La Salle
Experiment no. 3
Buro, Emilio
Panabi, Katrina
ENCH1
Professor
02/13/2019
THEORETICAL FRAMEWORK
This experiment aims to determine the amount calcium as calcium oxalate present in an
unknown substance.
The amount of calcium in the sample can be determined through the use of gravimetric
It is however important that the oxalate-containing solution must be basic for the calcium
ion to react with it. In addition to, the resulting precipitate is soluble in the presence of acidic
solution because the oxalate anion is a weak base. Large relatively pure crystals that are easily
filtered will be obtained if the precipitation is carried out slowly. This can be done by dissolving
Ca2+ and C2O4 2- in acidic solution and gradually raising the pH by thermal decomposition of
urea. Thereby, making the solution basic and thus allowing the reaction to occur in conducive
condition. It is for this reason that a pH indicator will be used (in this experiment methyl red).
can now calculate the mass of calcium present in the unknown sample and thereafter its
oxalate.
Evaluate results using gravimetric methods and concentration formula
To develop dexterity in using laboratory equipment like analytical balance, volumetric
METHOD
Apparatus:
Funnel, 250-ml Erlenmeyer flask, 250-ml beaker, 25-ml volumetric flask, burners, watch
glass, tripod, dropper, wire gauze, digital balance, analytical balance, desiccator.
Materials:
Filter paper, urea, HCl, Ammonium Oxalate (20%), unknown solution, methyl red.
Procedures:
B.
250-mL beakers.
2. Add each with 75 mL of 0.1 M HCl.
3. To each of the above solutions add 5 drops of methyl red indicator solution. This
on a beaker.
8. Add 3ml of ice-cold water to beaker upon filtration. (Repeat process until all solids from
mass prior to the first weighing. If not, repeat process until constant mass is obtained.
Concentration refers to the amount of a substance per defined space. It is the quantity of
are to identify the concentration of calcium form calcium oxalate. Calcium is one of the alkaline-
earth metals of main Group 2 (IIa) of the periodic table. It is the most abundant metallic element
in the human body and the fifth most abundant element in the Earth's crust. Calcium does not
occur naturally in the free-state, but compounds of the element are widely distributed. On the
other hand, Calcium oxalate is calcium salt of oxalic acid with the chemical formula CaC 2O4. It is
a chemical compound that forms envelope shaped crystals, known in plants as raphides. A
solution because the oxalate anion is a weak base (and therefore protonated at acidic
pH). Large, easily filtered, relatively pure crystals of product will be obtained if the
precipitation is carried out slowly. Urea is added to the mixture and the solution is made
less acidic slowly by heating of the solution. Urea decomposes to produce OH -which
then deprotonates the oxalate. This ionic form of the ligand then combines to the
precipitate
Set-up 1 Set-up 2 Set-up 3
(Calcium Oxalate)
1st Heating 2.2044g 2.3597g 2.1875g
2nd Heating 2.0837g 2.2833g 2.1430g
3rd Heating 2.0838g 2.2833g 2.1430g
Set-up 1 2 3
The filter paper with precipitate was weighed after heating for one hour in an oven. It is
again heated for 1 hour and weighed. Results showed that the constant mass was not attained
in the second heating but in the third. It has a corresponding of 2.0838g, 2.3833g, and 2.1430g
Given the mass of the filter paper with the precipitate (calcium Oxalate) and the mass of
the filter paper alone, we can get the mass of calcium oxalate by subtracting the mass of the
filter paper from the mass of the filter paper with precipitate.
the gravimetric analyses is the precipitation; it is the method of separating the analyte from the
unknown sample as a precipitate wher it will be filtered and converted into a known composition
Set-up 1
FW Ca
=0.6275g CaC2O4・H2O ( )
FW CaC 2O 4 ・ H 2O
g
40.08
mol
=0.6275g CaC2O4・H2O ( )
g
146.07
mol
=0.1722 g Ca
1 mol
0.1722 g( )
M of Ca = 40.08 g
0.025 L
M of Ca = 0.1722 M
Set-up 2
FW Ca
=0.7693g CaC2O4・H2O ( )
FW CaC 2O 4 ・ H 2O
g
40.08
mol
=0.7693g CaC2O4・H2O ( )
g
146.07
mol
=0.2111 g Ca
1mol
0.2111( )
M of Ca = 40.08 g
0.025 L
M of Ca = 0.2111 M
Set-up 3
FW Ca
=0.6605g CaC2O4・H2O ( )
FW CaC 2O 4 ・ H 2O
g
40.08
mol
=0.6605g CaC2O4・H2O ( )
g
146.07
mol
=0.1812 g Ca
1 mol
0.1812( )
M of Ca = 40.08 g
0.025 L
M of Ca = 0.1812 M
Trial 1 2 3
Molarity, M 0.1722 0.2111 0.1812
The concentration of each trials are as follows:
As observed, the values are close to each other. However, the difference of 0.009-
0.0389 between the values is caused by the mass of the filter papers, which vary from one
another. Therefore, the average molarity of calcium in the three trials is:
0.1722+ 0.2111+0.1812
= 3
= 0.1882 M
CONCLUSION
The major objective of a precipitation reaction is the separation of a pure solid phase in a
compact and dense form which can be filtered easily. The importance of a small degree of
supersaturation has been so helpful, and it is for this reason that a dilute solution of a
precipitating agent is added slowly and with stirring. Several works have shown that water at
25 o C will dissolve 0.7 mg of calcium oxalate, but the same volume of dilute ammonium oxalate
solution dissolves only a negligible weight of the salt. The use of dilute ammonium for washing
the precipitate helps for higher yield of the calcium oxalate. The goal of this experiment is to
determine the concentration of calcium. It is possible by the presence of oxalate which reacts
As experimented, the result obtained proves that the experiment has reached its
objectives and has calculated the concentration of calcium. In this case, the students have
However, the little difference is subsequently rooted from variation of masses. As such,
Nevertheless, the students have successfully calculated the molarity of calcium using
REFERENCES
Retrieved from Daniel, C.H. (2010). Quantitative Chemical Analysis. 8 th edition, W.H Freeman
Retrieved from David, H. (200). Modern Analytical chemistry, McGraw companies, Inc; U.S.A,
analytical chemistry, 5thedition, Blackwell Science Ltd, U.K, February 10, 2019.
urine journal of the Roclcefeller Institute for Medical Research, February 10, 2019.
Analysis 5th edition, John Wiley and Sons Inc., New York, February 10, 2019.