the beaker and heat to near boiling for 1 minute.
 6. While the solution are heating, put filter funnels with fine porosity ashless filter paper whattman#42
Schleicher and Schuell No. 598 or equivalent
7. Decant the hot supernate through the filter, wash the beaker 3 times with hot water for other
precipitate
8. Transfer precipitate in filter with 3 mL of hot H2O until the filtrate after, acidification with 2 drops
concentrated HNO3 gives only turbidity on addition of 0.1 AgNO3.
Job 4. Ignition
1. Remove the filter paper, fold and put inside the crucible. Char the paper, when no carbon remains,
ignite the precipitate for 20 minutes. Using the hottest flame possible with Mecker Burner.
2. Cool in desiccator at least 50 minutes and weigh. Repeat the ignition, sooling and weighing process
until constant weight (±0.50 mg) is achieved
3. Compute for the amount of sulfur as %SO3.

V. Data and Results:

TRIAL Weight of crucible with cover Weight of crucible with sample

1 37.7592 g 38.4147 g
2 37.7602 g 38.4123 g
3 37.7563 g 38.4127 g
4 37.7561 g 38.4139 g
5 37.7562 g 38.4127 g
6 37.7546 g 38.4141 g
7 37.7580 g 38.4141 g
8 37.7575 g
9 37.7575 g
Average

VI. Computation:

Weight of Sample (WS) = 0.4052 g

Average weight of crucible with cover=
Average weight of crucible with sample=

Find:
 Weight of BaSO4=
 %SO3

VII. Observation and Discussion

VIII. Conclusion:

IX. Guide Questions:

1. What is the chemical reaction when hydrochloric acid is added to the sample? Does this render the
sample more soluble or less soluble?
2. What is the purpose of digestion?
3. Why is the precipitate washed? Why is the silver nitrate used to test for completeness of washing?
4. What will happen if the wet precipitate and filter paper are washed over the burner too rapidly?

X. References: