CHEM 7L EXPERIMENT 1 Gravimetric Analysis Procedural Steps

Procedure 1. Prepare a desiccator for use

Procedure 2. a- Number three clean crucibles

Procedure 2. b- Add a filter paper to each crucible

Procedure 2. c- Place the crucibles in a 250- mL labeled beaker ready for the oven

Procedure 2. e- Let your crucibles cool for at least 30 minutes in the dessicator before weighing Procedure 2. d- TAs place all beakers with the crucibles on a designated rack in the oven for drying

Procedure 2. f- Weigh each of the cooled crucibles with filter paper

Procedure 3. Obtain a 25-mL aliquot of unknown solution

Procedure 4. a- Heat unknown sample to 70-80 C

Procedure 4. b- Add 8 mL of 8-hydroxyquinoline

c- Stir to redissolve the precipitate at the bottom of the beaker

d- Add 6M HCl to help redissolve the precipitate

e- No more precipitate!

Procedure 5. a- Add 2M NH4CH3COO drop-wise

b- Continue to add more 2M NH4CH3COO until the precipitate stops dissolving with stirring

c- Add an additional 20 mL of 2M NH4CH3COO to complete the precipitation

d- Parafilm your beaker and let the precipitate digest overnight in your 4 drawer

Stopper #6 with Stopper #6 with glass tubing glass tubing

Attach black hose to the vacuum line Attach black hose to the vacuum line

Crucible

For vacuum trap, use filtering flask # 5320

Vacuum adapter

Filtering flask with side arm

5 5

Procedure 6. Vacuum Filtration Setup

Procedure 6. a- Start the vacuum

Procedure 6. b- Set the filter paper in place by wetting it with DI water (vacuum is on)

All perforations must be covered at the bottom of the crucible and the filter paper must not be creased

Procedure 6. c- Add the solution to the ceramic crucible with pre-determined mass

Procedure 6. c- Use a stirring rod to guide the solution onto the filter paper

The filtrate in the filter flask should be clear (i.e., with no solid particles ) and light yellow in color

Procedure 6. d- Wash the beaker quantitatively with water, adding the wash to the crucible

Procedure 6. e- Filtration is done!

Procedure 6. f- Close the vacuum

Procedure 6. g- Take the crucible of the filter flask

Procedure 6. h- Place your crucibles in a 250 mL labeled beaker ready for the oven

TAs place all beakers with the crucibles on a designated rack in the oven for drying 7

Procedure 6. i- After drying , let your three crucibles with product cool for at least 30 minutes in the dessicator before weighing Procedure 6. j- Weigh each of the cooled crucibles with the product

You are now done !!!!!