University of St.

La Salle

Experiment no. 3

GRAVIMETRIC DETERMINATION OF CALCIUM AS CALCIUM OXALATE

Buro, Emilio

Magtunao, Maria Cassandra

Panabi, Katrina

Rivera, John Vincent

ENCH1

Engr. Rafael Diamante

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

analysis. In this experiment the Ca2+-containing sample will be scrutinized by allowing it to

precipitate using oxalate (C2O42-).

Ca2+(aq) + C2O42-(aq) + H2O (l)  CaC2O4.H2O(s)

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).

By experimentally obtaining the mass of calcium oxalate monohydrate (CaC2O4.H2O), we

can now calculate the mass of calcium present in the unknown sample and thereafter its

concentration expressed in its percent by mass.

Gravimetric Factor (GF) = Formula Weight Ca2+ / Formula Weight CaC2O4.H2O

Mass of Ca2+ = Mass of CaC2O4.H2O * GF

Molarity = moles solute / liters solution

OBJECTIVES

 To determine the concentration of calcium in a sample by precipitating the ion as calcium

oxalate.
 Evaluate results using gravimetric methods and concentration formula
 To develop dexterity in using laboratory equipment like analytical balance, volumetric

flask and desiccator

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:

A. For filter paper:

1. Get a filter paper and shape it in a funnel.

2. Contain the filter paper in an oven for 10-20 minutes.
3. Weigh and record data.

B.

1. Using a volumetric flask, transfer exactly 25 mL of unknown solution to each of three

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

indicator is red below pH 4.8 and yellow above pH 6.0.

4. Add ~25 mL of ammonium oxalate solution to each beaker while stirring with a glass rod.
5. Add ~15 g of solid urea to each sample.
6. Cover beaker with watch glass and boil gently until it reaches a shade of yellow.
 7. Filter each of the solution (preferably still hot but not boiling) using the heated filter paper

on a beaker.
8. Add 3ml of ice-cold water to beaker upon filtration. (Repeat process until all solids from

the beaker are transferred.

9. For the final washing, rinse each of the beaker with 2 10ml portions of ice-cold water and

pour the washings over the precipitate.

10. Dry precipitate in filter paper for 5 minutes, then in oven at 100C for 1 hour. Weigh.
(Note: In weighing, be sure not to touch the filter papers to avoid moisture and impurities

to the specimen. Use tongs.)

11. Heat again for 1 hour in oven, weigh, and record the mass. Be sure to obtain the same

mass prior to the first weighing. If not, repeat process until constant mass is obtained.

RESULTS AND DISCUSSION

Concentration refers to the amount of a substance per defined space. It is the quantity of

a solute that is contained in a particular quantity of solvent or solution. In this experiment, we

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

major constituent of human kidney stones is the calcium oxalate.

Calcium ion can be analyzed by precipitation with oxalate in a basic solution to

form calcium oxalate monohydrate (CaC 2O4.H2O).The calcium is soluble in acidic

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

calcium ion to form the precipitate.

Ca2+(aq) + C2O42- (aq) + H2O (l)→ CaC2O4・H2O (s)

Weight of filter with

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

Mass of filter with

precipitate (Calcium 2.0838g 2.2833g 2.1430g
Oxalate)
Mass of filter paper 1.4563g 1.5140g 1.4825g
 Mass of Calcium
Oxalate 0.6275g 0.7693g 0.6605g

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

for the first, second, and third filter papers, respectively.

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.

In obtaining the concentration of calcium, gravimetric methods shall be utilized. One of

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

that can be weighed to determine its mass.

Set-up 1

Camass = CaC2O4・H2Omass (Gf)

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

Camass = CaC2O4・H2Omass (Gf)

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

Camass = CaC2O4・H2Omass (Gf)

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

Concentration of Calcium = 0.2 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

with calcium ion and produces the calcium oxalate.

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

arrived at a result of 0.2 moles/liters or 0.2 M.

However, the little difference is subsequently rooted from variation of masses. As such,

there is always the possibility of inaccuracies with measurements, perception of measurement,

inaccuracies of equipment, and such errors.

Nevertheless, the students have successfully calculated the molarity of calcium using

gravimetric analysis and concentration formula.

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