Experiment 2
The sulfate content in a soluble sample can be found by precipitation of the slightly soluble BaSO4 according to the reaction: . This analysis illustrates procedures used for precipitating and washing an almost insoluble precipitate of very small crystals. The precipitate adsorbs many substances strongly but is not peptized by being washed with water. The method described in this experiment can also be used in the analysis of other sulfur-containing compounds by first converting S to SO42-.
Procedure A. Constant Weighing of the Crucibles a. Bring two porcelain crucibles to constant weight by heating to redness for 15 min over a burner (not including the cover; follow instructors demo of the setup) b. Cool the crucibles briefly on clean Al foil-covered wire gauze at room temperature for ~ 5 min and into the desiccator for 25 minutes. c. Weigh each crucible accurately on an analytical balance. Repeat procedure a and b until successive weighings agree within 0.3 mg. Be sure that all oxidizable substances on the entire surface of each crucible have been burned off. B. %SO3 Determination a. Dry the soluble sulfate sample at 100C for 1-2 hours, and cool in desiccators. Weigh out 0.5 0.7 g ( 0.1 mg) duplicate samples. Transfer to 800-mL beakers. Dissolve each in 200 mL of dist. H2O + 4 mL of 6M HCl. b. Precipitant is prepared by dissolving 1.3 g BaCl2 H2O in 100 mL water. Filter if solution is not perfectly clear. c. Heat the BaCl2 solution nearly to boiling, and then add the entire amount to the HOT sulfate sample solution while stirring vigorously. Wash stirring rod with distilled water and include washings in your final mixture.
Adamson University
Page 5
Clay Triangle
Guide Questions [1] What type of precipitate is BaSO4? [2] Why is a filter paper preferred over a sintered glass filter? [3] What made an ashless filter paper ashless? [4] Why is a porcelain crucible used in this procedure? [5] Why do we need to precipitate from a hot solution? [6] Why is the precipitating agent added all at once? [7] What is the purpose of adding 6M HCl in the sample solution? [8] Why do we need to test the washings with AgNO3? [9] What is ignition? [10] What is the product after the precipitate was ignited? [11] What are the advantages of performing ignition? [12] Cite the sources of errors for this experiment and how to circumvent these problems.
Adamson University
Page 7
Sample Data Sheet (You may devise your own on your logbook. Make sure that it presents your data in a CLEAN, LEGIBLE, COMPLETE, and TRUTHFUL manner).
A. Constant Weighing of Crucibles Crucible A Mass of Trial 1 Mass of Trial 2 Mass of Trial 3 Mass of Trial 4 Mass of Trial 5 Mass of Trial 6 Crucible B
B. Analysis of Sample Trial 1 Wt. of Sample (g) Wt. after ignition (g) %SO3 Mean %SO3 SD %RSD Trial 2
Adamson University
Page 8