EXPERIMENT 2: GRAVIMETRIC ANALYSIS 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. Buret
2. Beaker
3. Stirring rod
4. Filter paper
5. Porcelain crucibles
6. Watch glass
7. Magnetic stirrer
8. Hot plate
9. Weighing bottle

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 PROCEDURES
Required PPE : Goggles/safety glass, Lab Coat, Shoes, Gloves
NO SEQUENCE OF STEPS POTENTIAL PREVENTATIVE
HAZARDS MEASURES
i Chemicals HNO3 : Corrosive i . Wear proper PPE
AgNO3 : oxidizer. May ii. Handle chemicals
Nitric acid (HNO3) (concentrated)
cause cyanosis carefully to avoid spillage
Silver nitrate (AgNO3) (solid)
NaCl : Irritant iii. Safety Briefing prior
Sodium chloride (NaCl) (solid)
start the class
iv. Use fume hood
1 Weigh a sample solid sodium chloride of i . Spillage i. Handle chemicals
about 0.2 – 0.3 g into 400 mL beaker. carefully to avoid spillage
ii. Wear proper PPE
2 Dissolve the sample in distilled water and i . Spillage i . Training on handling of
dilute to about 150 mL. ii. Hazardous chemical pipette
ii. Handle chemicals
Add about 0.5 mL of concentrated nitric carefully to avoid spillage
acid. iii. Wear proper PPE

3 Calculate gram of silver nitrate powder i . Spillage i. Handle chemicals

needed to make 150 ml of 0.1 M silver ii. Hazardous chemical carefully to avoid spillage
nitrate solution (Hint: use molecular weight ii. Wear proper PPE
AgNO3).

4 Heat the sample solution of sodium chloride i . Spillage i. Handle chemicals

with constant stirring. ii. Bumping/splash of carefully to avoid spillage
boiling solution ii. Wear proper PPE
Add an excess of 10% of silver nitrate iii. Wash thoroughly after
solution slowly into the sample solution handling
until the coagulation process stop. iv. Avoid facing too close to
hot beaker
5 The stirring helps prevent bumping of the i . Spillage i. Handle chemicals
solution during heating and the danger of carefully to avoid spillage
loss of precipitate. ii. Wear proper PPE
iii. Avoid facing too close to
hot beaker
6 Let the precipitate settle and test for i . Spillage i . Training on handling of
complete precipitation by carefully adding a ii. Hazardous chemical pipette / burette
few drops of silver nitrate to the clear ii. Handle chemicals
supernatant liquid. carefully to avoid spillage
iii. Wear proper PPE
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 Nil Nil
wait for the solution to cool off for about 1
hour.

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 Filtration and washing of the precipitate
8 Decant the solution, pouring the solution i . Spillage i. Handle chemicals
down a stirring rod. The precipitate should carefully to avoid spillage
be disturbed as little as possible. ii. Wear proper PPE

9 To the precipitate in the beaker add about i . Spillage i. Handle chemicals

25 mL of the wash solution, stir well, let the ii. Hazardous chemical carefully to avoid spillage
precipitate settle, and decant the solution ii. Wear proper PPE
through the filter paper. iii. Wash thoroughly after
handling
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 i. Hot surface area i. Wear proper PPE
precipitate in a covered beaker in the oven ii. Electrical shock
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 Nil Nil

weigh.

EXERCISE

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?