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All Roads Lead to Rome: Triple Stoichiometry with a Lithium Battery

Violeta A. Martínez and Jorge G. Ibanez*
Cite This: J. Chem. Educ. 2020, 97, 4103−4107 Read Online

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ABSTRACT: This activity allows students to visualize how to obtain different stoichiometries
with various techniques in a single experiment. The involvement of three phases adds to the
See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

student’s interest. Instructional materials are provided to facilitate the experimental procedures,
interpretation of results, and error analysis. The reaction of Li from a Li battery with water inside
a syringe allows measurement of the gas evolved, the metal consumed, and the hydroxide
produced. Li batteries can be obtained for less than US $1.00. This report describes the
Downloaded via Jorge Ibanez on November 25, 2020 at 22:33:39 (UTC).

development of a 2 h activity that has been tested in whole or in part in various teacher
workshops in Mexico, Panama, El Salvador, and Thailand, and it has been implemented and
assessed in a general chemistry laboratory.

KEYWORDS: Stoichiometry, First-Year Undergraduate/General, Titration/Volumentric Analysis

■ INTRODUCTION
Stoichiometry is at the very heart of chemical education. To
• Use the atomic weight of an elemental reagent and its
weight loss after a reaction to calculate the number of
reinforce its concepts, experiments are continuously designed so reacting moles
that students can better understand molar ratios from a practical Alkali metal reactivity is well-known to attract students’
standpoint. For example, in the past decade, the Journal of attention. The classical example of adding a small piece of
Chemical Education published papers on the subject whereby the sodium metal to water with phenolphthalein has captivated
favorite techniques to ascertain stoichiometric relationships many generations.26,27 In spite of its relative safety when
included mainly colorimetry/spectrophotometry,1−6 conductiv- correctly performed, accidents do happen and must be
ity,7,8 electrochemistry,9−11 gravimetry,12−15 titrimetry,10,12 gas prevented.28−31 This reaction is even more dangerous when
generation,16−21 thermochemistry/thermal analysis,15,22−24 and using potassium metal.32−33 In the present experiment, such
catalysis.25 dangers are minimized by using lithium metal from a 3 V button-
We describe herein an experiment suitable for the general type battery whose reaction with water produces an easily
chemistry laboratory that combines three techniques: titrimetry, confined gas evolution. The reaction is
gas generation, and weight loss. This combination is aimed at
Li(s) + H 2O(l) → LiOH(aq) + 1/2H 2(g) (1)
finding an equation for the stoichiometry of the reaction
between an alkali metal and water. To add to the beauty of the When the reaction was performed inside a plastic syringe (of
experiment, the reaction involves three phases (solid, liquid, and at least 20 mL with 1 mL volume graduations hereby called the
gas). Parts of this experiment have been tested during teacher reaction chamber) equipped with a three-way valve, the number
workshops in Thailand, Panama, Mexico, and El Salvador, and in of moles of H2(g) produced by the reaction can be estimated by
full with two groups of chemical engineering general chemistry measuring the volume of gas produced and by using the ideal gas
students at the Universidad Centroamericana (53 and 20 law. At the same time, by weighing the portion of the battery
students, respectively, accounting for a total of 25 teams) that containing the Li before and after the experiment, the number of
completed the experimental procedure in an average of 2 h. participating moles of Li can be estimated. Last, by titrating the
The general objectives include resulting LiOH solution with normalized HCl, the number of
• Verify the stoichiometric relationships among species that
participate in a chemical reaction Received: June 29, 2020
Revised: August 19, 2020
• Perform a titration to determine the number of moles of Published: September 24, 2020
an aqueous product
• Use the ideal gas law to calculate the number of moles of a
gaseous product generated
© 2020 American Chemical Society and
Division of Chemical Education, Inc. https://dx.doi.org/10.1021/acs.jchemed.0c00876
4103 J. Chem. Educ. 2020, 97, 4103−4107
Journal of Chemical Education pubs.acs.org/jchemeduc Laboratory Experiment

moles of OH− produced can also be estimated. Results using the When it is time to initiate the experiment, open the valve
three techniques are discussed below. passage between the reaction chamber and the feed syringe and

■ EXPERIMENT
Li Preparation and Placement in the Reaction Chamber
slowly add 1 or 2 mL of water until it floods the lid containing Li.
The rapid production of hydrogen gas, through the displace-
ment of the plunger, and the color change of the indicator should
be observed. These observations together enforce the
Li metal is obtained from low-cost, readily available, small concurrent productions of H2(g) and OH−(aq). Add the
button-type Li batteries (e.g., of the CR1616-type that contains water in small increments until no more gas is produced. Then,
approximately 0.017 g of the metal) which are pried open with add the remaining water into the reaction chamber. Water is
pliers.34 See Figure 1a. Weigh only the half containing Li (hereby therefore in excess, and Li is the limiting reagent.
Hazards
Although we have opened several hundreds of Li batteries from
at least five brands without facing hazardous conditions, some
manufacturers state that they pose a risk of fire and can explode
or leak if disassembled. The Li batteries should be opened away
from water or aqueous solutions, and a fire extinguisher should
be available. LiOH and HCl are caustic and/or corrosive to
human tissue. Wear eye and body protection during the entire
experiment. By its titration with HCl, the LiOH solution
produced from the experiment is neutralized; the resulting LiCl
solution is of very low toxicity and can be disposed of according
to local regulations. Accidental use of a battery larger than what
is recommended may result in excessive gas production and the
violent release of the syringe plunger and the aqueous contents.
Hydrogen gas is produced during the experiment, and therefore,
Figure 1. Setting up the reaction chamber, three-way valve, and metal
the entire procedure must be performed away from fire or
lid with Li. sparks. If desired, the H2 gas produced by this experiment may
be transferred to a third syringe that can be connected to the
three-way valve and stored for further use, or else it can be
vented to the atmosphere away from students.
called the lid) with an analytical balance, record its mass, and Calculation of the Number of Moles of H2 Produced
then drop it inside the reaction chamber from which the plunger
had been previously removed (Figure 1b). Lubricate the outside When the reaction is over (i.e., gas production stops), record the
surface of the plunger’s tip with a small amount of silicone oil to position of the reaction chamber’s plunger. Compare this value
facilitate its displacement. Then, insert the plunger back into the to its initial value; the difference represents the volume of gas
syringe barrel of the reaction chamber to remove all the air produced, in milliliters. Using the ideal gas law, the temperature
contained in it, and fix a three-way valve (or stopcock, of the type of the liquid at the end of the reaction, and the local atmospheric
used in medical operations) at the bottom end, as shown in pressure, the number of moles of gas can be estimated. (An
Figure 1c. example of this computation is included in the Supporting
Information).
Reaction of Li with H2O
Calculation of the Number of LiOH Moles Produced
Draw 5.0 mL of deionized water (containing a few drops of
phenolphthalein) into a 10 mL feed syringe. Then, connect this Transfer the liquid remaining in the reaction chamber to the
feed syringe to the side end of the three-way valve described feed syringe. Close the reaction chamber with the three-way
above. See Figure 2. valve. Remove the feed syringe and transfer its liquid content to a
20 mL Erlenmeyer flask for titration. Measure its temperature
with a thermometer, and use it for the ideal gas law calculation
described earlier. An acid−base titration is now used to find out
the concentration of the LiOH generated, by its titration with a
0.600 M HCl solution according to the following reaction:

LiOH(aq) + HCl(aq) → LiCl(aq) + H 2O(l) (2)

A microtitration system is then assembled (for example, like

the one shown in Figure 3) by connecting a 10 mL feed syringe
filled with the HCl solution to a 1 mL syringe (e.g., insulin- or
tuberculin-type) through another 3-way valve. To increase the
precision by decreasing the diameter of the drops delivered,
insert a plastic automatic delivery pipet tip at the bottom end of
this titrating syringe.
Record the titrant volume delivered at the pink to transparent
Figure 2. Connection between the reaction chamber containing Li and end point, and from a 1:1 stoichiometry and a 0.600 M HCl
the feed syringe containing H2O. concentration, calculate the number of moles of LiOH titrated.
4104 https://dx.doi.org/10.1021/acs.jchemed.0c00876
J. Chem. Educ. 2020, 97, 4103−4107
Journal of Chemical Education pubs.acs.org/jchemeduc Laboratory Experiment

• The equipment used for gas and liquid volume measure-

ments is rather simple. In particular, the precision of the
20 mL plastic syringe is not expected to be high.
Upon completion of the lab session, the pedagogical
effectiveness was assessed with three tools: (a) a 30 min postlab
quiz (50% of the total grade), (b) a lab report (30% of the total
grade), and (c) a case study focused on the solution of a related
problem (20% of the total grade). The quiz was solved by the
same 2−3 member groups that performed the experiment and
consisted of using the experimental data to calculate the mol
LiOH/mol Li, mol H2/mol Li, and mol LiOH/mol H2 ratios.
For the report, the student groups were requested to submit a
document containing (a) an introduction to the principles of
stoichiometry, including the derivation of the main equations
needed for the lab calculations; (b) a description of the
methodology; (c) data summary and discussion of the results;
(d) possible causes of error; (e) recommendations; and (f)
conclusions. Along with this document, students were given a
Figure 3. Microtitration system. case study that included a problem involving stoichiometric
calculations similar to the ones covered in the postlab quiz.
(A sample calculation is included in the Supporting The quiz was graded on the basis of how close the
Information.) experimental ratio of mol LiOH/mol Li was to the
moles = molarity × volume used in titration (3)
stoichiometric value of 1. Since the experimental work was
also intended to be part of the evaluation, the deviation from the
Calculation of the Number of Li Moles That Reacted real value (i.e., % error) was taken as a grading criterion. In this
Remove the Li-free lid from the reaction chamber; rinse, pat dry way, 76% of the students were able to get a % error below 10%
with a paper towel, and weigh it. Compare the mass of this Li- and received full credit, 16% obtained a % error in the range of
free lid to the initial one, and the difference is the Li that 11−13% and were assigned 75% of the credit, and only 8% got a
participated in the reaction. With its atomic mass of 6.94 g/mol, % error greater than 13% that accounted for 50% of the total
calculate the number of moles of reacted Li. (See an example in credit. The other ratios (i.e., mol H2/mol Li and mol LiOH/mol
the Supporting Information.) H2) were not rigorously evaluated due to the limitations when
Last, compare the number of moles of reacted Li, of LiOH obtaining the moles of hydrogen by application of the ideal gas
titrated, and of H2 generated, and evaluate their closeness to the law to experimental data (i.e., the intrinsic inaccuracies when
theoretical stoichiometries from reaction 1 (Table 1). measuring the temperature of the liquid instead of that of the
gas, and the use of a commercial syringe for volume
measurement).
Table 1. Stoichiometry Results of Two Student Groupsa
For the reports, a rubric was used to grade the documents.
mol LiOH/mol Li mol H2/mol Li mol LiOH/mol H2 The main focus of this assignment was to evaluate the ability to
Group (Theoretical = 1) (Theoretical = 0.5) (Theoretical = 2) explain the results and relate the experimental findings to the
A 1.09 ± 0.04 0.60 ± 0.04 1.84 ± 0.12 stoichiometric theory. Therefore, a large part of the credit was
B 1.00 ± 0.07 0.60 ± 0.05 1.67 ± 0.14 oriented to the discussion of results and conclusions. On this
a
Results are rounded-off to three significant figures. basis, 84% of the 73 students obtained 85−100% of the credit,
8% received 75−85%, and the remaining 8% were graded below
85%. A similar instrument was used to grade the case study. As
the goal of such an activity was to develop problem-solving skills,
As observed, for such a simple, quick, and low-cost experiment the grading focused more on the approach rather than on the
that uses three different methods to study a reaction correctness of the answers. Here, 95% of the students obtained
stoichiometry, there is a reasonable correlation between the full credit, and the remaining 5% obtained 75% of the total
obtained results and the theoretical expectations. Among the points. (The two instruments utilized to evaluate the reports and
possible sources of error are the following: the case study are included in the Supporting Information.)
• The calculation of the number of moles of H2 uses the Overall, all of the students obtained a final grade greater than
ideal gas law, assuming that the gas temperature 80%, resulting from the weighted average of the credits obtained
in the postlab quiz, report, and case study.

■
originated by this exothermic reaction is the same as
that of the aqueous solution. This may not be exactly the
case. In addition, the temperature distribution may not be ASSOCIATED CONTENT
homogeneous in the entire system, as some of the heat is *
sı Supporting Information
dissipated to the surroundings by convection and The Supporting Information is available at https://pubs.ac-
radiation since this is not an adiabatic system. Therefore, s.org/doi/10.1021/acs.jchemed.0c00876.
the ideal gas law calculations may introduce some error.
• The procedure assumes that the Li is 100% pure, which is Student handout, sample results, sample calculations, case
not necessarily the case since manufacturers do not report study evaluation, and the rubric utilized to grade the lab
this information. report (PDF)

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J. Chem. Educ. 2020, 97, 4103−4107
Journal of Chemical Education

■
pubs.acs.org/jchemeduc Laboratory Experiment

AUTHOR INFORMATION Undergraduate Laboratory Experiment. J. Chem. Educ. 2014, 91 (6),

898−901.
Corresponding Author (11) Davis, T. A.; Athey, S. I.; Vandevender, M. I.; Crihfield, C. L.;
Jorge G. Ibanez − Departamento de Ingenieriá Quimica,
́ Kolanko, C. C. E; Shao, S.; Ellington, M. C. G.; Dicks, J. K.; Carver, J. S.;
Industrial, y de Alimentos, Universidad Iberoamericana, 01219 Holland, L. A. Electrolysis of Water in the Secondary School Science
Mexico City, Mexico; orcid.org/0000-0003-3247-6751; Laboratory with Inexpensive Microfluidics. J. Chem. Educ. 2015, 92
Email: [email protected] (11), 116−119.
(12) Koga, N.; Kimura, T.; Shigedomi, K. Laboratory Inquiry for
Author Determining the Chemical Composition of a Component in a Daily
Use Detergent: Sodium Sesquicarbonate. J. Chem. Educ. 2011, 88 (9),
Violeta A. Martínez − Departamento de Ingenieriá de Procesos y 1309−1313.
Ciencias Ambientales, Universidad Centroamericana “José (13) Furlong, W. R.; Rubinski, M. A.; Indralingam, R. The Method of
Simeón Cañas”, Antiguo Cuscatlán, San Salvador, El Salvador Continuous Variation: A Laboratory Investigation of the Formula of a
Precipitate. J. Chem. Educ. 2013, 90 (7), 937−940.
Complete contact information is available at:
(14) Davis, E.; Cheung, K.; Pauls, S.; Dick, J.; Roth, E.; Zalewski, N.;
https://pubs.acs.org/10.1021/acs.jchemed.0c00876 Veldhuizen, C.; Coeler, J. Gravimetric Analysis of Bismuth in Bismuth
Subsalicylate Tablets: A Versatile Quantitative Experiment for
Notes Undergraduate Laboratories. J. Chem. Educ. 2015, 92 (1), 163−166.
The authors declare no competing financial interest. (15) Vannatta, M. W.; Richards-Babb, M.; Sweeney, R. J. Oxalate

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Synthesis and Pyrolysis: A Colorful Introduction to Stoichiometry. J.
Chem. Educ. 2010, 87 (11), 1225−1229.
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We thank Dolores Rovira, Josué Valdez, Ruth Masferrer, Carlos L. S.; Gasparotto, L. H. S. Determination of Al Content in Commercial
Mina, and Carolina Chávez (UCA, El Salvador) and Virgina Samples Through Stoichiometry: A Simple Experiment for an
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dia Camacho-Zúñ iga, Irma Jessica Medina-Hurtado, and Chem. Educ. 2014, 91 (9), 1473−1476.
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