Chemistry 109, York College/CUNY. Spring 2020.

Online Experiment #8: Percent Composition of Ca in a Salt by

Gravimetric Analysis

Introduction:

Gravimetric analysis is the use of mass measurements to find out some information about a
compound. For example, in this experiment, you will “perform” a precipitation reaction involving
calcium (Ca), and measure the mass of the solid precipitate. You are given a powder with an
“unknown” ionic calcium compound; ie we know the compound contains calcium, but the exact
composition of the powder is unknown. This can be represented as:

CaX y

where X is an anion (could be an element like Br or polyatomic ion like NO3) and y is the appropriate
subscript. Alternatively, we might know the identity of the calcium salt, but there are impurities in the
powder besides the calcium salt and we can figure out what proportion is calcium salt.

Calcium cation reacts with oxalate anion to produce a hydrated solid product. The net ionic equation
for the precipitation reaction is:

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

If we measure the mass of the solid CaC 2O4·H 2O, and determine the % of Ca by mass from the
empirical formula, then we can find out the mass of the just the Ca in the solid.

The amount of Ca in the solid product equals the mass of soluble calcium on the reactant side of the
equation. Therefore, if we know the total mass of CaXy (because we weighed it on a balance before
doing the reaction), and the mass of Ca (from the experiment), then we can determine the percent of
Ca by mass in CaXy . With some luck, we can go on to determine what X and y are, giving us the
identity (or purity) of the original unknown compound.

One reason why gravimetric analysis is useful is because mass is a quantity that is easy to measure
and very precise – for example, your analytical balance is very simple to operate, and gives you 3 or
4 decimal places of precision. This is way better than, say, a graduated cylinder or even a buret.

Procedure:

We will follow two students from another college, Josh and Dahlia, as they perform this experiment in
their class on Youtube. Before watching the video, please do the calculations on the following page.
You lab instructor might help you with these.
Preliminary calculations
A. Molecular weight of Calcium Oxalate Monohydrate
Fill in the following table to determine the MW of CaC 2O4·H2O
Element Atomic weight Weight of each element
Ca x1

C x2

O x5

H x2

Molecular
weight

B. Percent Ca in CaC2O4·H2O
Divide the atomic weight of calcium by the molecular weight of CaC2O4·H2O to determine the
percent of Ca:
Atomic Weight MW of Atomic Weight of Ca
of Ca CaC2O4·H2O MW of CaC2O4·H2O x 100 (to get %)

Video demonstration
The video can be found here: https://www.youtube.com/watch?v=R_ne_Vff0-Q. As you watch this video,
please pay specific attention to the information/activities that occur at the following times, and answer
questions where there is a fillable box:

C. At about 0:26 of the video, the students start making a “stock solution”. What is in this
solution, and what is its volume?

D. At about 2:43 of the video, Josh tells us what volume of solution they will use in each trial.
What is this volume? What fraction of total stock solution gets used in each trial?

E. Pay attention to the equation in the bottom line at about 4:13. This is important!

F. At about 4:30, why is Dahlia weighing the funnel, watchglass and weighing paper?
G. At about 6:10, Josh transfers the precipitate to the funnel, and he tells you to make sure to
rinse the beaker carefully. Think about *why* you need to do this. There will be a question
about this later in the lab.

H. At about 7:20, you get a good peek at Dahlia’s lab notebook. Transfer the important values to
your “lab notebook” here, and calculate an average mass of product
Mass of unknown:

Trial 1 Trial 2
Mass of Equipment

Mass of Equipment +
CaC2O4·H2O Product

Mass of
CaC2O4·H2O Product

Average Mass of ORDINARILY WE WOULD TAKE AN AVERAGE HERE,

CaC2O4·H2O Product BUT ONE OF THE LAB PARTNER #1 MESSED UP.
PROCEED USING DATA FROM TRIAL 2

I. Multiply the mass of product from trial 2 by the %Ca that you calculated above in part B to get
the average mass of Ca in 25 mL of unknown solution.

J. Multiply the value you obtained in step I by 4. This is the total mass of calcium in the stock
solution. What value do you get? Why do you multiply by 4?
Value Reason

K. Divide the value from step J by the mass of unknown to find the %Ca in the original sample!
This is your final answer! Congratulations! Does it make sense? Why or why not?

J. One more question to think about. What would happen to your answer in K if Josh did not rinse
the beaker enough?