Experiment No. 1 Gravimetric Determination of Calcium: Objectives

Experiment No.
1
Gravimetric Determination of Calcium
Objectives
1. To be familiar with the Gravimetric methods of analysis.

2. To determine the weight of Ca in the calcium oxalate dihydrate
[CaC2O4 2H2O] unknown sample.
Background
Gravimetric methods are based upon on the measurement of mass. Precipitation

and volatilization are the two major types of gravimetric methods.
Precipitation methods involve converting the analyte to a sparingly soluble

precipitate. The precipitate is then filtered, washed free of impurities and converted
to a product of known composition by suitable heat treatment.
In a precipitation method of determining Ca, an excess of oxalic acid, H2C2O4, is

added to a carefully measured volume of the sample. The addition of ammonia
causes all of the calcium in the sample to precipitate as CaC2O4∙2H2O.
Ca2+ + C2O42- ---- C2O4∙2H2O (g)
The precipitate is soluble in acidic solutions because oxalate ion is a weak base. Large,
easily filtered, relatively pure crystals of product will be obtained if the precipitation is
carried out slowly. This can be done by dissolving Ca+2 and C2O4-2 in acidic solution and
gradually raising the pH by the thermal decomposition of urea. The precipitated is
collected in a previously weighed ashless filter paper (folded properly to provide air
passage between the funnel and filter paper), drying through constant weight between
103oC to 110oC.
a. Drying to a Constant Weight
All solids have a certain affinity for water, and may absorb moisture from the
laboratory air. Reagents that readily pick up water are termed hygroscopic. Those
that absorb so much water that they will dissolve in it and form a concentrated solution
are called deliquescent (e.g., sodium hydroxide, trichloroacetic acid). These types of
substances will continually increase in weight while exposed to the air. For this
reason, many types of laboratory procedures require that a sample be dried to a
constant, reproducible weight (i.e., absorbed moisture removed to some standard,
Page 1of 3 Experiment 1 CM124-1L

low level). This is especially important for the gravimetric methods. Generally, the
sample is dried in a 103° C to 110° C oven for about 1 hour and allowed to cool to
room temperature in a desiccator. It is then weighed, and heated again for about 30
minutes. The sample is cooled and weighed a second time. The procedure is
repeated until successive weighings agree to within 0.3 mg.
This process converts the precipitate entirely to calcium oxalate represented by

the equation:
CaC2O4∙2H2O (s) --- CaC2O4 (s) + 2H2O (g)
The filter paper and precipitate are cooled and weighed and the mass of calcium
oxalate is determined by difference. The calcium content of the sample is then
computed using the appropriate gravimetric factors.
Reagents
0.1 M HCl solution Ammonium
oxalate
Distilled water (previously boiled and cooled) Filter
paper
Methyl red indicator Urea
Apparatus / Glassware
25-mL volumetric pipette

250-mL beaker Analytical
balance Desiccator
Funnel support
Glass funnel
Glass rod
Hotplate
Oven
Petridish
Suction bulb
Watch glass
PROCEDURE
1. Clean and oven-dry 1 pair of petridish.

2. Cool in a desiccator.
3. Weigh the filter paper.

Determination of calcium as calcium oxalate
1. Use a few of small portions of the unknown to rinse a 25-mL transfer

pipette and discard the washings.
2. Transfer exactly 25 mL duplicate portions of the unknown to a 250-mL
beaker and dilute with about 75 mL of 0.1 M HCl.
3. Add 5 drops of methyl red indicator. This indicator is red below a pH of
4.8 and yellow above a pH of 6.0.
4. Add about 25 mL of ammonium oxalate solution to each beaker while
stirring with a glass rod. Be sure to rinse the rod before removing.
5. Add about 15 g of solid urea to the sample. Cover with a watch glass and
boil gently for 30 minutes until the indicator turns yellow.
6. Filter each hot solution through a funnel.
7. Add about 3 mL of ice cold water to the beaker and, using a rubber
policeman, transfer the remaining solid to the funnel.
8. Repeat this procedure with small portions of ice cold water until all of the
precipitate has been transferred.
9. Finally, use 10 mL portion of ice cold water to rinse each beaker and pour
the washings over the precipitate.
10. Transfer the filtered precipitate to the dried petridish and dry in an oven
set at 103oC to 110oC (follow the constant drying procedure stated above).
11. Cool down the petridish and place inside the dessicator for 30 minutes.
12. Immediately weigh the petridish with CaC2O4 precipitate.
13. Reheat again as prescribed in the constant drying procedure.
14. Calculate the weight of Ca in the CaC2O4 precipitate.
15. Calculate the mean weight of Ca and the uncertainty based on 95%
confidence level. Record in your notebook.
DATA SHEET
Sample No. Trial 1 Trial 2 Trial 3
Volume of sample analyzed, mL
Weight of petridish + filter paper, g
Weight of CaC2O4 precipitate, g
Weight of Ca in CaC2O4 precipitate, g

Average weight of Ca in
CaC2O4 precipitate, g

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Experiment No.

1. To be familiar with the Gravimetric methods of analysis.

Gravimetric methods are based upon on the measurement of mass. Precipitation

Precipitation methods involve converting the analyte to a sparingly soluble

In a precipitation method of determining Ca, an excess of oxalic acid, H2C2O4, is

Ca2+ + C2O42- ---- C2O4∙2H2O (g)

a. Drying to a Constant Weight

Page 1of 3 Experiment 1 CM124-1L

This process converts the precipitate entirely to calcium oxalate represented by

CaC2O4∙2H2O (s) --- CaC2O4 (s) + 2H2O (g)

25-mL volumetric pipette

1. Clean and oven-dry 1 pair of petridish.

Page 2of 3 Experiment 1 CM124-1L

1. Use a few of small portions of the unknown to rinse a 25-mL transfer

Sample No. Trial 1 Trial 2 Trial 3

Volume of sample analyzed, mL

Weight of petridish + filter paper, g

Weight of CaC2O4 precipitate, g

Weight of Ca in CaC2O4 precipitate, g

Page 3of 3 Experiment 1 CM124-1L

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