Abstract

Gravimetric analysis is a quantitative method focused on identifying the weight of a pure

compound from the analyte being tested. The objectives of this experiment are to be familiar
with the different methods of gravimetric analysis and to determine the Calcium weight in the
unknown sample of calcium oxalate dihydrate (CaC2O42H2O). Precipitation gravimetry was used
to determine the pure calcium from the precipitate. It includes the conversion of analyte into a
sparingly soluble precipitate, and this shall be filtered, washed free of impurities, and suitably
heated to convert it into a product with a known composition. Upon doing this process, the
recorded weights of the precipitate were 2.7029 g, 2.1400 g, and 2.3613 g. With the use of
stoichiometry, the results obtained for the calcium weight were 0.8457 g, 0.6695 g, and 0.7388 g.
Keywords: gravimetric analysis; precipitation; precipitate; drying; calcium; percent weight

Introduction
Gravimetric analyses are methods of
analyzing substances based on
measurement of mass. There are different
types of gravimetric methods including
volatilization gravimetry, electrogravimetry,
and precipitation gravimetry.
Volatilization gravimetry is a method
wherein the analyte, through the conversion
of gas into a known compound, is isolated
from other substances of the sample. The
gas mass is the analyte concentration’s
measure.
Electrogravimetry is a method that
uses deposition on an electrode by the means
of electric current in order to isolate the
analyte. The analyte concentration is based
the on the mass of this product.
Precipitation gravimetry includes the
conversion of analyte into a sparingly
soluble precipitate, and this shall be filtered,
washed free of impurities, and suitably
heated to convert it into a product with a
known composition. Precipitation
gravimetric analysis was used to determine
the calcium component of calcium oxalate
dihydrate (CaC2O42H2O). The excess oxalic
acid, H2C2O4, is added to the sample.
Ammonia which is added to the sample
caused the calcium to precipitate as
CaC2O42H2O.
2−¿→C 2 O4 2 H 2 O (g) ¿
Ca2+¿+C O2 4 ¿

Oxalate ion is a weak base, making
the calcium oxalate dihydrate soluble to
acidic solutions. If the process
precipitation is slowly done, the product
obtained would be large relatively pure
crystals that are easily filtered. This is
+2 -2
carried out by dissolving Ca and C2O4 in
an acidic solution and increasing the pH
gradually by the urea thermal composition.
The precipitated component will
collected from the filter paper, which should
be weighed beforehand, and then dried with
heat ranging from 103C to 110C.
a) Drying to a Constant Weight
Solids have properties that absorb
moisture because of its somewhat
affinity to water. This property is
called hygroscopic. Another
property, called deliquescent, is a
characteristic of a substance to
absorb too much water, transform
into a concentrated solution as it
completely dissolves in the mixture.
Hygroscopic and deliquescent
substances will continue to add up its
weight as it continues to be exposed
to air. As a solution, some methods
require the analyte to dry to a
constant weight and remove the
absorbed moisture at some point.
Doing these are essential for
gravimetric analyses of compounds.
First, the sample is dried in an oven
of with a temperature of 103C to
110C for 1 hour. Then it is cooled
in a desiccator (room temperature),
and then it is weighed. The sample
will be reheated for 30 minutes, and
the process will be repeated again
until a difference of 0.3 mg from
be consecutive weight measurements
are achieved.
The precipitate will be converted to
calcium oxalate upon doing the
process:
CaC 2 O 4 ∙ 2 H 2 O →Ca C2 O 4 ( s) +2 H 2 O
Methodology
The objectives of this experiment are
to be familiar with the different methods of
gravimetric analysis and to determine the
Calcium weight in the unknown sample of
calcium oxalate dihydrate (CaC2O42H2O).
The researchers used the following materials
to execute the experiment: 0.1M HCl
solution, Ammonium oxalate, distilled
water, filter paper, methyl red indicator urea,
25-mL volumetric pipette, 250-mL beaker,
analytical balance, desiccator, glass funnel
and support, glass rod, hot plate, oven, petri dish + filter
paper, g
dish, suction bulb, and watch glass. Weight of 2.7029 2.1400 2.3613
CaC2O4
precipitate, g
For the determination of calcium as Weight of Ca in 0.8457 0.6695 0.7388
CaC2O4
calcium oxalate, rinse first the 25-mL pipette precipitate, g
Average
with small portions of the unknown and weight of Ca in 0.7513
discard the washings. Then, transfer 25 mL CaC2O4
precipitate, g
of unknown to three 250-mL beakers. Dilute
each with 75 mL of 0.1M HCl solution. Calculations
Next, add five drops of methyl red indicator, 1. Average Weight of CaC2O4
then add 25 mL of ammonium oxalate Trial 1
(NH4)2C2O4 while stirring with a glass rod, 2.7361+2.6940+ 2.6785
Average weight of CaC 2 O 4 = =2.70
and add 15g of solid urea to the sample. 3

Cover the beakers with a watch glass and

then heat the water for 30 minutes until the Trial 2

indicator turns yellow. Filter each boiled 1.9072+2.1406+ 2.3722

Average weight of CaC 2 O 4 = =2.14
3
solution through a funnel. After that, add
around 3 mL of ice-cold water to the beakers
Trial 3
and use a rubber policeman to scrape off and
2.6712+2.0074 +2.4054
transfer the remaining solid. Repeat this step Average weight of CaC 2 O 4 = =2.36
3
until all the precipitate has been transferred.
Transfer the precipitate that was filtered, 2. Weight of Ca in CaC2O4 precipitate
into a dried petri dish. Dry in an oven for an CaC2O4 (MW) = 128.097g/mol
hour, cool it down in the desiccator for 30 Ca (MW) = 40.078g/mol
minutes, and then weigh. Trial 1
1 mol CaC 2 O 4 1 mol Ca 40.078
2.7029 gCa C 2 O 4 × × ×
Results 128.097 g 1mol Ca C 2 O 4 1 mol C
Table 1. Determination of Calcium in a Sample
Sample No. Trial 1 Trial 2 Trial 3
Volume of 25 mL 25 mL 25 mL Trial 2
sample 1 mol CaC 2 O4 1 mol Ca 40.078
analyzed, mL 2.1400 g CaC 2 O4 × × ×
Weight of petri 1.2609 1.2588 1.2589 128.097 g 1mol Ca C 2 O4 1 mol C
 Gravimetric methods are used to
Trial 3 separate the analyte by the use of
1 mol CaC 2 O4 1 mol Ca precipitation.
40.078 g The analyte detached from the
2.3613 gCa C 2 O 4 × × × =0.7388 g Ca
128.097 g 1mol Ca C 2 O 4 sample
1 mol Ca
and went through chemical reactions
resulted to the subtraction of the substance
3. Average weight of Ca in CaC2O4 in the precipitation. It is identified by paying
precipitate attention with the change in the weights. The
0.8457+ 0.6695+0.7388
Average weight= =0.7513 gsteps
Ca in gravimetric analysis are first, the
3
conversion of the analyte into a sparingly
soluble precipitate. Then, it is filtered,
Calculations for the percent of Ca in CaC2O4
washed free of impurities, and heated to
Trial 1
convert into a product of known
0.8457 g Ca
% Ca= ×100=31.29 % Ca composition. When conducting gravimetric
2.7029 g CaC 2 O 4
analysis, stoichiometry calculations were
Trial 2
performed.
0.6695 g Ca
% Ca= ×100=31.29 % Ca
2.1400 g CaC 2 O 4
Trial 3 In Table 1, the process of

0.7388 g Ca determining the calcium in the sample was

% Ca= ×100=31.29 % Ca
2.3613 g CaC 2 O 4 shown. There were three trials for this
experiment. Each beaker was poured with 25
Calculations for the uncertainty based on mL of the sample. The indicator was
95% confidence level: dropped into the samples, and then put into a

d 21+ d 22+ d 23 … boil. The sample was then filtered and the
Standard deviation=
√ n−1 precipitate in the filter paper was dried in the
oven. Each)2trial underwent three drying and
( 0.7513−0.8457 )2 + ( 0.7513−0.6695 )2 + ( 0.7513−0.7388
s . d=
√ 2
=0.0888
cooling procedures. The data of the first trial
were 2.7361 g, 2.6940 g, and 2.6785 g. The
zσ data for the second trial were 1.9072 g,
CI ()= x́ ±
√N 2.1406 g, and 2.3722 g. For the third trial,
(1.96)( 0.0888) the data were 2.6712 g, 2.0074 g, and 2.4054
¿ 0.7513 ± =0.7513 ± 0.1005
√3 g. The group has not yet finished the drying
Discussions
process due to the cancellations of classes Conclusion
because of the COVID-19 pandemic. These Gravimetric analysis is a quantitative
recorded data served as their basis for this method focused on identifying the weight of
experiment. Getting the average of each a pure compound from the analyte being
trial, the results were 2.7029 g, 2.1400 g, tested. There are different gravimetric
and 2.3613 g. Using stoichiometry methods: volatilization, electrogravimetry,
calculations, the weight of calcium from the and precipitation. Precipitation gravimetry is
precipitate was acquired. The calcium the method used in this experiment. The
weights attained were 0.8457 g, 0.6695 g, analyte was converted into a sparingly
and 0.7388 g. The average weight of the soluble precipitate, filtered, washed free
calcium was also computed. from contaminants, and heated to convert
The next calculations are for the into a product of known composition.
percent of calcium found in the calcium Stoichiometry calculations were conducted
oxalate. Each calcium weights were divided for gravimetric analysis.
to the weights of the precipitate. The answer
is then multiplied to 100 percent. The results With the use of stoichiometry,
were all 31.29% Ca for each trial. desirable calculations were obtained.
Results were achieved by using the ratio of
In calculating the uncertainty based the molar weight of the compound and the
on 95% confidence level, the z-value, acquired weight of the substance. Therefore,
standard deviation, and mean are needed. the weight measurements were calculated to
The standard deviation was computed first, be 0.8457 g, 0.6695 g, and 0.7388 g. The
and the mean (0.7513) and the z-value (1.96) percent weight of calcium in the calcium
were substituted in the equation. The result oxalate is 31.29%.
was 0.7513 ± 0.1005.
References
Holler, F. C. (2013). Fundamentals of Analytical Chemistry (9th ed.).
Medd, K. (2014, November 30). Gravimetric Stoichiometry Lesson. Retrieved from YouTube:
https://www.youtube.com/watch?v=LCqipyPtfcU
Experiment 1: Gravimetric Determination of Calcium. (n.d.).