Professional Documents
Culture Documents
Lab Coordinators:
Dr. Eric Sheagley
sheagley@pdx.edu
Dr. Dean Atkinson
atkinsdb@pdx.edu
Table of Contents
General Chemistry Laboratory ....................................................................................................... 3
Grading Criteria .............................................................................................................................. 4
Laboratory Safety Rules and Procedures ........................................................................................ 5
Keeping a Lab Notebook ................................................................................................................ 9
Report Guidelines ......................................................................................................................... 14
General Chemistry Lab Report Checklist ..................................................................................... 19
CH227 LABS ................................................................................................................................. 21
Lab: Scientific Measurements: Precision and Accuracy .............................................................. 21
Pre-Lab: Who has the same solid that I have? ............................................................................. 26
Pre-Lab: How much sugar is in a can of coke? ........................................................................... 33
Pre-Lab: A Cycle of Copper Reactions ....................................................................................... 43
Pre-lab: Which Alkali Metal Carbonate? ..................................................................................... 50
Pre-lab: Using Conductivity to Find an Equivalence Point ......................................................... 57
Prelab: Atomic Emission Spectra ................................................................................................ 65
Pre-Lab: Determining the Concentration of a Solution: Beers Law ........................................ 72
CH228 LABS ................................................................................................................................. 84
Pre-Lab: Enthalpy of Neutralization of Phosphoric Acid ............................................................ 84
Pre-Lab: Hesss Law .................................................................................................................... 91
Deriving the Gas Laws Using Computer Simulations .................................................................. 97
Pre-Lab: Decomposition of Hydrogen Peroxide........................................................................ 102
Pre-Lab: Vapor Pressure and Heat of Vaporization .................................................................. 108
Pre-Lab: Using Freezing-Point Depression to Find Molecular Weight..................................... 116
Pre-Lab: The Rate and Order of a Chemical Reaction .............................................................. 123
Pre-Lab: Chemical Equilibrium: Finding a Constant, Kc .......................................................... 130
Le Chateliers Principle in a Cobalt Complex ............................................................................ 138
CH229 LABS ............................................................................................................................... 142
Pre-lab: Acid Rain....................................................................................................................... 142
Pre-lab: Acid Ionization Constant, Ka......................................................................................... 149
Pre-lab: Titration of a Diprotic Acid: Identifying an Unknown ................................................. 158
Pre-lab: Buffers ........................................................................................................................... 167
Pre-lab: Determination of the Ksp of Calcium Hydroxide .......................................................... 173
Pre-lab: Thermodynamics of the Solubility of Potassium Nitrate .............................................. 180
Pre-lab: Redox Titration: Analysis of a Commercial Bleach ..................................................... 186
Pre-lab: Synthesis of Acetaminophen ......................................................................................... 191
Pre-lab: Electrochemistry: Galvanic Cells and the Nernst Equation .......................................... 199
borrow tables or graphs from another stud ent (learning how to properly create a table
or graph is an im portant skill, learn how to do it on your ow n!). You cannot paraphrase
the internet, your book or any other source w ithout the proper reference. Ad d itionally,
it w ill be consid ered an act of plagiarism if you borrow d ata w ithout prior approval
from your TA. There are ad d itional resources online to help you avoid plagiarism .
Please be sure to check http://www.lib.pdx.edu/instruction/survivalguide/writeandcitemain.htm
or http://web.pdx.edu/~b5mg/plagweb.html, and feel free to discuss the issue with your TA or
the lab coordinator. Depending on the severity of the offense(s), you will receive, at a minimum,
a zero score for the report. Additionally, a report may be made to the Office of Student Affairs.
Grading Criteria
Unless otherwise noted in the course schedule, every lab report is worth 120 points, including the
prelab, notebook and technique. Each lab report will be graded according to the following point
distribution:
Prelab: 20 points
Abstract: 10 points
Introduction: 10 points
Data: 10 points
Results: 15 points
Discussion: 15 points
In addition to the above points each lab meeting will have an additional 40 points
assigned on the following basis:
Notebook: 20 points
These points are awarded by the TA based upon the quality of your lab notebook. Your
TA will be looking to see that you are including a title, a statement of purpose, the
procedures, data tables and that all data is present.
Lab technique: 20 points
The basis for assigning these points includes (but is not limited to) general lab technique
and methods, safety, general mannerism in lab and cleanliness.
Both of these criteria will be evaluated by your TA during each lab meeting. At the end of
each lab you must check out with your TA so that he or she can assess your lab
notebook and verify that you have cleaned your work area.
Grading: Your grade will be assigned based on the percentage of total points scored in
the class approximating the following scale (Note: this scale is subject to change
based on class performance):
Grade
Score
A
90%
B
80%
C
70%
D
55%
F
< 55%
More than one absence will result in a grade of F for the class.
Do not copy your partners, friends, old lab reports. That is plagiarism!
Safety Procedures
Know location of safety equipment; fire extinguisher, fire blanket, first aid kit, safety
shower, eyewash fountain and all exits.
In case of fire or accident, call the instructor at once.
Small fires may be extinguished by wet towels.
If a persons clothing catches fire, roll the person in the fire blanket to extinguish the
flames.
In case of a chemical spill on the body or clothing, stand under the safety shower and
flood the affected area with water. Remove clothing to minimize contamination with the
chemical.
If evacuation of the lab is necessary, leave through any door that is safe, or not
obstructed; doors that lead to other labs may be the best choice. Leave the building by the
nearest exit and meet your TA on the field next to Hoffmann Hall. This would also be the
meeting place in the event of an earthquake or other emergency. It is good to know the
nearest exits of your lab on the first day of class.
Spilled chemicals must be cleaned up immediately. If the material is corrosive or
flammable, ask the instructor for assistance. If acids or bases are spilled on the floor or
bench, neutralize with sodium bicarbonate, then dilute with water. Most other chemicals
can be sponged off with water.
Avoid contact with blood or bodily fluids. Notify the instructor or stockroom personnel if
ANY blood is spilled in the lab so that proper clean up and disposal procedures may be
followed.
If a mercury thermometer is broken, do not attempt to clean up yourself. Notify students
around you, so that mercury is not spread, then notify your lab instructor or stockroom
personnel. The stockroom is equipped for proper clean up and disposal of mercury.
containers can lead to injury from unexpected chemical reactions. Mixing waste can also
make it more difficult or expensive for PSU to dispose of them. Only chemicals should go
into waste jars. Waste jars for each experiment will be provided in the lab. They will be
labeled specifying which contents should be placed inside. It is important that you replace
the lids to the waste containers. When done with the waste jar, make sure it is placed in a
secondary container. Do not put anything down the sink unless you are explicitly told to
dispose of it this way. Your instructor will provide specific disposal guidelines when
needed. Following these guidelines assists us in lowering the environmental impact of the
labs.
There are several locations for very specific waste.
i. Chemical waste these containers are ONLY for chemical waste generated
in the lab. They are each specifically labeled for each lab and waste type.
READ THE LABELS.
ii. Contaminated paper waste this is ONLY for paper towels used for
clean-up of chemical spills.
iii. Broken glass this is ONLY for broken glassware.
iv. Gloves this is ONLY for used gloves.
v. Normal trash this is for all other trash that is not chemically
contaminated, glass, or gloves.
Clean your bench and equipment Clean all your glassware- dirty glassware is harder to
clean later. Wash with water and detergent scrubbing with a brush as necessary. Rinse well
with water. Do not dry glassware with compressed air, as it is frequently oily. The water
and gas should be turned off and your equipment drawer locked.
Clean the common areas before you leave the lab. Point deductions for the entire class
will be imposed if the instructor or stockroom is not satisfied.
Return any special equipment to its proper location or the stockroom.
Handling Chemicals:
Obtaining reagents:
Read the label CAREFULLY. The Chemicals are organized by experiment in secondary
containment bins. Make sure the chemical name and concentration match what is required
by the experiment!
Do not take the reagents to your bench.
We recommend always picking up bottles by the label. If all students do this, then any
unnoticed spills when pouring will not cause possible problems for the next user.
Remember to wear gloves while working with reagents.
Do not put stoppers or lids from reagents down on the lab bench. They may become
contaminated. Be sure that the lids or stoppers are replaced.
7
Do not place your own pipet, dropper, or spatulas into the reagent jar. Pour a small amount
into a beaker and measure from that. Please pour on the conservative side to minimize
waste and cost of labs. You can always go back for more.
Do not put any excess reagent back in the reagent jar. Treat it as waste and dispose of it
properly.
When weighing chemicals on the balances, never weigh directly onto the weighing pan.
Weigh into a weighing boat or beaker. Any spills on the balances MUST be cleaned up
immediately. If you are unclear how to clean a spill, notify your instructor. The balances
you are using are precision pieces of equipment and costs up to $4000.
All chemicals should be treated as potentially hazardous and toxic. Never taste a chemical
or solution. When smelling a chemical, gently fan the vapors toward your nose.
Any chemicals that come in contact with your skin should be immediately washed with soap
and copious amounts of water.
Laboratory Procedures
Never pipet any liquid directly by mouth! Use a rubber bulb to draw liquid into the pipet.
Never weigh hot chemicals or equipment.
When heating a test tube, always use a test tube holder and be certain never to point the
open end of the test tube toward yourself or another person.
Handling glass tubing or thermometers: to insert glass tubing into a rubber stopper,
lubricate the glass tubing with a drop of glycerin, hold the tubing in your hand close to the
hole, and keep all glass pieces wrapped in a towel while applying gentle pressure with a
twisting motion.
To prepare a dilute acid solution from concentrated acid, acid should be added slowly to
water with continuous stirring. This process is strongly exothermic, and adding water to
acid may result in a dangerous, explosive spattering.
Use the fume hood for all procedures that involve poisonous or objectionable gases or
vapors.
Never use an open flame and flammable liquids at the same time.
10
11
12
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Report Guidelines
At the end of every experiment in this manual, you will find instructions on what type of report
will be required. Some experiments require only a worksheet, which can be found on D2L. Other
experiments will require a formal report. The reports are due by the beginning of class the week
following completion of the experiment. Below is a description of what should be included in
each section. The sections are presented here in the order they should appear in your lab report.
It is expected that you will complete each experiment and do the necessary calculations and
analysis during the scheduled lab period each week. You may discuss the calculations and
analysis with your lab mates or TA; however, your written lab report should be your own
individual work!! The lab report sections should be complete but CONCISE. For most
experiments this term, your report should be 2-3 pages long.
Writing Style
You will write your reports using a formal scientific writing style. A lab report must be written in
the third person, passive voice. It must also be in the past tense. It should not contain personal
pronouns such as, I, we or he neither should it contain proper names of persons. This
includes referencing your TA, groups of students, your lab drawer, your lab group, or the class as
a whole.
Good: 50 mL of 1.0 M HCl were poured into a 125 mL Erlenmeyer flask
Bad: I poured 50 mL of hydrochloric acid into a flask.
Also bad: Lab groups poured 50 mL of hydrochloric acid into a flask This is not the correct
form of 3rd person.
Also bad: Joe Shmoe poured 50 mL of hydrochloric acid into a flask. This is not the correct
form of 3rd person. It includes Joes name.
Also bad: We are going to put 50 mL of acid into the flask. Uses future tense; also, we.
After you write your report, there is one more thing to do before you print it and hand it in:
Proofread it! Read it out loud. If is doesnt sound right, it isnt. Fix it. Then do it again until it
is right. You will enjoy writing reports more if you take pride in what you hand in.
Abstract:
This is a condensed version of your lab report. It is a stand-alone document. Abstracts are, in
fact, often published separately from the articles they describe. A library search of the literature
generally involves reading abstracts. This is done with the aim to identify articles that need to be
read in full, and eliminate many others whose abstract makes it clear that they are not relevant to
the study at hand. So, the abstract needs to be brief, but complete. For your work, this section
should usually be between two and three sentences long.
14
There are three questions that should be answered in any good abstract
1. What did you do?
2. How did you do it?
3. What did you find?
Even though it sequentially appears first, you should consider writing this part of the lab report
after you have finished the remaining sections. Doing so will better help you identify the major
results and allow you to include the appropriate percent errors when possible.
To answer the first question, you should look back to your purpose in your lab notebook. If your
purpose was to determine the molar mass of an unknown solid compound, then the first question
would be answered by stating that the molar mass of an unknown compound was experimentally
determined.
For the second and third questions, you want to be brief, stating the type of methods used, such
as gravimetric analysis, rather than trying to explain the procedure. Remember to keep this
section brief. Be sure to include the units for your numerical results.
Introduction:
Here, you want to address WHY you did this experiment. Your introduction begins with a
statement of the purpose of the experiment. You should use your purpose statement as a
guideline for the rest of the introduction. Your Abstract answers the question, What did you do?
In the introduction, your purpose statement is what you will do. For example, The purpose of this
experiment was to determine the color of the sky. You will find that as you write the report that
you will be repeating yourself a bit.
The rest of your Introduction section should flow from the purpose. How can this purpose be
achieved? Provide any relevant background to put the experiment in context. This is where you
will talk about the key concepts of the experiment. Which laws are being used to help you fulfill
the purpose? What are those laws? Why are they important to this experiment? As a general rule,
if you use a law in the labs procedure to determine something, you should talk about it in the
introduction.
Be sure to include any mathematical equations that are new to this experiment when appropriate.
These equations should be on their own line, but part of the paragraph itself as they come up.
Chemical equations should be handled the same way.
Your Introduction will often include some explanation of the theory behind the experiment.
Dont just write the equations, provide information as to why they are relevant. Your
introduction should follow a logical pattern from your statement of purpose to your data section
without relying on a statement of the procedure. You will write your procedure in your lab
notebook, there is no need to rewrite it here.
15
Data:
This section is where your experimental data belong. In this section you would also include
observations and descriptions of other pertinent events, when appropriate. This section is not
where the calculations, interpretation and discussion of your results belong. (In published
papers, a data section is usually not included, but, this is a class so this section will be included.)
Tables
Whenever possible, data should be presented in the clearest format possible, usually in the
form of a table. When you present your data in a table it is necessary to take the following
into account.
Number tables sequentially as they appear (Table 1, Table 2.).
Be sure to refer the reader to view the tables in the text.
Construct a descriptive table caption and place it above the table.
Tables should include descriptive column headings, including units.
Tables should not be divided across page boundaries
For a simple example, see Table 1.
Table 1: Mass and volume measurements when a portion of an unknown solid
was dissolved to make 10.0 mL of aqueous solution.
Trial
1
2
3
Graphs
When a table does not provide a clear picture of the data, a graphical presentation of data is
necessary. Do not present the exact same information as both a table and a graph. Pick the
format that best displays the data and stick to that. Please prepare graphs using the following
guidelines.
Number figures sequentially as they appear (Figure 1, Figure 2.).
In your writing, be sure to cite the figures in the text.
Insert a caption below the graph that briefly explains what the graph is presenting.
Each axis should be clearly labeled, including units.
Figures should not be divided across page boundaries
Remove gridlines, titles and equations from the graph. If this information is pertinent, it
should be included in the caption.
If the slope or intercept is necessary for other parts of the experiment, then place the
values in the caption with proper units.
16
Absorbance at 470 nm
0.8
0.6
0.4
0.2
0
0
0.02
0.04
0.06
0.08
0.1
0.12
Concentration (mM)
Figure 1. A calibration curve for the absorbance at 470 nm of aqueous Allura Red solutions as a function of
the concentration. A best fit line was rendered resulting in a slope of 5.86 mM -1.
Results:
The results section is where you should report all of your results. Anything that you are
calculating, including your significant results, should be stated here. This section will usually
contain either tables or figures, and should always display the significant result of the
experiment. The Introduction states the purpose. The Data section shows the collected data. The
Results section gives the final results.
You do not need to write out your calculations here. Any calculations that you do should be
attached at the end of the report.
Discussion:
In this section, you will discuss interpretations of the experimental results. This is where you
get to present your thinking process. You will want to draw everything together in this section.
Your introduction provided the purpose and followed a logical pathway to measuring Data. Your
Discussion section should bring everything from the results section to your final result along a
similar pathway. For any labs that have questions to answer, this is also where the answers get
written up.
The discussion is one of the most important parts of the lab report! It is your chance to
show WHAT YOUR RESULTS ARE and that you UNDERSTAND what you did in the
lab. This DOES NOT mean to include detailed procedures or that you need to re-explain your
calculations in words. It DOES mean that a general description of the experiment can be useful
in explaining your results and putting them in context.
In this section you should also discuss error analysis. For your error analysis you should be able
to look at whether your results were greater than or less than (in magnitude) the expected results.
You should be able to identify plausible sources of error from that. Try to see what could explain
away the direction of your error. If you measure too much heat, for example, it would not be
plausible that the primary error source was loss of heat to the atmosphere.
It is possible that nothing actually went wrong. If this is the case, you will need to dig deeper to
explain away any error. This happens when your percent error is very small. Try to investigate
what might have caused your results to vary. If something did go wrong, like your lab partner
17
forgot to write down the exact molarity of your reagent, then that should go here, too, along with
an explanation of how you attempted to correct for the error. Just keep it in third person passive
voice
When answering any additional questions that are posed at the end of the lab, make sure that you
approach the question from the context of the lab. There are many possible methods that might
be used to solve a particular problem or determine a particular characteristic of a chemical. Each
experiment is designed to show you how a specific problem can be solved using some set of
theories and laws. Use that information to answer additional questions.
Adapted courtesy of Keith James and Jonathan Frankel.
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Abstract
The abstract is a condensed summary of the report's findings. Abstracts are often written last.
They should be clear, concise, and self-contained and, in the context of this lab, approximately
three sentences long.
_____What did you do? (Identify the rationale behind the investigation)?
_____How did you do it (summarize the procedure, without using specific steps)?
_____Present the important findings numerically including error statistics?
Introduction
The introduction will provide the reader information on what you are doing why you did it and
critical background information necessary in understanding the methods and results of your
experiment.
_____Did you include a statement of purpose?
_____Is there sufficient background so that the reader can understand what you did?
_____Are necessary equations, chemical or mathematical, included?
Data
This section should give only the data and observations from the lab, without results
_____Are your data tables properly formatted?
_____Are your figures and tables numbered sequentially and referred to in the text. Table
captions above and figure captions below. Tables and figures are not broken over
multiple pages
_____Are the axes on your graphs formatted properly with labels?
_____Are all graphs and tables accompanied by a written description relating the same
information to the reader?
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Results:
This section is for any significant results that you calculated. The results here should reflect what
you stated in your purpose. Your readers must easily find your results in order to evaluate and
interpret them. You should have a paragraph here that clearly states your results in addition to
the tables or figures.
_____Units? Significant Figures?
_____Is a straight forward presentation of the results of your experiment included in
either a table or in text?
_____Can your key results be understood by a reader without reliance on figures and
tables?
Discussion:
In this section, you will discuss interpretations of the experimental results. It will be necessary to
describe your results, cite tables or figures. You should bring everything together in this section
following a logical progression similar to the introduction. You will need to present plausible
sources of error, with an explanation as to how that source caused your results to differ from the
accepted or expected values.
_____Can your key results and discussion be understood by a reader without reliance on
figures and tables?
_____Are key results highlighted and carefully explained?
_____Did you make logical deductions based on the results (usually questions are given
in the lab manual to help this)?
_____Have you referenced any figures, tables or key results?
_____Have you discussed sources of error or ambiguities in the data?
_____Did you confirm all relationships that were stated in purpose or abstract?
_____Do your conclusions clearly contribute to the understanding of the overall
problem?
_____Are all of your calculations attached at the end?
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CH227 LABS
Lab: Scientific Measurements: Precision and Accuracy
Background
Accuracy is a measure of how close a measurement is to the correct value. For example, the
accepted density of zinc is 7.14 g/mL. One student may experimentally determine it to be 7.27
g/mL and another may determine it to be 7.20 g/mL. Because the value 7.20 g/mL is closer to the
accepted value, it is considered to be a more accurate measurement. You will find that in some
cases there is no accepted value to compare a result to. In those cases, accuracy cannot be
measured.
Precision is a measure of the reproducibility of a measurement, how close a set of measurements
are to one another. If, in a series of trials, you measured the density of zinc to be 7.26 g/mL,
7.28 g/mL and 7.25 g/mL, your values are quite close to each other. This suggests that your
precision is good.
Precision also deals with how small of a change can accurately be measured. For instance, think
about measuring your weight on a bathroom scale as compared to a roadside scale, a scale the
measures the weight of large trucks. On a bathroom scale your mass might read 155.6 pounds
but on the roadside scale, your mass may be given as 140 pounds. The bathroom scale has the
ability to measure relatively small masses to the nearest 0.1 pounds, while the roadside scale has
the ability to measure large masses to the nearest 20 pounds. Measurements made of relatively
small masses will be more precise with the bathroom scale; reproducibly, you will be able to
measure a mass to the nearest 0.1 pounds. The limited precision of the roadside scale would
create a level of uncertainty in measuring small masses. This uncertainty will restrict the
conclusions that can be made from the measurement so a roadside scale would not be the
instrument of choice for measuring a persons weight. Scientists represent this precision in the
equipment by putting writing error after the measurement. For example, the first scales
measurement would be written as 155.6 0.1 lb. This shows that there is an uncertainty in the
last digit of the measurement. The roadside scale measurement would be written as 140 20 lb.
In this class, we will use significant figures to indicate the level of precision with which a
measurement has been made instead of writing the error using the error notation.
The greater the level of precision, the greater the number of digits in that measurement that are
significant (Signficant Figures). For instance, 155.6 lb has four significant figures, meaning
that all of the digits in the value are known with a relatively high degree of certainty. The value
140 lb, on the other hand, has only 2 significant figures, the one and the four. Because of the
scale used above, we can only have a relatively high degree of certainty of the value to the tens
place. The more significant figures that are reported the more precise our measurement. Just be
sure not to report more significant digits than the instrument used for measuring will allow.
The manipulation of measurements with a know precision (number of significant figures) is
included in your text book. In general, when making a measurement, it is customary to include
all the known values of a measurement plus one digit that is estimated. Assuming that the
bathroom scale is not digital, suppose that when weighing yourself in the example above, the
needle points somewhere between 155 and 156 pounds. You know your weight greater than 155
pounds but less than 156 pounds. To arrive at the 155.6 pounds reported above, you had to
21
estimate the 0.6 pounds (the estimated value in the measurement). In general, estimate the value
to one decimal place more than the level of graduation. In the example above, the graduation is
every 1 lb. Therefore, the measurement is reported to the 0.1 lb
Every measurement you make in this lab must include the proper number of significant figures.
To determine this, one only needs to look at the graduations on the instrument used to make a
measurement. You will be limited to 1/10 of the smallest known graduation.
Procedures
You will be graded on the number of digits used, the presence of units on your measurements,
and explanations. Use a pen to record all measurements!!!
1) Measurements using a graduated cylinder.
Your TA will have a large graduated cylinder filled with some amount of a liquid on
display. Without consulting anyone in your class and without sharing your value,
determine the volume of the liquid and record the value here__________
Before continuing, report your value to your TA. Your TA will lead a quick discussion
about your results before allowing you to continue.
When measuring volume using a graduated cylinder, one always records the
volume as the level at the TOP / BOTTOM of the meniscus. Circle the best
response.
Take out a 25-ml graduated cylinder. Check to see whether your graduated cylinder is
calibrated to every 1 mL or every 0.5 mL.
The 25-mL cylinder is calibrated to every ______ mL.
Since the graduations are every 0.5 mL it is difficult to report your measured
volume beyond one decimal place. Use the following info to estimate the the
measured value:
22
With certainty, you can see the liquid is slightly above 12.5 mL. The bottom of
the meniscus sits just above 12.5 mL. Lets approximate that the liquid is 4/10
(0.4) of the distance between the graduations 12.5 and 13.0 mL. Since each
graduation is 0.5 mL, 0.4 x 0.5 mL = 0.2 mL. Add this to your certain digits: 12.5
mL + 0.2 mL = 12.7 mL. 12.7 mL should be recorded.
Place about 10-20 ml of water into your 25-mL cylinder and make a sketch of it below,
with at least two labeled graduations (as in the previous drawing). Be as accurate in your
drawing as possible.
________________
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2) Measuring lengths
Now find a small plastic ruler and measure your pencil. Always use the smallest
graduations on your instrument when taking a measurement
Length (cm) = ______________________
Length (mm) = ______________________
Obtain a meter stick and record the length in meters (if the meter stick is graduated to the
mm, be sure to add the appropriate number of digits in your response).
Length (m) = ______________________
Does your measurement have a different precision when you use a meter stick? Explain.
3) Measuring mass
Obtain something with mass. Use the balance to measure the mass of the weight. With a
digital balance, always record every digit the balance displays. Record your units.
Mass _________________
Based on your observations, how many decimal places does this balance report?
How many significant figures can you report based on the graduations? ________ sig
figs (circle the digit above that was estimated).
Now take the contents of your beaker (the 25 mL of water) and pour it into your 100 or
150 -ml graduated cylinder. Thinking about what you learned earlier (looking at the
graduations), record a measurement for the volume of water.
_______________ mL(using a 100 or 150 -ml graduated cylinder)
Which is more precise, the volume measurement using the beaker or the graduated cylinder?
Given a choice, which glassware would you use to measure volumes more precisely? Explain.
Suppose a 10-mL graduated cylinder has an uncertainty of about 0.01 mL. If it is filled with
water to the mark (10-mL), the volume should be reported as (include the necessary decimal
places):
_______________ mL
Provide a measurement for each of the following pieces of glassware filled to the level indicated
by the arrow. Use the correct number of significant figures in your answer. Always use units.
Remember to estimate one digit more than the level of graduation (image B is correct, do not
modify).
25
Part B
Prepare your lab notebook for the experiment. This includes stating the purpose of
the experiment and summarizing the procedure in a bulleted-list format (be sure to
include space for observations).
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
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identify the elemental composition of a substance. For instance, potassium produces a violet
color while lithium will emit a vibrant red.
5) Acidic, basic or neutral aqueous solutions: Some substances will make a solution acidic or
basic when they dissociate into ions when dissolved in water. Some ions have the ability to act as
acids in solution while others act as bases. When a substance is dissolved in water, these
properties can easily be tested using pH paper.
6) Reactivities: Each compound has a characteristic reactivity that may or may not be easily
elucidated. By mixing an aqueous solution of the unknown with an aqueous solution containing
another compound, reactivity patterns may become visible. Reactions are usually visualized by
looking for the formation of a solid, gas or change in color.
This lab is based upon the journal article "Who Has the Same Substance that I Have?": A Blueprint for
Collaborative Learning Activities, Brian P. Coppola, Richard G. Lawton, Journal of Chemical
Education 1995 72 (12), 1120 and Identification of Ionic and Molecular Compounds,
http://tinyurl.com/3jf6oq6, n.p. n.d. Web. 24 Aug. 2011
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Equipment Information
Each bin should contain:
Hazards
toxic, oxidizer, corrosive, health and environmental hazard
corrosive
corrosive
Toxic
none
health and environmental hazard
none
none
toxic
29
PROCEDURES
1. Physical characteristics
a. Obtain a small (pea-sized) sample of your assigned unknown.
b. Using a magnifying glass, examine the sample and record your observations in
your lab notebook
2. Determine conductivity in the solid state
a. Using the sample obtained previously, test for electrical conductivity using the
conductivity meter supplied by touching the probes to the sample. [Be sure the
probes are dry!]
b. Record your observations
3. Determine the relative solubility of each unknown
a. Add of your pea-sized sample of the unknown to a small test tube. Add 2 cm
or approximately 1 fingers width of deionized water to the test tube.
b. Mix with your scoopula.
c. Record your observations as S = soluble or IN = insoluble (soluble means that a
clear solution has formed, insoluble means that the sample is cloudy or that there
is undissolved solid left in the test tube).
d. Do not discard the contents of the test tube!
4. Determine the conductivity of the solution made in step 3
a. As a control, use the conductivity meter to check the conductivity of deionized
water and record your observations.
b. Pour a little of your unknown aqueous solution into one well of the microplate,
test for conductivity, and Rrecord your observations.
c. Do not discard the contents of the microplate!
5. Determine if the aqueous solution is acidic, basic or neutral.
a. Dip your scoopula in your solution and wipe it on a piece of pH paper. The paper
is normally orange. It will turn red if the solution is acidic or blue if basic.
b. Record your observations
6. Determine the reactivity of your unknown.
a. Using a dropper, equally divide your solution amongst three wells (including the
one you already used) in your multi-well microplate. (The wells should not be
full.)
b. Add 5 drops of 1M hydrochloric acid (HCl) to the first well. (The symbol M
represents molarity, a unit of concentration. The greater the molarity, the greater
the concentration.)
c. Add 5 drops of 0.1 M lead(II) nitrate (Pb(NO3)2) to the second well.
d. Add 5 drops of 1.0 M sodium hydroxide (NaOH) to the third well. Waft a watermoistened piece of pH paper over the third well to see if a gas (ammonia) is
produced. Note: aqueous solutions of ammonia are basic, and the pH paper would
turn blue in the presence of ammonia gas.
e. Record your observations, such as turned cloudy or no change.
f. Clean your test tube, multi-well plate and dropper as directed by your TA.
30
DATA
Guided by your TA, you will construct a table to report your results and observations.
For the TA
The most important practical aspect of setting up this experiment is to ensure that the identification is based on the
experimental data that are collected by the students.
Please discuss contamination and how to avoid contaminating the stock solutions and unknowns. Possible unknowns
include: ammonium iodide, sodium acetate, silver nitrate, calcium carbonate, sugar, lithium carbonate, aluminum
chloride, citric acid, potassium iodide, some of which are hazardous chemicals.
31
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
33
INTRODUCTION:
If you were to measure out identical volumes of Coke and diet Coke, you would find that
the two liquids have different masses. This difference in the mass of the two liquids is best
discussed by looking at the mass per unit volume (or density) of the two liquids.
M
D
Density = Mass Volume
V
Density is a convenient quantity because it is independent of the volume used (scientists describe
properties like this as intensive). Intensive properties like density are independent of the amount
of substance and thus the density of two different solutions can be compared without needing to
have the same volume of the two solutions. .
When comparing Coke and diet Coke, it is found that Coke is more dense than its sugar
free relative. To understand why, a molecular view of the two substances is useful. The main
difference between the two solutions is the presence of the dissolved sugar in Coke that is
absent in diet Coke. The sugar makes Coke more dense than diet Coke. To a first approximation,
Coke can be represented as a solution of sugar dissolved in water. As the amount of sugar
dissolved in a given volume of water increases, so does the density of the resulting solution. This
makes it possible to determine the mass of sugar in Coke by comparing it to solutions with
known concentrations of sugar.
The relationship between the amount of dissolved sugar and the density of sugar water
solutions will be determined using a calibration curve. Calibration curves are constructed using
known quantities, called standards. Calibration curves allow you to determine the content of an
unknown by comparing it to observations made on the standards with known values of the
property being measured. In this case, you will prepare standard solutions of known volume with
a known amount of dissolved sugar. After obtaining the mass of these standards using an
instrument called a balance and calculating the density of each solution, you will prepare a graph
of density vs. mass of dissolved sugar . You will then determine the mathematical relationship
between the two quantities. Once the relationship between density and sugar content is
determined, you will use this relationship to determine the amount of sugar in Coke.
SCIENTIFIC GRAPHS:
This experiment will also serve to introduce you to scientific graphing. Here, we will
introduce what must be included in any scientific graph. Whenever you are asked to produce a
graph from laboratory data (either by hand or using a computer program) all of the following
criteria must be met:
1. All graphs should have a title (except when included in a report or other scientific
writing, in which case you substitute a figure caption below the figure for the title)
2. Both axes must be labeled with a name and units
3. The graphed data must take up the full space of the graph
34
4. When a best-fit line to the data is computed and used, the line should be shown on the
graph. The equation should be included in the caption below the graph.
5. The independent variable is the x-axis and the dependent variable is the y-axis, and the
graph is referred to as dependent vs. independent for example the graph below is
Mass (in grams) vs. Volume (in mL)
6. Gridlines should only be included if they enhance the understanding of the graph.
Figure 1 shows an example of an acceptable scientific graph of raw data. Figure 2 demonstrates
the proper way to represent a linear fit on a graph.
The Relationship Between Mass and Volume for Water
60
50
Mass (g)
40
30
20
10
0
0
10
20
30
40
50
60
Volume (ml)
50
Mass (g)
40
30
20
10
0
0
10
20
30
40
50
60
Volume (ml)
Figure 2: The relationship between Mass and Volume for Water. Varying
volumes of water were massed. A linear relationship exists between mass
and volume. A best fit line was calculated using Microsoft Excel yielding
the following equation: y = 1.0015x + 0.009.
Graphing Using Microsoft Excel:
An excellent tutorial on graphing with MS-Excel can be found at the following website:
http://www.ncsu.edu/labwrite/res/gt/gt-menu.html
35
This is a list of the basic steps necessary to graph data and do a linear regression (the generation
of a best-fit line) using Excel:
Basic Graphing:
1. With the program open, enter the data to be graphed in the cells. Enter x data in one
column followed by y data in an adjacent column.
2. Click and drag the mouse to highlight all the data to be graphed.
3. Click on the chart wizard icon
4. Choose XY (Scatter) for the chart type and the unconnected points icon for the Chart
sub-type
5. Click next. A preview of your chart will appear. If it appears correctly, click next.
6. Enter a chart title and the axis labels and click finish
7. With the chart selected you can also access the title and axis labels by selecting Chart
then chart options from the drop down menu
Adding a Linear Trendline to a Graph:
1. With the graph selected, select Chart then add trendline from the drop down menu.
2. Select linear as your regression type
3. Select the options tab in the popup window
4. Select the display equation on chart button and click ok
36
Equipment Information
Each bin should contain:
Hazards
none
none
37
PROCEDURE:
Calibration Curve:
You will make one sample without sugar and five sugar water solutions to start. Each
solution should have a different amount of dissolved sugar covering a range from about 1 8 g
of sugar per 50 mL of solution volume. To make the solutions in a quantitative manner, they
must be prepared in volumetric flasks. Volumetric flasks are designed to accurately contain a
specific volume. Volumetric flasks are marked with a fill line. When filled to the marked line,
the flask accurately holds the stated volume (these devices are called TC for to contain). When
putting the last bit of solvent into volumetric flasks, it is best to bring the fluid to the line
carefully by using a wash bottle or eyedropper to assure that the flask is not overfilled (causing
you to have to start over).
For the sample without sugar:
1. Weigh the empty flask and record the mass.
2. Add water carefully to the fill line.
3. Weigh the flask containing the solution and record the mass. (The difference between this
mass and the first one is the mass of the solution the volume is 50 ml, if you carefully
followed these instructions.)
To accurately know the mass of sugar used in each of your five standard solutions, follow these
steps:
1. Weigh the empty flask and record the mass.
2. Weigh out the desired mass of sugar in a weigh boat. (This mass does not need to be
recorded.)
3. Add the sugar to the flask. Weigh the flask containing the sugar and record the mass.
(The difference between the two masses is the mass of sugar.)
4. Add water to the flask until it is approximately half way to the fill line. Swirl the flask to
dissolve the sugar. Do not shake the flask.
5. Once the sugar has completely dissolved, add water carefully to the fill line. Put the
stopper in the flask or cover the top of the flask with Parafilm and invert it ten times to
ensure that the solution is thoroughly mixed. (The bubble should run all the way down
the neck of the flask to the stopper each time you invert the flask.)
6. Weigh the flask containing the solution and record the mass. (The difference between this
mass and the first one is the mass of the solution the volume is 50 ml, if you carefully
followed these instructions.)
As noted above, the mass of sugar used for each solution is found by subtracting the mass of
the empty stoppered flask from the mass of the stoppered flask containing sugar. The mass of the
solution is found by subtracting the mass of the empty stoppered flask from the mass of the
stoppered flask containing the solution.
Below is an example of an acceptable table to present the data from this experiment. In this
experiment, a table is supplied for you. In later experiments, you will be expected to produce
your own data tables for your notebook and the Results section of your lab reports. Be sure that
you add an appropriate caption to the table. See the report guidelines section of the manual for a
discussion on this.
38
Mass of
Empty
Flask +
Stopper
(g)
Pure H2O
Mass of
Flask +
Stopper
With
sugar (g)
------
Mass of
Mass of
Flask +
Sugar
Stopper
(g)
With
solution (g)
------
Mass of
Solution
(g)
Density
of
Solution
(g/ml)
Dissolved
sugar per
mL
solution
(g/ml)
0.0
Flask 1
Flask 2
Flask 3
Flask 4
Flask 5
Using the data in the above table, construct a graph of density of solution (y) vs.
dissolved mass of sugar per mL of solution (x) and fit the data to a linear relationship as
described above. Report the equation for the line on the graph. Graphs must be prepared using
the computer. Your TA will assist you with this, if needed. This graph represents the relationship
between the density of the sugar water solution (something that can be measured) and the
amount of dissolved sugar in the solution (something that cannot be measured directly, but could
be controlled in making the standards).
Determine the amount of sugar in a can of Coke:
Weigh and record the mass of a dry, clean 50 mL volumetric flask before carefully filling
the flask to the fill line with the flat Coke provided. Weigh and record the mass of the flask
containing Coke. Determine the density of the Coke. Put the used Coke in the provided waste jar.
RESULTS:
When a linear relationship exists between two quantities (density and amount of sugar) it
is only necessary to measure one of the quantities (density) and know the relationship (found
from your calibration curve) before the other quantity (amount of sugar) can be determined. By
finding the density of coke (y-axis) and drawing a line to your calibration curve, then drawing a
vertical line down to the x-axis (mass of sugar per mL solution) you can graphically determine
the amount of sugar dissolved in each mL of Coke. Alternatively, you can invert the relationship
given by the calibration line equation to solve for x from the observed density (y). Both
methods should give the same result for mass of sugar per mL of Coke.
In order to find the mass of sugar in one can of Coke, you will need to consider the
volume of a can of Coke (12 ounces). One liter contains 33.8 fluid ounces. Calculate the percent
error in your determined value, based on nutritional information given on the label on a can of
Coke.
39
Provide a brief statement of the purpose of this activity and explain the idea behind a calibration
curve.
Data:
Mass of
Empty
Flask +
Stopper
(g)
Pure H2O
Mass of
Flask +
Stopper
With
sugar (g)
------
Mass of
Mass of
Flask +
Sugar
Stopper
(g)
With
solution (g)
------
Mass of
Solution
(g)
Density
of
Solution
(g/ml)
Dissolved
sugar per
mL
solution
(g/ml)
0.0
Flask 1
Flask 2
Flask 3
Flask 4
Flask 5
40
Results:
Copy and paste your calibration curve in the space below. Make sure you have
formatted it as described in the Report Guidelines located in the front of this
manual.
Report the amount of sugar in 1 mL and 1 can of coke, showing any necessary
calculations.
Present the percent error for your amount of sugar in a can of coke with respect to
the number given on the label, showing any necessary calculations.
41
Based upon if your value is greater or less than the labeled sugar content, provide
any valid sources of error
There is not a form al lab report for this lab. Com plete the
above pages using the Microsoft version of this file that is
available for d ow nload on the lab D2L page. Once the
w orksheet is com plete, subm it the w orksheet on tim e and
to your TA in the d ropbox on D2L.
42
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
43
INTRODUCTION:
This experiment will cycle elemental copper through a series of five reactions
summarized below:
Cu(NO3)
NaOH
Cu(OH)
2
HNO3
heat
Cu
Zn, HCl
CuSO4
H2SO
CuO
The cycle will both begin and end with pure elemental copper. At different stages of the
cycle, copper will be present in different chemical forms. At times copper will be present in solid
compounds and other times in ionic form. Each chemical change that copper undergoes is
observable as a change in the physical properties of the solution (or precipitate). As you perform
each reaction, be certain to observe and record your observations of all physical changes.
At this point in the term, you should have been introduced (in the lecture class) to three
different types of aqueous reactions: precipitation reactions, acid-base reactions, and oxidationreduction (or redox) reactions (in addition, the text may have discussed gas-forming reactions).
In precipitation reactions, soluble cations and anions combine to form an insoluble compound
that leaves the solution as a solid precipitate. In acid-base reactions, an acid and base react to
produce water and a salt. Redox reactions involve the transfer of electrons. As you go through
the series of reactions you should be able to classify each reaction (with the exception of reaction
3) as one of the three above-described types of aqueous reactions.
Reaction 1: The first reaction proceeds according to the following balanced chemical
equation:
4 HNO3 (aq) + Cu (s) Cu(NO3)2 (aq) + 2 H2O (l) + 2 NO2 (g)
44
In this first reaction, elemental copper metal is reacted with concentrated aqueous nitric acid
solution. The result of this reaction is that copper changes from its elemental state (charge = 0) to
an aqueous, ionic state (Cu2+) in an oxidationreduction reaction.
Reaction 2: The second reaction then converts the aqueous Cu2+ into the solid copper (II)
hydroxide (Cu(OH)2) through a precipitation reaction with sodium hydroxide according to the
following balanced chemical equation:
Cu(NO3)2 (aq) + 2 NaOH (aq) Cu(OH)2 (s) + 2 NaNO3 (aq)
Reaction 3: The third reaction takes advantage of the fact that Cu(OH)2 is thermally unstable.
When heated, Cu(OH)2 decomposes (breaks down into smaller molecules) into copper (II) oxide
and water according to the following decomposition reaction equation.
Cu(OH)2 (s) + heat CuO (s) + H2O (l)
Reaction 4: When solid CuO is reacted with sulfuric acid, the copper is returned to solution as
an ion (Cu2+) according to the following acid-base metathesis / double displacement reaction
equation.
CuO (s) + H2SO4 (aq) CuSO4 (aq) + H2O (l)
Reaction 5: The cycle of reactions is completed in this reaction where elemental copper is
regenerated according to the following oxidation-reduction reaction equation. Thhis reaction
changes copper from its ionic state (Cu2+) to its elemental state by exchanging electrons between
zinc and copper.
CuSO4 (aq) + Zn (s) ZnSO4 (aq) + Cu (s)
Here, zinc and copper exchange physical (and oxidation) states in and out of acidic solution.
Hydrochloric acid is then used to dissolve any excess zinc. The solid copper can then be
collected, washed, dried and weighed. Some copper is bound to be lost in all of the chemical
transformations, so the percent recovery (mass copper remaining/initial mass x 100%) is
expected to be less than 100%.
45
Equipment Information
There are no bins this week.
Notes:
a. Concentrated acids are being used this week. Restrict their use to the hoods.
b. If any concentrated acid is spilled, use spill neutralizer to neutralize the
spill. Then, clean up the solid waste using the hand broom and dustpan
found near the broken glass container.
Hazards
oxidizer, corrosive
corrosive
corrosive
corrosive
flammable, environmental hazard
flammable, environmental hazard
46
PROCEDURE:
Reaction 5:
Caution: Concentrated hydrochloric acid is hazardous. Avoid getting it on your skin or
clothing. If you do get any on your skin or clothing, wash it off immediately with water. Do
not breathe vapors.
DO THIS NEXT STEP IN THE HOOD. Hydrogen gas is generated which is extremely
flammable. There should be no open flame in the room. Additionally, there is some
possibility of producing more nitrogen dioxide gas, so do not breathe the vapors.
Add (all at once) 1.0 g of 30-mesh zinc or zinc powder. Stir until the supernatant liquid is
colorless (not blue); the solution can be murky and grey. Decant the supernatant liquid. Remain
in the hood and add 5 mL of distilled water followed by 10 mL of concentrated hydrochloric
acid. The hydrochloric acid removes any excess zinc according to the following balanced
chemical equation.
Zn (s) + 2 HCl (aq) ZnCl2 (aq) + H2 (g)
If the hydrogen gas evolution stops before all of the solid zinc has been removed, more acid (in 1
mL aliquots) can be added. Once the evolution of hydrogen gas has become very slow, the flask
may be returned to the workbench. You may warm the mixture on a hot plate to speed up the
reaction, but do not boil the solution. Once the hydrogen gas evolution has completely stopped,
remove the flask from heat and carefully decant the liquid. Transfer the solid copper to a clean
pre-weighed beaker. Using a wash bottle to wash the copper metal into the dish can facilitate the
transfer. Wash the copper at least twice with about 5 mL of distilled water each time. Decant the
water after each wash. Wash the copper with an additional 5 mL of methanol. Allow the copper
to settle and decant the methanol. Gently heat the copper on a hot plate to evaporate any
remaining methanol and dry the copper. Once dry, remove the copper from the hot plate and
allow the beaker to cool before determining the mass of the recovered copper. Be sure to record
all observations and the final mass of the copper.
RESULTS:
Once the mass of recovered copper is known (difference between the pre-weighed beaker
plus copper and beaker alone), the percent recovery can be calculated from the following
formula:
Percent recovery = (mass of copper recovered/initial mass of copper)*100%
REFERENCE:
1. Condike, GF, J. Chem. Ed. 1975, 52, 615.
48
Part B
Prepare your notebook for the lab. This includes stating the purpose of the experiment,
summarizing the procedure in a bulleted-list format (be sure to include space for observations)
and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you completed the above work
from your lab notebook and turn them into your TA.
50
51
Equipment Information
There are no bins this week.
Notes:
a. Use two pieces of filter paper for filtering.
b. Dry the barium carbonate (BaCO3) using the filter flask.
c. There are two waste streams this week. Be sure to use the correct one for
each stage of your procedure.
Hazards
toxic
toxic
toxic
toxic
corrosive
52
PROCEDURE:
Be sure to discard all waste in the waste jars as directed by your TA
1. Add a 0.5 g (approximately, but massed to mg accuracy and recorded in your notebook)
sample of your carbonate to a 250 mL beaker. Add 50 mL of water and stir until the
carbonate is completely dissolved.
2. To precipitate the barium carbonate, add 20.0 mL of 1.0 M BaCl2 solution to the sample
and stir until well-mixed. CAUTION: Use gloves to handle the barium compounds.
3. Heat the BaCO3 formed to digest the precipitate (causing the precipitate to form larger
aggregates). This involves boiling the solution for 5 minutes with little agitation.
4. Weigh one piece of filter paper and your watch glass. Be sure to record the masses in
your notebook.
5. Filter the barium carbonate using the filter paper in a Buchner funnel using vacuum
filtration as demonstrated by your TA.
6. Wash the precipitate with water using the vacuum to pull the water through the filter and
allow the solid to dry for 10 minutes with the vacuum still on.
7. Carefully remove the solid and filter paper from the funnel and place your product on a
pre-weighed watch glass. Allow the solid to dry until near the end of the lab period. It
may be necessary to put the watch glass on a hot plate (on LOW heat for 10 minutes) to
speed up the drying process. CAUTION: The filtrate (solution left after filtration to
isolate barium carbonate) contains excess Ba2+. Dispose of in the proper waste
container (see TA if you are unsure of the proper procedure). DO NOT DUMP
THIS SOLUTION DOWN THE SINK.
8. Weigh the combined dry solid and filter paper and record the mass in your notebook.
Calculate the mass of barium carbonate by difference (removing mass of watch glass and
filters).
Analysis
Use the following questions to lead you to the identity of M:
Determine the mass of barium carbonate produced as above. How many moles of barium
carbonate is this?
Use stoichiometry to determine how many moles of M2CO3 reacted to produce the barium
carbonate, and hence were present in the 1.00 g sample you started with.
Determine the molar mass of the unknown metal carbonate (not the metal itself) and compare it to
the molar mass of the possible alkali metal carbonates (Li2CO3, Na2CO3, K2CO3).
What alkali metal carbonate is your sample most likely to be?
Where are the errors most likely to enter into the experiment?
53
PROCEDURE:
1. Place 0.5 g of your unknown in a pre-weighed 250 mL beaker.
2. Measure 40.0 mL of 1 M HCl in a pre-weighed graduated cylinder.
(Determine the actual mass of HCl added.) Pour the HCl slowly onto the
unknown metal carbonate.
3. Measure the mass of the beaker after the reaction has ceased (no further
generation of carbon dioxide gas).
Analysis:
Use the following questions to lead you to the identity of M:
Determine the mass of CO2 produced (use the average from the three trials).
How many moles of CO2 were produced?
Use stoichiometry to determine how many moles of M2CO3 were present in the 1.0 g
sample you started with.
Determine the molar mass of the unknown metal carbonate (not the metal itself) and
compare it to the molar mass of the possible alkali metal carbonates (Li2CO3, Na2CO3,
K2CO3).
What alkali metal carbonate is your sample most likely to be?
Where are errors most likely to enter into the experiment? Which direction do these
errors bias the final answer (molar mass of metal carbonate)?
54
Flame test
In this experiment you will make use of the fact that metal salts, when heated in a flame, emits
light whose color is characteristic to the metal ion in the salt (see Table 1). The heat excites the
electrons in the metal. When the excited electrons relax to what is called their ground state,
the release a photon of light that has a characteristic energy or color (if the photon is in the
visible portion of the electromagnetic spectrum). This property is used to identify unknown
metals and even quantify their amounts present in a sample.
Table 1: Characteristic Colors for the Flame
Test of Certain Group 1 Salts.
Group 1
Element
Li
Na
K
Rb
Flame
Color
Crimson
Golden Yellow
Violet
Blue-violet
PROCEDURE:
1. Soak a toothpick in water for 1 minute.
2. Touch the wet toothpick into the previously unused half of your unknown
solid to pick up a small quantity of the solid. Place the portion of the
toothpick with the solid on it in the hot part of the flame. Observe the
color of the flame.
3. Record your results.
4. Repeat steps 1-3 if necessary.
55
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
57
Hypothesize about the conductivity of a solution of sulfuric acid and barium hydroxide at
various stages during the reaction.
Use a Conductivity Probe to monitor conductivity during the reaction.
Observe the effect of ions, precipitates, and water on conductivity.
INTRODUCTION
In this experiment, you will monitor conductivity during the reaction between sulfuric acid
(H2SO4) and barium hydroxide (Ba(OH)2) in order to determine the equivalence point. [In this
reaction, sulfuric acid will function as a diprotic acid and barium hydroxide as a dibasic base.]
From the volume used and known concentration of the sulfuric acid, you can find the
concentration of the Ba(OH)2 solution. You will also directly observed the effect of ions,
precipitates, and water on solution conductivity. The balanced chemical equation for the reaction
in this experiment is:
When the Conductivity Probe is placed in Ba(OH)2, prior to the addition of H2SO4.
As H2SO4 is slowly added, producing BaSO4 and H2O.
When the moles of H2SO4 added equals the moles of BaSO4 originally present.
As excess H2SO4 is added (beyond the equivalence point).
When you have reached a consensus about what will happen during the experiment, proceed
with the procedure below.
58
Equipment Information
Each bin should contain:
1 conductivity probe
Notes:
a. Use two pieces of filter paper per filtration.
b. Parafilm can be reused.
Hazards
corrosive
corrosive, toxic
59
d. Next, use 2-drop increments (~0.1 mL) until the minimum conductivity has been reached
at the equivalence point. Read and enter the volume after each 2-drop addition. When you
have passed the equivalence point, continue using 2-drop increments until the
conductivity is greater than 100 S/cm again.
e. Finally use 1.0 mL increments (read and enter the volume at each increment) until the
conductivity reaches about 2000 S/cm.
8. When you have finished collecting data, click
waste jar as directed by your TA.
of H+ to moles of OH ).
4. From the moles and volume (25 mL) of Ba(OH)2 used, calculate the concentration of Ba(OH)2, in
molarity (mol/L).
Provide a brief statement of the purpose of this activity. Be sure to define equivalence point.
Explain conductivity and the idea behind why conductivity can be used in determining the
equivalence point in a titration.
62
Copy and paste your titration curve in the space below (include a descriptive caption).
Report your determined concentration of Ba(OH)2 from both analysis methods (if they
differ). Show any relevant calculations.
63
Discussion:
Briefly discuss which of the two analysis methods you feel was the most accurate (be
sure to support your answer with an explanation)? Why does the conductivity not go to
zero?
There is not a form al lab report for this lab. Com plete the
above pages using the Microsoft version of this file that is
available for d ow nload on the lab D2L page. Once the
w orksheet is com plete, subm it the w orksheet on tim e and
to your TA in the d ropbox on D2L.
64
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
65
To view the hydrogen emission spectrum and other atomic line spectra
To contrast the line spectra with other broad-band sources
To measure the wavelengths of the bright lines in the visible emission spectra of
hydrogen and mercury, and calculate the energy of each line
To gain an understanding of the quantized nature of the hydrogen atom
Supplies
Definitions
1. A spectroscope is an instrument that allows you to analyze light in some way. In this case,
your spectroscope acts like a prism, splitting the light into different wavelengths.
2. A continuous spectrum is one in which a rainbow of colors is seen when viewed through a
spectroscope or prism.
3. A line spectrum, when viewed through a spectroscope, appears as one or more sharp narrow
lines (colors).
4. A band spectrum is intermediate in appearance there will be a brightest color, but a range of
nearby wavelengths are emitted.
Background
The understanding of the internal structure of the atom was advanced when Niels Bohr explained
the cause of the emission spectra of atoms using the concept of quantization. He stated that
electrons in the atom could exist at finite energy levels, but not in between them. Electrons
within an atom can be excited to higher energy states through various means, including heating
the atoms or using an electric discharge, like a spark. After exciting the electrons, the atoms emit
electromagnetic radiation as the excited electrons relax into a lower energy state. The energy of
the light emitted is equal to the difference between the energy levels in the atom. This emitted
light can be passed through a prism or reflected from a diffraction grating to spatially separate it
into its individual wavelength components (colors) generating an atomic emission spectrum, a
line spectrum characteristic of the particular sample of atoms.
As an example, the emission spectrum of hydrogen consists of only four visible lines: red, bluegreen, violet and deep violet (although your eyes may not be sensitive to the last one, since
individuals visual acuity varies). Each color corresponds to the transition of an electron from an
excited state, a higher principal energy level, to a lower principal energy level, possibly the
66
ground state or some other allowed energy level in between. As the electron drops, it emits
energy in the form of a photon which may or may not be in the visible region.
In this experiment you will use a spectroscope and gas discharge lamps to measure the
wavelength of each bright line in the visible atomic emission spectra of both hydrogen and
mercury. You will then use these measurements to calculate the photon energy for each bright
line. Recall that the energy of light is related to the wavelength and frequency of the light,
through Plancks constant h = 6.626 x10-34 J sec and the speed of light in a vacuum c = 3.00 x
108 m/sec.
67
WARNING!!
The power supply for the discharge lamps operates at 5000 volts !
DO NOT TOUCH
Figure 1 How a Spectroscope Works. A spectroscope is a small box, with a transparent grating in one
side and a narrow slit directly opposite the grating. To observe a spectrum you point the slit toward a
light source and look through the grating. You will see an image of the spectrum along the back wall of
the box, just over the wavelength scale.
Figure 2: Observing a Spectra Using the Spectroscope. To determine the wavelength of the light you
observe, you will make use of the calibrated wavelength scale which is in hundreds of nanometers.
One band of light that you should observe is a violet band the far right of the spectra. This band should
be at 436 nm, note where that band appears on your spectroscope. A very rough correction factor can be
made using the difference between your measurement and the accepted value (436 nm). If for instance
you measured the violet band at 455 nm, your spectroscope is miscalibrated by about 19 nm. Any
additional measurements made with this spectroscope should be corrected by subtracting 19 nm from the
measurement.
68
Wavelength (nm)
Corrected using calibration factor1
Qualitatively compare the 3 brightest lines from the emission spectra of the elemental mercury lamp to
the spectra of a fluorescent lamp and an incandescent bulb and the red and green colored sources
provided.
If daylight is available and after giving time for your eyes to adjust, observe the solar spectra by looking
at the ambient daylight through a window (no worries if it is cloudy, just aim at the sky). Never aim
directly at the sun. Comment, whether or not the solar spectra a continuous spectra. If not, what do you
think the discontinuities represent?
69
Data Analysis
1) For the first four electronic transitions in the Balmer Series, calculate the change in energy of the
electron (E), the predicted energy of the emitted photon (Ephoton) and the predicted wavelength of the
emitted photon (photon). Put the calculated values in Table 2 and be sure to clearly show an example of
each calculation in the space provided.
Table 2: Calculated Values for the Balmer Series of Hydrogen.
Electronic Transition
E (J)
photon (nm)
Ephoton (J)
n3 n2
n4 n2
n5 n2
n6 n2
Clearly show the following calculations for the n3 n2 transition.
-- the change in energy of the electron, E
2) Based on your theoretical calculations, match the electronic transitions in the Balmer Series to the
spectral lines you observed, and document your choices in Table 3. Then calculate the percent error
between your experimentally determined and calculated wavelengths.
Table 3: Comparison of Experimental and Accepted Wavelengths from the Balmer Series.
Spectral Line
Electronic
Experimental (nm)
Accepted (nm) from
Color Observed
Transition
from Table 1
Table 2
Percent Error
n3 n2
n4 n2
n5 n2
n6 n2
Below, clearly show your percent error calculation for the n3 n2 transition.
70
3) It is not possible to observe the n7 n2 transition in the Balmer Series. Why do you think that is?
4) Emission spectra are sometimes referred to as atomic fingerprints. Is it possible to use them to identify
elements in an unknown sample? Explain your reasoning: think about the Hg spectrum and that of a
fluorescent bulb.
5) Why do you think sodium vapor lights cast a different color (yellowish) than fluorescent lamps?
6) Calculate the ionization energy of the hydrogen atom. Think about this process as taking an electron
from its ground state, n = 1, to a position/energy level far, far away from the nucleus, n = .
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
72
INTRODUCTION
The primary objective of this experiment is to determine the concentration of Allura Red in a
commercially available beverage. You will be using the Colorimeter shown in Figure 1. In this
device, light from the LED light source will pass through the solution and strike a photocell. A
higher concentration of the colored solution absorbs more light (and transmits less) than a
solution of lower concentration. The Colorimeter monitors the light received by the photocell
and reports either an absorbance or a percent transmittance value as compared to a blank, a
solution containing no absorber.
Figure 1
Figure 2
You are to prepare five Allura Red solutions of known concentration (standard solutions) and
conduct a calibration procedure. Each standard solution is transferred to a small, rectangular
cuvette that is placed into the Colorimeter. The amount of light that passes through the solution
and strikes the photocell is used to compute the absorbance of each solution. When a calibration
graph of absorbance vs. concentration is plotted for the standard solutions, a linear relationship
should result, as shown in Figure 2. This linear relationship between absorbance and
concentration for a solution is known as Beers law.
The concentration of Allura Red in an unknown solution (Gatorade) is then determined by
measuring its absorbance in the same way with the Colorimeter. By locating the absorbance of
the unknown solution on the vertical axis of the graph, the corresponding concentration can be
found on the horizontal axis (follow the arrows in Figure 2). The concentration of the unknown
can also be found using the slope of the Beers law line, assuming that the y-intercept of the
calibration line is zero.
73
Equipment Information
Each bin should contain:
Notes:
a. Todays waste can go down the drain.
b. Do not leave a cuvette in the colorimeter at the end of class.
c. The colorimeter should be left out on the lab bench at the end of class. It
should not be put away in a bin.
74
PROCEDURE
1. Obtain and wear goggles
2. Obtain about 30 mL of Allura Red stock solution in a 100 mL beaker. Add about 30 mL of
distilled water to another 100 mL beaker. Be sure to record the concentration of the stock
solution of Allura Red from the container.
3. You will prepare five solutions of Allura Red varying in concentration from approximately 6
x 10-6 M to 2 x 10-5 M. You may wish to check your concentrations and calculations with
your TA before making the solutions. Make the solutions by pipetting the correct quantity of
the Allura Red stock solution into the volumetric flask and then filling to the line with
distilled water. Be careful to avoid getting liquid above the fill line. Thoroughly mix each
solution by inverting the stoppered flask ten times.
4. Connect the Colorimeter to the computer interface. Prepare the computer for data collection
by opening the file Lab 11: Beers Law from the Chemistry 227 folder of Logger Pro. Set
the colorimeter to a wavelength of 470 nm.
5. You are now ready to calibrate the Colorimeter. Prepare a blank by filling the cuvette 3/4 full
with distilled water. To correctly use a Colorimeter cuvette, remember:
All cuvettes should be wiped clean and dry on the outside with a tissue.
Handle cuvettes only by the top edge of the ribbed sides.
All solutions should be free of bubbles.
Always position the cuvette with its reference mark facing toward the white reference mark
at the top of the cuvette slot on the Colorimeter.
10. Be sure to record the absorbance and concentration data pairs that are displayed in the table.
11. Examine the graph of absorbance vs. concentration. To see if the curve represents a linear
relationship between these two variables, click the Linear Fit button, . A best-fit linear
regression line will be shown for your five data points and your blank. This line should pass
near or through the data points and the origin (0,0) of the graph. [Note: Another option is to
choose Curve Fit from the Analyze menu, and then select Proportional. The Proportional fit
has a y-intercept value equal to 0; therefore, this regression line will always pass through the
origin of the graph.]
12. Obtain a small amount of Gatorade in a small clean beaker. Use the pipette to deliver 5 mL
of the Gatorade to a clean volumetric flask. Finish preparing your unknown by diluting the
Gatorade to a total volume of 50 mL with distilled water and mix thoroughly. Rinse the
cuvette twice with the unknown solution and fill it about 3/4 full. Wipe the outside of the
cuvette, place it into the Colorimeter, and close the lid. Read the absorbance value displayed
in the meter. (Important: The reading in the meter is live, so it is not necessary to click
to read the absorbance value.) When the displayed absorbance value stabilizes,
record its value.
13. Discard the solutions in the waste jar as directed by your teacher.
76
With the help of your TA, calculate the molar mass of Allura Red.
Use the molar mass to determine what mass of Allura Red you would consume if you drank one
20 ounce bottle of Gatorade.
Finally, determine the number of molecules of Allura Red you would consume if you drank one
20 ounce bottle of Gatorade (is molar mass necessary for this step?).
This lab was modified from lab 11 Determining the Concentration of a Solution: Beers Law from Chemistry with
Computers, Third Edition, Vernier, Inc.
77
78
Name_____________________________
Electron Density Lab: There is not a formal lab report for this lab. Complete the below
pages using the Microsoft version of this file that is available for download on the lab D2L page.
Once the worksheet is complete, submit the worksheet on time and to your TA in the dropbox on
D2L.
6. Briefly describe the difference between a nonpolar covalent and polar covalent bond.
79
Simulation
In this atomic-level simulation, you will investigate how an atoms' electronegativity value affects the
types of bonds they produce.
Part A
Select the two atom tab in the upper left hand corner of the simulator. Turn on (check) all
View options. Investigate how the bond behaves when the atom's electronegativity is changed.
1. What does
represent?
4. How does changing the electronegativity of the atoms affect the bond polarity?
6. What scenarios can bring about a higher electron density around a particular atom?
80
8. Explain how the direction of the arrow in the bond dipole symbol (
) relates to the
electron density, the partial charges and the electrostatic potential on a molecule.
9. What happens to a polar molecule when the electric field is turned on? Make sure to spin
the molecule several times while making observations. What if the molecule is nonpolar?
81
Part B
Select the three atoms tab in the upper left hand corner of the simulator. Turn on (check) all
view options. Investigate how the bond behaves when the electronegativity of the individual
atoms is changed. In addition to changing the electonegativities, orient the radial atoms relative
to one another by dragging them with the mouse.
1. Provide a summary as to how the bond dipoles affect the molecular dipose. Also,
describe how the geometric orientation of the bonded atoms affect the molecular dipole?
2. Provide a scenerio in which a molecule with two strong bond dipoles can have no
molecular dipole at all? Explain your answer with a drawing showing individual bond
dipoles and the overall molecular dipole.
3. Provide a scenerio in which a molecule may have a very large molecular dipole. Explain
your answer with a drawing showing individual bond dipoles and the overall molecular
dipole.
Part C
One property between molecules which is explored more in CH222 is the solubility of one
substance in another. There is an adage that describes this ability, "Like dissolves like";
molecules with similar molecular dipoles will tend to interact favorably and mix. For instance,
a polar molecule will mix well (dissolve) other polar molecules (ethanol readily dissolves in
water, both are polar molecules and possess strong molecular dipoles). Octane (a major
component of gasoline) will not dissolve in water because it does not have a molecular dipole
and is thus a nonpolar molecule.
Being able to predict the polarity of a molecule is extremely important since many properties
of molecules depend on whether they are polar or non-polar. Predicting a molecules polarity is a
82
multi-step process that starts with drawing the Lewis structure. Using VSEPR, predict the
molecules molecular geometry. Individual bond polarities are finally used to predict the
molecular polarity.
1. For the following molecules complete this step-by-step process.
Molecule
Lewis Structure
Molecular
Geometry
Polar or
nonpolar?
*
Tetrahedral
CH3F
POLAR
N2
BF3
CH2F2
C is the
central
atom
HCN
C is the
central
atom
*Make a prediction, and then check it in the Real Molecules section of the simulation.
2. Using the molecular dipoles/polarity of BF3, explain why BF3 does not mix with H2O?
CH228 LABS
Pre-Lab: Enthalpy of Neutralization of Phosphoric Acid
Part A
Answer the following questions in your lab notebook (be sure to show
work for any calculations):
1. A neutralization reaction was carried out in a calorimeter. The temperature of the
solution rose from 20.0 C to 25.6 C. Is this reaction endothermic or exothermic?
2. A neutralization reaction was carried out in a calorimeter. The change in
temperature (T) of the solution was 5.6 C and the mass of the solution was
100.0 g. Calculate the amount of heat energy gained by the solution (qsol). Use
4.18 J/(gC) as the specific heat, Cs, of the solution.
3. What is the value of qreaction for the neutralization reaction described in number 2?
4. How many moles of phosphoric acid are contained in 50.0 mL of 0.60 M H3PO4?
5. What is the value of Hreaction (in kJ/mol phosphoric acid) if 50.0 mL of 0.60 M
H3PO4 was used in the reaction described in number 2?
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to
include space for observations) and preparing any tables necessary for data
collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them
into your TA.
84
OBJECTIVES
In this experiment, you will
Measure the temperature change of the reaction between solutions of sodium
hydroxide and phosphoric acid.
Calculate the enthalpy, H, of neutralization of phosphoric acid.
Compare your calculated enthalpy of neutralization with the accepted value.
Calculate the enthalpy, H, of neutralization per ionizable hydrogen for
phosphoric acid.
INTRODUCTION
A great deal can be learned by conducting an acid-base reaction as a titration. In
addition, acid-base reactions can be observed and measured thermodynamically. In this
case, the reaction is carried out in a calorimeter. If the temperature of the reaction is
measured precisely, the enthalpy of neutralization of an acid by a base (or vice versa)
can be determined. In this experiment, you will react phosphoric acid with sodium
hydroxide.
You will use a Styrofoam cup nested in a beaker as a calorimeter, as shown in Figure 1.
For purposes of this experiment, you may assume that the heat loss to the calorimeter
and the surrounding air is negligible. Phosphoric acid will be the limiting reactant in
this experiment, and you will accordingly be determining the enthalpy, H, of
neutralization of the acid. Selecting a limiting reactant helps ensure that the temperature
measurements and subsequent calculations are as precise as possible.
Pages 246-248 and 257-258 in your text will provide background information.
Figure 1
85
Equipment Information
Each bin should contain:
1 temperature probe
2 coffee cups
Notify TA if damaged
Notes:
a. Coffee cups are reusable. Do not throw them in the trash.
Hazards
corrosive
corrosive
86
PROCEDURE
1. Obtain and wear goggles. It is best to conduct this experiment in a well-ventilated
room.
2. Connect a Temperature Probe to Channel 1 of the Vernier computer interface.
3. Start the Logger Pro program on your computer. Open the file Lab 1
Phosphoric from the Chemistry 228 folder.
4. Nest a Styrofoam cup in a 250 mL beaker as shown in Figure 1. Measure out 50.0
mL of 0.60 M H3PO4 solution into the foam cup. CAUTION: Handle the
phosphoric acid with care. It can cause painful burns if it comes in contact with the
skin.
5. Use a utility clamp to suspend the Temperature Probe from a ring stand (see
Figure 1). Lower the Temperature Probe into the phosphoric acid solution.
6. Measure out 50.0 mL of 1.85 M NaOH solution in a graduated cylinder and
transfer it to a 250 mL beaker. CAUTION: Sodium hydroxide solution is caustic.
Avoid spilling it on your skin or clothing.
7. Conduct the experiment.
a. Click
to begin the data collection and obtain the initial temperature of the
H3PO4 solution.
b. After you have recorded three or four readings at the same temperature, add the
50.0 mL of NaOH solution to the Styrofoam cup all at once. Use a glass stirring
rod to stir the reaction mixture gently and thoroughly.
c. Data will be collected for 10 minutes. You may terminate the trial early by
clicking
, if the temperature readings are no longer changing.
d. Click the Statistics button, . The minimum and maximum temperatures are
listed in the statistics box on the graph. If the minimum temperature is not a
suitable initial temperature, examine the graph and determine the initial
temperature.
e. Record the initial and maximum temperatures for Trial 1.
f. Close the Statistics box by clicking the X in the corner of the box.
8. Rinse and dry the Temperature Probe, Styrofoam cup, and stirring rod. Dispose of
the solution as directed.
9. Repeat Steps 48 to conduct a second trial. If directed, conduct a third trial. Print
a copy of the graph of the second trial to include with your data and analysis.
87
DATA TABLE
Trial 1
Trial 2
Trial 3
DATA ANALYSIS
6. Write the balanced equation for the reaction of phosphoric acid and sodium hydroxide.
7. Use the equation below to calculate the amount of heat energy gained by the solution
(qsol). In determining the mass, m, of the solution use 1.00 g/mL for the density (be sure
to use the total volume of the solution after the acid and base are mixed). The change in
temperature (T) is a directional change where T = Tf Ti. Use 4.18 J/(gC) as the
specific heat, Cs, of the solution.
qsol = Cs m T
8. The heat calculated above represents the heat gained by the solution (the solution being
predominantly water). Since we are interested in the heat of neutralization of phosphoric
acid we need the heat transfer associated with the reaction (qrxn). If the solution gained
heat, the reaction must have given off heat. This relationship can be expressed by the
following equation:
qsol = -qrxn
9. Determine the number of moles of phosphoric acid used in the reaction. Use the moles
of phosphoric acid along with qrxn to determine the enthalpy change, H, for the reaction
in terms of kJ/mol of phosphoric acid. This is your experimental value of H.
H = qrxn/moles H3PO4
10. The accepted value for the H of neutralization for phosphoric acid is -156.44 kJ/mol.
Calculate the percent error in your experimental value.
88
Describe coffee cup calorimetry and how it is used to find the enthalpy of various reactions
that occur in aqueous solutions. Make sure to include the relevant equations. Why can you
use the specific heat capacity and density of pure water to determine the enthalpy of reaction?
What assumptions must be made in order to do this?
.
Data: Insert your data table (with a caption) below that captures all of the relevant
information.
89
Results:
Report your calculated average value of H of neutralization for phosphoric acid.
Include hand written sample calculations.
Report the percent error for the H of neutralization for phosphoric acid. Include any
calculations..
Discussion: Is your value for the H of neutralization for phosphoric acid greater than or less
than the accepted value. Think of some valid sources of error to account for your
difference and explain how they would contribute to the direction of your error.
H = -1299.5 kJ
H = -393.5 kJ
H = -285.8 kJ
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to
include space for observations) and preparing any tables necessary for data
collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
91
H 1
H 2
H 3
H 4
You w ill d eterm ine the heat of reaction for reactions 1 and 2 experim entally, then use
the know n value of the enthalpy of form ation of w ater (H 3 = -285.9 kJ/ m ol) to
calculate H 4 w hich is the enthalpy of form ation of MgO . Be aw are that equation (2)
is the reverse of the reaction you actually run and m easure. (N ote: the enthalpy of
form ation of MgO cannot easily be m easured .)
92
Equipment Information
Each bin should contain:
1 temperature probe
2 coffee cups
Notify TA if damaged
Notes:
a. Coffee cups are reusable. Do not throw them in the trash.
Hazards
corrosive
none
flammable
93
Experimental Procedure
Part A
1. Obtain a coffee cup calorimeter from the stockroom. Make sure the cup is clean
and dry. Nest a Styrofoam cup in a 250 mL beaker and put 50. mL of 1.0 M HCl
into the calorimeter.
2. Using a weighing boat, weigh out a sample containing between 0.45 - 0.55 grams
of magnesium.
3. Connect a Temperature Probe to Channel 1 of the Vernier computer interface.
Start the Logger Pro program on your computer. Open the file Lab 1
Phosphoric from the Chemistry 228 folder.
4. Use a utility clamp to suspend the Temperature Probe from a ring stand (see
Figure 1). Lower the Temperature Probe into the acid solution.
5. Conduct the experiment.
a. Click
to begin the data collection and obtain the initial temperature
of the acid solution.
b. After you have recorded three or four readings at the same temperature,
add the magnesium to the styrofoam cup all at once. Use a glass stirring rod
to stir the reaction mixture gently and thoroughly.
c. Data will be collected for 10 minutes. You may terminate the trial early by
clicking
, if the temperature readings are no longer changing.
d. Click the Statistics button, . The minimum and maximum temperatures
are listed in the statistics box on the graph. If the minimum temperature is
not a suitable initial temperature, examine the graph and determine the
initial temperature.
e. Record the initial and maximum temperatures for Trial 1.
f. Close the Statistics box by clicking the X in the corner of the box.
6. Rinse and dry the Temperature Probe, Styrofoam cup, and stirring rod. Dispose
of the solution as directed.
7. Conduct another trial as above. Make sure the calorimeter is clean and mostly
dry before repeating the experiment.
94
Part B
Repeat the above procedure, this time replacing Mg with MgO. (Use a clean, dry
calorimeter.) You should use a molar equivalent of MgO (24.3 g Mg is the molar
equivalent of 40.3 g MgO, why?, your measurement should be within 5%) Be certain
all the MgO dissolves, this will require vigorous stirring!! Conduct another trial as
above.
Calculations
To relate heats of reactions (in energy units of Joules) with temperature differences we
use:
q = m x cs x T
For the reactions above, it is a good approximation to take specific heat of the solution
to be the specific heat capacity of water, cs = 4.184 J/g-C. For mass, because you are
using the specific heat of pure water, use the mass of the water only, not the combined
mass of water and solute. Calculate q for reaction 1 and 2.
Report Hrxn for reaction 1 and 2, be certain to use units of kJ/mol.
Calculate H4
95
If you have not already done so, on the lower right side of the screen, click on the
RESET button.
5. On the right side of the screen, click on the MEASURMENT TOOLS button. Next,
click on the RULER option to activate the ruler.
97
CLICK
HERE
6.
In the upper right hand corner, click on the TEMPERATURE button under the
Constant Parameter heading. This will hold temperature constant while allowing you to
observe the relationship between pressure and volume.
CLICK
HERE
7. Using the mouse and the right button, drag the ruler into a position that will allow you to
measure the length of the container.
8. Using the mouse and the right button, grab hold of the man pushing against the container
and expand the length of the container so that it measures 9.0 nm. Record this as your
initial length (the height of the box will remain 5.0 nm and the width of the box will
remain 5.0 nm)
GRAB
AND
DRAG
98
9. Using the mouse and the right button, grab hold of the pump handle and inject one cycles
worth of gas into the chamber by pulling the handle up then pushing it back down.
MOVE UP THEN DOWN
10. Once the pressure has somewhat stabilized, record your pressure value for the chamber
length of 9.0 nm. This will represent your initial pressure in atmospheres.
PRESSURE (ATM)
11. Using the mouse and right button, grab hold of the man pushing on the container and
decrease the length of the container to approximately 8.0 nm. Once the pressure has
stabilized (again, this may take a short period of time to happen), record the new pressure
for a length of 8.0 nm.
PUSH IN
99
12. Repeat step 9 for approximate lengths of 7.0 nm, 6.0 nm, 5.0 nm, 4.0 nm, 3.0 nm, and
2.0 nm (you will probably not get to exactly 2 nm). For each trial, record the length
value and resulting pressure value in a properly labeled data table.
13. Record any qualitative observations on the behavior of the gas molecules as the volume
decreases.
14. Click the RESET button to remove all the gas particles from the chamber before moving
on to the next section.
Analysis:
For this lab, you will need to submit neat labeled data tables for each procedure. You must also
submit a graphical representation for each relationship. Be sure to label each axis and include a
title for each graph (Please see the information on pages 15 and 16 of this lab manual). I suggest
that you utilize Microsoft Excel or some other comparable spreadsheet software to produce your
tables and graphs. Along with the graphs and tables for each procedure, answer completely the
questions below that correlate with each section.
Analysis: Procedure 1: Pressure Volume Relationship
1. Graphically represent the Pressure (atm) Volume (nm3) relationship with volume on the
x-axis.
2. Graphically represent the Pressure (atm) and Inverse Volume, 1/V (nm-3) relationship
with 1/V on the x axis
3. Identify the mathematical relationship that exists between pressure and volume, when
temperature and quantity are held constant, as being directly proportional or inversely
proportional. Explain your answer and write an equation that relates pressure and volume
to a constant, using variables, not the mathematical equation from the best fit line.
4. Why were you asked to graph pressure and the inverse of volume?
100
5. Calculate the slope of the line for your pressure vs. 1/volume graph. What properties does
this number represent? Would you expect it to be the same for other gases? Explain your
answer.
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
102
INTRODUCTION
Hydrogen peroxide spontaneously decomposes to form oxygen gas according to the
following equation:
2 H2O2 (aq) 2 H2O (l) + O2 (g)
This process usually occurs very slowly. Many different compounds or ions are capable of acting
as catalysts increasing the rate of the reaction. Here, potassium iodide (KI) will be used as a
catalyst to make the reaction produce products rapidly enough to study the reaction in the lab.
The apparatus we will use to collect oxygen gas in this experiment is shown in figure 1.
Hydrogen peroxide will be placed in the Erlenmyer flask. The catalyst (KI) is located in the
syringe and can be added to the Erlenmyer flask to initiate the reaction. As the reaction proceeds
oxygen gas will be produced in the Erlenmyer flask and travel through the tubing. The gas will
be collected in the graduated cylinder. The graduated cylinder is initially filled with water. As
the gas enters the cylinder it displaces water allowing the volume of the gas to be measured.
Figure 1
103
Equipment Information
Each bin should contain one 100mL graduated cylinder and:
1 temperature probe
Gas capture kit components: 1x rubber stopper, 2x plastic Luer tips, 1x syringe,
1x tubing, and 1x stopcock
Notes:
a. When cleaning up, do not put temperature probe in gas capture kit bag.
b. Parafilm is reusable.
c. Water from the water displacement bath is not waste.
Hazards
corrosive
toxic
104
PROCEEDURE
1. Place an 125 mL Erlenmyer flask on a balance and tare the scale. Add approximately 5 g
of hydrogen peroxide solution into the Erlenmyer flask. Record the actual mass used.
Obtain a ring stand and clamp the flask as shown in figure 1. Place the rubber stopper
tightly in the flask (this should be air tight).
2. Place approximately 600 mL of water in an 800 mL beaker.
3. Completely fill a 100 mL graduated cylinder with water. Cover the cylinder with parafilm
and invert the cylinder in the 800 mL beaker. Carefully clamp the cylinder in place such
that the opening of the cylinder is below the surface of the water in the beaker. Remove
the parafilm and carefully place the end of the tubing just inside the graduated cylinder as
shown in figure 1. The graduated cylinder should be completely filled with water. If there
is a small amount of air present in the cylinder record the volume. If there is more than 10
mL of air in the cylinder, you will need to redo the setup.
4. In a small beaker obtain a small amount (approximately 10 mL) of 0.5 M KI. Draw up 3
mL of the KI solution into the syringe. Add your magnetic stir bar. Attach the syringe to
the adaptor in the rubber stopper. Place on the magnetic stirrer on and turn on to a low
setting
5. Initiate the reaction by depressing the stopper on the syringe and adding the KI to the
hydrogen peroxide.
6. Allow the reaction to proceed until no further production of oxygen gas is observed
(around 10 to 15 minutes).
7. Measure and record the temperature of the water.
8. Record the final level of the water in the graduated cylinder. Be sure to record your
measurement to 2 decimal places.
9. Repeat the above procedure two more times for a total of three trials. At least two of your
trials should agree well with one another.
DATA ANALYSIS
1. Determine the pressure of the oxygen gas:
Because the oxygen gas was collected over water some of the gas collected is water
vapor. The gas collected is therefore a mixture of both oxygen and water. The total
pressure of the gas is the sum of the pressures exerted by the oxygen gas and water vapor.
To determine the pressure of oxygen gas we must apply Daltons law of partial pressure.
PTot = pO2 + pH2O
In other words, you can find the pressure of oxygen gas by subtracting the partial
pressure of water at the temperature of the water (also known as the vapor pressure of
water) from the total pressure (or atmospheric pressure). Your TA will provide the
current barometric pressure. A table of the vapor pressure of water at various
temperatures follows.
105
Vapor
Pressure
(torr)
12.8
13.6
14.5
15.5
16.5
17.5
Temperature
o
( C)
21
22
23
24
25
26
Vapor
Pressure
(torr)
18.6
19.8
21.1
22.4
23.8
25.2
Temperature
o
( C)
27
28
29
30
31
32
Vapor
Pressure
(torr)
26.7
28.3
30
31.8
33.7
35.7
106
107
3. If the heat of vaporization of water is 40.7 kJ/mol, how much energy is required to
vaporize 5.0 g of liquid water at 100 C?
4. Would you expect most of the components in a perfume to have a low or high vapor
pressure? Explain.
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
108
H vap 1
C
R T
where ln P is the natural logarithm of the vapor pressure, Hvap is the heat of vaporization, R is
the universal gas constant (8.31 J/molK), T is the temperature (in Kelvin) and C is a constant not
related to heat capacity. Thus, the Clausius-Clayperon equation not only describes how vapor
pressure is affected by temperature, but it relates these factors to the heat of vaporization of a
liquid. Hvap is the amount of energy required to cause the vaporization of one mole of liquid at
constant pressure.
In this experiment, you will introduce a specific volume of a volatile liquid into a closed vessel,
and measure the pressure in the vessel at several different temperatures. By analyzing your
measurements, you will be able to calculate the Hvap of the liquid.
OBJECTIVES
In this experiment, you will
Measure the pressure inside a sealed vessel containing a volatile liquid over a range of
temperatures.
Determine the relationship between pressure and temperature of the volatile liquid.
Calculate the heat of vaporization of the liquid.
Figure 1
109
Equipment Information
Each bin should contain:
1 temperature probe
Hazards
flammable, toxic
110
PROCEDURE
1. Obtain and wear goggles. CAUTION: The alcohol used in this experiment is flammable and
poisonous. Avoid inhaling the vapors. Avoid contact with your skin or clothing. Be sure that
there are no open flames in the room during the experiment. Notify your teacher immediately
if an accident occurs.
2. Use a hot plate to heat ~200 mL of water in a 400 mL beaker.
3. Prepare a room temperature water bath in an 800 mL beaker. The bath should be deep
enough to completely cover the gas level in the 125 mL Erlenmeyer flask.
4. Connect a Gas Pressure Sensor to Channel 1 of the Vernier computer interface. Connect a
Temperature Probe to Channel 2 of the interface.
5. Start the Logger Pro program on your computer. Open the file Lab 4 Vapor Pressure from
the Chemistry 228 folder.
6. Use the clear tubing to connect the white rubber stopper to the Gas Pressure Sensor. (About
one-half turn of the fittings will secure the tubing tightly.) Twist the white stopper snugly
into the neck of the Erlenmeyer flask to avoid losing any of the gas that will be produced as
the liquid evaporates (see Figure 1). Important: Open the valve on the white stopper.
8. Condition the Erlenmeyer flask and the sensors to the water bath.
a. Place the Temperature Probe in the room temperature water bath.
b. Place the Erlenmeyer flask in the water bath. Hold the flask down into the water bath to
the bottom of the white stopper.
c. Click
to begin data collection.
d. After 30 seconds, close the valve on the white stopper. Your first measurement will be of
the pressure of the air in the flask and the room temperature. When the pressure and
temperature readings stabilize, record these values.
e. When the readings stabilize, click
.
f. Record these values in your notebook.
9. Obtain a small amount of ethanol. Draw 3 mL of ethanol into the 20 mL syringe that is part
of the Gas Pressure Sensor accessories. Thread the syringe onto the valve on the white
stopper (see Figure 1).
10. Add ethanol to the flask.
a.
b.
c.
d.
11. Gently rotate the flask in the water bath for a 1 minute, using a motion similar to slowly
stirring a cup of coffee or tea, to accelerate the evaporation of the ethanol.
12. Monitor and collect temperature and pressure data.
13. While gently rotating the flask in the water bath, add a small amount of hot water, from the
beaker on the hot plate, to warm the water bath by 35C. Use the syringe to transfer the hot
water. Stir the water bath slowly with the Temperature Probe. Monitor the pressure and
temperature readings. When the readings stabilize, click
. Record these values in your
notebook.
111
14. Repeat Step 13 until you have completed five total trials. Add enough hot water for each trial
so that the temperature of the water bath increases by 3-5C, but do not warm the water bath
beyond 40C because the pressure increase may pop the stopper out of the flask. If you must
remove some of the water in the bath, do it carefully so as not to disturb the flask.
15. After you have recorded the fifth set of readings, open the valve to release the pressure in the
flask. Remove the flask from the water bath and take the stopper off the flask. Dispose of the
ethanol in the liquid waste receptacle and the water from the bath down the sink.
16. Click
to end the data collection. Record the pressure readings, as Ptotal, and the
temperature readings in your data table.
17. Do not exit the Logger Pro program until you have completed 14 of the Data Analysis
section.
DATA TABLE
Initial
Trial 1
Trial 2
Trial 3
Trial 4
Trial 5
Ptotal (kPa)
Pair (kPa)
Pvap (kPa)
Temperature (C)
112
DATA ANALYSIS
1. The Pair for Trials 2-5 must be calculated because the temperatures were increased. As you
warmed the flask, the air in the flask exerted pressure that you must calculate. Use the gas
law relationship shown below to complete the calculations. Remember that all gas law
calculations require Kelvin temperature. Use the Pair from before the volatile liquid was
added to the flask as P1 and the Kelvin temperature of Trial 1 as T1.
P1 P2
T1 T2
2. Calculate and record the Pvap for each trial by subtracting Pair from Ptotal.
3. Prepare and print a graph of Pvap (y-axis) vs. Celsius temperature (x-axis).
a. Disconnect your Gas Pressure Sensor and Temperature Probe from the interface.
b. Choose New from the File menu. An empty graph and table will be created in Logger Pro.
c. Double-click on the x-axis heading in the table, enter a name and unit, then enter the five
values for temperature (C) from your data table above.
d. Double-click on the y-axis heading in the table, enter a name and unit, then enter the five
values for vapor pressure from your data table above.
e. Does the plot follow the expected trend of the effect of temperature on vapor pressure?
Explain.
4. In order to determine the heat of vaporization, Hvap, you will first need to plot the natural
log of Pvap vs. the reciprocal of absolute temperature.
a.
b.
c.
d.
There is not a form al lab report for this lab. Com plete the
below pages and subm it them to your TA.
113
Provide a brief statement of the purpose of this activity. Be sure to include the meaning of
enthalpy of vaporization and why vapor pressure is temperature dependent. Additionally show
the Clausius-Clapeyron equation and describe how vapor pressure and temperature data can be
manipulated to find the enthalpy of vaporization.
114
Data:
Initial
Trial 1
Trial 2
Trial 3
Trial 4
Trial 5
Ptotal (kPa)
Pair (kPa)
Pvap (kPa)
Temperature (C)
Report your value for Hvap of ethanol. Show the calculation used to arrive at the
reported value. Include a copy of your graph of ln Pvap vs. 1/T (K).
Report the percent error in your calculated value of Hvap for ethanol.
Is your value for the Hvap greater than or less than the accepted value. Think of some
valid sources of error to account for your difference and explain how they would
contribute to the direction of your error.
115
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
116
OBJECTIVES
In this experiment, you will
Figure 1
117
Equipment Information
Each bin should contain:
1 temperature probe
1 copper stirrer
Notes:
a. Use the 100mm test tube.
b. Use the copper stirrer to stir. Do not use the temperature probe to stir.
c. Water from water bath should be poured down the drain (not into the waste
container) unless contaminated with cyclohexane.
Hazards
flammable, toxic, health and environmental hazard
toxic, environmental hazard
118
PROCEDURE
1. Obtain and wear goggles.
2. Connect the Temperature Probe to the computer interface. Prepare the computer for data
collection by opening the file 15 Freezing Pt Depression from the Chemistry with
Computers folder.
Part I Freezing Temperature of Pure cyclohexane
3. Fill your 250 mL beaker with ice. Add tap water until it is about 2/3 full. The cyclohexane
used in this experiment is flammable. Do not use Bunsen burners during this lab.
4. Weigh a CLEAN, DRY test tube. It can be propped in a plastic 250 mL beaker to facilitate
measuring; this is useful when the tube is not empty. Add 3 mL of cyclohexane to your test
tube (C6H12, density = 0.779 g/ml). Do this carefully so that you do not get any solvent on the
upper portion of the test tube. MAKE SURE IT LOOKS LIKE 3 mL, compare to a similar
test tube with 3 mL of water in it. Weigh the test tube with solvent in it and compare the
masses to determine the mass of solvent.
5. Insert the Temperature Probe into the cyclohexne. About 30 seconds are required for the
probe to warm up to the temperature of its surroundings and give correct temperature
readings. During this time, fasten the utility clamp to the ring stand so the test tube is above
the ice water bath. Then click
to begin data collection.
6. Lower the test tube into the water bath. Add a small amount of ice to your water bath to bring
the temperature down. Make sure the water level outside the test tube is higher than the
solvent level inside the test tube.
7. With a very slight stirring motion with the probe, continuously stir the solvent during the
cooling.
8. Once the solid begins to form, stop stirring. Continue with the data aquisition until data
collection has stopped (10 minute run). Allow the test tube to sit at room temperature to melt
the probe out of the solid cyclohexane. Do not attempt to pull the probe outthis might
damage it. Carefully wipe any excess cyclohexane liquid from the probe with a paper towel
or tissue and dry the sides of the test tube. reweigh the test tube and cyclohexane to
determine if there is a change in mass of the solvent.
9. To determine the freezing temperature of pure cyclohexane, you need to determine the mean
(or average) temperature in the portion of graph with nearly constant temperature. Move the
mouse pointer to the beginning of the graphs flat part. Press the mouse button and hold it
down as you drag across the flat part of the curve, selecting only the points in the plateau.
Click on the Statistics button, . The mean temperature value for the selected data is listed
in the statistics box on the graph. Record this value as the freezing temperature of
cyclohexane. Close the statistics box.
10. Store your data by choosing Store Latest Run from the Experiment menu. Hide the curve
from your first run by clicking on the vertical axis label and unchecking the appropriate box.
Click
. Repeat steps 5-10 so that you have two trials of the freezing point
cyclohexane.
Part II Freezing Temperature of a Solution of biphenyl and cyclohexane
11. Measure out approximately 0.06 grams of biphenyl into a weighing boat. Add the biphenyl to
the cyclohexane already in the 4 test tube. Try to prevent the biphenyl from sticking to the
inside wall of the test tube where it will be difficult (or impossible) to get into solution. If
you do, you will have to dump the solvent in the waste recepticle, clean and dry your
apparatus, and start all over by weighing out a new portion of cyclohexane. Determine the
mass of the biphenyl by weighing the test tube, solvent and biphenyl. It may take several
119
minutes for the biphenyl to dissolve. Dissolution can be encouraged through gentle agitation
(be careful not to splash). Repeat Steps 3-8 to determine the freezing point of this mixture.
12. When you have completed Step 8, click on the Examine button, . To determine the
freezing point of the biphenyl- cyclohexane solution, you need to
determine the temperature at which the mixture initially started to
Freezing Point
freeze. Unlike pure cyclohexane, cooling a mixture of biphenyl
and cyclohexane results in a gradual linear decrease in
temperature during the time period when freezing takes place. As
you move the mouse cursor across the graph, the temperature (y)
and time (x) data points are displayed in the examine box on the
Time
graph. Locate the initial freezing temperature of the solution, as
shown here. Record the freezing point in your data table.
13. Repeat the process with by adding another portion of biphenyl.
14. To print a graph of temperature vs. time showing all data runs:
a. Click on the vertical-axis label of the graph. To display both temperature runs, click More,
and check the Run 1 and Latest Temperature boxes. Click
.
b. Label both curves by choosing Text Annotation from the Insert menu, and typing
cyclohexane (or Biphenyl- cyclohexane mixture) in the edit box. Then drag each box
to a position on or near its respective curve.
c. Print the graph.
120
3. Now press the mouse button and drag over the next linear region of the curve (the gently
sloping section of the curve where freezing took place). Press the mouse button and hold it
down as you drag only this linear region of the curve.
4. Click
again. The graph should now have two regression lines displayed.
5. Choose Interpolate from the Analyze menu. Move the mouse pointer left to the point where
the two regression lines intersect. When the small circles on each cursor line overlap each
other at the intersection, the temperatures shown in either examine box should be equal to the
freezing temperature for the biphenyl-cyclohexane mixture.
6. Use the temperature to calculate T and your molar mass for biphenyl. Compare your results
from the two methods.
121
122
1. Write the general form of the rate law for the reaction you will be studying this week.
2. A first order reaction has a rate constant of 2.90 x 10-4 s-1. Calculate the half-life for this
reaction.
3. What is the overall order of a reaction that has the following rate law? Rate = [A]2[B]
4. For a reaction where the general form of the rate law is rate = [A]m[B]n, the following
data were collected. What is the order of the reaction with respect to A? What is the
order of the reaction with respect to B?
Initial Rate
0.01 M/s
0.01 M/s
0.09 M/s
[A]
0.025 M
0.025 M
0.075 M
[B]
0.025 M
0.050 M
0.025 M
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
123
INTRODUCTION
A basic kinetic study of a chemical reaction often involves conducting the reaction at varying
concentrations of reactants. In this way, you can determine the order of the reaction in each
species, and determine a rate law expression. Once you select a reaction to examine, you must
decide how to follow the reaction by measuring some parameter that changes regularly as time
passes, such as temperature, pH, pressure, conductance, or absorbance of light.
In this experiment you will conduct the reaction between solutions of potassium iodide and iron
(III) chloride. The reaction equation is shown below, in ionic form.
2 I (aq) + 2 Fe3+ (aq) I2 (aq) + 2 Fe2+ (aq)
As this reaction proceeds, it undergoes a color change that can be precisely measured by a
Colorimeter (see Figure 1). By carefully varying the concentrations of the reactants, you will
determine the effect each reactant has on the rate of the reaction, and consequently the order of
the reaction. From this information, you will write a rate law expression for the reaction.
Figure 1
124
Equipment Information
Each bin should contain:
2 10mL graduated
cylinders
Notes:
a. This lab is very time sensitive. To succeed in this lab:
o Ensure good technique and decrease waste by practicing the procedure using tap
water first.
o Work in a team.
o Measure the KI and the water into the same graduated cylinder. Then mix them
with the FeCl3.
Hazards
toxic
corrosive, toxic
125
PROCEDURE
1. Obtain and wear goggles.
2. Connect a Colorimeter to Channel 1 of the Vernier computer interface.
3. Start the Logger Pro program on your computer. Open the file 30b. Crystal Violet from the
Chemistry with Computers folder.
4. Set up and calibrate the Colorimeter.
a) Prepare a blank by filling an empty cuvette full with distilled water. Place the blank in
the cuvette slot of the Colorimeter and close the lid.
b) If your Colorimeter has a CAL button, set the wavelength on the Colorimeter to 470 nm,
press the CAL button, and proceed directly to Step 5. If your Colorimeter does not have a
CAL button, continue with this step to calibrate your Colorimeter.
c) Choose Calibrate CH1: Colorimeter from the Experiment menu, then click
.
d) Turn the wavelength knob on the Colorimeter to the 0% T position.
e) Type 0 in the edit box.
f) When the displayed voltage reading for Reading 1 stabilizes, click
.
g) Turn the knob of the Colorimeter to the Blue LED position (470 nm).
h) Type 100 in the edit box.
i) When the voltage reading for Reading 2 stabilizes, click
, then click
.
5. Obtain the materials you will need to conduct this experiment.
a) Two 10 mL graduated cylinders.
b) Approximately 50 mL of 0.020 M KI solution in a 100 mL beaker.
c) Approximately 50 mL of 0.020 M FeCl3 solution in a separate 100 mL beaker.
CAUTION: The FeCl3 solution in this experiment is prepared in 0.1 M HCl and should
be handled with care.
d) Approximately 60 mL of distilled water in a third 100 mL beaker.
6. During this experiment you will conduct 6 trials. This step describes the process for
conducting the trials using the Trial 1 volumes. When you repeat this process, use the correct
volume for each trial based on the table below.
Trial
FeCl3 (mL)
KI (mL)
H2O (mL)
5.0
5.0
0.0
5.0
5.0
0.0
5.0
2.5
2.5
5.0
2.5
2.5
2.5
5.0
2.5
2.5
5.0
2.5
a) Consider opening an online stopwatch to make sure that all measurements are started
reproducibly at the same time after mixing.
b) Prepare a clean cuvette.
c) If adding water, measure out the water using a graduated cylinder and add to the test tube
first.
d) Measure the FeCl3 solution using a graduated cylinder and pour it into the test tube.
126
e) Measure the KI solution using a graduated cylinder. Cover the end of the test tube with
your thumb and quickly invert to mix.
f) Within 15 seconds of mixing the two solutions, fill the cuvette full with the mixture.
Wipe the outside of the cuvette with a tissue, place it in the Colorimeter, and close the
lid and begin collecting absorbance data. The timing of this step is imperative to
receiving useful data; practice several times with water before attempting with the KI and
FeCl3 solutions.
7. Click
to begin collecting absorbance data. Data will be gathered for 2 minutes.
Observe the progress of the reaction in the beaker.
8. When the data collection is complete, carefully remove the cuvette from the Colorimeter.
Dispose of the contents of the beaker and cuvette as directed. Rinse and clean the beakers
and the cuvette for the next trial (this needs to be done as soon as the trial is over).
9. Examine the graph of the first trial. On the toolbar, select the Slope button.
Slide the
cursor to the initial time point. This tool will determine the initial slope and thus approximate
the initial rate of the reaction. Record the slope as the initial rate of the Trial 1 reaction.
NOTE, IT IS IMPORTANT THAT THE SLOPE HAVE MORE THAN ONE
SIGNIFICANT FIGURE.
10. Repeat Steps 69 to conduct Trials 26. Add the solutions to your medium sized test-tube in
this order: water followed by Fe3+, followed by I-. When you complete Step 9, use the same
technique to analyze Trials 25 that you used to analyze Trial 1.
DATA ANALYSIS
1.
2.
3.
Calculate the initial molar concentration of FeCl3 and KI for each reaction and
prepare a data table containing the concentrations of each reaction and the initial
reaction rate.
What is the order of the reaction in FeCl3 and KI?
Write the rate law expression for the reaction.
127
There is not a form al lab report for this lab. Com plete the below pages and su bm it them
to your TA before leaving lab.
Briefly state the purpose of the lab. Why can the absorbance versus time data can be used as
a rate. How does absorbance relate to concentration? How can you use rate and
concentration data to determine the order in a particular reactant and thus a rate law?
.
128
Results:
Complete the following table.
Trial
[FeCl3](M)
[KI] (M)
1
2
3
4
5
6
Incl
ude
one
gra
ph
sho
win
g
all
of
the
Compare the average rate from trials 1 and 2 to the average rate of trials 5 and 6 to
determine the order in Fe3+. Report the order in Fe3+. Show your work.
Using the units of rate as units of absorbance/s, determine a value for the rate constant.
Show your work.
129
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
130
FeSCN2+(aq)
Fe3+(aq) + SCN(aq)
iron(III) thiocyanate
thiocyanoiron(III)
When Fe3+ and SCN- are combined, a dynamic equilibrium is established between these two
ions and the FeSCN2+ ion. In order to calculate the equilibrium constant, Keq, for the reaction, it
is necessary to know the concentrations of all the ions at equilibrium. In this experiment four
separate equilibrium systems, or trials, containing different concentrations of these three ions
(Fe3+, SCN-, and FeSCN2+) will be determined experimentally. The values for these equilibrium
concentrations will be substituted into the equilibrium constant expression to see if Keq is indeed
constant despite varied initial concentrations for the reactants. The Keq, is determined by using
the Law of Mass Action.
aA + bB cC + dD
This equation gives the equilibrium constant expression of:
Keq = [C]c[D]d/[A]a[B]b
In order to determine the equilibrium concentrations for the three ions a standard solution needs
to be prepared. To prepare the standard solution, a very large concentration of Fe3+ will be added
to a small initial concentration of SCN (hereafter referred to as [SCN-]i. The initial [Fe3+] in the
standard solution is 900 times larger than [SCN-]i. According to LeChatelier's principle, which
states that when a system in dynamic equilibrium is disturbed, the system responds so as to
minimize the disturbance and return the system to a state of equilibrium. This high initial
concentration Fe3+ ions on the left side of the equation forces the reaction far to the right, using
up nearly 100% of the initial SCN ions. Using stoichiometry and the balanced equation, it is
assumed that for every mole of FeSCN2+ produced, one mole of SCN is used up. Thus since
nearly all of the SCN- ions are consumed in order to minimize the disturbance, the products
concentration, [FeSCN2+]std, at equilibrium is assumed to be equal to the [SCN]i.
Since the reaction produces the FeSCN2+ ions and this ion transmits the color red, the solutions
absorbance of blue light can be measured through the use of a colorimeter (see Figure 1).
Because the red solutions absorb blue light very well, the blue LED setting on the Colorimeter is
used. The computer-interfaced Colorimeter measures the amount of blue light absorbed by the
colored solutions (absorbance, A).
131
Figure 1
Figure 2
According to Beers Law, there is a direct relationship between a solutions concentration and its
absorbance. In this case the concentration is the FeSCN2+ ion and the absorbance is blue light
(470 nm). In other words, as the concentration of FeSCN2+ increases so will the absorbance of
blue light (see Figure 2). The concentration of FeSCN2+ for any of the equilibrium systems,
trials 1-4, can be found by comparing the absorbance of each equilibrium system, Aeq, to the
absorbance of the standard solution, Astd, according to the following equation:
[FeSCN2+]std/Astd = [FeSCN2+]eq/ Aeq
Since the concentration of [FeSCN2+]std is known and the all of the absorbances for the
equilibrium solutions and the standard are measured and recorded all that needs to be done is to
solve for the unknown.
Aeq
[FeSCN2+]eq = A
X [FeSCN2+]std
std
Knowing the [FeSCN2+]eq allows you to determine the concentrations of the other two ions at
equilibrium. For each mole of FeSCN2+ ions produced, one less mole of Fe3+ and SCN- ions will
be found in the solution (see the 1:1 ratio of coefficients in the equation on the previous page).
At equilibrium the [Fe3+] and [SCN-] can be determined according to the following equations:
[Fe3+]eq = [Fe3+]i [FeSCN2+]eq
[SCN]eq = [SCN]i [FeSCN2+]eq
Knowing the values of [Fe3+]eq, [SCN]eq, and [FeSCN2+]eq, you can now calculate the value
of Kc, the equilibrium constant.
132
OBJECTIVE
In this experiment, you will determine the equilibrium constant, Kc, for the following chemical
reaction:
FeSCN2+(aq)
Fe3+(aq) + SCN(aq)
iron(III) thiocyanate
thiocyanoiron(III)
Equipment Information
Each bin should contain:
1 temperature probe
1 10mL serological
pipet with bulb
Do not aspirate
liquid into the bulb.
Notes:
a. This lab is done on the micro scale. To help reduce waste, only procure
small amounts of the chemicals you need.
Hazards
corrosive, oxidizer
toxic
133
PROCEDURE
1. Obtain and wear goggles.
2. Label four 20 150 mm test tubes 1-4. Pour about 30 mL of 0.0020 M Fe(NO3)3 into a
clean, dry 100 mL beaker. Pipet 5.0 mL of this solution into each of the four labeled test
tubes. Use a pipet pump or bulb to pipet all solutions. CAUTION: Fe(NO3)3 solutions in this
experiment are prepared in 1.0 M HNO3 and should be handled with care. Pour about 25 mL
of the 0.0020 M KSCN into another clean, dry 100 mL beaker. Pipet 2, 3, 4 and 5 mL of this
solution into Test Tubes 1-4, respectively. Obtain about 25 mL of distilled water in a 100 mL
beaker. Then pipet 3, 2, 1 and 0 mL of distilled water into Test Tubes 1-4, respectively, to
bring the total volume of each test tube to 10 mL. Mix each solution thoroughly with a
stirring rod. Be sure to clean and dry the stirring rod after each mixing. Measure and record
the temperature of one of the above solutions to use as the temperature for the equilibrium
constant, Kc. Volumes added to each test tube are summarized below:
Test Tube
Number
Fe(NO3)3
(mL)
KSCN
(mL)
H2O
(mL)
1
2
3
4
5
5
5
5
2
3
4
5
3
2
1
0
All cuvettes should be wiped clean and dry on the outside with a tissue.
Handle cuvettes only by the top edge of the ribbed sides.
All solutions should be free of bubbles.
Always position the cuvette with its reference mark facing toward the white reference mark
at the top of the cuvette slot on the Colorimeter.
6. Calibrate the Colorimeter.
a. Open the Colorimeter lid.
b. Holding the cuvette by the upper edges, place it in the cuvette slot of the Colorimeter.
Close the lid.
c. If your Colorimeter has a CAL button, Press the < or > button on the Colorimeter to select
a wavelength of 470 nm (Blue) for this experiment. Press the CAL button until the red
LED begins to flash. Then release the CAL button. When the LED stops flashing, the
calibration is complete. Proceed directly to Step 7. If your Colorimeter does not have a
CAL button, continue with this step to calibrate your Colorimeter.
First Calibration Point
d. Choose Calibrate CH1: Colorimeter (%T) from the Experiment menu and then click
.
134
h. Turn the knob of the Colorimeter to the Blue LED position (470 nm).
i. Type 100 in the edit box.
j. When the displayed voltage reading for Reading 2 stabilizes, click
.
, then click
7. You are now ready to collect absorbance data for the four equilibrium systems and the
standard solution.
a. Click
to begin data collection.
b. Empty the water from the cuvette. Rinse it twice with ~1 mL portions of the Test Tube 1
solution.
c. Wipe the outside of the cuvette with a tissue and then place the cuvette in the Colorimeter.
After closing the lid, wait for the absorbance value displayed in the meter to stabilize.
Then click
, type 1 (the trial number) in edit box, and press the ENTER key.
d. Discard the cuvette contents as directed by your teacher. Rinse the cuvette twice with the
Test Tube 2 solution and fill the cuvette 3/4 full. Follow the Step-c procedure to find the
absorbance of this solution. Type 2 in the edit box and press ENTER.
e. Repeat the Step-d procedure to find the absorbance of the solutions in Test Tubes 3, 4,
and 5 (the standard solution).
f. From the table, record the absorbance values for each of the five trials in your data table.
g. Dispose of all solutions as directed by your instructor.
135
(0.0020
M)
[FeSCN2+]std
where Aeq and Astd are the absorbance values for the equilibrium and standard test tubes,
respectively, and [FeSCN2+]std = (1/10)(0.0020) = 0.00020 M. Calculate [FeSCN2+]eq for
each of the four trials.
5. [Fe3+]eq: Calculate the concentration of Fe3+ at equilibrium for Trials 1-4 using the equation:
[Fe3+]eq = [Fe3+]i [FeSCN2+]eq
6. [SCN]eq: Calculate the concentration of SCN- at equilibrium for Trials 1-4 using the
equation:
[SCN]eq = [SCN]i [FeSCN2+]eq
7. Calculate Kc for Trials 1-4. Be sure to show the Kc expression and the values substituted in
for each of these calculations.
8. Using your four calculated Kc values, determine an average value for Kc. How constant were
your Kc values?
136
137
Equipment Information
There are no bins this week.
Notes:
a. Cobalt is highly toxic.
b. Concentrated hydrochloric acid is very corrosive.
Hazards
corrosive, toxic, health and environmental hazard
corrosive
oxidizer, corrosive, toxic, environmental hazard
138
Hazards: HCl is very corrosive! Exercise caution around solution and vapors. Always make sure
to add acid to less concentrated solutions, rather than adding less concentrated solutions to the
acid. Sliver nitrate will stain skin and clothes, exercise caution and be sure to wash your hands
after the lab. Always clean up any spills!
Disposal: Cobalt chloride and silver nitrate as well as any excess acid must be properly disposed
in the labeled waste jars.
Procedure
1. Prepare a hot bath by half filling a beaker with water and placing it on a hot plate. Heat to
boiling on medium heat. Additionally, prepare an ice/water cold in a second beaker.
2. Obtain 10 mL of a 0.1 M cobalt chloride solution. Note the color.
3. Do this step in the fume hood. Obtain 15 mL of Concentrated HCl solution and while
gently stirring with your stir rod, slowly add 10 mL drop wise to your cobalt chloride
solution until vivid color change is observed. Here, you have just produce the [CoCl4]2(aq) complex ion. If no color change, then add additional HCl drop wise. Note the color.
4. Divide the resulting solution amongst 4 small test-tubes, filling only half-way. Do not
overfill the test-tubes (about 5 mL in each). Keep one as a control, something that you
can use to compare any color changes to.
5. To one test-tube add distilled water drop wise, while gently stirring with your stir rod,
until the color changes.
6. Keeping track of which test-tube is which, take a test-tube from step 4 and the test-tube
generated in step 5 and place them in the hot bath for 2 minutes. Note any color changes.
7. Take the test-tubes from step 6 and place in your ice bath for two minutes. Note any color
changes.
8. To a test-tube from step 4, add 0.1 M silver nitrate drop wise until a precipitate forms.
Note any color changes.
9. Be sure to dispose of all waste properly.
139
Last Name___________________
[CoCl4]2-(aq)
[Co(H2O)6] 2+(aq)
Questions:
1. What was the effect of adding excess chloride ions. Use Le Chatliers principle and
provide evidence.
140
2. Based upon the heating and cooling of the two equilibrium mixtures, propose if the
reaction is endothermic or exothermic. Use Le Chatliers principle and provide evidence
(would heat be considered as a reactant or product?).
[CoCl4]2-(aq) + 6H2O(l)
3. How did the addition of silver nitrate affect the equilibrium if neither silver ions nor
nitrate ions are in the equilibrium expression? Use Le Chatliers principle and provide
evidence. Additionally, write a net ionic equation to describe the precipitation reaction.
4. When perturbing the equilibrium with heating and cooling, how many times do you think
the equilibrium can be shifted before it stops working? Why? How about modification of
the equilibrium through changes in concentration?
There is not a formal lab report for this lab. Com plete the above pages
u sing the Microsoft version of this file that is available for d ow nload on
the lab D2L page. Once the w orksheet is com plete, su bmit the
w orksheet on tim e and to you r TA in the d ropbox on D2L .
141
CH229 LABS
Pre-lab: Acid Rain
Part A
Answer the following questions in your lab notebook (be sure to show your work
for any calculations):
1. Carbon dioxide (CO2) reacts with water to produce carbonic acid (H2CO3). Write the
balanced chemical equations for this reaction and showing what happens when carbonic
acid is dissolved in water.
2. What is the conjugate base of nitrous acid (HNO2)?
3. Which is a stronger acid, nitrous acid (HNO2) or nitric acid (HNO3)?
4. Which is a stronger base, nitrite (NO2-) or nitrate (NO3-)?
5. Describe the method you will use in this lab to generate the acids found in acid rain.
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
142
CO 2
NO 2
H 2 CO 3
H NO 2
H NO 3
H2SO3
SO2
OBJECTIVES
In this experiment, you will
143
Equipment Information
Each bin should contain:
1 pH probe
7 plastic pipets
Notes:
a. Check the pH probe for breakage.
b. Refill pH probe with storage solution if needed. Storage solution available in the
stockroom.
Hazards
corrosive
none
corrosive
oxidizer, acutely toxic, environmental hazard
144
PROCEDURE
1. Obtain and wear goggles.
2. Obtain three short-stem and three long-stem Beral pipets as shown in Figure 1.
Label the short-stem pipets with the formula of the solid they will contain:
NaHCO3, NaNO2, and NaHSO3. Label the long-stem pipets with the
formula of the gas they will contain: CO2, NO2 and SO2. You can use a
100 mL beaker to support the pipets.
3. Obtain a beaker containing solid NaHCO3. Squeeze the bulb of the pipet
labeled NaHCO3 to expel the air, and place the open end of the pipet into
the solid NaHCO3. When you release the bulb, solid NaHCO3 will be drawn
up into the pipet. Continue to draw solid into the pipet until there is enough to
fill the curved end of the bulb, as shown in Figure 1.
Figure 1
4. Repeat the Step 3 procedure to add solid NaNO2 and NaHSO3 to the other two
Beral pipets. CAUTION: Avoid inhaling dust from these solids.
8. Use a utility clamp to attach a 20 200 mm test tube to the ring stand. Add about
4 mL of distilled water to the test tube. Remove the pH Sensor from the pH
storage solution, rinse it off with distilled water, and place it into the distilled
water in the test tube.
6. Connect the pH Sensor to the computer interface. Prepare the computer for data
collection by opening the file Exp 23 acid rain from the Chemistry with
Computer folder of Logger Pro.
Figure 2
10. Squeeze all of the air from the bulb of the long-stem pipet labeled CO2. Keep the bulb
completely collapsed and insert the long stem of the pipet down into the gas-generating pipet
labeled NaHCO3, as shown in Figure 3. Be sure the tip of the long-stem pipet remains
above the liquid in the gas-generating pipet and does not collect any unreacted solid. Release
the pressure on the bulb so that it draws gas up into it. Store the gas-generating pipet in the
100 mL beaker and invert the long stem pipet to keep the CO2 in until the next step.
11. Insert the long-stem pipet labeled CO2 into the test tube, alongside the pH Sensor, so that
its tip extends into the water to the bottom of the test tube (see Figure 4).
12. To begin collecting data on the computer, click
. After 15 seconds have elapsed,
gently squeeze the bulb of the pipet so that CO2 slowly bubbles up through the solution. Use
both hands to squeeze all of the gas from the bulb. When data collection stops after
120 seconds, examine the data in the table and determine the initial pH value (before CO2
was added) and the final pH value (after CO2 was added and the pH stabilized). To confirm
these two values, click the Statistics button, , and examine the minimum and maximum
values in the pH box displayed on the graph. Record the initial and final pH values in your
lab notebook. Close the Statistics box by clicking in the upper left corner of the box.
13. Remove the pH Sensor from the test tube and rinse its tip
thoroughly with distilled water and return it to the sensor storage
solution. Discard the contents of the test tube as directed by your
TA. Rinse the test tube thoroughly with tap water. Add 4 mL of tap
water to the test tube. Place the pH Sensor in the test tube and
check to see that the input display shows a pH that is about the
same as the previous initial pH value. If not, rinse the test tube
again and refill it.
14. From the Experiment menu, choose Store Latest Run. This stores
the data so it can be used later, but it will be still be displayed
while you do your second and third trials.
15. Repeat the procedure in Steps 5-13 but this time adding HCl to the
pipet containing solid NaHSO3. Sulfur dioxide, SO2, is generated
in this pipet.
16. Repeat the procedure in Steps 5-13 finally adding HCl to the pipet
containing solid NaNO2. Nitrogen dioxide, NO2, is generated in
this pipet. Leave all three gas-generating pipets in the 100 mL
beaker until Step 18.
Figure 4
17. When you are finished, rinse the pH Sensor with distilled water and return it to the sensor
storage solution. Clean and return the seven Beral pipets to the stockroom.
18. Label all three curves by choosing Text Annotation from the Insert menu, and typing carbon
dioxide (or nitrogen dioxide, or sulfur dioxide) in the edit box.
19. and copy/paste each graph to the digital copy of the worksheet that you will submit to your
TA.
146
There is not a form al lab report for this lab. Com plete the below pages and su bm it them
to your TA before leaving lab.
Briefly describe the purpose of the lab. Say something about the effects of acid rain. Include
information as to how the acids were generated. With the technique used, describe if it is it
possible to control how much of each acid dissolved in the water before measuring the final
pH.
Data: Neatly draw a data table below that captures all of the relevant information. Make sure
to include the final pH and change in pH for all three gases.
147
2. Which gas (or gases) caused the largest drop in pH? What was the change in pH?
3. Coal from western states such as Montana and Wyoming is known to have a lower
percentage of sulfur impurities than coal found in the eastern United States. How would
burning low-sulfur coal lower the level of acidity in rainfall? Use specific information
from this lab to answer the question.
4. High temperatures in the automobile engine cause nitrogen and oxygen gases from the
air to combine to form nitrogen oxides. Can the nitrogen oxides in automobile exhaust
contribute to acid rain? Use specific information from this lab to answer the question.
5. All three gases from this lab are produced by man but one occurs naturally at relatively
high and constant concentrations. Which gas from this experiment would cause rainfall
in unpolluted air to have a pH value less than 7 (sometimes as low as 5.6)?
6. Ka (the acid ionization constant) is a measure of acid strength; the higher the value of
the Ka the stronger the acid. Use the internet or the appendix in your text to look up the
Ka values for HNO2, H2SO3, and H2CO3. Which acid is the weakest? Which is the
strongest?
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
149
OBJECTIVES
In this experiment, you will
MATERIALS
Vernier pH Sensor
pipet bulb
10 mL graduated cylinder
50 mL volumetric flasks
Figure 1
150
Equipment Information
Each bin should contain:
1 10mL graduated
cylinder
1 pH probe
1 50mL volumetric
flask
Notes:
a. Have your TA check your calculations before you start.
b. Check the pH probe for breakage.
Hazards
corrosive
corrosive
151
PROCEDURE
1. Obtain and wear safety goggles.
2. Put approximately 25 mL of distilled water into a 50 mL volumetric flask.
3. Your TA will assign each group two different concentrations of HC2H3O2 between 0.20 and
1.0 M. Calculate the volume of a 2.0 M HC2H3O2 stock solution necessary to make 50 mL of
each solution you were assigned. Using your graduated cylinder, measure the required
volume of ~2 M (write down the actual concentration) acetic acid and pour into the
volumetric flask. CAUTION: Use care when handling the acetic acid. It can cause painful
burns if it comes in contact with your skin or gets into your eyes. Fill the flask with distilled
water to the 50 mL mark. To prevent overshooting the mark, use a wash bottle filled with
distilled water or a dropper for the last few mL. Mix thoroughly.
4. Use a utility clamp to secure a pH Sensor to a ring stand as shown in Figure 1.
5. Connect the probe to the computer interface. Prepare the computer for data collection by
opening the file Exp 27 Acid Dissociation Ka from the Chemistry w/ Computer folder of
Logger Pro.
6. Calibrate the pH probe following this procedure:
Use the 2-point calibration option of the Vernier data-collection program. Rinse
the tip of the electrode in distilled water. Place the electrode into one of the
buffer solutions. When the voltage reading displayed on the computer or
calculator screen stabilizes, enter the pH value on the bottle.
For the next calibration point, rinse the electrode and place it into a second buffer
solution. When the displayed voltage stabilizes, enter the pH value on the bottle.
Rinse the electrode with distilled water. It is now ready to beplaced in the sample
to be measured.
7. Determine the pH of your solution as follows:
152
HC2H3O2(aq)
H+(aq) + C2H3O2 (aq)
153
There is not a form al lab report for this lab. Com plete the below pages and su bm it them
to your TA before leaving lab.
Briefly describe Ka. How does Ka relate to acid strength? Describe how you can use the pH
of an aqueous acid solution and its initial concentration to determine the Ka.
Data: Insert a data table below that captures all of the relevant information. Make sure to
include the concentrations of the HC2H3O2 solutions you made and the volume of
the stock solution and water used to make the solutions. Include the pH of vinegar
.
154
Results:
2. Report your calculated Ka value for the first concentration used. Include a copy of the
ICE table.
3. Report your calculated Ka value for the second concentration used. Include a copy of the
ICE table.
5. Compare the class average experimentally determined Ka with the accepted value at
25 C (1.8 x 10-5) and calculate the percent error.
155
6. Should the initial HC2H3O2 concentration have any effect on Ka? Briefly explain.
7. Calculate the percent ionization of acetic acid for each concentration you used.
8. What effect does initial HC2H3O2 concentration seem to have on the percent ionization?
9.
10. In the past, many students have listed that the accidental addition of too much acetic acid
contributed greatly to the difference between the experimental value and the accepted
value. Suppose that Student A was supposed to make a 0.18 M solution by diluting 9.0
mL of 2.0 M acetic acid to 100.0 mL. The expected pH for this solution is 2.74. The Ka of
acetic acid is 1.8 x 10-5.
a. What would be the expected pH if a Student A accidentally diluted 9.1 mL
(instead of 9.0 mL) of the acid to 100 mL?
b. If student A measured the above calculated pH, what would be the resultant Ka
of acetic acid given that they expected the acid to have an initial concentration
of 0.18M ?
157
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
158
H+(aq) + HX(aq)
(1) H2X(aq)
H+(aq) + X2 (aq)
(2) HX(aq)
Because of the successive dissociations, titration curves of diprotic acids can have two
equivalence points, as shown in Figure 1. The equations for the acid-base reactions occurring
between a diprotic acid, H2X, and sodium hydroxide base, NaOH, are
from the beginning to the first equivalence point:
NaHX + H2O
(3) H2X + NaOH
from the first to the second equivalence point:
pH
Na2X + H2O
(4) NaHX + NaOH
from the beginning of the reaction through the
second equivalence point (net reaction):
Na2X + 2 H2O
(5) H2X + 2 NaOH
The primary purpose of this experiment is to identify an unknown diprotic acid by finding its
molecular weight. A known mass of a diprotic acid is titrated with NaOH solution of known
concentration. Molecular weight (or molar mass) is found in g/mole of the diprotic acid.
Weighing the original sample of acid will tell you its mass in grams. Moles can be determined
from the volume of NaOH titrant needed to reach the first equivalence point. The volume and the
concentration of NaOH titrant are used to calculate moles of NaOH. Moles of unknown acid
equal moles of NaOH at the first equivalence point (see Equation 3). Once grams and moles of
the diprotic acid are known, molecular weight can be calculated, in g/mole. Molecular weight
determination is a common way of identifying an unknown substance in chemistry.
You may use either the first or second equivalence point to calculate molecular weight or both.
The first is somewhat easier, because moles of NaOH are equal to moles of H2X (see Equation
3). If the second equivalence point is more clearly defined on the titration curve, however,
simply divide its NaOH volume by 2 to confirm the first equivalence point; or from Equation 5,
use the ratio:
1 mole H2X / 2 mol NaOH
159
Equipment Information
Each bin should contain:
1 pH probe
Notes:
a. Check the pH probe for breakage.
b. Refill pH probe with storage solution as needed. See the stockroom if needed.
Hazards
toxic
corrosive
flammable, toxic
none
toxic
160
MATERIALS
Vernier pH Sensor
Stir plate
50 mL buret
Magnetic stir bar
PROCEDURE
1. Obtain and wear goggles.
2. Weigh out about 0.120 g of the unknown diprotic acid on a piece of
weighing paper. Record the mass to the nearest 0.001 g in the data
table in your lab notebook. Transfer the unknown acid to a 250 mL
beaker and dissolve in 100 mL of distilled water. CAUTION:
Handle the solid acid and its solution with care. Acids can harm
your eyes, skin, and respiratory tract.
4. Add 6 drops of the indicator mixture. The indicator mixture contains
a mixture of bromocresol green and phenol red.
4. Use a utility clamp to suspend a pH Sensor on a ring stand as shown
here. Position the pH Sensor in the diprotic acid solution and adjust its position toward the
outside of the beaker so it will be easier to stir the solution with a magnetic stir bar without
striking the sensor. Get the stir bar spinning rapidly but smoothly and leave it on.
5. Obtain approximately 60 mL of ~0.1 M NaOH solution in a 250 mL beaker. Obtain a 50 mL
buret and rinse the buret with a few mL of the ~0.1 M NaOH solution. Record the precise
concentration of the NaOH solution in the data table in your lab notebook. Use a utility
clamp to attach the buret to the ring stand. Fill the buret a little above the 0.00 mL level of
the buret. Drain a small amount of NaOH solution into a waste beaker so it fills the buret tip
and leaves the NaOH close to (but below) the 0.00 mL level of the buret. Be sure to record
the actual buret reading. ALL BURET READINGS NEED TO BE RECORDED TO TWO
DECIMAL PLACES. Dispose of the waste solution from this step in the waste jar as directed
by your teacher. CAUTION: Sodium hydroxide solution is caustic. Avoid spilling it on your
skin or clothing.
6. Connect the pH Sensor to the computer interface. Prepare the computer for data collection by
opening the file Exp 24a Acid Base Titration from the Chemistry w/ Computer folder of
Logger Pro.
7. Calibrate the pH probe following this procedure:
Use the 2-point calibration option of the Vernier data-collection program. Rinse
the tip of the electrode in distilled water. Place the electrode into one of the
161
8. You are now ready to begin the titration. This process goes faster if one person manipulates
and reads the buret while another person operates the computer and enters buret readings.
Pay special attention to the color of the solution and be sure to write down the pH when color
changes happen.
a. Before adding NaOH titrant, click
and monitor the pH for 5-10 seconds. Once the
pH has stabilized, click
. In the edit box, type in the initial buret reading, and press
ENTER to store the first data pair for this experiment.
b. Add enough NaOH to raise the pH by about 0.20 units. When the pH stabilizes, again
click
. In the edit box, type the current buret reading, to the nearest 0.01 mL. Press
ENTER. You have now saved the second data pair for the experiment.
c. Continue adding NaOH solution in increments that raise the pH about 0.20 units and enter
the buret reading after each addition. Proceed in this manner until the pH is 3.5.
d. When pH 3.5 is reached, change to 2-drop increments. Enter the buret reading after each
increment. Additionally, note any change in the color of the solution.
e. After pH 4.5 is reached, again add larger increments that raise the pH by about 0.20 units
and enter the buret reading after each addition. Continue in this manner until a pH of 7.5 is
reached.
f. When pH 7.5 is reached, change back to 2-drop increments. Enter the buret reading after
each increment.
g. When pH 10 is reached, again add larger increments that raise the pH by 0.20 units. Enter
the buret reading after each increment. Continue in this manner until you reach a pH of
11.
9. When you have finished collecting data, click
waste jar as directed by your TA.
10. Print a copy of the table. Then print a copy of the graph.
162
Formula
H2C2O4
H2C3H2O4
H2C4H2O4
H2C4H4O5
H2C4H4O6
Molecular weight
90
104
116
134
150
8. Determine the percent error for your molecular weight value in Step 6.
9. For the alternate equivalence point (the one you did not use in Step 1), use your graph and
data table to determine the volume of NaOH titrant used. Examine the data to find the largest
increase in pH values during the 2-drop additions of NaOH. Find the NaOH volume just
before and after this jump. Underline both of these data pairs on the printed data table and
record them in the Data and Calculations table. Note: Dividing or multiplying the other
equivalence point volume by two may help you confirm that you have selected the correct
two data pairs in this step.
10. Determine the volume of NaOH added at the alternate equivalence point, using the same
method you used in Step 3.
11. On your printed graph, clearly specify the position of the equivalence point volumes you
determined in Steps 3 and 10, using dotted reference lines like those in Figure 1. Specify the
NaOH volume of each equivalence point on the horizontal axis of the graph.
163
Extension
Using a half-titration method, it is possible to determine the acid dissociation constants, Ka1 and
Ka2, for the two dissociations of the diprotic acid in this experiment. The Ka expressions for the
first and second dissociations, from Equations 1 and 2, are:
[H+][HX-]
[H+][X2-]
Ka1 = [H X]
Ka2 =
[HX-]
2
The first half-titration point occurs when one-half
of the H+ ions in the first dissociation have
been titrated with NaOH, so that [H2X] = [HX ]. Similarly, the second half-titration point occurs
when one-half
of the H+ ions in the seconddissociation have been titrated with
NaOH, so that
2
[HX ] = [X ]. Substituting [H2X] for [HX ] in the Ka1 expression and, [HX ] for [X2 ] in the Ka2
expression, the following are obtained:
Ka1 = [H+]
Ka2 = [H+]
logKa2 = log[H+]
pK a2
pH
pK
a1
1st EP
2nd EP
Volume NaOH
Figure 2
1. Determine the precise NaOH volume for the
first half-titration point using one-half of the first equivalence point volume (determined in
Step 2 or Step 9 of Processing the Data). Then determine the precise NaOH volume of the
second half-titration point halfway between the first and second equivalence points.
2. On your graph of the titration curve, draw reference lines similar to those shown in Figure 2.
Start with the first half-titration point volume (Point 1) and the second half-titration point
volume (Point 2). Determine the pH values on the vertical axis that correspond to each of
these volumes. Estimate these two pH values to the nearest 0.1 pH unit. These values are the
pKa1 and pKa2 values, respectively. (Note: See if there are volume values in your data table
similar to either of the half-titration volumes in Step 1. If so, use their pH values to confirm
your estimates of pKa1 and pKa2 from the graph.)
3. From the pKa1 and pKa2 values you obtained in the previous step, calculate the Ka1 and Ka2
values for the two dissociations of the diprotic acid.
164
165
Pre-lab: Buffers
Part A
Answer the following questions in your lab notebook (be sure to show work for
any calculations):
1. Buffer A: Calculate the mass of solid sodium acetate required to mix with 50.0 mL of
0.1 M acetic acid to prepare a pH 4 buffer. The Ka of acetic acid is 1.8 105
2. Buffer B: Calculate the mass of solid sodium acetate required to mix with 50.0 mL of
1.0 M acetic acid to prepare a pH 4 buffer. The Ka of acetic acid is 1.8 105
3. Write a reaction to show how a sodium acetate/acetic acid buffer would respond to a
small amount of added strong acid.
4. Write a reaction to show how a sodium acetate/acetic acid buffer would respond to a
small amount of added strong base.
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
167
Lab: Buffers
A buffer is a mixture of a weak acid and its conjugate base, or a weak base and its conjugate
acid. A buffers function is to absorb small amounts of acids (H+ or H3O+ ions) or bases (OH
ions) so that the pH of the system changes by a smaller amount than it would with most other
solutions.
In many systems, buffers are critical. Blood plasma, a natural example in humans, is a
bicarbonate buffer that keeps the pH of blood between 7.2 and 7.6.
By design, a buffer is an equilibrium system. For example, a buffer can be prepared with nitrous
acid, HNO2. The weak acid establishes an aqueous equilibrium as shown below.
HNO2 (aq) H+ (aq) + NO2 (aq)
The equilibrium constant expression is shown below.
[H ][ NO -2 ]
Ka
[HNO2 ]
To prepare a buffer system with nitrous acid, a comparable amount of the conjugate base is
added, such as sodium nitrite (NaNO2). The resulting system is a mixture of HNO2 and NO2
ions. The nitrous acid molecule will neutralize hydroxide ions and the nitrite ion (the conjugate)
will neutralize hydronium ions; and in each case the product will be one of the original
conjugates, resulting in a solution that is similar to the original one.
A variation of the equilibrium expression above, called the Henderson-Hasselbalch equation, is a
useful reference in preparing a buffer solution. For our nitrous acid/sodium nitrate buffer
example, the Henderson-Hasselbalch equation is shown below.
pH pK a log
[ NO 2 ]
[HNO2 ]
The pH range in which a buffer solution is effective is generally considered to be 1 of the pKa
corresponding to ten-fold excesses of either the acid over the conjugate base, or vice versa.
In this experiment, you will use the Henderson-Hasselbalch equation to determine the amount of
acetic acid and sodium acetate needed to prepare two acidic buffer solutions. You will then
prepare the buffers and test their buffer capacities by adding solutions of NaOH and HCl while
monitoring the pH.
OBJECTIVES
In this experiment, you will
168
Equipment Information
Each bin should contain:
1 pH probe
Notes:
a. Parafilm is reusable.
b. Check the pH probe for breakage.
Hazards
corrosive
corrosive
corrosive
none
169
MATERIALS
Vernier pH Sensor
two 50 mL burets
PROCEDURE
Part I Prepare and Test Buffer Solution A
Figure 1
6. Start the Logger Pro program on your computer. Open the file 19 Buffers from the
Advanced Chemistry with Vernier folder.
7. Calibrate the pH probe following this procedure:
Use the 2-point calibration option of the Vernier data-collection program. Rinse
the tip of the electrode in distilled water. Place the electrode into one of the
buffer solutions. When the voltage reading displayed on the computer or
calculator screen stabilizes, enter the pH value on the bottle.
For the next calibration point, rinse the electrode and place it into a second buffer
solution. When the displayed voltage stabilizes, enter the pH value on the bottle.
Rinse the electrode with distilled water. It is now ready to beplaced in the sample
to be measured.
9. You are now ready to test Buffer A. Once you verify the initial pH of the buffer, you will
slowly and carefully add 0.5 M NaOH solution to the buffer solution.
a. Take an initial pH reading of the buffer solution. Click
and monitor pH for
510 seconds. Once the displayed pH reading has stabilized, click
. In the edit box,
type the starting volume on the buret. Press the ENTER key to store the first data pair.
Record the initial pH value. NOTE: if the initial pH is not within 0.3 pH units of 4.0 you
should remake the buffer and begin again.
b. Add a small amount of the NaOH solution, up to 0.30 mL. When the pH stabilizes click
. Enter the current buret reading and press ENTER to store the second data pair.
170
c. Continue adding the NaOH solution in small increments that raise the pH consistently and
enter the buret reading after each increment. Your goal is to raise the pH of the buffer by
precisely 2 pH units.
d. When the pH of the buffer solution is precisely 2 units greater than the initial reading,
continue to add the NaOH solution in small increments until you have reached, and
passed, the equivalence point of the titration. (The pH will begin to rise rapidly at the
equivalence point.) Reaching the equivalence point is important for ensuring consistency
in your data.
e. Click
. Print a copy of the first trial.
10. Dispose of the reaction mixture in the waste jar as directed. Rinse the pH sensor with
distilled water in preparation for the second titration.
11. Repeat Steps 7 and 8, using a fresh 10.0 mL sample of the Buffer A solution. For the second
trial, repeat using the sodium hydroxide. For the third trial, titrate the buffer with 0.5 M HCl
solution. Carefully add HCl in small increments until the pH of the solution has been lowered
by precisely 2 units or no significant change continues to occur. Record the volume of HCl
that was used. There is no need to print a copy of the graph, but either print the data table or
copy the data into your lab notebook.
Part II Prepare and Test Buffer Solution B
12. Use your calculations from the Pre-Lab Exercise to prepare 50 mL of Buffer B. Weigh out
the precise mass of sodium acetate and dissolve it in 50.0 mL of 1.0 M acetic acid solution. If
necessary, refill the burets of NaOH and HCl solution.
13. Use a graduated cylinder to measure out 10.0 mL of the Buffer B solution. Repeat the
necessary steps to test Buffer B in a manner similar to the Part I trials. Print a copy of your
graph of the titration using the NaOH solution. Record the volume of HCl that was used to
lower the pH of Buffer B by 2 units or until no significant change continues to occur.
171
Part B
Prepare your notebook for the lab. This includes stating the purpose of the experiment,
summarizing the procedure in a bulleted-list format (be sure to include space for observations)
and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
173
INTRODUCTION
Calcium hydroxide is a strong base that is sparingly soluble in water. In solution it completely
dissociates into ions as represented by the following balanced chemical equation:
(aq)
The solubility product expression describes, in mathematical terms, the equilibrium that is
established between the solid substance and its dissolved ions in an aqueous system. The
equilibrium expression for calcium hydroxide is shown below.
Ksp = [Ca2+][OH-]2 (Equation 1)
The constant that quantifies a substances solubility in water is called the solubility product Ksp.
All compounds, even highly soluble ones like sodium chloride, have a Ksp. However, the Ksp of a
compound is usually only considered in cases where the compound is slightly soluble and thus
the concentration of solvated ions is small.
The primary objective in this experiment is to test a saturated solution of calcium hydroxide and
use your observations and measurements to calculate the Ksp of the compound. You will do this
by three methods: The first will be to determine the concentration of Ca(OH)2 by titrating with a
standardized hydrochloric acid solution. By determining the molar concentration of dissolved
hydroxide ions in the saturated Ca(OH)2 solution and assuming they all come from calcium
hydroxide, you will have the necessary information to calculate the Ksp. The second method will
be to measure the pH of the saturated solution and calculate the concentration of the OH-(aq) ions
and use that information to determine the Ksp. The third method will use gravimetric analysis to
determine the quantity of Ca(OH)2 dissolved in a known volume of solution. The mass of
dissolved solid can be used to determine the solubility and thus the Ksp of Ca(OH)2.
OBJECTIVES
In this experiment, you will use three separate methods to determine the Ksp of calcium
hydroxide and will compare the ease of use and reliability of the three
174
Equipment Information
Each bin should contain:
1 pH probe
Notes:
a.
b.
c.
d.
e.
Hazards
corrosive
corrosive
environmental hazard
flammable, toxic
175
PROCEDURE
CAUTION: Calcium hydroxide solution is caustic. Avoid spilling it on your skin or
clothing.
1. Obtain and wear goggles.
2. Obtain about 50 mL of a saturated calcium hydroxide solution.
3. Set up a ring stand, ring, filter funnel, and filter paper as demonstrated by your instructor.
Filter your sample of Ca(OH)2 and transfer to a clean beaker. When you are done with
the filtering apparatus, be sure to clean the flask out with ~5 mL of acid. The acid rinse
should be deposited in the waste receptacle. Follow the acid rinse up with a thorough rise
with distilled water.
Method 1 - Gravimetric Determination (begin one lab period in advance)
1. Using a 25 mL graduated cylinder transfer exactly 20 mL of the filtered solution into a
pre-weighed and labeled 250 mL beaker. The beaker must be labeled with your section
number and your drawer number.
2. Place the beaker in the warming oven until the end of the lab period.
3. After the drying period, determine the mass of the beaker plus dry calcium hydroxide and
by difference, the mass of the calcium hydroxide.
Method 2 - Determination by pH
1. Connect a pH Sensor to Channel 1 of the Vernier computer interface. Connect the
interface to the computer using the proper interface cable.
2. Start the Logger Pro program on your computer and allow the default program to open.
3. Calibrate the pH probe following this procedure:
Use the 2-point calibration option of the Vernier data-collection program.
Rinse the tip of the electrode in distilled water. Place the electrode into
one of the buffer solutions (e.g., pH 7). When the voltage reading
displayed on the computer or calculator screen stabilizes, enter a pH value,
7.
For the next calibration point, rinse the electrode and place it into a second
buffer solution (e.g., pH 10). When the displayed voltage stabilizes, enter
a pH value, 10.
Rinse the electrode with distilled water. It is now ready to be placed in the
sample to be measured.
4. Using the remaining 30 mL of the filtered solution in a 100 mL beaker and measure and
record the pH of the filtered solution in your lab notebook. Retain this solution.
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177
178
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
180
K+(aq) + NO3-(aq)
As the concentration of dissolved K+ and NO3- increases, the rate at which the ions will
recombine into solid potassium nitrate, KNO3, also increases. At one set of ion concentrations
the rate of dissolution will equal the rate of precipitation. At this point the reaction is said to be at
equilibrium. The solution is now considered saturated. An equilibrium expression, Ksp, for this
process is shown in equation (1).
Ksp = [K+][NO3-] (Equation 1)
The value for Ksp is characteristic of each compound and changes with the temperature.
Thermodynamics may be used to understand the energy changes that occur when a salt
dissolves in water. The energy difference between the solid salt and its dissolved ions is known
as the enthalpy change (H), and the relative disorder of the dissolved ions is an indication of the
entropy change (S). A positive enthalpy change will occur if heat must be added to dissolve the
salt in water. The enthalpy change will be negative if the dissolution process releases heat. The
entropy change for a solid salt dissolving in water will always be positive because the dissolved
ions possess more disorder than a solid crystalline salt.
The free energy change (G) for a process will indicate if the process is spontaneous as
written (reactants going to products). A negative value indicates that the process is spontaneous
while a positive value denotes a nonspontaneous process. The Gibbs-Helmholtz equation, shown
in Equation 2, is a mathematical expression that relates changes in free energy, enthalpy, and
entropy.
G = H - TS (Equation 2)
G can also be expressed in terms of Ksp , (equation 3).
G = -RTlnKsp (Equation 3)
By combining Equations 2 and 3, it is possible to derive an equation that relates Ksp and the
Kelvin temperature to the values associated with H and S (equation 4).
H 1 S
lnK sp
(equation 4)
R T R
181
By plotting lnKsp versus 1/T, we get a line where the slope of the line is H/R and the yintercept is S/R (R is the ideal gas constant 8.314 Jmol-1K-1). The enthalpy and entropy of
dissolution can be determined by evaluating the temperature dependence of Ksp.
OBJECTIVES
In this experiment, you will
Equipment Information
Each bin should contain:
1 10mL graduated
cylinder
1 temperature probe
1 copper stirrer
Notes:
a. Hot water bath is not waste. It should be poured down the drain unless
contaminated.
Hazards
oxidizer
182
PROCEDURE
1. Obtain and wear goggles.
2. Connect a Temperature Probe to Channel 1 of the Vernier computer interface.
3. Start the Logger Pro program on your computer. Allow Logger Pro to open the default
program. It should list columns for collecting time and temperature.
4. Prepare a hot water bath by heating a halffilled 400 mL beaker on a hot plate
5. Mass ~2 grams of potassium nitrate and record the actual mass in your lab book.
6. Transfer the salt into your 10 mL graduated cylinder.
7. Add distilled water to 2 mL in your graduated cylinder and observe if the dissolution of
KNO3 is an exothermic or endothermic process (feel the outside of the cylinder).
8. In your hot water bath, while stirring gently with the temperature probe, heat the cylinder
containing the salt and water mixture. Do not leave it in the water any longer than necessary
to get the salt into solution.
9. Remove your sample from the hot water bath and record the total volume of the solution
(only do this after all the salt has gone into solution and do not forget to remove the
temperature probe from the solution when measuring the volume).
10. While monitoring the temperature, allow the sample to cool while slowly stirring. Record the
temperature at the point when the first crystals appear. The solution will appear to be
snowing. The solution is considered to be at equilibrium when the first crystals begin to
appear. At higher concentrations the process happens quite quickly.
11. Remove the probe and add 0.5 mL of distilled water. Be careful not to lose solid as you
remove the thermometer probe from the cylinder to add the water.
12. Repeat steps 8 - 11 four more times until a total of 5 sets of data at different concentrations
have been recorded.
13. Disposal: Place the KNO3 solution into the waste jar labeled KNO3 Waste. For easier
removal of the KNO3 reheat the solution until the entire solid has re-dissolved and quickly
pour it into the waste jar. In this case, the water can be evaporated and the potassium nitrate
reused.
183
184
185
3. Use the equations given below in the introduction of this experiment to determine the
mole ratio of thiosulfate (S2O32-) to hypochlorite (ClO-).
4. 5.00 mL of commercial bleach was diluted to 100.0 mL. 25.0 mL of the diluted sample
was titrated with 4.56 mL of 0.100 M S2O32-. What is the concentration of hypochlorite in
the original bleach solution? Assume the density of the commercial bleach is 1.08 g/mL.
Calculate the average percent by mass of NaClO in the commercial bleach.
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
186
Equipment Information
There are no bins this week.
Hazards
corrosive, environmental hazard
toxic
none
none
corrosive
PROCEDURE
1. Obtain about 100 mL of diluted commercial bleach. Note that this bleach solution has been
made by diluting 3.5 mL of commercial bleach into 100 mL, meaning that the sample you
are working with is 20 times more dilute than the commercial strength. You will need to
scale back up for the final answer to this experiment.
2. Weigh out approximately 1 g solid KI. This is a large excess over what is needed.
3. Pipet 25.00 mL of the dilute bleach into an Erlenmeyer flask. Add the solid KI and about
25 mL distilled water. Swirl to dissolve the KI.
4. Working in a fume hood, slowly and with swirling, add approximately 2 mL of 3 M
HCl. The solution should be dark yellow to red-brown from the presence of the I3- complex
ions.
5. Obtain 70 mL of the sodium thiosulfate solution and use a few mL to rinse your buret, then
fill it as usual. Record the concentration of the thiosulfate in your lab notebook. Bring the
red-brown triiodide solution back to your bench and titrate the iodine with the standard
0.10 M sodium thiosulfate solution until the iodine color becomes light yellow. Add one
dropper-full of starch solution. The blue color of the starch-iodine complex should appear.
Continue to titrate until one drop of Na2S2O3 solution causes the blue color to disappear.
6. Repeat the titration, beginning with step 2, two more times.
188
189
190
Part B
Prepare your notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted-list format (be sure to include
space for observations) and preparing any tables necessary for data collection.
At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.
191
Synthesis of Acetaminophen
Acetaminophen (N-(4-hydroxyphenyl)ethanamide) is a relatively simple organic compound that
is a common over-the-counter pain reliever and fever reducer (Figure 1). Acetaminophen is
generally considered a safe medication in the U.S. although overdoses are relatively common
and can cause fatal liver damage. Organic compounds such as Acetaminophen are generally
classified by their functional groups. Acetaminophen consists of a benzene ring core that has a
hydroxyl functional group (-OH) attached to one side and an amide functional group (Figure 2)
on the opposite side (referred to as the para position see Figure 1).
each line represents a carbon atom potentially bound with various numbers of
hydrogen to give each carbon a total of four bonds.
192
Rf
The relative movement of the components is called the retention factor, symbolized Rf. The
distance traveled by one compound is measured from its point of origin to the center of the spot.
The distance traveled by the solvent is measured from the point of origin to the highest point that
mobile phase traveled. Rf values may change from day to day due to temperature differences,
changes in humidity, or variations in the paper or solvent. Their relative values should remain
constant. You will be comparing your final acetaminophen produce with the raw unpurified
sample and a given sample of pure unreacted p-aminophenol.
Safety Precautions:
193
Equipment Information
Each bin should contain:
1 well plate
Notes:
a. Do not put standards in the well plate. The solvent used will degrade the
plastic.
b. Phosphoric acid is very corrosive.
Hazards
toxic, health and environmental hazard
flammable, toxic
corrosive
flammable, toxic
flammable, toxic, health and environmental hazard
flammable, corrosive, toxic
toxic, health and environmental hazard
194
Procedures:
Synthesis of Acetaminophen
1. Weigh out 2.5 g of p-aminophenol. Place it in a 125-mL Erlenmeyer flask.
2. Add 25 mL of water and 25 drops of 85% H3PO4.
3. Gently heat to dissolve.
4. Move to the hood once all of the solid has dissolved. Working in the hood, while swirling
the flask add 2 mL of the acetic anhydride. Allow this to react for 5 minutes.
5. Place the mixture on ice and allow the solid to crystalize for 20 minutes. If crystallization
does not occur, it may be necessary to scratch the side of the flask with a stir rod or add a
small seed crystal of pure acetaminophen (ask your TA).
6. Collect the crystals by vacuum filtration using a Buchner funnel.
7. Wash the crystals twice on the filter with 5 mL portions of ice cold water.
Recrystallization of the Acetaminophen
1. Place the crude acetaminophen crystals in a clean 150 mL beaker. Add 20 mL of distilled
water and heat on a hot plate until all of the solid has dissolved. If the solution starts to
boil and undissolved solid still remains, add more water, a few mL at a time until the
solid dissolves.
2. Remove the beaker from the heat and allow the solution to cool. When crystals begin to
appear, put the solution on ice, cooling for 20 minutes. If crystallization does not occur, it
may be necessary to scratch the side of the flask with a stir rod.
3. Collect the crystals on a pre-weighed piece of filter paper using the Buchner funnel.
Wash the product on the filter paper with two 5 mL portions of ice cold water. Allow the
purified product to dry for 10 minutes under vacuum.
4. Weigh the product. It may be necessary to dry for a few more minutes, if it still appears
wet. Record the final dry weight in your lab notebook for the calculation of % yield.
TLC of the Acetaminophen Sample
1. In separate clean test tubes, dissolve a small spatula full (less than the the size of a
small pea) of p-aminophenol, your crude product and your purified product in 1 mL of
ethanol.
2. Using a pencil, carefully draw a line roughly 2 cm from the bottom of the
chromatography plate. Make marks along this line at approximately 1 cm intervals. You
should have three marks (one for p-aminophenol, one for the raw sample and one for the
purified).
3. Label the spots on the bottom line to indicate the identity of each sample
4. Utilize a clean toothpick to transfer your dissolved samples on to the TLC plate. This is
done by dipping the toothpick in your sample and quickly tapping the toothpick to the
corresponding spot on the TLC sheet. Allow the solvent to dry and repeat the transfer
procedure 15 times.
5. Place about 1 cm of aqueous ethyl acetate mobile phase in a 250 ml beaker. The solution
must not go above the 2 cm mark on the TLC plate or touch the spots when the paper is
placed in the beaker.
195
6. Carefully prop the chromatography paper in the beaker. The solvent will wick up the
plate.
7. When the mobile phase comes to within 1 cm of the top of the TLC plate, remove the
TLC plate from the beaker.
Immediately mark the position
solvent front with the pencil.
8. Allow the TLC plate to dry in the
hood.
9. Illuminate the TLC plate with the
handheld UV lamp and circle the
spots as shown in the diagram on
the right.
196
Mass of p-aminophenol
_________________ g
_________________ g
_________________ %
Roughly sketch what the TLC plate looks like when illuminated with UV light.
Solvent front
Origin
197
According to your TLC, is there a difference between your raw and purified sample? Explain.
During the crystallization of acetaminophen, what was the purpose of cooling the sample in an
ice bath?
Why should you use a minimum amount of hot solvent to dissolve the raw product during the
recrystallization step?
There is not a formal lab report for this lab. Com plete the above pages
u sing the Microsoft version of this file that is available for d ow nload on the
lab D2L page. Once the w orksheet is com plete, subm it the w orksheet on
tim e and to you r TA in the d ropbox on D2L.
198
Introduction
Please read the introduction page. Once finished, click on the link in the bottom right
of the page to progress to the next page.
Yes / No
___
3. Write the balanced redox reaction for the combination of AgNO3(aq) and Sn(s)
Once the 3x3 square is complete, click on the link in the bottom right of the page to
progress to the next page.
199
Once finished, click on the link in the bottom right of the page to progress to the next
page.
Yes / No
Yes / No
Why?
Why?
Once finished, click on the link in the bottom right of the page to progress to the next
page.
200
Finish this page off by reading the description of Carrou cells. Once finished, click on the
link in the bottom right of the page to progress to the next page.
||
1. Is the reduction or oxidation half cell written on the left side of the cell diagram?
2. What is the color of the wire that leads to the oxidation half cell (this is the anode) in
the above diagram?
3. What color of wire leads to the reduction half cell (this is the cathode) in the above
diagram?
201
Now, construct your own Carrou cell for the following cell Zn|Zn2+||Ag+|Ag. Please
remember that in order for the Carrou cell to function, a piece of paper must connect the
cells to each other through the well containing KNO3
4. What is the voltage of the Zn|Zn2+||Ag+|Ag voltaic Carrou cell (remember, when
correctly set up to be a galvanic cell, the voltage will be positive)?
5. What is the half reaction that is occurring at the cathode in the above cell?
6. Is this
Once finished, click on the link in the bottom right of the page to progress to the
next page.
Ag |Ag+
Cu |Cu2+ Sn | Sn2+
Ag+ | Ag
Cu2+| Cu
Sn2+| Sn
Once finished, click on the link in the bottom right of the page to progress to the
next page.
2. What cell did you use for comparison (write the balanced half reaction)? What was
the voltage listed on the volt meter?
3. What value did you obtain for the half-cell reduction potential of metal X?
4. Referencing the linked table of standard reduction potentials, try to identify the
unknown metal.
203
answer)
2. The concentration of Cu2+ will
answer)
b. Reaction 2:
2. Add water to dilute by dragging the beaker of water from the bottom right of the
screen over the cell that you want to dilute. The half cell should now show the word
Diluted in it. What is the new voltage?
a. Reaction 1:
b. Reaction 2:
204
3.
In one reaction the voltage increases, in the other it decreases. Briefly speculate
why.
4.
Using the Nernst equation, determine the diluted concentration for both cells. Show
your work.
Sn| Sn2+(diluted)||Cu2+|Cu
Once finished, put your name and your TAs name on a hardcopy of this document. You
must submit your Voltaic Cells results to your TA by your normally scheduled lab period
on Week 10.
205