NAME: Sonia Najib

COURSE: CHEM 371, M/W Lab

EXPERIMENT: Gravimetric Determination of Calcium (as a

CaC2O4•H2O)
DATE OF LAB: 30th January 2013

INTRODUCTION

The purpose of this lab was to find the average molarity and average weight percent
of calcium in an unknown solid that was provided to students. The experiment also
exposed students to the gravimetric analysis technique that quantified the unknown
substance while keeping the students aware about the chemistry behind
crystallization and precipitation of the substance.

Gravimetric analysis is basically a method that helps scientists determine “the

amount of analyte through the measurement of mass” (Yoder, 2012). This method
is observable by crystallization or precipitation of the analyte. The experiment
aimed at making calcium precipitant in “large, easily filtered, relatively pure crystals
of product” by carrying out a slow precipitation. A slow precipitation indicates
“particle growth dominates over nucleation” (Harris, 2012).

MATERIALS

i. medium-porosity, sintered- vi. 25mL transfer pipet w/

glass funnels (3) rubber bulb
ii. Vial of Unknown #6 T/Th vii. 100mL volumetric flask
Exp #2 viii. glass rod w/ rubber
iii. Dessicator policeman
iv. Vacuum suction apparatus ix. microwave oven
v. Side-arm filter flask x. hot plate

PROCEDURE

i. Three sintered-glass funnels were cleaned and rinsed thoroughly before

usage.
TECHNIQUE: The funnels were, individually, placed on a side-arm filter
flask that was already attached to a vacuum suction apparatus via a thick
tube. The vacuum suction apparatus was checked to make sure that it
was working before performing the filtration. A beaker containing
distilled water was also prepared beforehand. Once everything was set
up, the vacuum was turned on, and the funnel was filled with the distilled
water. The distilled water passed through into the filter flask indicating
that the funnel was working well. Same test was done to the other two
funnels
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

ii. The funnels were dried by microwaving them using a 900-W kitchen
microwave oven provided in the lab. The funnels were dried in two
heating periods of 4 min and 2 min with 15mins of cooling down time in
between heating. The funnels were weighed on the electronic balance
after each 15min-cooling period, before the next round of heating period.
These steps stopped once the weights reach to a constant measurement
within 0.3mg. A dessicator was chosen to ensure that the funnels were
further dehydrated and was also used to store the funnels. Paper towels
were used to handle the funnels.
iii. A vial of solid CaCO3 unknown was provided to every student to make an
unknown solution. To make the solution, 1.5775g of the unknown were
weighed on the electrical balance (4 repetitive weighing) and transferred
into the calibrated 100mL volumetric flask. 3.8mL of 12M HCl was added
and the flask was filled up to the 100mL point with distilled water.
iv. A small portion of the unknown solution was used to rinse a 25mL
transfer pipet. The washings were discarded.
v. Exactly 25mL of unknown was transferred to three 250mL beakers.
vi. Each beaker was diluted with 75mL of 0.1M HCl.
vii. 5 drops of methyl red indicator was added to the each beaker.
viii. 25mL ammonium oxalate was added to each beaker while stirring with a
cleaned glass rod. The rod was removed and rinsed into the beaker with
small portions of distilled water.
ix. 15g of urea were added to each sample and each beaker was covered
with a watchglass, and boiled gently until the indicator turned pale
yellow.
x. Each solution was filtered through a weighed funnel using suction. 3mL of
ice-cold water was added to the beaker and a rubber policeman was used
to help transfer the remaining solid to the funnel. The procedure was
repeated with small portions of ice-cold water until all precipitate has
been transferred to the funnel. For the final rinsing, two portions of 10mL
ice-cold water were poured over the precipitate.
xi. The precipitate was dried with vacuum suction, and then dried in the
microwave exactly as in the beginning.
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

RESULTS

i. Data:

Funnel # 20 404 480

mass of empty sintered glass 20.808
funnel 20.929 3 20.5793
21.329
mass of funnel + samples 21.4553 1 21.097
difference/mass of CaC2O4•H2O 0.5263 0.5208 0.5177
0.1428
mass of Ca2+ in 25mL 0.14436 5 0.14200
wt% 0.58% 0.57% 0.57%

ii. Calculation to find the wt% of calcium in 25mL

Eg. Funnel #20

Density of water at 24C = 0.997296 g/ml
Mass of water at 24C = 24.9324 g

Mass of Ca2+ in 25mL

= Mass of CaC2O4•H2O x MM Ca2+/MM CaC2O4•H2O
= 0.5263g x (40.0784g/mol / 146.1130g/mol)
= 0.14436g

wt% = mass of Ca2+ in 25mL/mass of soln. x 100%

= 0.14436g/24.9324 g x 100%
= 0.57%

iii. Calculation to find the molarity of Ca2+ in 25mL

Eg. Funnel #20

# of moles of Ca2+
= Mass of CaC2O4•H2O/ MM CaC2O4•H2O = # of moles of CaC2O4•H2O
= 0.5263g/146.1130g/mol
= 0.003602 moles of CaC2O4•H2O
= 0.003602 moles of Ca2+

Molarity
= moles of Ca2+/L
= 0.003602/0.025L
= 0.1441 M
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

DISCUSSION

Based on the calculations method in the Result section, the wt% for the calcium
unknown # 6 for T/Th lab was 2.30%. One the other hand, the molarity of the
calcium unknown was 1.428M.
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

APPENDIX I
Raw Data

Empty taret
boat
Trial 1 1.5775
Trial 2 1.5761
Trial 3 1.5760
Trial 4 1.5760

Mass of sintered glass funnels (g)

Funnel
#20 Funnel # 404 Funnel # 480
20.9766 20.8575 20.5943
20.9293 20.8085 20.5799
20.9293 20.8079 20.5795
20.929 20.8083 20.5795
20.929 20.8083 20.5793

Mass of samples after being in the dessicator

~5days
Funnel #20 Funnel # 404 Funnel # 480
21.4553 21.3289 21.0959
21.4553 21.329 21.0958
21.4551 21.3293 21.0963
21.4556 21.3294 21.0966
21.4553 21.3291 21.0970

APPENDIX II
Mass of CaC2O4•H2O

Sintered-glass funnels 20 404 480

mass of empty funnel 20.929 20.8083 20.5793
mass of funnel + samples 21.4553 21.3291 21.0970
difference/mass of CaC2O4•H2O 0.5263 0.5208 0.5177
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

Finding wt % of Ca2+
Sintered-glass
funnels 20 404 480
Mass of Ca2+in 25mL 0.1444 0.1429 0.1420

Average mass 0.1431

Mass of Ca2+in 100mL 0.5723
wt% 2.30%

Finding Molarity of Ca2+

Sintered-glass funnels 20 404 480

#moles of Ca2+ 0.003602 0.003564 0.003543
Molarity 0.1441 0.1426 0.1417

Average Molarity 0.1428

Average #moles of Ca2+ 0.003570
Molarity of Ca2+ 1.428

APPENDIX III
 NAME: Sonia Najib
COURSE: CHEM 371, M/W Lab

SOURCES

Harris, D.C. (2013). Exploring Chemical Analysis 5th Edition. New York: W. H. Freeman
and company

Yoder, C. (2012). Wired chemist. Retrieved from

http://www.wiredchemist.com/chemistry/instructional/laboratory-
tutorials/gravimetric-analysis