Experiment 7

Determining Stoichiometry of a Chemical Formula by

Complexation Titration
BASIC INFORMATION
In this experiment you will determine the empirical formula of a compound composed of only two
elements. The molecular formula of a compound reports the actual number of Formulae atoms
of each of the elements in a molecule of that compound. An empirical formula reduces that
molecular formula to a small, whole-number ratio of the atoms. A classic example of the difference
between these two kinds of formulae is that of glucose, C6H12O6: its empirical formula is found by
dividing the #atoms of each element by the common factor, 6, which gives CH2O.

TO REVIEW from LECTURE or TEXTBOOK and APPENDICES

Using volumetric glassware, including volumetric flask and burette titration
techniques using an indicator
Interrelationship between atomic and molecular mass, chemical formulae and
concentration units.

BACKGROUND INFORMATION
Chemical
Formulae

The molecular formula of a compound reports the actual number of

atoms of each of the elements in a molecule of that compound. An empirical
formula reduces that molecular formula to a small, whole-number ratio of the
atoms. A classic example of the difference between these two kinds of formulae
is that of glucose, C6H12O6: its empirical formula is found by dividing the #atoms
of each element by the common factor, 6, which gives CH2O.

Complexation
Titration

As with acid-base analysis, the concentration of a metal cation capable of

complexing with a ligand can be determined by titrating a measured mass
and thus, a known number of moles with a standardized titrant; the equivalence
point is estimated by observing an indicator color change marking the titration
end-point.
Ligands are molecules or ions capable of donating a pair of unshared electrons
to a metal cation. In the experiment to be performed, a poly-protic weak acid,
ethylenediamine tetraacetic acid (EDTA) carries four negative charges (ie. 4
unshared electrons) when strong base has deprotonated all four acid groups at
a pH of 10; those electrons can interact with divalent cations like Mg2+, Ca2+
and Zn2+ to complex them. The following equation describes the reaction:
Ca2+(aq) + EDTA4-(aq) [CaEDTA2-](aq)
The indicator used is Eriochrome Black T (EBT); its structure includes a
SO3 group which interacts electrostatically with the free metal cation in
Page 1 of 10

solution. When chelated with the cation, or when acidified, it produces a PINK
RED solution. The addition of EDTA during the titration creates a competition
between the indicator and EDTA for the free metal cation; it is a competition
which EBT always loses. As a result, when all of the metal has been
complexed with EDTA, EBT is no longer chelated and it is free in the basic
conditions; its color under these conditions is BLUE.
The endpoint is observed as the red solution goes from red to purple to all
blue. A pictorial depiction of the color change sequence which will be observed
during the titration appears at
http://homepages.ius.edu/DSPURLOC/c121/week13.htm.

PROCEDURE
CAUTION: Wear departmentally approved safety goggles while doing this experiment
NOTE: Record all data in your lab notebook. Reproduce the Data Form at the
end of the experiment in the notebook. You will neatly copy that data onto
the sheet included in the protocol to submit with the report. Sloppy forms
with scratched-out data will not be graded.
Solution preparation and titration will be performed by a pair of students.
1. Each pair of students: Carefully clean and rinse a 100-mL volumetric flask and
two 50-mL burets, as described in Appendix B of the Reference Background
material found in Course Documents of the Blackboard course, finishing with
a rinse of deionized water.
2. Record the mass of a dry, clean watch glass to the maximum allowable
number of significant figures. Place ~0.2 grams of zinc chloride on the watch
glass and weigh and record the mass of them together. Place the watch glass
aside where it cannot be disturbed.
3. Tare an empty 50-mL beaker. Add ~0.29 -0.32 grams of zinc chloride;
carefully record the exact mass of the salt.
4. Dissolve the zinc chloride with ~10-20 mL distilled, deionized water.
Following the instructions in Appendix B4 of the Background Material,
carefully transfer all of the dissolved salt to the volumetric flask.
Use a squirt bottle filled with deionized water to add 10-mL samples to
the beaker to thoroughly rinse it.
Empty the rinse into the flask.
Repeat with two more small water rinses.
5. Use a 10-mL graduated cylinder to add 10 mL of 0.1 M HCl to the flask.
Then fill the flask to the volume marker with distilled water, being
careful to add the last few drops one at a time using a disposable
pipette.
Page 2 of 10

Stopper the flask, or cover with a piece of Parafilm; gently invert the
flask several times to thoroughly mix the solution.

6. Use a buret clamp to mount the burets; label one zinc chloride and the other
EDTA. Rinse each with a small amount of the appropriate solution; drain the
rinse out into a waste collection beaker. Repeat. Fill the buret until the
meniscus is at eye-level with its solution.
7. Record the initial volume of the zinc chloride solution, to the maximum number
of significant figures allowed (decide as a team on this value before beginning
titration).
Deliver 20-25 mL of the solution into a clean 125-mL Erlenmeyer
flask.
Record the final buret reading.
8. Use a clean, dry 10-mL graduated cylinder to transfer 2-mL of the pH 10 buffer
to the flask. Mix by swirling. Add 3 drops of EBT indicator to the solution; swirl
to mix.
9. Record the initial buret volume of EDTA.
Titrate the zinc chloride, adding 1-2 mL of EDTA at a time, until the
blue color appears at the point where the EDTA initially hits the
solution. At that point, begin adding the EDTA drop by drop.
After each addition, swirl to thoroughly mix.
When the solution turns blue with no evidence of either red or
purple color, the end-point has been reached. Record the final
buret volume.
Pour the reaction mixture into the designated waste container
10. Refill the burets. Perform at least two additional titrations, repeating steps 7-9.
11. Reweigh the watch glass and zinc chloride which had been placed aside.
Record any changes in the appearance of the zinc chloride.
12. Drain the solutions out of the burets into a collection beaker. Rinse with three
samples of water, draining them after each rinse. Refill with distilled water.

Page 3 of 10

Page 4 of 10

Name ____________________________ Sec# ______ Lab TA __________________

Teammates ____________________________________________________________

EXP 7 DATA: DETERMINING the STOICHIOMETRY of an CHEMICAL FORMULA

Mass of watch glass, g

___________________

Mass of watch glass plus zinc chloride, g

(Start of lab)

___________________

Mass of watch glass plus zinc chloride, g

(End of lab)

___________________

OBSERVATIONS: Report changes in the appearance of the zinc chloride:

Mass of zinc chloride weighed out , g

__________________

Volumetric flask volume (total volume of zinc chloride

solution prepared), mL

__________________

Concentration of EDTA solution used, mol/L

__________________

TITRATION DATA:

Titration Trial #
1
2
3
4

Initial volume zinc chloride, mL

_________

__________

_________

__________

Final volume zinc chloride, mL

_________

__________

_________

__________

Initial volume EDTA, mL

_________

__________

_________

__________

Final volume EDTA, mL

_________

__________

_________

__________
Page 5 of 10

Page 6 of 10

Name __________________________________

Date _________________________

Teammates___________________________

Sec # ____ Lab TA _____________

____________________________________

Grade:

____________ + ______________ + _______________

Report (25 pts)
Pre-lab (10 pts)
Data sheet (5 pts)

______________ (40 pts)

The report is to be completed individually. While based on team discussion with teammates, the
answers given must be written in full sentences, in your own words, in ink.
Honor Pledge: I pledge, on my honor, that I have neither given, nor received, any unauthorized
assistance on this assignment. Signed: ___________________________________________

RESULTS SHEET

Titration Trial #
1
2
3
4

Volume zinc chloride sample, mL

_________

_________

_________

__________

Mass zinc chloride in the sample, g

_________

_________

_________

__________

Volume EDTA used in titration, mL

_________

_________

_________

__________

# moles EDTA used, mol

_________

_________

_________

__________

Mass Zn in titrated sample, g

_________

_________

_________

__________

Mass Cl in sample, g

_________

_________

_________

__________

#moles Cl in titrated sample, mol

_________

_________

_________

__________

Molar ratio Zn:Cl in zinc chloride

_________

_________

_________

__________

2+

Empirical formula zinc chloride

____________________

Page 7 of 10

CALCULATIONS:
Present a model calculation for each of the quantities required in the RESULTS Table. Consider
the following approaches to each:

Mass of zinc chloride in titrated sample:

[(sample zinc chloride weighed out)/(volume of zinc chloride soln prepared)] x (volume zinc chloride
soln titrated)

Volume EDTA used in the titration, mL =

Mass zinc in the titrated sample, g =

moles zinc =

moles EDTA =

vol final

- vol initial

# moles zinc
;
atomic mass zinc

moles EDTA used in titration

EDTA volume x [EDTA]

Mass chlorine in titrated sample, g = mass zinc chloride sample -

Moles chlorine

Molar ratio =

mass zinc

mass chlorine
atomic mass chlorine

(moles Zn / moles Cl)

Empirical formula

moles Zn : moles Cl

Page 8 of 10

INTERPRETATION OF RESULTS:
1. Consider the experimental protocol: Why did you make a known volume of solution containing
a known mass of zinc chloride and analyze multiple known volume samples of it? Specifically,
would results (the molar ratio of the elements) have been more accurate, if three separate
mass samples of zinc chloride were titrated? Explain your answer.

2. Zinc chloride absorbs water from the atmosphere.

a. Describe any experimental evidence you have which supports this statement.

b. If the mass sample of zinc chloride used to make the 100.0 mL of solution had absorbed
water after it was removed from the dessicator but before it was weighed and dissolved in
the final volume, what would be the effect on the number of moles of zinc determined by
the titration (higher? lower? the same?)? Explain your choice.

c. What would be the consequent effect on the mass of chlorine assumed to have been in
the titrated sample? Explain. As a result, would the determined molar ratio be less than,
equal to, or larger than the actual ratio?

Page 9 of 10

2. Hard water contains relatively high concentrations of Mg2+ and Ca2+, both of which are also
complexed by EDTA. You were instructed to dilute the mass of zinc chloride which was
analyzed with deionized (ion-free), distilled water. If you had used hard tap water instead:
a. Would the volume of EDTA needed to perform the titration been changed? If so,
how?

b. How would the calculated mass of zinc in the sample been affected? Explain your
answer.

c. What effect would that have had on the calculated mass of chlorine in the sample?
Explain.

d. As a result of the answers above, how would the determined empirical formula
compare to the real formula? Explain.

Page 10 of 10