CHM 1045L Lab Manual Fall 2016

CHM 1045L
General Chemistry I Laboratory

Experiment Packet
(Revised August 7, 2016)
Authors
Jose C. Barreto, Ph.D.
David Brown, Ph.D.
Kevin Davies, Ph.D.
Terry Dubetz, Ph.D.
Mustafa Mujtaba, Ph.D.
Austin Raabe, Ph.D.
John T. Reilly, Ph.D.
David Deiros, M.S.
Jacilynn Brant, M.S.
Rachel Campbell, M.S.
Enrico Avallone & Chemistry Faculty
1
Table of Contents
Laboratory Safety Contract
Experiments:
Solutions and Spectroscopy Unit:
o Density................5
o Chromatography.............12
o Concentration from Color.... 20
o Copper content in Brass ..27
o Solutions and Spectroscopy Exam.................33
Chemical Reactions Unit:

o Copper Hydrate..................34
o Molar Mass of Gas.................40
o Titration................... 44
o Alum Synthesis ...48
o Neutralization............. 54
o Missing Label Problem.................... 60
o Reactions Exam...61
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.

Wear Proper Protective Clothing: Long Pants, Shirt that covers the shoulders (Tee shirt). Wear shoes that cover
the foot completely, at all times in the laboratory (Sandals are NEVER allowed). If you cannot remember to wear
the proper shoes on the day of lab, put them in your car and leave them there for the semester!
Notify your instructor immediately if you are pregnant, color blind, allergic to any insects, or chemicals, taking
immunosuppressive drugs, or have any other medical condition (such as diabetes, immunological defect, etc.)
that may require special precautionary measures in the laboratory. Also notify your instructor if you wear contact
lenses.
Upon entering the laboratory, place all books, coats, purses, backpacks, etc. in the designated areas, not on the
bench tops.
Conduct yourself in a responsible manner at all times in the laboratory.
Follow all written and verbal instructions carefully.
Perform only those experiments authorized by the instructor. Unauthorized experiments are prohibited.
Observe good housekeeping practices. Work areas should be kept clean and tidy at all times.
Keep aisles clear. Push your chair under the desk when not in use.
Locate, and when appropriate, learn to use exits, fire extinguisher, fire blanket, chemical shower, eyewash, first
aid kit, broken glass container, and cleanup materials for spills.
In case of fire, evacuate the room and assemble outside the building, as directed by the instructor.
Do not eat, drink, smoke, or apply cosmetics in the laboratory.
Confine long hair, loose clothing, and dangling jewelry.
Cover any cuts or scrapes with a sterile, waterproof bandage before attending lab.
Students MUST wear laboratory safety glasses/goggles any time that chemicals, heat, or glassware is being used.
Eye protection must meet American National Standards Institute, Z87.1 (ANSI Z87.1). Safety glasses/goggles
protect eyes from chemical splashes and flying debris.
Never pipette by mouth. Always use mechanical pipetting devices.
Wash skin immediately and thoroughly if contaminated by chemical or microorganisms.
Do not use equipment without instruction.
Report all spills and accidents to your instructor immediately.
Never leave heat sources unattended.
When using hot plates, note that there is no visible sign that they are hot (such as red glow). Always assume that
hot plates are hot.
Use appropriate apparatus when handling hot glassware.
Keep chemicals away from direct heat or sunlight.
Keep containers of alcohol, acetone, and other flammable liquids away from flames.
Do not allow any liquid to come into contact with electrical cords. Always handle electrical connectors with dry
hands. Never attempt to disconnect electrical equipment that is crackling, snapping, or smoking. Keep cords out
of the sinks!
Upon completion of laboratory exercises, place all materials in the areas designated by your instructor.
Do not pick up broken glassware with your hands. Use a broom and dustpan, and discard the glass in the
designated glass waste containers; never discard with paper waste.
Wear disposable gloves when working with blood, other body fluids, or mucous membranes. Change gloves after
possible contamination or damage. Wash hands immediately after gloves are removed.
Place gloves, swabs, toothpicks, etc. that may have come in contact with body fluids in the Biohazardous Waste
container.
Leave the lab clean and organized for the next student.
ALWAYS WASH YOUR HANDS with soap prior to leaving the laboratory.

I, ________________________________, have read and agree to follow all of the safety rules set
forth in this contract. I realize that I must obey these rules to insure my own safety and the safety of
my fellow students and instructors. I recognize that my failure to abide by the safety rules may
result in exposure to damages to me, my fellow students and/or university property. As a
consequence thereof, I realize that I may be subject to liability for my actions related to the safety
rules. I will read the directions for each laboratory before starting the experiment.
I am aware that any violation of this safety contract that results in unsafe conditions may result in
being removed from the laboratory and/or dismissal from the course.
______________________________________
Student Signature
___________________
Date
Please list any known health problems; or characteristics that may be of laboratory safety concern,
such as handicap, hemophilia, color blindness, diabetes, pregnancy, bee sting, or other severe
allergy.
______________________________________________________________________________
______________________________________________________________________________
Person and phone number to be contacted in case of emergency.

_____________________________________________________________________________
Students Printed Name _________________________________________________________
Class___________________________________________ Lab Time______________________
Students Signed Name________________________________________ Date______________
(if student is a minor)

Parent/Guardian Signed Name___________________________________ Date______________
Density
Using the density of a mixture to determine its composition
Introduction:
Density is defined as mass per unit volume:
Eqn 1.
Density typically is reported with units of g/mL, but sometimes other units are used. It is correct to
say that a pound of Styrofoam possesses the same exact weight as a pound of lead, but we have all
developed an intuitive feeling that there is something fundamentally different about the two
materials. One difference is density. Due to this density difference a pound of Styrofoam will occupy
a much larger volume than the pound of lead. Every object has a measurable density because every
object, regardless of its state of matter, has a mass and occupies space.
Density is an intensive property. Since pure substances have a constant composition of parts, it is
fair to say that the density of a pure substance will be constant regardless of the size of the sample.
Similarly, a homogenous mixture of two components of fixed composition will also have the same
density regardless of the size of the sample. However homogeneous mixtures of different
composition will have different densities.
Solutions and the Calibration Graph

Today we will be making several solutions and constructing a calibration graph. In a solution, one
substance (the solute) is dissolved in another substance (the solvent). The solute is designated as
the minor component of the mixture. Concentration is the ratio of the solute to the solvent or the
ratio of the solute to the solution (i.e. solute plus solvent). The concentration unit we are using
today is molarity. Molarity is defined as the ratio of moles of solute (such as salt or a food dye
molecule) per one liter of solution:
Eqn 2.
If we know the relationship between density and concentration, measurement of the density will
allow us to calculate the concentration of the solute in the solution.
To construct the curve it is necessary to prepare a number of standard solutions of known
concentrations and calculate their densities. Commonly these standards are prepared by diluting a
stock solution using Eqn 3 below:
Eqn 3.
MbVb = MaVa
The subscripts b means before dilution and a means after dilution. Mb is the molarity of the
stock solution, Vb is the volume of stock solution used, Va is the total volume after water is added.
Assume that the volumes are additive. Calculate Ma. Remember to stir the solutions and describe
5
in your lab notebook how you prepared the standards. Your goal in preparing your standards is to
create a symmetrical graph, that is, you do not want all of the points grouped at either end of line.
After constructing the calibration graph and determining the relationship between density and
concentration, you will determine the concentration of an unlabeled Epsom salt solution.
Safety tip (Hazards): All solutions can be discarded down the sink with water. Always check with
your lab instructor.
Procedure:
Materials required:
Five 50 mL beakers:
One for source beaker (DI water)
Four for recording masses
MgSO4 (Epsom salt)
Top loader balance
A.
Two 10 mL Graduated
Pipets & Pipet filler
100 mL volumetric flask
Deionized (DI) water

Weigh boat
Unknown solution
Scoopula
Pure Liquid Density:

1. Pour (or squeeze) a small volume (~20 mL) of deionized water (DI) water into a clean 50 mL
beaker.
a. Note: this beaker will be the source for pure DI water. Use pipet to draw liquid from
this beaker. Do NOT insert pipet into Stock DI squeeze bottle to avoid
contamination.
2. Place a dry, empty beaker on the balance. Press On/Zero button. This will automatically
subtract the mass of the beaker from the liquid masses in the following steps. This process
is called taring.
3. Using the graduated pipet and pipet filler, transfer a sample of water to a dry, pre-tared
beaker. Record the volume to the correct number of significant digits. Record the total
mass of the water.
4. Empty and dry the beaker and repeat step 3 two more times. Use significantly different
volumes for your three samples. For best results, use approximately ~2mL, ~5mL, and
~10mL samples. Although the samples do not need to be exactly as listed, the actual
volume and mass measurements must be recorded to the correct number of significant
digits. The measuring device determines the number of significant figures.
B.
Solution Density, creating standard mixtures:
Make a MgSO4 stock solution
1. Tare an empty weigh boat. Using a scoopula transfer about 33 g of MgSO4 (aka Epsom salt)
into the weigh boat. Record the actual mass shown on the balance.
2. Place a dry, empty 100 mL volumetric flask on the balance. Tare the flask. Remove the flask
from the balance.
3. Carefully, transfer all of the salt from the weigh boat into the volumetric flask. Add a small
amount of water to the weigh boat, swirl and pour the water into the volumetric flask.
4. Add enough DI water to the flask to fill the bulb about full. Swirl to start dissolving the
salt. You may also want to place your thumb over the flask opening and invert the flask
several times to facilitate mixing.
5. When the salt is mostly dissolved, add water until the bottom of the meniscus is about
inch from the line (graduation) on the neck. Mix again.
6. When the salt is completely dissolved add water to raise the bottom of the meniscus to the
graduation.
7. Measure the mass of the solution. Record the mass in your lab notebook.
Creating standard solutions (aka Dilutions)
8. Place a dry, empty 50 mL beaker on the balance. Tare the beaker. Remove the beaker from
the balance.
9. Using the graduated pipet and pipet filler, transfer a sample of water to your tared beaker.
Record the volume from the graduated pipet.
10. Using a separate graduated pipet, transfer a sample of MgSO4 stock solution to the
graduated cylinder containing the water. Record the volume from the graduated pipet.
11. Weigh the beaker and contents. Record this mass.
12. Repeat steps 8 - 11 with a significantly different ratio of water and salt solution
For best results, for the two trials use mixtures:
more water than salt solution
more salt solution than water
Always record the actual mass and volume of water, salt solution, and the mixture
to the correct number of significant figures. The measuring device determines the
number of significant figures.
C.
Density and Mass Percent Water of Unknown Solutions:

1.
Place a dry, empty beaker on the balance. Tare the beaker.
2.
Use the pipet to collect a sample of the unknown. Record the volume pipetted.
3.
Dispense the sample of Unknown into the pre-weighed beaker and record the total mass
of beaker and contents.
Suggested Data tables

Remember this is just an organization suggestion. Collect data first, then work on calculations.
Data: Remember to record the correct number of significant digits!
Part A Data
Substance
Water
Water
Quantity
(with unit)
Volume (mL)
Mass (g)
Sample 1
Sample 2
Sample 3
Part B Data stock solution

Stock solution mass (g)
Part B Data standards
Substance
Quantity (with
unit)
Water
Salt solution
Total Mixture
(Salt + water)
Standard Mixture 1
Standard Mixture 2
Volume (mL)
Volume (mL)
Mass (g)
Part C Data unknown

Volume (mL)
Mass (g)
Remember to include units! Work calculations after ALL data has been collected to maximize time in
lab.
Calculations & Graphs:

Remember to adjust all calculations for significant figures using the rules in your textbook Appendix
II pages A-6 through A-9.
Part A
1. Calculate the density of each sample (Equation 1)
a. Calculate the mean density and standard deviation of the density for pure DI water. The
sample standard deviation equation is given below:
Sx
1
N 1i
xi
Remember standard deviation is an indication of precision

b. For Post-lab Write-up:
i. Look up accepted densities for pure water at 25C
ii. Calculate percent error for density of pure DI water.

% = (
) 100%
To measure accuracy, one method is to calculate the percent error. (Note! The %
in 100% is a unit)
2. Plot the mass vs. volume for each sample of water.
Mass (in g)
Plot the mass vs. volume means that mass will be the y-axis and volume will be the x-axis.
Always plot "y vs. x".
0
0
Volume (in mL)
A straight line should resultdraw the best straight line. The line of best fit does not
necessarily touch all or any data points. Calculate the slope (include units), y-intercept, and
correlation coefficient (R2 value). Recall that the slope (m in y = mx+b) is equal to rise/run or
y 2 y1
y
. The y-intercept (b in y = mx+b) can be found by plugging the
x
x 2 x1
calculated slope and the x and y values of a given data point into the equation y = mx+b and
solving for b. ***You will need to know how to calculate this for future labs as well. (Read
Appendix III section D page A-15 to A-16 in the textbook for more help. The R2 value is the
error analysis for the line of best fit. An R2 value equal to 1 is ideal.
m
Part B
1. Calculate the following for each mixture:
Density of the mixture, Equation 1: =
2. Calculate the moles of magnesium sulfate (MgSO4) in the stock solution by dividing the mass (in
g) used by the molar mass of the salt.
4 =
4
120.37 4 /
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3. Calculate the concentration of the stock solution using equation 2. Remember to convert the
volume of the stock solution to L first.
4. Calculate the concentration of each of the two standard solutions using the dilution equation
(Equation 3).
Density (in g/mL)
5. Create the calibration graph: Plot Density vs. Concentration (M) for all the solutions and pure
liquid. Graph should be formatted as:
0 M Pure water
Concentration (M)
Stock Solution Molarity
The density should be plotted on the y-axis and concentration should be plotted on the x-axis.
Include the mean density from part A on this graph, pure water is 0 M MgSO4. There should be
four data points (2 standard mixtures, stock solution, pure water). A straight line should result.
Draw the best straight line through all the data points. Calculate the slope and y-intercept.
Report the full equation for the line of best fit and correlation coefficient (R2). ***See note for
Part A graph.
Part C
1. Calculate the density of each sample.
2. The solutions made in part B are called standards. You will use the data pertaining to the
standards to characterize the unknowns. The graph from Part B is a calibration graph and will
allow you to determine the concentration of salt in the unknown solution for part C. Use the
linear equation from your graph in Part B to determine the concentration in your unknown.
Remember y=density; m=slope; x=concentration; b = y-intercept.
Discussion: Answer the discussion questions below:
1. Using your graphical data from part A, discuss the relationship between mass and volume.
What is the significance of the slope of the line in your graph?
2. Discuss how you used the graph from part B to determine the composition of the unknown.
How does increasing the amount of water in the mixture affect the density of the mixture?
Why?
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3. Suppose you were to determine the density of a solid and gashow will the procedures and
results differ from that of a liquid? Note: a good answer will address procedure differences
between all three states of matter and will compare density results for all three states of
matter.
For information on Measurement, Density, Precision and Accuracy please refer to Chapter 2
sections 2-3 in your textbook Chemistry: Structure and Properties.
For information on molarity and dilutions please refer to Chapter 9 section 2 of your textbook.
For information on significant figures in calculations please refer to Appendix II in your
textbook.
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Chromatography & Spectroscopy

Introduction:
Colored liquid solutions, such as prepared Kool-Aid, are homogeneous mixtures. These mixtures
have components that are thoroughly and uniformly mixed, which is why every sip of Kool-Aid
tastes just as sweet. Mixtures can be separated using differences in chemical and physical
properties of the mixture components. The three primary methods of separation are filtration,
distillation, and chromatography. We will use the chemical properties of the solution components
to separate the solution using chromatography. Remember chemical properties are due to both the
chemical formula and the arrangement of the elements (and their electrons) in the compound.
Chromatography
Chromatography separates compounds based on differences in attraction as compounds travel with
a liquid over a solid. Some components of the solution will be more attracted to the liquid and will
travel quickly along with the liquid. Some components of the solution will be more attracted to the
solid and will travel slowly with the liquid. This process can be easily seen with colored mixtures and
leads to the name "chromatography", which literally means "the writing of colors".
Paper Chromatography from Chemistry: The Central Science by Brown, et al. 12th ed.
Spectroscopy
One definition of spectroscopy is the study of the interaction of matter and radiated energy. In
an atom or a molecule, electrons can move between orbitals by absorbing or emitting a photon of
light. If an electron is to move from an orbital of lower energy to an orbital of higher energy, a
photon of light must be absorbed. Absorption of a photon provides the energy that kicks the
electron up the energy ladder. If the energy gap between the orbitals is small (Fig 1), then low
energy light (perhaps red) will be sufficient to move the electron up; if the energy gap is large (Fig
2), a higher energy (perhaps blue) is required.
From the preceding discussion it is easy to see that the energy gap between orbitals can be
estimated by observing the colors that are absorbed by a molecule, since the color of light is
12
directly related to its energy. Some electron energy gaps are so great, or so small, that they do not
fall within the visible spectrum and cannot be seen. These correspond to infrared (small gap) or xray (large gap) radiation. The color of a solution is produced by the absorption of one or more of the
colors (wavelengths) of the visible spectrum and the transmission of the remaining colors
(wavelengths). For instance, a green solution may absorb radiation between 650nm and 750nm or
at several wavelengths. The graph shown in Fig 3 is the spectrum of a solution of two compounds
dissolved in water.
Fig 3
Neither of the compounds is green, but the combination produces a green solution. It must be
emphasized that no electrons in the solution will absorb energy corresponding to green radiation.
Green photons are transmitted, not absorbed.
Electromagnetic Radiation (light)
Visible light (400 nm - 750 nm) is one form of electromagnetic radiation and comprises only a small
portion of the entire electromagnetic spectrum. "White" light is the entire visible light spectrum (all
colors of the rainbow, red-orange-yellow-green-blue-indigo-violet). The different colors become
easy to see when white light interacts with something that separates these wavelengths, such as
water droplets after a rain resulting in a rainbow. We perceive visible light as colors based on how
the individual wavelengths of light interact with molecules and structures in our eyes. Colored
opaque objects absorb most visible wavelengths and reflect light of a single color (wavelength).
Transparent objects (such as our Kool-Aid solution) also absorb some of the visible wavelengths but
the rest of the visible light is transmitted through the solution. The color we perceive is the sum of
the unabsorbed light.
Perceived colors may either be a pure single wavelength color resulting from a single electron
transition (such as from a single dye) or a mixture of colors resulting from multiple simultaneous
electron transitions (as with a mixture of dyes). In the visible region of light, energy increases
across the spectrum in the following manner: Red-Orange-Yellow-Green-Blue-Indigo-Violet, with
Red being the lowest, and Violet being the highest in energy.
In this experiment we will use chromatography to separate our colored solutions. Once separated
into multiple colored components we can further analyze each component separately with visible
spectroscopy. Visible spectroscopy measures the light that passes through a substance under
controlled conditions. In the spectrophotometers you will be using, a special light bulb will emit
visible light and with a prism, select a specific wavelength of that light to direct at your sample for
analysis with a detector. The light that passes through the solution is compared to the initial light
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entering the solution. Any light that did not pass through the solution is absorbed and matched the
energy level gap of certain molecules in the solution. If the light was in the visible light range, the
solution should appear colored. A basic spectrophotometer set-up is shown below.
Basic Spectrometer from Chemistry: Structure and Properties by Tro, 1st ed. Page 562.
Safety Tip (Hazards): Isopropyl alcohol solution is a flammable liquid; keep away from open flame.
All solutions will be collected in a waste container. Wear chemical splash goggles and protective
clothing and shoes.
Procedure:
Materials Required:
One 10mL Syringe
One C18 Sep-Pak column
One SpectroVis Plus and USB

Cable
Grape Kool-Aid unsweetened

solution. One pack per 2000mL
DI water
Isopropanol solutions (5%, 25%,
and 70%)
Four cuvets
Plastic dropping pipets
Two 150mL or 250mL beakers

or one of each
Four 50mL beakers

One LabQuest 2, cradle, and
power adapter
Three 25mL graduated
cylinders
LabQuest 2 Setup:
1)
If the LabQuest 2 has not already been setup and powered on, connect the USB cable to
the SpectroVis Plus and LabQuest 2.
2)
Put the LabQuest 2 in its cradle.
3)
Plug in the power adapter.
4)
Press and release the power button ( ) located at the top edge of the LabQuest 2.
Glassware and Solutions

1)
Fill one of the 50mL beakers with 20mL-30mL of Grape Kool-Aid solution.
2)
Fill one of the 50mL beakers with about 20mL of 5% isopropanol solution.
14
3)
4)
5)
Fill a 150mL or 250mL beaker with ~ 40 mL of DI (deionized) water.
6)
The other 150mL or 250mL beaker will be the waste container.
Part 1: Chromatography
1) Draw about 10mL of the 70% isopropanol into the syringe.
2) Attach the short end of the Sep-Pak to the syringe and push the isopropanol through the
Sep-Pak at a rate of 2 drops per second into the waste beaker.
3) Detach the Sep-Pak from the syringe and fill the syringe with about 10mL of DI water.
4) Attach the short end of the Sep-Pak to the syringe and push the DI water through the SepPak at a rate of 2 drops per second into the waste beaker. Steps 1-4 prepare the sep-pack
column for use.
5) Detach the Sep-Pak from the syringe and fill the syringe with exactly 10mL of the Grape
Kool-Aid solution.
6) Attach the short end of the Sep-Pak to the syringe and push the Grape Kool-Aid solution
through the Sep-Pak at a rate of 2 drops per second into the waste beaker.
7) Detach the Sep-Pak from the syringe and fill the syringe with about 10mL of the 5%
isopropanol solution.
8) Attach the short end of the Sep-Pak to the syringe and push the 5% isopropanol solution
through the Sep-Pak at a rate of 2 drops per second into one of the 25mL graduated
cylinders.
9) Detach the Sep-Pak from the syringe and fill the syringe with another 10mL of the 5%
through the Sep-Pak at a rate of 2 drops per second into the same 25mL graduated cylinder
until it appears all of the red dye has eluted from the Sep-Pak.
a. Elution involves washing a species through a column by continuous adding of fresh
mobile phase (either liquid or gas solvent).
11) Fill the 25mL graduated cylinder to the 25mL mark with DI water and stir the contents. This
is the red dye solution.
15
through the Sep-Pak at a rate of 2 drops per second into one of the empty 25mL graduated
cylinders.
14) If it appears that not all of the blue dye has eluted, repeat steps 12 and 13.
15) Fill the second 25mL graduated cylinder to the 25mL mark with DI water and stir the
solution. This is the blue dye solution.
through the Sep-Pak at a rate of 2 drops per second into the waste container.
18) Using the syringe, transfer exactly 10mL of the Grape Kool-Aid solution to the empty 25mL
graduated cylinder. Fill the cylinder to the 25mL mark with DI water and stir. This is the
diluted Kool-Aid solution.
Part 2: Spectroscopy
1)
Using a Plastic dropping pipet, fill the first cuvet with DI water and place the cuvet into the
SpectroVis Plus. Fill the second cuvet with the diluted Grape Kool-Aid solution. Fill the third
cuvet with red dye solution. Fill the fourth cuvet with blue dye solution. Note! Always fill
the cuvets to about 1/4 inch from the top of the cuvet.
2)
The screen of the SpectroVis Plus should be as shown below:
Tap Sensors and from the drop-down menu tap Calibrate. Tap USB
Spectrophotometer. Wait for warm up to complete (90 sec) and then tap Finish
Calibration. After Calibration Completed appears, tap OK.
3)
Replace the cuvet containing the DI water with the cuvet containing the diluted Grape KoolAid solution. Tap the start button (
complete tap the stop button (
).
4)
). The scan takes about 5 seconds and when
You should see two maxima in the graph. To obtain the maximum absorbance and the
wavelengths at each maximum tap the Left Examine Button (
) or the Right Examine
Button (
) to move the cursor on the graph. The absorbance will be displayed at the
16
top-right of the screen and the wavelength will be displayed at the bottom right of the
screen. Record the absorbance and wavelength data for the two peaks in Table 1.
5)
the
part
will
Send a screenshot of this graph to your FGCU email. Using the stylus, tap File and from
drop-down menu tap Email. You will need to print the graph and add to your notebook as
of the postlab analysis. Note: If you are writing a formal lab report on this experiment, you
additionally need the data table to create an Excel graph for the report.
6)
Replace the diluted grape Kool-Aid cuvet with the cuvet containing the red dye solution.
Tap the start button. A warning appears. Select Discard. When the scan is complete, tap
the stop button. Use the Examine buttons to find the maximum and then record the
lambda max and absorbance at the lambda max. Record the data in Table 1.
7)
Repeat step 5 & 6 with the blue dye solution. Note: you should have a total of three graphs.
7)
Pour all solutions in the waste beaker and dispose the waste as directed by you lab
instructor.
8)
Rinse the beakers, graduated cylinders, and cuvets with DI water and return them to the
location you found them.
9)
To obtain the wavelength ranges associated with the red, orange, yellow, green, blue,
indigo, and violet colors displayed on the graph use the Examine buttons to move the
cursor across the spectrum. Record the data in Table 2. Note that these are the
wavelengths absorbed, not transmitted or reflected.
10)
If this is the last lab period of the day, tap the home button ( ) and then tap the Systems
folder. Tap the Shut Down button and ignore the warning and tap OK.
17
Data Tables (Create these tables in your lab notebook):

Table 1
Lambda Max, max (nm)
Solution
Absorbance
Diluted Kool-Aid
Red Dye
Blue Dye
As indicated in Part 2 step 4 there should be two maxima for the diluted Kool-Aid solution.
Color
Table 2
Wavelength Range (nm): starting to end
Red
Orange
Yellow
Green
Blue
Indigo
Violet
Calculations:
1. For each max, calculate the energy of one photon. The fundamental equations for light,
energy and wavelength are:
=
=
Where c and h are the speed of light and Planks constant, respectively.
2. Calculate percent recovery for each dye extract using the grape Kool-Aid spectrum as the
starting value. Generically, percent recovery is calculated using this formula:
18

100%

Since absorbance is directly related to concentration, the ratio of absorbances will be the
same as the ratio of concentrations.
% =
Discussion Questions:
1)
Is your percent recovery greater than, equal to, or less than 100% both dyes from the 10mL
sample of Grape Kool-Aid? Discuss reasons why the calculated recovery might be either
high or low. Assume all calculations were done correctly.
2)
How does absorbance relate to wavelength? To determine the percent recovery, is it

important to measure the absorbances of the separated dyes at the same wavelengths
(max) as determined in the diluted Grape Kool-Aid solution? Explain.
3)
Why do you think the blue dye did not elute in the 5% isopropanol while the red dye did
elute? Hint: refer to the other experiment mentioned above and the supplemental pages on
Canvas.
4)
How do the colors absorbed by the dyes relate to the colors transmitted by the solutions?
For additional information read the following sections in the textbook: Chemistry: Structure and
Properties by Tro, 1st ed.
Chapter 3 section 3.2-3.3 (pages 64-76) for more information about light and electronic
structure
For help with graphs read Appendix III section D (page A-15-16) in the textbook.
Additional research may be necessary to answer the discussion questions.
19
Color and Concentration

Can solution color be used to determine concentration?
Introduction:
Beers Law
Beers Law states that the magnitude of the absorbance of photons in a colored solution is
directly proportional to the concentration (equation 1 below). In other words, the more molecules
there are to absorb photons, the higher the absorbance will be. In Beers law, A is the absorbance
(measured by use of a spectrophotometer), is the path length of the cell used in experiment and
will most often be equal to 1.00cm, is the molar absorptivity constant that is specific for a given
molecule, and c is the concentration (or molarity) in moles of solute per liter of solution.
(Eq 1)
A= c
Before we can apply Beers Law in the determination of the concentration of a colored substance,
we must first find the wavelength of maximum absorbance, that is, lambda max (max). This is
accomplished by plotting the absorbance vs. the wavelength as shown below (Fig 1):
Fig 1
As can be seen in Fig 1, the max for the compound is 628.30 nm.
A spectrophotometer was employed to generate the absorbance vs. wavelength spectrum. A
diagram of the components of a spectrophotometer is shown below in Fig 2:
Fig 2: Basic Spectrometer from Chemistry: Structure and Properties by Tro, 1st ed. Page 562.
20
The Calibration Curve

You will again be constructing a calibration curve to make determination about concentration of an
unknown. Instead of measuring masses and volumes like you did during the density experiment,
absorbance will be measured and related to the concentration via Beers law. If we know the path
length and the molar absorptivity constant, measurement of the absorbance will allow us to
calculate the concentration of the solute in the solution. If the molar absorptivity constant is not
known, we can create a calibration curve as illustrated in Fig 3:
Absorbance
Absorbance vs. Concentration
= Unknown
= Standards
Concentration (M)
Fig 3
To construct the curve it is necessary to prepare a number of standard solutions of known
concentrations and then measure their absorbances at the max. Commonly these standards are
prepared by diluting a stock solution. The new concentrations can be calculated using the dilution
equation Eq 2:
(Eq 2)
MbVb = MaVa
After measuring the absorbance of the commercial product, the calibration curve is used to
determine the concentration of the dye.
Safety Tips (Hazards): Solutions used are safe to dispose down the drain.
Procedure:
Materials Required:
One SpectroVis Plus and USB
Cable
One LabQuest 2, cradle, and

power adapter
Plastic dropping pipets

One pipet pump
Six cuvets
Six 50mL beakers:

One for DI water
One for pure stock
One for commercial product
Three for standard dilutions
Two 10mL graduated pipets
Kimwipes
7.75x10-6M
4.27x10-5M
3.69x10-5M FD&C Yellow #5
FD&C Blue #1
Iceberg Blue Mouthwash
FD&C Red #40
Diet Cherry 7-Up
Cepacol
21
LabQuest 2 Setup:
1)
If the LabQuest 2 has not already been setup and powered on, connect the USB cable to the
spectrophotometer (SpectroVis Plus) and to the LabQuest 2.
2)
Put the LabQuest 2 in its cradle.
3)
Plug in the power adapter.
4)
Press and release the power button ( ) located at the top edge of the LabQuest 2.
Determinations of wavelength of maximum absorbance (lambda max, max):

1)
Add about 40mL of DI water to one of the empty and dry 50mL beakers.
2)
Add about 40mL of the stock dye solution on your lab bench to one of the empty and dry
50mL beakers.
3)
Fill one cuvet with DI water. Fill another cuvet with stock dye solution. Note! Fill the cuvets
to about inch from the top.
4)
Place the cuvet containing the DI water into the spectrophotometer. Note! When placing
the cuvets in the spectrophotometer, align the arrow on the cuvet with the white arrow on
the spectrophotometer.
5)
The screen of the spectrophotometer should be as shown below (Fig 7):
Fig 7
Using the stylus, tap Sensors and from the drop-down menu tap Calibrate. Tap USB
Calibration. After the Calibration Completed message appears, tap OK.
22
6)
Replace the cuvet containing the DI water with the cuvet containing the stock dye solution.
Tap the start button (
). The scan takes about 5 seconds and when complete tap
the stop button (
). The screen should be similar to Fig 8. Move the cursor to the
point with highest absorbance. Record the lambda max (max) which is shown at the bottom
right column. Note that the lambda max displayed in Fig 8 may not be the same as the
lambda max for your dye. Record the lambda max.
record max
Fig 8
7)
So that you can associate the wavelengths of absorbed radiation with transmitted or
reflected colors, move the cursor across the spectrum 400nm to 750nm and record the
wavelengths and colors at 50nm intervals. To do this tap the Left Examine Button (
) or
the Right Examine Button (
) to move the cursor on the graph. The wavelength will be
displayed at the bottom right of the screen. Record the wavelength and color data.
Note that the colors on the screen are the colors of absorbed radiation. The colors of the
solutions are due to transmitted radiation. If the radiation that is absorbed is in the orangered region of the spectrum, the color you see will be in the blue-green region of the
spectrum.
8)
Send a text file of this data to your FGCU email so you can make an Excel graph for your
write up. Using the stylus, tap File and from the drop-down menu tap Email.
Preparation of the Calibration Standards

1)
Prepare the three other calibration standard solutions in three empty and dry 50mL
beakers. Use the 10mL graduated pipets and pipet pump to transfer the stock solution and
water to the beakers. Use one pipet for stock solution and the other pipet for water to
minimize cross contamination. Use different ratios of water to stock dye solution:
more stock dye than water
about equal amounts of stock dye and water
more water than stock dye solution
Record the actual volumes of stock dye solution and water used. The cuvets are small so the
total solution volume does not need to be large (~10 mL is sufficient).
23
2)
After adding the water and stock solutions to the beakers, remember to mix the contents.
Use dilution equation (Eqn 2) to calculate the concentrations of dye in each solution
created. Calculate Ma and record. Label the beakers.
3)
Using the plastic dropping pipets, transfer the three standards you prepared to three of the
cuvets. Note! Fill the cuvets to about inch from the top. Put the cuvets next to the
beakers so that you can identify the liquids in the cuvets.
Creating the Calibration Graph:

1)
Tap the file button and then tap open. Select the Conc From Color file and then tap
Open. When the warning message appears, tap Discard.
2)
Tap the screen and then tap Change wavelength. Key-in the lambda max wavelength of
your dye and then tap OK.
3)
Put the cuvet containing the DI water into the spectrophotometer. Tap the Sensors
button, the Calibrate button, the USB: Spectrometer button, allow warm up to run (90
seconds), and the Finish Calibration button. When the Calibration completed message
appears, tap the OK button.
4)
Tap the start button (

). Wait 5 seconds and then tap the KEEP (
)button
and enter the concentration, which in this case is zero and tap OK. Note! When placing a
new solution into the spectrophotometer, always wait a 5 seconds for the absorbance to
stabilize before tapping KEEP. Record the absorbance and concentration data for the DI
water.
5)
Replace the DI water with the stock dye and tap KEEP. Enter the concentration in
scientific notation. To do this for the blue dye, type in the given concentration 7.75E-6
(exactly as written) and then tap OK. If your dye is not blue, type in the concentration of
your stock solution. See materials list for concentrations of stock solutions. Remember to
use E notation instead of proper scientific notation for entering concentrations into the
lab quest.
6)
Record absorbance and concentration
7)
Repeat steps 5-6 for the remaining standards entering the concentration of each of the
standards in scientific notation (use "E" notation as directed in step 5).
8)
After the last standard, place the cuvet containing the commercial product into the
spectrophotometer but do not tap the KEEP button. Record the absorbance. After you
record the absorbance of the unknown, tap the Stop button.
24
9)
Tap Analyze, tap Curve Fit, tap the check-box, tap Chose Fit, tap Linear, and then
tap OK.
10)
Record the correlation coefficient, the slope, and the y-intercept.
11)
Use equation of line of best fit (y = mx + b) along with recorded absorbance to solve for
concentration of commercial product.
12)
Tap the File and the Quit button. Tap Discard.
13)
If this is the last lab period of the day, tap the home button ( ) and then tap the Systems
folder. Tap the Shut Down button. Ignore the warning and tap OK.
Data and Calculation Tables:

1. Create organized data tables in your lab notebook. Tables should be clearly labeled and
include units, if appropriate. You will need tables for the following
a. Wavelength and Color of light at 50 nm intervals covering the visible light spectrum
(400 nm 750 nm)
b. Creating standard solutions: Should include spaces for volume stock, volume water,
total volume, concentration of stock solution, and concentration of diluted solution.
You will need all of these values for a total of 3 dilutions.
c. Creating the calibration graph: Should include spaces for absorbance and
concentration for a total of 5 solutions (DI water, 3 dilutions, and stock solution).
Include an additional space for recording absorbance of commercial product.
2. Plot the absorbance vs. wavelength for your dye using Excel. Remember to include a copy of
the graph in your lab notebook.
3. Plot the absorbance vs. concentration using Excel. Include the line of best fit (linear
regression), equation of the line, and correlation coefficient (R2). Remember the correlation
coefficient is the error analysis for the line of best fit. Remember to include a copy of the
graph in your lab notebook.
Chemistry in Context:
Most plants use a green pigment named chlorophyll that functions to capture solar energy. The
photons absorbed by chlorophyll are converted to ATP by the plant in a series of energy
transduction steps, so that the sunlight that illuminates a plant becomes a direct source of energy.
Some plants capture other portions of the solar spectrum by using antenna pigments of different
colors, and then direct a transfer of the energy to chlorophyll. You have no doubt seen multicolored
plants and plants which are one solid color (other than green), but the most popular plant color is
25
clearly green. What photons does a green plant absorb? What would happen if you continuously
illuminated a green plant with green light?
1) Nickel(II) chloride solution is green in color. Using the color wheel as a reference, at what
wavelength would you set the spectrophotometer to analyze a sample of NiCl2 by Beers
Law. Explain your choice. In addition, explain why you think you see the green color for
the solution when you look at the solution in white light.
2) In a new set of experiments on your group's colored dye solution:
a) Explain how your calibration graph relates to Beers law.
b) A solution of your colored dye showed an absorbance of 0.400 when studied at the
wavelength you used in your experiment. What is the molarity of the solution?
Show your calculations.
c) A solution of your dye has a concentration of 1/8 of the stock solution. What is the
expected absorbance at the wavelength you used to analyze the commercial
product? Show your calculations.
3) The slope of the line is the proportionality between the absorbance and the concentration.
How would you determine the molar absorptivity constant? What units would it have?
4) The equation for your line has a nonzero y-intercept. Beers law does not have an analogous
term. Explain the discrepancy between your experimental best fit equation and the
theoretical Beers law equation.
For additional information read the following sections in the textbook: Chemistry: Structure and
Properties by Tro, 1st ed.
Chapter 3 section 3.2-3.3 (pages 64-76) for more information about light and electronic
structure
Chapter 9 section 2 (pages 304 - 306) for more information on molarity and dilution
calculations
26
Determining the Copper Content in Brass

Introduction
Brass is an interesting metal that has a wide variety of uses. It is a good example of how elements
can be combined to produce a new solid substance with a collection of properties that take
advantage of the best, or desired, properties of the individual elements.
Brass is a member of the family of solid substances called alloys. An alloy, simply put, is a mixture of
two or more solid elements. A mixture of molten copper and zinc is the simplest form of brass.
Commercial forms of brass may also contain small amounts of other elements such as nickel and
iron.
In this investigation, the objective is to determine how much copper is in a sample of brass. By
treating a brass sample with nitric acid, the neutral atoms will be converted to ionic form, which
allows for easier analysis.
Copper and nitric acid react according to the following equation:
2 HNO3(aq) + Cu(s)
Cu2+(aq) + 2 NO2(g) + 2 OH-(aq)
Figure 1: Copper reacting with nitric acid. Royal Society for Chemistry,
http://www.rsc.org/Education/EiC/issues/2011November/DissolvingCopperInNitricAcid.asp
After the brass sample has been converted to ions in aqueous solution, you will use a Vernier
SpectroVis Plus spectrophotometer to determine the copper content. However, this investigation
presents an interesting challenge because a sample of brass may contain as many as seven different
elements, which may interfere with a spectrophotometric analysis.
Safety Hazards: The nitrogen dioxide gas formed is a toxic, brown gas. Complete this reaction in
the hood. DANGER: Nitric acid causes severe skin burns, eye damage, and respiratory inflammation.
Wear goggles at all times. Immediately wash skin with lots of water if exposed. Wear gloves while using
27
the 6M HNO3 solution. Copper (II) nitrate, zinc nitrate, and iron (II) sulfate cause mild skin and eye
irritation.
Materials:
Commercial brass sample
Zn(NO3)2 solution
100 mL beaker
DI water
Five 50 mL beakers
Gloves
6 M HNO3
Fe(NO3)3 solution
Watch glass
100 mL volumetric flask
Six cuvets
Cu(NO3)2 solution
FeSO4 solution
10 mL graduated cylinder
Lab Quest 2 & SpectroVis unit
Forceps
INITIAL INVESTIGATION
The Initial Investigation is composed of three parts: (1) you will conduct the reaction of brass and
nitric acid; (2) you will measure the absorbance spectra of solutions of copper (II) nitrate, zinc
nitrate, iron (III) nitrate, and iron (II) sulfate; and (3) you will measure the absorbance of a set of
standard copper (II) nitrate solutions.
Part I Conduct the Reaction Between Brass and a Solution of Nitric Acid (HNO 3)
Work carefully and measure accurately. In Part I, you will convert the elements in a sample of brass
to their ionic forms to be able to determine the copper content.
Important: Wear goggles and gloves. Work in a fume hood.
1. Obtain a sample of brass. Use an analytical balance to measure the mass of the brass
sample. The sample should have a mass about 1 g.
2. Measure out about 10 mL of 6 M HNO3 solution. The nitric acid will be in excess. Transfer
the HNO3 solution to a small beaker (100 mL or 150 mL) and place the beaker in a fume
hood.
3. Carefully add the brass sample to the HNO3 solution. Cover the reaction vessel with a watch
glass. Note: While the reaction proceeds, continue to Part II.
4. After the reaction is complete, prepare and dilute the reaction mixture.
a. Carefully add 50 mL of DI water to the beaker.
b. Using forceps, carefully remove any undissolved solid. Rinse and dry with a paper
towel. Place into tared weigh boat/weigh paper. Record the mass.
c. Remove the beaker from the fume hood and transfer the mixture to a 100 mL
volumetric flask. Rinse the beaker at least three times with ~5 mL of distilled water
and pour the rinse into the volumetric flask.
28
d. Add distilled water to the mark on the flask. Save this flask of solution for testing in
the Final Investigation.
Part II Measure the Absorbance Spectra of Solutions

5. Obtain small volumes (~ 5 mL) of copper (II) nitrate, zinc nitrate, iron (III) nitrate, and iron (II)
sulfate solutions.
6. To prepare the SpectroVis Plus Spectrophotometer for use, connect it to LabQuest or a
computer. In the data-collection program, choose New from the File menu.
7. Prepare a blank by filling a cuvette 3/4 full with distilled water.
8. Calibrate the spectrophotometer.
a. Place the blank cuvette in the spectrophotometer.
b. Calibrate.
In LabQuest App, choose Calibrate USB:Spectrometer from the Sensors menu on the
Meter screen.
c. After the spectrophotometer warms up, select Finish Calibration, and then select OK.
9. Measure the absorbance spectrum of the copper (II) nitrate solution.
a. Remove the blank cuvette from the spectrophotometer. Refill the cuvette with the copper (II)
nitrate solution.
b. Start data collection. A full spectrum graph of the solution will be displayed. Stop data
collection.
c. Store the run.
In LabQuest, tap the File Cabinet icon.
d. Repeat Steps ac for the remaining three solutions.
10. Email a screen shot of the graphs.
a. Tap Run, choose All Runs
b. In LabQuest App, from the File menu, choose Email
Screenshot.
11. Dispose of all solutions as directed by your instructor.
Part III Create and Use Calibration Graph for Cu(NO3)2

12. Obtain about 40 mL of 0.10 M copper (II) nitrate solution. Use this as the stock solution from
which to prepare a set of 3 dilute solutions. Make sure to prepare the standard solutions in the
same range as the molar concentration of Cu2+ you expect to find in the reacted brass mixture.
29
13. In LabQuest App, examine the graph of absorbance vs. wavelength for the 0.10 M solution of
copper (II) nitrate from Part I of the Initial Investigation. Choose a wavelength that fits these
three criteria:
(1) the wavelength is 550740 nm
(2) the absorbance is 0.701.00
(3) none of the ionic species tested in Part II will interfere at the wavelength you choose.
Values that fit these criteria provide a more accurate measure of the Cu(NO3)2 solutions.
14. Set up the data-collection mode.
a. Tap the file button and then tap open. Select the Conc From Color file and then tap
Open. When the warning message appears, tap Discard.
b. Tap the screen and then tap Change wavelength. Key-in the lambda max wavelength of
your dye and then tap OK.
15. Collect absorbance-concentration data for the copper (II) nitrate standard solutions.
a. Fill a cuvette 3/4 full with the 0.10 M copper (II) nitrate solution and place the cuvette in the
spectrophotometer. Start data collection.
b. After the absorbance value displayed on the screen has stabilized, select Keep and enter the
concentration in mol/L. Select OK.
c. Remove the cuvette, pour out the solution and rinse the cuvette. Refill the cuvette with the
next copper (II) nitrate standard solution. Place the cuvette in the spectrophotometer.
d. After the value displayed on the screen has stabilized, select Keep and enter the
concentration in mol/L. Select OK.
e. Repeat Steps c and d for the remaining standard solutions.
16. After the last standard, place the cuvet containing a sample from your dissolved brass (from
volumetric flask) into the spectrophotometer but do not tap the KEEP button. Record the
absorbance. After you record the absorbance of the unknown in your notebook, tap the Stop
button.
17. Tap Analyze, tap Curve Fit, tap the check-box, tap Chose Fit, tap Linear, and then tap
OK.
18. Record the correlation coefficient, the slope, and the y-intercept in your lab notebook.
19. Send a screenshot of this graph to your FGCU email. Using the stylus, tap File and from the
drop-down menu tap Email. You will need to print the graph and add to your notebook as
part of the postlab analysis.
20. Use equation of line of best fit (y = mx + b) along with recorded absorbance to solve for
concentration of copper(II) ions in solution.
21. Tap the File and the Quit button. Tap Discard.
30
Note: If the conc from color file is missing or does not show USB: Abs @ XXX nm after opening
the file, use the following instructions to reset the file.
In LabQuest App, Tap Mode on the Meter screen. Change the Mode to Events with Entry. Enter
the Name (Concentration) and Units (mol/L). Select OK.
Part IV Record Absorbance Spectrum of Dissolved Brass Solution

Note: procedure identical to the Concentration from Color experiment.
22. The screen of the spectrophotometer should be as shown below:
23. Using the stylus, tap Sensors and from the drop-down menu tap Calibrate. Tap USB
Calibration. After the Calibration Completed message appears, tap OK.
24. Replace the cuvet containing the DI water with the cuvet containing the Dissolved Brass
solution. Tap the start button (
). The scan takes about 5 seconds and when
complete tap the stop button (
).
25. Send a screenshot of this graph to your FGCU email. Using the stylus, tap File and from
the drop-down menu tap Email. You will need to print the graph and add to your
notebook as part of the postlab analysis.
Data & Calculations

1. Create data tables in your lab notebook to record mass brass before and after reaction,
solution dilution information for standards, and calibration curve data and equation.
2. Calculate the concentrations of each standard created.
3. Using the absorbance of the dissolved brass solution and the calibration equation,
calculate the concentration of copper(II) ions in the sample.
4. Using the volume of the diluted brass solution (100 mL volumetric flask) and
concentration of copper(II) ions, calculate the number of moles copper in solution.
31
a. Remember, that molarity is in mol/L. Check volume units.

5. Calculate the mass of copper dissolved (in g) in the solution.
a. Remember to use the molar mass of copper.
6. Calculate the total mass of brass dissolved in g.
7. Calculate the percent copper in the brass sample.
=

100%

Discussion:
1. Consider the experimental procedure. What were the most likely sources of error?
Remember that experimental error is not the same thing as a calculation mistake or
incorrectly following the procedure.
2. Based the absorbance vs. wavelength spectrum of the dissolved brass solution, is there
evidence of the presence of elements other than copper and zinc in the brass sample? If
yes, what elements do think are present? Explain your answer.
Experiment modified from Vernier Chemistry Investigations for Use with AP Chemistry
http://www.vernier.com/products/books/apchem/
Vernier Software & Technology
13979 S.W. Millikan Way Beaverton, OR 97005-2886
Toll Free (888) 837-6437 (503) 277-2299 FAX (503) 277-2440
info@vernier.com www.vernier.com
32
Lab Exam
Solutions and Spectroscopy
This exam is a paper exam and will be cumulative over the first four experiments.
The exam is open notebook. You may use information written in or permanently attached to your
lab notebook. Other information sources are prohibited.
Do NOT write any information from the exam into your lab notebook. Scratch paper will be
provided.
Correct use of significant figures are required for all numerical answers. Answers must also
include units if applicable.
You may use a calculator. Graphing calculators are allowed.
You may use pencil for this exam.
1. You will need to know how to use Beers Law equation, Dilution equation, molarity equation,
percent error and percent composition equations.
2. You may be asked to evaluate data both numerical and graphical.
3. You may be asked about experiments performed including results, procedures, actual or
hypothetical sources of error, discussions, calculations, background information and concepts.
The more complete your lab notebook is before the exam, the easier the lab exam will be.
For additional information read sections 2.2 2.3, 3.2-3.3 and the dilution subsection in chapter 9
section 2 (pages 304 - 306) in the textbook: Chemistry: Structure and Properties by Tro, 1st ed.
33
The Determination of the Empirical Chemical Formula

of a Hydrate
Introduction:
An empirical formula is the lowest whole number ratio of the elements in a compound and provides
information about the composition of a compound. For instance, the compound sodium sulfate
decahydrate has the chemical formula Na2SO410H2O. This formula conveys the information that
there are ten water molecules per two sodium ions per one sulfate ion. You might wonder: How
were these ratios determined? To answer the question it is necessary to recognize that the ratio
of atoms (or ions) is identical to the ratio of moles. That is, for sodium sulfate decahydrate, there
are ten moles of water per two moles of sodium ions per one mole of sulfate. This conception of
the molar ratio is essential since there is no way to count atoms in the lab but mass can be
measured and mass can be converted to moles by the formula:
Eq. 1
The goal of this lab is to determine x, y, and z in the chemical formula of the hydrate:
CuxCly zH2O
Compounds with a zH2O in the formula are called hydrates and have water molecules
incorporated into the lattice structure of the ionic compound. When heated, hydrates decompose
to produce water and an anhydrous salt. Anhydrous salt have no water molecules in their lattice
structure. Removal of water molecules from the salt creates a change in the lattice structure, which
is often accompanied by a change in color. For example, cobalt(II) chloride hexahydrate is pink.
Heating the hydrate salt removes the six waters causing a color change from pink to a purple-blue.
Figure 1: Hydrate to anhydrous color transition example.

Chemistry: Structure and Properties by Tro, 1st ed, page 160.
Under the conditions of the reaction, the evolved water will vaporize.
CuxCly zH2O
CuxCly +
hydrate
anhydrous salt
z H2O
evolved water
34
Thus, the difference in the mass before and after the reaction will be the mass of the water in the
compound and the mass of water can be converted to moles of water by applying Eq. 1.
The next step in the analysis is to determine the mass of copper in the sample. This is done by
reducing the copper ion to elemental copper using aluminum as the reducing agent:
3 Cuy+ + y Al y Al3+ + 3 Cu
The mass of the copper metal produced is the same as the mass of the copper in the original
sample. Since the sample contains only copper, water, and chloride, subtracting the mass of the
water and copper from the mass of the sample or subtracting the mass of the copper from the mass
of the anhydrous salt will yield the mass of the chloride.
Safety tips (Hazards): Never leave heating chemicals unattended. Always wait for containers to cool
before touching. Liquid waste should be poured into the waste container in the hood. Solid waste
may be disposed of in the regular trash.
Materials:
crucible and cover
5.5cm, plastic Bchner funnel
wash bottle
crucible tongs
250mL filter flask
balance
spatula
copper chloride hydrate
10mL graduated cylinder
hot plate
forceps
aluminum weighing dish
aluminum wire, 18 gauge
5.5cm qualitative filter paper
plastic transfer pipets
50mL beaker
deionized water (DI)
ruler
ring stand
ring stand clamp and clamp

holder
Aspirator
Glass rods (for breaking apart

solid)
Procedure:
Caution! The stirring hot plate may be hot. Do not touch the surface.
1.
Obtain and wear goggles.
2.
When you first enter the lab and after you have put-on your safety goggles, adjust the heat
dial of the Fisher Isotemp hot plate to 400 or adjust the dial of the Corning hot plate to 7.
Allow at least ten minutes for the temperature to equilibrate before placing the crucible
containing the hydrate on the hot plate.
35
3.
Zero the balance. Use the crucible tongs to place the clean and dry crucible and lid on the
balance. Record the mass. Add about 1 gram of the hydrate to the crucible and record the
mass of the lid and crucible containing the hydrate. It is not important to measure exactly 1
gram of the hydrate to the crucible but you must record all of the digits displayed.
4.
Use the crucible tongs to transfer the crucible and lid to the hot plate. Place the lid on the
crucible so that there is a gap to allow the water vapor to escape. Wait for fifteen minutes.
Remove the lid with the crucible tongs and, using the metal spatula or glass rod, break the
solid and observe the color of the solid. Do not remove the crucible from the hot plate until
the color has completely changed from blue to brown. Place the lid on the crucible and
place the crucible on the lab bench until it has cooled. Note! Never place hot objects on a
balance.
5.
Measure and record the mass of the cool crucible and lid.
6.
Remove the crucible from the balance. You may use your hands. Add 10mL of DI water to
the graduated cylinder. Pour the solid from the crucible into the 50mL beaker. Some of the
solid will stick to the inside of the crucible. The water in the graduated cylinder and the
plastic transfer pipet are used to wash the solid from the crucible into the beaker. When
the crucible is clean, pour any water remaining in the graduated cylinder into the beaker.
Swirl the beaker and observe the color change. Continue swirling until the solid has
dissolved.
7.
Measure out about 20 cm of aluminum wire, coil the wire,
and place the wire in the 50mL beaker so that it is completely immersed in the copper
chloride solution.
The reaction will take about 10 minutes to complete.

If the solution is still blue after ten minutes wait until the blue color disappears.
8.
The elemental copper will be on the aluminum wire. Hold the wire with the forceps and use
the spatula to scrape the copper from the aluminum wire into the beaker. Use the forceps
to remove the wire from the beaker. If some copper remains on the wire, scrape the wire
with the spatula. Rinse the wire with DI water into the beaker.
36
9.
Collect and wash the copper produced in the reaction following the procedure below:
a. Set-up a Bchner funnel for vacuum filtration.
b. Obtain a piece of filter paper. Wet the paper with DI water, place the paper on the
Buchner
funnel, and ensure all of the holes are covered. Turn-on the water.
a. Pour the contents of the beaker onto the filter paper. Use the spatula and wash bottle
to
transfer all of the copper from the beaker onto the filter paper. Wash the residue on
the filter paper with DI water. Allow the copper on the filter paper to dry for a few
minutes.
d. Disconnect the vacuum hose from the aspirator.
10.
Zero the balance and weigh an aluminum weighing dish. Remove the top of the Buchner
and use the spatula to transfer the copper from the filter paper to the aluminum weighing
dish. Place the weighing dish and contents on the hot plate for a few minutes. Use the
forceps to place the hot weighing dish on the lab bench and allow the dish to cool. Zero the
balance and weigh the weighing dish and contents.
Aluminum Weighing Dish
11. Dispose of the of the contents of the vacuum flask, filter paper, weighing dish and aluminum
wire as directed by your laboratory instructor.
12. Turn-off the hot plate.
Make a data table to record the following items
Mass of empty crucible and lid
Mass of crucible, lid, and hydrate
Mass of crucible, lid, and anhydrous salt
Mass of empty aluminum dish
Mass of aluminum dish and copper
37
Calculations:
Determining x and y in CuxCly. For the compound CuxCly, there are y moles of Cl- per x moles
of Cuy+. To determine the moles of y and x it is necessary to find the mass of copper ions and
chloride in the sample.
1. Calculate the mass and moles of copper
2. Calculate the mass and moles of chloride.
a. To determine the mass of chloride it is necessary to find the mass of the anhydrous salt.
This is done by subtracting the mass of the crucible and lid from the mass of the crucible,
lid and anhydrous salt (C-A below).
Crucible, Lid,
and Hydrate
Cux Cly zH2 O
Empty Crucible
and Lid
Crucible, Lid,
and Anhydrous
Salt CuxCl y
b. Subtract the mass of the copper from the mass of the anhydrous salt. This is the mass of
the chloride ions.
3. To find x and y divide by the smaller number of moles. Moles copper should be smaller
than moles chloride.
a. Since the empirical formula can represent the mole ratio of atoms within the
compound, rewrite the compound's formula with the moles calculated in steps 1 and 2
above:
Rewrite
as
b. Divide the both moles by the smaller number of moles (either moles copper or moles
chloride). Moles copper should be the smaller number. This will give you the subscripts
x and y.
c. Divide the moles of chloride by the smaller number of moles (either moles copper or
moles chloride). Moles copper should be the smaller number. This will give you the
whole number ratio of moles of chloride y to one mole of copper ions (x) in the
formula. Note: These calculations follow the same method illustrated in Examples 5.14
and 5.15 (page 173) in the textbook. See the textbook for additional details.
38
The determination of z in CuxCly zH2O follows the same strategy described above.
1. Calculate the molar mass of CuxCly (anhydrous salt) based on your subscripts x and y you
calculated earlier.
2. Calculate the moles CuxCly by dividing the mass of CuxCly (anhydrous salt) by the molar mass
of CuxCly, (use Equation 1).
3. Determine the mass of water by subtracting the mass of the crucible, lid, and anhydrous salt
from the mass of the crucible, lid, and hydrate (B-C, below).
A
Empty Crucible
and Lid
B
Crucible, Lid,
and Hydrate
Cux Cly zH2 O
Crucible, Lid,
and Anhydrous
Salt CuxCl y
4. Calculate the moles of water by dividing the mass of water by the molar mass of water.
5. Calculate z by dividing the moles of water by the moles of CuxCly.
Note! In general, when determining the formula of a compound, dividing the moles of one element
by the moles of another element may yield a ratio that is not a whole number, that is, the result
may a value such as 1.5. This might occur, for instance, when experimentally determining the
chemical formula of an iron sulfide compound. In this situation you would multiply the x and y
values by 2 to see if the result both x and y are whole numbers. You would continue the
process (i.e., multiplying x and y by 3, then 4, etc.) until both x and y are whole numbers.
1. A student did not notice that after ten minutes some of the contents of the crucible
remained blue. Would this cause your z value to be erroneously high, erroneously low, or
would this error not affect z? Explain.
2. Would the procedural error described in Discussion Question #1 cause your y value to be
erroneously high, erroneously low, or would this error not affect y? Explain.
3. A 5.123g sample of the hydrate MxClyzH2O decomposed into 1.122g My+, 1.984g chloride,
and 2.017g water. If the molar mass of M is 40.078 g/mol, what is the empirical formula
of the compound? Show your calculations. What is the most likely identity of metal M?
Explain your answer.
For additional information about mole calculations and empirical formulas read sections 5.10-5.11
(pages 167 - 177) in the textbook: Chemistry: Structure and Properties by Tro, 1st ed.
For additional information about reduction reactions read section 9.9 (pages 328 - 334).
39
Gas
Determining the molar mass of an unknown gas
Introduction: The ideal gas law PV=nRT, can be utilized to determine the moles of gas in a system
via a simple algebraic manipulation, so that
(1)
where the gas constant R is defined as R = 0.0821

per mole for a given substance
(2)
L atm
mol K
. Recall that molar mass is defined as mass
= /
Clearly, when the number of moles of gas which occupy a container are known, the formula weight
of the gas can be determined by measuring the grams of gas in the system. The moles of gas, (n) in
a system can be obtained if the pressure (P), temperature (T), and volume (V) are measured and
entered into equation (1). In this experiment you will be given an unknown solid that generates a
gas when it encounters an acidic solution. By measuring the temperature of the water through
which the gas is bubbled, the volume of water displaced, and the pressure in the room, P,V and T
are easily determined. Recall from physics class that when the water level and gas level are of equal
height in a submerged cylinder, the gas pressure in the cylinder will equal the ambient room
pressure. Pressure within the cylinder can be determined under these conditions by reading a
barometer placed in the room.
(3)
Ptotal (room) = Punknown gas + Pwater vapor
By weighing the gas generating apparatus before and after the reaction, it will be possible to
determine the mass of gas produced. The mass of the gas produced will be equal to the difference
between the initial and final masses. The molar mass of the unknown gas can then be calculated
from equations (1) and (2).
Safety: The unknown solid and the unknown gas are not toxic except at very high concentrations.
The acid is dilute but can harm your eyes. All solutions can be poured down the sink.
Materials:
Gas-generating solid tablets
Erlenmeyer flask (for holding the
Ring stand and clamp (to stabilize
(broken into pieces ~1/4 tablet
test tube)
the "Apparatus")
size)
0.1 M HCl
Deep tray (for water)
Test tube with side arm
Stopper
Hose
Thermometer
Barometer
Procedure:
1. Place approximately 10mL of 0.1M HCl into a long test tube and stopper the tube (this
volume is not exact and does not need to be recorded). Place the test tube in an
Erlenmeyer flask. The test tube, flask, stopper and HCl together are the "Apparatus".
40
2. Place the gas-generating solid on the balance NEXT TO the apparatus (DO NOT ADD THE
SOLID TO THE HCl AT THIS POINT). Measure the combined mass of the apparatus together
with the mass of the gas-generating solid. This is the starting mass before the reaction.
3. Invert a 100 mL graduated cylinder filled with water into a large container full of water in
such a way that no air bubbles are present at the top of the cylinder. Place the hose leading
from the tube into the cylinder. Attach the other end of the hose to the apparatus.
4. Working quickly, drop the solid into the tube and stopper it to deliver the gas into the
cylinder. Wait until the reaction ceases (no more bubbling). Any leaks at the stopper or hose
will lead to an incorrectly low number of moles in the cylinder. No gas leaks can be
tolerated!
1
2
3
4
5
Figure 1: Experiment set-up immediately after

Figure 2: Experiment set-up with gas
adding gas-producing solid
collecting at the top of the inverted cylinder
5. Remove tubing from Apparatus. Re-weigh the Apparatus after the reaction is completed.
The mass lost in the reaction (the unknown gas) should equal the difference in mass before
and after the reaction.
6. Measure the temperature of the water in which the graduated cylinder was inverted and
the gas was bubbled through.
7. Using the barometer, measure the pressure of the room. Bubbling the gas through water
will also cause some water vapor (gas) to mix with the unknown gas. Look up the vapor
pressure of water at the recorded temperature.
Data:
41
Make a table in your notebook and record the total mass of the apparatus and solid before the
reaction (Erlenmeyer flask + test tube + stopper + HCl + gas-generating solid). Record the volume of
water displaced in the graduated cylinder to the nearest 0.1mL. Be careful reading the upside-down
graduated cylinder and pay close attention to the numbers that the graduations correspond to
(reading this will be similar to reading a buret). Record the total mass of the apparatus after the
reaction (Erlenmeyer flask + test tube + stopper + solution). Record the temperature of the water
and pressure of the room. Repeat experiment for total of three trials. HCl can be reused for multiple
trials.
Calculations:
A. Subtract final mass of apparatus from starting mass (apparatus + solid side by side). Obtain
the mass of the gas which was delivered into the cylinder.
B. Subtract water vapor pressure from total room pressure to find pressure of the unknown
gas (Equation 3). See Appendix IV "Useful Data" section E (page A-28) of textbook for water
vapor pressures indexed by temperature. Be careful with units. Only values with the same
units can be subtracted from one another.
C. Convert all measured values to appropriate units: Volume (liters), Pressure (atmospheres),
and Temperature (Kelvin).
D. Use the ideal gas law to calculate the moles of gas produced (Equation 1)
E. Calculate molar mass using the grams of gas and moles gas produced (Equation 2)
F. Report the mean and standard deviation of the molar mass.
Chemistry in Context: There are several simple chemical reactions that can generate the common
gases hydrogen, carbon dioxide, oxygen and nitrogen from a solid. An air bag in an automobile
contains a sodium azide, a chemical that can be turned into nitrogen very quickly with an electrical
discharge. When a car decelerates at too high a rate (like when it hits a phone pole) a sensor sends
an electrical discharge that ignites the powder in an air bag. Effectively, an air bag deployment is an
explosion. All explosives function in the same way, they generate a great deal of nitrogen gas from a
small amount of solid, at very high rates. The fast rise in gas pressure in an explosion creates a
shock wave that can be used to destroy a container, and objects near the container, when the air is
compressed into a shock wave. The air bag powder is designed to inflate the bag in milliseconds,
but the reaction ends before the pressure raises high enough to cause the bag to explode. An error
in the amount of powder would be devastating because, with too little powder, the bag might not
completely inflate, or, with too much powder, the bag will explode and kill the passenger! You
noticed in todays experiment that a small amount of solid produces a large volume of gas, but
todays reaction was not an explosion because the reaction rate was very slow.
Discussion:
1. The unknown gas generating solid used is a well-known antacid, Alka Seltzer.
a. What is the reaction occurring that produces gas? Include balanced chemical reaction.
b. What is the identity and the molar mass of the gas produced in the Alka Seltzer
reaction?
c. Calculate a percent error for the molar mass using the formula:
% =

100%

42
2. The lab manual states no gas leaks can be tolerated! Discuss what the following errors or
changes in procedure will have on your gas collection and on the calculated molar mass of your
unknown gas:
a. You did not replace the stopper quickly after adding the gas-generating solid.
b. You stopped the gas collection and recorded the gas volume before the bubbling has
stopped.
c. The bubbling within the apparatus was vigorous and some HCl + tablet solution spilled
into the hose through the test tube side arm.
d. The apparatus accidentally picked up a few drops of water before the final mass was
recorded.
**Correct answers will clearly state if the calculated molar mass is higher or lower than the
correct value or if there is no effect.
3. How does Alka Seltzer work as an antacid?
For additional information about acid base and gas evolution reactions read section 9.7 - 9.8, the
ideal gas law read section 11.4-11.5 (pages 401-407) and section 11.6 about partial pressure
calculations (pages 407-413), with emphasis on pages 412-413 Collecting gases over water in the
textbook: Chemistry: Structure and Properties by Nivaldo Tro 1st ed. Partial pressures for water
vapor can be found in Appendix IV section E (page A-28) of the textbook.
43
Titration
What is the molar mass of an unknown diprotic acid, (H2A)?
Introduction:
You do not need to utilize a mass spectrometer to determine the molar mass of a compound. As
long as the number of moles can be obtained in some manner, and the grams of the substance are
determined by weighing, the molar mass can be calculated with a high degree of accuracy. For an
acid, the number of moles of acid can be obtained in a titration as long as the number of protons
(H+ ions) the acid donates is known. The unknown acid in this experiment is diprotic, which means
two H+ ions will be donated by the acid in the chemical reaction. As a result, the formula for the
unknown diprotic acid we plan to analyze will be designated as H2A. Each sample of acid will be
neutralized using sodium hydroxide solution of a known molarity as shown by the following
balanced equation:
(1)
H 2A+ 2NaOH
2H2O + Na2A
Recall that for any solution, the number of moles of solute can be determined using the following
equation:
(2)
(M solution) x (Vsolution used) = moles of solute used
In a titration, you will add enough sodium hydroxide solution to completely neutralize the preweighed amount of H2A in each sample. Phenolphthalein is an acid-base indicator that signals the
endpoint of the titration (complete neutralization of the acid) by changing the color of the solution
from colorless to faint pink. The purpose of the titration is to determine the volume of sodium
hydroxide needed to neutralize the H2A solution. Since the molarity of the sodium hydroxide is
known, the number of moles of base used to completely neutralize the acid can be calculated (eq.
2). The stoichiometric coefficients in the balanced chemical equation (eq. 1) allows for calculation of
the moles of acid present in each sample. Finally, since the grams of acid in each sample are known
from simply weighing the solid prior to dissolving, the molar mass can now be computed. (eq. 3)
(3)
Safety tips (Hazards): The solutions present at the end of the titration can be poured down the sink
because they have been neutralized. Flush solutions with tap water. Wear eye protection at all
times because acids and bases are corrosives. The unknown acid is a compound found in spinach
and is a metabolic poison--do not ingest the acid powder and wash your hands well before eating
after class. (Also, do not eat excessive amounts of spinach -- see Chemistry in Context section).
Procedure:
Materials:
Ring stand and buret clamp
Top loader balance
Unknown diprotic acid solid
Buret
Weigh paper
Phenolphthalein indicator
125 mL Erlenmeyer flask

0.1000 M NaOH solution (base)
44
Diprotic Acid Titration--Measure all masses to 0.001g and ALL buret volumes to the nearest 0.01mL
Weigh approximately 0.10 g of the solid, unknown, diprotic acid and carefully transfer ALL the
acid to a 125 mL Erlenmeyer flask. Be sure to record the exact mass of your sample of H 2A.
Add an arbitrary amount of deionized water (approximately 20 mL, this volume does not need
to be measured exactly or recorded) to the flask to dissolve ALL of the acid. (NOTE: Initially, the
acid may not be completely dissolved-- do not be concerned-- the addition of base will help the
acid be more soluble. However, at the endpoint the acid must be completely dissolved.)
Add a drop of phenolphthalein indicator to the Erlenmeyer flask.
Fill a buret with 0.1000 M NaOH very close to the top of the buret, but not exactly at zero, (this
avoids a reading bias) and record this initial volume of NaOH in the buret.
Open the valve and add base (titrate) while stirring. The endpoint is signaled by the first
PERMANENT light pink color observed. As you approach the endpoint, slow down the flow of
titrant (NaOH) to 1 drop per second and try to hit the endpoint to within one drop. Record the
final volume of NaOH solution in the buret. The difference between the final and initial buret
readings is equal to the titrant volume delivered.
Repeat the experiment for two more samples of diprotic acid. You should have at least three
trials total.
Buret filled with base solution.

Record initial and final
volumes.
Erlenmyer flask containing acid,

water, and phenolphthalein
indicator solution.
Data: Make a table in your notebook and record the mass of each sample and the initial and final
buret volumes for each trial. You should have at least three trials total.
Calculations:
45
1. Calculate the volume of base solution used. Volume used = Final volume - Initial volume
2. Calculate the moles of base used. Use equation 2, be sure to convert volumes to L first.
3. Calculate the moles of acid used in each titration. Use stoichiometry of balanced reaction,
equation 1.
4. Calculate the molar mass of the unknown acid from equation 3.
5. Report the mean molar mass and standard deviation of the molar mass.
Chemistry in Context: Titration is a very useful analytical tool to determine unknown solution
concentrations. Your stomach secretes hydrochloric acid to the extent that the gastric juice pH can
drop to a value of zero. Stress, gastric cancer, or something as simple as smelling food on an empty
stomach can trigger a hyper-secretory burst of acid secretion. Hyper-secretion can be damaging
when food is not present in the stomach to neutralize the acid. If hyper-secretion occurs in a
chronic fashion, a gastric ulcer may result. How can a clinician determine the amount of acid that a
patient is secreting in order to establish whether or not the acid secretion is in the normal range?
This is typically done by titration. A naso-gastric tube is inserted and used to obtain a gastric juice
sample by suction. Titration of the gastric juice sample with a known concentration of base will
reveal the number of moles of acid in the sample. Dividing the number of moles by the sample size
in liters will reveal the concentration of acid in the stomach. Very high concentrations of acid can be
indicative of the problems described above. The solution to hyperacidity used to be the ingestion of
antacids (Maalox, Alka-Seltzer, Tums) which are simply bases capable of neutralizing the acid.
Today, there are a number of drugs available (Prevacid, Pepcid, Zantac) which attempt to inhibit
acid secretion at the cellular level.
1. Discuss what the following errors or changes in procedure will have on your titration and on
the calculated molar mass of your acid:
a. Reached the endpoint prior to all of the acid dissolving.
b. You stopped the titration and recorded the final buret volume when a deep
pink/red color was seen.
c. You used twice the amount of water to dissolve the acid.
**Correct answers will clearly state if the calculated molar mass is higher or lower than the
correct value or if there is no effect.
2. What if the unknown acid was really a triprotic acid (three H+ ions to be donated) instead of
a diprotic acid
a. Write the formula for the triprotic acid and a balanced equation for the titration
reaction.
b. Using your experimental data from trial #2 (assuming the acid mass is really that of
the triprotic acid), calculate the molar mass of the triprotic acid.
c. Compare the calculated molar masses of the triprotic acid with the diprotic acid
molar mass.
46
3. Consult the supplemental page on Canvas with a list of possible diprotic acids. Using molar
masses, what is/are the most likely identity(ies) of the unknown acid?
For additional information about acid-base reactions, calculations involving molarity and titrations
read sections 9.2-9.3 & 9.7 (pages 302-308, 319-326) in the textbook: Chemistry: Structure and
Properties by Nivaldo Tro, 1st ed.
For description and uses of a Mass Spectrometer read Chapter 1 section 1.9 Mass Spectrometry:
Measuring the Mass of Atoms and Molecules (page 24-25).
47
Alum Synthesis from Solid Aluminum

Aluminum is the most abundant metal in the earths crust. Aluminum is also very stable since it forms an
oxide coating (Al2O3), which stays attached to the aluminum and protects the metal rather than flaking
off like iron rust. This coating protects the aluminum from further oxidation and among other attributes
makes it highly desirable for industrial and commercial use. However, the durability of the aluminum
can also make it difficult to process aluminum waste. One way to deal with aluminum waste is to
convert aluminum solid into alum, which is a widely used chemical in manufacturing.
Alums are ionic compounds that are made up of a monovalent cation (e.g. alkali metal ions), a trivalent
cation (e.g. Al3+, Cr3+, Fe3+), two sulfate anions (SO42-), and twelve water molecules. You will prepare the
alum: potassium aluminum sulfate dodecahydrate, KAl(SO4)212H2O. The inclusion of water molecules
makes alum a hydrate similar the copper chloride hydrate we used previously. Remember the waters
must be included in the molar mass of the hydrate.
To convert the aluminum from solid metal to alum, we will use several reactions. The first reaction is a
single replacement redox reaction where the aluminum displaces some hydrogen from water to form
hydrogen gas. Recall that in solution, soluble (aq) ionic compounds exist as separate hydrated ions not
as one unit.
1) 2 Al(s) + 2 KOH(aq) + 6 H2O(l)
2 K[Al(OH)4](aq) + 3 H2(g)
The second reaction is an acid-base neutralization reaction that only partially neutralizes the potassium
aluminum hydroxide. The second step occurs on initial addition of the sulfuric acid. Gentle heating and
stirring will allow the aluminum hydroxide to further react to completely neutralize the base as shown in
reaction 3.
2) 2 K[Al(OH)4](aq) + H2SO4(aq)
2 Al(OH)3(s) + K2SO4(aq) + 2 H2O(l)
3) 2 Al(OH)3(s) + 3 H2SO4(aq) 2 Al3+(aq) + 3 SO42-(aq) + 6 H2O(l)

The final reaction is the crystallization, pulling together the necessary ions to form the alum. However,
due to the solubility of this alum in water this crystallization only occurs at lower temperatures.
4) K+(aq) + Al3+(aq) + 2 SO42-(aq) + 12 H2O(l)
KAl(SO4)212H2O(s)
Safety Hazards:
KOH is a caustic solution (strong base) and H2SO4 is a strong acid. At the concentrations used in this
experiment both will cause chemical burns and severely damage your eyes. Wear goggles at all times.
Immediately wash skin if exposed to either solution with lots of water. Wear gloves while using the 9M
H2SO4 solution.
H2 gas is flammable. Avoid flames.
48
Week 1:
Materials:
Aluminum weigh boat
150 mL beaker
Scissors
1.5 M KOH
Hot/Stir plate and stir bar
600 mL beaker
Ice
Beaker Tongs (for 150 mL

beaker)
Bchner funnel with neck

adapter
Filter paper
DI water
Gloves
9 M H2SO4
Storage container
Label tape
250 mL filter flask
Procedure
1. Obtain and wear goggles
2. Tare a 150 mL beaker. Cut small pieces off the aluminum boat, transferring them into the
beaker until approximately 0.5 grams aluminum has been collected. Record the actual mass of
aluminum transferred.
3. Measure out approximately 50 mL of 1.5 M KOH in 100mL graduated cylinder (record the actual
volume). Transfer the KOH solution to the beaker with the aluminum. Place the beaker on a hot
1
4
1
3
plate located in the hood and add a stir bar. Turn the heating dial on to about to the
maximum setting. Adjust the stir dial to get a vortex that is about a half an inch deep.
4. The reaction that will begin to occur is a gas generating reaction. Monitor the mixture while the
reaction proceeds making sure that the solution does not boil or splash onto the upper edges of
the beaker. Adjust the stir and heat dials as necessary. This reaction should be complete within
10-20 minutes. Water will evaporate from the solution. Add deionized (DI) water if necessary
to maintain a liquid level at about 30 mL.
5. While waiting for the reaction to go to completion assemble the filtration apparatus (as shown
below, remember you did this earlier this semester) and obtain a 600 mL beaker with ice bath.
49
6. When the reaction appears complete use tongs to remove the beaker from the plate. If no
bubbles form after removing the beaker from the hot plate, the reaction is complete. Turn off
both the stir and heat dials. Filter the contents of the beaker. While filtration is occurring rinse
out the 150 mL beaker once with tap water and subsequently with DI water. After all of the
liquid has passed through the filter, transfer the liquid back into the rinsed 150 mL beaker.
Place the beaker into the ice bath and allow it to cool to or below room temperature. Once
cooled remove the 150 mL beaker from the ice bath.
7. While the solution cools rinse the Bchner funnel and stir bar with DI water, retrieve the stir bar,
and dispose of the filter paper in the regular trash.
8. Remember to wear gloves while handling sulfuric acid containers. Transfer approximately 30 mL
9M sulfuric acid from the stock bottles into a 50 mL beaker. Transfer approximately 20 mL
sulfuric acid into a 25 mL graduated cylinder from the 50 mL beaker (record actual volume).
Place the 150 mL beaker on the hot plate, add the stir bar, and adjust the stir dial to stir gently.
Pour the contents of the graduated cylinder slowly into the cooled 150 mL beaker. Fluffy solid
aluminum hydroxide will appear. Increase the stir dial until a inch vortex is obtained and turn
the heat setting to slightly less than half the maximum setting.
If time is running short, check with your instructor. If advised by your instructor, skip step 9
for now and pour your solution into your storage container. Next week begin with step 9 of
week 1 procedure instead.
9. The solid should dissolve within 10 minutes. Once the solid is dissolved remove the beaker from
the hot plate (use tongs). Allow the solution to cool. Transfer cooled solution to the storage
container for next week.
Note: The volume after 10 minutes should be between the 40 and 50 mL mark. If it is
above the 50 mL mark continue heating until the volume drops within the appropriate
range. If it is below 40 mL add DI water to increase the volume to the appropriate range.
10. Clean up your hood and station before leaving the room. Clean and return all glassware to the
designated areas. Dispose of waste as directed by your instructor.
50
Calculations
1. Calculate the moles of aluminum, potassium hydroxide, and sulfuric acid used in your
experiment.
2. Given the following overall reaction and your results from calculation 1 determine the limiting
reactant for the experiment. Show all work.
2 Al(s) + 2 KOH(aq) + 4 H2SO4(aq) + 22 H2O(l)
2 KAl(SO4)212H2O(s) + 3 H2(g)
3. Calculate the theoretical yield (in g) of the alum produced.
51
Week 2:
Materials
Storage container with week 1
solution
600 mL beaker
Ice
50 mL beaker
50% ethanol
Glass rod
Fiberglass Filter paper
250 mL filter flask
Bchner funnel with neck adapter
100% ethanol
DI water
Gloves
Rubber policeman
Aluminum weigh boat
Procedure
1. Make an ice bath in a 600 mL beaker. Obtain your container from week 1 and place it in the ice
bath. While the container is cooling measure out approximately 30 mL of a 50% ethanol
solution in a 50 mL beaker and place it in the ice bath.
2. Assemble the filtration apparatus.
3. After 10 minutes crystallization should start to occur in your sample container. If nothing no
crystals have formed, take a glass stir rod and scratch the sides of the container. The crystals
should start forming. Place the container back into the ice bath for another 5 minutes.
4. Quickly pour the entire contents of the container into the Bchner funnel. Transfer about 1/3 of
the 50% ethanol into the container swirl and pour contents into the Bchner funnel. Repeat
twice.
5. Transfer approximately 10 mL 100% ethanol into the 50 mL beaker. Carefully pour the entire
contents over the crystals in the Bchner funnel making sure to wash the entire sample. Allow
the crystals to dry by aspirating for an additional 10 minutes.
6. Using a rubber policeman transfer the crystals from the filter paper and Bchner funnel into a
pre-weighed dry aluminum dish. Measure the mass of the crystals and the dish. Put the dish
into the hood and wait 5 minutes. Weigh the dish with the crystals again. Repeat once more for
a total of three masses.
7. Clean up your hood and station before moving on to calculations. Clean and return all glassware
to the designated areas. Dispose of waste as directed by your instructor.
52
Calculations
1. Calculate the percent yield for your experiment.
Discussion Questions
1. Provide three reasons why a theoretical yield may differ from an experimental yield even when
properly following this procedure.
2. When determining the limiting reactant is it reasonable to make the determination that water is
not the limiting reactant without calculations. Why or why not?
3. How would the results be affected if the alum was not weighed to a constant mass during the
step 6 of the second weeks procedure?
4. If your starting source of aluminum was a coke can would the procedure need to change?
Explain your answer. Would you expect the theoretical yield to be the same, higher or lower?
5. The aluminum weigh boat is thin. Would you expect the length of time needed to dissolve the
aluminum to change if an aluminum sphere with the same mass was used? Explain your
answer.
The reactions used are redox and gas evolution experiments, consult Chapter 9 sections 8-9 of Chemistry:
Structure and Properties.
For stoichiometry and limiting reactant calculations, refer to Chapter 8 sections 4-5 and Chapter 9
section 3 for more information.
53
Neutralization
What is the heat of neutralization when H+ and OH- combine to form water?
Introduction:
A neutralization reaction involves the reaction of an acid with a base to produce water and a salt.
The reaction of phosphoric acid with sodium hydroxide to produce water and sodium phosphate
(Eq 1) is an example of a neutralization reaction:
(Eq 1)
H3PO4(aq) + 3NaOH(aq)
1 mole
3 mole
3H2O(l) + Na3PO4(aq)
3 mole 1 mole
The net ionic reaction for Eq 1, and for all neutralizations reaction, is shown below (Eq 2):
(Eq 2)
H+(aq) + OH-(aq)
1 mole 1 mole
H2O(l)
1 mole
The reaction of H+ and OH- ions to form water is exothermic (heat is produced) and the purpose of
this lab is to determine the heat of reaction (Hrxn) for Eq 2, that is, how much heat is produced
when one mole of hydroxide ions react with one mole of hydrogen ions to produce one mole of
water molecules. Other acids and bases, in theory, should yield the same heat of reaction for Eq 2.
Although there are other ions (spectator ions) in the reaction flask, their presence does not
contribute to the generation of heat.
If stoichiometric quantities of phosphoric acid and sodium hydroxide are mixed (in this example a
ratio of one mole of acid per three moles of base), both reactants will be completely consumed and
the amount of heat produced can be calculated from the quantity of either reactant. If nonstoichiometric quantities of acid and base are used, the limiting reactant will predict the amount of
water produced and the amount of heat evolved. An important task of this lab is to determine the
limiting reactant for each of the experiments performed.
The heat produced by any of the experiments you will perform is qreaction. To determine qreaction you
must first calculate qsolution which is the quantity of heat that was absorbed by the solution. The
difference between qreaction and qsolution is the sign (Eq 4). That is, the numerical value for the
amount of heat produced by the reaction is the same as the amount of heat absorbed by the
solution but the sign is opposite. To determine qsolution you will use Eq 3.
(Eq 3)
qsolution = msolution Cssolution T
(Eq 4)
qreaction = -qsolution
(Eq 5)
density =
The mass of the solution, msolution, is the combined mass of the sodium hydroxide and phosphoric
acid solutions. To calculate the mass of the sodium hydroxide solution, first solve Eq 5 for mass.
54
Next, insert the density and volume of the sodium hydroxide solution. Repeat this process to
determine the mass of the phosphoric acid solution. It should be emphasized that the mass of the
sodium hydroxide or phosphoric acid solutions is not the mass of the sodium hydroxide or
phosphoric. The solutions are composed of the solute (sodium hydroxide or phosphoric acid) and
the solvent (water).
The change in the temperature in Eq 3 (T) is equal to the final temperature minus the initial
temperature, Tfinal-Tinitial.
The specific heat of the solution in Eq 3 (Cssolution) is an intensive property and is equal to the heat
required to change the temperature of one gram of the solution one degree Celsius. We will use
4.184 for Cssolution.

The heat of reaction (Hrxn) for Eq 2 is not qreaction, but qreaction can be used to calculate Hrxn. The
value for Hrxn assumes that exactly one mole of water is produced, but in none of the experiments
that you will perform will one mole of water be produced. You will use Eq 6 to calculate Hrxn, that
is, the heat produced by the formation of one mole of water.
(Eq 6)
Hrxn(Eq2) =
(Note! Although Eq 6 will yield the correct numerical value for Hrxn(Eq2), heats of reaction are
expressed in J (or kJ) and not J/mol).
In the calculation of qreaction, several assumptions are made. These assumptions are listed below:
).
a)
The Cssolution is the same as the Cswater (4.184
b)
The temperature of the phosphoric acid solution is the same as the temperature of the
sodium hydroxide solution.
The calorimeter is a perfect insulator, that is, no heat conducts from the interior to the
exterior of the calorimeter.
Neither the temperature probe, nor the Styrofoam cup, nor the magnetic stir bar absorbs
the heat.
c)
d)
Safety tips:
1M NaOH is very caustic, immediately rinse off all spills on your skin, an eye injury with this
substance will be severe Wear Safety Glasses or Goggles! 1M phosphoric is not as harmful to the
skin but will damage your eyes if spattered, take care. The final salt is non-toxic; however, since the
reactions are not in ideal proportions the solutions are not neutralized. All waste solutions should
be collected in the waste containers.
55
Materials:
One Styrofoam calorimeter
with lid
1.00 M NaOH base solution

Density= 1.035 g/mL
1.00 M H3PO4 acid solution

Density= 1.046 g/mL
One magnetic stir bar
One LabQuest 2
One Vernier stainless steel

temperature probe
One 500mL beaker
One 100 mL graduated

cylinder
One 250mL beaker (for waste)
plastic dropping pipets
One ring stand
One 25mL graduated cylinder
One 100 mL beaker

One magnetic stir plate
One plastic forceps
One two-prong clamp

Procedure:
Two Prong
Clamp
Temperature
Probe
Styrofoam
Cup
Ring
Stand
Magnetic
Stir Bar
LabQuest 2
Stir
Heat
Magnetic
Sitrrer
Fig 1 Calorimeter
Procedure:
1)
The apparatus should be assembled as illustrated in Fig 1.
2)
If the LabQuest 2 is not on, press and release the power button ( ) located at the top edge
of the LabQuest 2.
5)
Add about 240 mL of the 1.00 M sodium hydroxide to the 500 mL beaker.
6)
Add about 60 mL of the 1.00 M phosphoric acid to the 100 mL beaker.
7)
Add exactly 60.0 mL of the 1.00 M sodium hydroxide to the 100 mL graduated cylinder. You
can adjust the volume in the graduated cylinder using the plastic dropping pipets. Transfer
this solution to the calorimeter.
8)
Turn-on and adjust the magnetic stirrer to about 600. Note! Do not turn-on the heat.
9)
Measure exactly 7.5 mL of the phosphoric acid in the 25 mL graduated cylinder.
10)
After ensuring the tip of the temperature probe is beneath the surface of the sodium
hydroxide solution, tap the start button (
). If a warning appears, tap Discard. After
the program starts, wait a few seconds and then add the phosphoric acid to the calorimeter.
11)
After the run has completed, tap the left (
) and right (
) Examine buttons to find
the minimum (Ti) and maximum (Tf) temperatures.
12)
Turn off the magnetic stirrer, use the forceps to remove the stir bar, empty the calorimeter
into the 250 mL beaker, rinse the calorimeter with DI water, and dry the calorimeter.
13)
Repeat steps 7-12, three more times but instead of the 7.5 mL, measure other volumes, up
56
14)
to 25mL, of the phosphoric acid solution. If the LabQuest 2 displays a warning after tapping
the start button, tap Discard.
After the last run, tap the File button, tap New and then tap Discard.
Data Table(Create this table in your lab notebook)

Record the exact volumes of acid and base used and the initial and final temperatures for each
experiment.
Experiment
1
2
3
4
Vol Base(mL)
Vol Acid(mL)
Tinitial(oC)
Tfinal(oC)
Calculations:
a) Calculate the mass of the base solution and the acid solution by solving Eq 5, density
= for mass and then insert the density and volume for the sodium hydroxide or
phosphoric acid solutions. The densities of the sodium hydroxide and phosphoric acid solutions
are given in the Materials table.
a. Density of 1.00 M NaOH = 1.035 g/mL
b. Density of 1.00 M H3PO4 = 1.046 g/mL
c. Remember density of a solution is mass solution (not just solute) per volume of solution.
b) Calculate qsolution from Eq 3.
qsolution = msolution Cssolution T
a. Remember we assume Cssolution is the same as the Cswater (4.184
).
b. msolution = mass acid solution + mass base solution

c) Calculate qreaction from Eq 4.
qreaction = -qsolution
d) Use stoichiometry (dimensional analysis) to predict the moles water actually produced in each
trial.
a. Convert volumes to liters
b. For all solutions, M x V (in liters) = moles.
c. Remember the units must be the same to determine limiting reactant. Choose the
smaller amount.
e) Determine the limiting reactant in each trial.
f) Calculate the experimental heat of reaction to form water from its ions (Eq 6).
(Eq 6)
Hrxn(net reaction) =
a. This gives the enthalpy in J per 1 mole water. This is the Hrxn for the net ionic reaction
(Eqn 2).
b. Report the mean and standard deviation of all the trials.
c. The mean Hrxn(net reaction) is the experimental value.
g) Calculate the heat of reaction for the overall neutralization reaction (Eq 1). Hint: enthalpy is an
extensive property. Correct for the stoichiometric number of moles water in the overall reaction.
57
h) If you have covered Hess Law, calculate the theoretical heat of reaction to form water from its
ions. The Hof values of the reactants and products can be found in Appendix IV: Useful Data
section B of the textbook. Remember your net reaction is:
(Eq 2)
H+(aq) + OH- (aq) H2O(l)
The heat of a reaction is the heat of formation of products minus the heat of formation of the
reactants, where m and n are the coefficients of the products and reactants. This result is
the "accepted" or theoretical value.
(Eq 7)
i) Show the percent error between the accepted value (h) and your experimental value (f
above). Note: The % sign in the equation below (100%) is the unit.

= (
) 100%

Results Table (Create this table in your lab notebook):
Experimen
t
Calculatio
na
Mass of
Base
Solution
(g)
Calculatio
na
Mass of
Acid
Solution
(g)
Calculatio
nb
qsolution
(J)
Calculatio
nc
qreaction
(J)
Calculatio
nd
Limiting
Reactant
Calculatio
ne
Moles
Water
Produced
(mol)
Calculatio
nf
Hrxn
Eq 2 (J)
Net Ionic
Reaction
Calculation g
Hrxn
Eq 1 (J)
Overall
Neutralizatio
n
Reaction
1
2
3
4
Error Analysis Table
Calculation f
Sx
Mean Hrxn
Eq 2 (J)
Standard
Net Ionic Reaction Deviation
Experimental value
Calculation h
Hrxn Eq 2 (kJ)
Net Ionic Reaction
Hess's Law
(Accepted value)
Convert kJ to J
Calculation i
Hrxn Eq 2 (J)
Net Ionic Reaction
Accepted Value
Percent Error
Chemistry in Context:
There are commercially available a variety of hand warmers which use a chemical reaction to
produce heat. Typically, these consist of a plastic bag with a divider. In the instructions the user is
asked to knead the bag, this kneading action ruptures the divider and mixes two previously
separate solutions. Upon kneading, the bag immediately begins to heat up. The warmth lasts for a
while and then fades away. Can you speculate on the nature of the reaction in the bag? Can you
58
find a reaction in your text for a cooler bag that would function by getting cold.? How would the
cooler bag reaction differ in its thermochemistry and in the sign of H?
Discussion Question:
1. For this experiment we assumed the calorimeter was a perfect insulator (no heat was lost to
the surroundings). Is this a good assumption? Explain your answer.
2. A student is supposed to add 25mL of 3M sodium hydroxide and 25mL of 3M phosphoric
acid to a calorimeter. By mistake, and without his knowledge, he adds 25mL of 2.5M
sodium hydroxide instead of 25 mL of 3M sodium hydroxide. How will this impact the
accuracy of his calculated heat of reaction? Will his results be erroneously high, erroneously
low or will his results be accurate? Explain in detail. Refer to the equations you used in
your calculations.
For additional information about

calorimetry read sections 10.7 (pages 362 - 364)
standard enthalpies of formation read section 10.10 ( pages 370 375)
in the textbook: Chemistry: Structure and Properties by Nivaldo Tro, 1st ed.
59
The Missing Labels Experiment

In class we will develop procedures to identify aqueous solutions and water based on known
reactions and properties. We will use pH, solubility, and other observations.
What you need to do before you perform this experiment:
You will need to familiarize yourself/review/research the following topics (Review Chapter 9 of your
textbook):
Chemical Reactions involving aqueous solutions
Acid-Base reactions
Solubilities of Ionic Compounds
Identifying Gases and Precipitates
pH scale and acid-base classification
You should copy the solubility table and the gas generating reactions table into your lab notebook.
Materials Provided:
pH paper
Phenolphthalein
Well-plates for mixing
Vials with unknown aqueous solutions
60
Lab Exam
Reactions
This exam is a paper exam and will be cumulative over the last six experiments (the reactions
unit).
The exam is open notebook. You may use information written in or permanently attached to your
lab notebook. Other information sources are prohibited.
Do NOT write any information from the exam into your lab notebook. Scratch paper will be
provided.
Correct use of significant figures are required for all numerical answers. Answers must also
include units if applicable.
You may use a calculator. Graphing calculators are allowed.
You may use pencil for this exam.
4. You will need to know how to use all of the equations from these experiments.
5. You may be asked to evaluate data both numerical and graphical.
6. You may be asked to write chemical reactions, including predicting products, net and complete
ionic reactions.
7. You may be asked about experiments performed including results, procedures, actual or
hypothetical sources of error, discussions, calculations, background information and concepts.
The more complete your lab notebook is before the exam, the easier the lab exam will be.
61

CHM 1045L Lab Manual Fall 2016

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CHM 1045L

General Chemistry I Laboratory

Chemical Reactions Unit:

Laboratory Safety Contract

Laboratory Safety Contract

Person and phone number to be contacted in case of emergency.

Students Printed Name _________________________________________________________

Class___________________________________________ Lab Time______________________

Students Signed Name________________________________________ Date______________

(if student is a minor)

Solutions and the Calibration Graph

100 mL volumetric flask

Deionized (DI) water

Pure Liquid Density:

Density and Mass Percent Water of Unknown Solutions:

Suggested Data tables

Part B Data stock solution

Part C Data unknown

Calculations & Graphs:

Remember standard deviation is an indication of precision

Volume (in mL)

Density (in g/mL)

Stock Solution Molarity

Chromatography & Spectroscopy

One C18 Sep-Pak column

One SpectroVis Plus and USB

Grape Kool-Aid unsweetened

Plastic dropping pipets

Two 150mL or 250mL beakers

Four 50mL beakers

Put the LabQuest 2 in its cradle.

Plug in the power adapter.

Glassware and Solutions

Fill a 150mL or 250mL beaker with ~ 40 mL of DI (deionized) water.

The other 150mL or 250mL beaker will be the waste container.

The screen of the SpectroVis Plus should be as shown below:

). The scan takes about 5 seconds and when

Data Tables (Create these tables in your lab notebook):

How does absorbance relate to wavelength? To determine the percent recovery, is it

Color and Concentration

The Calibration Curve

Absorbance vs. Concentration

One LabQuest 2, cradle, and

Plastic dropping pipets

Six 50mL beakers:

3.69x10-5M FD&C Yellow #5

Iceberg Blue Mouthwash

FD&C Red #40

Diet Cherry 7-Up

Put the LabQuest 2 in its cradle.

Plug in the power adapter.

Determinations of wavelength of maximum absorbance (lambda max, max):

The screen of the spectrophotometer should be as shown below (Fig 7):

Preparation of the Calibration Standards

Creating the Calibration Graph:

Tap the start button (

Record absorbance and concentration

Record the correlation coefficient, the slope, and the y-intercept.

Tap the File and the Quit button. Tap Discard.

Data and Calculation Tables:

Determining the Copper Content in Brass

Cu2+(aq) + 2 NO2(g) + 2 OH-(aq)

Part II Measure the Absorbance Spectra of Solutions

b. In LabQuest App, from the File menu, choose Email

Class_____________________ Lab Time

Students Signed Name__________________________ Date