Andrew Major

CHMY 151
Wed. 3:30
Lab Report 1
Title: Gravimetric Determination of Calcium as CaC2O4H2O
Purpose: To empirically determine the percent mass of calcium in an unknown sample of calcium
carbonate (CaCO3) through formation of CaC2O4 .
Procedure:
1. Place a 400ml beaker, two filter crucibles, and weigh vial of calcium carbonate in oven.
2. Remove from oven after 1 week.
3. Mass two 250 ml beakers. Record in Data.
4. Mass two filter crucibles once cooled. Record in Data.
5. Mass between .4 and .6 g of calcium carbonate (may be less than .4 but not more than .6g).
6. Add calcium carbonate to each beaker. Record mass of beaker + sample in Data.
7. Add 25 ml of .45 mol HCl to each beaker while stirring with a glass stirring rod.
8. Add 75 ml of .75 mol HCl to each beaker while stirring with a glass stirring rod.
9. Mass out 15g of urea.
10. Add about urea to each beaker while stirring with a glass stirring rod. Record actual amount in
Data.
11. Add 5 drops methyl red to each beaker and stir.
12. Place on hot plate and boil until the solution turns white (about 30 minutes).
13. Remove from hot plate and set on a paper towel at work station.
14. Allow precipitate to settle for a few minutes.
15. Prepare a 1000ml ice bath with DI water and ice in hallway.
16. Pour solution through filtering apparatus at station using the filter crucible and running water to
create suction.
17. Rinse beaker with cold water and filter until no particles of precipitate are left. Repeat for both
trials.
18. Place filter crucibles with CaC2O4H2O in 400ml beaker in oven.
19. Remove from oven after 1 week.
20. Find the mass of the crucibles with CaC2O4H2O. Record in Data.
21. Calculate percent mass of Ca in CaC2O4H2O. Record in Data.
22. Rinse crucibles in sink, and then place in H3NO3 bath. Clean up work area.

Data:
Trial 1:
Mass Beaker 1 (250ml) : 105.652 g
Mass Beaker 1 + CaCO3: 106.060 g

Mass Crucible 1
: 22.0565g
Mass Crucible 1 + CaC2O4 : 22.554 g

Mass Sample CaCO3

Mass Urea (NH2)2CO

:
.408 g
: 14.9989g

Mass Sample CaC2O4H2O : .4975g

Percent Calcium (Ca)
: 27.43%

Mass Beaker 2 (400ml) : 141.704 g

Mass Beaker 2 + CaCO3: 142.007 g

Mass Crucible 2
: 22.1022g
Mass Crucible 2 + CaC2O4 : 22.552 g

Mass Sample CaCO3

Mass Urea (NH2)2CO

Mass Sample CaC2O4H2O : .4498g

Percent Calcium (Ca)
: 27.43%

Trial 2:

:
.373 g
: 15.0017g

Calculations:
Trial 1:
Molar Mass CaC2O4: 146.1 g/mol

Molar Mass Ca

: 40.078g/mol

Mass Sample CaC2O4H2O? / MM of CaC2O4H2O x MM Ca = Mass Ca

.4975g / 146.1g/mol x 40.078g/mol = .1360 g Ca
Mass Calcium / Mass Sample CaC2O4H2O = Percent mass Ca
.1360g / .4975g x 100 = 27.43%
Trial 2:
Molar Mass CaC2O4: 146.1 g/mol

Molar Mass Ca

: 40.078g/mol

Mass Sample CaC2O4H2O? / MM of CaC2O4H2O x MM Ca = Mass Ca

.4498g / 146.1g/mol x 40.078g/mol = .1230 g Ca
Mass Calcium / Mass Sample CaC2O4H2O = Percent mass Ca
.1230g / .4498g x 100 = 27.43%

Conclusion: Using lot #146 of calcium carbonate, we found through the reaction between calcium
carbonate, hydrochloric acid and urea to produce calcium oxalate that the unknown sample was 27.43%
calcium for both trials. Our precision was exact to well over the billionth place based on our strict
attention to procedure and accuracy of measurement. Possible sources of error in this procedure
include incomplete filtration of the solution after boiling, inaccurate measurement, or incomplete
reaction on hot plate.