CHE 2A Student Lab Manual SS2023
CHE 2A Student Lab Manual SS2023
Lab Manual
Standard Operating Procedures
Summer Session 2023
Department of Chemistry
University of California - Davis
Davis, CA 95616
Student Name Locker #
Laboratory Information
Teaching Assistant’s Name
Laboratory Section Number
Laboratory Room Number
Dispensary Room Number 1060 Sciences Lab Building
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ii
Acknowledgments
This manual is the culmination of the efforts of many individuals.
Many faculty members have provided ideas for the creation of these laboratories and have made
numerous suggestions regarding their implementation. Stockroom Dispensary Supervisors, both
past and present, have had a role in helping to develop these experiments and, in particular, helping
to ensure that the experiments are tailored to our laboratories here at UC Davis. Safety TAs, both
past and present, have edited this manual to ensure that the experimental procedures are clear and
current. In addition, many undergraduates have been involved in the development of experiments
as part of undergraduate research projects.
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Table of Contents
Preface i
Acknowledgments iii
Introduction vii
Experiments
Introductory Laboratory Techniques 3
Observing Chemical Reactions 11
Chemical Equilibrium 19
Strong Acid-Strong Base Titration 31
Acid Dissociation Constants and the Titration of a Weak Acid 49
Polyprotic Systems 63
Acid-Base Buffers 75
Solubility Products 89
Appendix
General Experimental Guidelines A-5
Laboratory Work Grading Policies A-7
Late Reports & Make-Up Policy A-8
Chemistry Department Safety Policy A-9
Safety in the Chemistry 2 Laboratories A-11
Maps and Emergency Evacuation Procedures A-15
General Emergency Procedures A-19
Dispensary Procedures A-20
Safety Data Sheet A-21
Hazardous Chemicals A-30
Statistical Treatment of Data A-33
An Introduction to Excel A-37
Common Laboratory Procedures A-49
Locker Inventory A-75
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Table of Contents
vi
Introduction
Time Allocation and Grading
Below is an indication of the time allocation of each experiment. At the end of the quarter, the
student’s TA will sum the scores and give this to the instructor, who will modify it as described in
the course syllabus.
On-Line Pre-laboratory Quizzes: Each 2 point pre-lab quiz must be completed at least 1 hour
prior to attending the student’s scheduled lab class. All three quiz questions must be answered
correctly before the student will be allowed to perform the laboratory experiment. If the quiz
is failed on the first attempt, the student has four more attempts to pass the quiz. Because the
questions are chosen randomly, different questions may be generated on each attempt. Students
who fail these quizzes are considered unprepared and unsafe to work in the laboratory and will not
be allowed to begin the laboratory procedure until the TA is convinced the student is prepared.
The TA will check the pre-laboratory write-up and quiz the student. The TA will allow entry into
the laboratory only if the student answers the questions correctly and the pre-laboratory write-up
is complete. This policy will be strictly enforced.
vii
Introduction
Safety Policy
It is critical that you prepare for each experiment by reading it carefully before entering the
laboratory. Not only will this ensure that you get the maximum benefit of the experience, but it
also makes for a safer environment in the laboratory. This is important not only for your own safety
but also for those around you. A number of policies have been developed in order to make sure that
the laboratory is safe and that it runs smoothly.
In each experiment specific hazards are indicated by bold type and procedures are described that
must be adhered to. Accidents commonly occur when the following rules, as approved by the
Chemistry Department Safety Committee, are not followed.
U.C. Davis Department of Chemistry Chem. 2 Series
Standard Operating Procedures
SAFETY RULES FOR TEACHING LABORATORIES
The following rules are designed for your safety in the laboratory. The Laboratory Instructor (LI =
TA, Laboratory Supervisor, and/or Course Instructor) is required to enforce these rules and has the
full backing of the Department of Chemistry Staff and Faculty. The LI is also required to enforce
all laboratory experiment-specific safety procedures in carrying out the laboratory work. Violations
of these rules will result in expulsion from the laboratory.
1. No one is allowed in the laboratory without the supervision of a LI. No laboratory work
will be done without supervision. Perform only authorized experiments, and only in the
manner instructed. DO NOT alter experimental procedures, except as instructed.
2. Specific permission from your LI is required before you may work in any laboratory
section other than the one to which you have been assigned. Only laboratory rooms where
the same laboratory course is operating may be used for this purpose.
3. If you have a special health condition (asthma, pregnancy, etc.) or any personal health
concerns, consult your medical professional before taking chemistry lab.
4. If you come to the laboratory with non-compliant goggles, shoes, or clothing, you will
not be allowed to work in the laboratory. In that context, note there are no make-up
laboratories. Your course grade will be significantly lowered or you may fail the course if you
do not meet the lab attire requirements.
6. Approved safety goggles must be worn by all persons at all times. At no time are safety
glasses of any kind acceptable in the laboratory. Safety goggles may not be modified in any
manner.
viii
Introduction
7. Clothing that completely covers the legs—including the skin between the top of the shoe
and the bottom of the pant leg—must be worn at all times in the laboratory (tights or
leggings are NOT suitable leg covering). Inadequate protection often leads to injury. Avoid
wearing expensive clothing to lab as it may get damaged.
8. Closed-toe, closed-heel shoes that completely cover the entire foot must be worn at all times.
10. Horseplay and carelessness are not permitted and are cause for expulsion from the
laboratory. You are responsible for everyone’s safety.
11. Absolutely NO food or drinks are to be stored or consumed in the laboratory. Contact
lenses and cosmetics (hand lotion, lip balm, etc.) are not to be applied and medications are not
to be consumed while in the laboratory.
12. Skateboards, rollerblades, and other such personal equipment must be stored outside of the
laboratory. Personal electronics are only permitted when needed for the laboratory. Because
cell phones or other personal electronic media can easily be damaged or contaminated in the
laboratory, use of such devices is at the student’s own risk.
13. Learn the location and how to operate the nearest eyewash fountain, safety shower,
fire extinguisher, and fire alarm box. Basic first aid for any chemical splash is to wash the
affected area for at least 15 minutes and seek medical attention. Use the emergency shower if
appropriate, removing contaminated clothing for thorough washing. If the safety shower or
eyewash is activated, the exposed person should be accompanied to the Student Health Center
for further evaluation.
14. Laboratory doors must remain closed except when individuals are actively entering or
exiting the lab.
15. The student must have at least one ungloved hand when outside the laboratory. Gloves
are presumed to be contaminated and must not come into contact with anything outside the
laboratory except chemical containers. Only use the ungloved hand to open doors, hold on to
stair rails, or push elevator buttons.
16. All activities in which toxic gases or vapors are used or produced must be carried out in
the fume hood.
18. Containers of chemicals may not be taken out of the laboratory except to the dispensary
for refill/replacement or to exchange full waste jugs for empty ones. All containers must
be closed with the appropriate cap before you take them into the hallway to the dispensary.
Always use a bottle carrier when transporting chemicals and waste.
19. Put all hazardous waste into the appropriate waste container(s) provided in your laboratory.
Do not overfill waste containers.
ix
Introduction
20. All incidents, near misses, injuries, explosions, or fires must be reported at once to the LI.
In case of serious injury or fire (even if the fire is out), the LI or Lab Supervisor must call 911.
The student must always be accompanied to the Student Health Center.
21. Keep your working area clean – immediately clean up ALL spills or broken glassware.
Dispose sharps in the appropriate container. Do not dispose pipette tips in regular trash.
Clean off your lab workbench before leaving the laboratory.
You must sign the Safety Acknowledgement sheet before you may work in the lab. If you have
questions about these rules and procedures, please ask your LI before starting any laboratory
work in this course.
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Experiments
2
Introductory Laboratory Techniques
Introduction
Welcome to the Chemistry 2 laboratory! Chemistry is an experimental science, and you will find
that experimentation can help you better understand lecture material. In the laboratory you will
go over many practical applications of theories you learn in class. Use the laboratory as a study aid
to help you understand chemistry, and to have fun!
Many students do not enjoy laboratory and do not find it helpful because they take a “cookbook”
approach to chemistry. That is, they are thinking, “I mix 1 gram of this with 5 mL of that to get
a blue solution with white stuff at the bottom.” They do nothing more than follow the “recipe”
without thinking about what is happening in the test tube and how it relates to their studies, the
world, or even existence as we know it. Since we do not let you eat the end results of what you
cook in lab, if you take the cookbook approach, you are going to have a poor experience in the
laboratory and an especially hard time completing your laboratory reports.
This lab manual is written to help you avoid such a bad experience and to help you develop skills
in solving problems. You will not find recipes in your experiments; you are given considerable
leeway in designing your own experiments. Whenever you need a lab technique, you will be given
complete instructions on how to execute it, but you must be able to figure out how to apply those
techniques in discovering the solutions to the problems presented. It is critical that you read the
experiment before coming to the laboratory, and attempt to understand the theory behind the
experiment and the methods you will use in the laboratory to investigate that theory.
Consider yourself an investigator while you are in the laboratory. For example, in a typical reaction,
first find out “who done it”; what chemicals take part in the reaction? Then find out the culprits’
“method”; is energy taken in or given off? Finally, you need to find out the consequences; what
compound is formed? If you take this approach you will have a better laboratory experience, and
you will have a much easier time writing the experimental report. In short, you will learn more
and learn more easily.
This lab is designed to 1) acquaint you with the equipment in your locker, and 2) introduce
you to some basic laboratory techniques. A word of warning: a few of you may find this and
other beginning laboratories to be somewhat tedious, especially if you’ve had a good high school
chemistry laboratory course. However, please be patient as the goal is to give all students a good
common background so every student has an excellent chance of success with the later, more
difficult experiments.
Remember that as pre-laboratory preparation, you should come to the laboratory with Title,
Purpose, Procedure, and Data Tables written in your duplicating paper laboratory notebook. At
the end of the laboratory period, you should have your TA sign and date your laboratory notebook
near your data tables. You will turn in a completed post-lab report by your next lab period.
3
Introductory Laboratory Techniques
Learning Goals
The following is a list of skills that you will use in this experiment.
• Using a balance
• Handling lab glassware
Laboratory • Using a buret
• Using a volumetric pipet
• Using a Bunsen burner
• Precision and accuracy
Conceptual
• Temperature dependence of the density of water
• Calculation of density
• Statistical analysis (average, standard deviation, 90%
Data Analysis confidence limits
• Calculation of mass percent
• Percent Error
4
Introductory Laboratory Techniques
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
than “to contain” (TC). The last drop of liquid should not drain out of
the tip of a TD pipet in normal use.
Hint
However, there should be no water drops left on the side walls. The
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5
Introductory Laboratory Techniques
7. Repeat steps 5 and 6 at least two additional times without emptying out
your flask between trials.
B. Using a Buret to Measure Volume
8. Discard the water in your Erlenmeyer flask, and re-measure the mass
of the flask. The inside of the flask does not need to be completely dry
because any water left in it is from the previous procedure and is at the
same temperature as the new water you will be adding.
9. Use a 25 mL buret and accurately measure out about 12 mL of room
temperature deionized water from part A into the flask. You should read
the buret to the closest one-hundredth mL (e.g., 12.14 mL). You will
have to estimate the last digit.
In your laboratory notebook, record your initial buret reading and your
•
final buret reading. The volume of water delivered by the buret is the
difference between the final and initial buret reading.
10. Measure and record the mass of the flask and the water.
11. Repeat steps 9 and 10 at least two additional times without emptying
out your flask between trials.
Always clean your buret after use and rinse it with deionized water before
storage. Furthermore, be sure you follow the instructions given in the
Appendix for proper use of the buret.
C. Using a Beaker to Measure Volume
12. Measure and record the mass of a clean and dry 100 mL beaker. Note
that this beaker needs to have a 50 mL graduation mark.
13. Use your clean and dry 100 mL beaker and carefully measure out 50 mL
of your room temperature water.
14. Measure and record the mass of the beaker and the water.
15. Empty out your beaker and carefully measure out another 50 mL of
your room temperature water. There is no need to reweigh the empty
beaker.
16. Measure and record the mass of the beaker and water.
17. Repeat steps 15 and 16 at least two additional times.
Part II. Drying a Hydrate
1. As demonstrated by your TA, place a clean crucible on a wire triangle
on an iron ring above a Bunsen burner. With the TA watching, light
the Bunsen burner and adjust the flame and the iron ring so that the
crucible is positioned in the hottest part of the flame.
6
Introductory Laboratory Techniques
2. Heat the crucible for 5 minutes to make sure it is dry, and then remove it
from the wire triangle using crucible tongs and place it on your benchtop
on top of a piece of wire gauze to cool.
3. After the crucible has returned to room temperature (approximately
5 minutes), measure and record its mass to one-thousandth of a gram
(milligram).
4. Weigh into your crucible 1.0–1.2 g of manganese(II) sulfate monohydrate,
MnSO4·H2O, recording the exact mass to one-thousandth of a gram
(milligram).
5. Heat the crucible with its contents for 5 minutes, and then remove it
to your benchtop on top of a piece of wire gauze using crucible tongs.
6. After the crucible and its contents have returned to room temperature,
measure and record the mass.
7. Repeat steps 5 and 6 until the mass readings are consistent and the mass
no longer decreases after heating.
8. Calculate the mass loss by your sample upon heating.
9. Transfer the contents of your crucible to the waste container located in
the fume hood.
Clean-Up:
• Solid dry manganese(II) sulfate may be disposed of in the proper
waste container found in the fume hood.
• Clean your volumetric pipet and buret with deionized water only.
All other glassware may be cleaned with tap water and rinsed with
deionized water.
• You may also use pipet cleaning solution to clean your volumetric
pipet if any drops cling to the sides after draining.
• Always let your glassware air-dry; do not attempt to dry your
glassware with a paper towel as the towel may become lodged in
the glassware.
• If time permits, now would be a good time to also clean any other
dirty glassware in your locker.
• Return the burets and pipets to their proper locations and place all of
the glassware from your locker back in your locker.
• Clean your laboratory bench with your deionized water wash bottle
and sponge. Once finished, ask your TA to sign your data sheets and
lock your locker.
7
Introductory Laboratory Techniques
Data Analysis
Calculating the Density of Water:
An important skill learned in the CHE 2 series is coming to lab with tables prepared in your
lab notebook for any data that you will collect during the experiment (i.e. masses of substances,
volumes of solvents, temperatures, observations, etc.). An example of a data table is given below:
formula.
mass of water delivered (g) = mass of flask with water (g) - mass of flask (g)
•
volume of water delivered (mL) = final buret reading (mL) - initial buret reading (mL)
•
3. For each trial, calculate the density of water by dividing the mass of water delivered by the
volume of water delivered:
𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑜𝑜𝑜𝑜 𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤 𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑 (𝑔𝑔)
𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷𝐷 (𝑔𝑔/𝑚𝑚𝑚𝑚) =
𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣 𝑜𝑜𝑜𝑜 𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤𝑤 𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑 (𝑚𝑚𝑚𝑚)
4. Based on your 3 trials, what is the average density of water?
5. Calculate standard deviation for your average density of water. For help with any statistical
analyses of your data, including calculating the average, standard deviation, and 90% confidence
limit, please see the Statistical Treatment of Data section in the Appendix.
6. Calculate the 90% confidence limit for your average density of water.
8
Introductory Laboratory Techniques
7. Use the temperature of your water along with the values of mass and volume of water given in
Table 1 to calculate the accepted values for the density of water.
8. Use the following formula and the accepted literature value for the density of water to calculate
relative error.
Table 1:
The volume occupied by 1.0000 g water weighed in air against stainless steel
weights.
Temperature (°C) Volume (mL)
18 1.0024
19 1.0026
20 1.0028
21 1.0030
22 1.0033
23 1.0035
24 1.0037
25 1.0040
26 1.0043
Table 1 gives the corrected volume in mL occupied by 1.0000 g of water when weighed in
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air against stainless steel weights for different temperatures. Two effects are included in this
volume per 1.0000 g: first, the change in the density of water with temperature, and second, a
much smaller correction due to buoyancy.
The buoyancy correction arises since the balance was set to zero with a certain mass of air on
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the balance pan. The volume of water displaces some of this air from the balance pan, and the
displacement makes the water appear lighter than it really is. The contribution of buoyancy to
the results in Table 1 is roughly 0.0011 mL per 1.0000 g of water.
9. Complete steps 1-8 to calculate the density of water when measured using a pipet, a buret, and
a beaker.
Calculating Mass Percent of Water:
1. What was the mass, in grams, of your MnSO4·H2O sample before heating?
2. What was the mass, in grams, of your MnSO4·H2O sample after heating?
3. What was the mass, in grams, of water lost from your sample after heating?
4. Calculate the experimental mass percent of water in your MnSO4·H2O sample. Use the
following formula:
9
Introductory Laboratory Techniques
5. Calculate the theoretical mass percent of water by using the molecular weights for MnSO4·H2O
for the initial mass, and MnSO4 for the final mass.
• The molecular weights for MnSO4·H2O and MnSO4 are 169.0 g/mol and 151.0 g/mol
respectively.
6. Use the formula for relative error, the experimental mass percent of water in your MnSO4·H2O
sample, and the theoretical mass percent of water to calculate relative error.
10
Observing Chemical Reactions
Introduction
An integral part of any experimental science is observing how the world behaves and drawing
conclusions from the observed behavior. In this laboratory exercise you will mix chemicals and
make observations about the resulting solutions. Your observations of these attempts will tell you
whether or not the reactions actually occur, and from this data you will be able to plan a procedure
for identifying and separating the salts in an unknown.
How do you know that mixing two chemicals results in a chemical reaction? Look for as many
physical indications as possible. Does the color of the solution change? Does it heat up? Does it
cool down? Is gas evolved? Use all of your senses except smell and taste; remember, never smell or
eat any chemicals in the laboratory!
It cannot be emphasized enough that making good observations and writing them down, is critical
to successful investigations in science. Think about how often you have said to yourself, “I’ll
remember the phone number until I get home,” and then promptly forgotten it. It is much easier
to forget something you have noted about a new chemical reaction, especially something you did
not realize was significant at the time, than something you considered important in the first place.
If you note a change or a lack of change, write it down!
The types of changes that you may observe in this lab can include color changes, bubbling, or
precipitation reactions. Precipitation reactions are a particular type of reaction that results when an
insoluble compound is formed from the mixing of two chemicals, and these types of reactions are
very important in everyday life.
After determining which chemicals react in Part I of this lab, you will need to develop a scheme
for the separation of a mixture of salts for Part II. Check with you TA to ensure that your scheme
will work. Once you have an acceptable scheme, you will identify which two of the salts you have
worked with are in your unknown solution.
11
Observing Chemical Reactions
Learning Goals
The following is a list of skills that you will use in this experiment.
12
Observing Chemical Reactions
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
13
Observing Chemical Reactions
4. Add a couple more drops and record your observations. Continue until
you are sure that you have added an excess of the reagent. It will not take
more than 0.5 mL to reach an excess of the reagents.
5. There are sixteen possible combinations of salts with reagents. Try them
all and record any reactions you observe. You may also want to see what
happens if you add more than one reagent to the salt solution.
As you work on this portion of the experiment, compare your results with
your neighbors. If you seem to get different results, talk about why your
results differ. Did one of you make an error, or are you just going about
things differently?
Clean-Up:
• Pour any solutions or solids containing silver or aluminum into the
Cation Metal Waste jar in the fume hood.
• Pour the rest of the solutions into a 400 mL beaker for clean-up at the
end of the laboratory.
14
Observing Chemical Reactions
As there are likely to be more people using the centrifuge, make sure
•
that your test tubes are labeled so that you can identify them when the
centrifuge stops.
3. Turn on the centrifuge and allow it to spin for a minute. When the
centrifuge stops spinning, remove your test tube carefully—you do not
want to disturb the solid at the bottom of the tube.
4. Decant the supernatant solution from the solid and reserve. Avoid
disturbing the precipitate when pouring off the solution.
5. Add a few milliliters of deionized water to the precipitate and stir. This
washes any excess reagent away from the precipitate. Re-centrifuge.
Decant the supernatant and combine with the reserved solution from
Step 4.
You have now completed the separation of your precipitate from solution.
Separate tests may be performed (as needed) on the precipitate or the
supernatant solution.
Question C: Why do you test for complete precipitation if you are going
to do any further chemical tests on the supernatant?
Clean-Up:
• Pour any solutions or solids containing silver or aluminum into the
Cation Metal Waste container in the fume hood.
• Pour the rest of the solutions into your 400 mL beaker.
• Slowly add 3 grams of sodium bicarbonate to the solution in the
beaker to neutralize the acid.
• Pour the neutralized solution in the sink with copious amounts of
water.
15
Observing Chemical Reactions
Data Analysis
Observing Reactions of the Metal Salt Solutions
An important skill learned in the CHE 2 series is coming to lab with tables prepared in your
lab notebook for any data that you will collect during the experiment (i.e. masses of substances,
volumes of solvents, temperatures, observations, etc.).
Please copy the table below into your lab notebook. Make sure that each of the cells are large
enough to write detailed observations during the experiment (feel free to take up a whole page in
your lab notebook if needed).
Reagents
Metal Ions
HCl NaOH HNO3 H2SO4
Ag+
Sr2+
Mg2+
Al3+
An example of a detailed observation may include some of the following information (be as
descriptive as possible):
• Color change upon mixing of two reactants
• Formation of a precipitate (or insoluble solid)
• Formation of gas (seen as bubbling without heating the mixture)
• Temperature change (the vessel feels colder/warmer after reacting, indicating an endo- or
exothermic reaction)
16
Observing Chemical Reactions
Possible Ions:
Ca2+(aq), Mg2+(aq)
Ask Your TA
Observations: Some transition
Ca2+(aq) + SO42-(aq) → CaSO4(s) metals can have very
Mg2+(aq) + SO42-(aq) → no reaction interesting results. Talk
to your TA if you want
Add H2SO4. further information.
Yes CaSO4 is formed. Ca2+ Try another reagent to
Is a reaction
is present. test for Mg2+.
observed?
No
Solubility Rules
These rules are provided to help you understand the basic solubility rules of
chemistry. These rules always have exceptions, as many things in chemistry
do. As a consequence, remember to trust your observations.
1. Compounds that are soluble or mostly soluble:
• Group 1, NH4+, chlorates, acetates, nitrates
• Halides (except Pb2+, Ag+, and Hg22+)
• Sulfates (except Ca2+, Sr2+, Ba2+, Pb2+, and Hg22+)
2. Compounds that are insoluble:
• Hydroxides, sulfides (except above rules, and group 2 sulfides)
• Carbonates, phosphates, chromates (except above rules)
17
Observing Chemical Reactions
18
Chemical Equilibrium
Introduction
Previously, you have only experienced reactions in lab that proceed to completion. An example of
this type of reaction is the dissociation of HCl in water. Since hydrochloric acid is a strong acid, it
completely dissociates in water. A 1.0 M HCl solution is essentially a solution of 1.0 M hydrogen
ions and 1.0 M chloride ions in water. We can write this as:
HCl(aq) → H + (aq) + Cl -(aq)
The same does not occur when the weak acid HF is dissolved in water. While a 1.0 M HF solution
does contain hydrogen and fluoride ions, it also contains a significant quantity of undissociated
hydrofluoric acid. We can write this as:
HF(aq) ⇌ H + (aq) + F -(aq)
The double arrow, as seen above, is used to indicate that the acid does not completely dissociate,
and that the system has established chemical equilibrium. Equilibrium can be thought of as a
balance between the reactants and products. Most reactions do not go to completion, but instead
proceed to a point where both reactants and products are present. An important aspect of chemical
equilibrium is that it can be established by starting with either reactants or products. The reaction
will proceed in the forward or backward direction until coming to equilibrium, which depends on
the concentration of reactants/products, temperature, and pressure.
In 1884, French chemist Henri Louis Le Châtelier presented his findings on the behavior
of chemical systems at equilibrium. He found that when equilibrium was disturbed, by either
changing concentration, pressure, or temperature, the reaction would re-establish equilibrium by
proceeding in the direction that “relieved stress” on the system. This principle is generally referred
to as Le Châtelier’s Principle, and is as follows: when a stress is applied to a chemical system at
equilibrium, the equilibrium shifts in a direction that reduces the effect of the stress.
In this qualitative experiment, you will observe different systems of equilibrium, and note the
effect of added stress on each system. Make sure to record detailed observations and consider how
the results relate to equilibrium topics you are studying in lecture.
19
Chemical Equilibrium
Learning Goals
The following is a list of skills that you will use in this experiment.
20
Chemical Equilibrium
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
21
Chemical Equilibrium
Thus, the system will change color depending on the quantity of the complex
ion present. In this part of the experiment, you will observe the change in
the equilibrium position by adding various chemicals.
0.25 mL
1
1 mL
22
Chemical Equilibrium
Clean-Up
• Pour the content from the test tubes into the waste container in the
fume hood labeled “Cation Metal Waste.”
23
Chemical Equilibrium
3. Keep your remaining 6 M HCl for use in other parts of the experiment.
Methyl orange indicator
1. Place 3 mL of deionized water into each of three test tubes. Add two
drops of methyl orange indicator to each of the test tubes. Observe the
color of the solutions.
a. To the first test tube, add two drops of 6 M HCl. Observe any color
change.
b. To the second test tube, add 4 drops of 6 M NaOH. Observe any
color change.
c. Use the third test tube as a reference.
Question B: What are the colors of the protonated and unprotonated forms
of phenolphthalein?
Question C: What are the colors of the protonated and unprotonated forms
of methyl orange?
Clean-Up
• Save the HCl solution until the end of the experiment.
• Using a small stream of no more than 5 mL of DI water total, rinse
the contents of the other test tubes into an 800 mL beaker. Save this
solution until Part IV.
24
Chemical Equilibrium
25
Chemical Equilibrium
Clean-Up
• Save the HCl solution until the end of the experiment.
• Using a small stream of no more than 5 mL of DI water total, rinse the
contents of the other test tubes into the 800 mL beaker.
• Dissolve approximately 1 gram of sodium bicarbonate in the solution
in the beaker. Dispose of the solution in the sink with copious
amounts of water.
(blue) (red-pink)
Safety First
EtOH is the abbreviation for ethanol—CH3CH2OH. You will note that
Ethanol is a flammable “heat” has been shown to be a “product” of the reaction as it is read from left
liquid. Keep the test
tube capped and keep to right. In other words, as the reaction occurs from left to right, the system
the test tube away from gives off energy in the form of heat. Thus, the system will change color
sources of ignition. depending on whether heat is added or removed from the system.
1. Fill a 400 mL beaker half way with ice. Add a small amount of water.
2. Acquire a capped test tube containing 1% cobalt chloride dissolved in
95% ethanol. Place the test tube inside the ice bath, be careful to leave
half the solution above the ice. Observe the color change.
3. Remove the test tube from the ice water bath and allow it to warm back
to room temperature. Observe the color change.
4. Return the test tube to your TA.
26
Chemical Equilibrium
27
Chemical Equilibrium
Clean-Up
• Using a small stream of no more than 5 mL of DI water total, rinse the
contents of all test tubes into the 800 mL beaker.
• Dissolve approximately 1 gram of sodium bicarbonate in the solution
in the beaker.
• Dispose of the solution in the sink with copious amount of water.
28
Chemical Equilibrium
Data Analysis
Data Table Preparation & Recording Observations
Observations will be the primary data collected in this qualitative lab. An example of a table for
Part I can be found below. You may use this table for Part I, then use it as a guide for making your
own tables for the other parts of this experiment.
Record your detailed observation of what happens in each test tube. Note any color change,
precipitation, change in temperature, or bubbling.
• For more information on recording observations, refer back to the Data Analysis section of
Observing Chemical Reactions.
• Make note of any reference samples, and remember that depending on how you create your
table, not every cell will be filled in depending on what the procedure entails.
Le Châtelier’s Principle
The equilibrium reactions observed in this lab can be explained using Le Châtelier’s principle. If a
chemical system is “stressed” via the introduction of excess reactants/products, change in pressure,
or change in temperature, the system will adjust in order to re-establish equilibrium. To understand
how stress affects a system, follow the procedure below:
1. Write out the chemical reaction in question.
• Tip: Endothermic reactions require heat to proceed, so heat is listed as a reactant.
Exothermic reactions generate heat, therefore heat is a product for these reactions.
2. Indicate which chemicals are being added to the system.
3. Draw an arrow indicating the overall direction that the reaction will proceed in order to relieve
the stress of the added chemicals.
4. Consider how the shift will change the concentrations of both reactants and products, including
heat, if applicable.
29
Chemical Equilibrium
• Tip: Concentration is often indicated by writing brackets around a chemical formula (i.e.
[HCl] means “the concentration of HCl”).
Below is an example of this process applied to the equilibrium of oxalic acid after the addition of
6 M HCl:
6 M HCl
added
From this analysis, we can see that when 6 M HCl is added, in order to re-establish equilibrium:
1. Equilibrium shifts to the left.
2. [H2C2O4] increases.
3. [H3O+] decreases.
4. [HC2O4-] decreases.
The oxalate ion equilibrium in Part V is the most complex systems in this experiment. Changes
in concentrations of one component (particularly something that appears as a product in one
equation and as a reactant in another) will affect the equilibria of the whole system.
30
Strong Acid-Strong Base Titration
Introduction
Standardization
These next four experiments permit you to explore important aspects of acid-base chemistry. We
start by exploring a straightforward reaction between a strong acid and strong base. The solutions
you prepare in the strong acid-strong base experiment will be used as standardized solutions when
you explore the titration of a weak-acid, a polyprotic acid, and a buffered system. Titration is
a technique used to determine the concentration of a substance in solution. For example, food
chemists often use titrations to determine the sugar, salt, or vitamin content in a sample. A
standard solution is one whose concentration is accurately known, and can be used to determine
the concentration of other solutions.
In this experiment, you will prepare a few standard solutions. If a solute can be obtained in a
very pure, stable, weighable form, a primary standard solution of it can be prepared directly. To
prepare a primary standard, an accurately determined amount of the solute must be dissolved in
the desired solvent with an accurately known final volume. Care must be taken to ensure that the
solution is homogeneous and that it is at ambient temperature when the final adjustment of its
volume is made.
If the desired reagent cannot be obtained in primary standard form, one can only prepare a
secondary or tertiary standard solution of it. A secondary or tertiary standard solution is prepared
by dissolving an approximate amount of the solute in the desired solvent to the desired final
volume, and standardizing the solution. A reagent solution may be standardized in a few ways:
1.) By titration against a measured mass of a suitable primary standard substance;
2.) By titration against another reliably known secondary standard solution;
3.) By direct analysis for the reagent in question by some suitable non-titrimetric method such as
spectroscopic analysis.
In this experiment, you will prepare a primary standard consisting of an accurately weighed mass
of potassium hydrogen phthalate (KHP). You will use this primary standard to determine the
concentration of a sodium hydroxide (NaOH) solution, which will then be used as a secondary
standard to determine the concentration of a hydrochloric acid (HCl) solution. The HCl solution
will become your tertiary standard. Solid sodium hydroxide and hydrochloric acid are hygroscopic
(i.e. they attract and hold water molecules from the surrounding environment), which makes it
difficult to accurately weigh and determine molar amounts in a sample. For this reason they must
be standardized against a primary or secondary standard.
Titrations
In this experiment you will determine the concentration of sodium hydroxide and hydrochloric acid
solutions using a titration. The titration of HCl with NaOH takes advantage of the neutralization
31
Strong Acid - Strong Base Titration
reaction between a strong acid and a strong base. According to the Arrhenius Acid-base Theory,
when acids and bases dissociate, or “ionize”, in water, an acid raises the concentration of hydrogen
ion, H+, and a base raises the concentration of hydroxide ion, OH-. When reacted together, the
acid and base will neutralize each other according to net ionic equation (1). Note that H+ can also
be written as H3O+, as a result of H+ associating with H2O.
32
Strong Acid - Strong Base Titration
Learning Goals
The following is a list of skills that you will use in this experiment.
33
Strong Acid - Strong Base Titration
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
34
Strong Acid - Strong Base Titration
Clean-Up:
• Using less than 5 mL of DI water, rinse any excess 6.0 M HCl and 6.0 M
NaOH into an 800 mL beaker.
• Save this solution for the clean-up procedure at the end of lab.
Weighing by difference
• This technique eliminates systematic errors from the balance during
weighing.
• First, measure the mass of the container with the material from which
you are going to draw your sample. Then, remove some of the material
and place it in a separate container. Re-measure the mass of the
original container and the remaining material.
• Calculate the mass removed, and repeat the process until you have
removed the mass desired.
35
Strong Acid - Strong Base Titration
36
Strong Acid - Strong Base Titration
37
Strong Acid - Strong Base Titration
d. You may wish to record the buret volume of several successive drops
as you approach the endpoint in case you discover that you have
overshot the endpoint. Record the final buret reading to the nearest
0.02 mL.
e. Refill the buret and similarly titrate the remaining two KHP samples.
f. Clean up by pouring the solution in the titration flasks into your
800 mL beaker.
6. Calculating the concentration of your NaOH solution:
a. Since NaOH and KHP react in a 1:1 molar ratio, the equivalence
point occurs when the moles of NaOH added to the flask equals the
moles of KHP present.
b. The number of moles of KHP present in the flask can be determined
using the mass of KHP added to the flask.
c. Calculate the molarity of your prepared NaOH solution using the
moles and volume of NaOH added to the flask at the equivalence
point.
d. Determine the molarity of NaOH for all three titrations.
7. Following directions found in the appendix, perform a Q-test on the
calculated molarities from all three titrations.
a. If a value fails the Q-test, perform another titration and discard the
outlier.
b. You should discard the data from the first cursory titration if this
titration was performed quickly.
Part III. Strong Acid-Strong Base Titration Curve
This part of the experiment requires the use of a pH meter to measure the
pH of various solutions. The pH meter and the accompanying electrode
are both very expensive and fragile. Treat both pieces of equipment with
great care. Read and understand the pH meter operation instructions in
the Common Laboratory Procedures section of Appendix of this manual.
Follow the directions provided very carefully.
38
Strong Acid - Strong Base Titration
The information you generate in this part of the experiment has two
goals: 1) to standardize the approximately 0.2 M HCl solution, and
2) to demonstrate the classic titration curve of acid-base chemistry. You
will be doing the titration procedure at least twice. The first titration will
familiarize you with the critical pH and volumes for your specific solutions’
concentrations, after which you may adjust your technique to more
accurately locate the endpoint for the specific solutions you are using.
1. Calibrate the pH meter.
a. The pH meter will need to be calibrated before starting the experiment.
There is no need to recalibrate later during the experiment.
b. Dispense the pH 4.00, pH 7.00, and pH 10.00 buffers into the mini
buffer bottles, taking care not to overfill.
Standardize the pH meter using the three buffer solutions following
the procedure outlined in the Appendix of this manual, pH Meter
Operating Instructions.
Always keep the pH electrode in the electrode storage solution when
not in use.
2. Prepare the titration vessel.
a. Use your volumetric pipets to quantitatively transfer 15.00 mL of
the approximately 0.2 M HCl solution you prepared in Part I into
a 150 mL beaker. Without measuring precisely, add about 15 mL
of deionized water to this beaker. Place a magnetic stir bar into the
beaker gently so no reagent splashes.
b. Place a magnetic stir plate under a buret clamp that is adjacent to the
pH meter you have just standardized near your work area and place
the beaker on the stir plate.
c. Use the previously conditioned buret from Part II filled with the
approximately 0.2 M NaOH solution that you standardized in Part
II and clamp it in place above the beaker.
39
Strong Acid - Strong Base Titration
d. Clamp the pH electrode in place below the level of the liquid in the
beaker and away from the stir bar. Adjust the position of the buret
tip so that it is inside the beaker, away from the side but with the
stopcock at a convenient location for you to manipulate. Position
the beaker so that the stir bar is somewhat displaced away from the
center of the beaker to allow room for the pH electrode but make
sure that the stir bar is above the center of the stir plate.
3. You will now standardize the HCl solution by titrating it with the
previously standardized NaOH solution, and following the course of the
acid neutralization reaction by monitoring the pH with the pH meter.
Tip
4. Begin with a quick titration.
When recording data on
a spreadsheet, leave an To do so, you will add the titrant (0.2 M NaOH) in small increments,
•
empty column between and recording the volume reading in the buret and the pH reading from
the buret reading and
the corresponding pH.
the pH meter in your note book.
This column can be used
to calculate the total
Follow the instructions closely and add the titrant in the correct
•
40
Strong Acid - Strong Base Titration
NaOH at a time from well below the endpoint to well above the endpoint.
Record your buret readings after the addition of each increment.
Allow time for the reaction vessel to become equilibrated and for the
•
Clean-Up
• Tightly cap and store the bottles containing the standardized NaOH
and HCl solutions for use in later experiments.
• Drain the remaining NaOH from the buret into the 800 mL beaker.
Add any left-over KHP, and any excess 6 M HCl into the 800 mL beaker.
• Slowly and carefully, add 1 gram of sodium bicarbonate to the
solution in the 800 mL beaker.
• Pour the solution into the sink with copious amount of water.
▶ SAVE your standardized 0.2 M HCl and 0.2 M NaOH. You will
use these solutions for the next 3 experiments.
41
Strong Acid - Strong Base Titration
Data Analysis
Calculating concentration of NaOH solution
1. Using the mass of KHP you weighed out in part 2, determine how many moles of KHP were
present in the sample for your first good titration.
• Tip: KHP has the chemical formula KHC8H4O4, with a formula mass of 204.23 g/mol.
2. Write down the chemical equation for the neutralization reaction of NaOH with KHP.
Determine the stoichiometric ratio between these two reagents. In other words, how many
moles of NaOH react with each mole of KHP?
3. Using the information you found in steps 1 and 2, determine how many moles of NaOH were
dispensed in your first titration at the equivalence point.
• Tip: Keep in mind the equivalence point occurs when the KHP is fully neutralized by
NaOH. This means all moles of KHP will have reacted with NaOH.
4. Using the moles of NaOH calculated in step 3 and the volume of NaOH added at the equivalence
point, determine the molarity of your NaOH solution. Remember to pay attention to units!
• Tip: When calculating the volume of NaOH added, take the difference between the
equivalence point buret reading and initial buret reading.
5. Repeat steps 1-4 to calculate the molarity of your NaOH for each titration.
6. Calculate the average molarity of your NaOH solution. This solution has now been
“standardized”, and can be used as a titrant to determine the concentration of other analytes.
7. Calculate the standard deviation of the average molarity of your NaOH solution.
8. Calculate the 90% confidence limit for your average molarity.
Generating titration curves
9. Use a spreadsheet program such as Excel to enter the buret readings and corresponding pH
for each titration. Use the buret readings to calculate the total volume of NaOH added at each
point in the titration.
• Tip: The total volume of NaOH added at any point in the titration can be calculated by
taking the difference between that buret reading and the initial buret reading.
10. Generate a scatter plot of the total volume of NaOH added vs. pH. Make sure to include a plot
title and labeled axes with units.
11. Repeat steps 9 and 10 for each titration of NaOH with HCl.
42
Strong Acid - Strong Base Titration
12
10
pH level
8
0
5 10 15 20 25 30
Volume of NaOH added (mL)
��� � ���� )
��� =
2
•
43
Strong Acid - Strong Base Titration
In the column labeled “Vm”, enter the formula that will calculate the volume midway between
•
Vi and Vi+1, but instead of “Vi”, select the spreadsheet cell containing the first volume of
NaOH, and instead of “Vi+1”, select the cell containing the second volume of NaOH added.
Apply this equation to the rest of the cells in the column by clicking in the bottom right-hand
corner of the cell and dragging downwards.
4. Next we will calculate values for D1. D1 is the rate of change in pH as NaOH is added. This
can be expressed using the following equation, where Vi and Vi+1 are the same as in step 3, and
pHi and pHi+1 are the pH readings corresponding to those volumes.
������ � ��� )
��� =
����� � �� )
•
In the column labeled “D1”, enter the formula for D1 using the cells containing data from the
•
first and second volumes of NaOH added and the corresponding pHs. Apply this equation to
the rest of the cells in the column. Notice that you will not be able to apply this calculation to
the last row of the data since there are no data values beyond the last row to use for pHN+1 or
VN+1.
5. Generate a 1st derivative graph by plotting your calculated midpoint volumes (Vm) on
the x-axis of a scatter plot, and the 1st forward divided differences (D1) on the y-axis. The
equivalence point of the titration is the maximum point on this curve.
First Derivative
35
30
25
20
15
D1
10
0
5 10 15 20 25 30
-5
Volume of NaOH added (mL)
Now we will calculate the derivative midpoint volume, Vd. Vd is calculated the same way as Vm,
but instead of finding the midpoint volume between original volumes of NaOH added, you will
find the midpoint between Vm values. This can be mathematically expressed using the following
equation, where Vmi is one of the Vm data points and Vmi+1 is the next data point in the sequence.
���� � ����� )
��� =
•
2
In the column labeled “Vd”, enter this formula to calculate the volume midway between Vmi
•
and Vmi+1. Just like with calculating Vm, select the appropriate spreadsheet cell containing the
values for Vmi and Vmi+1. Apply this equation to the rest of the cells in the column by clicking
44
Strong Acid - Strong Base Titration
in the bottom right-hand corner of the cell and dragging downwards. Notice that you will not
be able to apply this calculation to the last row of data.
6. Next we will calculate values for the 2nd forward divided difference, D2. D2 is calculated
the same way as D1, but instead of finding the rate of change in pH, you will find the rate of
change in D1. This can be expressed using the following equation, where Vmi and Vmi+1 are
the same as in step 3, and D1i and D1i+1 are the 1st forward divided differences corresponding
to those midpoint volumes.
������ � ��� )
��� =
������ � ��� )
•
In the column labeled “D2”, enter this formula to calculate the 2nd forward divided difference.
•
Just like with calculating D1, use the appropriate spreadsheet cells containing values for D1i,
D1i+1, Vmi and Vmi+1. Apply this equation to the rest of the cells in the column. Notice that
you will not be able to apply this calculation to the last row of data.
7. Generate a 2nd derivative graph by plotting your calculated derivative midpoint volumes (Vd)
on the x-axis of a scatter plot, and the 2nd forward divided differences (D2) on the y-axis. The
equivalence point of the titration is the value at which the plot passes through the x-axis..
Second Derivative
280
230
180
130
80
30
D2
-20
5 10 15 20 25 30
-70
-120
-170
-220
Volume of NaOH added (mL)
or printed copies). Make sure your name is on each graph, and that you have included a
title and labeled axes with units.
45
Strong Acid - Strong Base Titration
46
Strong Acid - Strong Base Titration
47
Strong Acid - Strong Base Titration
48
Acid Dissociation Constants
and the Titration of a Weak Acid
Introduction
One of the most important applications of equilibria is the chemistry of acids and bases. The
Brønsted-Lowry acid-base theory defines an acid as a species that donates a proton and a base
as a species that accepts a proton. In the case of an aqueous solution of a strong acid, such as HCl,
the acid reacts completely with the water and dissociates into the hydronium ion, H3O+, and the
chloride ion, Cl- as shown by
ൣுయ ைశ ൧ሾష ሿ
ܭ ൌ (3)
ሾுሿ
The equilibrium constant, Ka, is called the acid dissociation constant. Recall that water is not
included in the equilibrium constant expression since it appears in the reaction as the pure
49
Acid Dissociation Constants and the Titration of a Weak Acid
liquid. The magnitude of the dissociation constant provides information regarding the degree of
dissociation of the acid in water. For example, the Ka values for HF and HCN are 7.2 ×10-4 and
4.0 × 10-10, respectively. The larger Ka value of HF indicates that the equilibrium reaction between
HF and H2O (4) lies further to the right than the equilibrium reaction between HCN and H2O
(5).
50
Acid Dissociation Constants and the Titration of a Weak Acid
ሾ ିܣܪሿሾܱ ିܪሿ
ܭ ൌ (9)
ሾ ିܣሿ
The equilibrium constant, Kb, is called the base dissociation constant. Knowing the original
amount of HA placed into the flask, measuring the pH, and making the assumption that
the concentration of the OH- is the same as the concentration of HA, you can determine the
concentrations of all three of the species in this equilibrium constant expression.
The Ka of a weak acid and the Kb of the corresponding conjugate base are related to each other by
the equilibrium constant, Kw.
Kw = KaKb (10)
51
Acid Dissociation Constants and the Titration of a Weak Acid
By subtraction, you should be able to calculate the concentration of A- in solution. Finally, using
the relationship shown by equation (10), you will be able to re-calculate the value of Ka for the
weak acid.
Beyond the equivalence point in the titration, the strong base, OH-, will be in excess. Here, the
excess base determines the pH of the solution. The amount of OH- formed from the equilibrium
reaction shown by equation (8) is negligible. You will then plot all the pH measurements made in
this experiment against the quantity of strong base added to form a pH titration curve.
In this experiment, you will be titrating the weak acid, acetic acid, with the strong base, sodium
hydroxide. After you find the volume of strong base needed to reach the equivalence point of the
titration, you will use this information to calculate the concentration of the original weak acid
solution. You will calculate the acid dissociation constant, Ka, of acetic acid using several measured
pH readings along the titration. You will also compare the titration curves of a strong acid titration
and weak acid titration.
Learning Goals
The following is a list of skills that you will use in this experiment.
52
Acid Dissociation Constants and the Titration of a Weak Acid
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
53
Acid Dissociation Constants and the Titration of a Weak Acid
Titration Set Up
1. Calibrate the pH meter.
a. The pH meter will need to be calibrated before starting the experiment.
There is no need to recalibrate later during the experiment.
b. Dispense the pH 4.00, pH 7.00, and pH 10.00 buffers into the mini
buffer bottles, taking care not to overfill.
Standardize the pH meter using the three buffer solutions following
the procedure outlined in the Appendix of this manual, pH Meter
Operating Instructions.
Always keep the pH electrode in the electrode storage solution when
not in use.
54
Acid Dissociation Constants and the Titration of a Weak Acid
and recording the volume reading in the buret and the pH reading
from the pH meter in your note book after each addition. Follow the
instruction closely and add the titrant in the correct increments.
55
Acid Dissociation Constants and the Titration of a Weak Acid
Titration Tips
• DO NOT use your wash bottle to rinse down the sides of the beaker,
as any added volume will change the pH readings and invalidate the
titration curve data being collected.
• Record your buret readings after the addition of each increment.
• Allow time for the reaction vessel to become equilibrated and for the
pH reading to become stabilized and then record the pH value in your
notebook alongside the buret reading.
• When collecting data, leave an empty column between the buret
reading and the pH in which to place the volume of NaOH added
(difference between present buret reading and initial buret reading).
a. Before adding any titrant, record the pH of the dilute acetic acid
solution.
b. Carefully add NaOH in 1 mL increments to the beaker until
pH > 11. Record the buret reading and the pH reading. Note any
color changes that occur alongside your buret and pH readings in
your notebook.
c. When you have completed this titration, transfer the solution in the
titration flask to an 800 mL beaker.
6. Estimate the equivalence point and the midpoint by graphing pH vs.
volume of NaOH added.
a. Convert your buret readings to volumes of NaOH added.
b. In your notebook, graph a titration curve by plotting the pH level
on the y-axis and the volume of NaOH added on the x-axis.
c. Find the area of the graph where the change in pH is the greatest, in
other words, where the slope is the highest. The equivalence point
is in this region.
d. Consider the volumes of NaOH that bracket this region and estimate
the volume of NaOH needed to reach the equivalence point.
e. Estimate the volume of NaOH needed to reach the midpoint of the
titration.
7. Refill your buret with the appropriate solutions and prepare another
sample to be titrated following the same set up procedures as the
first titration.
8. Perform a precise titration to accurately determine the midpoint and the
equivalence point.
To do so, you will add the titrant in very small increments before and
•
after the estimated midpoint and equivalence point, while recording the
56
Acid Dissociation Constants and the Titration of a Weak Acid
volume reading in the buret and the pH reading from the pH meter in
your note book after each addition. Follow the instruction closely and
add the titrant in the correct increments.
a. Before adding any titrant, record the pH of the dilute acetic acid
solution.
b. Add 1 mL increments of NaOH until you are within 2 mL of the
midpoint. Record the buret volume reading and the pH reading
after each addition.
c. Once you are within 2 mL of the estimated midpoint, add NaOH
2 drops at a time until you are 2 mL beyond the midpoint. Record
the buret reading and the pH after each 2-drop addition.
d. Add 1 mL increments of NaOH until you are within 2 mL of the
endpoint. Record the buret reading and the pH after each addition.
e. Once you are within 2 mL of the estimated end point, add NaOH
2 drops at a time until you are 2 mL beyond the estimated end
point. Record the buret reading and the pH after each addition.
f. Add 1 mL increments of NaOH until pH > 11. Record the buret
reading and the pH after each addition.
g. When you have completed this titration, pour the solution in the
titration flask into an 800 mL beaker.
9. Perform another precise titration following the steps from 8a–g.
Clean Up
• Tightly cap and store the standardized NaOH and HCl solutions for
later use.
• Adjust the pH of the used solution before disposal.
• Drain the remaining NaOH from the buret into the 800 mL beaker.
Slowly and carefully add any remaining 0.05 M acetic acid to the
beaker.
• Slowly and carefully, add 1 g of sodium bicarbonate to the solution
in the 800 mL beaker. Pour this solution into the sink with copious
amount of water.
• Rinse the buret and return it to the correct storage cabinet.
• Store the pH electrode in the appropriate storage solution container.
57
Acid Dissociation Constants and the Titration of a Weak Acid
Data Analysis
Generating titration curves
1. Use a spreadsheet program such as Excel to enter the buret readings and corresponding pH
for each titration. Use the buret readings to calculate the total volume of NaOH added at each
point in the titration.
• Tip: The total volume of NaOH added at any point in the titration can be calculated by
taking the difference between that buret reading and the initial buret reading.
2. For each trial, generate a titration curve scatter plot of the total volume of NaOH added vs.
pH. Make sure to include a plot title and labeled axes with units.
Generating 1st and 2nd derivative curves
1. As instructed in the “Strong Acid-Strong Base Titration” experiment, calculate “Vm” (midpoint
volume), “D1” (1st forward divided difference), “Vd” (derivative midpoint volume), and “D2”
(2nd forward divided difference) for each trial. Use these values to graph the approximations to
the 1st and 2nd derivatives as you did in the previous laboratory. You may find it convenient to
copy and modify the spreadsheet program you prepared to work up the data for that experiment
and use it here.
Check with your teaching assistant to see how they want the graphs turned in (i.e. by email
•
or printed copies). Make sure your name is on each graph and that you have clearly titled and
labeled the vertical and horizontal axes.
If you completed 3 trials, you will only turn in graphs for the 2nd and 3rd trials (6 graphs
•
total). You will still need to make graphs for the 1st trial to determine the endpoint and
midpoint, but you do not need to turn in these graphs.
2. Using the derivative graphs, estimate the volume of NaOH required to reach the equivalence
point for each of your trials. You should be able to make this estimate to within 0.02 mL, e.g.
10.98 mL.
Calculating molarity of acetic acid solution
1. Write down the chemical equation for the neutralization reaction of acetic acid with NaOH.
Determine the stoichiometric ratio between these two reagents. In other words, how many
moles of NaOH react with each mole of acetic acid?
2. Using the molarity of your standardized NaOH solution and the volume of NaOH dispensed
at the equivalence point, determine how many moles of NaOH were dispensed in your first
titration at the equivalence point.
3. Using the molar ratio of NaOH reacting with acetic acid, the moles of NaOH calculated in
step 2, and the acetic acid sample volume, determine the molarity of your acetic acid solution.
Remember to pay attention to units!
4. Repeat steps 1-3 to calculate the molarity of acetic acid for each titration.
58
Acid Dissociation Constants and the Titration of a Weak Acid
C -x -- +x +x
E molarity - x -- x x
3. Based on the dissociation chemical equation for acetic acid, write an equilibrium constant
equation describing Ka using concentrations.
• Tip: equation (3) in the introduction is a generic version of this Ka equation.
4. Insert the “equilibrium” concentration of each reagent from the ICE table into the Ka equation.
The equation for Ka should now be written using the molarity of acetic acid solution and a
variable (i.e. “x”).
5. For your first trial, determine the concentration of H3O+ in the acetic acid solution using pH.
• Tip: the concentration of H3O+ is equal to 10-pH.
6. Using the equation for Ka, the molarity of acetic acid solution, and the concentration of H3O+,
determine Ka of acetic acid prior to the titration.
7. Calculate Ka prior to titration for each trial, and then determine the average Ka of acetic acid.
8. Calculate the standard deviation of the average Ka prior to titration.
9. Calculate the 90% confidence limit for the average Ka prior to titration.
59
Acid Dissociation Constants and the Titration of a Weak Acid
60
Acid Dissociation Constants and the Titration of a Weak Acid
6. Based on the equation for re-establishment of dissociation equilibrium between acetate ion and
acetic acid, write an equilibrium constant equation describing the base dissociation constant,
Kb.
• Tip: equation (9) in the introduction is a generic version of this Kb equation.
7. Insert the equilibrium concentration of each reagent from the re-establishment of equilibrium
ICE table into the Kb equation. The equation for Kb should now be written using the acetate
ion concentration and a variable (i.e. “x”).
8. Determine the pOH of the solution at the equivalence point. pOH can be calculated using the
equation pOH = 14 - pH.
9. Determine the concentration of OH- in solution after the re-establishment of dissociation
equilibrium between acetate ion and acetic acid. Similarly to how the concentration of H3O+
can be calculated from pH using 10-pH, the concentration of OH- can be calculated from pOH
using 10-pOH.
10. Using the equation for Kb, the molarity of acetate ion, and the concentration of OH-, determine
Kb of the re-establishment of dissociation equilibrium at the equivalence point.
11. Ka can now be calculated using equation (10) from the introduction, Kw = KaKb.
12. Calculate Ka for each trial, and determine the average Ka of acetic acid at the equivalence point.
13. Calculate the standard deviation of the average Ka at the equivalence point.
14. Calculate the 90% confidence limit for the average Ka at the equivalence point.
Determining concentration of acetic acid and acetate ion at midpoint
1. Write down the chemical equation for the reaction of acetic acid with NaOH.
• Tip: equation (7) in the introduction is a generic version of this reaction.
2. Set up and complete an “ICE” table for this reaction using the initial molarity of acetic acid.
• Tip: Your equilibrium concentration for acetic acid and acetate ion should reflect that ½
of the acetic acid has been converted to acetate ion.
3. Use the initial concentration of acetic acid, the midpoint point volume of NaOH, and the
starting volume of acetic acid solution to determine the concentration of both acetic acid and
acetate ion at the midpoint.
4. Now we will consider how the re-establishment of dissociation equilibrium affects the
concentration of acetic acid and acetate ion. Write down the chemical equation for the
dissociation of acetic acid in water, which results in acetate ion and hydronium ion (H3O+ ).
5. Set up and complete an “ICE” table for this reaction using the molarity of acetic acid and
acetate ion calculated above, and a variable (i.e. “x”).
6. Determine the concentration of H3O+ in solution using the midpoint pH.
61
Acid Dissociation Constants and the Titration of a Weak Acid
7. Apply the midpoint concentration of H3O+ to the equilibrium concentrations in the ICE table
from step 5. Calculate the midpoint concentrations of acetic acid and acetate ion.
62
Polyprotic Systems
Introduction
Until now you have dealt primarily with monoprotic acids such as hydrochloric and nitric acid in
the laboratory. This leaves an entire world of polyprotic acids unexplored. Polyprotic acids, acids
that have more than one acidic proton, are common. For example, you have worked with sulfuric
acid and with KHP that comes from diprotic phthalic acid. In this experiment, you will trace out
the entire titration curve of the diprotic acid, carbonic acid H2CO3.
In this experiment we will start with Na2CO3, which dissociates into 2 Na+ and carbonate, CO32-, in
water. We will then add acid, detecting the formation of each of the two endpoints of the titration
curve using a pH meter. One aspect of polyprotic acids that is different from monoprotic acids is
that they always make buffer solutions. Think about your list of strong acids: all except sulfuric acid
are monoprotic acids, and only the first proton of sulfuric acid is considered strong. This buffering
action can make experiments more complicated. In the experiment you are about to perform,
titration of the first endpoint that you encounter establishes a buffer solution that complicates
the analysis and determination of Ka for that equivalence point. We should note here that this
buffering action can also be used to your benefit. Some reactions take place only in a specific pH
range, and buffers can be used to maintain this pH during an experiment. You will be examining
the nature of buffer solutions in the next experiment in the series on acid-base chemistry.
Polyprotic acids can generate very complex systems at equilibrium, and can undergo multiple
separate dissociations. Carbonic acid undergoes two separate dissociations:
H2CO3(aq) ⇌ H+(aq) + HCO3-(aq) Ka1 = 4.4 × 10-7
63
Polyprotic Systems
ାሿ
ܭଶ ሾܱܥܪଷ ି ሿ ܭ௪
ሾܪଷ ܱ ൌඩ
ሾܱܥܪଷ ି ሿ
ͳ
ܭଵ
While this formula looks difficult to work with, the specific circumstances of the carbonic acid
equivalence point simplify it greatly. Firstly, for convenient laboratory concentrations, and
specifically, for those used in this experiment, it will be true that [HCO3-] >> Ka1. Consequently,
we may neglect the unity in the denominator.
64
Polyprotic Systems
Further, it will also be the case that Ka2[HCO3-] >> Kw, so that Kw may be neglected in the numerator.
Canceling and simplifying then gives:
While this does not give us either of the acid constants directly, if we know one of them, we can
use this relationship to determine the other.
From the equilibrium at the second observed equivalence point we get the necessary additional
information that enables the determination of both acid dissociation constants. At the second
observed equivalence point, the solution has had two equivalents of protons added to the analyte.
For purposes of consideration of the pH equilibria, the solution is then simply that of carbonic
acid H2CO3 (with some extra NaCl in solution that does not affect the acid equilibria).
H2CO3(aq) ⇌ H+(aq) + HCO3-(aq) Ka1
ሾܪା ሿሾܱܥܪଷ ି ሿ ି
ሾܪା ሿൣܱܥଷ ଶି ൧
ሾܪଶ ܱܥଷ ሿ ൌ ǡ ሾܱܥܪଷ ሿ ൌ
ܭଵ ܭଶ
Using substitution:
ሾܪା ሿଶ ൣܱܥଷ ଶି ൧
ሾܪଶ ܱܥଷ ሿ ൌ
ܭଵ ܭଶ
Since [H+] = [HCO3-], solving for [CO32-] in the previous expression gives:
ଶି ሾܱܥܪଷ ି ሿ
ൣܱܥଷ ൧ൌ ܭଶ ൌ ܭଶ
ሾ ܪା ሿ
ሾ ܪା ሿଶ
ሾܪଶ ܱܥଷ ሿ ൌ
ܭଵ
65
Polyprotic Systems
ሾ ܪା ሿଶ
ܭଵ ൌ
ܯ (2)
ା
ሾ ܪሿ ൌ ඥܭܯଵ
In the titration, M = a/(V + v), where a = g/(105.99 g/mol), the number of moles of sodium carbonate
in the sample, g = grams of Na2CO3 in the titrated sample, V is the original volume of water in
which the sample was dissolved, and v is the volume of HCl added to reach the second observed
equivalence point in the titration. Of course in both equations (1) and (2), [H+] = antilog10(−pH).
Once Ka1 is found, equation (1) may be used to find Ka2.
In preparation for the Acid-Base Buffer experiment, obtain your group number for your
assigned pH values from your TA.
Write your Group Number here: ___________________
Learning Goals
The following is a list of skills that you will use in this experiment.
66
Polyprotic Systems
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
Titration Set Up
1. Prepare the sodium carbonate solution.
a. For this procedure, you will need dried sodium carbonate, which
you have prepared and stored in a desiccator during the previous
experiment.
b. Accurately weigh one sample of 0.10–0.15 g sodium carbonate by
difference into a 150 mL beaker. Record the mass in your notebook.
c. Add 30 mL of precisely measured DI water to the titration vessel.
Record the volume added to the nearest 0.02 mL. Make sure the
sodium carbonate is fully dissolved before starting the titrations.
2. Prepare the titrant.
a. Find your 1 L bottle of your standardized HCl from the previous Safety First
experiments. Before opening the bottle, carefully invert it several Before inverting the
times to ensure that your solution is uniform. HCl bottle, make sure
it is properly capped.
b. Condition a 25 mL buret with your standardized HCl solution.
Remember to check that the stopcock is closed before filling a buret.
While holding the buret at a safe level, use a beaker to pour in your
hydrochloric acid solution.
67
Polyprotic Systems
Lab Skill Tips c. After conditioning, fill the buret to above the zero mark with a
Read the buret at or beaker, place the buret in the clamp, and dispel any air bubbles from
slightly below eye the stopcock. Record the initial buret reading to two decimal places,
level. Do not hold your e.g. 1.24 mL. Remember to check that the stopcock is closed
hands or lab manual
before filling the buret.
behind the buret.
You can hold a sheet of Tips on using a buret
colored paper behind
the buret to read the • Be careful when filling the buret. Only one person should be filling the
meniscus clearly. buret. Be sure the stopcock is closed before filling.
• Use a 100 or 150mL beaker to fill the buret. Never use flasks, 1L plastic
bottles, or large beakers to fill the buret.
68
Polyprotic Systems
from the center to allow room for the pH electrode but make sure
that the stir bar is above the center of the stir plate.
The Titrations
5. Perform the first titration.
To do so, you will add the titrant (0.2 M HCl) in small increments
•
throughout the titration, and in very small increments before and after
the estimated equivalence points. Follow the instruction closely and add
the titrant in the correct increments. Record all relevant observations in
your notebook.
Work efficiently by having one partner add the titrant and report the
•
buret reading while the other read the pH meter and record the data.
Make sure that each partner has a complete set of data after a complete
titration is finished. Make sure the data for the sodium carbonate
(including the mass of the sodium carbonate and volume of water
added) are clearly recorded in your notebook.
Titration Tips
• DO NOT use your wash bottle to rinse down the sides of the beaker,
as any added volume will change the pH readings and invalidate the
titration curve data being collected.
• Record your buret readings after the addition of each increment.
• Allow time for the reaction vessel to become equilibrated and for the
pH reading to become stabilized and then record the pH value in your
notebook alongside the buret reading.
• When collecting data, leave an empty column between the buret
reading and the pH in which to place the volume of NaOH added
(difference between present buret reading and initial buret reading).
a. Turn on the magnetic stir bar slowly and increase the setting
gradually until you have it rotating at a moderate speed.
b. Before adding any titrant, record the buret reading the pH of the
analyte solution.
c. Add HCl in 1 mL increments until the pH reaches 9.6. Record the
buret volume reading and the pH reading after each addition.
d. Once the pH reaches 9.6, add HCl in 0.10 mL increments until a
pH of 7 or lower is reached. Record the buret reading and the pH
after each addition.
i. The solution should turn clear within this pH interval. Record
any color change you observe next to the corresponding pH
reading.
69
Polyprotic Systems
ii. After the solution turns clear, add 3–5 drops of bromocresol
green indicator.
iii. Continue to add HCl in 0.10 mL increments until you have
added a total of 1 mL of titrant past the volume at which the
solution turned clear. Record the buret volume reading and
the pH reading after each addition.
e. Add HCl in 1 mL increments until the pH reaches 5.5. Record the
buret volume reading and the pH reading after each addition.
f. Once pH is reaches 5.5, add HCl in 0.10 mL increments until you
observe a color change. Record the buret reading and the pH after
each addition. Record any color change you observe next to the pH
reading.
g. After you observe the color change, continue adding HCl in 0.10
mL increments until you have added a total of 2 mL of titrant after
the color change. Record the buret volume reading and the pH
reading after each addition.
h. Add HCl in 1 mL increments until you have added a total of 3 mL
after the last step. Record the buret volume reading and the pH
reading after each addition.
i. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.
Lab Skill Tip 6. You will now repeat the titration for the remaining two samples by
You do not need to repeating steps 1–5.
calibrate the pH meter
again after each titration. a. Exchange roles if you did not trade off during the first titration.
Each partner needs to have performed all roles.
b. You should modify your technique for the remaining two samples
based on your experience with the first one. You may find these
general directions need to be slightly adjusted to improve the quality
of data for your curve, for example by choosing a somewhat different
specific pH at which to change the increment sizes.
70
Polyprotic Systems
Clean Up
• Tightly cap and store the bottles containing the standardized NaOH
and HCl solutions for use in later experiments.
• Adjust the pH of the used solution before disposal.
• Drain the remaining HCl from the buret into the 800 mL beaker.
• Slowly and carefully, add your remaining sodium carbonate
sample into the 800 mL beaker. Pour this solution into the sink
with copious amount of water.
• Rinse the buret and return it to the correct storage cabinet.
• Store the pH electrode in the appropriate storage solution container.
71
Polyprotic Systems
Data Analysis
Generating titration curves
1. Use a spreadsheet program such as Excel to enter the buret readings and corresponding pH for
each titration. Use the buret readings to calculate the total volume of HCl added at each point
in the titration.
• Tip: The total volume of HCl added at any point in the titration can be calculated by
taking the difference between that buret reading and the initial buret reading.
2. For each trial, generate a titration curve scatter plot of the total volume of HCl added vs. pH.
Make sure to include a plot title and labeled axes with units.
Generating 1st and 2nd derivative curves
1. As instructed in the “Strong Acid-Strong Base Titration” experiment, calculate “Vm” (midpoint
volume), “D1” (1st forward divided difference), “Vd” (derivative midpoint volume), and “D2”
(2nd forward divided difference) for each trial. Use these values to graph the approximations to
the 1st and 2nd derivatives as you did in the previous laboratory. You may find it convenient to
copy and modify the spreadsheet program you prepared to work up the data for that experiment
and use it here.
Check with your teaching assistant to see how they want the graphs turned in (i.e. by email
•
or printed copies). Make sure your name is on each graph and that you have clearly titled and
labeled the vertical and horizontal axes.
If you completed 3 trials, you will only turn in graphs for the 2nd and 3rd trials (6 graphs
•
total). You will still need to make graphs for the 1st trial to determine the endpoint and
midpoint, but you do not need to turn in these graphs.
2. Using the derivative graphs, estimate the volume of HCl required to reach the 2 equivalence
points for each of your trials. You should be able to make this estimate to within 0.02 mL, e.g.
10.98 mL.
Calculating Ka1 from the second observed equivalence point
As you calculate Ka1 and Ka2, keep in mind this titration was performed in “reverse”. Instead of
using a base to remove protons, as was observed in previous labs, HCl was used to add protons to
CO32- one at a time. The second proton was added first, at the first observed equivalence point.
The first proton was added at the second observed equivalence point. Therefore the dissociation
constant for the first proton, Ka1, is calculated using data from the second observed equivalence
point.
1. For your first trial, what is the pH at the second observed equivalence point? Use this value
to determine the concentration of H+.
2. Using the mass of Na2CO3 from your first trial, and the molar mass of Na2CO3, determine
how many moles of carbonate species are present in the sample.
72
Polyprotic Systems
3. Use the moles of carbonate species calculated above, the volume of water used to prepare
your solution, and the volume of HCl added at the second observed equivalence point to
determine the molarity of carbonate species in solution.
4. Following equation (2) in the introduction, determine the dissociation constant for the first
proton, Ka1, using the concentration of H+ and the molarity of carbonate species in solution.
5. Calculate Ka1 for each trial, and determine the average Ka1.
6. Calculate the standard deviation of the average Ka1.
7. Calculate the 90% confidence limit for the average Ka1.
Calculating Ka2 from the first observed equivalence point
Now that you have determined the acid dissociation constant for the first, most acidic proton,
Ka1, you can determine the acid dissociation constant for the second, less acidic proton, Ka2. As a
reminder, Ka2 will be found using data from the first observed equivalence point.
1. For your first trial, what is the pH at the first observed equivalence point? Use this value to
determine the concentration of H+.
2. Following equation (1) in the introduction, determine the dissociation constant for the second
proton, Ka2, using the concentration of H+ at the first observed equivalence point and the
dissociation constant for the first proton, Ka1. For our purposes, [H+] is equivalent to [H3O+].
3. Calculate Ka2 for each trial, and determine the average Ka2.
4. Calculate the standard deviation of the average Ka2.
5. Calculate the 90% confidence limit for the average Ka2.
73
Polyprotic Systems
74
Acid-Base Buffers
Introduction
In this experiment we will focus on the topic of acid-base buffers. An acid-base buffer is a solution
that resists pH change. Buffers are very important in chemistry since many reactions will only
occur in certain pH ranges. This is especially true of many biological systems in which the pH must
be maintained in very narrow ranges if the organism is to survive.
Buffers are solutions that simultaneously contain relatively large amounts of acid/base conjugate
pairs. An example that you are already familiar with is the acetic acid/acetate ion conjugate pair. A
solution containing both of these substances will be a buffer because the weak acid will react with
added base to produce the conjugate base via:
CH3COOH(aq) + OH-(aq) ⇌ CH3COO-(aq)+ H2O(l)
and the conjugate base present will react with added acid to produce the conjugate acid via:
CH3COO-(aq) + H3O+(aq) ⇌ CH3COOH(aq) + H2O(l)
In both cases the pH will change with the addition of acid or base, however the pH will change
very little if the amounts of added base or acid is small relative to the concentration of the buffer
conjugates already present in the solution.
Additionally, a buffer works best when the pH is about the same as the pKa for the acid component
of the buffer. To illustrate this, consider the reaction:
HA(aq) + H2O(l) ⇌ A-(aq) + H3O+(aq)
for which the Ka expression is:
��� �� ���� �
�� �
����
��
��� �
��o� �� � ��o���� � � �o�
����
or
��� �
�� � ��� � �o�
����
75
Acid-Base Buffers
Considering the second term in the above equation, we see that in order for the pH change to
be minimal, the contribution of the logarithm must be small. In fact, the logarithm will be zero
if [A-] = [HA] since log 1 = 0. Therefore, as strong acids or bases are added, we can expect a buffer
solution to work best at stabilizing the pH when [A-] = [HA]. If the pH is the same as the pKa, it
follows that [A-] = [HA]. The above equation, called the Henderson-Hasselbalch equation, can
also be used to determine the conjugate acid-base concentrations required to make a buffer of
specified pH. We can rearrange this equation to express the conjugate acid-base concentration ratio
in terms of pH. We do this by subtracting pKa from both sides of the equation then taking the
antilog of both sides. Recall that the antilog function is 10x.
ሾ ିܣሿ
ൌ ͳͲሺுିೌ ሻ
ሾܣܪሿ
Given a target pH for the buffer and a desired concentration for either the conjugate acid or
base, one can then find the concentration and thus a mass or volume required of the unspecified
conjugate to complete the buffer solution.
Table 1 contains a list of useful pKa values needed for this lab.
In this experiment, you will prepare two buffers and study the effects of adding acid and base.
For each of the buffers you will calculate the amounts of the conjugates required to prepare the
buffer solutions. Then you will make small additions of acid and base to the buffer solutions and
observe the pH changes that occur. You will graph these pH changes against volume and make
comparisons to the previous experiments.
76
Acid-Base Buffers
Pre-Lab Preparation
The calculations for this experiment are not trivial. For this reason, you are
required to prepare for this experiment by calculating the needed amounts
of your reagents to make your buffer solutions at the assigned pH values. The
Data Analysis section of this experiment contains questions to help guide your
calculations.
You should have been assigned a group number during the previous laboratory
session. (You were asked to write it down in your lab manual immediately
following the introduction of the Polyprotic System Experiment.)
You must have the calculations checked by the teaching assistant before you
can begin the laboratory experiment.
77
Acid-Base Buffers
Learning Goals
The following is a list of skills that you will use in this experiment.
78
Acid-Base Buffers
Procedure
Work in pairs for this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partners or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
79
Acid-Base Buffers
80
Acid-Base Buffers
81
Acid-Base Buffers
82
Acid-Base Buffers
Titration Tips
• DO NOT use your wash bottle to rinse down the sides of the beaker,
as any added volume will change the pH readings and invalidate the
titration curve data being collected.
• Record your buret readings after the addition of each increment.
• Allow time for the reaction vessel to become equilibrated and for the
pH reading to become stabilized and then record the pH value in your
notebook alongside the buret reading.
83
Acid-Base Buffers
84
Acid-Base Buffers
85
Acid-Base Buffers
Clean Up
• Adjust the pH of the used solution before disposal.
• To your 800 mL beaker, add 1 gram of sodium bicarbonate. Pour
the solution down the sink with copious amount of water.
• Consolidate the left over HCl, NaOH, acetic acid, and the buffer
solutions in a 1 L bottle. Add 3 grams of sodium bicarbonate. Pour
the solution in the sink with copious amount of water.
• Rinse the buret and return it to the correct storage cabinet.
• Store the pH electrode in the appropriate storage solution container.
86
Acid-Base Buffers
Data Analysis
Preparing an acidic buffer
1. What is the target pH of your acidic buffer?
2. Using M1V1 = M2V2, calculate the volume of 2.5 M sodium acetate needed to make 250 mL of
the acetic acid/acetate ion buffer that has an acetate ion concentration of 0.10 M.
3. Given the pKa of acetic acid and a concentration of 0.10 M acetate ion, what concentration of
acetic acid must be added to make a solution of your target pH?
• Tip: Use the Henderson-Hasselbalch equation found in the introduction.
4. Using M1V1 = M2V2, calculate the volume of 6 M acetic acid needed to make 250 mL of the
acetic acid/acetate ion buffer with the acetic acid concentration that you calculated in step 3.
Preparing a basic buffer
1. What is the target pH of your basic buffer?
2. What mass of sodium hydrogen carbonate was needed to make the buffer solution 0.050 M in
sodium hydrogen carbonate? Show your calculations.
3. What was the concentration of the sodium carbonate in the hydrogen carbonate ion/ carbonate
ion buffer solution? Show your calculations.
4. What mass of anhydrous sodium carbonate was required to make the 250 mL hydrogen
carbonate ion/carbonate ion buffer at that pH? Show your calculations.
5. Provide reasons as to why the measured pH level is different from the calculated value.
Generating titration curves
1. Use a spreadsheet program such as Excel to enter the volumes dispensed and corresponding
pH for each titration. Generate the following titration curves and make sure to label them all
appropriately:
a. pH vs. added volume of HCl for your acidic buffer solution.
b. pH vs. added volume of HCl for your basic buffer solution.
c. pH vs. added volume of HCl for your 0.2 M acetic acid solution.
d. pH vs. added volume of NaOH for your acidic buffer solution.
e. pH vs. added volume of NaOH for your basic buffer solution.
f. pH vs. added volume of NaOH for your 0.2 M acetic acid solution.
g. pH vs. added volume of NaOH for the acetic acid buffer/HCl mixture used in step 4 of
Part IV.
Check with your teaching assistant to see how they want the graphs turned in (i.e. by email
•
or printed copies). Make sure your name is on each graph and that you have clearly titled and
87
Acid-Base Buffers
labeled the vertical and horizontal axes. If you completed all trials, you will turn in 7 graphs
total.
Comparing buffer ranges
1. Let’s compare corresponding graphs. First, take the two graphs for the titrations of your acidic
buffer. Within your spreadsheet program, place the graph for the titration using NaOH on the
right, and the graph for the titration using HCl on the left. Select the graph on the left, and
using the formatting options, flip it horizontally. Keep the pH axis (y-axis) aligned. You should
now have a curve that looks like an “S” laying on its side. What is the pH range over which
the buffer effectively neutralizes the added acid and base and maintains a reasonably constant
pH? This is referred to as the buffer range, and is usually defined as the volume across which
the buffer is able to maintain a pH equal to the pKa ± 1.
2. Repeat this procedure for the graphs involving the basic buffer. What is the buffer range for
the basic buffer?
3. Repeat this procedure for the graphs involving the 0.2 M acetic acid solution. How do these
graphs compare to the graphs of the acidic buffer? For example, compare the slopes of the
curve of each graph at corresponding points. At corresponding pH values, compare how much
HCl or NaOH is added before ∆pH = 1.
To deepen your understanding of buffer systems, consider the following questions:
1. Considering the ranges of pH of each buffer, write an equation in terms pH and pKa that
defines buffer range.
2. Buffer capacity is defined as the amount of acid or base that can be added to a buffer before any
substantial change in pH. When is the buffer capacity at its maximum?
3. Consider the titration curve you plotted for the “Titration of a Weak Acid” experiment. How
does the titration curve compare to the graph involving the acetic acid/acetate ion buffer in this
experiment? Does the titration curve include a buffer region? If so, where is the buffer region?
If not, why not?
88
Solubility Products
Introduction
The solubility product constant, Ksp, is the equilibrium constant for a process when an ionic solid
substance dissolves into an aqueous solution at a given temperature. This experiment involves the
determination of the Ksp for calcium iodate. The calcium iodate chemical system to be analyzed is
described by the reaction
Ca(IO3)2(s) ⇌ Ca2+(aq) + 2IO3-(aq)
with a solubility product of
Ksp = [Ca2+][IO3-]2
In the first part of the experiment, you will determine the solubility of calcium iodate in pure
water. The solubility (x) of the calcium iodate will be equal to the concentration of the calcium
ion since for every mole of calcium iodate that dissolves, one mole of calcium ion forms.
Recall that the iodate ion concentration will be twice the calcium ion concentration in solution.
Thus, if you can obtain the concentration of one ion you can calculate the concentration of the
other ion. With the two concentrations, you can easily calculate the solubility product constant.
During Part I, you will determine the concentration of the iodate ion via what is known as an
iodometric titration. In this process you will add excess iodide ion to a solution that is known
to contain iodate ion in the presence of acid. The iodate reacts with the iodide by the following
reaction:
IO3-(aq) + 5I-(aq) + 6H+(aq) → 3I2(aq) + 3H2O(l)
The I2 thus produced will then react via a titration with thiosulfate by the reaction:
I2(aq) + 2S2O32-(aq) → 2I-(aq) + S4O62-(aq)
I2(aq) + I-(aq) ⇌ I3-(aq)
It should be noted that the progress of the latter reaction can be followed because the iodine
formed reacts with the excess iodide ion to form the triiodide ion, I3-. The presence of this species
is easily observed by its reaction with starch indicator to form a deep blue complex. Thus, in the
presence of starch, the endpoint of this latter titration is when the deep blue color disappears. Once
the concentration of the iodate has been determined, you can easily calculate the concentration of
the calcium ion and then the Ksp for the system.
In the second part of this experiment, you will be able to observe the “common ion effect”. In this
part of the experiment you will be given a saturated solution of calcium iodate in a 0.01 M potassium
iodate solution. Once you determine the concentration of iodate by the method described above,
you will be able to calculate the concentration of iodate from the dissolution of the calcium iodate
and thus calculate the concentration of calcium ion in solution.
89
Solubility Products
Using the concentration of the two ions, you will be able to calculate the solubility product
constant for this system. By comparing the two parts, you will note the dramatic effect that the
iodate ion from the potassium iodate has on the solubility of calcium iodate. Lastly, as part of
the data workup of this experiment, you will incorporate activity effects in the calculation of the
solubility product from your data. The correct incorporation of activity effects makes the treatment
of equilibria and equilibrium constants more rigorous.
You have discussed some of the effects of the polarity of water, including the effect that polarity
can have on the solubility of solids. It should not be surprising to find that water interacts with
various ions differently and that a more highly charged particle has a greater interaction with water
molecules. The higher the charge on an ion in solution, the greater will be the interaction of the
ion with the dipole of the water molecule and with other ions in the solution. These interactions
can be significant enough that they cannot be ignored when salt concentrations exceed hundredth
molar values.
Equilibrium constants are properly defined in terms of thermodynamic activity rather than
concentration. The thermodynamic activity is a function of concentration, but is not necessarily
equal to the concentration. However, it is true that in the limit of extremely dilute solutions,
the activity is equal to the concentration. Because the equilibrium constant expressions using
concentrations in place of activity are rigorously correct in the limit of dilute concentration, they
are conceptually parallel with the use of activities. Because the results are useful, if not exactly
correct, we commonly discuss equilibria and equilibrium constants using the concentrations. In
this experiment, however, we will recognize that the true expressions are in terms of activities.
Based on the equilibrium constant of 1.3 × 10-18 for the dissolution of mercury(I) iodate, you
would expect a saturated solution of the salt to be 6.9 × 10-7 M in mercury(I) ion.
Hg2(IO3)2(s) ⇌ Hg22+(aq) + 2IO3-(aq) K = 1.3 × 10-18 (1)
K = [Hg22+][IO3-]2 = x(2x)2
(2)
x = [Hg22+] = 6.9 × 10-7
So far, when you have determined the effect of other dissolved ions on a specific equilibrium,
you have only considered the common ion effect. Based on this reasoning, you would not predict
that potassium nitrate in solution would have any effect on the solubility of mercury(I) iodate.
However, if you were to saturate a 0.05 M potassium nitrate with mercury(I) iodate you would
find that the solubility of the mercury(I) iodate has increased by about fifty percent.
This turns out to be a general observation; any time you add an inert soluble salt to a solution of a
sparingly soluble salt you will increase the solubility of the sparingly soluble salt.
The explanation for the observed increase in solubility is that the positively charged potassium
ions can cluster around the negatively charged iodate ions, and the negatively charged nitrate ions
cluster around the positively charged mercury(I) ions. When a mercury(I) ion comes close to an
iodate ion surrounded by potassium ions, the positive charge on the potassium ions will repel
the positive charge on the mercury(I) ion, preventing it from combining with the iodate ion and
precipitating out of solution. Thus the mercury(I) iodate becomes more soluble.
90
Solubility Products
The definition of the equilibrium constant represented in equation (2) above does not take this
phenomenon into account. Instead of looking only at the concentration of a species in solution,
the activity of that species should be also examined when equilibrium is considered. The activity of
an ion includes both concentration and how susceptible the ion is to the kinds of effects described
in the preceding paragraph. To incorporate these and other effects arising from molecular and ionic
interactions in solution, we simply use the activity of the ion in place of the concentration in the
equilibrium constant expression.
The general way for incorporating activities into equilibrium constants for the general reaction
mW + nX ⇌ pY + qZ
is to form the equilibrium constant in the usual way, but employing activity in positions in the
equation where you were previously using concentration:
� �
�� ��
�� � �
�� ��
Following this procedure for our example solubility problem, equation (2) becomes:
𝐾𝐾𝐾𝐾 = 𝑎𝑎𝑎𝑎𝐻𝐻𝐻𝐻𝐻𝐻𝐻𝐻22+ + 𝑎𝑎𝑎𝑎𝐼𝐼𝐼𝐼𝐼𝐼𝐼𝐼3−2 (3)
A convenient way to quantitatively account for the molecular interaction part of the activity is to
express the activity as the product of an activity coefficient times the concentration. For example,
the mercury iodate equilibrium requires the activities
ܽுమమశ ൌ ߛுమమశ ሾ݃ܪଶଶା ሿ
ܽூைయష ൌ ߛூைయష ሾܱܫଷି ሿ
where γHg22+ and γIO3- are the activity coefficients for Hg22+ and IO3-. Substituting these expressions
into equation (3):
�
� � ������� ������ �� ������ ����� �� � ������ � ����� � ������ ������ ��
From this form, we can see that expressing the equilibrium constant using concentrations alone is
identical to assuming that the activity coefficients are equal to 1.0. This assumption is also called
the ideal solution approximation.
Because it is impossible to get a solution containing just the cation or just the anion, it is impossible
to experimentally determine γHg22+ and γIO3- individually. Instead their product is replaced by γ±,
the mean ionic activity coefficient, raised to the power equal to the sum of the exponents of the
individual ion activity coefficients.
� � ��� ������ ������ ��
Since they account for molecular and ionic interactions, the values of activity coefficients change
as the concentration of the solution changes. It has been found that a convenient quantity to use
when expressing the functional dependence of the activity coefficients of ions on concentration is
the ionic strength of the solution, which is defined by the expression:
91
Solubility Products
1
�� � �� �� � (4)
2
�
where ci is the concentration of the ith species and Zi is its signed charge in multiples of the
elementary charge, e.g. ZHg22+ = +2 and ZIO3- =−1. This sum extends over all ions in solution.
In this example, when contrasting the solubility of mercury(I) iodate in pure water and in 0.05 M
potassium nitrate, it becomes very clear that the ionic strength of the solution in pure water is
vastly different from the solution in 0.05 M potassium nitrate when we apply this definition,
�
In pure water: � � �������� � � ����� ��
�
since Hg22+ and IO3- are the only ions in solution. However, in the solution containing potassium
nitrate,
1
�� �������� � � ����� � � �� � � � ����� ���
2
Because mercury(I) iodate is so sparingly soluble, calculations will give the result that in pure
water, μ = 0.0, whereas in 0.05 M potassium nitrate, μ = 0.05.
While it is impossible to experimentally determine the values of individual ion activity coefficients,
various theoretical and empirical methods for consistently separating the observed mean ionic
activity coefficients into individual ion coefficients have been developed. These methods are by no
means perfect, but they often give much better results than the alternative very simple assumption
that the solutions are ideal. Table 1. presents results for one such method of representing individual
ion coefficients as a function of the ionic strength of the solution.
92
Solubility Products
As an example of how to use activities, here is a calculation of the concentration of calcium ion
in a 0.0125 M solution of magnesium sulfate MgSO4 saturated with calcium fluoride CaF2. The
concentration of calcium is going to depend on how much calcium fluoride dissolves, so the
chemical equilibrium and initial set-up of interest is
Initial: solid 0 0
Final: solid x 2x
� � ������ )���� � )
� ������ ����� ])����� �� � ]� )
� ������ ��])����� ���]� )
� �� � ������ ���� )
In order to look up the activity coefficients in the table, it is necessary to know the ionic strength
of the solution. The ionic strength is due to the dissolved magnesium sulfate and the dissolved
calcium fluoride. Since the equilibrium constant for the dissolution of calcium fluoride is quite
small, assume that its contribution will be negligible, as in the earlier ionic strength calculation,
and the only ions that need to be considered are the magnesium and sulfate ions. This gives an
ionic strength of 0.050 M:
1
�� ��0.0125� ⋅ 2� � �0.0125� ⋅ ��2�� � � 0.050��
2
Using this value for the ionic strength, the activity coefficients for calcium and fluoride ions are
0.485 and 0.81 respectively. Plugging into the equilibrium constant equation and solving for x
gives
�.� � 10��� � ��� ∙ 0.485 ∙ ����� ∙ 0.81�
� � ����� �
� �.1 � 10�� ��
If you had neglected the activity of the ions in solution you would have calculated the calcium ion
concentration to be 2.1 × 10-4 M. This is a thirty-two percent error.
In this experiment, you will examine the effect of activities in determining an equilibrium
constant, the solubility product. You will do a calculation similar to the example given, but you
will determine the concentrations of the species in solution, and you will use these to calculate the
solubility product both with and without including activity effects.
Your solutions are not likely to have an ionic strength exactly equal to one of those given in
the table. While more sophisticated interpolation between values in the table are possible, it is
sufficient for this experiment to simply use the tabulated value for that ionic strength that is closest
to the value you calculate for your solution of interest. If your solution has an ionic strength exactly
midway between two tabulated values, then use the value for the lower ionic strength.
93
Solubility Products
Learning Goals
The following is a list of skills that you will use in this experiment.
94
Solubility Products
Procedure
Work in pairs on this experiment.
Each student must collect data and submit a separate report. The actual data
analyses and the written reports must be done entirely independently of
your lab partner or other students. Make sure that you avoid unauthorized
collaboration and plagiarism. All suspected violations of the Code of
Academic Conduct will be referred to Student Judicial Affairs.
0.05 M Na2S2O3 solution. You should do this using the 1.0 M Na2S2O3
stock solution provided. Some calculations are required here.
95
Solubility Products
Titration Tips
• Do not use assembly line techniques when preparing flasks for
titration; prepare a flask, titrate it, and then prepare the next flask. If
you do not begin the titration immediately, iodine may crystallize out
of solution and your titration results will be inaccurate.
• Do not waste time. Only your limiting reagent needs to be measured
out with volumetric glassware. The other reagents in the iodate-to-
iodine reaction can be measured out reasonably roughly without
affecting your results.
96
Solubility Products
Make sure you read the labels on the bottles provided carefully; there are
two calcium iodate solutions, and for this part of the experiment you are
interested in the solution that has only calcium iodate dissolved in water.
2. Pour out the required amount carefully so that you do not disturb the
solid Ca(IO3)2 settled at the bottom of the bottle. You do NOT want
any of the solid Ca(IO3)2 in your Erlenmeyer flask. Pour out enough
sample in a beaker so that you can conveniently but not wastefully use
your 5.00 mL pipet to transfer the sample to an Erlenmeyer flask for the
titration.
3. Add the same amount of KI and 6 M HCl in 50 mL of DI water that
you did to standardize the thiosulfate solution, then add the 5.00 mL of
saturated Ca(IO3)2 solution for the titration.
4. When you have completed this titration, pour the solution in the
titration flask into an 800 mL beaker.
Part V. Solubility and Ksp from a Saturated Calcium Iodate
Solution in 0.010 M KIO3
1. Determine the iodate concentration in a saturated solution of calcium
iodate in 0.010 M KIO3 using standard sodium thiosulfate solution.
This saturated solution is prepared by dissolving enough potassium
iodate in water to make it 0.010 M in iodate and then saturating the
solution with calcium iodate. This solution will also be provided by the
stockroom. Again, read the label carefully; do not confuse this solution
with the saturated calcium iodate solution you used in the previous part
of this experiment.
2. Pour out the required amount carefully so that you do not disturb the
solid Ca(IO3)2 settled at the bottom of the bottle. You do NOT want
any of the solid Ca(IO3)2 in your Erlenmeyer flask. Pour out enough
sample in a beaker so that you can conveniently but not wastefully use
your 5.00 mL pipet to transfer the sample to an Erlenmeyer flask for
the titration. Add the same amount of KI and 6 M HCl in 50 mL of
DI water that you did to standardize the thiosulfate solution, then add
97
Solubility Products
Clean Up
• Pour any remaining HCl into the 800 mL beaker. Slowly and carefully
add 3 grams of sodium bicarbonate. Pour this solution down the sink
with copious amounts of water.
98
Solubility Products
Data Analysis
Standardization of Na2S2O3
1. The following equations represent two reactions that take place during the iodometric titration
and standardization of your sodium thiosulfate. The iodate from KIO3 reacts with iodide and
acid to form iodine. The iodine then reacts with the thiosulfate from Na2S2O3. Fill in the
stoichiometric values to determine the number of moles of Na2S2O3 that react in the presence
of one mole of KIO3. Make sure to balance the charge!
__ IO3-(aq) + __ I - (aq) + __ H+(aq) → __ I2(aq) + __ H2O(l)
__ I2(aq) + __ S2O32-(aq) → __ I -(aq) + __ S4O62-(aq)
2. For each of your three trials, use the volume and molarity of KIO3 to determine the number
of moles of KIO3 in solution.
3. For each of your three trials, use the number of moles of KIO3 present in solution and the
stoichiometric ratio between KIO3 and Na2S2O3 to determine the number of moles of Na2S2O3
in solution.
4. For each of your three trials, use the volume of Na2S2O3 at the equivalence point and the
number of moles of Na2S2O3 present in solution to determine the molarity of your Na2S2O3
solution.
5. What is the average molarity, standard deviation, and 90% confidence limit of the Na2S2O3
solution based on your three trials?
Calculating solubility (x) of Ca(IO3)2 in pure water
1. In your titration of saturated Ca(IO3)2 solution in pure water, what volume of standardized
Na2SO3 was required to reach the endpoint?
2. Use the volume and molarity of your standardized Na2S2O3 to determine the number of moles
of Na2S2O3 dispensed at the equivalence point.
3. Use the number of moles of Na2S2O3 at the equivalence point and the stoichiometric ratio
between Na2S2O3 and KIO3 to determine how many moles of IO3- were present in solution.
4. Use the number of moles of IO3- and the volume of saturated Ca(IO3)2 in water to calculate
the molarity of IO3-.
5. Based on the molarity of IO3- present in your sample, what is the solubility (x) of Ca(IO3)2 in
pure water?
• Tip: the solubility (x) of calcium iodate will be equal to the concentration of the calcium
ion since for every mole of Ca(IO3)2 that dissolves, one mole of Ca2+ forms. It may help
to set up an ICE table detailing the dissociation of Ca(IO3)2 in water to see how the
concentration of IO3- and Ca2+ are related.
99
Solubility Products
100
Solubility Products
2. Use the volume and molarity of your standardized Na2S2O3 to determine the number of moles
of Na2S2O3 dispensed at the equivalence point.
3. Use the number of moles of Na2S2O3 at the equivalence point and the stoichiometric ratio
between Na2S2O3 and KIO3 to determine how many moles of IO3- were present in solution.
• Tip: the moles of IO3- present in this solution are from both the dissociation of Ca(IO3)2
and the dissociation of 0.01 M KIO3.
4. Use the number of moles of IO3- and the volume of saturated Ca(IO3)2 in 0.01 M KIO3 to
calculate the molarity of IO3-.
5. Based on the molarity of IO3- present in your sample, what is the solubility (x) of Ca(IO3)2 in
0.01 M KIO3?
• Tip: you must take into account the fact that 0.01 M of the total IO3- concentration comes
from the dissociation of 0.01 M KIO3. This means that the total concentration of IO3- you
calculated above is equal to 0.01M + 2x.
Calculating solubility product (Ksp) of Ca(IO3)2 in 0.01 M KIO3 based on
concentration
1. Write an equation that describes the solubility product, Ksp, of Ca(IO3)2 in pure water in terms
of the concentration of Ca2+ and IO3-.
2. Re-write this equation by substituting solubility (x) of Ca(IO3)2 in for the concentrations of
Ca2+ and IO3-. Your equation should now be written in terms of x.
• Tip: you must take into account the fact that 0.01 M of the total IO3- concentration comes
from the dissociation of 0.01 M KIO3. This means that the total concentration of IO3- is
equal to 0.01M + 2x.
3. Use the solubility (x) of Ca(IO3)2 that you determined in step 5 of "Calculating solubility (x)
of Ca(IO3)2 in 0.01 M KIO3" to solve for the solubility product, Ksp, of Ca(IO3)2.
Calculating solubility product (Ksp) of Ca(IO3)2 in 0.01 M KIO3 based on activity
1. Use equation (4) from the Introduction to write out an equation calculating the ionic strength
(μ) of Ca(IO3)2 in 0.01 M KIO3 using the concentration (ci) and charge (Zi) of each ion,
including K +.
2. Re-write this equation by substituting solubility (x) of Ca(IO3)2 in for the concentrations of
Ca2+, IO3-, and 0.01 M for the concentration of K+. Your equation should now be written in
terms of x.
• Tip: you must take into account the fact that 0.01 M of the total IO3- concentration comes
from the dissociation of 0.01 M KIO3. This means that the total concentration of IO3- is
equal to 0.01M + 2x.
3. Use the solubility (x) of Ca(IO3)2 you calculated in step 5 of "Calculating solubility (x) of
Ca(IO3)2 in 0.01 M KIO3" to solve for the ionic strength (μ) of Ca(IO3)2 in 0.01 M KIO3.
101
Solubility Products
4. Use Table 1 in the Introduction and your calculated ionic strength (μ) to find the activity
coefficients (γ) for Ca2+ and IO3-.
5. Write an equation that describes the solubility product, Ksp, of Ca(IO3)2 in 0.01 M KIO3 in
terms of both the concentration and activity coefficients (γ) of Ca2+ and IO3-.
6. Re-write this equation by substituting solubility (x) of Ca(IO3)2 in for the concentrations of
Ca2+ and IO3-. Your equation should now be written in terms of x and γ.
• Tip: you must take into account the fact that 0.01 M of the total IO3- concentration comes
from the dissociation of 0.01 M KIO3. This means that the total concentration of IO3- is
equal to 0.01M + 2x.
7. Use the solubility (x) of Ca(IO3)2 and activity coefficients (γ) of Ca2+ and IO3- that you
determined previously to solve for the solubility product, Ksp, of Ca(IO3)2 in 0.01 M KIO3.
102
Chem 2 Series
Laboratory
Procedures
and Safety
Handbook
you will be deemed unsafe to perform the experiment and must leave the laboratory until the
pre-laboratory write up is complete and your TA is convinced that you are prepared to begin
the experiment.
2. Data Collection
All data must be recorded in blue or black ink directly into your laboratory notebook. At the
•
completion of the experiment, you must turn in a copy of your data sheet to your TA before
you leave the laboratory.
3. Unknowns
Students will obtain all unknowns from the TA. Students must be explicit in their request for
•
an unknown; that is, they must know the name of the experiment and unknown. If a student
needs more unknown, they should notify the TA who will then write a note of explanation
that the student can take to the dispensary. The note should contain the student’s name, the
student’s locker number, the laboratory section number, the TA’s name, the experiment name,
and the name of the unknown.
written in your laboratory notebook and others will be submitted on-line as part of the post
laboratory exercises. Post laboratory exercises are due one week after the completion of the
laboratory.
•
A-5
General Experimental Guidelines
Below is a general outline of a common format that is often used in science laboratory courses.
•
Discuss this format with your TA during the first laboratory period so that you clearly understand
what will be expected. All reports must be written in non-erasable blue or black ink. A date
should be indicated on each report. Your notebook should be organized and written in such a
manner that another chemist could read it and repeat the experiment in precisely the same way.
• Title: The report should have a title that concisely describes the experiment.
• Purpose: A brief and concise statement that describes the goals of the experiment and
the methods employed. Any pertinent chemical reactions are generally indicated. State
the purpose of the experiment in the form of a complete sentence. Do not start with the
word “To.”
• Procedure: A brief and concise outline of each step of the experiment should be
included. If you are using a published procedure, you should also cite the literature or
laboratory manual. A drawing of the apparatus may also be included.
• Data and Observations: Report all measurements and observations that are pertinent
to the experiment. Be sure to note any problems or unexpected occurrences. It is
important that this section be as neat and as organized as possible. The use of tables
will often help in this regard. All data must be recorded in blue or black ink directly into
the notebook at the time it is collected. A severe penalty will be imposed for pencil or
transcribed data entries. Do not erase mistakes. Simply draw a line through the error and
record the correction. Your notebook is subject to examination at any time.
The following sections are to be submitted on-line as part of the post-laboratory exercise. You
•
should complete the post-lab report as soon as possible after the completion of the experiment
as this is much more efficient than waiting until the night before the experiment is due.
• Calculations: This section generally includes any complicated calculations that are
involved in the experiment. Again, it is important to use foresight when organizing this
section.
A-6
Laboratory Work Grading Policies
A-7
Late Reports & Make-Up Policy
completion of the experiment. The last report each quarter is due at the time indicated by the
TA. Late reports will be met with a 5-point deduction for every calendar day the report is late.
a laboratory class with an excused absence, it must be made up before the end of the
following week of laboratory. No laboratory make-ups will be offered after one week
from the scheduled date of the lab. If you miss the last lab of the quarter, it must be made up
immediately. No make ups for unexcused absences.
Excused absences include an extended illness, accidents, or family emergencies. Vacation,
•
cruises, and IM sports are not considered excused. Bring documented proof of your
excused absence to your TA or head TA immediately upon return. If you cannot present this
documentation or have an unexcused absence, you may receive a failing grade in the course.
You are required to complete all labs in order to pass the course and it is your responsibility to
•
find an open laboratory in the same course promptly. Failure to make up a lab may result in a
failing grade for the course.
your responsibility to find an open laboratory in the same course. Consult the Class Schedule
and Room Directory for a listing of rooms and times. Go to the selected laboratory section
and ask the teaching assistant if you may be admitted to make up a lab. You must be on time
for the start of the lab period. If there is room in the class, the teaching assistant will allow you
in the lab, unlock your locker, and allow you to do the lab. Make sure to record the teaching
assistant’s name, date, time and room number where you made up the laboratory. Have the
TA collect your data sheet and he or she will give it to your regularly assigned teaching assistant.
No laboratory report will be accepted without a valid copy of the data sheet.
data and its analysis and interpretation with your lab partner, other students and the TAs.
However, the actual data analyses and the written reports must be done entirely independently
of your lab partner or other students. Make sure that you avoid unauthorized collaboration
and plagiarism. All suspected violations of the Code of Academic Conduct will be referred to
Student Judicial Affairs.
A-8
Chemistry Department Safety Policy
A-9
Chemistry Department Safety Policy
12. Skateboards, rollerblades, and other such personal equipment must be stored outside of the
laboratory. Personal electronics are only permitted when needed for the laboratory. Because
cell phones or other personal electronic media can easily be damaged or contaminated in the
laboratory, use of such devices is at the student’s own risk.
13. Learn the location and how to operate the nearest eyewash fountain, safety shower,
fire extinguisher, and fire alarm box. Basic first aid for any chemical splash is to wash the
affected area for at least 15 minutes and seek medical attention. Use the emergency shower if
appropriate, removing contaminated clothing for thorough washing. If the safety shower or
eyewash is activated, the exposed person should be accompanied to the Student Health Center
for further evaluation.
14. Laboratory doors must remain closed except when individuals are actively entering or
exiting the lab.
15. The student must have at least one ungloved hand when outside the laboratory. Gloves
are presumed to be contaminated and must not come into contact with anything outside the
laboratory except chemical containers. Only use the ungloved hand to open doors, hold on to
stair rails, or push elevator buttons.
16. All activities in which toxic gases or vapors are used or produced must be carried out in
the fume hood.
17. Mouth suction must never be used to fill pipets.
18. Containers of chemicals may not be taken out of the laboratory except to the dispensary
for refill/replacement or to exchange full waste jugs for empty ones. All containers must
be closed with the appropriate cap before you take them into the hallway to the dispensary.
Always use a bottle carrier when transporting chemicals and waste.
19. Put all hazardous waste into the appropriate waste container(s) provided in your laboratory.
Do not overfill waste containers.
20. All incidents, near misses, injuries, explosions, or fires must be reported at once to the LI.
In case of serious injury or fire (even if the fire is out), the LI or Lab Supervisor must call 911.
The student must always be accompanied to the Student Health Center.
21. Keep your working area clean – immediately clean up ALL spills or broken glassware.
Dispose sharps in the appropriate container. Do not dispose pipette tips in regular trash.
Clean off your lab workbench before leaving the laboratory.
You must sign the Safety Acknowledgement sheet before you may work in the lab. If you have
questions about these rules and procedures, please ask your LI before starting any laboratory
work in this course.
A-10
Safety in the Chemistry 2 Laboratories
2. Follow Instructions
The Chemistry 2 laboratory is designed to minimize the hazard exposure to students. Failure to
follow the lab manual instructions may result in accidents and injuries to you and others around
you.
Always follow the manual unless directly instructed by your Laboratory Instructor or the teaching
lab staff.
Follow all instructions posted in the laboratory.
3. Safety Equipment
There are many safety types of equipment in the Chemistry 2 laboratory. Learn where they are and
how to operate them.
• Exits
The ability to remove yourself from a dangerous situation is one of the most important
safety skills you have.
Keep the exits clear. Do not block exits with backpacks, skateboards, bicycles, etc.
Keep the doors closed. Do not prop the door open.
• Fire Extinguisher
Learn the location of the fire extinguisher. It is usually placed next to an exit.
A-11
Safety in the Chemistry 2 Laboratories
• Eyewash
Learn the location of the eyewash. For chemical spills in your eyes, use the Eyewash
fountain. Hold your eyelids open and wash affected area water for 15 minutes with water.
Seek medical attention.
• Drenching Hose and Safety Shower
Learn the location of the drench hose and safety shower.
For large spills on your body, use the safety shower.
• Remove contaminated clothing and wash affected area with water. Seek medical
attention immediately.
• When the safety shower is used, all other students must evacuate the room.
The TA must dial 911 and inform the Fire Department that the safety shower is used.
For small chemical spills on your arms and hands, use the drench hose.
• Wash affected area water for 15 minutes with water and contact your TA. You may
also use the tap water faucet if it is adequate for washing the affected area. It is advised
that you seek medical attention for even minor burns.
• Fire Alarm Box
The fire alarm boxes in the Science Lab building are located in the hallway.
A-12
Safety in the Chemistry 2 Laboratories
of liquids. For the Chemistry 2 laboratories, students are required to have long sleeves, long
pants, and shoes that cover the entirety of the foot.
• Long sleeve shirt and long pants:
You must wear clothing that covers your arms, legs, wrists and ankles to protect you from
small spills. Long skirts, tights or leggings do not qualify. Do not wear clothing with holes
in them as they will not protect you from spills.
• Shoes that cover the entirety of the foot and socks to cover the ankles:
You must wear closed-toe, closed-heeled shoes that completely cover your foot. Do not wear
sandals, slippers, or shoes that expose the back of your foot. Broken glassware and spilled
chemicals are more likely to land on your foot than anywhere else. Also remember to wear
socks to cover your ankles. The area between your shoes and pants should not be exposed
when you are seated.
A good rule of thumb to keep in mind is: No skin exposure from the neck down to the
feet in the laboratory.
2. Goggles
Lab goggles are designed to protect your eyes. Injury to the eyes is often irreversible and may
•
severely impact your future. Always wear approved goggles when working in the laboratory.
• Approved Goggles
ANSI Z87.1-compliant chemical splash goggles with indirect venting is required for the
Chemistry 2 course. Approved lab goggles may be purchased at the MU Bookstore, the Silo
Bookstore or the ARC Pro Shop in the Activity and Recreation Center.
A-13
Safety in the Chemistry 2 Laboratories
• Goggles Rules
Modified goggles will not be allowed in the lab. Do not modify the goggles by adjusting or
removing the indirect venting system.
Goggles strap must be adjusted to fit properly at all times.
Never take off your goggles in the laboratory. If you need to adjust your goggles or if they
fog up, leave the laboratory and return when your goggles issues are resolved.
3. Lab Coat
You must provide your own lab coat for all chemistry lab courses. Only wear lab coats during
•
the laboratory. Take off your lab coat immediately after lab. Do not wear lab coat outside the
laboratory.
•Your lab coat must be made of 100% cotton. Disposable, synthetic lab coats are not acceptable.
Your lab coat must be properly fitted so that it protects your arms and body. The sleeves of your
•
lab coat must fully extent to the wrists. Do not wear a lab coat that that’s too small or too big
for you.
•Keep your lab coat buttoned at all times.
4. Gloves
You will be provided with disposable nitrile gloves in lab for you protection. Do not bring your
•
own gloves.
Wear gloves when handling hazardous chemicals or contacting potentially contaminated
•
surfaces.
•Never re-use disposable gloves. Remove and replace contaminated nitrile gloves immediately.
• Allergy
If you are allergic to nitrile gloves, contact your TA and the laboratory staff. You will be
provided with hypoallergenic lab gloves.
• Fit
Make sure you wear the correct sized gloves. Gloves that are too large for your hand greatly
increase the likelihood of accidents.
A-14
Maps and Emergency Evacuation Procedures
possible. Remember that you may not be allowed back into the building for an extended time.
3. Assembly Area
After exiting the building, all occupants should follow the evacuation route to the pre-arranged
•
assembly area.
DO NOT return to the building until notified by emergency personnel. Supervisors must take
•
A-15
Maps and Emergency Evacuation Procedures
A-16
Maps and Emergency Evacuation Procedures
A-17
Maps and Emergency Evacuation Procedures
A-18
General Emergency Procedures
A-19
Dispensary Procedures
Dispensary Procedures
1. Dispensary Location and Policies
The CHE2 dispensary is located on the first floor of the SLB in Room 1060. Go to the dispensary
roll-up window (1060E) for service.
You must wear the proper PPE to the dispensary. This includes your lab coat and goggles.
Remember that you should have at least one ungloved hand while outside your laboratory.
2. Dispensing Policies
a.) Policies at the Beginning of the Quarter
Goggles and Lab Coat: You are required to provide your own goggles and lab coats.
Locker Supplies: It is required that you do a locker inventory during the first week of labs.
Make sure that you have everything on your locker list by the end of the second week of
instruction.
b.) Policies During the Quarter
Locker Supplies: If a locker item is broken after the initial two-week period, go to the
dispensary to request a replacement. You must know the exact name and specification of the
item to be replaced.
Refilling of Chemical and Supply Containers: When replacing or refilling general
laboratory chemicals or supplies, be sure to bring the empty containers to the dispensary.
Be sure all containers are closed with the correct cap and placed in the correct bottle carrier.
To avoid chemical contamination and equipment breakage, please refrain from bringing
personal bags and backpacks to dispensary window when seeking replacement chemical
containers or lab equipment.
Waste Containers: Call the dispensary for replacements when waste containers are full.
c.) Policies at the End of the Quarter
Surplus Stores: Any item you may have in surplus should be placed in the area set aside for
surplus items in the laboratory (a box at the back of the lab).
Filling Locker Requirements: If your locker is short of any items when you are checking
your locker equipment against your locker list, obtain the missing items from the surplus
items in the laboratory. If the missing item is not in the surplus area, obtain it from the
dispensary.
Preparing Your Locker for Check-Out: Clean and quickly dry all equipment. Replace
all broken or missing items by checking them out from the dispensary. Return all extra
equipment to the extra glassware box in the lab. Have your TA check the contents of the
locker and if everything is present and clean then they will lock the drawer.
A-20
Safety Data Sheet
A-21
SAFETY DATA SHEET
Creation Date 24-Aug-2009 Revision Date 24-Feb-2014 Revision Number 1
1. Identification
Product Name Hydrochloric Acid Solution, 6N (Certified)
2. Hazard(s) identification
Classification
This chemical is considered hazardous by the 2012 OSHA Hazard Communication Standard (29 CFR 1910.1200)
Label Elements
Signal Word
Danger
Hazard Statements
May be corrosive to metals
Causes severe skin burns and eye damage
May cause respiratory irritation
______________________________________________________________________________________________
Page 1 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Precautionary Statements
Prevention
Do not breathe dust/fume/gas/mist/vapors/spray
Wash face, hands and any exposed skin thoroughly after handling
Wear protective gloves/protective clothing/eye protection/face protection
Use only outdoors or in a well-ventilated area
Keep only in original container
Response
Immediately call a POISON CENTER or doctor/physician
Inhalation
IF INHALED: Remove victim to fresh air and keep at rest in a position comfortable for breathing
Skin
IF ON SKIN (or hair): Take off immediately all contaminated clothing. Rinse skin with water/shower
Wash contaminated clothing before reuse
Eyes
IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing
Ingestion
IF SWALLOWED: Rinse mouth. DO NOT induce vomiting
Spills
Absorb spillage to prevent material damage
Storage
Store locked up
Store in a well-ventilated place. Keep container tightly closed
Store in corrosive resistant polypropylene container with a resistant inliner
Store in a dry place
Disposal
Dispose of contents/container to an approved waste disposal plant
Hazards not otherwise classified (HNOC)
None identified
4. First-aid measures
General Advice If symptoms persist, call a physician.
Eye Contact Rinse immediately with plenty of water, also under the eyelids, for at least 15 minutes.
Immediate medical attention is required.
Skin Contact Wash off immediately with plenty of water for at least 15 minutes. Immediate medical
attention is required.
Inhalation Move to fresh air. If breathing is difficult, give oxygen. Do not use mouth-to-mouth method if
victim ingested or inhaled the substance; give artificial respiration with the aid of a pocket
mask equipped with a one-way valve or other proper respiratory medical device. Immediate
______________________________________________________________________________________________
Page 2 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Ingestion Do not induce vomiting. Call a physician or Poison Control Center immediately.
Most important symptoms/effects Causes burns by all exposure routes. Product is a corrosive material. Use of gastric
lavage or emesis is contraindicated. Possible perforation of stomach or esophagus should
be investigated: Ingestion causes severe swelling, severe damage to the delicate tissue
and danger of perforation
Notes to Physician Treat symptomatically
5. Fire-fighting measures
Suitable Extinguishing Media Substance is nonflammable; use agent most appropriate to extinguish surrounding fire.
NFPA
Health Flammability Instability Physical hazards
3 0 1 N/A
Methods for Containment and Clean Soak up with inert absorbent material. Keep in suitable, closed containers for disposal.
Up
Storage Keep containers tightly closed in a dry, cool and well-ventilated place.
______________________________________________________________________________________________
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Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Engineering Measures Use only under a chemical fume hood. Ensure that eyewash stations and safety showers
are close to the workstation location.
Eye/face Protection Wear appropriate protective eyeglasses or chemical safety goggles as described by
OSHA's eye and face protection regulations in 29 CFR 1910.133 or European Standard
EN166.
Skin and body protection Wear appropriate protective gloves and clothing to prevent skin exposure.
Respiratory Protection Follow the OSHA respirator regulations found in 29 CFR 1910.134 or European Standard
EN 149. Use a NIOSH/MSHA or European Standard EN 149 approved respirator if
exposure limits are exceeded or if irritation or other symptoms are experienced.
Hygiene Measures Handle in accordance with good industrial hygiene and safety practice.
______________________________________________________________________________________________
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Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Conditions to Avoid Incompatible products. Excess heat. Exposure to moist air or water.
Incompatible Materials Metals, Oxidizing agents, Reducing agents, Acids, Bases, Aldehydes
Hazardous Decomposition Products Hydrogen chloride gas, Carbon monoxide (CO), Carbon dioxide (CO2), Hydrogen
Hazardous Reactions May react with metals and lead to the formation of flammable hydrogen gas. Corrosive to
metals.
Product Information
Oral LD50 Based on ATE data, the classification criteria are not met. ATE > 2000 mg/kg.
Dermal LD50 Based on ATE data, the classification criteria are not met. ATE > 2000 mg/kg.
Vapor LC50 Based on ATE data, the classification criteria are not met. ATE > 20 mg/l.
Component Information
Component LD50 Oral LD50 Dermal LC50 Inhalation
Water - Not listed Not listed
Hydrochloric acid LD50 238 - 277 mg/kg ( Rat ) LD50 > 5010 mg/kg ( Rabbit ) LC50 = 1.68 mg/L ( Rat ) 1 h
Carcinogenicity The table below indicates whether each agency has listed any ingredient as a carcinogen.
Symptoms / effects,both acute and Product is a corrosive material. Use of gastric lavage or emesis is contraindicated.
delayed Possible perforation of stomach or esophagus should be investigated: Ingestion causes
severe swelling, severe damage to the delicate tissue and danger of perforation
Endocrine Disruptor Information No information available
Other Adverse Effects The toxicological properties have not been fully investigated.
______________________________________________________________________________________________
Page 5 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Component TSCA DSL NDSL EINECS ELINCS NLP PICCS ENCS AICS IECSC KECL
Water X X - 231-791-2 - X - X X X
Hydrochloric acid X X - 231-595-7 - X X X X X
Legend:
X - Listed
E - Indicates a substance that is the subject of a Section 5(e) Consent order under TSCA.
F - Indicates a substance that is the subject of a Section 5(f) Rule under TSCA.
N - Indicates a polymeric substance containing no free-radical initiator in its inventory name but is considered to cover the designated
polymer made with any free-radical initiator regardless of the amount used.
P - Indicates a commenced PMN substance
R - Indicates a substance that is the subject of a Section 6 risk management rule under TSCA.
S - Indicates a substance that is identified in a proposed or final Significant New Use Rule
T - Indicates a substance that is the subject of a Section 4 test rule under TSCA.
XU - Indicates a substance exempt from reporting under the Inventory Update Rule, i.e. Partial Updating of the TSCA Inventory Data Base
Production and Site Reports (40 CFR 710(B).
Y1 - Indicates an exempt polymer that has a number-average molecular weight of 1,000 or greater.
Y2 - Indicates an exempt polymer that is a polyester and is made only from reactants included in a specified list of low concern reactants
that comprises one of the eligibility criteria for the exemption rule.
______________________________________________________________________________________________
Page 6 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
SARA 313
Component CAS-No Weight % SARA 313 - Threshold
Values %
Hydrochloric acid 7647-01-0 22 1.0
______________________________________________________________________________________________
Page 7 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________
Canada
This product has been classified in accordance with the hazard criteria of the Controlled Products Regulations (CPR) and
the MSDS contains all the information required by the CPR
End of SDS
______________________________________________________________________________________________
Page 8 / 8
Hazardous Chemicals
Hazardous Chemicals
Hazardous Chemicals
The laboratory is a chemical use area for potentially hazardous compounds. The following are the
hazard classes of chemicals used in this course and for which this laboratory is designated as a use
area:
1. Carcinogens
2. Corrosives
3. Flammable and combustible solids and liquids
4. Reproductive Toxins
A-30
Hazardous Chemicals
Hazardous Waste
Cation Metal Waste: Label is WHITE and is used in all CHEM 2 courses.
HAZARDOUS WASTE
Chem 2 Experiment
Cation Metal Waste
Follow these instructions:
Ø Cap lid when not in use
Ø Leave in fume hood
Ø Call Dispensary when full
ONLY
Cobalt, Copper, Iron, Lead,
Manganese, Silver, Zinc,
DANGER
A-31
Hazardous Chemicals
Dithizone in Chloroform Waste: Label is BLUE and is used only in CHEM 2C.
WASTE ONLY
DO NOT LEAVE BOTTLE UNCAPPED DO
-Flammable-
Toxic
A-32
Statistical Treatment of Data
∑ 𝑥𝑥�
𝑥𝑥̅ �
𝑛𝑛
∑��� � �̅ ��
���
��1
The smaller the value of s, the more closely packed the data is about the mean—or, in other words,
the measurements are more precise.
A-33
Statistical Treatment of Data
2. Confidence Limits
In general chemistry with a relatively small number of trials, we use a t-distribution (also called
Student t-distribution) for a population mean estimation.
The t-statistic is determined by
𝑥𝑥 � �
�� 𝑠𝑠
√𝑛𝑛
where 𝑥𝑥̅ is the sample mean, 𝜇𝜇 is the population mean, s is the standard deviation, and n is the
sample size. The t-statistic distribution is called the t-distribution. The t-distribution approximates
the normal distribution curve as the sample size increases (n).
The particular t-distribution is determined by the number of degrees of freedom. For the purposes
of estimating the mean from a sample in the general chemistry experiments, the degree of freedom
is calculated as the number of independent trials minus one. Then, the t-distribution determined
by the specified n - 1 degrees of freedom represents the sample mean distribution with respect to
the true mean divided by 𝑠𝑠 . Using this information, an experimenter can formulate a confidence
√𝑛𝑛
limit for that mean.
Confidence limits provide an indication of data precision. For example, a 90% confidence limit of
±2.0 indicates that there is a 90% probability that the true average of an infinite collection of data
is within ±2.0 of the calculated average of a limited collection. Clearly, the more precise a set of
data, the smaller the confidence interval. Thus, a small confidence interval is always the goal of any
experiment. In General Chemistry, you will be required to calculate the 90% confidence interval
for all experimental collections of data. The formula to do this is:
𝑠𝑠
𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶𝐶 �𝐶𝐶�𝐶𝐶� � ���������� � � �
√𝑛𝑛
where s is the standard deviation, n is the number of trials, and tcritical is the critical value in a t-
distribution table in statistics. A small section of the t-distribution table is shown at the end of
this section. For the calculation of 90% confidence limits in General Chemistry, please use the
following values:
You should always report your result as the average ± the 90% confidence limit.
A-34
Statistical Treatment of Data
t-distribution table
Confidence level
90% 95% 99%
n
2 6.314 12.71 63.66
3. Relative Deviation
The relative average deviation, d, like the standard deviation, is useful to determine how data are
clustered about a mean. The advantage of a relative deviation is that it incorporates the relative
numerical magnitude of the average.
The relative average deviation, d, is calculated in the following way.
a.) Calculate the average, 𝑥𝑥̅ , with all data that are of high quality.
b.) Calculate the deviation, |𝑥𝑥� � 𝑥𝑥|, of each good piece of data.
c.) Calculate the average of these deviations.
d.) Divide that average of the deviations by the mean of the good data.
This number is generally expressed as parts per thousand (ppt). You can do this by simply
multiplying by 1000.
Please report the relative average deviation (ppt) in addition to the standard deviation in all
experiments.
A-35
Statistical Treatment of Data
and compare the value to that given in the table below. The values in the table below are given for
the 90% confidence level. If the QData is greater than the QCritical then the data can be discarded with
90% confidence (the value has a less than 10% chance of being valid).
4 0.76
5 0.64
6 0.56
While the Q test is very popular, it is not always useful for the small samples you will have (you
will generally only do triplicate trials).
Keep in mind that you also always have the right to discard a piece of data that you are sure is of
low quality. That is, when you are aware of a poor collection. However, beware of discarding data
that do not meet the Q test. You may be discarding your most accurate determination!
A-36
An Introduction to Excel
An Introduction to Excel
In chemistry, as well as in other analytical sciences, it is important to not only know how to collect
quality data, but also know how to analyze and manipulate that data to investigate your hypothesis.
A spreadsheet program, such as Microsoft Excel, is an especially helpful tool to use for viewing and
manipulating data, as it can be used to quickly perform complex calculations on large sets of data,
as well as to rearrange raw data into easy to understand graphical representations.
In this guide, you will learn how to create a basic spreadsheet in Excel, and use formulas to quickly
perform calculations on your data. You will also learn how to make graphs for your post-lab reports.
This guide uses Microsoft Excel 2016, which is available as a free download for students via:
▶ http://officedownload.ucdavis.edu
The above link can be accessed by logging in with your campus Kerberos (CAS) account. If you do
not wish to download Microsoft Office onto your personal computer, Excel is also available for use
at all of the computer labs on campus.
Figure 1. Use your UC Davis login information to access Microsoft Office 365.
<Your Name>
Figure 2. You can install Microsoft Office 2016 by clicking on the “Install Office 2016” button once you’ve
logged in.
A-37
An Introduction to Excel
Excel Basics
1. Open a new spreadsheet in Excel 2016. The image below shows a section of the blank worksheet.
Ribbon Menu
Formula bar
Cell reference
Columns
Active cell
Rows
Cells
you are currently typing in, has a green outline around it with a handle at the bottom right.
Each cell has its own cell reference that consists of the letter of the column and the number
•
of the row it is currently in. The cell reference is analogous to a variable in algebra, where the
reference refers to the data inside of the cell. In the image above, the cell reference of the active
cell is A1.
The formula bar displays the formulas in the active cell. If there are no formulas in the active
•
spreadsheet. In this guide, we will mainly be using the Home and Insert menus to edit our
spreadsheet.
2. For this section of the guide, we will use sample data from the 2A experiment, Volumetric
Analysis.
Enter the data in columns, using one cell for each data point. Make sure all the data points
•
a header row is not required for the program to create graphs or perform calculations.
As you can see in the image below, each row represents a separate trial for the experiment.
•
Column B shows the mass of KHP used, and column C shows the volume of NaOH needed
to reach the endpoint.
A-38
An Introduction to Excel
make it the active cell. Hold the Shift key down and click on the bottom-most cell containing
data to select the rest of the data points. The green outline will expand around the entire
selected area.
Hover your mouse cursor over the handle at the bottom right of the active area. The cursor will
•
change into a small plus sign (+). Left-click and drag the handle down to another cell in the
column to expand the green outline to that cell. A small hover box near the cursor also shows
the value that cell will have once the series is expanded.
Let go of the mouse button to fill the selected area with the expanded series. In the following
•
image, notice how the series can be expanded from just two initial values.
A-39
An Introduction to Excel
4. We may also want to change how many decimal places are displayed in each column or row,
depending on what the experiment requires.
To add or remove decimal places, select an area and right click anywhere in that area. Select
•
Format Cells... from the context menu to bring up the Format Cells window.
A-40
An Introduction to Excel
The default category for a cell is General. Change the category to Number and set the number
•
you will still need to remember the rules for rounding significant figures in order to determine
the number of decimal places to use.
A-41
An Introduction to Excel
Calculations in Excel
5. Now that we’ve entered our raw data, we can use Excel to quickly perform calculations with
that data using formulas.
Excel formulas always start with an equal sign (=). Formulas can use one or more operators or
•
functions, and can contain a mix of constants and cell references. Note that Excel formulas using
math operators follow the mathematical order of operations.
Functions are a type of procedure you can perform in Excel, denoted with an equal sign (=),
•
a function name, such as SUM or AVERAGE, and a set of parentheses containing one or
more parameters separated by commas. There are many different functions in Excel, and you
can press the ƒx button next to the Formula bar to view the full list. However, in the Chem 2
course, you will most likely only need to use use the mathematical functions listed below.
In the Volumetric Analysis experiment, we perform multiple titrations of KHP with NaOH to
•
determine the molarity of an NaOH solution. We use the following stoichiometric equation to
calculate the molarity of NaOH:
We can type this equation as an Excel formula using cell references to refer to the data we
•
entered earlier. In this example, the mass of KHP is recorded in column B, and the volume of
NaOH added is recorded in column C.
Move to the next blank column in the spreadsheet and give it an appropriate header, such
•
as [NaOH] (M). In the row corresponding to the first trial, type out the formula using cell
references to the data points from that trial. Trial 1 is recorded in row 2, so we refer to cells B2
and C2 in the formula.
Be careful to follow the order of operations and use parentheses to group operations together if
•
needed. Excel will highlight each cell being referenced in a different color, which you can use
as a visual guide to double check that you are referring to the correct cells.
A-42
An Introduction to Excel
the cell to show the formula again if you wish to make any edits.
Now, we can expand that formula to apply to the other rows in the spreadsheet. Click and drag
•
Figure 9. Click and drag the handle down to the last row of data.
Excel will automatically perform the calculation for every row in the selected area. Note how
•
the cell references are updated for row 4 in the picture below.
Figure 10. The formula bar showing the updated cell references.
When you have a large number of trials and you need to use multiple steps in your calculation,
•
it may be easier to do your calculations in Excel rather than on a calculator, because you only
need to enter the calculation once.
A-43
An Introduction to Excel
6. Now, we can use functions in other cells to find the average, standard deviation, and so on. The
image below shows the average for each of the 3 columns, again starting from cell B6 and using
the fill handle to expand the formula across the 3 columns in row 6.
Figure 11. The formula bar shows the formula used to calculate the value in the cell.
A-44
An Introduction to Excel
Graphing in Excel
7. Excel is also useful for making graphical representations of data. Graphs are an extremely
valuable tool in data analysis, because they depict the relationships between data points in a
format that is easy to view at a glance.
For this section of the guide, we will use the sample data found at the end of the Strong Acid -
•
holding down shift, click on the bottom rightmost cell containing data to select the entire field
of data. Then, go to the Insert tab of the ribbon menu to find the graphing options.
Figure 12. After selecting the data range, go to Insert > Scatter to plot the points on a graph.
There are a variety of different graph types you can create in Excel. In General Chemistry, we
•
points on an xy-axis. This inserts a basic scatter graph into your spreadsheet, but we will want
to edit the graph to add more information, such as axes labels or connecting lines.
8. First, let’s add some lines to connect the data points and create the titration curve.
You can open up the options menu for the data points by right clicking on any one of the
•
points and clicking on Format Data Series from the context menu. A menu will pop up on
the right side of the screen.
A-45
An Introduction to Excel
Figure 13. Select Format Data Series from the context menu to access more options.
In the Format Data Series menu, there are options to edit the Line and Marker appearances.
•
You may have to click on the menu text to reveal all of the options.
•To add lines between the points, click on the bubble next to Solid line.
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An Introduction to Excel
9. Next, we want to add descriptive labels to the x- and y- axes so others viewing the graph can
understand what each axis represents. Select any part of the graph and click on the + button to
insert chart elements. Check the box next to Axis Titles to insert text fields you can edit next
to the x- and y- axes.
axis titles, and don’t forget to give your graph a descriptive title as well.
Figure 16. The titration curve with a title and axis labels added.
A-47
An Introduction to Excel
10. Finally, we can optionally change the range of each axis to minimize the amount of empty
space on the graph. Right click on either axis and click on Format Axis to bring up the Format
Axis options menu. Here, you can change the bounds on the axis to your liking.
On this graph, there are no data points between 0 and 5, and 30 and 35 on the x-axis, so we
•
will change the bounds to 5 and 30. The graph will automatically change to fit the new bounds.
Figure 17. Changing the minimum and maximum bounds of the x-axis.
A-48
Common Laboratory Procedures
A-49
Common Laboratory Procedures
Notice
• Always keep the desiccator upright and closed in your locker.
• Clean up Calcium Chloride spill immediately. Moisture will damage drawers.
A-50
Common Laboratory Procedures
Handling Liquids
1. Drawing Solutions from a Reagent Bottle
Most reagent bottles in your laboratory have a small test tube holder attached for a disposable
(dispo) plastic pipette. To avoid cross-contamination, always use the assigned dispo pipette to draw
solutions from the reagent bottle. Do not use your glass pipet with reagent bottles.
Caution
• Improper use of disposable pipets may cause serious injuries!
• Never point the pipet at yourself or others!
• Do not squeeze air into solutions with the dispo pipet. This may result in chemical splashes.
• Always put full dispo pipet in a test tube when carrying it to another part of the lab.
0.25 mL
1
1 mL
A-51
Common Laboratory Procedures
3. Transferring Liquid
a. When transferring liquids from a reagent bottle, always remove the cap/stopper and hold
it in your hand. Never place the cap/stopper on the bench or contamination could result.
Pour the liquid slowly and carefully to avoid spillage. You may find the use of a glass rod
helpful, as shown below.
A-52
Common Laboratory Procedures
However, the accuracy of such a transfer is only as good as the technique of the operator will allow.
In making any volume measurement, the liquid level should always be the same as your eye level.
Erlenmeyer flasks and graduated cylinders are usually filled/read by raising them to your eye level
rather than by squatting down to bring your eye level to the bench top. The liquid level in a pipet
is always lowered to the mark while the mark is held steady at eye level.
Burets: With practice, the position of the meniscus of a liquid in the 25 mL burets used in the
Chemistry 2 labs can be estimated to within 0.02 mL.
Figure 4. shows the use of a card with a dark strip on it to sharpen the image of the meniscus. You
will find by experiment that if the top of the strip is positioned slightly below the level of the liquid
in the buret, the bottom of the meniscus will be very easy to see.
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Common Laboratory Procedures
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Common Laboratory Procedures
2. Beakers
Beakers can be used in the laboratory to estimate volume, storing liquids temporarily, and carry
out certain reactions.
a. Always hold beakers from the bottom or the side. Never hold a beaker by the rim.
b. All beakers in the Chemistry 2 laboratories have a
pouring lip to make pouring solutions easier.
Pouring
c. All beakers in the Chemistry 2 laboratories have marks lip
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Common Laboratory Procedures
5. Volumetric Flasks
Volumetric flasks are very precisely calibrated glassware designed to contain one specific volume
of liquid. You will only be allowed to have a limited number of volumetric flasks. If you need to
make multiple solutions accurately with a volumetric flask, do not use multiple volumetric flasks.
Instead, pour solutions you made in another container and reuse the same volumetric flask.
a. The 250 mL volumetric flask used in the Chemistry 2 laboratories has only one graduation
mark for volume of 250 mL. As noted on the glassware, there is a ±0.12 mL error at 20 °C.
b. To fill a volumetric flask to the mark, quickly fill the flask to where the round base meets
the neck. Cap the bottle and swirl or invert if needed. Then use a 250 mL water squeeze
bottle to fill to the volume mark. Notice that the volume between the neck and the 250 mL
volume mark is only 10 mL.
c. Never use glass pipets or dispo pipets to draw solutions from volumetric flasks. Pipets will
become stuck inside the flasks.
250 mL
mark
10 mL
240 mL
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Common Laboratory Procedures
6. Burets
Burets are used to deliver a precise amount of solution. Unlike the volumetric flask and graduated
cylinder, which are calibrated to measure the liquid contained in the glassware, burets are calibrated
to measure the liquid delivered from the glassware. In the Chemistry 2 labs, the buret is mostly
used for titrations.
a. Filling the buret:
• Always use a small beaker (100 mL or 150 mL) to transfer
0 mL
liquid into the buret. A funnel may be used to prevent spills as
mark long as it is cleaned immediately after.
• Remove the buret from the buret clamp and hold it over a sink,
below eye level.
• Check to make sure the stopcock is in the closed position.
Graduation
25 mL marks
• Hold the buret slightly below the 0mL mark with one hand.
With your other hand, slowly pour the solution from the
beaker into the buret. Stop before the liquid level reaches 0 mL
• If you used a funnel, place the funnel in the sink to clean.
• Replace the buret back in the buret clamp.
b. Cleaning the buret:
Stopcock
(closed when • To clean a buret, fill it to half way with DI water.
horizontal)
• At the sink, open the stopcock and drain out ~10 mL of water
and close it. Then invert the buret and open the stopcock and
drain out the rest from the top.
c. Conditioning the buret:
You should always condition your buret with your working solution before using it.
• Clean the buret with DI water.
• Fill the buret with 8-10 mL of the solution to be used. Open the stopcock to drain out a
small amount from the tip into an appropriate waste container.
• Cap the top end with Parafilm. At the sink, hold the top of the buret between the thumb
and finger of one hand, and hold the tip of the buret with another. Turn the buret horizontal
and rotate the tip of the buret. Make sure all sides of the buret are washed with the solution.
• Pour the remaining solution in the buret into an appropriate waste container.
d. Dispensing solution from the buret:
• First, fill the buret with your solution to near the 0mL mark, but do not attempt to fill it
to exactly 0.00 mL. Open the stopcock and drain out a very small amount to ensure no air
bubbles exist in the tip. Record in your lab notebook your buret initial reading.
• Open the stopcock and drain the solution. Stop when the target volume is reached. Record
the buret final reading in your lab notebook. The difference between the initial reading
and the final reading is the volume dispensed.
• To dispense in small quantities, quickly turn the stopcock clockwise exactly 180 degrees.
Repeat as needed.
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Common Laboratory Procedures
7. Volumetric Pipet
Similar to the buret, the volumetric pipet is designed to deliver a precise amount of solution.
a. The volume of liquid each pipet is designed to deliver is labeled
on the glassware. Use the volumetric pipet only when you need
to deliver the exact amount of solution with precision.
b. There is a bottle of volumetric pipet cleaning solution in each
laboratory. Draw the cleaning solution into the pipet with a
pipet bulb and dispel the solution
c. To condition a volumetric pipet, draw a small amount of your
working solution into the pipet just above the volume mark.
Drain the solution into an appropriate waste container.
d. Follow the illustration on the next page to learn how to use
the volumetric pipet. You should practice using deionized
water first to become proficient with the techniques.
Caution
• Never mouth pipet. Always use the pipet bulb with tip attached.
• Never point your pipet or pipet bulb at yourself or others.
• Never squeeze air into solutions as it may cause chemical splash.
• Never draw solutions into the bulb. Corrosive solutions will dissolve the rubber and contaminate
the pipet.
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Common Laboratory Procedures
1. To begin:
• With one hand, hold the conditioned pipet vertical and the pointed end downward inside
the container of your working solution. Place your other hand near the top of the pipet and
keep the index finger free so that it can easily cap the pipet.
• With your other hand, deflate the rubber pipet bulb with tip with your thumb.
• Place the plastic pipet tip on the top of the pipet.
2. To draw the solution:
• Slowly release your thumb and draw the liquid up the pipet and a few centimeters above the
mark on the pipet. Keep the pipet submerged in solution to avoid drawing up air.
• Lower the pipet so that it reaches the bottom of the container. Quickly remove the pipet
bulb with tip and cap the pipet with your index finger.
3. To adjust the volume:
• Raise the over-filled pipet. Raise the mark on the pipet to your eye level, tilt the receiver
slightly, and touch the pointed tip of the pipet to a dry spot on its sidewall.
• Rotate the pipet left and right slightly and let a small amount of air to enter the pipet and
thereby allow the meniscus to fall exactly on the volume mark. Be patient, because if you
overshoot the mark you must begin the whole process again.
4. To deliver the liquid:
• Remove the accurately filled pipet from its container. Quickly dry the lower portion of the
shaft with a single downward stroke of a laboratory tissue.
• Tilt the final receiver slightly and while holding the pipet vertical, place its tip against the
receiver wall so that when you take your finger off of the pipet mouth, liquid will flow
smoothly down to the bottom of the vessel. Avoid splashing.
• Do not squeeze solution out with the pipet bulb with tip and do not blow out the last
drop. The pipet is calibrated to deliver with one last drop left in the pipet.
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Common Laboratory Procedures
Draft Shield
Weighing Pan
LCD Display
Keys
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Common Laboratory Procedures
Notice
• Always use weighing boats when weighing solids to protect the balance. To do this, place the
plastic weighing boat on the balance pan and be sure it is not touching the sides.
• Always use the balance with extreme care, as it is very expensive.
3. Taring
To measure the mass of sample inside a container, perform the following procedures:
a. Place the empty container (e.g. a weighing boat) on the balance.
b. Press the 0/T key briefly. The display should read 0.000 g.
c. Add the sample to the container. Read the displayed mass to 0.0001 g.
Figure 6. Taring
4. Weighing by Difference
To measure the mass of a sample by difference:
a. Clear the weighing pan. Press 0/T. The reading should be 0.000 g.
b. Place the container with the sample on the balance. Record the mass.
c. Remove a portion of the sample from the container.
d. The difference between the two readings is the mass of the removed portion of the sample.
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Common Laboratory Procedures
Cover Latches
(one on each side)
On/off Switch
Warning
• Improper use of the centrifuge machine may result in serious injury. Follow all safety
precautions when operating the centrifuge machine.
2. Safety Precautions
a. Operate the centrifuge only when the cover is securely closed.
b. Never open the cover when the centrifuge is running.
c. Always balance the tubes before loading. Only spin 2, 4, or 6 tubes.
d. Never spin 1, 3, or 5 tubes.
e. Turn off the machine immediately if there are signs that the load is unbalanced.
f. Never open the cover before the rotor comes to a complete stop.
g. Never stop the rotor with your hand. Serious injury may result.
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Common Laboratory Procedures
Ceramic Top
Indicator Light
Heating/Stirring
Control Knobs
Warning
• The hot plate may cause serious burns. Avoid touching the top plate and follow all safety
precautions.
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Common Laboratory Procedures
2. Safety Precautions
a. Keep the power cord away from the heating surface. The cord may melt and cause an
electrical hazard.
b. Do not hit the top with heavy objects. It may break if impacted.
c. Do not heat volatile or flammable materials.
d. Do not operate near volatile or flammable materials.
The hot plate must not be used during these experiments:
• 2B. Colligative Properties
• 2B. Determination of Avogadro’s Number
e. Avoid spilling liquids on the ceramic top. Do not over boil solutions.
It takes approximately 15 minutes to boil 400 mL of water at Heat setting 6. Avoid turning the
heat setting too high. Spills from over-boiling will damage the hot plate and may result in personal
injury.
f. Never use a container larger than the top plate.
g. Never boil a solution to dryness.
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Common Laboratory Procedures
Warning
• Only use the Bunsen burner when specifically instructed by the lab manual.
• Keep all flammable materials away from the Bunsen burner.
• Heated lab ware including iron rings can be extremely hot and may cause serious burns!
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Common Laboratory Procedures
Filtration
You will often need to separate a liquid from a solid. At times you will simply decant, that is, you
will carefully pour out the liquid, leaving the solid behind. At other times you will need to filter the
solution. To do this you will use filter paper and a funnel. You must first fold the paper in order to
accelerate the process; this is shown in Figure 7.
You will then set the paper in the funnel using your wash bottle. To do this simply place the paper
into the funnel and add a small amount of water to the bottom of the filter.
Slowly add water to the sides with a circular motion to avoid air bubbles between the paper and the
funnel. Once the paper has set, transfer the solution to be filtered. If the solid has settled, decant
the liquid through the filter first in order to save time.
Never overwhelm the filter; don’t add the solution too quickly and never come to within one
centimeter of the top of the paper. Transfer the solid using a wash bottle and rubber policeman,
and then wash the solid as directed by the experimental procedure.
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Common Laboratory Procedures
buret clamp
buret
stopcock
(open position)
flask
stir bar
stir plate
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Common Laboratory Procedures
6. Do NOT let electrode dry out. Always store electrode in saturated KCl solution when
not in use.
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Common Laboratory Procedures
6. Repeat step B-1 to B-5 with the pH 4 buffer standard (red) and then with the pH 10 buffer
standard (blue).
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Common Laboratory Procedures
1. After calibration, place the electrode in sample solution and press Read.
2. Wait for the reading to stabilize.
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Common Laboratory Procedures
Flow Monitor
with Emergency button
and Mute button
Light Switch
Certification Sticker
Sash
Sash Stop
Work Surface
Airfoil
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Common Laboratory Procedures
6. When increased airflow is needed, press the Emergency button and the Mute button.
7. Clean up spills immediately.
8. Cap all containers immediately.
9. Turn off Emergency mode and close hood sash all the way at the end of lab.
4. Using the fume hoods in the Chemistry 2 Laboratories
1. Always use the fume hood when directed by the Laboratory Manual.
Certain reactions in the Chemistry 2 curriculum generate toxic or flammable gases. Follow
instructions to protect yourself and others in the lab.
2. Many hazardous chemicals are kept in the fume hood. Never remove these containers unless
specifically directed by the Laboratory Manual.
3. All Hazardous Waste containers for the Chemistry 2 course are kept in the fume hood.
5. Fume Hood Emissions
1. Minimize fume hood emissions to protect the environment and air quality.
2. Never evaporate waste in the fume hood.
3. Minimize use of volatile liquids. Close and seal after using.
If you have questions, contact your TA or safety coordinator.
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Locker Inventory
Centrifuge Tube
Casserole Dish
Crucible
(with Cover)
Test Tube
Beaker
Erlenmeyer Flask
Evaporating Dish
Test Tube
Brush
Volumetric Pipet
Crucible
Tongs
Washing Bottle
Scoopula
Beaker Tongs
Locker Inventory
Procedure for beginning of quarter locker check-in:
1. Count the numbers of items currently present in locker.
2. Place excess items from locker into the extra glassware box in the back of lab.
3. Return community supplies to the appropriate storage location.
4. Check out missing items from the following sources:
a) from the extra glassware box in the back of lab
b) from the Dispensary service window (1st floor, SLB 1060E)
5. Clean and dry all equipment.
COMMUNITY SUPPLIES
(not in student lockers)
Lab Island Lockers Wall Side Drawers
8” Extension Clamp Beaker Tongs
Clamp Holder Crucible Tongs
4” Support Ring Test Tube Clamp
Overhead Storage Cabinet Bunsen Burner
Pipet Bulb Silicone Rubber Tubing
1 mL Pipet Storage Cabinet
5 mL Pipet 25 mL Buret
10 mL Pipet
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Locker Inventory
COMMUNITY SUPPLIES
(not in student lockers)
Lab Island Lockers Wall Side Drawers
8” Extension Clamp Beaker Tongs
Clamp Holder Crucible Tongs
4” Support Ring Test Tube Clamp
Overhead Storage Cabinet Bunsen Burner
Pipet Bulb Silicone Rubber Tubing
1 mL Pipet Storage Cabinet
5 mL Pipet 25 mL Buret
10 mL Pipet
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