02-05-2016

Name: Alicia Kotek

Experiment: Gravimetric determination of Calcium in a Solid Sample
Procedure from: Chem 55 Lab Manual Spring 2016 (authors: Prof. Joseph J. Pesek, J. Neptune, R.
Terrill, Matyska-Pesek and M. Stephens), Page 19
Observations:
1. Take out crucibles from desiccator and place in the oven (1050C) at 10:39 AM.
2. Calculate how to prepare 0.1 M HCl from 3 M HCl solution.
M1V1 = M2V2
(3 M HCl)(V1) = (0.1 M HCl)(500 mL)
V1 = 16.66 mL HCl
Add approximately 50 mL of DI water into a 500 mL beaker. Then take approximately 16 or 17 mL of 3
M HCl and add it into the 500 mL beaker. Use DI water to fill the solution to the 500 mL mark on the
beaker. Now the 0.1 M HCl is prepared.
Dilute each of the three 250 mL beakers with approximately 75 mL of 0.1 M HCl (using a 100 mL
beaker).
3. Add 5 drops of methyl red indicator in each of the three beakers. This indicator turned the solution in
the beakers a pink color.
4. Add approximately 25 mL of ammonium oxalate solution (using a 100 mL beaker) to the three beakers
containing the indicator and solution while stirring with a clean glass rod (use separate rod for each
beaker). Once done stirring, do not remove glass rod from beaker since Dr. Matyska-Pesek suggested
not to (although lab manual called for removing rod and rinsing it with DI water).
5. Measure out approximately 15 g of solid urea into three small clean beakers and add it to the 3
beakers of solution, then cover each of the three beakers with a watch glass.
At 11:56 AM, boil the solution (three 250 mL beakers) on a hot plate for approximately 30 minutes until
the methyl red indicator turns the solution yellow.
6. While waiting for the indicator to turn yellow, crucibles were taken out of the oven at 11:59 AM. Then
the crucibles were cooled in the desiccators for 30 min.
7. Check the indicators in each beaker to see if they turned yellow. None of the beakers changed to
yellow, therefore while waiting, crucibles were taken out of desiccator and weighed out on the analytical
balance.

Data:
Crucible 1 Crucible 2 Crucible 3
21.8280 g 22.7294 g 21.1560 g
21.8279 g 22.7287 g 21.1559 g
Difference 0.1 Difference 0.1
Difference 0.7 mg
mg mg
Requirement: Requirement:
Requirement:
difference difference
difference <0.3mg
<0.3mg <0.3mg
Pass Fail Pass

8. At 12:16 PM, the indicator turned a light yellow color in beaker #2. Beaker #2 is taken off of the hot
plate. After 10 minutes later, the indicator turned a clear, light yellow in Beaker #3. It is taken off of the
hot plate. The last remaining indicator in beaker #1 was a light pink color and was taken off of the hot
plate since lab period was over.
The indicator in beaker #1 will be heated again next lab period. Beaker #2 and #3will be heated and will
be filtered while hot through a crucible (at constant mass) next lab period.

Date: 02-05-2016 Signature: