EXPERIMENT 2: GRAVIMETRIC ANALYSIS IN SOLUTION

OBJECTIVES
1. To understand the concept of gravimetric analysis.
2. To determine amount of analyte precipitate.
3. To predict the percentage of analyte precipitate.
INTRODUCTION
Gravimetric analysis, by definition, includes all methods of analysis in which the final
stage of the analysis involves weighing. Gravimetric analysis is one of the most
accurate and precise methods of macro quantitative analysis. In this process the
analyte is selectively converted to an insoluble form. The separated precipitate is dried
or ignited, possibly to another form, and is accurately weigh. From the weight of the
precipitate and knowledge of its chemical composition, the weight of analyte can be
calculated in the desired form.
EQUIPMENT/APPARATUS
1.

Concentrated HNO3

2.

Solid AgNO3

3.

Solid NaCl

4.

Buret

5.

Beaker

6.

Stirring rod

7.

Filter paper

8.

Porcelain crucibles

9.

Watch glass

10.

Magnetic stirrer

11.

Hot plate

12.

Weighing bottle

PROCEDURES
Precipitation
1. Weigh a sample solid sodium chloride of about 0.2 0.3 g into 400 mL beaker.
2. Dissolve the sample in distilled water and dilute to about 150 mL. Add about 0.5 mL
of concentrated nitric acid.
3. Calculate gram of silver nitrate powder needed to make 150 ml of 0.1 M silver nitrate
solution (Hint: use molecular weight AgNO 3). Then put the beaker of silver nitrate
solution onto the heater.
4. Heat the sample solution to boiling and with constant stirring, add an excess of 10% of
silver nitrate solution slowly until the coagulation process stop.
5. The stirring helps prevent bumping of the solution during heating and the danger of
loss of precipitate.
6. Let the precipitate settle and test for complete precipitation by carefully adding a few
drops of silver nitrate to the clear supernatant liquid. If more precipitate or a
cloudiness appears, add a few more milliliters silver nitrate solution, stir well, heat, let
the precipitate settle, and test again until precipitation complete.
7. Cover the beaker with aluminium foil and wait for the solution to cool off for about 1
hour.
Filtration and washing of the precipitate
8. Decant the solution, pouring the solution down a stirring rod. The precipitate should
be disturbed as little as possible.
9. To the precipitate in the beaker add about 25 mL of the wash solution, stir well, let the
precipitate settle, and decant the solution through the filter paper. Then, bring the
precipitate onto the filter and put into porcelain crucibles. Use small portions of the
wash solution for transfer.
Drying and weighing of the precipitate
10. Place the crucibles containing the precipitate in a covered beaker in the oven for 1 day
at 40 50 oC. Make sure you do not leave it more than 1 day.
11. Cool the crucibles in the desiccator, and weigh.

EXERCISES
1. Explain the function of wash solution (HNO3) during washing step.
2. Calculate the percentage of chloride in the sample.
3. How to obtain large precipitate during the experiment?