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Laboratory Experiment

pubs.acs.org/jchemeduc

Following Precipitation Reactions with Conductivity Measurements


Zeynep Eslek and Aysen Tulpar*
Division of Chemistry, Dogus University, Istanbul 34722, Turkey
S Supporting Information
*

ABSTRACT: This general chemistry laboratory exercise is based on the analysis of


precipitation reactions via conductivity. In the rst part of the experiment, the aim is to
teach students how to prepare solutions from a solid (Na2CO3) and by dilution from a
stock solution [Cu(NO3)2]. In the second part of the experiment, the students use the
solutions to perform precipitation reactions: (1) Cu(NO3)2 (aq) + Na2CO3 (aq) and (2)
Cu(NO3)2 (aq) + 2 NaOH (aq). Observations are made on the appearance of the
solutions and the precipitates. Conductivities of the solutions are measured at each step of
the experiment. For the laboratory report, students perform stoichiometric calculations to
determine the theoretical conductivities of the reaction mixture. The students also
calculate hypothetical conductivities of the mixture in the case of no precipitation reaction
and compare them with the measured data. Most of the students conclude that the number
and concentration of free ions decrease during these precipitation reactions. Overall, the
students learn how to prepare solutions and gain experience in doing conductivity
measurements and stoichiometric calculations.
KEYWORDS: First-Year Undergraduate/General, Physical Chemistry, Laboratory Instruction, Collaborative/Cooperative Learning,
Hands-On Learning/Manipulatives, Aqueous Solution Chemistry, Conductivity, Precipitation/Solubility, Solutions/Solvents,
Stochiometry

solutions and the precipitates) before, during, and after


precipitation. After the lab, students perform stoichiometric
calculations to determine the concentration of species
remaining in solution after the precipitation reaction, and
using the appropriate molar conductivity values for those
species, they determine the theoretical conductivity of solutions
following the precipitation reaction. The students also predict
the conductivity of the reaction mixture if there were no
precipitation reaction, assuming that the conductivities are
additive. This analysis leads to the conclusion that the solution
conductivity decreases in these precipitation reactions.
Two precipitation reactions are studied

recipitation reactions have been used in general chemistry


laboratories1 to teach solubility rules,2 the stoichiometry of
reactions, and the concepts of the limiting reactant, percent
yield, and equilibrium.3 The commonly employed method for
quantitative investigation of precipitation reactions is to
determine the mass of dried precipitates. For cases where
drying time is a constraint, we oer a new approach for
investigating precipitation reactions via conductivity measurements. Conductivity measurements are ideal for studying
precipitation reactions as only the free ions in solution will
elicit a response.
Conductimetric titrations using precipitation reactions have
been used to determine the concentrations of species in
solution in general chemistry laboratories.4 The measured
conductivity minimum is used to determine the stoichiometric
point. However, there is no formal calculation of conductivity
of reaction mixtures in those experiments. We propose an
experiment that analyzes a single point on the titration curve
and provides a formal calculation of conductivity. Students
compare the conductivities of solutions before and after a
precipitation reaction using their conductivity data and their
calculated conductivity values. A drawback for conductivity
measurements may be the cost of providing an instrument for
each student pair.5 In our lab, a single portable conductivity
meter was used to perform all the measurements for 8 student
pairs.
There are two major aims of this experiment during the lab
period: (1) to teach students how to prepare solutions (from a
solid and by dilution from stock solution)6 and (2) to
encourage students to make observations (the color of
2013 American Chemical Society and
Division of Chemical Education, Inc.

Cu(NO3)2 (aq) + Na 2CO3(aq) 2NaNO3(aq) + CuCO3(s)


(1)

Cu(NO3)2 (aq) + 2NaOH(aq) 2NaNO3(aq) + Cu(OH)2 (s)


(2)

For the rst reaction, the amounts of the reactants are equal,
so the reaction is stoichiometric. For the second reaction,
Cu(NO3)2 is the limiting reagent.

PRELABORATORY EXERCISES
This is the rst experiment of the semester; therefore, one week
before this experiment, students go through a safety training
and watch a demonstration performed by the instructors in the
laboratory for a total of two hours. The details of the
prelaboratory exercises are explained elsewhere.6
Published: November 20, 2013
1668

dx.doi.org/10.1021/ed300594f | J. Chem. Educ. 2013, 90, 16681670

Journal of Chemical Education

Laboratory Experiment

EXPERIMENTAL PROCEDURE

also show the students a mixture for the reaction of eq 1 and a


mixture for the reaction of eq 2 that have been standing for 15
days so that they can observe the greenish CuCO37 and the
black CuO, respectively. The color of the solutions and the
precipitates is the most well liked part of the experiment.

Overview

This laboratory exercise takes two hours of laboratory time.


The students work in pairs. Each student pair prepares two
solutions at the same concentrationone Na2CO3 solution
from solid, one Cu(NO3)2 solution by dilution from 2.0 M
Cu(NO3)2 solutionand measures the conductivities of these
solutions before and after mixing the two solutions (eq 1). Each
student pair also mixes the Cu(NO3)2 solution with a 0.25 M
NaOH solution already prepared by the instructors (eq 2) and
measures the conductivity. All conductivity measurements are
normalized to a standard temperature of 25 C. Each student
uses his or her groups data and observations to turn in a formal
laboratory report in one week.

EXPERIMENTAL DATA AND ANALYSIS


The experimental conductivity data for the rst reaction (eq 1)
are listed in Table 1. For analysis, the students are asked to
Table 1. Experimental Conductivity Data for Na2CO3 and
Cu(NO3)2 Solutions and Their Mixture
Concentration/ M
0.020
0.040
0.060
0.080
0.100
0.120

Apparatus and Materials

Portable conductivity meter, balance (0.001g), volumetric


ask (100 mL), pipet (5 mL), graduated cylinder (50 mL),
pipet bulb, funnel, stirring rod, 5 beakers (100 mL), 0.25 M
sodium hydroxide (NaOH) solution, 2.0 M copper(II) nitrate
[Cu(NO3)2] solution, sodium carbonate (Na2CO3), and
deionized water.

Na2CO3/
(mS/cm)
4.1
7.3
10.0
13.1
14.9
17.8

0.5
0.4
0.3
0.7
0.5
0.3

Cu(NO3)2/
(mS/cm)
3.3
6.3
9.4
13.2
14.1
17.0

0.1
0.4
0.2
1.0
0.5
0.2

after rxn/
(mS/cm)
2.2
4.1
5.8
7.6
9.3
11.4

0.1
0.2
0.1
0.2
0.4
0.3

compare their experimental conductivity data of the reaction


mixture with the theoretically determined values. Only the ions
from NaNO3 contribute to conductivity. The theoretical
conductivity of the reaction mixture is determined by the
product of the molar conductivity of NaNO3 [98 mS/(cm M)]
and the molarity of NaNO3 at the end of the reaction. This
conductivity, , is calculated for the whole range of
concentrations by eq 3

Preparation of Solutions

Each student group is asked to calculate the mass (in grams) of


solid Na2CO3 to be weighed out to prepare 100 mL of one of
the following solutions: 0.0200, 0.0400, 0.0600, 0.0800, 0.1000,
and 0.1200 M Na2CO3. Each student group is also asked to
calculate the volume (in milliliters) of the stock 2.0 M
Cu(NO3)2 solution needed to prepare 100 mL of one of the
following solutions: 0.020, 0.040, 0.060, 0.080, 0.10, and 0.12 M
Cu(NO3)2. Students follow the procedures in the laboratory
handout to prepare the solutions in 100 mL volumetric asks
and measure the conductivity of the resulting solution using the
conductivity meter.

= 98

mS
[NaNO3]
cm M

(3)

Equation 3 assumes that conductivity of NaNO3 is directly


proportional to concentration and, therefore, the molar
conductivity is constant within the concentration range of the
experiment.
The molarity of NaNO3 in eq 3 is determined using
stoichiometric calculations as shown in eq 4

Precipitation Reactions

Students mix 40 mL of Cu(NO3)2 solution with 40 mL of


Na2CO3 solution in a 100 mL beaker and measure the
conductivity of the resulting mixture. Students also mix 40 mL
of Cu(NO3)2 solution with 40 mL of 0.25 M NaOH solution
and measure the conductivity of the resulting mixture. The
NaOH solution is readily available for students in order to save
time.

[NaNO3] =

HAZARDS
Skin protection is necessary while using NaOH and Cu(NO3)2
solutions. Sodium hydroxide is caustic and causes burns to any
area of contact. Leftover Cu(NO3)2 solutions and all mixtures
are collected in waste containers at the end of the experiment.
The Cu(NO3)2 solution is precipitated using Na2CO3 and
reused for other purposes. The mixtures are ltered and the
solid is collected for reuse for other purposes. Leftover
solutions of NaOH and Na2CO3 go down the drain.

[Cu(NO3)2 ] VCu(NO3)2 2
VCu(NO3)2 + VNa 2CO3
[Na 2CO3] VNa 2CO3 2
VCu(NO3)2 + VNa 2CO3

(4)

where the values of [Cu(NO3)2] and [Na2CO3] are dierent


for each student group and are listed in Table 1 in the
concentration column, the factor 2 is the stoichiometric
coecient of NaNO3 in eq 1, and VCu(NO3)2 and VNa2CO3 are
the volumes of Cu(NO3)2 and Na2CO3 solutions, respectively,
each being equal to 40 mL.
The students also calculate a hypothetical conductivity value
for the mixture if there were no precipitation reaction. They use
their measured conductivity values for Cu(NO3)2 and Na2CO3
solutions and assume that the conductivity is directly
proportional to concentration and is additive (eq 5)
Cu(NO3)2
Na 2CO3
=
+
(5)
2
2
The same amount of each solution (40 mL) is used, so the
molarity of each compound decreases by half in the nal
mixture. Because conductivity is directly proportional to

OBSERVATIONS
Students are asked to note down the color of the solutions and
the precipitates. For the preparation of Cu(NO3)2 solutions by
dilution of 2.0 M Cu(NO3)2, the students are expected to
notice the eect of dilution on the color of Cu(NO3)2 solution.
For precipitation reactions of eq 1 and eq 2, the students can
clearly see the turquoise color of solid CuCO3 and the blue
Cu(OH)2, respectively, and the remaining clear solution. We
1669

dx.doi.org/10.1021/ed300594f | J. Chem. Educ. 2013, 90, 16681670

Journal of Chemical Education

Laboratory Experiment

column, the factor 2 is the stoichiometric coecient of NaOH


in eq 2, and VCu(NO3)2 and VNaOH are the volumes Cu(NO3)2
and NaOH solutions, respectively, each being equal to 40 mL.
The students use eq 5 to determine the hypothetical
conductivity of the mixture in the case of no precipitation
reaction, but this time, they replace Na2CO3 with NaOH.

concentration, the conductivity of each compound also


decreases by half, as seen in eq 5. Table 2 reports the
calculated conductivity in case of no precipitation reaction as eq
5.
Table 2. Comparison of the Experimental Conductivity Data
with the Calculated Values for Mixtures of Cu(NO3)2 and
Na2CO3 Solutions
Concentration/ M
0.020
0.040
0.060
0.080
0.100
0.120

after rxn/
(mS/cm)

Eq 3a/
(mS/cm)

Percent
Error (%)

2.0
3.9
5.9
7.8
9.8
11.8

10
5
2
3
5
3

2.2
4.1
5.8
7.6
9.3
11.4

0.1
0.2
0.1
0.2
0.4
0.3

DISCUSSION
Students discuss the possible sources of error in their lab
reports. Most of them mention the uncertainty of volume,
mass, and conductivity measurements. A few of them mention
the assumptions made during the theoretical determination of
conductivity values. The students also discuss the reason why
their calculated values from eq 5 are larger than the measured
conductivity data for the precipitation reactions. The answer of
80% of the students is that the number of free ions decrease
during these precipitation reactions.

Eq 5b/
(mS/cm)
3.7
6.8
9.7
13.2
14.5
17.4

0.3
0.3
0.2
0.6
0.4
0.2

The calculated conductivity after the reaction. bThe calculated


conductivity in the case of no precipitation reaction.

SUMMARY
During the lab period, students learn how to prepare solutions,
and then by mixing these solutions, they observe precipitate
formation. The choice of the chemicals is such that colorful
precipitates form and the remaining solution is clear. To follow
the precipitation reactions, the conductivity of solutions is
measured before and after the reaction. While writing the lab
report, students learn to write and practice writing balanced
equations, to perform stoichiometric calculations, and to
calculate conductivity values for the reaction mixtures.

Table 3 shows both the theoretical and experimental


conductivity data for the mixture of Cu(NO3)2 and 0.25 M
Table 3. Comparison of the Experimental Conductivity Data
with the Calculated Values for Mixtures of Cu(NO3)2 and
0.25 M NaOH Solutions
Concentration/ M
0.020
0.040
0.060
0.080
0.100
0.120

after rxn/
(mS/cm)

Eq 6a/
(mS/cm)

Percent
Error (%)

24.2
21.9
19.7
17.4
15.1
12.8

4.1
3
12
5
9.3
2

25.2
22.5
22.1
18.3
16.5
13.0

0.4
1.0
0.9
1.3
1.8
0.8

Eq 5b/
(mS/cm)
28.2
29.7
31.2
33.1
33.6
35.0

1.0
1.0
1.0
1.1
1.0
1.0

* Supporting Information

Instructor notes and student handout. This material is available


via the Internet at http://pubs.acs.org.

The calculated conductivity after the reaction. bThe calculated


conductivity in the case of no precipitation reaction.

*Corresponding Author E-mail: atulpar@dogus.edu.tr.


Notes

The authors declare no competing nancial interest.

REFERENCES

(1) Ricci, R. W.; Ditzler, M. A. Discovery Chemistry: A LaboratoryCentered Approach to Teaching General Chemistry. J. Chem. Educ.
1991, 68, 228231.
(2) Blake, B. Solubility Rules: Three Suggestions for Improved
Understanding. J. Chem. Educ. 2003, 80, 13481350.
(3) DeMeo, S. Using Limiting-Excess Stoichiometry to Introduce
Equilibrium Calculations: A Discrepant Event Laboratory Activity
Involving Precipitation Reactions. J. Chem. Educ. 2002, 79, 474475.
(4) Randall, J. Advanced Chemistry with Vernier; Vernier Software &
Technology: Beaverton, OR, 2004; p 161.
(5) Baksa, K. Advanced Chemistry with Vernier (Jack Randall). J.
Chem. Educ. 2007, 84, 1611.
(6) Eslek, Z.; Tulpar, A. Solution Preparation and Conductivity
Measurements: An Experiment for Introductory Chemistry. J. Chem.
Educ. 2013, No. 10.1021/ed300593t.
(7) The students are asked where they have seen this compound in
daily life and some of them mentioned old copper Turkish coee pots
and some mentioned the Statue of Liberty.

53 mS
mS

[NaNO3] +
[NaOH]excess
0.25 cm M
cm M
(6)

The molarity of NaNO3 is determined using [Cu(NO3)2], as


shown in the rst half of eq 4, because Cu(NO3)2 is the limiting
reagent. The molarity of excess NaOH is calculated as
[NaOH]excess
=

AUTHOR INFORMATION

Corresponding Author

NaOH solutions. A solution of 0.25 M NaOH with a


conductivity of 53 2 mS/cm is used for the entire
concentration range of Cu(NO3)2 solutions. The students
determine the theoretical conductivity for the mixture by
accounting for the conductivities of NaNO3 and the excess
reagent NaOH, as seen in eq 6. The conductivity of NaNO3 is
determined by the product of the molar conductivity of NaNO3
[98 mS/(cm M)] and the molarity of NaNO 3 . The
conductivity of excess NaOH is determined by the product
of the molar conductivity of NaOH [(53/0.25) (mS cm1
M1)] and the molarity of excess NaOH.
= 98

ASSOCIATED CONTENT

[NaOH]initial VNaOH ([Cu(NO3)2 ] VCu(NO3)2) 2


VCu(NO3)2 + VNaOH
(7)

where [NaOH]initial is 0.25 M, [Cu(NO3)2] has a dierent value


for each group and is listed in Table 3 in the concentration
1670

dx.doi.org/10.1021/ed300594f | J. Chem. Educ. 2013, 90, 16681670

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