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CHM 256: Basic Analytical Chemistry

Tutorial 6: Gravimetric Analysis


1. Define :
i. Gravimetric method
ii. Peptization
iii. Digestion process
iv. Precipitating agent
v. Supersaturation solution

2. Explain the difference between:


i. A colloidal and crystalline precipitate
ii. Precipitation and coprecipitation
iii. Precipitation methods and volatilisation methods

3. Justify the purpose of the following steps in gravimetric analysis


i. Digestion
ii. Filtration
iii. Washing
iv. Ignition

4. List the properties that are needed in a precipitation reagent


5. State 2 advantageous of using gravimetric analysis over volumetric analysis

6. Show a flowchart of the main step in carrying out the precipitation method in
gravimetric analysis.

7. Name four criteria of good precipitate.

8. Phosphate ion (PO43-) is determined by converting it into ammonium


phosphomolybdate (NH4)4PO4.12MoO3 (MW=1876.5) precipitate. If 0.2711 g sample
produced 1.1682 g of precipitate. Calculate the % of PO43-
Answer: 23.21%

9. An ore containing magnetite, Fe3O4, was analyzed by dissolving a 1.5419 g sample in


concentrated HCl, giving a mixture of Fe 2+ and Fe3+. After adding HNO3 to oxidize any
Fe2+ to Fe3+, the resulting solution was diluted with water and the Fe3+ precipitated as
Fe(OH)3 by adding NH3. After filtering and rinsing, the residue was ignited, giving
0.8525 g of pure Fe2O3. Calculate the % w/w Fe3O4 in the sample.
Answer: 53.4 %

10. In one gravimetric analysis to determine the % of Mn from the manganese ore,
0.6443g manganese ore was found to yield 0.4211 g Mn 3O4. Calculate the % of Mn in
the ore.
Answer: 47.09%

11. Name the analyte, precipitating reagent, precipitate and the form of product weighed
in the respective space below:

Analyte Precipitating agent Precipitate Product weighed


i) AgNO3 ii) AgCl
Na2SO4 iii) BaSO4 iv)
v) Aqueous NH3 vi) Fe2O3
Mg ? ? ?
Ca ? ? ?
CHM 256: Basic Analytical Chemistry
Tutorial 6: Gravimetric Analysis

12. 0.2560 g of an unknown compound containing chloride ions (CI) dissolved in water is
treated with excess NaCI solution. If the mass of the AgCI (rmm=143.32) precipitate
formed is 0.5367 g, what is the mass percent of CI (ram=35.45) in the original
unknown compound?

16. In a gravimetric analysis, 50.12 g sample of iron ore is analyzed for the iron (55.85 g
mol-1) content by precipitating it as Fe2O3 (159.68 g mol-1). After filtering, washing and
drying, the mass of precipitate was found to be 8.95 g.
a) Calculate the gravimetric factor of Fe.
b) Calculate the percentage of Fe in the iron ore.

17. A sample of 0.3220 g of an ionic compound containing the bromide ion, Br - (AW =
79.90) is dissolved in water and treated with an excess of AgNO 3. If the mass of the
AgBr (MW = 187.8) precipitate that formed is 0.6964 g, calculate the percentage by
mass of Br in the original compound.

18. Aluminium in an ore sample is determined by dissolving it and then precipitating with
base AI(OH)3 and igniting it to Al 2O3 which is then weighed. What is the mass of Al in
the sample if the ignited precipitate weighs 0.2385 grams?

19. Barium sulfate, BaSO4 is a salt that has a very low solubility in water. Explain how the
sulfate content in an aqueous solution can be determined by a gravimetric method
using BaCI2 solution as the precipitating reagent.

20. Pyrite ore (impure FeS2) is analysed by converting the sulfur to sulfate and
precipitating to BaSO4. Determine the percent FeS2 (MW = 119.977) in the sample if
2.5623 g pyrite ore produced 0.3987 g BaSO4 (233.40).

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