Lab Manual PDF

Elementary Inorganic Chemistry
CHEM 112 Laboratory

Manual
Chemistry Department
Morehouse College
Spring 2017
This laboratory manual is the product of adaptation, modification, and new
experiments initiated by the grant from U.S. Department of Education
award number P120A030117. Partial support of W. M. Keck Foundation
Grant number 031875 is also acknowledged. The authors have tried to
follow the guided-inquiry approach in compiling these experiments.
Subhash C. Bhatia
Chemistry Department
Morehouse College
&
Natarajan Ravi
Physics Department
Spelman College
Copyrighted Fall 2004
Revised 12/14/2010
Troy L. Story
2
Table of Contents
A. Laboratory Safety and Housekeeping

Page number
B. Safety Agreement
C. Guidelines for the Laboratory Report

4
1. Investigation of the Effect of Solute on the Physical Properties of a Solvent 9
7
2. Determination of Molar Mass of a Compound using a Colligative Property 13
8
3. Enthalpy of a Chemical Reaction
4. Enthalpy and Entropy
5. Rate and Order of a Chemical Reaction 32
6. Determination of an Equilibrium Constant 38
7. Acids and Buffers 46
8. Determination of the Concentration of an Acid 51
9. Electrochemistry: Voltaic Cells, Determination of Equilibrium Constant 57
APPENDIXES
16
A. Common Instruments 67
B. Logger Pro Instructions 79
C. Calibration procedures for different sensors 84
D. Frequently Asked Questions about Data Analysis 88
22
3
MOREHOUSE COLLEGE
Department of Chemistry
Laboratory Safety and Housekeeping
Students are asked to be particularly mindful of the following as they conduct chemistry
experiments in Morehouse College instructional laboratories.
Safety
EYE PROTECTION IS MANDATORY WHILE WORKING IN THE

LABORATORY. NO STUDENT WILL BE PERMITTED TO WORK
WITHOUT EYE PROTECTION.
Be aware of the hazardous nature of the chemical being used. Consult your
instructor or teaching assistant if there are questions regarding the use of any
chemical. Do not substitute chemicals in a procedure unless instructed to do so.
Become familiar with the procedures to be employed prior to their performance.

Exercise extra care when necessary.
Be aware of potentially hazardous situations such as open flames, spills, etc.

Alert other students to the problem then correct and/or seek advice from your
instructor or teaching assistant.
Food and beverages are not allowed in the laboratory.
Housekeeping
Ask permission to remove equipment or chemicals from cabinets or shelves.

Unauthorized removal of equipment or chemicals will result in a failing
grade for the experiment being performed.
Keep your work area free from chemicals and equipment not being used in the
procedure.
Be careful when obtaining chemicals from bottles and jars. Do not take more
than what is needed. Replace the cap on the bottle or jar immediately after
obtaining the chemical therein.
Inform the professor or lab instructor of any spills immediately. Dispose of

broken glass in the proper receptacle (not the trash can).
4
CHEMICAL LABORATORY SAFETY INSTRUCTIONS
Read the following required policies/procedures carefully before entering any

laboratory. Failure to following these rules and regulations will result in
expulsion from the laboratory.
1. In case of fire or accident, notify the instructor immediately
2. Approved eye protection must be worn at all times in the laboratory where
chemicals are stored or handled. The approved type of eye protection is
safety glasses. Contact lenses are prohibited in the laboratory. A student
will not be allowed to work in the lab without eye protection.
3. During the first laboratory period, become familiar with the location of the
safety features of the laboratory. Note the locations of fire extinguishers,
fire blanket, safety shower, eyewash, the nearest telephone and the list of
important telephone numbers.
4. Confine long hair when in the laboratory. Shoes must be worn. Shorts,
miniskirts and sandals are not allowed in the laboratory. Aprons or lab coats
are highly recommended and are provided in the bookstore.
5. Unauthorized experiments are prohibited.
6. Working alone in the laboratory is prohibited.
7. Horseplay or other acts of carelessness are prohibited.
8. Laboratory areas are not to be used as eating or drinking areas; do not eat or
drink from lab glassware.
9. Mouth suction is not to be used to fill pipettes. Rubber suction bulbs will be
provided.
10. Exercise great care in noting the odor of fumes; avoid breathing fumes of
any kind. (Inhalation of high concentrations of certain chemicals, particularly
volatile solvents, can cause respiratory failure; other chemicals are chronic
poisons after inhalation over time.)
11. Avoid skin or eye contact with any chemical. If you receive a chemical burn
from acid or alkali, immediately wash the burned area with copious amounts
of water and call an instructor immediately.
5
12. Broken glass, flammable materials, paper and solid must be deposited in the
provided containers, not in the sinks.
13. Cuts and burns can be prevented by following a few simple rules:
a) When inserting glass tubing or thermometers into rubber stoppers,

always protect your hands by wrapping the glass tubing with a towel.
In addition, place a drop of glycerin on both the glass and the hole of
the stopper.
b) Fire polish all sharp edges of broken glass.
c) Discard cracked or broken glass immediately.
d) NEVER heat a graduated cylinder with a burner flame.
14.Never pour water into concentrated acid. Concentrated acids and bases may
be diluted by pouring the reagent into water while stirring it carefully and
continuously. Also, never add concentrated acid to concentrated base or vice
versa.
15. When heating a test tube, never point the test tube toward your laboratory
partner, neighbor, or yourself.
16.The Bunsen burner should be burning only when it is being used. Before
lighting a burner, make sure that flammable reagents such as acetone,
benzene, ether, alcohol, etc. are not in the vicinity.
17.Do not carry reagent bottles to your bench. This is a matter of safety and
courtesy to the other students in the class, and it minimizes the possibility of
contamination of the reagent.
18. Do not insert spatulas or pipets into reagent bottles.
19. At the end of the laboratory period, wash and wipe off your bench area. Be
sure to return all equipment to the proper place.
20. WASH HANDS BEFORE LEAVING THE LABORATORY.
6
SAFETY AGREEMENT
I have studied, I understand, and I agree to follow the safety regulations required for
this course. I have located all emergency equipment and now know how to use them.
I understand that I may be dismissed from the laboratory for failure to comply with
stated safety regulations.
Signature
Print Name
_____________________________________________________________________
Date
Course
Section
Instructor
Person(s) who should be notified in the event of an accident:
I grant permission to post my grades in this course at mid-semester and again at the
end of the semester, if my grades are identified by only a portion of my I.D. number.
∼ yes ∼ no
Signature
7
GUIDELINES FOR THE LABORATORY REPORT
Each laboratory report should be written individually, not as a group;

duplications are not accepted. In this way, students develop experience
translating experimental data and calculations into written form. This
process also supports the College’s writing skills program.
The laboratory report should be written in the past progressive tense (passive
voice), using an essay style. Avoid the use of pronouns (e.g., I, we, they, us). For
example, write “the use of pronouns should be avoided” rather than “you should avoid
the use of pronouns.” The lab format consists of the following five topics, with topics 1
and 2 prepared before class. All reports should be typed.
1. Introduction {(10 + 5 + 5) points}

• State clearly the raw data measured and name the systems, reactions,
compounds, etc., for which these measurements are performed.
Example: In this experiment the volume of nitrogen is measured as a function of
temperature at constant pressure.
• What major instruments are used?
• What properties are calculated from the raw data?
2. Theory {(10 + 10) points}

• List the fundamental equations used to calculate the properties referred to in
the introduction; define all symbols.
• Write a detailed explanation for using the fundamental equations to convert
raw data into calculated data.
3. Experiment {(5 + 10 + 5) points}

• Draw diagram(s) of the overall experimental set-up. Label the important
elements; do not diagram individual pieces.
• Using your diagram, describe the lab procedure followed. Do not itemize; write
an essay. You’ll know when you’ve written a suitable procedure if you can
repeat the experiment using your own write-up.
• Construct tables to display raw data. Attach computer print-outs of raw data.
4. Calculations {(10 + 10) points}

• Use the equations from the theory section for all calculations. Provide a
detailed example of each type of calculation; explain. Calculate uncertainties.
• Construct tables to display calculated data and uncertainties.
5. Conclusion {(10 + 10) points}

• Summarize the experimental and calculated data, and state whether these
results are compatible with standards.
• Discuss possible sources of error.
• Solve all questions and problems associated with the experiment.
8
Experiment 1
Investigation for the Effect of Solute on the Physical

Properties of a Solvent
Objectives:
a) to learn how to establish relationships between experimentally determined
variables.
b) to learn how to search the literature for accepted values of physical
quantities.
c) to determine what is needed to calculate a defined concentration unit.
d) to calculate a defined quantity from the experimental data.
e) to solve problems such as “The freezing point of water is 00C and butanol
freezes at –89.50C. Predict the freezing point of a solution prepared by
mixing 10 mL of water and 1 mL of butanol. The molal freezing point
depression constant of water is 1.86 K kg/mol.”
I. Introduction
Consider a binary solution containing components 1 and 2, with partial pressures
P1 and P2 , and mole fractions X1 and X2 . These mole fractions are defined by
X1 = n1 /n and X2 = n2 /n
where n = n1 + n2 = the sum of the number of moles of components 1 and 2. If
X1 > X2, then component 1 is defined as the solvent since it is present in the largest
concentration; component 2 is the solute. The partial pressures are just the vapor
pressures of the individual components over the solution. Assume that the vapor
pressure of the pure solute is very much less that that of the pure solvent, then the
solute is called non-volatile. The overall effect of adding a non-volatile solute to a
solvent is to decrease the vapor pressure of the resulting solution. Such an effect is
called a colligative property, since this property depends only on the relative number of
particles present. In this experiment you will investigate the freezing point of a binary
solution consisting of a solvent (water) and a solute (butanol). The materials required
for this experiment are as follows:
Computer utility clamp
Vernier Computer interface 18 × 150 mm test tube
Logger Pro distilled water
2 Vernier Temperature Probes butanol
ring stand sodium chloride
Thermometer ice
400 mL beaker
9
II. Theory
The mathematical model for quantitative description of a freezing point
depression problem is
ΔTfp = −i m Kf
where
ΔTfp = Tfp (solution) – Tfp (solvent)

m = molality of solution = moles of solute/kilograms of solvent
Kf = molal freezing point depression constant
i = number of particles produced when solute dissolves in water, e.g.,
NaCl produces 2 particles, Na+ and Cl−, and so i = 2.
For butanol in water, i = 1, since butanol does not decompose into ions in aqueous
media. In this experiment plots of ΔTfp vs m will yield a straight line with a negative
slope equal to − Kf .
III. Experiment
1. Calibrate the Temperature Probe (see instructions – Appendix C, p.68).
2. Prepare the Computer for data collection.
3. Freezing point of water:
a. Transfer 10 mL of water into a test tube.

b. Immerse Temperature Sensor connected to channel 1 of the interface into
the water in the test tube.
c. Lower the test tube with sensor into the ice bath which is prepared by
adding ice to 400 mL beaker. Make sure that the meniscus of water in the
test tube is below the ice level.
d. Immerse the Temperature sensor connected to channel 2 of the interface
into an ice bath.
4. Click on to begin data collection.
5. With a very slight up and down motion of the Temperature probe in the test tube,
continuously stir the water during cooling. Hold the top of the probe and not its
wire. Make sure that the water is frozen. If not, what can do to freeze water?
6. Continue with the experiment until data collection has stopped.
7. Take the test tube out of the ice bath and let ice turn into liquid water.
10
8. To determine the freezing temperature of pure water you need to determine the
mean (or average) temperature in the portion of graph with nearly constant
temperature. Move the mouse pointer to the beginning of the graph’s flat part.
Press the mouse button and hold it down as you drag across the flat part of the
curve, selecting only the points in the plateau. Click on the Statistics button, .
The mean temperature value for the selected data is listed in the statistics box on
the graph. Record this value as the freezing temperature of pure water. Click
on the upper-right corner of the statistics box to remove it from the graph.
9. Add 0.5 mL of butanol to the test tube in step 7 and repeat steps 4 to 8. Make
sure that the mixture is uniform and freezes. Then go to steps 10, 11, and 12.
10. Add 0.5 mL more of butanol to the test tube from step 9 and repeat steps 4 to 8.
11. Add 0.5 mL more of butanol to the test tube in step 10 and repeat steps 4 to 8.
12. Add 0.5 mL more of butanol to the test tube in step 11 and repeat steps 4 to 8.
13. Steps 8 through 12 will give you the freezing point of pure water, and freezing
points of four solutions of water and butanol.
14. Find the freezing points of pure water and butanol from the CRC Handbook of
Chemistry and Physics. Compare the freezing point of pure water and butanol with
your experimentally determined values. Can you make any conclusion based on
the literature and experimental values?
15. What should you do to establish a relationship between the two measured
quantities? Ask your instructor if you do not know what to do.
16. Based on the lecture and recitation, what measured and calculated quantities
should you graph to obtain a linear relationship?
17. Calculate the quantities you decided to graph from the experimental data.
18. Enter the data into a spreadsheet. Follow the direction given in step 10 of
Experiment 2.
19. What is the mathematical relationship? What constant is related to the slope of the
graph?
20. Prepare a table which lists the amount of water, butanol and the freezing point for
each part of the experiment. Attach all graphs.
11
Vbutanol Vwater # kg water Freezing Pt
Pure 0 10 mL 0.010 kg
water
#1 0.5 mL 10 mL 0.010 kg
#2 1.0 mL 10 mL 0.010 kg
#3 1.5 mL 10 mL 0.010 kg
#4 2.0 mL 10 mL 0.010 kg
IV. Calculations
Show calculations for the number of moles of butanol and the molality of each of the
four butanol-water mixtures. Place this information in a data table along with the ΔTfp
values.
Run nbutanol molality ΔTfp

#1
#2
#3
#4
Plot ΔTfp vs m and compute the slope to obtain − Kf. Calculate the % error of your Kf
when compared to the literature value.
% error = 100%|Kf (lit) – Kf (exp)|/Kf (lit)
V. Conclusion
Refer to the lab write-up procedure.
12
Experiment 2
Determination of the Molar Mass of a Compound Using a

Colligative Property
Objectives:
a) to learn how to determine the boiling point of a liquid.
b) to learn how to determine the molar mass of an unknown compound.
c) to learn the differences between accuracy and reproducibility.
d) to learn why scientists repeat experiments under the same
conditions.
e) to learn how to solve problems such as “The normal boiling point of
cyclohexane is 80.70C; 1.00 mL of benzene (D = 0.8736 g/mL) is
dissolved in 20.00 mL of cyclohexane (D = 0.7785 g/mL). If the
molal boiling point elevation constant for cyclohexane is 2.790C/m
and the molar mass of benzene is 78.0 g/mol, then what is the
boiling point for the mixture of benzene and cyclohexane.”
I. Introduction
In experiment 8, you should have observed that the addition of a solute to a
solvent lowers (decreases) the freezing point of the solvent. The relationship
established is that ΔTf = −m Kf , where ΔTf is the change in the freezing point of the
solvent, m is molality of the solution and Kf is a proportionality constant known as the
molal freezing point depression constant. The present experiment investigates the
phenomena that addition of a non-volatile solute to a solvent also changes the boiling
point of the solvent. In addition, it will be shown that a closer observation of both
freezing point depression (exp 8) and boiling point elevation (exp 9) reveals a technique
for determining the molar mass of an unknown compound when dissolved in liquid
cyclohexane. The materials required for this experiment are as follows:
Computer cyclohexane
Vernier Computer Interface 500 mL or 1 liter beaker
Logger Pro Pipette, test tube
Temperature Probe Unknowns 1,2, and 3
II. Theory
The mathematical model for quantitative description of a boiling point elevation
problem takes the same form as for the freezing point depression problem, namely,
ΔTbp = i m Kb (1)
where
ΔTbp = Tbp (solution) – Tbp (solvent)
m = molality of solution = moles of solute/kilograms of solvent
nunknown = #moles of unknown sample
13
W = mass of unknown sample
M = molar mass of unknown sample
Kb = molal freezing point depression constant
i = number of particles produced when solute dissolves in water, e.g.,
NaCl produces 2 particles, Na+ and Cl−, and so i = 2.
For the unknowns used, i = 1.
Using this information, the equation ΔTbp = m Kb becomes
(2)
In this experiment the molar mass is computed by rearranging the above equation to
get
(3)
III. Experiment
1. Use 500-mL beaker to prepare a water bath.
2. Calibrate the temperature sensors (see the instructions – Appendix C, p.68).
3. Determine the mass of clean and dry test tube.
4. Take 10.00 mL of cyclohexane into the pre-weighed test tube and insert the test
tube into the water bath kept on the hot plate. Gently heat the water bath and
measure the boiling point of cyclohexane using the calibrated temperature
probe.
5. Clean and dry the test tube. Add a definite amount (0.25 to 0.5 g) of an
unknown 1 or 2 or 3, to 10.00 mL of cyclohexane. Make sure that the solution is
homogenous. Repeat step 4 to determine the boiling point of the solute-solvent
mixture. Repeat this procedure at least three times with the same amounts of
the solute and solvent. Record the pressure.
14
6. Complete the chart below for your raw data table.
W Vcyclohexane Boiling Pt ΔTbp

of
solution
Pure 0 10 mL xxxxxxxx
cyclohexane
#1 10 mL
#2 10 mL
#3 10 mL
#4 10 mL
IV. Calculations
For cyclohexane ( C6 H10 ): Kb = 2.79 K kg mol−1 ; TNbp = 356 K
Calculate the molar mass of the unknown sample from the following equation (refer
to theory section).
Run W #kg solvent ΔTbp M % error

#1
#2
#3
#4
% error = 100%|M(lit) – M(exp)|/M(lit)
Calculate the average value of the molar mass and the average % error of your
unknown.
The theory suggests another way of evaluating M,
namely, use of graphs of ΔTbp vs W yields a straight line whose slope is given by
slope = Kb / (#kg of solvent X M ) . In this way M = Kb / (#kg of solvent X slope ).
V. Conclusion. Refer to the lab write-up procedure.
15
Experiment 3
Enthalpy of a Chemical Reaction
Objectives
a) to measure the temperature change of the reaction between hydrochloric acid

solution and magnesium turnings.
b) to calculate the enthalpy, ΔH, of the formation of magnesium chloride.
c) to compare your calculated enthalpy of the reaction with the accepted value.
I. Introduction
Thermodynamics is the study of energy changes for macroscopic physical

systems. This experiment is designed to introduce techniques and concepts associated
with measuring energy changes of a chemical reaction. The energy change of interest is
the enthalpy change ΔH, which is a representation of an energy change in a (T, P) –
coordinate system, where T is the system temperature and P is the system pressure.
At constant pressure (denoted by subscript P ), qP = ΔHP , where qP is the heat
absorbed (or emitted) by a system at constant pressure. Fundamentally, heat is
identical to electromagnetic radiation.
In this experiment you will first determine the heat capacity of a calorimeter by
measuring: (1) the initial temperature of hot water, (2) initial temperature of (cold
water + calorimeter), and (3) the temperature of the mixture formed when hot water is
poured into the cold water. You will then measure the initial and final temperatures of
the chemical reaction of magnesium and hydrochloric acid, and use this information to
calculate the enthalpy change for this reaction.
Materials
Vernier computer interface Magnesium metal
computer 1.0 M Hydrochloric acid
Temperature Probe two 50 mL graduated cylinders
Styrofoam cup calorimeter ring stand
two 250 mL beakers utility clamp
Glass stirring rod
16
II. Theory
A convenient way to measure ΔHP is by placing the reaction vessel in thermal
contact (heat flows between the vessel and another object, in this case, water) with
water and measuring the temperature change of the water. Since it is known from
experiment that 75.38 Joules of heat will raise the temperature of one mol of water by
one Kelvin (called the heat capacity of water = C P , H2O(liq) ), then the experiment is a
simple matter of measuring the temperature change in the water after the reaction
occurs. This technique is referred to as calorimetry and the object containing the
water is called a calorimeter. Note that use of a calorimeter requires that the reaction
vessel and the calorimeter are isolated from the surroundings, implying that all energy
which is emitted by the chemical reaction is absorbed by the calorimeter; the converse
statement is true. This is a statement of the first law of thermodynamics; a
representation of the law of conservation of energy.
Some of the foregoing statements can be expressed in mathematical form,

namely, by the following equations for isolated reaction and calorimeter. According to
the first law of thermodynamics,
ΔHreaction + ΔHH O + ΔHcalorimeter = 0 (1)

2
But
ΔHP = nC P (Tfinal −Tinitial ) (2)
where
C P = Heat capacity at constant pressure P(units = Jmol -‐ 1K -‐ 1 )

= Amount of energy at constant P required to raise the temperature of
one mol of an object by one Kelvin
Tfinal = final Kelvin temperature, Tinitial = initial Kelvin temperature
Hence, eqn. (1) becomes
ΔHreaction + nH O C P,H2O(liq) (Tfinal −Tinitial ) + Ccal (Tfinal −Tinitial ) = 0 (3a)

2
Then ΔHreaction can be calculated from the equation
ΔHreaction = −nH O C P,H2O(liq) (Tfinal −Tinitial )−Ccal (Tfinal −Tinitial ) (3b)

2
17
To find the heat capacity of the calorimeter Ccal , hot water at temperature Th is
added to a calorimeter containing cold water at temperature TC , where the cold water
and the calorimeter are at the same temperature. Hence,
ΔHH O,T + ΔHH O,T + ΔHcalorimeter = 0 (4a)

2 h 2 c
Substituting for ΔH reveals the following result:
nh C P,H2O (Tfinal −Th ) +nc C P,H2O (Tfinal −Tc )+ Ccalorimeter (Tfinal −Tc ) = 0 (4b)
where C P , H2O = 75.38 J mol-1K-1 = heat capacity of liquid water, nh and nc are
symbols for the number of moles of hot and cold water respectively, and Ccalorimeter is
the heat capacity of the calorimeter. After measuring the temperatures, the only
unknown is Ccalorimeter , which can then be calculated from eqn. (4b), giving
− ⎡⎢nh C P,H2O (Tfinal −Th ) +nc C P,H2O (Tfinal −Tc )⎤⎥

Ccalorimeter = ⎣ ⎦ (5)
(Tfinal −Tc )
NOTE: Heat capacity at constant pressure CP or constant volume CV is a
more definitive term than specific heat.
III. Experiment
A Styrofoam cup nested in a beaker is used as a calorimeter, as shown in Figure
1. In Part I of this experiment, the heat capacity of the calorimeter will be determined
from temperature measurements and calculations.
Figure 1
In Part II, the reaction between magnesium and hydrochloric acid will be studied with
calorimetry in order to determine the enthalpy change at constant pressure for this
reaction.
18
Part I: Determination of Heat Capacity of the Calorimeter
1. Determine the mass of a dry foam coffee cup.
2. Place about 30 mL of cold tap water into the cup. Add a little ice to the water
so that when it is melted, the temperature will be below room temperature (try
around 10 to 150C). Determine the total mass of the water and the coffee cup.
3. Calibrate the temperature sensor and using the temperature sensor, measure the
temperature of the water.
4. Place approximately 30 mL of hot water (about 10 to 150C above room

temperature) into a second coffee cup. It is necessary to know the exact mass
of the hot water in the coffee cup, but this may be determined in different ways.
Determine the mass of hot water.
5. Measure the temperature of the hot water using the temperature sensor.
6. Add the hot water to the cold water in the first coffee cup, stir it gently, and
record the equilibrium temperature. You will need the masses of the hot and
cold water and the temperature changes to later perform the data analysis.
7. Use the law of conservation of energy to calculate the heat capacity of the
calorimeter.
Mass of hot water Mass of cold water Thot Tcold Tfinal
#1
#2
#3
Part II: Determination of Heat of a Reaction

1. Obtain and wear goggles.
2. Connect a Temperature Probe to Channel 1 of the Vernier computer interface.
Connect the interface to the computer with the proper cable.
3. Nest a Styrofoam cup in a 400 mL beaker as shown in Figure 1. Pour 100 mL of 1.0
M HCl into the Styrofoam cup. Keep stirring this and adjust the stirring rate to
vigorous but without splashing. Weigh 0.25 g of magnesium turnings on an
analytical balance.
19
4. Start the Logger Pro program on your computer.
5. Use a utility clamp to suspend the Temperature Probe from a ring stand (see Figure
1). Lower the Temperature Probe into the reaction mixture.
6. Conduct the experiment
a. Click to begin the data collection and obtain the initial temperature of
the HCl solution.
b. After you have recorded three or four readings at the same temperature,
quickly add the magnesium turnings. Use a glass stirring rod to stir the
reaction mixture gently and thoroughly.
c. Data may be collected for 5 minutes. You may terminate the trial early by
clicking , if the temperature readings are no longer changing. As the
reaction occurs, you should observe the temperature climb. Continue taking
data until a final, constant temperature plateau is well established. The
experiment can be stopped at this point.
d. Click the Statistics button, . The minimum and maximum temperatures are
listed in the statistics box on the graph. If the lowest temperature is not a
suitable initial temperature, examine the graph and determine the initial
temperature.
e. Record the initial and maximum temperatures, in your data table, for Trial 1.
7. Rinse and dry the Temperature Probe, Styrofoam cup, and stirring rod. Dispose of
the solution as directed.
8. Repeat Steps 3 and 5-7 to conduct a second trial. If directed, conduct a third trial.
Print a copy of the graph of the second trial to include with your data and analysis.
Sample mass Tinitial Tfinal
#1
#2
#3
IV. Calculations
Calculate the heat capacity of the calorimeter by using eqn. (5). Include a sample
calculation in your report.
20
Trial #1 Trial #2 Trial #3 Average Uncertainty
Ccalorimeter
Use the average heat capacity of the calorimeter and eqn.(3b) to calculate the enthalpy
change of the reaction, then divide this number by the number of mols of magnesium.
The result is the molar enthalpy change for the reaction with respect to consumption of
magnesium. Include a sample calculation in your report.
Trial #1 Trial #2 Trial #3 Average Uncertainty

ΔHreaction
ΔH reaction
ΔHreaction
=
nMg
V. Conclusion: Refer to the lab write-up procedure.
21
Experiment 4
Enthalpy and Entropy
Objectives
(a) to use an electrochemical cell for determining ΔG (the change in Gibbs energy),
ΔS (the change in entropy) and ΔH (the change in enthalpy), for the reaction
of solid zinc with aqueous copper sulfate.
(b) to determine ΔH for the same reaction as in (a), namely, the reaction of solid
zinc with aqueous copper sulfate, but this time with the use of calorimetric
methods.
(c) to compare enthalpy values ΔH obtained by the two methods in (a) and (b).
(d) to use ΔG for the reaction of solid zinc with aqueous copper sulfate to discuss
the criteria for deciding whether a reaction is spontaneous or at equilibrium.
I. Introduction
Thermodynamics is concerned with average energy changes and entropy
changes of macroscopic physical systems. Changes of a system referred to enthalpy
energy change ΔHT , entropy change ΔST and Gibbs free energy change ΔGT are
related according to the equation
ΔGT = ΔHT - TΔST (1a)
where the subscript T implies eqn.(1) is valid only at constant T. Another

thermodynamic equation for ΔGT is
ΔGT = −nFεT (1b)
where εT is the cell voltage (the electromotive force = emf) for an electrochemical
reaction at temperature T, e.g., reaction (2a).
Zn(s) + CuSO4(aq) → ZnSO4(aq) + Cu(s) (2a)
This experiment first uses electrochemical methods to determine ΔGT , ΔST and ΔHT ;
then, calorimetric methods are used to determine, once again, ΔHrxn . The results for
ΔHT and , ΔHrxn obtained by these two methods are compared.
Materials:
Vernier computer interface Copper sulfate solution
computer Zinc sulfate solution
Temperature Probe two 50 mL graduated cylinders
Styrofoam cup calorimeter ring stand
two 250 mL beakers utility clamp
Glass stirring rod Potassium nitrate solution
22
II. Theory
The electrochemical method:
The electrochemical method offers simple and accurate means for the
determination of thermodynamic quantities. Consider the electrochemical cell
Cu(s)/CuSO4(aq) || Zn(s)/ZnSO4(aq)
Cell voltage measurements are made in a Chem-Carrou-Cell, as will be shown and

described by your instructor. The overall voltaic cell reaction incated by the symbols
above is
Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s) (2b)
The half-cell reactions are
Oxidation (at anode) : Zn(s) → Zn2+(aq) + 2 e-1 ......... +0.76 V
Reduction (at cathode): Cu2+(aq) + 2 e-1 → Cu(s) ......... +0.34 V
Overall reaction: Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s) ... 1.10 V
Note that the procedure for calculating the cell voltage for an oxidation-reduction
reaction is simply to (a) write one half-cell reaction as an oxidation reaction with the
associated half-cell voltage, (b) write the other half-cell reaction with its’ half-cell
voltage and (c) add the reactants, products and half-cell voltages. Addition is the
only rule.
The quantity of electrical energy produced or consumed during a electrochemical

reaction can be measured accurately by means of electrochemical cells, where the
output measured is the cell voltage ε; this number is related to the energy change ΔG
by the following equation:
ΔGT = −nFεT (3)
where n = the number of moles of electrons transferred in a redox reaction.
F = Faraday’s constant of = 96,485 C /mole of electrons.
Equating equations (1) and (3), then dividing both sides by nF, gives a linear
relationship between the voltage ε and the temperature T, as given by
ΔHT TΔST
εT = − + (4a)
nF nF
23
or
⎛ ΔS ⎞ ΔHT
εT = ⎜⎜⎜ T ⎟⎟⎟T − (4b)
⎜⎝ nF ⎟⎠ nF
Assuming Δ H and Δ S are independent of temperature over the

temperature range Δ T of the experiment, then
⎛ ΔS ⎞⎟ ΔH
εT = ⎜⎜ ⎟⎟T − (4c)
⎜⎝ nF ⎟⎠ nF
To determine Δ S and Δ H , eqn.(4c) shows that if ε is plotted versus the absolute

temperature T, the resulting graph is of the form of a straight line y = mx + b, where
m is the slope and b is the y – intercept.
ΔS
Slope= (5a)
nF
−ΔH
y intercept = (5b)
nF
Hence,
(a) Calculation of Δ S : Measurement of slope yields Δ S ,since Δ S = nF (slope).
(b) Calculation of Δ H : Measurement of the y – intercept yields Δ H , since
Δ H = - nF (y intercept).
(c) Calculation of Δ GT : ΔGT values at different temperatures T are calculated by

inserting measured values of the cell voltage εT at T into eqn.(3), since
D GT = -‐ nF eT . Calculate ΔG = <ΔGT > = the average value of ΔGT , and compare to
ΔG calculated from ΔG = ΔH - T ΔS (use average T ).
(d) Calculation of equilibrium constant K : In contrast to experimental values of

ε , values of ε can be calculated with the use of the Nernst equation, given by
ν ν
RT ⎡⎣⎢C ⎤⎦⎥ ⎡⎣⎢D ⎤⎦⎥
C D
0 RT 0
ε =ε − lnQ = ε − ln (6a)
nF nF ⎡ A⎤ νA ⎡B ⎤ νB
⎢⎣ ⎥⎦ ⎢⎣ ⎥⎦
where Q is the reaction quotient for the prototype reaction given below, and ε 0 is the
standard potential measured at 250C and 1 atm.
24
nA A + nBB → nCC + nD D
For reaction (2b), eqn. (6a) is

1
⎡ 2+ ⎤
0 RT 0 RT ⎣⎢ Zn ⎦⎥
ε =ε − lnQ = ε − ln (6b)
nF nF ⎡Cu 2+ ⎤1
⎢⎣ ⎥⎦
At thermodynamic equilibrium ΔG = 0 and Q = Kexp ; hence, eqn. (3) implies ε =0 at

thermodynamic equilibrium. Therefore, for a reaction at thermodynamic equilibrium,
nA A + nBB ! nCC + nD D
ν ν
⎡ ⎤C⎡ ⎤D
0 RT RT ⎢⎣C ⎥⎦ eq ⎢⎣D ⎥⎦ eq
ε = lnK = ln (7)
nF nF ⎡ A⎤ νA ⎡B ⎤ νB
⎢⎣ ⎥⎦ eq ⎢⎣ ⎥⎦ eq
Eqn, (7) implies that the equilibrium constant K can be determined by measurements
of the standard cell voltage for the reaction, then using eqn.(7) in the form
K = exp (nFε 0/RT )

0
Note that ε is obtained experimentally by using an experimental
arrangement where [Zn2+] = [Cu2+], implying the logarithmic term of the Nernst
eqn.(6b) is zero. Under these conditions, the standard voltage of the cell is equal to
0
the measured voltage ε , i.e., ε = ε .
The calorimetric method:
Although calorimeters can be constructed to operate at constant pressure or

constant volume, constant pressure calorimeters are most convenient since they can
operate at the constant pressure of the atmosphere. A constant pressure calorimeter is
a perfectly insulated vessel which contains a large known mass of calorimeter solution
in perfect thermal contact with an accurate thermometer and a small reaction tube
(Figure 1). When measured quantities of reactants are introduced into the reaction
tube, the energy emitted by the reaction changes the temperature of the calorimeter
solution. Enthalpy changes are then calculated by inserting these temperature changes
into certain fundamental equations of thermodynamics.
The most important equation is the first law of thermodynamics, which states
that, for constant pressure calorimeters,
25
ΔHrxn +ΔHcalorimeter + ΔHcalorimeter = 0 (8)
solution
Since at constant pressure P,
ΔHP = nC P (Tfinal −Tinitial ) , constant P

(9)
! P T −T
= mC ( final initial ) , constant P
! P and
where nC P = mC
n = moles
C P = heat capacity in units of Jmol −1K −1
m = mass in units of grams,
C! P = heat capacity in units of Jg −1K −1
Then eqn. (8) becomes,
ΔHrxn = − ΔHcalorimeter − ΔHcalorimeter

solution
(10)
= −ncalorimeter C P , calorimeter
solution,
(Tfinal −Tinitial ) −Ccalorimeter (Tfinal −Tinitial )
solution
where
ncalorimeter = number of moles of solution in the calorimeter

solution
C P , calorimeter
solution,
= heat capacity of the solution in the calorimeter
Ccalorimeter = heat capacity of the calorimeter
Tfinal = final temperature (K ) of the solution in the calorimeter
Tinitial = initial temperature (K ) of the solution in the calorimeter
For this experiment the relevant heat capacities are
solution (
! P , calorimeter = m
C solution
3.8Jg −1K −1)
! P, calorimeter " 30JK −1
C
Hence, eqn. (10) becomes
26
ΔHrxn = −ncalorimeter C P , calorimeter
solution,
(Tfinal −Tinitial ) −Ccalorimeter (Tfinal −Tinitial )
solution
! P , calorimeter T −T
= −mcalorimeter C solution
( final initial ) −Ccalorimeter (Tfinal −Tinitial ) (11)
solution
= − ⎡⎢msolution (3.8Jg −1K −1) + 30JK −1 ⎤⎥ (Tfinal −Tinitial )

⎣ ⎦
III. Experiment
In Part I of this exercise, you will be measuring voltages and temperature,
displaying them on the screen, and sending stable voltage readings and the
corresponding temperatures to the spreadsheet.
In part II, you will be collecting temperature readings as a function of time. This
program should have an on-screen graphing temperature range between 150C and 300C
and on-screen graphing time running from 0 to 60 min.
Part I: Electrochemistry
Figure 1
1. Calibrate your temperature sensor with ice-cold and hot tap water.
2. Fill a 600 mL beaker three-quarters full of ice. Fill the rest of the beaker with
cold tap water until the beaker is filled to one cm from the top. Stir the ice/water
mixture to distribute the ice evenly. Using a rubber band, assemble three vials to form a
Chem-Carrou cell.
3. Place the beaker on a hot-plate – don’t turn the heat on yet! Rest the Chem-
Carrou-Cell on top of the beaker so that the bottoms of the wells of the cell are
immersed in the ice/water mixture. Let the set-up stand for 15 min until the
temperature stabilizes.
4. Pour about 5 mL of 0.1 KNO3 into the center well. Pour enough of 0.5 M ZnSO4
into well #1 to touch the salt bridge strip (soaked with KNO3). Into well #2, pour
enough of 0.50 M CuSO4 to touch the salt bridge strip (soaked with KNO3).
27
5. With clean tweezers, take a strip of filter paper and dip one end into the central
well (where immersion in the KNO3 solution will hold one end); dip the other end into
well #1. Repeat this procedure with another strip of filter paper, dipping the other end
into well #2. This creates the salt bridge for your galvanic cell.
6. With clean tweezers take a zinc metal strip and sand it to remove any oxide
coating. Bend 2 cm of one end of the strop and immerse it in the ZnSO4 solution (well
#1). The rest of the metal strip (3 cm) extends out to the edge of the cell and should
be bent over the rim. Repeat the same procedure with the copper metal strip and place
it in well #2. Later the electrical leads (alligator clips) from the interface will be
attached to the metal strips.
7. Fasten your temperature sensor to the ring stand with a clamp and adjust it such
that its tip can be immersed in the central well (KNO3 solution) of the cell. It is
assumed that the temperature of the ZnSO4 solution and CuSO4 solution well be very
close to the temperature of the KNO3 solution throughout the experiment.
8. Start the computer program to monitor the temperature.
9. Read and record the temperature. Attach the alligator clips to the metal strips
and take the voltage reading. If a negative number appears on the screen, reverse the
wires. Disconnect the wires immediately after the reading is recorded.
10. Turn on the hot plate to high and take voltage and temperature readings every
100C up to 400C. Connect the wires only while actually reading the voltage. Prolonged
connection of the wires will cause the electric current to flow through the cell. The
discharge will result in changes in concentrations of the solutions. Since the measured
voltage depends on these concentrations, there will be an error in the voltage readings.
11.
28
[CuSO4] ---
Volume ---
[KNO3] ---
Volume ---
Temperature T
Cell Voltage ε
Part II: Calorimetry:

1. Weigh a clean and dry 150 mL beaker on the top loading balance, then add 50 mL
of 0.5 M CuSO4 solution. Weigh the beaker a second time to determine the mass of
the solution in the calorimeter. Nest the 150 mL beaker inside a 400 mL and 600
mL beaker, thread the stirring rod and temperature sensor through the Styrofoam
lid and position the lid on the inner beaker. The temperature sensor should be as
deep into the solution as possible but without strain. Let the apparatus stand so
that the components attain the same temperature.
2. Using a top loading balance, weigh 0.5 g of zinc powder into a plastic weighing
boat, then weigh the boat plus its contents on the analytical balance.

3. Conduct the experiment.
a) Click to begin the data collection and obtain the initial temperature
of the copper sulfate solution.
b) After you have recorded three or four readings at the same temperature,
quickly add the zinc powder. Use a glass stirring rod to stir the reaction
mixture gently and thoroughly. Save the boat and any Zn stuck to it for
weighing at the end of run. Stir thoroughly and plot temperature vs time
until a well defined cooling trend is established. It is important that a
rubber policeman be used continually to ensure that any residue produced
(copper coated zinc powder) is broken up.
29
c) Data may be collected for 5 minutes. You may terminate the trial early by
clicking , if the temperature readings are no longer changing. As the
reaction occurs, you should observe the temperature climb. Continue
taking data until a final, constant temperature plateau is well established.
The experiment can be stopped at this point.
d) Click the Statistics button, . The minimum and maximum temperatures

are listed in the statistics box on the graph. If the lowest temperature is not
a suitable initial temperature, examine the graph and determine the initial
temperature.
e) Record the initial and maximum temperatures, in your data table, for Trial
1.
4. Weigh the weighing boat on the analytical balance and obtain the amount of Zn
added by difference.
5. Use the spreadsheet file to plot and print the graph of your data.
6. From your plot of temperature vs time, determine the initial and final temperatures
and calculate the heat of reaction per mole of zinc. Compare this value with ΔH
obtained in Part I.
#1 #2 #3 #4
Mass (beaker)
Mass (beaker +
CuSO4)
Mass (CuSO4 )
Volume (CuSO4 )
Mass (boat)
Mass (boat + Zn)
Mass (Zn)
30
IV. Calculations
Recall the equations
⎛ ΔS ⎞ ΔHT
ε = ⎜⎜⎜ T ⎟⎟⎟T −
⎜⎝ nF ⎟⎠ nF
ΔST ΔHT
Slope = ; y intercept = −
nF nF
ΔGT = ΔHT −TΔST
Plot the ε vs T data and calculate ΔS from the slope and ΔH from the y – intercept.
Calculate ΔGT from cell voltage measurements εT and average to get ΔG = <ΔGT> ;
compare to ΔG from ΔG = ΔH - <T > ΔS , where <T > is the average temperature.
Finally calculate ΔHrxn from the equation
ΔHrxn = − ⎡⎢msolution (3.8Jg −1K −1) + 30JK −1 ⎤⎥ (Tfinal −Tinitial )

⎣ ⎦
ΔS = (nF )(slope)
ΔH = −nF ( y intercept)
ΔG = ΔGT
ΔG = ΔH − T ΔS
ΔHrxn = − ⎡⎢msolution (3.8Jg −1K −1) + 30JK −1 ⎤⎥ (Tfinal −Tinitial )

⎣ ⎦
31
Experiment 5
Rate and Order of a Chemical Reaction
Objectives
(a) to learn, to define, and understand terms such as rate, order, mechanism, activation
energy, activated complex, etc., which are often encountered in kinetics.
(b) to plan and design an experiment to determine parameters of the kinetics of a
reaction.
(c) to calculate the specific rate constant and the rate law.
(d) to gain experience with the oscillation between experiment and theory.
Background material
In chemical kinetics, experiments are performed to determine the rate (speed),
order and mechanism of chemical reactions, and the results are compared to
mathematical models of these reactions. The interaction between experiments of this
type and mathematical models of the rate, order and mechanism of a chemical reaction
defines the study of chemical kinetics. When comparing this discipline to
thermodynamics, it is noted that the second law of thermodynamics provides a criteria
for determining whether reactions are spontaneous or not, but the law does not provide
information about the speed, order and mechanisms of reactions. Chemical kinetics
provides this information.
To define reaction rate, order and mechanism, consider the reaction 2A + B → P.
Several symbols are used for an expression of the speed (magnitude of the
velocity) or rate for this reaction, as given by the following equation:
⎛ −1 ⎞ d [ A] −d [B ] +d [P ]
Rate = ⎜ ⎟ = = (1)
⎝ 2 ⎠ dt dt dt
−1
The quantity d [ A] / dt is the rate of consumption of reactant A , −d [B] / dt is the
2
rate of consumption of reactant B, and +d [P ] / dt is the rate of formation of product
±1
P. In general, the rate of any component X is given by d [ X ] / dt , where nX is the
nX
stoichiometric coefficient in the balanced chemical equation. In order to make certain all
rates have a positive sign, a negative sign is attached to rates of consumption since
d [ A] < 0 and d [B] < 0 ; however, a positive sign is attached to the rate of formation
since d [P ] > 0 . Either symbol for the rate can be used, but for some computations, one
may be more convenient. Experiments in kinetics involve measuring changes in A, B
32
and P as functions of time, e.g., changes in concentration, partial pressure, pH ,
conductance, or absorbance of electromagnetic radiation as a function of time.
Suppose experimentation on the reaction 2A + B → P has led to the following
equation for describing the average reaction rate:
⎛ −1 ⎞ d [ A ]
⎜ ⎟ = k [ A ][B ] (2)
⎝ 2 ⎠ dt
where the rate of consumption of reactant A is expressed as a constant k times the

product of the concentrations of reactants A and B; k is called the specific rate
constant and eqn.(2) is called the rate law for the reaction. On the right side of
eqn.(2), since [A] is raised to the first power, then the reaction is called first-order in A;
similarly, the reactant is first-order in B since [B] is raised to the first power. Addition
of the exponents gives the number 2, and so the reaction is said to be second-order
overall.
According to chemical kinetics, the fact that the exponents in the rate law are
one, implies that the slowest step in the reaction is
(3)
where (AB)‡ is called the activated complex. In general, the exponents of the
reactant concentrations in the rate law are identical to the coefficients of the
reactants for the slowest reaction step. This slowest step is referred to as the
rate-determining step because the overall reaction cannot move faster than the slowest
step. A rate-determining step is called unimolecular if one reactant particle is present,
bimolecular if two reactant particles are present, and termolecular if three reactant
particles are present, etc. This concept of molecularity is used for the description of
all elementary steps in a multi-step reaction, including the rate-determining step.
The rate determining reaction
(4)
is one of the reactions referred to as the mechanism for the overall reaction 2A + B →
P. To illustrate this concept assume that, not only is the reaction first-order in A and
first-order in B, but that it is also a reaction which occurs in two steps. It is
emphasized that information on the rate, order and mechanism of any
chemical reaction is obtained only from experiments. Moving forward, note that
the remaining reaction in this hypothetical mechanism is obtained by subtracting the
rate-determining step from the overall reaction, as illustrated in the following
development:
33
I. Introduction
To illustrate basic principles in chemical kinetics, the reaction of solid calcium

carbonate with the strong acid HCl, is investigated. This is a familiar reaction observed
in everyday life (over time), since many historic monuments are constructed from
marble (a form of calcium carbonate) which slowly reacts with the acid content in rain,
and decomposes according to the reaction
CaCO3(s) + 2H+(aq) Ca2+(aq) + CO2(g) + H2O(liq) (5)
Using a gas pressure probe, the pressure of carbon dioxide is measured as a function of
time, allowing computation of the specific rate constant for this reaction. Using the
specific rate constant and the Arrhenius equation, the activation energy is calculated.
II. Theory
In this experiment the kinetics of reaction #5 is followed by setting the number

of moles of one of the reactants (H+) to be very large in comparison to the number of
moles of the other reactant (CaCO3), a kinetics technique called the isolation method;
it implies that some information about the kinetics of a reaction can be obtained by
following the exceptionally small component (CaCO3 in this case). The order obtained
for CaCO3, using the isolation method is called the “pseudo-order’” for CaCO3,.
Following this process, the isolation method is then employed for the remaining
component H+ by using a large number of moles of CaCO3. in comparison to the
number of moles of H+. If the rate law is pseudo x-order in CaCO3 and pseudo y-order
in H+, then this data implies that the reaction is pseudo ( x + y ) - order overall. Hence,
the overall rate law is of the form
−dnCaCO3
= knCaCO
x
nHy + (6a)
dt 3
Note that nA is used rather than [A] because calcium carbonate is a solid.
For this experiment it is only required to find the specific rate constant k, since
the value x ( = 1) is given and the number of moles of CaCO3 is exceptionally small;
hence, the time dependence of [H+] is ignored. According to the stoichiometry of
34
reaction (5) the number of moles of CaCO3 consumed is the number of moles of CO2
formed; hence, experimental measurements of the pressure of CO2(g) as a function of
time can be used to study the kinetics of reaction (5). With these considerations, the
following differential form of the pseudo-rate law is the correct model:
−dnCaCO3
= knCaCO3 (6b)
dt
where nCaCO3 = number of moles of calcium carbonate. The integrated form of the rate
law is
⎛ nCaCO ⎞ ⎛ nCO
final
− nCO2 ⎞
ln ⎜ 0 3 ⎟ = −kt ⇒ ln ⎜ 2
⎟ = −kt (7)
⎜ nCaCO ⎟ ⎜ final
nCO2 ⎟
⎝ 3 ⎠ ⎝ ⎠
where the stoichiometry of reaction (5) is given by
CaCO3 (s ) + 2H + ( aq ) → Ca 2+ (aq ) + CO2 (g ) + H2O ( liq )

nCaCO3 = nCaCO
0
3
−x ; nH + = nH0 + − 2 x nCa2+ = x ; nCO2 = x ; nH2O = x
= nCaCO
0
3
− nCO2
= nCO
final
2
− nCO2
The substitution in eqn. (7) is valid since at the end of the reaction, i.e., when t is very
large, the stoichiometry of the reaction predicts that
nCaCO3 = nCaCO
0
3
− x final = 0 , hence x final = nCaCO
0
3
final
and nCO 2
= x final = nCaCO
0
3
Using the ideal gas equation (PV = nRT) in eqn.(7) gives
⎛ PCO
final
V PCO2V ⎞
⎛ n − nCO2
final
⎞ ⎜ 2
− ⎟
ln ⎜
CO2
⎟ = −kt ⇒ ln ⎜ RT RT ⎟ = −kt
⎜ final
nCO ⎟ ⎜ final
PCO2 V ⎟
⎝ ⎠
⎜ ⎟
2
⎝ RT ⎠
Hence,
⎛ PCO
final
− PCO2 ⎞
ln ⎜ 2
⎟ = −k t (8)
⎜ PCOfinal ⎟
⎝ 2 ⎠
35
Focusing on eqn.(8), it is noted that it is the equation of a straight line (y = mx +b);
⎛ PCO
final
− PCO2 ⎞
hence a plot of ln ⎜ 2
⎟ versus t is predicted to give a straight line with a slope
⎜ P final ⎟
⎝ CO2 ⎠
–k. In this manner the specific rate constant k for the reaction is determined.
Once the rate constant k is known, it is possible to calculate an approximate
value of the activation energy Ea by use of the Arrhenius equation, given by
k = A exp (-Ea/RT) (9)
where A is a constant called the pre-exponential constant, Ea is the activation energy, T

is the absolute temperature and R is the gas constant.
Materials:
analytical balance 125 mL Erlenmayer flask

Vernier computer interface 1 liter beaker
Vernier Gas Pressure Sensor ~800 mL water
thermometer tubing
rubber stopper
III. Experiment
1. Set up the experiment as shown below.
Figure 1
2. Weigh a known quantity (0.01 – 0.05 g) of calcium carbonate and place it in the
flask.
36
3. Place the flask in a water bath and connect a Gas Pressure sensor to Channel 1
of the Vernier Computer interface. Connect the interface to the computer using
the proper cable.
4. Through a second hole in the stopper, add 1.5 mL of 1.0 – 2.0 M hydrochloric
acid.
6. Prepare to run the reaction and collect pressure data.
7. Gently shake the flask and click to begin the data collection. Gather
data till the pressure does not change.
8. Repeat the experiment at least three more times with different amounts of
calcium carbonate. Note that the number of moles of hydrogen ion is held large
and constant, according to the use of the isolation method.
9. The data should contain pressure-time graphs for four different amounts of
calcium carbonate used and the temperature at which the reaction was
performed.
10. Include in this section all graphs of raw data, and construct a table to display
raw data and experimental uncertainties.
IV. Calculations
Using theoretical considerations discussed in the theory, plot
⎛ PCO
final
− PCO2 ⎞
ln ⎜ 2
⎟ vs. t
⎜ final
PCO2 ⎟
⎝ ⎠
and determine the rate constant k from the slope. Calculate the activation energy Ea
from the Arrhenius equation. Tabulate values of k, Ea and the uncertainties in these
values, in a table. Assuming reaction (5) is pseudo first-order with respect to hydrogen
ion concentration, write the pseudo-rate law expression for the reaction.
V. Conclusion
Reference:
Adapted from Choi, Martin, M.F.; Wong, P.S., Experiment titled “Using a Datalooger To
Determine First-Order Kinetics and Calcium Carbonate in Egg Shells”, J. Chem. Ed. 81,
859, 2004.
37
Experiment 6
Determination of an Equilibrium Constant

Objectives
a) to experimentally investigate an equilibrium reaction and to determine the
equilibrium constant of a reaction.
b) to learn to define and use terms such as chemical equilibrium, equilibrium
constant.
(c) to plan and design an experiment to determine the equilibrium constant,
I. Introduction
In this experiment the absorbance of light by FeSCN 2+ is measured with a

Colorimeter when FeSCN 2+ is produced in the following equilibrium chemical reaction:
Fe 3+ (aq) + SCN − (aq) ! FeSCN 2+ (aq) (1)

light brown colorless dark red
Measurements of several (A, C ) pairs, where A is the Absorbance and C is the

concentration of FeSCN 2+ , are used to construct a calibration curve of Absorbance
versus known concentrations of FeSCN 2+ . This data is used
• to calculate the equilibrium constant of reaction (1) and
• to calculate the concentration of FeSCN 2+ from Absorbance measurements in an
unknown reaction equilibrium.
In addition, qualitative studies are conducted for the effect of adding certain chemicals
to reaction (1).
When a chemical reaction proceeds to completion, it can be assumed that the
reactants are quantitatively converted to products. However, there are many chemical
reactions that stop far short of completion. In these situations, it is concluded that
although the concentrations of the reactants and products changed as a function of
time, after a certain length of time no change in the concentrations of either the
reactant or the product is detected. Once this state is attained known, as the “chemical
equilibrium state”, an equilibrium constant can be calculated. Obviously, reactive
collisions of atoms and molecules which go to completion have an infinite equilibrium
constant, while for non-reactive collisions of atoms and molecules the equilibrium
constant is zero; there are a range of possibilities between these two extremes. From
the reaction kinetics point of view, the equilibrium position can be understood as a
point in time where the rate of the forward reaction is exactly equal to the rate of the
reverse reaction.
Consider a chemical reaction of the type,
38
nA A + nB B ! nCC + nD D
where A, B, C, and D represent atoms, molecules and/or ions and the ni are the
coefficients in the balanced chemical equation. The equilibrium constant K is
represented by the following equation:
nC nD
[C ] [D ]
K = n n
[ A ] [B ]
A B
where the square brackets indicate the concentrations of chemical species at

equilibrium.
Materials:
Vernier computer interface 0.200 M Fe(NO3)3 solution in 1.0 M HNO3
solution
computer 0.0020 M Fe(NO3)3 solution in 1.0 M
HNO3 solution
Vernier Colorimeter 0.0020 M SCN– solution in 0.10 M HNO3
Temperature Probe (optional) KSCN solution of unknown concentration
plastic cuvette in 0.10 M HNO3 solution
four 10.0 mL pipettes eight 100 mL beakers
pipet pump or bulb test tube rack
six 20 × 150 mm test tubes plastic Beral pipets
50 mL volumetric flask 0.1 M AgNO3, 1M Na3PO4, solid NaF
Concentrated HCl 0.1 M Hg(NO3)2, 0.1 M Na2C2O4 solution
II. Theory
Standard solutions; Concentrations of reactants at time t = 0:

Given a mixture of an aqueous solution of A, an aqueous solution of B, and
water, the resulting initial concentrations [A]0 and [B]0 are given by
nA nA nB nB
[ A]0 = ; and [B ]0 = ; (2)
Vsolution VA + VB + VH2O Vsolution VA + VB + VH2O
Colorimeter, Transmittance T, Absorbance A:

When light of intensity I0 travels a path length b through a cuvette containing a
liquid solution of concentration C, Beer’s law predicts that the light is attenuated, with
the fraction of light transmitted as I/I0 . According to Beer’s law,
⎛ I ⎞⎟ ⎛ I ⎞⎟ I
⎜ ⎜
log ⎜⎜ ⎟⎟⎟ α
⎜⎝ I ⎟⎠
(
−b C ) so log ⎜⎜ ⎟⎟⎟ = −ε b C and
⎜⎝ I ⎟⎠ I0
= 10−ε b C (3)
0 0
39
where the proportionality sign α is replaced by an equal sign and a constant ε, and
where the constant ε is called the molar absorptivity of the solution. The
quantity I/I0 is called the Transmittance T = I/I0 ; the Absorbance is defined
by A = log (1/T ). It follows that,
⎛ I ⎞⎟
⎜
( )
A = log 1 / T = log ⎜⎜ 0 ⎟⎟⎟ = log 10+ε b C
⎜⎝ I ⎟⎠
( ) (4)
Hence, the absorbance is
A = εb C (Beer’s law ) (5)
In this experiment, the stoichiometry of the following reaction is monitored by

measuring the absorbance of electromagnetic radiation (light in this case) by
FeSCN 2+ at different concentrations of FeSCN 2+ .
Fe 3+ (aq) + SCN − (aq) ! FeSCN 2+ (aq)

(6)
C−x x x
3+
Note that since Fe is a light brown color, SCN-‐ is colorless and FeSCN 2+ is a dark
red color, the most intense absorption lines are due to FeSCN 2+ . The procedure
requires an initial concentration of Fe3+ which is very much greater than the
concentration of SCN – ; SCN – is the limiting reactant. From the stoichiometry,
x = ⎡⎢FeSCN 2+ ⎤⎥ = ⎡⎢ SCN − ⎤⎥
⎣ ⎦ ⎣ ⎦
2+
A plot of Absorbance versus [FeSCN ] is expected to yield a straight line with a
positive slope, for example,
40
This curve can serve as a calibration curve to experimentally determine the
concentration of an unknown solution of the same reaction components. It is only
required to measure the Absorbance of FeSCN 2+ in the equilibrium reaction of the
unknown KSCN solution, then use the fitted curve A = m C + b to calculate C of the
unknown KSCN solution.
III. Experiment
Part I: Qualitative
Into a clean 400 mL beaker add 250 mL of distilled water, 1 mL of 1 M KSCN and
1 mL of 1 M Fe(NO3)3 solution. This stock solution will have an intense red color due to
the formation of the complex FeSCN2+. Obtain 10 clean medium-sized test tubes and
label them 1 through 9. Add 10 mL of this stock solution into each one of the test
tubes. Keep test tube 1 as a control and add the following reagents into test tubes 2
through 9 respectively:
2 2 mL 1 M Fe(NO3)3 solution
3 1 mL 1 M KSCN solution
4 0.5 mL (10 drops) 0.1 M AgNO3 solution
5 2 mL Conc. HCl solution
6 1 mL 1 M Na3PO4 solution
7 1 mL 0.1 M Na2C2O4 solution
8 several crystals of solid NaF
Cover each test tube with paraffin film and shake to mix. Compare the color intensity
of each of the test tubes with that of the control test tube 1. In each test record your
observations and make a table. Based on your observations, suggest a way to
determine the concentrations of the reactants and products at equilibrium.
Part II: Prepare and Test Standard Solutions
7. Label five 100 mL beakers (or other glassware) 1-5. Obtain 25 mL of 0.200M
Fe(NO3)3, 30 mL of 0.0020 M KSCN, and 220 mL of distilled water. CAUTION:
Fe(NO3)3 solutions in this experiment are prepared in 1.0 M HNO3 and should be
handled with care. Prepare four solutions according to the chart below. Use a 10.0
mL pipet and a pipet pump or bulb to transfer each solution to a 50 mL volumetric
flask. Mix each solution thoroughly. Measure and record the temperature of one of
the above solutions to use as the temperature for the equilibrium constant, Keq.
Complete the following table before proceeding:
Beaker 0.200 M Fe(NO3)3 0.0020 M SCN– H 2O Initial Conc. Of Initial Conc. Of

number (mL) (mL) (mL) Fe(NO3)3 KSCN
1 5.0 0.0 45.0
2 5.0 2.0 43.0
3 5.0 3.0 42.0
4 5.0 4.0 41.0
5 5.0 5.0 40.0
41
3. Connect a Colorimeter to Channel 1 of the Vernier computer interface. Connect the
interface to the computer with the proper cable.
5. Calibrate the Colorimeter.
a. Prepare a blank by filling an empty cuvette ¾ full with distilled water. Place the
blank in the cuvette slot of the Colorimeter and close the lid.
b. Click on EXPT, then set the wavelength on the Colorimeter to 470 nm, press the
CAL button, and proceed directly to Step 6. If your Colorimeter does not have a
CAL button, continue with this step to calibrate your Colorimeter.
c. Choose Calibrate } CH1: Colorimeter (%T) from the Experiment menu, then click
“one point calibration.” .
d. Turn the wavelength knob on the Colorimeter to the “0% T” position.
e. Type “0” in the edit box.
f. When the displayed voltage reading for Input 1 stabilizes, click .
g. Turn the knob of the Colorimeter to the Blue LED position (470 nm).
h. Type “100” in the edit box.
i. When the voltage reading for Input 1 stabilizes, click , then click .
6. You are now ready to collect absorbance data for the standard solutions. Click
to begin data collection. Note: Take readings within 4 minutes of preparing
the mixtures.
a. Empty the solution from the cuvette. Using the solution in Beaker 1, rinse the
cuvette twice with ~1 mL amounts and then fill it ¾ full. Wipe the outside with a
tissue, place it in the Colorimeter, and close the lid. Wait for the absorbance value
displayed in the Meter window to stabilize. Click , type the concentration
of FeSCN2+(obtain from table) in the edit box, and press the ENTER key
b. Discard the cuvette contents as directed. Rinse and fill the cuvette with the
solution in Beaker 3. Follow the procedure in Part a of this step to measure the
absorbance, and enter the concentration of this solution.
c. Repeat Part b of this step to measure the absorbance of the solutions in Beakers
4 and 5.
d. Click when you have finished collecting data to view a graph of
absorbance vs. concentration. Click the examine button, , and record the
absorbance values for each data pair.
7. Click the Linear Fit button, . A best-fit linear regression line will be shown for your
five data points. This line should pass near or through the data points and the origin
of the graph. (Note: Another option is to choose Curve Fit from the Analyze menu,
and then select Proportional. The Proportional fit has a y-intercept value equal to 0;
therefore, this regression line will always pass through the origin of the graph).
Leave the graph and best fit line displayed and proceed to Step 8.
Part III: Test an Unknown Solution of KSCN

8. Obtain about 10 mL of the unknown KSCN solution. Use a pipet to measure out 5.0
mL of the unknown into a clean and dry 100 mL beaker. Add precisely 5.0 mL of
42
0.200 M Fe(NO3)3 and 40.0 mL of distilled water to the beaker. Stir the mixture
thoroughly.
9. Using the solution in the beaker, rinse a cuvette twice with ~1 mL amounts and
then fill it ¾ full. Wipe the outside with a tissue, place it in the Colorimeter, and
close the lid. Watch the absorbance readings in the Meter window. When the
readings stabilize, record the absorbance value for your unknown in your data table.
Remove and clean the cuvette.
10. Determine the concentration of the SCN– in unknown solution.
j. With the linear-regression curve still displayed on your graph, choose Interpolate
from the Analyze menu.
k. A vertical cursor now appears on the graph. The cursor’s concentration and
absorbance coordinates are displayed in the floating box.
l. Move the cursor along the regression line until the absorbance value is
approximately the same as the absorbance value you recorded in Step 9. The
corresponding concentration value is the concentration of the unknown solution,
in mol/L. Record this value in your data table.
Part IV: Prepare and Test Equilibrium Systems

11. Prepare five 50 mL Erlenmeyer flasks of solutions, according to the chart below.
Follow the necessary steps from Part I to test the absorbance values of each
mixture. Record the test results in your data table. Note: You are using 0.0020 M
Fe(NO3)3 in this test.
Erlenmeyer Flask 0.0020 M 0.0020 M SCN– H2 O

number Fe(NO3)3 (mL) (mL)
(mL)
1 3.00 0.00 7.00
2 3.00 2.00 5.00
3 3.00 3.00 4.00
4 3.00 4.00 3.00
5 3.00 5.00 2.00
12. To get suitable data for the calculation of K, determine the net absorbance of the
solutions in Test Tubes 2-5. To do this, subtract the absorbance reading for Test
Tube 1 from the absorbance readings of Test Tubes 2-5, and record these values as
net absorbance in your data table.
This section should contain the table from part I, the graphs from parts II, and III, and
observations from part IV.
43
IV. Calculations
Concentrations:
As an example for calculating the initial concentrations of Fe(NO3)3 and KSCN,

consider the following portion of the chart in Part II-2:
Beaker 0.200 M Fe(NO3)3 0.0020 M SCN– H 2O Initial Conc. Of Initial Conc. Of

number (mL) (mL) (mL) Fe(NO3)3 KSCN
1 5.0 0.0 45.0
2 5.0 2.0 43.0 0.02 mol/L 8 x 10-5 mol/L
⎡Fe (NO ) ⎤ !
nFe(NO )
3 3
=
(0.200mol / L)(0.005L) = 0.02mol / L
⎣⎢ 3 3 ⎦⎥
2 V +VKSCN +VH O 0.005L + 0.002 + 0.043L
Fe(NO3 ) 2
3
⎡KSCN ⎤ ! nKSCN
=
(0.002mol / L)(0.002L) = 8×10−5 mol / L
⎢⎣ ⎥⎦ 2 V +VKSCN +VH O 0.005L + 0.002L + 0.043L
Fe(NO3 ) 2
3
Qualitative considerations:
a) Write the net ionic equations of any reactions that occur in test tubes 2 to 9
when chemicals 2-9 are added to the test tubes (Use the table below).
Complexes and Precipitates
Chemicals added to reaction (1) : Ag+, Hg2+ , Cl- , PO43 , F- , C2O42-

_________________________________________________________________
Possible products formed when the above chemicals are added to reaction (1):
FeCl4- FePO4 FeF63- Fe(C2O4)3- AgSCN(s) Hg(SCN)42-
Ag2C2O4(s)
________________________________________________________________
44
b) When equilibrium is re-established in the eight identical stock solutions after
addition of chemicals 2-9 (i.e., add Fe3+ to test tube #2, add SCN- to test tube
#3, etc.), use le Chatelier’s principle to predict whether the changes Δ[Fe3+] ,
Δ[SCN-], and Δ[FeSCN2+] are (+), (-) or (0). Write (+), (-) or (0) in the chart.
Fe3+ SCN- Ag+ Cl- Hg2+ PO43- C2O42- NaF(s)

3+
Fe
SCN-
FeSCN2+
Equilibrium constant:
Use data from part IV-11 to calculate the equilibrium constant for reaction(6).
Compute the average K and the uncertainty.
Concentration of unknown from graph:

Use the measured Absorbance for the unknown and the equation, A = m C + b ,
from the calibration curve, to calculate the concentration C of the unknown.
V. Conclusion
45
Experiment 7
Acids and Buffers

Objectives
(a) to explore the properties and role of buffers in daily life.

(b) to investigate the acid contents of common beverages.
(c) to prepare and test two acid buffer solutions.
(d) to determine the buffer capacity of prepared buffers.
I. Introduction
A buffer is a mixture of a weak acid and its conjugate base, or a weak base and
its conjugate acid. A buffer’s function is to absorb acids (H+ or H3O+ ions) or bases (OH-
ions) so that the change in pH of the system is very small. The pH in which a buffer
solution is effective is generally considered to be in the range ( pK a -‐ 1) to ( pK a + 1),
where pKa is the negative of the logarithm of the equilibrium constant for an acid.
In many biological systems, buffers are critical. Blood plasma, a natural buffer in
humans, is a bicarbonate buffer that keeps the pH of blood between 7.2 and 7.6. The
pH of the intercellular fluid in human body is around 7.2 and the pH of the fluid in the
stomach is very acidic ~1.0. With the intake of food, the pH of the stomach fluid
changes and can become more acidic. Antacid medication can then be taken which
contains bicarbonate and brings the pH close to the initial value.
In this experiment, a phosphate buffer will be prepared and the buffering

capacity of the prepared buffer will be tested.
Materials
Vernier computer interface 0.1 M sodium hydroxide, NaOH, solution
computer H3PO4 (aq)
Vernier pH Sensor NaH2PO4(s)
magnetic stirrer and stir bar Antacid solution
three 250 mL beakers Ring stand
100 mL graduated cylinder Utility clamp
25 mL graduated cylinder Distilled water
two 50 mL burets and two burets clamps
Balance
46
II. Theory
By design, a buffer is an equilibrium system, for example, a buffer can be
prepared with nitrous acid (HNO2) and its conjugate base (NO2-). This weak acid alone
establishes the equilibrium shown below.
HNO2 (aq) ! H + (aq) + NO2− (aq) (1)
with equilibrium constant expression given by,
[H + ][NO-2 ]
Ka = (2)
[HNO 2 ]
When NO2– is added to HNO2 the concentration of each component in reaction (1)
changes, but the equilibrium constant Ka remains constant. To prepare a buffer
system with nitrous acid, a conjugate base such as sodium nitrite (NaNO2) is added.
The resulting system is a mixture of HNO2, NO2–, and H+ ions.
If a strong base such as NaOH is added to a non-buffer (HNO2 alone), the pH
changes dramatically, but when added to the buffer (HNO2 + NaNO2), the following
reaction serves to resist a change in pH of the buffer:
OH − + H + (buffer ) ! H2O
If a strong acid such as HCl is added to a non-buffer (HNO2 alone), the pH changes
dramatically, but when added to the buffer, the following reaction serves to resist a
change in pH of the buffer:
H + + NO2− (buffer ) ! HNO2
Another form of eqn. (2) is obtained by first taking the logarithm of each side of
this equation to give
+ [NO-2 ] + [NO-2 ]
log K a = log [H ]+log or log [H ] = log K a −log
[HNO2 ] [HNO2 ]
By multiplying the latter equation by a minus sign, it becomes
[NO-2 ]
−log [H+ ] = −log K a + log
[HNO2 ]
For any chemical concentration (e.g., H+ ) or equilibrium constant (e.g., Ka ), the “p” of
that quantity is defined by pH ≡ −log ⎡⎢H + ⎤⎥ , pOH ≡ −log ⎡OH − ⎤ and pK ≡ −logK ,
⎢⎣ ⎥⎦
⎣ ⎦ a a
hence
47
[NO-2 ]
pH = pK a +log (3)
[HNO2 ]
The above equation for pH of the solution is called the Henderson-

Hasselbach equation; it is useful for calculating the pH of a buffer solution.
III. Experiment
Part I: Qualitative (Exploring Buffers)
1. Take 25.0 mL of three different beverages in three separate beakers. Fill the
burette with 0.1 M sodium hydroxide.
2. Connect the pH sensor with the interface and the computer and calibrate the pH
probe. Measure the initial pH of beverage A.
3. Add sodium hydroxide step wise to beverage A, and find out the volume of
sodium hydroxide required to bring the pH of beverage A to 7.0.
4. Repeat the experiment for beverages B and C.
5. Record your observations in the table below.
Beverage A Beverage B Beverage C

(pH)initial
Volume of NaOH
when pH = 7
Part II: Prepare and Test Buffer Solution A

2. Write down the procedure to prepare 100 mL of the phosphate Buffer with a pH of
2.0.
3. Set up two burettes, buret clamp, and ring stand (see Figure 1). Rinse and fill one
buret with cola product. Rinse and fill the second buret with anti-acid solution.
4. Use a pipet to measure out 10.00 mL of the Buffer solution into a 250 mL beaker
and add 15 mL of distilled water. Place the beaker on a magnetic stirrer, beneath
the buret of cola, and add a stirring bar. If no magnetic stirrer is available, you will
stir with a stirring rod during the testing.
48
5. Connect a pH Sensor to Channel 1 of the Vernier computer interface. Connect the
interface to the computer using the proper interface cable. Suspend the pH Sensor
in the pH =2 buffer solution, as shown in Figure 1. Make sure that the sensor is not
struck by the stirring bar.
Figure 1
7.You are now ready to test Buffer. You will slowly and carefully add cola product to the
buffer solution.
a. Take an initial pH reading of the buffer solution. Click and monitor pH for
5-10 seconds. Once the displayed pH reading has stabilized, click . In the
edit box, type “0” (for 0 mL added). Press the ENTER key to store the first data
pair. Record the initial pH value in your data table.
b. Add a small amount of the cola product, up to 0.50 mL. When the pH stabilizes
click . Enter the current buret reading and press ENTER to store the second
data pair.
c. Continue adding the cola product in small increments that raise/lower the pH
consistently and enter the buret reading after each increment. Your goal is to
raise the pH of the buffer by precisely 2 pH units.
d. When the pH of the buffer solution is precisely 1 unit smaller/larger than the
initial reading, stop further addition of cola product.
7. Repeat Step 7, using the antacid solution in the other buret. (Do not discard
excess anti-acid).
8. Click . Print a copy of the first trial.
9. Repeat this experiment with another beverage and record your results.
10. Record your observations in the table below.
11.
49
Cola Anti-acid Unknown
Beverage
(pH)initial
V1 0 mL 0 mL 0 mL
(pH)2
V2
(pH)3
V3
--- --- --- ---
(pH)final
Vfinal
where
ΔpH = (pH)finial – (pH)initial
=2
IV. Calculations
Beverage A Beverage B Beverage C
(pH)initial (from data)
Δ(pH) = 7 - (pH)initial
[H+]initial (from pHinitial)
[H+]final 10-7M 10-7M 10-7M
Δ[H+]
Relative buffer capacity
(Scale: 1,2,3, with 3
implying the greatest
Buffer capacity
50
Experiment 8
Determination of the Concentration of an Acid

Objectives
a) to learn how to prepare a standard solution.
b) to distinguish primary and secondary standards.
c) to use the pH probe to monitor a chemical reaction.
d) to calculate a defined quantity from the experimental data.
e) to learn to work problems such as: “0.5 mole of hydrogen chloride gas is
bubbled through and dissolved in 0.25 L of water; calculate the molarity
of the aqueous hydrochloric acid.”
I. Introduction
Many acids are prepared by passing the corresponding gas through water. In
this process accurate determination of the concentration of the solution is not possible;
it can only be estimated. For example, to prepare aqueous hydrochloric acid, hydrogen
chloride gas is passed through water. Can you think of the possible scientific law that
can used to estimate the concentration of the hydrochloric acid?
One of the ways to determine the concentration of an acid is to react it with a

base of known concentration. This neutralization reaction lets you calculate the
concentration of the acid. Unfortunately, most bases are hygroscopic. Therefore, it is
not possible to prepare a solution of a base whose concentration is accurately known.
To determine the concentration of a base, an acid must be found whose solution can be
made with accurate concentration. This acid is known as a primary standard while the
base is known as the secondary standard.
A titration is a process to determine the volume of a solution needed to react

with a given amount of another substance. For example, a strong acid such as
hydrochloric acid and a strong base such as sodium hydroxide react to form an aqueous
solution of sodium chloride and water, with a pH of 7.0. When the number of
equivalents of acid equals the number of equivalents of base, the solution is
said to be at the equivalence point, this being the definition of the equivalent
point. Any further addition of the base causes a further increase in the pH (decrease
in H + concentration) solely due to the addition of base.
Generally, the pH values at the equivalence point differ depending upon the type
or nature of acid and the base. In this experiment, you will explore a chemical reaction
between (1) a weak acid and a strong base and (2) a strong acid and a strong base.
From the equivalence point, you will calculate the concentration of the base knowing
the concentration of the acid. The concentration of an unknown acid or base can be
determined by the titration method using the known concentration of the primary
51
standard. A hygroscopic substance can not be used as a primary standard (Why?). A
typical pH-Volume titration curve will look as shown below.
pH
Volume NaOH (mL)
Materials required for this experiment are as follows:
Computer Vernier Computer interface

Logger Pro Wash bottle
Vernier pH Sensor Distilled water
Ring stand Two 250 mL beaker
2, utility clamps Pipette (20 mL)
Burette (50 mL) Sodium hydroxide(pellets or solution)
Oxalic acid salt (powder) Hydrochloric acid (unknown)
Pipet pump
This experiment is designed to study a particular type of chemical reaction (acid-base)

by monitoring the change in pH as the reaction proceeds.
II. Theory
A very seldom used concentration unit, the normality, is particularly useful for
defining the equivalence point in an acid-base titration. Before discussion of normality,
however, the definition of molarity is presented. The molarity M is the ratio of the
number of moles of solute divided by the volume of the solution in liters, as given by
M=n solute /Vsolution
where n solute is the number of moles of solute and Vsolution is the volume of
solution in units of liters.
The normality N is defined in a similar fashion, namely by
N = n eqsolute / Vsolution
52
eq
where n solute = number of equivalents of solute. The number of equivalents is
defined in terms of the number of moles as follows:
eq
n =νn
where, for simple acids and bases, ν = # of replaceable H+ or OH− groups. For
example,
HCl ν =1
H2SO4 ν =2
H3PO4 ν =3
HNO3 ν =1
HC2H3O2 ν =1
NaOH ν =1
Ca(OH)2 ν =2
NH3 (aq) ν =1
Ca(OH)2 ν =2
CaCl2
Al(OH)3 ν=3
AlCl3
Hence,
N = n eqsolute / Vsolution
=ν n solute /Vsolutio
= ν M.
Therefore, once the molarity is known, it is a simple matter of multiplying the

molarity by ν in order to obtain the normality (units = equivalents per mole).
In titration reactions of acids and bases, the equivalence point is defined as

the point where
n eqacid = n eqbase
eq
or, upon rearranging N = n solute / Vsolution,
NA VA = NB VB or ν AMA VA = νB MB VB
III. Experiment
1. Prepare 100 mL of standard solution of oxalic acid which is 0.05 M. (For the
procedure, you may refer to your text book). Oxalic acid is used as the primary
standard.
2. Prepare 200 mL of approximately 0.1 M solution of sodium hydroxide.
53
3. Calibrate the pH Sensor (see instructions – Appendix C, p.70)
4. Place 20 mL of 0.1 M oxalic acid solution into a 250 mL beaker. Add 3 drops of
phenolphthalein acid-base indicator.
5. Use a utility clamp to suspend a pH sensor on a ring stand as shown in Figure 1.

Situate the pH sensor in the acid solution and make sure that the tip of the pH
sensor is fully covered by acid.
6. Obtain a 50 mL burette and rinse the burette with a few mL of the ~ 0.1 M
sodium hydroxide solution. Fill the burette to about the 0 mL mark. CAUTION:
Sodium hydroxide solution is caustic. Avoid spilling it on your skin or clothing.
Use diagram in previous experiment. Complete the box for the “volume” column.
Figure 1
7. Prepare the computer for data collection by clicking on the clock icon. Choose
events with entry under mode option. The pH reading should be between 1.0 and
2.0 for the acid solution.
8. You are ready to begin collecting data. Before adding the titrant, Click on
and monitor pH for 5-10 seconds. Once the displayed pH reading has stabilized,
enter the values of pH and the volume of the titrant (0 mL) in the spreadsheet.
9. This process goes faster if one person manipulates and reads the burette while
another person operates the computer and enters volumes.
a. Add the next increment of sodium hydroxide titrant (about 1 mL). When the
pH stabilizes, enter the corresponding values in the spreadsheet. You have
now saved the second data pair for the experiment.
b. Continue adding sodium hydroxide solution in increments of 1 mL and enter
the burette reading after each increment. Proceed in this manner until the
pH is 5.0.
54
c. When the pH value of approximately 5.0 is reached, change to increments of
a few drops. Enter a new burette reading after each increment. Note: It is
important that all increment volumes in this part of the titration be equal;
that is, one-drop increments.
d. After a pH value of approximately 10 is reached, again add larger increments
(1 mL), and enter the burette level after each increment.
e. Continue adding sodium hydroxide solution until the pH value is constant
(around pH = 12).
11. When you have finished collecting data, click . Dispose of the beaker
contents as directed by your teacher.
12. Print copies of the table and the graph.
13. Take 20 mL of hydrochloric acid instead of oxalic acid as indicated in step 2 and
repeat steps 3 through 10 to determine the concentration of hydrochloric acid.
Equivalence Point Determination: One way of determining the precise equivalence

point of the titration is to take the first and second derivatives of the pH-volume data.
The equivalence point volume corresponds to the peak (maximum) value of the first
derivative plot, and to the volume where the second derivative equals zero on the
second derivative plot.
Derivative on Logger Pro 3.8.4.2
To take the derivative on Logger Pro, the data acquisition must be stopped. Under
the heading “Data”, select “New Calculated Column.” Toward the bottom left of the new
window that pops up, select “Functions”, then “Calculus”, then “Derivative.” In the
middle button of this window, select “Variable” and “pH.” Click “Done” to complete the
process. To verify that Logger Pro did calculate the derivative, there should be a third
data column (most likely blue text) labeled “CC” (for calculated column) displayed in
Logger Pro to the right of your titration curve data. To plot this new data, right click on
the column and select “Graph Options” followed by “Y-Axis Column”, then select
“Calculated Column”, then hit “Done.” Repeat the process for the second derivative
(CC2). Print the data and perform calculations for the experiment.
14. Your raw data table for this experiment consists of the computer print-
out which has been cut and pasted onto your report. Attach the graphs after
the data table.
IV. Calculations
Provide detailed calculations of all molarities and molarities for sodium hydroxide
and hydrochloric acid. Include answers to the following questions in this section.
1. Write chemical and the net-ionic equations for reactions in this experiment.
2. Why is the pH increasing upon addition of sodium hydroxide and reaches a
constant value towards the end of the experiment? Explain.
55
3. Why is it required to take the derivative of the data to get the equivalence point?
4. Why not use sodium hydroxide to standardize hydrochloric acid?
V. Conclusion Refer to the lab write-up procedure.
56
Experiment 9
Electrochemistry: Voltaic Cells, Determination of

an Equilibrium Constant
Objectives
(a) to measure the redox potential of a chemical reaction using an electrochemical
cell.
(b) to learn the method of constructing voltaic cells and develop an
electrochemical series based on potential differences between half-cells.
(c) to learn the use of the Nernst Equation; calculate equilibrium constant.
I. Introduction
In Parts I and II of this experiment, a Voltage Probe is used to measure the
potential of a voltaic cell whose electrodes are copper and lead. Two different voltaic
cells each with unknown metal electrodes are then used, and through careful
measurements of the cell potentials, the unknown metals are identified. In Part III of
the experiment, measurements are made of the potential of a special type of voltaic cell
with identical electrodes; it is called a concentration cell. In the first concentration
cell, the cell consists of two copper (Cu) electrodes, one in each well of the cell, with
one well having a concentration c1 of CuSO4 solution (reduction occurs) and the other
cell also containing CuSO4 solution but with a concentration c2 (oxidation occurs). In the
second concentration cell, the cell consists of two lead (Pb) electrodes, one in each well
of the cell, with one well having a concentration c1 of Pb(NO3)2 solution (reduction
occurs) and the other cell containing a mixture of Pb(NO3)2 (concentration c2) solution
and KI (oxidation occurs). Most of the Pb2+ from Pb(NO3)2 and I- from KI, form the
precipitate lead iodide PbI2 , with the equilibrium between PbI2 (sol ) , Pb2+ and I- ions
given by
PbI2 (sol) ! Pb 2+ (aq) + 2I − (aq)
In this experiment, the Nernst equation is used to calculate the solubility product
constant, Ksp, for PbI2.
Materials
Vernier computer interface 0.10 M Cu(NO3)2 solution
computer 0.10 M Pb(NO3)2 solution
Voltage Probe 1.0 M CuSO4 solution
three 10 mL graduated cylinders 0.050 M KI solution
24-well test plate 1 M KNO3 solution
string 0.10 M X nitrate solution
Cu and Pb electrodes 0.10 M Y nitrate solution
two unknown electrodes, labeled X and Y steel wool
150 mL beaker plastic Beral pipets
57
II. Theory
Any chemical reaction involving the transfer of electrons from one substance to
another is an oxidation-reduction (redox) reaction. If the experimental arrangement
allows the electrons to flow through an external circuit, electrical work is done. In an
oxidation half-cell reaction, the reactant loses electrons and is said to be oxidized, but is
a reducing agent. In a reduction half-cell reaction, the reactant gains electrons and is
said to be reduced, but is an oxidizing agent. Consider the following redox reaction:
Zn(s) + Pb2+(aq) → Zn2+(aq) + Pb(s) (1)
This redox reaction can be divided into oxidation and reduction half-reaction, namely
Zn(s) → Zn2+(aq) + 2e− : oxidation half-rxn; Zn is oxidized; Zn is a reducing agent.
Pb2+(aq) + 2e− → Pb(s): reduction half-rxn; Pb2+ is reduced; Pb2+ is an oxidizing agent
Figure 1.
A voltaic cell (Figure 1) is a device used to separate a redox reaction into its two
component half-reactions in such a way that the electrons are transferred through an
external circuit rather than by direct contact of the oxidizing agent and the reducing
agent. This transfer of electrons through an external circuit produces an electric
current. Each side of the voltaic cell is known as a half-cell. For the redox reaction (1),
each half-cell consists of an electrode (the metal of the half-reaction) and a solution
containing the corresponding cation of the half-reactions. The electrodes of the half-
cells are connected by a wire along which the electrons flow through an external circuit.
In the cell, oxidation takes place at the zinc electrode, liberating electrons to the
external circuit. Reduction takes place at the lead electrode, consuming electrons
coming from the external circuit. By definition,
- the electrode at which oxidation occurs is called the anode; it has a negative sign.
- the electrode at which reduction occurs is called the cathode; it has a positive sign.
58
When all the concentrations in the zinc/lead systems are 1 molar and the
temperature is 250C, the cell voltage is 0.63 volts. It would be a monumental task to
assemble a list of all possible cells and report their voltage. Instead potentials are
tabulated for half-reactions. Since half-cell potentials cannot be measured directly, one
half-cell reaction serves as a standard and all other half-cell potentials are measured
relative to the standard. The process is to construct a cell with one electrode as the
standard electrode, then the cell voltage is measured. This voltage serves as the half-
cell voltage for the remaining cell. The standard chosen by convention is:
2H+ + 2e− → H2(g) ε 0 = 0.00 V
The notation ε 0 is called the standard electrode potential and is the assigned potential
of the standard hydrogen electrode when the concentration of H+ is 1 M and the
pressure of the hydrogen gas is 1 atm. The measured cell voltage using the standard
hydrogen electrode is therefore the half-cell potential of the other half reaction.
In the zinc/lead cell the measured potential of 0.63 volts can be deduced from
the sum of the potentials of the two half-reactions.
Zn → Zn2+ + 2e− ε 0 = +0.76 V
Pb2+ + 2e− → Pb ε 0 = -0.13 V

______________________________
Zn + Pb2+ → Zn2+ + Pb ε 0 = +0.63 V
Note: The sign of the standard reduction potential for the zinc half-reaction is reversed
to give the potential of the oxidation half reaction.
The Nernst Equation
The voltage difference between electrodes, the cell voltage, is also called the
electromotive force, or emf ( ε or ε cell ). Under standard conditions (25oC, 1M solution
concentration, a atm gas pressure), these voltages are known as Standard emfs ( ε 0 or
ε cell
0
).
In reality, standard conditions are often difficult if not impossible to obtain. The
Nernst Equation allows cell voltages to be predicted when the conditions are not
standard. Nernst developed the following equation while studying the thermodynamics
of electrolyte solutions:
59
⎛ 2.303RT ⎞⎟
εcell = ε0cell − ⎜⎜ ⎟ logQ (2)
⎜⎝ nF ⎟⎟⎠
In equation (2), R is the gas constant (8.314 J mole-1 K-1), T is the temperature
(Kelvin), F is Faraday’s constant (96,485 coulombs/mole), n is the number of electrons
transferred in the balanced oxidation/reduction reaction, and
n n
⎡C ⎤ C ⎡D ⎤ D
⎢ ⎥ ⎢ ⎥
Q = ⎣ ⎦ n ⎣ ⎦n for reaction nA A + nBB → nCC + nD D (3)
⎡ A⎤ A ⎡B ⎤ B
⎣⎢ ⎦⎥ ⎣⎢ ⎦⎥
At room temperature (250C, i.e., 298.15 K ), the Nernst equation becomes
⎛ 0.0591⎞⎟
εcell = ε0cell − ⎜⎜ ⎟ logQ (4)
⎜⎝ n ⎟⎟⎠
In equations (2) and (4), note that if Q = 1, then ε cell = ε cell

0
.
At equilibrium, εcell = 0 then Q→ K eq , and eqn(3) becomes
⎛ 0.0591⎞⎟
0= ε0cell − ⎜⎜ ⎟ logK eq
⎜⎝ n ⎟⎟⎠
Hence, measurement of ε cell

0
allows computation of the equilibrium constant Keq,
where
n ε0cell
K eq = 10 0.0591
(5)
Concentration Cell
For a concentration cell both electrodes are made of the same metal, e.g.,
copper. In this case the half-cell and cell reactions are
Oxidation Cu (s ) → Cu 2+ (c 2 ) + 2e−1 0
; EOX =− 0.34V
Reduction Cu 2+ (c1) + 2e−1 → Cu (s ) 0
; ERED =+ 0.34V
_____________________________________________________
Cell Cu 2+ (c1) → Cu 2+ (c 2 ) 0
; Ecell =0
60
Hence
⎛ 0.0591⎞⎟ ⎛ 0.0591⎞⎟ c 2
0
Ecell = Ecell − ⎜⎜ ⎟⎟logQ = 0 −⎜⎜ ⎟log
⎜⎝ n ⎟⎠ ⎜⎝ n ⎟⎟⎠ c1
⎛ 0.0591⎞⎟ c 2
= −⎜⎜ ⎟log
⎜⎝ n ⎟⎟⎠ c1
where c1 and c2 are concentrations of the indicated ions. For a known concentration
c1 and cell voltage measurement E 0, concentration c2 can be calculated. In addition
to a concentration cell with two copper electrodes, in this experiment a concentration
cell is also constructed with two lead Pb electrodes. The electrolyte solutions in this
case have Pb 2+ ions at concentration c1 being reduced and Pb 2+ ions at concentration
c2 being oxidized.
III. Experiment
Part I: Determine the Eo for a Cu-Pb Voltaic Cell
2. Use a 2-vial set-up as your voltaic cell. Use Beral pipets to transfer small amounts of
0.10 M Cu(NO3)2 and 0.10 M Pb(NO3)2 solution to two neighboring wells in the test
plate. CAUTION: Handle these solutions with care. If a spill occurs, ask your
instructor how to clean up safely.
3. Obtain one Cu and one Pb metal strip to act as electrodes. Polish each strip with
sand paper or steel wool. Place the Cu strip in the well of Cu(NO3)2 solution and
place the Pb strip in the well of Pb(NO)3 solution. These are the half cells of your
Cu-Pb voltaic cell. Wash hands!
4. Make a salt bridge by soaking a short length of string in a beaker than contains a
small amount of 1 M KNO3 solution. Connect the Cu and Pb half cells with the string.
5. Connect a Voltage Probe to Channel 1 of the Vernier computer interface. Connect
the interface to the computer with the proper cable.
6. Start the Logger Pro program on your computer. Open the file “20 Electrochemistry”
from the Advanced Chemistry with Vernier folder.
7. Measure the potential of the Cu-Pb voltaic cell. Complete the steps quickly to get the
best data.
a. Click to start the data collection.
b. Connect the leads from the Voltage Probe to the Cu and Pb electrodes to get a
positive potential reading. Click immediately after making the connection
with the Voltage Probe.
61
c. Remove both electrodes from the solutions. Clean and polish each electrode.
d. Put the Cu and Pb electrodes back in place to set up the voltaic cell. Connect the
Voltage Probe to the electrodes, as before. Click immediately after making
the connection with the Voltage Probe.
e. Remove the electrodes. Clean and polish each electrode again.
f. Set up the voltaic cell a third, and final, time. Click immediately after
making the connection with the Voltage Probe.
g. Click the Statistics button, . Record the mean in your data table as the average
potential.
Part II: Determine the Eo for Two Voltaic Cells Using Pb and Unknown Metals
8. Obtain a small amount of the unknown electrolyte solution labeled “0.10 M X” and
the corresponding metal strip, X.
9. Use a Beral pipet to transfer a small amount of 0.10 M X solution to a well adjacent
to the 0.10 M Pb(NO3)2 solution in the test plate.
10. Make a new salt bridge by soaking a short length of string in the beaker of 1 M
KNO3 solution. Connect the X and Pb half cells with the string.
11. Measure the potential of the X-Pb voltaic cell. Complete this step quickly.
a. Click to start the data collection.
b. Connect the leads from the Voltage Probe to the X and Pb electrodes to get a
positive potential reading. Click immediately after making the connection
with the Voltage Probe.
c. Remove both electrodes from the solutions. Clean and polish each electrode.
d. Set up the voltaic cell again. Connect the Voltage Probe as before. Click
immediately after making the connection with the Voltage Probe.
e. Remove the electrodes. Clean and polish each electrode again.
f. Test the voltaic cell a third time. Click immediately after making the
connection with the Voltage Probe.
g. Click the Statistics button, . Record the mean in your data table as the average
potential.
12. Repeat Steps 8-11 using the unknown and its corresponding electrolyte solution
labeled “Y”.
Cu/Pb Cell voltage Concentrations Concentrations

Voltaic cell of species in cell of species in cell
for oxidation for reduction
#1
#2
#3
62
X/Pb Cell voltage Concentrations Concentrations
#1
#2
#3
Y/Pb Cell voltage Concentrations Concentrations

#1
#2
#3
63
Part III: Prepare and Test Two Concentration Cells
13. Set up and test a copper concentration cell.
a. Prepare 40 mL of 0.050 M CuSO4 solution by mixing 2 mL of 0.5 M CuSO4 solution
with 38 mL of distilled water.
b. Set up a concentration cell in two vials by adding enough (to touch the salt
bridge) 0.050 M CuSO4 solution to one well and enough (to touch the salt bridge)
0.5 M CuSO4 solution to a neighboring well. Use Cu metal electrodes in each well.
Use a KNO3-soaked string or paper strip as the salt bridge, as in Parts I and II.
c. Click to start the data collection.
d. Test and record the potential of the concentration cell in the same manner that
you tested the voltaic cells in Parts I and II.
Cu/Cu Cell voltage Concentration c2 Concentration c1
concentration
Voltaic cell
#1
#2
#3
14. Set up a concentration cell to determine the solubility product constant, Ksp, of PbI2.
(a) Prepare 10 mL of 0.050 M Pb(NO3)2 solution by mixing 5 mL of 0.10 M Pb(NO3)2
solution with 5 mL of distilled water.
(b) Mix 9 mL of 0.050 M KI solution with 3 mL of 0.050 M Pb(NO3)2 solution in a
small beaker. In this reaction, most of the Pb2+ and I– will form the precipitate PbI2,
but a small amount of the ions will remain dissolved.
(c) Set up the half cells in neighboring wells of the 24-well test plate. Place 5 mL of
0.050 M Pb(NO3)2 solution in one half cell, and 5 mL of the PbI2 mixture, from the
small beaker, into an adjacent half cell. Use Pb electrodes in each half cell. Use a
KNO3-soaked string as the salt bridge.
(d) Test and record the potential of the cell in the same manner that you tested the
voltaic cells and the copper concentration cell.
15. Handle the electrodes and the electrolyte solutions as directed. Rinse and clean the
vials. CAUTION: Handle these solutions with care. If a spill occurs, ask your
instructor how to clean up safely.
64
Pb/PbI2 Cell voltage Concentration c2 Concentration c1
concentration
Voltaic cell
#1
To be calculated
#2
To be calculated
#3
To be calculated
IV. Calculations - Complete the following tables:

Average cell Uncertainty in Name of unknown
voltage cell voltage (reference table)
Cu/Pb cell xxxxxxxxxxxxxx
X/Pb cell
Y/Pb cell
Cu/Cu cell xxxxxxxxxxxxxx

Pb/PbI2 cell c2 = ±
Cell Oxidation half-cell reaction Reduction half-cell reaction

Cu/Pb
X/Pb
Y/Pb
Cu/Cu
Pb/PbI2
65
Cell Balanced Net Ionic Cell Reaction…………………
Cu/Pb
X/Pb
Y/Pb
Cu/Cu
Pb/PbI2
Include in the section for calculations answers for the following questions:
a) 1. Draw a diagram for the Pb/PbI2 cell.

2. Name electrodes and label with a plus or minus sign.
3. Indicate the electrode where oxidation occurs and the electrode where
reduction occurs.
4. Label the wire with an arrow to specify the direction of electron flow.
5. Write the names of ions and precipitates in solution.
6. Include a salt bridge and describe its’ purpose.
b) Perform the following calculations:
1. Note: PbI2 ! Pb2+ + 2I-

c2 2 c2
so [I-] = 2 c2 = ?
2. Ksp = [Pb2+] [I-]2 = (c2 ) (2 c2 )2 = 4 (c2 )3
3. The accepted value of the Ksp of PbI2 is 9.8 x 10-9. Calculate the percent
error for your experimental Ksp of PbI2 .
c) What is the difference between a voltaic cell and an electrolytic cell?
66
Appendix A
Common Laboratory Equipment
Some common laboratory equipment are depicted below. Some of these are
used for measurements, and these are described in the section on instruments.
However, some of these are not used for measurements, and these will be described
here.
Bunsen Burner
A Bunsen burner is shown in the figure below. It is used for heating at higher
temperatures than that which can be achieved by a hot plate. The rubber tube supplies
gas, where the screw at the bottom can be turned to control the rate of flow of gas into
the burner. The other end of the rubber tube is connected to the gas supply in the
laboratory. This gas supply is equipped with a
lever. If the lever is perpendicular to the gas
supply pipe, then it is closed; and if the lever is
parallel to the gas supply line, it is maximally
open.
The Bunsen burner allows air as well as gas

to enter to supply the flame. The amount of air
is controlled by turning the top part of the
burner above where the tube is connected. The
amount of air will affect the temperature of the
flame. The blue flame is the hottest.
To light the burner, use a device that

produces a spark. Do not use matches or a
lighter. Turn the lever on the gas supply in the
lab so that a small amount of gas flows.
Immediately use the spark to light the burner. You may then turn the lever for more
gas and change the settings on the burner.
Crucible
The crucible and lid are made of a material that can be heated to high
temperatures. Use this when you want to heat something to a high temperature. The
lid should be slightly tilted when heating.
67
68
69
Meter Stick/Ruler
Use: Length measurements for ordinary size objects or distances
Scale: Metric –1 mm between smallest lines (see figure below),

1 cm between largest lines
Uncertainty: ±0.05 cm
Calibration: Unless the meter stick is deformed or warped, assume that the
manufacturer calibrated it properly. However, for metal rulers, this is more of a
problem than for wood or plastic. Metals tend to expand or contract more
depending on the temperature.
Proper Technique:
The end of the meter stick is usually worn or not clear. Therefore, it is a good
practice to measure the length starting from the 1 cm mark, and to subtract 1
cm from the value you read from the other end.
Place the meter stick and the object on a firm surface. To read the meter
stick, cover one of your eyes and position your other eye so that a line drawn
from this eye to the point that you are reading is approximately perpendicular
to the meter stick. Estimate the last digit as shown in the example below.
The reading is 47.64 ± 0.05 cm. The second decimal digit of 4 is estimated.
70
Graduated Cylinder
Use: To measure the volume of a fluid
Scale: The smallest divisions are 0.5 ml for the graduated cylinder shown in the
Figure. Other graduated cylinders with different diameters or lengths may
have different scale divisions.
Uncertainty: ± 0.25 ml for the graduated cylinder shown in the Figure. Check the
graduated cylinder you use and take one-half of the smallest division for
the uncertainty.
Calibration: Unless the graduated cylinder is obviously defective, assume that it is

calibrated by the manufacturer.
Proper Technique:
Check the liquid in the graduated cylinder to make sure that there are no
bubbles; you may tap the cylinder to remove the bubbles. The level of the
liquid should have a parabolic shape, which is called the meniscus. Read the
volume at the bottom of the meniscus. The reading in the Figure is 20.3 ± 0.5
ml. The last digit of 3 is estimated, but any error is accounted for by the
uncertainty.
meniscus
71
Vernier Caliper
Use: Length measurements for small ordinary objects and distances less than
about 10 cm
Scale: Metric – 1 cm for the largest division

1 mm for the smallest division
Vernier – 0.9 cm equally spaced divisions located on the sliding part just below
the main metric scale
Uncertainty: ± 0.01 cm
Calibration: Assume that the manufacturer calibrated the caliper for accurate
reading at room temperature, unless it is deformed or visibly damaged
Proper Technique:
The caliper has two sets of jaws – the main jaws and the inside jaws (see the Figure
on the next page). Use the inside jaws to measure inner diameters of hollow tubes;
otherwise, use the main jaws.
Move the wheel to grasp the object, as shown. Do not excessively squeeze the
object. The first mark on the vernier scale indicates the reading on the metric
scale. The Figure shows a reading of between 4.5 and 4.6 cm. You obtain the
second (hundredths) decimal digit by finding the number on the vernier scale
where the marks of the vernier scale and the metric scale coincide. The
reading below is 4.56 cm. Read the scale with one eye closed, and where a
line drawn from your other eye to the reading is perpendicular to the caliper.
You must also obtain a zero reading for the caliper. This is the reading where
the jaws are as close together as possible. If the first mark on the vernier
scale is not aligned with the zero on the metric scale, then you must obtain a
reading that you subtract each time that you use the caliper. This reading may
be positive or negative, depending on whether the first mark on the vernier
scale is to the right or left of the zero on the metric scale, respectively. If it is
positive, then read the instrument normally. If it is negative, then find the
number on the vernier scale that coincides with a mark on the metric scale.
The negative reading is (10 – this number)/10 cm.
72
inside jaws vernier scale
metric
scale
wheel
main jaws
The reading is between 4.5 and 4.6 cm. The sixth

number coincides for a reading of 4.56 ± 0.01 cm.
73
Analytical Balance
Use: For mass measurements up to 210 grams. The advantage that the analytical
balance has over other balances is its precision. Use this balance if you require
great precision. Sometimes, this precision is not possible, as is the case of
measuring the mass of a chemical that is very volatile.
Scale: The scale is digital and the output is to the ten-thousandths of a gram (see
figure below)
Uncertainty: ± 0.0003 g
Calibration: You may calibrate the balance using an object whose mass is known very
accurately. You may also test whether the balance gives reasonable
results by measuring the mass of a standard object, whose mass is
approximately known. Otherwise, assume that the manufacturer
calibrated it.
Proper Technique:
The analytical balance is a delicate instrument; do not handle it roughly. It
should rest on a level surface. Turn it on by pressing on the lower left or right
on the front panel. Wait until the reading stabilizes to zero.
Gently open the door on the left or right side and place the object in the center
of the pan. It is best to avoid touching the object so as not to transfer any
oil or dirt; use tongs instead. Do not
press down on the pan. Wait until the
reading stabilizes. The example in the
figure shows a reading of 0.2336 ±
0.0003 g.
Close the door after use. The instrument

will turn itself off automatically.
74
Top-Loading Balance
Use: For mass measurements up to 510 grams. This balance has less precision than
the analytical balance, but it is still precise. Use it when you require intermediate
precision
Scale: The scale is digital and the output is up to the hundredths of a gram (see figure
below)
calibrated it.
Proper Technique:
The balance should rest on a level firm surface. Turn on the balance by pressing
on the lower left or right on the front panel. Wait until the reading stabilizes to
zero.
Gently place the object on the center of the balance. Do not press down on the
balance. It is best to avoid touching the object so as not to transfer any oil or
dirt; use tongs instead. Wait until the reading stabilizes. The figure shows a
reading of 3.04 ± 0.01 g.
The instrument will turn itself off

automatically.
75
Triple-Beam Balance
Use: For mass measurements up to 610 grams. This is the least precise of the three
balances. Use this based on your precision requirements, and for objects greater
than 100 grams.
Scale: There are three scales – one from 0 to 10 grams, one from 0 to 500 grams in
steps of 100 grams, and one from 0 to 100 grams in steps of 10 grams. After
you balance the object, you add the reading from each scale to obtain the mass
of the object.
calibrated it.
Proper Technique:
Position the balance so that it is level. Check that it reads zero when it is empty
and all of the sliding masses are in the zero position. When the lever comes to a
stop, the horizontal lines must be aligned. If this is not the case, then turn the
screw on the left below the pan so that the horizontal lines are aligned.
Place the object in the center of the pan. It is best to avoid touching the object
so as not to transfer any oil or dirt; use tongs instead. Move the sliding masses
so that the lever is in a position where the horizontal lines are aligned; you must
wait until the lever comes to a stop. Make sure that the tens and hundreds
sliding masses are securely placed in the grooves. Add the masses from each
beam to obtain the mass of the object. Estimate the digit corresponding to the
hundredths of a gram by observing the distance between the smallest divisions
where the reading occurs.
screw to zero the balance horizontal lines
76
Barometer
Use: Pressure measurements
Scale: mm of Hg or inches of Hg
Uncertainty: ± 0.1 mm of Hg or ± 0.01 inches of Hg
Calibration: Assume that the instrument is calibrated by the manufacturer. However,

you can measure atmospheric pressure and it should be in the vicinity of
760 mm of Hg.
Proper Technique:
The picture on the top right shows the full barometer. There is a screw at
the bottom of the barometer to level the mercury – see the picture in the
bottom left. Turn the screw so
that the small white pointer
(cannot be seen in the picture) just
barely touches the mercury
(cannot be seen in the picture).
This is called zeroing the
barometer. The mercury level
forms a parabolic shape called a
meniscus. Position your eye level
to the bottom of the meniscus,
where you will read the scale.
Read inches on the right and mm
on the left, as shown. For the mm
side, note that the top number in
the figure is 800, so that the 90
actually means 790 mm.
pointer
leveling Screw
meniscus
inches mm
77
The reading on the main mm scale is between 734 and 735 mm of Hg. The
amount in between is found on the vernier scale. Find the number on the
vernier scale that aligns with a marking on the main scale. In this case it is
6, so the reading is 734.6 ± 0.1 mm of Hg. Do the same for the inches scale.
The reading is 28.80 ± 0.01 inches of Hg.
78
Appendix B
LOGGER PRO/LAB PRO
Instructions for Logger Pro
• Plotting and analyzing data points

• Launching Logger Pro with the interface
• Calculations
• Saving your work
• Formatting the Axes
Plotting and Analyzing Data Points
Suppose that you have collected data without the use of a sensor or with the use
of a sensor connected to the computer. You can use Logger Pro to plot and analyze
that data. Follow these instructions.
Launch Software Launch the Logger Pro software by double-clicking on the icon on
the desktop. Close the Tip of the Day dialogue box, if it appears.
Select Continue without Interface on the Connect to LabPro
dialogue box, then click OK. You should see two blank columns on
the left, labeled X and Y, and a set of coordinate axes on the right.
Label Columns You may re-label the column X by selecting, from the Menu bar, Data -
-> Column Options --> X. Change the Name and Short Name, and
enter the appropriate units. You may do the same for column Y.
Enter Data You can now click on a cell in one of the columns and start entering
data. As you enter a data point, it is automatically plotted. Data
points are automatically connected by lines. To remove this option,
double-click anywhere on the graph and de-select Connect Points from
the dialogue box, then select Done. To circle each data point, double-
click anywhere on the graph and select Point Protectors.
Format Axes Double-click anywhere on the graph. Select Axes Option to change
label or to choose autoscale or to enter your own scale. Select Done
when you are finished.
You may also choose which column to plot on which axes. Click on the
label on the x- or y-axis and select the column that you wish to plot on
that axis.
79
Calculations You may create a new column to calculate a quantity using the values
in the other columns. From the Menu bar, choose Data --> New
Calculated Column. Enter the Name, Short Name, and Units for the
new column. Enter the formula for the new calculated quantity on the
Equation line; use the pop-down Variables when you want to insert the
value from another column and use *, /, +, -, or an operation from the
Functions button in your formula. Click on Done when you are
finished. The new column should now appear to the right of the other
columns with the calculated values. To change the formula, go to
Data --> Column Options --> Name of Column.
Statistics The Stat button allows you to perform statistics on selected data
points. Click and drag to select the data points on the graph, and
press the Stat button. A box appears with information on maximum,
minimum, mean, median, standard deviation, and number of points.
This feature is useful, for example, in finding the average of
measurements after the value has stabilized to an equilibrium, such as
measuring the freezing point.
Linear Fit You may want to try a linear fit to some or all of the data. Click and
drag on the graph to select the data points that you want to include in
the fit; they will become shaded. From the Menu bar, choose Analyze
--> Linear Fit. The software uses the Method of Least Squares to
determine the best fit line, which is drawn. A box appears with the
values of the slope, intercept, and correlation. Click on the x in the
upper left corner of this box to delete the line and the fit.
Curve Fit You may want to try to fit the points to a curve. From the Menu bar,
select Analyze --> Curve Fit. Choose a type function from the General
Equation box, or define your own function by clicking on the Define
Function button (use the Short Name for the variable when you define
your own function). Press the Try Fit button. The best-fit values for
the parameters appear on the right with the RMSE value in the lower
right. The RMSE value is a number that relates to how close the data
points are to the curve – the higher the number, the further away the
data points are. Use this number to compare different fits. You may
continue to try other functions; select the function and press the Try
Fit button. Select OK when you are finished. The fitted curve and a
box with the values for the parameters appear on the graph. You may
click on the x in the upper left of this box to delete the fit and the box.
Launching Logger Pro with an Interface
The interface box is a device that is shaped like a calculator. It is used as an

interface between the computer and a sensor. Sensors are used for specific
measurements. For example, you use a pressure sensor to measure pressure. Other
80
types of sensors include temperature sensor, pH sensor, force probe, and motion
detector, among others. However, the sensor does not connect directly to the
computer. It is first connected to the interface box, which is connected to the
computer. Follow the general procedures below to set up the system.
Connections Connect the interface to the computer using a cable with a USB
connection at one end and a round 8-pin connection at the other end.
The USB end connects to USB port on the computer. Plug the round
end of the connection cord into the interface box – there is only one
place that it will fit (you may need to slide a plastic cover out of the
way to make the connection).
Connect the AC Adapter to the interface box and to a power outlet.

You must use the AC Adapter that has the word Vernier on it with a
picture of a vernier caliper. If you use any other, you may cause the
interface box to burn out and not function properly.
You may now connect a sensor to the interface box. There are many
slots on the interface where sensors are connected. They are labeled
DIG/SONIC 1, DIG/SONIC 2, CH1, etc. Use a connection cord with
ends that resemble a telephone connector. Insert one end in the
appropriate slot in the interface box (it usually only fits into one type
of slot), and the other end in the sensor itself, if needed
Launch Software Launch the Logger Pro software by double-clicking on the icon on the
desktop. Close the Tip of the Day dialogue box, if it appears. You
need to tell the computer the port at the back or front of the computer
where the interface is connected. This port is usually com1. Select
this. If that does not work, try com2.
You need to inform the software which sensors are connected. Click
the ‘Lab Pro’ button. A picture of the interface box will appear. Click
the button that represents the appropriate slot, and select the type of
sensor that is connected.
Setting Up Under Experiment à Data Collection, you may set the length of time
to collect data, and the sampling rate (the number of data points
collected per unit of time). If you want to remove measuring as a
function of time, you may click on the button with an image of a clock
and select by events.
When the data is collected it is stored in columns that are displayed in

a data table on the left of the screen. The data is also usually
displayed graphically on the right of the screen.
81
Calculations
You may create a new column to calculate a quantity using the values in the other
columns. From the Menu bar, choose Data --> New Calculated Column. Enter the
Name, Short Name, and Units for the new column. Enter the formula for the new
calculated quantity on the Equation line; use the pop-down Variables when you want to
insert the value from another column and use *, /, +, -, or an operation from the
Functions button in your formula. Click on Done when you are finished. The new
column should now appear to the right of the other columns with the calculated values.
To change the formula, go to Data --> Column Options --> Name of Column.
Saving Your Work
Do not save any work on the hard drive of the computer. It may not be available
the next time you look for it.
You may save work as a Logger Pro 3 File. Use the File menu, and select Save or
Save As. You may double click on previously saved file to start the Logger Pro software
with previous work. The appropriate sensor does not have to be connected when you
work with previously saved files where you will use the software for data analysis as
opposed to data collection. If not, click on Ignore Sensors when a dialogue box pops
up. You can even work without the Lab Pro interface attached.
You may also save your work as a text file that can be opened using Excel, for
example. Select File à Export as Text. To open the text file in Excel, first launch
Excel. Open the text file in Excel. Click Next when a dialogue box pops up that says
that Delimiters have been found. Keep clicking Next, then Finish. The data will appear
in Excel, along with some preliminary stuff that can be deleted or edited.
82
Formatting the Axes
To format the axes, right click anywhere on the coordinate system to get a pull-down
menu with a list of options. The most important is Coordinate Graph Options and
Autoscale Graph. There are several options under these; some are self-explanatory,
such as the option not to connect the points. Play with the others to see what
happens. Under Coordinate Graph Options, you also have Axes Options, where you
may set the scale, and maximum and minimum.
You may also double-click anywhere on the numbers on an axis to get a dialogue box
to set the scale. You may set it to autoscale or you can set the scale manually.
You can change the variable that is on one of the axis. Click on the axis to see a list of
variables. Select the one that you want.
83
Appendix C
Calibrations
Pressure Sensor
The pressure sensor with an attached syringe is illustrated in the figure below.
For the situation shown, the sensor is measuring the pressure of the gas in the
syringe, which has a volume of 5.0 ± 0.5 ml, as measured from the position of
the front edge of the inside black ring.
Connections Attach the cord to an appropriate slot in the interface box (probably
CH1 or CH2); it is appropriate when it fits. By clicking on the Lab Pro
button after you have launched the Logger Pro software, check to
make sure that the Logger Pro software is informed that a pressure
sensor is connected and in which slot it is connected. See the section
Launching Logger Pro with an Interface.
Calibration
• Click on the Lab Pro button.

• When the image of the interface box appears, click on the button where
the pressure sensor is connected to get a pull-down menu, where you
select Calibrate.
• A Calibrate dialogue box appears; click on the Calibrate Now button.
• Enter the appropriate units, e.g., mmHg
• Expose the sensor box to the atmosphere (remove the syringe, if it
attached) and enter the reading from a barometer. Click on Keep.
• Go to Reading 2
• Push the plunger of the syringe to the 0-ml mark and connect it to the
pressure sensor. Pull the plunger all the way to the 20-ml mark (you will
have to hold it). This should correspond to zero-pressure. Enter 0 for the
pressure and click on Keep.
• Click on Done
84
Collecting Data
• If you want to measure the pressure as a function of time, then press Collect to
begin, and Stop to end; see the section on formatting the graph to change the
display
• If you do not want to measure the pressure as a function of time, then turn off
the timing mechanism by clicking on the button that has the image of a clock; if
you want to enter other data such as volume, select Events with Entry and one
column to represent volume (type name, short name, and units); go to the
remaining steps
• Click on the Collect button to begin data collection
• When the pressure reading has stabilized, click Keep
• Enter the volume or other data, and click OK
• Repeat for different volume or whatever variable
• Press Stop when you are finished collecting data
Uncertainty: ± 0.40 mmHg
Temperature Probe
The temperature probe is illustrated below. It is used as you would use a

thermometer for experiments.
Connections:
The long needle end is inserted into the system where you want to measure the
temperature. The other end is inserted into the Lab Pro interface, either CH1 or
CH2. By clicking on the Lab Pro button after you have launched the Logger Pro
software, check to make sure that the Logger Pro software is informed that a
temperature probe is connected and in which slot it is connected. See the section
Launching Logger Pro with an Interface.
Calibration:
• Click on the Lab Pro button

• When the image of the interface box appears, click on the button where the
temperature probe is connected to get a pull-down menu, where you select
Calibrate
• A Calibrate dialogue box appears; click on the Calibrate Now button
85
• Enter the appropriate units, e.g., 0C
• Insert the temperature probe into the center of an ice bath. Measure the
temperature of the ice bath with a thermometer and enter that value in the
dialogue box. Press Keep
• For Reading 2, insert the temperature probe into the center of a beaker
containing tap water. Measure the temperature with a thermometer and
enter this value in the dialogue box. Press Keep
• Repeat the procedure for another temperature, such as a beaker of hot
water. With this, you have a three-point temperature calibration
• Click on Done
Collecting Data
• Place the temperature probe in the center of the system for which you are
measuring the temperature; for a liquid, do not allow the probe to touch the
walls of the container
• If you want to measure the temperature as a function of time, then press Collect
to begin, and Stop to end; see the section on formatting the graph to change the
display
• If you do not want to measure the temperature as a function of time, then turn
off the timing mechanism by clicking on the button that has the image of a clock;
if you want to enter other data such as volume or pressure, select Events with
Entry and one column to represent volume or pressure (type name, short name,
and units); go to the remaining steps
• Click on the Collect button to begin data collection
• When the temperature reading has stabilized, click Keep
• If you have other data to enter, enter the them and click OK; if not, press Stop.
• Repeat for other data points for whatever variable you are collecting
• Press Stop when you are finished collecting data
Uncertainty: 0 – 400 C: ± 0.050 C

40 – 1000C: ± 0.10 C
PH sensor
Connect pH sensor to the channel 1 of the interface.

a. Click on Lab Pro icon on the screen.
b. Click on the pH Sensor and click on Calibrate icon. Click on Calibrate Now.
c. Insert the pH sensor into a solution of known pH and the voltage will be
shown on the window. Enter the known value of the pH in the box and
press .
86
d. Go to Reading 2. Now insert the pH sensor into a beaker containing a a
second solution of known pH. Once the voltage reading stabilizes as seen
on the window, enter the value and press . Click on Done.
Repeat the procedure at another solution of known pH. With this you have obtained a
three-point pH calibration.
Uncertainty: ± 0.005 units
Conductivity Probe
The Conductivity Probe can be easily calibrated at two known levels, using any of the
Vernier data-collection programs. The calibration units can be µS/cm (microsiemens
per centimeter).
• Connect the Conductivity Probe to the interface (channel 1).

• Click on Lab Pro icon on the screen.
• Click on the Conductivity Probe and click on calibrate icon. Click on
Calibrate Now.
• Enter appropriate units of conductivity (e.g., µS/cm) and Select the
conductivity range setting on the probe box: low = 0 – 200 µS, medium
= 0 – 2000 µS, and high = 0 – 20,000 µS. Note: If you are not sure
which setting to use, you may first want to start with a highest range and
go down depending on the value shown).
• Zero Calibration Point: Simply perform this calibration point with
the probe out of any liquid solution (e.g., in the air). A very small
voltage reading will be displayed on the computer. Call this value 0
µS.
Standard Solution Calibration Point: Place the Conductivity Probe into a standard
solution (solution of known concentration), such as the sodium chloride standard that is
supplied with your probe. Be sure the entire elongated hole with the electrode surface
is submerged in the solution. Wait for the displayed voltage to stabilize. Enter the
value of the standard solution (e.g., 1000 µS). Click on Done. With this method you
have calibrated the Conductivity Probe.
87
Appendix D
Frequently Asked Questions about Data Analysis
1. When I use my calculator or computer to calculate a quantity, how do I know

how many digits to keep from the result as shown on the display of the
calculator or computer?
2. How do I know if my results or measurements are good?
3. Do I need to repeat my measurement?
4. How does Logger Pro determine the best-fit line or curve?
5. How do I determine the uncertainty of a calculated quantity from the

uncertainties of the numbers used in the calculation?
6. How do I determine the best-fit line or curve to my data points?
7. What do I graph to get a straight line when it is obvious that the data points do
not lie on a straight line?
1. How do I compare numbers in science?
1. When I use my calculator or computer to calculate a quantity, how do I

know how many digits to keep from the result as shown on the display of
the calculator or computer?
This is essentially a question about the number of significant figures and

uncertainty. The principle here is that any calculated value cannot have less
uncertainty or more significant figures than the quantities used in the calculation.
Let us illustrate this idea with an example. Suppose you measured the
diameter, D, and length, L, of an object that is modeled as a cylinder, and you
measurements are
D = 0.85 ± 0.05 cm ,
L = 4.33 ± 0.05 cm .
Using the calculator, you now determine the volume from the known formula
for the volume of a cylinder, as follows,
πD 2 L π (0.85 cm )2 ⋅ 4.33 cm
Volume = = = 2.457059249 cm 3 .
4 4
88
Excel normally displays 7 figures, and will show 2.457059. You may set the number
of decimal digits that are displayed in Excel by selecting Format à Cells à Number,
and changing the number in the appropriate box. In Excel, the syntax for π is PI( ).
If your calculator does not have a button for π, then type 3.141592654 or calculate
cos-1(-1) with your calculator in the radian mode.
To answer the original question, note that you measured the diameter and
length to 2 and 3 significant figures, respectively. Therefore, the number of
significant figures of the calculated result is 2, which is the smaller of the significant
figures of the measured values. Your calculated volume is 2.5 cm3. If you will use
the volume for further calculations, then keep at least 1 more significant figure.
Therefore, for further calculations, use at least 2.46 cm3.
Another problem, in addition to determining the number of significant figures

of the calculated result, is to determine the uncertainty of the calculated result. Is
the uncertainty on the volume ± 0.05, the same as for the diameter and length. The
answer is no! One method to determine the uncertainty of the calculated result is to
determine the maximum and minimum. This method works when it is clear, from
the formula, how to get the maximum and minimum. For example, you obtain the
maximum that the volume could be by using the maximum diameter and maximum
length, as follows
π (0.85 + 0.05)2 ⋅ (4.33 + 0.05)

Volume max = = 2.79 cm 3 ,
4
where I have kept only 3 figures because of my previous analysis. Similarly, the
minimum that the volume could be is
π (0.85 − 0.05 )2 ⋅ (4.33 − 0.05 )

Volume min = = 2.15 cm 3 .
4
These calculations show that the volume is between 2.15 and 2.79 cm3, where the
best value is 2.5 cm3. The situation is pictured below:
0.35 0.29
2.15 2.5 2.79
where 0.35 and 0.29 represent the differences between the best value and the
minimum and maximum, respectively. The uncertainty is 0.32, the average value of
these differences. The volume is 2.5 ± 0.3 cm3.
2. How do I know if my results or measurements are good?
This is a question about accuracy or precision. The words accuracy and

precision, although similar in meaning in everyday English, have different meanings
89
in a scientific context. Before answering the question, you must decide whether you
are concerned about the accuracy or precision of the results or measurements.
In measuring physical quantities, one assumes that there is a true value. The
accuracy of the measurement is how close you came to the true value. Of course,
one does not a priori know the true value. Therefore, at times, a scientist will use a
value that is accepted by the scientific community to gauge the accuracy of a
measurement. This accepted value arises from the agreement of various
measurements by many scientists. If you are comparing your measurement with an
accepted value, you may say that your measurement is accurate if the accepted
value lies within the range determined by your uncertainty. For example, if the
accepted value is 4.75, a measurement of 5.1 ± 0.5 is more accurate than a
measurement of 4.635 ± 0.001.
The example above illustrates the scientific meaning of the term precision.
The second measurement is more precise because it is measured to more significant
figures. Thus, the uncertainty determines the level of precision. The uncertainty
can be determined by considering the instrumental uncertainty and/or by repeating
the measurement and calculating the standard deviation. Repeating the
measurement is a good idea when there are factors that affect the measurement,
which are beyond instrumental uncertainty.
The situation, however, is not as simple as stated above. How can the first
measurement in the example be considered accurate when it is not precise? Is the
result meaningful? One must strive for both accuracy and precision. An important
job of an experimentalist is to honestly determine the accuracy and precision of a
measurement. You should not overstate either in order to make your work seem
better than it is. You should find the level of accuracy and precision based on your
instruments and techniques.
3. Do I need to repeat my measurement?
To answer this question, you must consider the purpose of repeating a

measurement. In measuring physical quantities, one assumes that there is a true
value and the measurement process is to discover this true value. However, it is not
assumed that this process is perfect; there are factors that influence the result of a
measurement. Repeat the measurement in order to see how these factors affect
the outcome of the measurement. The variation of different measurements will
inform you about the precision of the measurement.
The instrumental uncertainty is one factor that affects the outcome of a

measurement. If other factors influence the measurement smaller than the
instrumental uncertainty, then repeating the measurement will not yield any
variation. In this case, there is no need to repeat the measurement, and the
instrumental uncertainty is the uncertainty of the measurement. This is usually the
90
case in measuring the mass using a balance. However, it is a good idea to check
this by repeating the measurement once.
On the other hand, if there are factors that affect the measurement greater
than the instrumental uncertainty, then repeated measurements will give a variation
of results. The best value of the measurement (not to be confused with true value)
is the average of the repeated measurements, and the uncertainty is a statistical
quantity called the standard deviation. If there are N measurements labeled,
x1 , x2 ,…, xN , then the formula for the standard deviation, labeled σ, is
N
(x − xi )2
σ≡ ∑
i =1 N −1
,
where x is the symbol for the average.
4. How does Logger Pro determine the best-fit line or curve?
Logger Pro uses a method called the Method of Least Squares. To determine
the best-fit line or curve, one needs a criterion. The Method of Least Squares
assumes the following criterion: out of all possible lines or curves, the best-fit line or
curve is the one that comes closest to all the points. This closeness is calculated by
summing up the square of the distances from each point to the line or curve. The
line or curve with the least sum of square of distances is the best-fit line or curve.
You may wonder why the method uses the square of the distances rather than
the distance itself. One answer is that the distance is calculated by finding the
difference between the y-coordinate of the point and the line or curve. You may
imagine that some points are above the line or curve and some are below. This
gives rise to distances, some of which are positive and some of which are negative.
Using the square of the distances makes everything positive and gives a better idea
about the closeness of the line or curve.
The mathematical procedure for implementing this criterion involves calculus

for finding the minimum sum of squares of distances. It also involves algebra. The
results are complex formulae for the best-fit slope and intercept, in the case of a
line. Logger Pro programs these formulae to calculate the best-fit slope and
intercept for you.
5. How do I determine the uncertainty of a calculated quantity from the

uncertainties of the numbers used in the calculation?
The procedure for doing this is called propagation of uncertainty. This procedure
is outlined in the answer to question 1. Refer to the answer to question 1.
91
6. How do I determine the best-fit line or curve to my data points?
The criterion for the best-fit curve or line is the curve or line that comes “closest”
to your data points. How is this closeness determined? It is determined from the
distances of the data points to the curve (by curve here I mean curve or line).
However, some of the data points will be above the curve (positive distance) and
some will be below the curve (negative “distance”). It is better to determine the
closeness by summing the square of the distances. Thus, if we define a quantity
∑ [y i − f ( xi ) ]
2
,
where (xi , yi ) is the ith data point and f is the curve that you are trying to fit to the
data, then the smaller this quantity, the better the fit. Note that the expression in
the square brackets is the distance between the ith data point and the curve. A
method of this type to determine the best-fit curve is called Method of Least
Squares.
How do you carry out the method of least squares in practice? Let us take the
example of a straight line. The idea is to examine all possible lines and to pick the
one that minimizes the expression above. The line is describes by its slope and
intercept. These quantities are called parameters. Thus the expression above can
be thought of as a function of the slope and intercept of the line. One can then use
calculus to find the values of the slope and intercept that minimizes the expression.
For those who are familiar with calculus, this means finding where the derivatives
with respect to the slope and the intercept are zero. You can do the same
procedure for other types of functions, once you define the parameters. A
polynomial of degree two has three parameters – the coefficient of the three terms.
The software – Excel or Logger Pro – are set up to perform the above procedure
and to determine the values of the parameters for the best-fit in the type of function
that you specify. They will not compare different types of function. For example,
you may use Logger Pro to determine the best-fit straight line. However, Logger
Pro will not tell you whether an exponential function is a better fit. To compare fits
in Logger Pro, use the R2 value for a straight line or the RMSE value functions that
are not straight lines. These values are related to the expression above with some
slight differences. For R2, the values that are closer to 1, the better; and for RMSE,
the smaller the better.
7. What do I graph to get a straight line when it is obvious that the data
points do not lie on a straight line?
Suppose that it is obvious that a graph of y vs. x is not a straight line. You may
graph other quantities, such as y vs. 1/x, or y vs. x2, or 1/y vs. x , etc. Each time,
you may try a linear fit either in Excel or using Logger Pro. The closeness of the
92
value of the correlation or R2 to 1 indicates the goodness of the fit. The idea of the
correlation is a concept from statistics.
To graph the other quantities, you will have to compute them. In Excel, you can
write a formula preceded by an equal (=) sign to compute another quantity. In
Logger Pro, you can get another column by choosing Data --> New Calculated
Column, and writing a formula (see the section of Plotting and Analyzing Data Points
not Obtained from a Sensor).
8. How do I compare numbers in science?
This depends on which numbers you are comparing and why. Possible numbers
for comparison include a measurement you made, a number that you calculated
from measurements or obtained from data analysis, a number you predicted from a
theory, a number that you obtained from the literature as an accepted value, or a
number from another person’s experiment. Reasons for comparing numbers include
checking to see whether your instruments are operating properly, testing the
predictions of a theory, testing to see if you can reproduce the results of an
experiment, and checking whether the technique you used is valid.
You can compare two experimental results for agreement or disagreement. (You
are not trying to determine who is right or who is wrong.) To do this, check
whether the ranges of the numbers, as determined by their perspective
uncertainties, overlap. If they overlap, then you have agreement. You may also get
more quantitative in the comparison by computing a percent difference (not error),
as follows
number 1 - number 2
% difference = × 100 .
average of the two numbers
You may also compute percent difference to compare your number to the accepted
value. In general, percent difference is a way to compare numbers without
specifying which is correct.
Another reason for comparing numbers is to test whether your instrument or

technique is working properly. The idea here is that you have a number from
another source (e.g., accepted value or theoretical value) that you assume is
correct. Your instrument or technique is set up to reproduce this result. Again, if
the ranges overlap, as determined from the uncertainties, then your instrument or
technique is assumed to be valid. A quantitative measure of the accuracy of your
technique or instrument is the percent error, defined as
your value - value assumed correct

% error = × 100 .
value assumed correct
93
You may also want to compare your number to the prediction of a theory, in
order to test the theory. Here, it is unknown whether the theory is valid, unlike the
situation above, where the theory is assumed valid and you are testing the
technique or instrument. To test the theory, you want to determine if the prediction
of the theory falls within the range determined by the experimental uncertainty.
You may also want to calculate a percent error to indicate the level of disagreement.
If you are satisfied that the experiment is correct, then the error is on the theory,
not on the experiment. In that case, the theory needs to be modified.
94

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Elementary Inorganic Chemistry

CHEM 112 Laboratory

Copyrighted Fall 2004

A. Laboratory Safety and Housekeeping

C. Guidelines for the Laboratory Report

4. Enthalpy and Entropy

5. Rate and Order of a Chemical Reaction 32

6. Determination of an Equilibrium Constant 38

7. Acids and Buffers 46

8. Determination of the Concentration of an Acid 51

9. Electrochemistry: Voltaic Cells, Determination of Equilibrium Constant 57

EYE PROTECTION IS MANDATORY WHILE WORKING IN THE

Become familiar with the procedures to be employed prior to their performance.

Be aware of potentially hazardous situations such as open flames, spills, etc.

Food and beverages are not allowed in the laboratory.

Ask permission to remove equipment or chemicals from cabinets or shelves.

Inform the professor or lab instructor of any spills immediately. Dispose of

Read the following required policies/procedures carefully before entering any

1. In case of fire or accident, notify the instructor immediately

5. Unauthorized experiments are prohibited.

6. Working alone in the laboratory is prohibited.

7. Horseplay or other acts of carelessness are prohibited.

a) When inserting glass tubing or thermometers into rubber stoppers,

b) Fire polish all sharp edges of broken glass.

c) Discard cracked or broken glass immediately.

d) NEVER heat a graduated cylinder with a burner flame.

18. Do not insert spatulas or pipets into reagent bottles.

20. WASH HANDS BEFORE LEAVING THE LABORATORY.

Person(s) who should be notified in the event of an accident:

Each laboratory report should be written individually, not as a group;

1. Introduction {(10 + 5 + 5) points}

2. Theory {(10 + 10) points}

3. Experiment {(5 + 10 + 5) points}

4. Calculations {(10 + 10) points}

5. Conclusion {(10 + 10) points}

Investigation for the Effect of Solute on the Physical

where n = n1 + n2 = the sum of the number of moles of components 1 and 2. If

ΔTfp = Tfp (solution) – Tfp (solvent)

2. Prepare the Computer for data collection.

3. Freezing point of water:

a. Transfer 10 mL of water into a test tube.

4. Click on to begin data collection.

6. Continue with the experiment until data collection has stopped.

Run nbutanol molality ΔTfp

Determination of the Molar Mass of a Compound Using a

Using this information, the equation ΔTbp = m Kb becomes

1. Use 500-mL beaker to prepare a water bath.

2. Calibrate the temperature sensors (see the instructions – Appendix C, p.68).

3. Determine the mass of clean and dry test tube.

W Vcyclohexane Boiling Pt ΔTbp

Run W #kg solvent ΔTbp M % error

% error = 100%|M(lit) – M(exp)|/M(lit)

The theory suggests another way of evaluating M,

slope = Kb / (#kg of solvent X M ) . In this way M = Kb / (#kg of solvent X slope ).

V. Conclusion. Refer to the lab write-up procedure.

Enthalpy of a Chemical Reaction

a) to measure the temperature change of the reaction between hydrochloric acid

Thermodynamics is the study of energy changes for macroscopic physical

Some of the foregoing statements can be expressed in mathematical form,

ΔHreaction + ΔHH O + ΔHcalorimeter = 0 (1)

ΔHP = nC P (Tfinal −Tinitial ) (2)

C P = Heat capacity at constant pressure P(units = Jmol -­‐ 1K -­‐ 1 )

Tfinal = final Kelvin temperature, Tinitial = initial Kelvin temperature

C P = Heat capacity at constant pressure P(units = Jmol -‐ 1K -‐ 1 )