0% found this document useful (0 votes)
212 views191 pages

CHE 2A Student Lab Manual SS2023

Uploaded by

ritahape91
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
212 views191 pages

CHE 2A Student Lab Manual SS2023

Uploaded by

ritahape91
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 191

Chemistry 2A

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

Location of Safety Equipment Nearest to Your Laboratory


Safety Shower
Eye Wash Fountain
Fire Extinguisher
Fire Alarm
Safety Chemicals

Revision Date: June 2023


Preface
Chemistry is an experimental science. Thus, it is important that students of chemistry do
experiments in the laboratory to more fully understand that the theories they study in lecture and
in their textbook are developed from the critical evaluation of experimental data. The laboratory
can also aid the student in the study of the science by clearly illustrating the principles and
concepts involved. Finally, laboratory experimentation allows students the opportunity to develop
techniques and other manipulative skills that students of science must master.
The faculty of the Chemistry Department at UC Davis clearly understands the importance of
laboratory work in the study of chemistry. The Department is committed to this component of
your education and hopes that you will take full advantage of this opportunity to explore the
science of chemistry.
A unique aspect of this laboratory program is that a concerted effort has been made to use
environmentally less toxic or non-toxic materials in these experiments. This was not only done
to protect students but also to lessen the impact of this program upon the environment. This
commitment to the environment has presented an enormous challenge, as many traditional
experiments could not be used due to the negative impact of the chemicals involved. Some
experiments are completely environmentally safe and in these the products can be disposed of by
placing solids in the wastebasket and solutions down the drain with copious amounts of water.
Others contain a very limited amount of hazardous waste and in these cases the waste must be
collected in the proper container for treatment and disposal. The Department is committed to
the further development of environmentally safe experiments which still clearly illustrate the
important principles and techniques.
The sequence of experiments in this Laboratory Manual is designed to follow the lecture curriculum.
However, instructors will sometimes vary the order of material covered in lecture and thus certain
experiments may come before the concepts illustrated are covered in lecture or after the material
has been covered. Some instructors strongly feel that the lecture should lead the laboratory while
other instructors just as strongly believe that the laboratory experiments should lead the lecture,
and still a third group feel that they should be done concurrently. While there is no “best” way,
it is important that you carefully prepare for each experiment by reading the related text material
before coming to the laboratory. In this way you can maximize the laboratory experience.
Questions are presented throughout each experiment. It is important that you try to answer each
question as it appears in the manual, as it will help you understand the experiment as you do it. In
addition, you are encouraged to complete the report as soon after laboratory as possible, as this is
much more efficient than waiting until the night before it is due.
In conclusion, we view this manual as one of continual modification and improvement. Over
the past few years, many improvements have come from student comments and criticisms. We
encourage you to discuss ideas for improvements or suggestions for new experiments with your
TA. Finally, we hope you find this laboratory manual helpful in your study of chemistry.

i
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.

iii
iv
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

v
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.

Title of Experiment Lab Periods Allocated


Introductory Laboratory Techniques 1
Online Nomenclature Test N/A
Observing Chemical Reactions 1
Chemical Equilibrium 1
Strong Acid- Strong Base Titration 1
Acid Dissociation Constants and the Titration of a Weak Acid 1
Polyprotic Systems 1
Acid/Base Buffers 1
Solubility Product 1
On-Line Prelab Quizzes N/A
Lab Notebooks - Pre-lab (eight) N/A

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.

5. 100% cotton lab coats are REQUIRED.

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.

9. Confine long hair while in the laboratory.

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.

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.

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.

x
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

Common Laboratory Procedures


You will now do a set of simple experiments to learn the proper techniques for using the different
equipment in the laboratory. You must read the common laboratory procedures section of this
manual before beginning this part of the exercise. These pages describe the proper use of equipment.
A record of all data should be placed in your laboratory notebook. Also, all calculations should be
clearly shown in the notebook. Finally, be sure to answer all questions before turning in your report
to the teaching assistant.

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.

Stock Chemicals Used


Safety First
Chemical Maximum Amount Used
Wear your PPE.
Manganese Sulfate, monohydrate (s) 1.0-1.2 g
Use a pipet bulb to fill
Part I. Measuring Volumes your pipet. Never use
another form of suction.
A. Using a Pipet to Measure Volume
1. Draw about 400 mL of deionized water into a clean beaker, and let Hint
it stand for 15 minutes to equilibrate to room temperature. Note that You will need to take
there is only one deionized water tap at each sink in the lab room; make turns with your locker-
sure you use the correct tap. mate using the 10.00
mL volumetric pipet.
2. Confirm that your 10.00 mL volumetric pipet is clean by filling to above One of you should start
part B, using a buret to
the mark with deionized water and then letting it drain. measure volume, while
the other is doing part A.
Your pipet is a transfer pipet that is calibrated “to deliver” (TD) rather

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

You will use pipets in


presence of such drops indicates that your pipet is dirty. Pipet cleaning many of the experiments
solution is located in a 1 L bottle at the reagent counter. Follow the in Chemistry 2.
instructions on the label for cleaning. Remember that your pipet is It is important that you
calibrated to deliver. always clean the pipet
at the end of the lab,
3. Measure and record the mass of a clean 125 mL Erlenmeyer flask. and rinse it thoroughly
with deionized water
4. Measure and record the temperature of the room and the temperature of before returning it to
storage. Be sure to follow
the water that was set aside in step 1. The two temperatures should agree
the instructions given
before you continue. Read the thermometer to the closest one-tenth of in the Appendix for
a degree, using your best estimate. Please be especially careful with the proper use of pipets.
thermometer.
5. Use your pipet to deliver 10.00 mL of the equilibrated water into the
Erlenmeyer flask. Note the precision used here.
6. Measure and record the mass of the flask and the water.

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:

Data Type Collected (Units) Data

Temperature of water in beaker (°C)

Mass of 125 mL Erlenmeyer flask (g)

Trial 1 Trial 2 Trial 3

Volume of DI water delivered using a


volumetric pipet (mL)

Mass of flask with water (g)

Mass of water delivered (g)

1. For each trial, calculate the mass of water delivered.


For Part I.A, calculate the mass of water deivered by the volumetric pipet using the following

formula.
mass of water delivered (g) = mass of flask with water (g) - mass of flask (g)

2. For each trial, determine the volume of water delivered.


For Part I. B, calculate the volume of water delivered by the buret using the following formula.

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.

|𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒𝑒 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 − 𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣|


𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅𝑅 𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸𝐸 = × 100 %
𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎 𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣𝑣

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

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

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

𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖 − 𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓


𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃𝑃 (%) = × 100 %
𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆𝑆 𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖

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.

Is that mold in my kettle?


Water quality is one example in which precipitation chemistry is commonly used. Both surface
and ground water may contain high levels of dissolved calcium and magnesium minerals, the
primary cause of hard water. The higher the Ca2+ and Mg2+ content of water, the greater the degree
of hardness. Aside from leaving unsightly stains in bathtubs, toilets, and sinks, hard water can
leave mineral deposits, called "scale", in appliances and pipes, which reduces their efficiency and
may cause pipes to burst. If you use a kettle to boil water, you may have noticed a white film of
scale develop on the inside. Lime (Ca(OH)2) and soda ash (Na2CO3) are often added to hard water
in order to precipitate Ca2+ and Mg2+. The insoluble precipitate settles at the bottom of the water
tank and can be collected safely.

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.

• Recording detailed observations


• Proper handling of acids/bases
Laboratory
• Using a centrifuge
• Decanting a solution
• Solubility rules
Conceptual
• Double replacement reactions
• Comparing and contrasting qualitative data (observation)
Data Analysis
• Developing experimental procedures from observations

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.

Stock Chemicals Used


Chemical Maximum Amount Used
Safety First
0.1 M Magnesium Nitrate (aq) 5 mL
Use care when handling
0.1 M Strontium Nitrate (aq) 5 mL
acids and bases.
0.1 M Aluminum Nitrate (aq) 5 mL
Silver nitrate will stain
0.1 M Silver Nitrate (aq) 5 mL clothing and skin, so
6 M Hydrochloric Acid <5 mL always wear gloves.
6 M Nitric Acid <5 mL Wear your goggles.
3 M Sulfuric Acid <5 mL
6 M Sodium Hydroxide <5 mL Recording
Observations
Part I. Reactions of the Metal Salt Solutions Use care when recording
In this part of the experiment, you will experiment with four metal salts and your observations.
four other reagents. Acquire approximately 5 mL of each metal salt solution Be detailed, write
in test tubes and bring them to your lab bench. The acids and bases will be them legibly in the
table, and make sure
found on the trays by your lab station. you understand what
you recorded!
Before Starting the Experiment:
• Please copy the observation table from the Data Analysis section into
your lab notebook (be sure to make the table large).
Mix Slowly &
Thoroughly
React each reagent with the individual metal salts
Take care in slowly and
1. Acquire approximately 5 mL of 6 M HCl in a test tube and bring it to thoroughly mixing
your lab bench at the beginning. reagents to ensure
that every possible
2. Using a disposable transfer pipet, transfer approximately 1 mL of a reaction is observed
0.1 M metal salt solution to a clean test tube. within a homogeneous
mixture. Failure to
3. Using the dedicated transfer pipet attached to the reagent bottles, slowly remove an ion can also
lead to false positives.
add a couple of drops of one of the reagents to one of the metal salts.
Record your observations.

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?

Question A: In performing these reactions and any required dilutions,


should you use tap water or deionized water? Why?

Question B: For each observed reaction between a reagent and a metal


salt write a balanced chemical equation that shows what is occurring.

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.

Part II. Analyzing an Unknown


In this part of the experiment you will use the data you have accumulated to
tell which of the salts are present in an unknown.
Your unknown contains two of the four metal salts you have worked with.
Develop a procedure that will distinguish between these four compounds
Hint utilizing the table you have completed, and use it to identify the composition
The centrifuge will also
of your unknown. For help with this, see the Data Analysis section.
be evenly balanced
if you place your test
You may need to be able to separate a solid precipitate from a solution.
tube opposite another Instructions for separation follow.
group’s test tube
containing a similar 1. Transfer the solution and the precipitate to a centrifuge test tube. Fill a
volume of unknown. second test tube with water until the volumes in the two test tubes are
Be sure to label your test approximately the same.
tube with graphite so
you can identify it when 2. Place the two test tubes in the centrifuge. The test tubes should be
the centrifuge stops! placed opposite each other so that their weight is balanced as the
centrifuge spins.

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.

Complete removal of a salt from a solution


• If you are trying to completely remove a salt from a solution, add a
little more of the reagent that caused the precipitation. If more solid
forms in the solution, re-centrifuge and repeat this step.

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).

Observation Table for Part I. Reaction of Metal Salt Solutions

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

Analyzing an Unknown Metal Salt Solution


Use the observations collected in Part I to determine which 2 metal salts are
present in your unknown. Trust your data, do not blindly follow solubility
rules. In general, these tips may help:
• Using your observations, create a flowchart of which ions react with
which reagents, similar to the one below.
• If multiple reactions are observed with the same reagent, compare your
observations with Part I to identify the metals present in your unknown.

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

Ca2+ not present (gives Try another reagent to


no info about Mg2+). test for Mg2+.

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.

Kidney Stones: a painful product of chemical equilibrium


Systems of equilibrium are extremely important for everyday life, particularly for living organisms.
Many systems within organisms follow equilibrium dynamics, such as maintaining proper blood
pH and oxygen levels, or the formation of kidney stones. Kidney stones can develop when
the concentration of dissolved minerals and salts in urine is too high. In order to re-establish
equilibrium, the minerals and salts will precipitate out of the urine and form solid, crystal masses.
Kidney stones can be prevented with a special diet or by drinking plenty of water, both which keep
the concentration of minerals and salts low enough that they won’t precipitate.

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.

• Use of indicators to interpret chemical systems


Laboratory (phenolphthalein and methyl orange)
• Estimating volume with a disposable transfer pipette
• Le Châtelier’s principle
Conceptual
• Precipitation reactions in acidic or basic solutions
• Interpretation of observations (color changes, precipitation
Data Analysis formation, etc.) in relation to equilibria of systems studied

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.

Stock Chemicals Used


Chemical Maximum Amount Used
6 M Hydrochloric Acid < 15 mL
6 M Sodium Hydroxide < 15 mL
6 M Acetic Acid < 5 mL
6 M Ammonium Hydroxide < 15 mL
1 M Ammonium Chloride Drops Safety First
0.1 M Potassium Thiocyanate < 5 mL Remember to wear
0.2 M Ferric Nitrate < 5 mL gloves and use caution
whenever handling
1 M Sodium Acetate < 5 mL acids and bases.
0.5 M Oxalic Acid < 5 mL
Wear your goggles!
0.2 M Potassium Oxalate < 5 mL
0.1 M Calcium Chloride <5 mL
1% Cobalt Chloride in 95% Ethanol < 10 mL
1% Phenolphthalein Indicator Drops
1% Methyl Orange Indicator Drops

Before Starting the Experiment:


• Prepare data tables to record your observations. For part I, you may
use the sample table given in the Data Analysis section, then use it as
a guide to create your own data tables for the rest of the experiment.

Part I. Equilibria of Complex Ions


In this procedure, you will study the properties of a chemical system containing
a complex ion. Many metal ions will bond with ions and molecules to form
species called complex ions. An example of such a system is the combination
of iron(III) ion with thiocyanate ion (SCN-). When these two species are
mixed they establish an equilibrium in water which can be described as:
Fe 3+(aq) + SCN -(aq) ⇌ FeSCN 2+(aq)
(pale yellow) (deep red)

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.

Estimating Volume with a Disposable Transfer Pipet


Because this experiment is mostly qualitative, you may use the disposable
polypropylene transfer pipet to estimate the volume of reagents used.

0.25 mL

1
1 mL

To draw 1mL of solution into an empty disposable transfer pipet:


1. Squeeze the bulb to remove some air from the transfer pipet.
2. Submerge the tip of the transfer pipet in the solution.
3. Slowly release the pressure on the bulb and draw solution to the 1
mL mark.
4. Without releasing pressure on the bulb, steadily remove the pipet
from the solution.
5. Release pressure on the bulb, allow the solution to enter the bulb of
the pipet.
6. Place the pipet inside the receiving vessel, squeeze the bulb and
release the solution.
Safety First
Keep chemical bottles
in the spill tray and cap 1. Place 1 mL of 0.2 M Fe(NO3)3 and 1 mL of 0.1 M KSCN in two
them when you are
different test tubes. These will serve as your stock solutions and allow
finished using them.
you to work from your bench without having to retrieve more.
In case of spills on
hands, change gloves 2. Preparation of the Fe(SCN)2+ solution:
immediately.
a. Add 12 mL of DI water to a 50 mL Erlenmeyer flask. To this flask,
add 10 drops of 0.2 M Fe(NO3)3 and 5 drops of 0.1 M KSCN
Recording from the 2 stock solution test tubes you prepared in step 1. Mix the
Observations solution in the Erlenmeyer well with a disposable pipet. Record the
Remember to record color of the solution.
detailed observations b. Make sure that you can see through the solution; if the color is
on the changes you see!
For more help with this,
too dark you will have trouble observing any color changes as you
see the data analysis proceed. You may continue to dilute the solution if it looks too dark.
section of Observing The volume given here is a general guideline.
Chemical Reactions.
c. Place four 3 mL portions of this solution into four separate test
tubes.
3. Add different reagents to the test tubes containing the Fe(SCN)2+
solution (NOT the test tubes with the stock solutions from step 1) and
record any color changes observed:

22
Chemical Equilibrium

a. To the first test tube of Fe(SCN)2+ add 0.5 mL of 0.2 M Fe(NO3)3


from the stock solution test tube.
b. To the second test tube of Fe(SCN)2+ add 0.5 mL of 0.1 M KSCN
from the stock solution test tube.
c. To the third test tube of Fe(SCN)2+ slowly add 6 M NaOH solution
drop-wise. You will notice two changes. You should address this in
Question A below.
d. Use the last test tube of Fe(SCN)2+ as a reference for comparison.
Question A: Compare the color of the solution in each of the four test
tubes. Explain the color changes in terms of the equilibria
described above and what you believe happened in Step 3.

Clean-Up
• Pour the content from the test tubes into the waste container in the
fume hood labeled “Cation Metal Waste.”

Part II. Equilibria of Acid/Base Indicators


In this procedure, you will study the properties of two acid-base indicators, Safety First
phenolphthalein and methyl orange. Many indicators are weak acids that Do not rest your hands
establish equilibrium in water: or arms on the edges
of fume hood.
+ -
HIn(aq) + H2O(l) ⇌ H3O (aq) + In (aq) Always keep containers
at least 6 inches away
(color 1) (color 2) from the edge and
Thus, indicators can be thought of as dyes which change color depending inside the fume hood.
on whether they are in a protonated (HIn) or unprotonated (In-) form. In
this part of the experiment you will observe the change in the equilibrium
position of the indicators by adding acids and bases to solutions that contain
these indicators.
Phenolphthalein indicator
1. Make sure you have approximately 5 mL of 6 M HCl in a test tube at
the beginning of the experiment.
2. Place 3 mL of deionized water into each of three test tubes. Add two
drops of phenolphthalein 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.

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?

Question D: Write the equilibrium expression for each indicator as shown


above for HIn. Be sure to indicate the color of each form. Use
Hph for the protonated form of phenolphthalein and Hmo for
the protonated form 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.

Part III. Equilibria of Weak Acids and Bases


In this procedure, you will study the equilibrium properties of weak acids
and bases. As described in the chapter on acids and bases, weak acids and
bases establish equilibrium with water. In this part you will study this
concept by using an acetic acid/acetate ion equilibrium system and the
ammonia/ammonium ion equilibrium system. The pertinent equilibria for
each system are:
HC2H3O2(aq) + H2O(l) ⇌ H3O+(aq) + C2H3O2-(aq)
NH3(aq) + H2O(l) ⇌ NH4+(aq) + OH -(aq)
In this part of the experiment, you will observe the change in the equilibrium
position through the use of the indicators used in Part I.

24
Chemical Equilibrium

Procedure for the acetic acid/acetate ion equilibrium


1. Place 3 mL of 0.1 M acetic acid into each of three test tubes. You will
make this solution from 6 M stock solution. Add two drops of methyl
orange to each test tube. Observe the color of the solutions.
2. To one of these test tubes add 1.0 M NaC2H3O2 a few drops at a time
and observe any color changes. Remember to mix the solution well after
each addition. To another test tube, add 6 M acetic acid a few drops at a
time and observe any color changes. Again, mix well after each addition.
Repeat this step with another sample to confirm your results.

Question E: Explain your observations using both the equilibria presented


above and the one involving the indicator. What color
change did you observe? How is the acetic acid/acetate
ion equilibrium affected by adding acetate ion? How does
this change affect the concentration of H3O+? How does
the change in the concentration of H3O+ affect the Hmo/Hmo-
equilibrium?
Procedure for the ammonia/ammonium ion equilibrium
3. Place 3 mL of 0.1 M ammonium hydroxide into the other three test
tubes. You will make this from 6 M stock solution. Add two drops
of phenolphthalein indicator to each tube. Observe the color of the
solutions.
4. To one of these test tubes add 1 M NH4Cl a few drops at a time and
observe any color changes. Remember to mix the solution well after each
addition. Add more 6 M ammonium hydroxide to the test tube a few
drops at a time. Mix well after each addition and note any color changes.

Question F: Explain your observations using both the equilibria presented


above and the one involving the indicator.
5. To another test tube containing ammonium hydroxide, add 6 M HCl
a few drops at a time and observe any color changes. Remember to mix
the solution well after each addition.

Question G: Explain your observations using both the equilibria presented


above and the one involving the indicator.

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.

Part IV. Temperature Effects on Equilibria


In this procedure, you will again study the properties of a chemical system
containing a complex ion. The system in this study of the temperature effects
on equilibria can be described as:
-
Co(EtOH)2Cl2(aq) + 6H2O(l) ⇌ 2EtOH(l) + 2Cl (aq) + Co(H2O)62+(aq) + heat

(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.

Question H: Explain the color changes in terms of the equilibria described


above.

26
Chemical Equilibrium

Part V. Equilibria of Precipitation Reactions


In this procedure, you will study the properties of two chemical systems
involving the oxalate anion, C2O42-(aq). The chemical sources of the oxalate
ion are calcium oxalate, CaC2O4(s) and the weak diprotic acid, oxalic acid,
H2C2O4(aq). This system is particularly interesting because 3 simultaneous
equilibria occur in water. The equilibria in water that are important can be
described as:
Ca2+(aq) + C2O42-(aq) ⇌ Ca2C2O4(s)
H2O(l) + H2C2O4(aq) ⇌ HC2O4-(aq) + H3O+(aq)
H2O(l) + HC2O4-(aq) ⇌ C2O42-(aq) + H3O+(aq)
Clearly, this is a more complex system than we have thus far encountered.
However, we should be able to qualitatively understand the system. For
example, if you wanted to precipitate the calcium with oxalate, would you
want the solution to be basic or acidic based on the equilibria described
above? Take a guess! Now let’s see if you are right.
1. Mix 4 mL of 0.1 M CaCl2 with 4 mL of deionized water in a small
beaker. Split the resulting solution into three approximately equal
portions in three separate test tubes.
2. Add 15 drops of 0.2 M K2C2O4 solution to one of the test tubes
containing calcium chloride. Observe the results.
3. Add 6 drops of 0.5 M H2C2O4 solution to one of the other test tubes
containing calcium chloride. Observe the results.

Question I: Even though you added the same stoichiometric amount of


oxalate ion to these test tubes you have observed differing
amounts of precipitate. Why?
4. Now add 10 drops of 6 M HCl to the solution of calcium chloride and
oxalic acid. Observe the results.

Question J: Explain the results in terms the equilibria discussed above.


5. Now slowly add 20 drops of 6 M NH4OH to this test tube until a
change occurs.

Question K: Explain the results in terms the equilibria discussed above.

27
Chemical Equilibrium

6. You may wonder if the precipitate in Step 5 is really an oxalate or a


hydroxide precipitate. This can be checked by adding 20 drops of 6
M NH4OH to the solution in the last remaining test tube containing
calcium chloride. Observe the results.

Question L: Do you believe the precipitate is calcium oxalate or calcium


hydroxide? Explain.

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.

Part I. Observation Table for Part I-Equilibria of Complex Ions

Test tube # Contents Procedure Observations

1 3 mL dilute Fe(SCN)2+ add 0.5 mL of 0.2 M Fe(NO3)3

2 3 mL dilute Fe(SCN)2+ add 0.5 mL of 0.1 M KSCN

3 3 mL dilute Fe(SCN)2+ add 6 M NaOH dropwise

4 3 mL dilute Fe(SCN)2+ reference

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

H2C2O4(aq) + H2O(l) ⇌ H3O+(aq) + HC2O4-(aq)

Reaction will proceed in this


direction (Le Châtelier’s principle)
HC2O4-(aq) + H2O(l) ⇌ H3O+(aq) + C2O42-(aq)

Ca2+(aq) + C2O42-(aq) ⇌ Ca2C2O4(s)

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.

H+(aq) + OH-(aq) → H2O(l) (1)


An acid or base is considered strong if it completely ionizes in water. Thinking back to experiment
3, Chemical Equilibrium, this means the chemical equilibrium of a strong acid or base lays
completely to the right of its dissociation equation. In this lab you will be utilizing the strong base
sodium hydroxide to neutralize the strong acid hydrochloric acid according to the neutralization
reaction below.
HCl(aq) + NaOH(aq) → NaCl(aq) + H2O(l) (2)
The progression of the reaction will be observed using a pH meter and a titration curve will be
created using the experimental data. You will start with a sample containing acid and slowly add
your standardized base. A titration curve is simply a plot of the pH of an acid versus the volume
of base added, or vice versa.
The titration curve gives a good description of how an acid-base reaction proceeds. The pH will
start out low and acidic, then increase as it approaches the equivalence point. The equivalence
point is where the concentration of acid equals that of the base. If you know the concentration of
one of these components, you can determine the concentration of the other using the equivalence
point. As more base is added, the pH of the solution will continue to rise and then level off.
The progression of the reaction will also be monitored using the chemical indicator phenolphthalein,
which turns pink in the presence of a basic solution. This color change occurs at the endpoint
of the titration. It is important to note that the endpoint does not always correspond to the
equivalence point, as phenolphthalein changes color in a basic solution, where the concentration
of base has exceeded the concentration of acid.

32
Strong Acid - Strong Base Titration

Learning Goals
The following is a list of skills that you will use in this experiment.

• Calculating volume and mass of reagents used to prepare


solutions
Laboratory • Weighing by difference
• Using a buret
• Using a pH meter
• Arrhenius-Acid-Base theory
Conceptual • Properties of strong acids and bases (i.e. complete dissocia-
tion)
• Properties of a strong acid/base titration curve
• Using a spreadsheet to make a titration curve
Data Analysis • Determining molarity of a titrated analyte
• Statistical analysis (Q-test, standard deviation, 90% confi-
dence limit)

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.

Stock Chemicals Used


Safety First Chemical Maximum Amount Used
Remember to wear Potassium acid phthalate (KHP) 2.5 g
gloves and use caution 6 M Hydrochloric Acid According to calculation (< 30 mL)
whenever handling 6 M Sodium Hydroxide According to calculation (< 30 mL)
acids and bases.
1% Phenolphthalein Indicator Drops
Wear your goggles! pH Meter Calibration Buffer, pH 4
< 5 mL
(red)
pH Meter Calibration Buffer, pH 7
< 5 mL
(yellow)
pH Meter Calibration Buffer, pH 10
< 5 mL
(blue)

Part I. Preparing your Solutions


You will prepare about 500 mL of approximately 0.2 M sodium hydroxide
solution and 500 mL of approximately 0.2 M hydrochloric acid from 6.0 M
Hint stock solutions. Perform this calculation in the lab note book as part of the
When determining the pre-lab exercise.
amount of concentrated
stock solution needed 1. Preparing the 0.2 M NaOH solution:
to create a diluted
solution, use M1V1=M2V2. a. Label a 1 L bottle as 0.2 M NaOH.
b. Estimate approximately 400 mL of DI water using a beaker and
transfer it to the 1 liter plastic bottle.
c. Estimate the volume of 6.0 M NaOH needed using a graduated
cylinder, then quantitatively transfer the sodium hydroxide to a
clean 150 mL beaker using a water bottle filled with DI water.
d. Add DI water until the volume reaches 100 mL. Transfer this
solution to the 1 liter plastic bottle.
e. Cap the bottle securely, and mix the contents thoroughly by inverting
the bottle and swirling it repeatedly. The bottle should be shaken at
least 50 times in total.

34
Strong Acid - Strong Base Titration

2. Preparing the 0.2 M HCl solution:


a. Label another 1 L bottle as 0.2 M HCl.
b. Measure approximately 400 mL of DI water using a beaker and Safety First
transfer it to the 1 liter plastic bottle. Always add acid to water,
c. Calculate the volume of 6.0 M HCl needed to prepare your 0.2 M and never the reverse.
HCl solution.
d. Using a beaker, obtain 6.0 M HCl and bring it back to your lab
bench. At your bench, use a graduated cylinder to measure out the
calculated amount of HCl. Quantitatively transfer the HCl to a
clean 150 mL beaker using a water bottle filled with DI water.
e. Add DI water to the 150 mL beaker until the volume reaches 100
mL. Transfer this solution to the 1 liter plastic bottle.
f. Cap the bottle securely, and mix the contents thoroughly by inverting
the bottle and swirling it repeatedly. The bottle should be shaken at
least 50 times in total.

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.

Part II. Standardizing the base against Potassium Acid


Phthalate
In this step of the experiment, you will standardize your sodium hydroxide
solution against the primary standard, potassium acid phthalate, KHP.
You will also use a technique called weighing by difference. This is a very
important technique to use because it eliminates systematic errors from the
balance. Be sure to use the same balance so that systematic errors in the
balance will continue to be eliminated when you take the difference readings
between masses.

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

1. Prepare the KHP samples:


a. Accurately weigh a 0.5–0.6 g sample of dry KHP onto a weighing
boat. Using the appearance of this sample as a guide, accurately
Definitions
weigh by difference 3 more samples onto weighing boats.
Titrant: a solution of
known concentration b. Quantitatively transfer the first sample from the weighing boat into
used to determine a 250 mL beaker with the help of a small stream of DI water from
the concentration your wash bottle, and then add water to a total of about 30 mL and
of an analyte.
swirl it gently until the KHP dissolves. Transfer the other 3 samples
Analyte: a solution of KHP into small Erlenmeyer flasks using the same procedure.
whose concentration
is being measured. 2. Prepare the buret:
a. Read and understand how to fill and use a buret by reading the
Common Laboratory Procedures section in the Appendix of this
manual. Failure to fill the buret properly can result in spills and
injuries.
Tips on using a buret
• Do not waste time trying to hit 0.00 with the meniscus. Fill the buret
to slightly below the zero mark and read and record the actual starting
point to the nearest 0.02 mL.
• Be careful when filling the buret. Only one person should be filling the
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.
• Be sure always to wipe off the tip of a buret before you begin a
titration. Use a laboratory tissue and make one quick stroke downward
beginning at the stopcock and ending in the air beyond the buret tip.

b. Condition a 25 mL buret with your standardized NaOH solution.


Remember to check that the stopcock is closed before filling a buret.
While holding the buret at a safe level over the sink, use a beaker to
pour in your sodium hydroxide solution.
c. After conditioning, fill the buret to above the zero mark with a
beaker, dispel any air bubbles from the stopcock, and place the buret
in the buret clamp. Record the initial buret reading to two decimal
places, eg. 1.24 mL.

36
Strong Acid - Strong Base Titration

3. Set up your titration apparatus according to Figure 10 Titration Setup


in the Appendix.
a. Place the stir plate underneath the buret. Adjust the clamp height
so that there’s enough room to place the KHP beaker directly under
the buret.
b. Add three drops of phenolphthalein indicator and a stir bar to
the first KHP solution.
c. Place the beaker onto the stir plate underneath the buret and turn
on the stirrer and slowly increase the stirring speed. Don’t use the
heat control knob on the hot plate. Lower the buret tip well into the
250 mL beaker.
4. Perform a cursory titration using your KHP sample in a 250 mL beaker.
Lab Skill Tips
a. Record the initial buret reading. Read the buret at or
slightly below eye
b. Quickly add NaOH to the KHP beaker until the solution turns pink
level. Do not hold your
to determine the approximate endpoint of the titration. If the masses hands or lab manual
of KHP are almost the same across samples, then the endpoint of behind the buret.
each sample will occur at approximately the same volume. You can hold a sheet of
c. After you have reached your endpoint for your cursory titration, colored paper behind
record the buret reading at the endpoint and calculate the volume of the buret to read the
meniscus clearly.
NaOH needed to reach the endpoint.
d. Retrieve, clean, and dry your magnetic stir bar for your next titration
using the magnetic rod at the center sink. Pour the solution in the
titration flask into an 800 mL beaker.
5. Perform a series of duplicate, precise titrations:
a. From your cursory titration, you know the approximate position of
the endpoint. Now you will perform a more precise titration using
the following guidelines.
b. Initially add the titrant fairly rapidly, pausing every few milliliters
to allow the solution to mix thoroughly. Pay attention to the region
where the two solutions mix and as the indicator color begins to tail
out into the solution as you stir, reduce the next amount of titrant
added, keeping in mind the target volume. Stop adding titrant about
1 mL short of this volume.
c. Gently wash down the walls of the flask with water from your
wash bottle, and then resume adding base from the buret but
now dropwise. As you approach the endpoint, the pink color will
increasingly linger. You should frequently wash down the interior
sides of the flask to recover any reagent drops that may be clinging
to the sides. Stop adding base when the entire flask has a faint pink
color that persists.

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

Care of pH meter and pH electrodes


• Keep the tip of the electrode submerged in solution at all times.
• Never leave the electrode in deionized water.
• When rinsing the electrode use a light stream of deionized water.
• Be careful of the electrode when adding strong base or when stirring
the solution. Do not stir using the electrode.
• After completing the experiment, store the electrode in the storage
solution provided. Additional storage solution is available in the
laboratory if needed.

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

volume of NaOH added increments.


(the difference between
present buret reading a. When the assembly is complete, turn on the stir motor (left knob)
and initial buret reading). slowly so that the stir bar is rotating at a smooth, moderate speed
and clears the pH electrode. Do NOT turn on the heat.
b. Perform a quick titration by adding the titrant in 1 mL increments
until you reach pH 2.5; then 0.10 mL (2 drops) increments until
you reach pH 10.7. After that, add 1 mL increments until pH 11.5.
Stop the titration when you have reached pH > 11.5.
c. When the titration is complete, pour the solution from the titration
vessel into the 800 mL beaker.
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.

d. To find the endpoint, first convert your buret readings to volumes


of NaOH added. Determine between which 2 volumes the largest
change in pH occurs. The endpoint is between the volume readings
where the largest pH change occurred.
5. Set up your second titration by repeating step 2.

40
Strong Acid - Strong Base Titration

6. Your second titration should be more carried out more precisely.


Refine your procedure based on your first titration by adding 1 drop of

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

pH reading to become stabilized and then record the pH value in your


notebook alongside the buret reading.
a. Turn on the stir motor (left knob) slowly so that the stir bar is rotating
at a smooth, moderate speed. If necessary, adjust the position of the
pH electrode so that it does not touch the stir bar. Do NOT turn
on the heat.
b. Begin by adding the titrant in 1 mL increments until you are
approximately 2 mL away from the endpoint. Record the volume
and pH reading at each increment.
c. Now, add the titrant in drop-wise increments. Stop the titration
when you have reached pH > 11.5.
d. When the titration is complete, pour the solution from the titration
vessel into the 800 mL beaker.
7. Repeat the titration procedure as time allows so that you have as many
trials as possible to improve the statistics of your standardization of HCl.

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

Titration Curve (vol of NaOH vs. pH)


14

12

10

pH level
8

0
5 10 15 20 25 30
Volume of NaOH added (mL)

Generating 1st and 2nd derivative curves


As you’ll hopefully see from your titration curves, the pH of a solution is much more sensitive near
the equivalence point. This means that even a small volume of titrant can have a great effect on
the pH. Sometimes it is difficult to determine the exact volume of titrant at which the equilibrium
point occurs just from using the titration curve. To help determine this volume, we will construct
approximations of the 1st and 2nd derivative plots of the original titration curves. A derivative
is a mathematical concept used to describe rate of change at a certain point. By finding the 1st
derivative, we can see where the greatest change in pH occurs over the smallest amount of volume
(i.e. where the slope of our titration curve is the steepest). By finding the 2nd derivative, we can
see where there is an inflection point in the curve of the 1st derivative (the 2nd derivative will
change sign). This point will be the equivalence point. It is important to note that this method of
calculating derivatives, called “forward divided difference”, does tend to amplify experimental error
(commonly called noise), but your data should be good enough that these plots of the forward
divided differences can help you to identify the equivalence point.
1. For your first good titration, label the column containing total volume of NaOH added as “V”
and the column containing the pH as “pH”
2. Leave four empty columns to the right of these two columns for calculating values for the
derivatives. Label these columns as “Vm” (midpoint volume), “D1” (1st forward divided
difference), “Vd” (derivative midpoint volume), and “D2” (2nd forward divided difference).
Vm and D1 will be used to plot the 1st derivative, and Vd and D2 will be used to plot the 2nd
derivative.
3. We will start by calculating values for Vm. Vm is the midpoint between volumes of NaOH
added. For example, if the first addition of NaOH was 1.00 mL, and then you added another
1.00 mL (for a total of 2.00 mL), the midpoint volume would be 1.50 mL. This can be
mathematically expressed using the following equation, where Vi is one of the volume data
points and Vi+1 is the next data point in the sequence.

��� � ���� )
��� =
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)

8. Repeat steps 1-7 for the rest of your titrations.


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 included a
title and labeled axes with units.

45
Strong Acid - Strong Base Titration

Calculating concentration of HCl solution using titration curves


In part II of this lab, KHP was used as a primary standard to determine the concentration of
NaOH solution. This NaOH solution can now be used as a secondary standard to determine the
concentration of your HCl:
1. Using the titration curves and derivative plots you previously developed, what is the equivalence
point volume of NaOH for each of your titration curves? You should be able to determine this
value within 0.02 mL (eg. 18.46 mL).
2. Using the average molarity of your NaOH solution, and the equivalence point volumes
of NaOH determined from the derivative plots, calculate how many moles of NaOH were
dispensed in each titration at the equivalence point.
3. Write down the chemical equation for the neutralization reaction of NaOH with HCl.
Determine the stoichiometric ratio between these two reagents. In other words, how many
moles of NaOH react with each mole of HCl?
4. Use the moles of NaOH dispensed and the stoichiometric ratio between NaOH and HCl to
determine the number of moles of HCl present in each sample.
5. Using the number of moles of HCl and the volume of HCl in each sample, determine the
molarity of HCl for each titration. Remember to pay attention to units!
6. Calculate the average molarity of your HCl solution. This solution has now been “standardized”,
and can be used as a titrant to determine the concentration of other analytes.
• Keep the average values of your standardized NaOH and HCl solutions in a prominent
place in your notebook and perhaps write the value on the bottle labels. You will need these
values in subsequent experiments.
7. Calculate the standard deviation of the average molarity of your HCl solution.
8. Calculate the 90% confidence limit for your average molarity.

46
Strong Acid - Strong Base Titration

Sample Data and Plots


TITRATION EXAMPLE: Titration of 15 mL HCl with 0.20 M NaOH
NaOH
pH Vm D1 Vd D2
(Vol added, mL)
5.00 1.93 7.50 0.04 10.00 0.01
10.00 2.15 12.50 0.07 14.00 0.02
15.00 2.50 15.50 0.13 16.00 0.04
16.00 2.63 16.50 0.17 17.00 -0.10
17.00 2.80 17.50 0.07 18.00 -0.04
18.00 2.87 18.50 0.03 18.78 3.40
19.00 2.90 19.05 1.90 19.10 -17.00
19.10 3.09 19.15 0.20 19.20 3.00
19.20 3.11 19.25 0.50 19.30 16.00
19.30 3.16 19.35 2.10 19.40 4.00
19.40 3.37 19.45 2.50 19.50 37.00
19.50 3.62 19.55 6.20 19.60 247.00
19.60 4.24 19.65 30.90 19.70 -54.00
19.70 7.33 19.75 25.50 19.80 -208.00
19.80 9.88 19.85 4.70 19.90 -25.00
19.90 10.35 19.95 2.20 20.23 -2.65
20.00 10.57 20.50 0.74 21.00 -0.44
21.00 11.31 21.50 0.30 22.00 -0.11
22.00 11.61 22.50 0.19 23.00 -0.08
23.00 11.80 23.50 0.11 24.00 -0.46
24.00 11.91 24.50 -0.35 25.00 0.39
25.00 11.56 25.50 0.04 26.00 0.04
26.00 11.60 26.50 0.08 27.00 -0.04
27.00 11.68 27.50 0.04 28.00 0.01
28.00 11.72 28.50 0.05
29.00 11.77

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

HCl(aq) + H2O(l) → H3O+(aq) + Cl-(aq) (1)


In this reaction, HCl is the Brønsted-Lowry acid and H2O is the Brønsted-Lowry base. In an
aqueous solution of HCl, the associated species, HCl, does not exist. The species present are H3O+,
Cl-, and H2O. Since this reaction essentially goes to completion, a single-headed arrow pointing to
the right is used in the chemical equation.
Unlike strong acids, aqueous solutions of weak acids do not completely dissociate into the
hydronium ion and the corresponding anion but instead reach equilibrium. If we let “HA”
symbolize a weak acid, then the equilibrium reaction of a weak acid with water is represented by

HA(aq) + H2O(l) ⇌ H3O+(aq) + A-(aq) (2)


Similarly, in this reaction, HA is the Brønsted-Lowry acid and H2O is the Brønsted-Lowry base.
In an aqueous solution of HA, the species present are the associated species, HA, the hydronium
ion, H3O+, the anion, A-, and H2O. Note that double arrows pointing in opposite directions are
used in the chemical equation since this reaction does not go to completion but instead reaches
equilibrium. We explored multiple examples of weak acid equilibrium in the experiment Chemical
Equilibrium.
HA and A- are also referred to as a conjugate acid-base pair where HA is the acid and A- is its
conjugate base, formed when HA donates its proton. The species A- is also considered to be a
Brønsted-Lowry base since it can accept a proton. The species that make up a conjugate acid-base
pair only differ in structure by the presence of a single proton, H+. Likewise, H2O and H3O+ also
constitute a conjugate acid-base pair where H3O+ is the conjugate acid of H2O.
Since equation (2) is an equilibrium reaction, we can write an equilibrium constant expression as
shown below

ൣுయ ைశ ൧ሾ஺ష ሿ
‫ܭ‬௔ ൌ (3)
ሾு஺ሿ

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).

HF(aq) + H2O(l) ⇌ H3O+(aq) + F-(aq) (4)

HCN(aq) + H2O(l) ⇌ H3O+(aq) + CN-(aq) (5)


In other words, HF dissociates into the hydronium ion, H3O+, and its conjugate base, F-, to a
greater extent than does HCN. If we had a bottle of 0.1 M HF and a bottle of 0.1 M HCN, then
the hydronium ion concentration would be higher in the bottle of HF than in the bottle of HCN;
therefore, the pH would be lower in the bottle of HF.
Due to the establishment of equilibrium between a weak acid and its conjugate base in an
aqueous medium, the pH changes that take place when titrating a weak acid with a strong base
are significantly different than the pH changes that take place when titrating a strong acid with
a strong base. As a result, the titration curve of a weak acid has a slightly different shape than the
titration curve of a strong acid. For example, when a strong acid is titrated with a strong base,
the equivalence point is found to occur at pH = 7. However, when a weak acid is titrated with a
strong base the equivalence point does not occur at neutral pH. You will also find other significant
differences between the two titration curves due to equilibrium reactions.
Let us consider in more detail how pH will change when small amounts of strong base are added
to an aqueous solution of a weak acid, HA. Before any strong base is added to the weak acid, the
concentration of the hydronium ion can be assumed to originate only from the dissociation of the
weak acid.

HA(aq) + H2O(l) ⇌ H3O+(aq) + A-(aq) (2)


The assumption here is that the amount of hydronium ion resulting from the dissociation of water

H2O(l) + H2O(l) ⇌ H3O+(aq) + OH-(aq) (6)


is very small relative to the other sources of hydronium and can be neglected. This is a good
assumption since the equilibrium constant for water, Kw, at 25˚C is equal to 1.0 × 10-14. Therefore,
the pH corresponds to the [H3O+] generated by the dissociation of HA.
Looking at equation (2), for every mole of H3O+ that forms, one mole of A- is produced and
one mole of HA dissociates. Therefore, at equilibrium, [H3O+] = [A-] and [H3O+] represents the
concentration of HA that is lost in the dissociation. Once the initial concentration of HA is
known, then the equilibrium concentrations of H3O+, A-, and HA can be calculated, as well as the
Ka value of the weak acid from a measured pH value.
As base is added, the OH- ion will react with the major species in solution, HA, to produce more
conjugate base, A-.

50
Acid Dissociation Constants and the Titration of a Weak Acid

HA(aq) + OH-(aq) → H2O(l)) + A-(aq) (7)


This reaction can be assumed to go to completion followed by the re-establishment of the
dissociation equilibrium:
HA(aq) + H2O(l) ⇌ H3O+(aq) + A-(aq) (2)
If the equivalence point has not been reached, then the number of moles of leftover HA will be
equal to the original number of moles of HA minus the number of moles of OH- added. The moles
of HA lost in the dissociation reaction, shown by equation (2), will be negligible compared to the
number of moles of leftover HA.
[HA] then is calculated by dividing the number of leftover moles of HA by the total volume of
the mixture at this point in the titration. [H3O+] is determined by the number of moles of H3O+
formed in the dissociation reaction and is simply measured by pH. (Again, assuming that any
[H3O+] formed from the dissociation of water is negligible.) [A-] is equal to the number of moles
of A- formed in the strong base reaction, shown by equation (7), divided by the total volume of the
mixture. Like HA, the number of moles of A- produced in the dissociation reaction is negligible.
Another point of interest on a weak acid titration curve, other than the equivalence point, is the
midpoint. The midpoint occurs when ½ of the original acid, HA, has reacted with all the strong
base, OH-, that has been added. At the midpoint, the number of moles of the conjugate base, A- is
equal to the number of moles of weak acid, HA, remaining in the solution and thus, [HA] = [A-].
Applying this to equation (3), we obtain Ka = [H3O+] and taking the negative log of each side, the
equality is expressed as pH = pKa. Therefore, at the midpoint, the Ka of the weak acid can be easily
calculated from the measured pH level.
At the equivalence point, just enough strong base has been added to completely react with all the
weak acid. After the reaction, the only species present will be the conjugate base, A-. Since A- is
a conjugate base, it will accept a proton from water to reform HA and OH- in the equilibrium
reaction shown by:
A-(aq) + H2O(l) ⇌ HA(aq) + OH-(aq) (8)
The equilibrium constant expression is given by:

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.

Saponification: good for soap, bad for your skin


The process of making soap, called “saponification”, involves a reaction between weak fatty acids
from animals or plants, and lye, which is a solution of NaOH or KOH in water. The final soap product
consists of a fatty acid salt, which cleans by attracting grease and dirt to the nonpolar end of the
fatty acid chain, and water to the polar salt end. Saponification can also occur to the fatty acids in
skin, turning them into soap, which is why it’s important to be extra careful while handling strong
bases!

Learning Goals
The following is a list of skills that you will use in this experiment.

• Calculating volume and mass of reagents used to prepare


Laboratory solutions
• Performing a titration
• Properties of weak acids and bases (i.e. conjugate acid-base
Conceptual pairs, dissociation strength, equilibrium)
• Brønsted-Lowry acid base theory
• Properties of a weak acid/base titration curve
• Calculating acid-base dissociation constants
Data Analysis
• ICE tables
• Relationship between [H3O+] and pH

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.

Preparation for Next Lab


Before starting the Weak Acid Titration experiment, each pair of students needs to
dry a sample of solid sodium carbonate in preparation for next week’s Polyprotic
Acid experiment.
1. Fill one vial with approximately 1 g of anhydrous sodium carbonate.
2. Place the uncapped vial in your 100 mL beaker to keep the vial from spilling in
the oven.
3. Dry the sample in the oven for 1.5 hours. Do not adjust the temperature on
the oven. The temperature on the oven has been preset and will heat to the
correct temperature when the door remains closed.
4. After removing your sample from the oven, let it cool until it is warm but safe
to handle.
5. After the sample has cooled, carefully remove the vial from the beaker using
a test tube clamp and place it in the center of the desiccator in your locker. If
the lid of your desiccator can be removed easily, ask your TA for some vacuum
grease to properly seal your desiccator.

Stock Chemicals Used


Chemical Maximum Amount Used
6 M Acetic Acid < 10 mL
0.05% Thymolphthalein Indicator Drops Safety First
pH Meter Calibration Buffer, pH 4 Remember to
< 5 mL
(red) always wear gloves
pH Meter Calibration Buffer, pH 7 when handling all
< 5 mL
(yellow) acids and bases.
pH Meter Calibration Buffer, pH 10 Wear your goggles!
< 5 mL
(blue)
Sodium Carbonate(s) <1 g

53
Acid Dissociation Constants and the Titration of a Weak Acid

Part I. Solution Preparation


1. Prepare 200 mL of approximately 0.05 M acetic acid solution from 6 M
acetic acid.
a. Calculate the volume of stock solution required in this dilution.
b. Add the appropriate amount of 6 M acetic acid to approximately
150 mL of DI water in a 250 or 500 mL Erlenmeyer flask.
c. Add DI water to the flask until the solution level reaches 200 mL.
Safety First d. Mix well.
Before inverting the 2. Find your 1 L bottle of your standardized NaOH from the previous
NaOH bottle, make sure experiment. Before opening the bottle of NaOH, carefully invert it
it is properly capped.
several times to ensure that your solution is homogenized.
Part II. Weak Acid Strong Base Titration Curve
This 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.

Care of pH meter and pH electrodes


• Keep the tip of the electrode submerged in solution at all times.
• Never leave the electrode in deionized water.
• When rinsing the electrode use a light stream of deionized water.
• Be careful of the electrode when adding strong base or when stirring
the solution.
• After completing the experiment, store the electrode in the storage
solution provided. Additional storage solution is available in the
laboratory if needed.

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

2. Prepare your titrant.


a. Read and understand how to fill and use a buret by reading the
Common Laboratory Procedures section in the Appendix of this
manual. Failure to properly fill the buret properly can result in spills
and injuries.
b. Condition a 25 mL buret with your standardized NaOH solution.
Remember to check that the stopcock is closed before filling a buret.
While holding the buret at a safe level over the sink, use a beaker to
Lab Skill Tips
pour in your sodium hydroxide solution.
Read the buret at or
c. After conditioning, fill the buret to above the zero mark with a slightly below eye
beaker, dispel any air bubbles from the stopcock, and place the buret level. Do not hold your
in the buret clamp. Record the initial buret reading to two decimal hands or lab manual
places, eg. 1.24 mL. behind the buret.
You can hold a sheet of
3. Prepare your analyte. colored paper behind
the buret to read the
a. Using a 10 mL volumetric pipet, accurately transfer 30.00 mL of meniscus clearly.
0.05 M acetic acid to a 150 mL beaker.
b. To this solution, add 3–5 drops of thymolphthalein indicator and
carefully place a clean magnetic stir bar into the beaker, without
splashing.
4. Complete the titration set-up:
a. Set up the stir plate underneath the buret containing the sodium
hydroxide titrant.
b. Place the beaker containing your dilute acetic acid solution onto the
stir plate.
c. 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.
The Titration
5. First, you will perform a quick titration to find the approximate end
point.
To do so, you will add the titrant (0.2 M NaOH) in small increments,

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.

▶ Continue to SAVE your standardized 0.2 M HCl and 0.2 M


NaOH. You will use these solutions for the next 2 experiments.

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

Determining Kª of acetic acid prior to titration


1. Write down the chemical equation for the dissociation of acetic acid in water, which results in
acetate ion and hydronium ion (H3O+).
• Tip: equation (2) in the introduction is a generic version of this dissociation reaction.
2. Set up an “ICE” table for this reaction. “ICE” stands for “initial”, “change”, and “equilibrium”
concentrations. Complete the table using the molarity of acetic acid solution in your first trial
and a variable (i.e. “x”) to represent change in concentration over the course of dissociation.
Keep in mind that since water is a pure liquid, change in concentration is omitted from ICE
tables A sample ICE table has been provided below.

HA(aq) + H2O(l) ⇌ A-(aq) + H3O+


I molarity -- 0 0

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

Determining Ka of acetic acid at the midpoint


The midpoint of a titration occurs when ½ of the original acid has reacted with the added strong
base. This means ½ of the original acid remains in solution while ½ exists as the conjugate base. In
other words, the number of moles of the acid, HA, remaining in solution is equal to the number
of moles of conjugate base, A-, and thus [HA] = [A-].
1. For your first trial, determine the volume of NaOH necessary to reach the midpoint. This
should be equal to ½ of the volume required to reach the equivalence point.
2. Determine the pH of solution at the midpoint.
3. Examine the equilibrium constant equation for Ka for the dissociation of acetic acid. Given the
assumption that [HA] = [A-] at the midpoint, are there any simplifications that can be made
to this equation?
4. Using the midpoint pH, calculate the concentration of H3O+ at the midpoint.
5. Using the concentration of H3O+ at the midpoint and your simplified equation for Ka,
determine Ka of acetic acid at the midpoint.
6. Calculate Ka at the midpoint for each trial, and then determine the average Ka of acetic acid.
7. Calculate the standard deviation of the average Ka at the midpoint.
8. Calculate the 90% confidence limit for the average Ka at the midpoint.
Determining Ka of acetic acid at the equivalence point
When determining Ka at the equivalence point, there are two chemical reactions that need to
be considered: the reaction of acetic acid with sodium hydroxide, and the re-establishment of
dissociation equilibrium between acetic acid and its conjugate base
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.
• Tip: At the equivalence point, all moles of acetic acid have reacted with NaOH to become
acetate ion.
3. Use the initial molarity of acetic acid, the equivalence point volume of NaOH, and the starting
volume of acetic acid solution for your first trial to determine the concentration of acetate ion
at the equivalence point.
4. Write down the chemical equation for the re-establishment of dissociation equilibrium between
acetate ion and acetic acid.
• Tip: equation (8) in the introduction is a generic version of this reaction.
5. Set up an “ICE” table for this reaction. Complete the table for each trial, using the molarity
of acetate ion calculated above and a variable (i.e. “x”) to represent change in concentration.

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.

Carbonic acid in nature


The carbonic acid in our environment was formed by dissolving CO2 from the air into water, or
by water percolating through stone and rocks containing carbonate minerals. The carbonic acid
system plays a major role in the respiration of all animals, including humans. The equilibrium
among CO2(g), H2O(l), HCO3-(aq), and CO32-(aq) is critical for the proper transport of CO2, formed via
cellular metabolism, through the bloodstream to be expelled by the lungs. While carbonic acid is
not a strong acid by the dissociation definition, it is corrosive and does react with metals to form
carbonates.

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

HCO3-(aq) ⇌ H+(aq) + CO32-(aq) Ka2 = 4.7 × 10-11


Each of these dissociations is an equilibrium reaction with an acid dissociation constant. As a
result, calculating the concentrations of the species present in solution can become quite involved.

63
Polyprotic Systems

H+(aq) + CO32-(aq) ⇌ HCO3-(aq) Ka2 = 4.7 × 10-11


H+(aq) + HCO3-(aq) ⇌ H2CO3(aq) → H2O(l) + CO2(g) Ka1 = 4.4 × 10-7
We can also write the acid dissociation reactions of carbonic acid in reverse of the usual direction
to emphasize that we are starting from a solution of Na2CO3. Notice that during the titration you
will encounter the equivalence point of the second proton (Ka2) of diprotic carbonic acid as the
first observed equivalence point in the titration. It occurs at high pH. The first proton (Ka1) is
encountered as the second observed equivalence point in the titration. It occurs at low pH. One of
the goals of this experiment will be to make your own determinations of the two acid dissociation
constants of carbonic acid.
Because of the polyprotic nature of carbonic acid, the equilibrium analysis necessary to develop
the formulas for reduction of measurements of the pH into the acid dissociation constant are
somewhat involved for the second proton equilibrium (the first observed equivalence point that
you will encounter in the titration). We will not go through the details of the development, but will
just describe for you how to find the final formulas. You may want to go through the development
on your own, using the discussion as an aid to prove to yourself that the formulas are correct.
At the second proton equivalence point, the solution is identical in composition with a solution
of the sodium salt of the bicarbonate ion HCO3- (except for some extra dissolved NaCl(aq)). An
equilibrium treatment of the pH of that solution will yield precisely the formulas we need to work
with. The dominant species equilibria to be considered are:
HCO3-(aq) + H2O(l) ⇌ H2CO3(aq) + OH-(aq) Kb2 = Kw/Ka1
HCO3-(aq) + H2O(l) ⇌ H3O +(aq) + CO32-(aq) Ka2
We start by writing down the two conditions that are commonly referred to as a mass balance and a
charge balance. The mass balance sets the sum of all carbonate containing species equal to the total
concentration in the original sample as diluted to the present volume. The charge balance sets the
sum of the concentrations of all positively charged species equal to the sum of the concentrations
of all the negatively charged species (including the sodium cation needed for NaHCO3). These two
conditions are combined into an equality that must be observed.
We then use the two equilibrium expressions listed above and the Kw equilibrium to re-express
[H2CO3], [CO32-], and [OH-], and insert these into the combined equality. The combined equality
is then simplified and rearranged to get the result:

ାሿ
‫ܭ‬௔ଶ ሾ‫ܱܥܪ‬ଷ ି ሿ ൅ ‫ܭ‬௪
ሾ‫ܪ‬ଷ ܱ ൌඩ
ሾ‫ܱܥܪ‬ଷ ି ሿ
ͳ൅
‫ܭ‬௔ଵ

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:

ሾ‫ܪ‬ଷ ܱା ሿ ൌ ඥ‫ܭ‬௔ଵ ‫ܭ‬௔ଶ (1)

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

HCO3-(aq) ⇌ H+(aq) + CO32-(aq) Ka2


A fairly quick solution of these equilibria is available if Ka1 >> Ka2 because then we may assume that
the [H+] concentration arises dominantly from the first equilibrium, and then [H+] = [HCO3-].
Writing the equilibrium constant expressions:

ሾ‫ܪ‬ା ሿሾ‫ܱܥܪ‬ଷ ି ሿ ሾ‫ܪ‬ା ሿൣ‫ܱܥ‬ଷ ଶି ൧


‫ܭ‬௔ଵ ൌ Ǣ‫ܭ‬௔ଶ ൌ
ሾ‫ܪ‬ଶ ‫ܱܥ‬ଷ ሿ ሾ‫ܱܥܪ‬ଷ ି ሿ

Rearranging these expressions:

ሾ‫ܪ‬ା ሿሾ‫ܱܥܪ‬ଷ ି ሿ ି
ሾ‫ܪ‬ା ሿൣ‫ܱܥ‬ଷ ଶି ൧
ሾ‫ܪ‬ଶ ‫ܱܥ‬ଷ ሿ ൌ ǡ ሾ‫ܱܥܪ‬ଷ ሿ ൌ
‫ܭ‬௔ଵ ‫ܭ‬௔ଶ

Using substitution:

ሾ‫ܪ‬ା ሿଶ ൣ‫ܱܥ‬ଷ ଶି ൧
ሾ‫ܪ‬ଶ ‫ܱܥ‬ଷ ሿ ൌ
‫ܭ‬௔ଵ ‫ܭ‬௔ଶ

Since [H+] = [HCO3-], solving for [CO32-] in the previous expression gives:

ଶି ሾ‫ܱܥܪ‬ଷ ି ሿ
ൣ‫ܱܥ‬ଷ ൧ൌ ‫ܭ‬௔ଶ ൌ ‫ܭ‬௔ଶ
ሾ‫ ܪ‬ା ሿ

This reduces the expression for [H2CO3] to:

ሾ ‫ ܪ‬ା ሿଶ
ሾ‫ܪ‬ଶ ‫ܱܥ‬ଷ ሿ ൌ
‫ܭ‬௔ଵ

65
Polyprotic Systems

Now in a solution that is M molar in H2CO3, we must have:


[HCO3-]+ [CO32-] + [H2CO3] = M
[H2CO3] = M − ([HCO3-]+ [CO32-])
Since we are dealing with weak acid dissociation constants, we can expect

[HCO3-]+ [CO32-] << M


hence [H2CO3] = M
Using the concentrations in the expression for Ka1,

ሾ ‫ ܪ‬ା ሿଶ
‫ܭ‬௔ଵ ൌ
‫ܯ‬ (2)

ሾ‫ ܪ‬ሿ ൌ ඥ‫ܭܯ‬௔ଵ

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.

• Calculating volume and mass of reagents used to prepare


Laboratory solutions
• Performing a titration
Conceptual • Properties of polyprotic acids (i.e. multiple dissociations)
• Properties of a polyprotic acid titration curve
Data Analysis
• Calculating acid-base dissociation constants from [H3O+]

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.

Stock Chemicals Used Safety First


Chemical Maximum Amount Used Remember to always
0.04% Bromocresol Green Indicator Drops wear gloves and take
caution when handling
1% Phenolphthalein Indicator Drops
all acids and bases.
pH Meter Calibration Buffer, pH 4
< 5 mL Wear your goggles!
(red)
pH Meter Calibration Buffer, pH 7
< 5 mL
(yellow)
pH Meter Calibration Buffer, pH 10
< 5 mL
(blue)
Sodium Carbonate, (s) <1 g

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.

3. 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.
Care of pH meter and pH electrodes
• Keep the tip of the electrode submerged in solution at all times.
• Never leave the electrode in deionized water.
• When rinsing the electrode use a light stream of deionized water.
• Be careful of the electrode when adding strong base or when stirring
the solution.
• After completing the experiment, STORE THE ELECTRODE IN THE
STORAGE SOLUTION provided. Additional storage solution is available
in the laboratory if needed.

4. Complete the titration set-up:


a. Set up the stir plate underneath the buret containing the HCl titrant.
b. Place the titration vessel with your sodium carbonate solution onto
the stir plate.
c. To the titration vessel, add 3–5 drops of phenolphthalein indicator.
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 vessel, away from the side but with the
stopcock at a convenient location for you to manipulate. Position
the titration vessel so that the stir bar is somewhat displaced away

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.

▶ Continue to SAVE your standardized 0.2 M HCl and 0.2 M


NaOH. You will use these solutions for the next experiment.

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:

��� �� ���� �
�� �
����

If we take the −log of both sides then we have,

��
��� �
��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
ൌ ͳͲሺ௣ுି௣௄ೌ 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.

Table 1. pKa values for Acids used in the experiment


Name of Acid Dissociation Reaction pKa
Acetic acid CH3COOH(aq) + H2O(l) ⇌ H3O (aq) + CH3COO (aq)
+ - 4.74
Hydrogen carbonate ion HCO3-(aq) + H2O(l) ⇌ H3O+(aq) + CO32-(aq) 10.33

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.

Enzymes, the Goldilocks of chemical reactions


Enzymes play a critical role in catalyzing chemical reactions within living organisms. The activity
and function of an enzyme depends on its amino acid sequence. Intermolecular interactions
between amino acids are affected by whether they are protonated or deprotonated, which
in turn is affected by the pH of the surrounding environment. Enzymes can lose function or
denature completely if their surroundings are too acidic or basic, so buffers play an essential
role in maintaining environmental pH. For example, the cytoplasm within our cells contains a
buffering system consisting of monohydrogen phosphate (HPO42-) and dihydrogen phosphate
(H2PO4-). Monohydrogen phosphate has a pKa of 6.8, which makes it a good buffer for maintaining
an intracellular pH of about 7, the ideal pH for many enzymes in the human body.

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.)

Table 2 identifies the assigned pH values by group numbers. If you do not


complete the calculations before the laboratory session, you may not have time
to complete this experiment.

Table 2. pH of Buffer Solutions


Hint
Acidic Buffer Basic Buffer
Using M1V1=M2V2,
Group 1 4.5 10.0
calculate the volume of
Group 2 4.6 10.1 2.5 M sodium acetate
Group 3 4.7 10.2 solution needed to
prepare your dilute
Group 4 4.8 10.3 sodium acetate solution.
Group 5 4.9 10.4
Group 6 5.0 10.5

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.

• Using the Henderson-Hasselbalch equation to calculate


Laboratory buffered solutions of a specified pH
• Properties of buffers (i.e. resistance to pH change, presence
Conceptual of conjugate pairs)
• Generating and analyzing titration curves of a buffered
Data Analysis solution

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.

Stock Chemicals Used


Safety First
Chemical Maximum Amount Used
Remember to always
6 M Hydrochloric Acid According to calculation (< 10 mL) wear gloves and take
6 M Sodium Hydroxide According to calculation (< 10 mL) caution when handling
6 M Acetic Acid (CH3COOH) According to calculation (< 30 mL) all acids and bases.
2.5 M Sodium Acetate Wear your goggles!
According to calculation (< 25mL)
(NaCH3COO·3H2O)
Sodium Carbonate (Na2CO3) According to calculation (< 5 g)
Sodium Bicarbonate (NaHCO3) According to calculation (< 5 g)
pH Meter Calibration Buffer, pH 4
< 5 mL
(red)
pH Meter Calibration Buffer, pH 7
< 5 mL
(yellow)
pH Meter Calibration Buffer, pH 10
< 5 mL
(blue)

Part I. Preparing Your Buffers


You will be cooperating with another group of students to prepare two
250 mL buffer solutions, an acidic and a basic buffer. Divide the tasks
amongst yourselves so that each group receives approximately 120 mL of
the correct acidic buffer and 120 mL of the basic buffer at the end of Part I.
The acidic buffer will be prepared from a 6 M acetic acid (CH3COOH)
solution and 2.5 M sodium acetate trihydrate (NaCH3COO·3H2O). The
basic buffer solution is prepared from solid sodium hydrogen carbonate
(NaHCO3) and solid anhydrous sodium carbonate (Na2CO3). After
preparing the solutions you will measure the pH level of the solution and
adjust the levels by adding either strong acid or strong base as needed.

79
Acid-Base Buffers

1. Group Member Assignments: During the previous laboratory


experiment, the TA assigned your group a number between 1 and 6.
Work with the other group with the same buffer assignment to prepare
the 2 buffer solutions at the designated pH values given in Table 2.
Have one group prepare the 250 mL of the acidic buffer and the other

group prepare 250 mL of the basic buffer at the designated pH values.


2. Preparation of Acidic Buffer in a 250 mL volumetric flask:
a. Calculate the volume of 2.5 M sodium acetate solution needed to
prepare 250 mL of 0.10 M sodium acetate. DO NOT USE the 1.0
M sodium acetate.
b. First, transfer approximately 15 mL of the 2.5 M sodium acetate
solution into a small beaker, and then use a volumetric pipet to
transfer the appropriate volume—calculated from the previous
step—to your 250 mL volumetric flask. Add 120–150 mL of
deionized water to the 250 volumetric flask and mix.
c. Calculate the volume of 6 M stock acetic acid solution you need to
make 250 mL of the buffer solution to the designated pH.
d. Use your graduated cylinder to transfer this volume of 6 M acetic
acid to the volumetric flask. Using a water bottle, fill the flask to the
mark with deionized water to make a solution totaling 250 mL.
e. Mix the solution well, then transfer the solution to an appropriately
400 mL beaker.
3. Preparation of Basic Buffer in a 250 mL volumetric flask:
a. Calculate the mass of solid sodium hydrogen carbonate needed to
prepare 250 mL of 0.050 M sodium hydrogen carbonate solution.
b. Weigh out this mass of solid sodium hydrogen carbonate and
quantitatively transfer it to a clean 250 mL volumetric flask. Add
120–150 mL of deionized water to the 250 volumetric flask and
mix.
c. Calculate the mass of solid anhydrous sodium carbonate required to
make the basic buffer to the designated pH.
d. Weigh out this mass of anhydrous sodium carbonate and
quantitatively transfer it to your 250 mL volumetric flask. Now,
fill your flask to the mark with deionized water to make a solution
totaling 250 mL. After you have mixed the buffer solution well,
place the buffer solution into a clean and appropriately labeled 400
mL beaker.

80
Acid-Base Buffers

4. You will need to calibrate the pH meter at this point.


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.
Care of pH meter and pH electrodes
• Keep the tip of the electrode submerged in solution at all times.
• Never leave the electrode in deionized water.
• When rinsing the electrode use a light stream of deionized water.
• Be careful of the electrode when adding strong base or when stirring
the solution.
• After completing the experiment, store the electrode in the storage
solution provided. Additional storage solution is available in the
laboratory if needed.

5. Adjusting the pH of your buffer.


Your buffer solution may not be at the assigned pH. Use drop-wise

addition of 6 M HCl or 6 M NaOH to adjust the pH.


a. Measure the pH of your buffer.
b. Using a disposable pipet, add 6 M HCl drop-wise to lower the pH,
or add 6 M NaOH drop-wise to raise the pH.
c. Adjust the pH until it is equal to the assigned pH. Stir the solution
and record the pH to the nearest 0.02 pH unit.
d. Split the buffer between the groups. Carefully pour the buffers into
four labeled 250 mL Erlenmeyer flasks. Make sure that each group
has at least 80 mL of the acidic or basic buffer.

81
Acid-Base Buffers

Part II. Preparing Your Reagents


1. Find your 1 L bottle of your standardized HCl from the previous
Safety First
experiments. Before opening the bottle, carefully invert it several times
Before inverting the to ensure that your solution is uniform.
HCl and NaOH bottles,
make sure they are 2. Find your 1 L bottle of your standardized NaOH from the previous
properly capped.
experiments. Before opening the bottle, carefully invert it several times
to ensure that your solution is uniform.
3. Prepare 120 mL of 0.1 M acetic acid from the 6 M acetic acid stock
solution using a 150 mL beaker. Once the solution has been made,
transfer it to a 125 mL, 250 mL, or 500 mL Erlenmeyer flask for storage
Lab Skill Tips and label the Erlenmeyer flask with a graphite pencil.
Read the buret at or
slightly below eye 4. Condition and fill two 25 mL burets, one with the 0.2 M HCl solution
level. Do not hold your and the other buret with 0.2 M NaOH. Record the initial volume of
hands or lab manual HCl and NaOH to the nearest 0.02 mL.
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.

82
Acid-Base Buffers

Part III. Titration with 0.2 M HCl


In this part of the experiment, each group will treat each of the two buffer
solutions with 0.2 M HCl solution. You will add the titrant (0.2 M HCl)
in small increments throughout the titration. You will then plot the pH vs.
added volume of HCl to graphically observe the pH changes that occur.
You will also explore the effect of adding 0.2 M HCl to 0.1 M acetic acid
solution.

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.

1. Titrate the acidic buffer with 0.2 M HCl.


a. Place 40 mL of the acidic buffer in a clean 150 mL beaker. Gently
place a stir bar into the beaker.
b. Set up the beaker containing the buffer, stir plate, and pH electrode
under the buret containing the 0.2 M HCl solution. Start gently
rotating the stir bar. Record the initial buret reading and pH meter
reading.
c. Add HCl in 1 mL increments to the buffer until the pH of the
buffer has decreased by 1.5 pH units. Record the buret reading and
the pH reading after each addition.
d. Save this solution in an Erlenmeyer flask for use in the last part of
this experiment.

83
Acid-Base Buffers

2. Titrate the basic buffer with 0.2 M HCl.


a. Place 40 mL of the basic buffer in a clean 150 mL beaker. Gently
place a stir bar into the beaker.
b. Set up the beaker containing the buffer, stir plate, and pH electrode
under the buret containing the 0.2 M HCl solution. Start gently
rotating the stir bar. Record the initial buret reading and pH meter
reading.
c. Add HCl in 1 mL increments to the buffer until the pH of the
buffer has decreased by 1.5 pH units. Record the buret reading and
the pH reading after each addition.
d. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.
3. Titrate the 0.1 M acetic acid with 0.2 M HCl.
a. Place 40 mL of the 0.1 M acetic acid in a clean 150 mL beaker.
Gently place a stir bar into the beaker.
b. Set up the beaker containing the acetic acid solution, stir plate, and
pH electrode under the buret containing the 0.2 M HCl solution.
Start gently rotating the stir bar. Record the initial buret reading and
pH meter reading.
c. Add HCl in 1 mL increments to the buffer until the pH of the
solution has decreased by 1.5 pH units. Record the buret reading
and the pH reading after each addition.
d. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.

84
Acid-Base Buffers

Part IV. Titration with 0.2 M NaOH


In this part of the experiment each group will treat each of the two
buffer solutions with 0.2 M NaOH solution. You will add the titrant
(0.2 M NaOH) in small increments throughout the titration. You will
then plot the pH vs. added volume of NaOH to graphically observe the pH
changes that occur. You will also explore the effect of adding 0.2 M NaOH
to 0.1 M acetic acid solution.
1. Titrate the acidic buffer with 0.2 M NaOH.
a. Place 40 mL of the acidic buffer in a clean 150 mL beaker. Gently
place a stir bar into the beaker.
b. Set up the beaker containing the buffer, stir plate, and pH electrode
under the buret containing the 0.2 M NaOH solution. Start gently
rotating the stir bar. Record the initial buret reading and pH meter
reading.
c. Add NaOH in 1 mL increments to the buffer until the pH of the
buffer has increased by 1.5 pH units. Record the buret reading and
the pH reading after each addition.
d. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.
2. Titrate the basic buffer with 0.2 M NaOH.
a. Place 40 mL of the basic buffer in a clean 150 mL beaker. Gently
place a stir bar into the beaker.
b. Set up the beaker containing the buffer, stir plate, and pH electrode
under the buret containing the 0.2 M NaOH solution. Start gently
rotating the stir bar. Record the initial buret reading and pH meter
reading.
c. Add NaOH in 1 mL increments to the buffer until the pH of the
buffer has increased by 1.5 pH units. Record the buret reading and
the pH reading after each addition.
d. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.

85
Acid-Base Buffers

3. Titrate the 0.1 M acetic acid with 0.2 M NaOH.


a. Place 40 mL of the 0.1 M acetic acid in a clean 150 mL beaker.
Gently place a stir bar into the beaker.
b. Set up the beaker containing the acetic acid solution, stir plate, and
electrode under the buret containing the 0.2 M NaOH solution.
Start gently rotating the stir bar. Record the initial buret reading and
pH meter reading.
c. Add NaOH in 1 mL increments to the buffer until the pH of the
solution has increased by 1.5 pH units. Record the buret reading
and the pH reading after each addition.
d. When you have completed this titration, pour the solution in the
titration vessel into an 800 mL beaker.
4. Titrate your acetic acid buffer/HCl solution with 0.2 M NaOH.
a. Transfer the acidic buffer/HCl mixture from Part III step 1 to a
clean 150 mL beaker. Gently place a stir bar into the beaker.
b. Set up the beaker containing acetic acid buffer/HCl solution, stir
plate, and pH electrode under the buret containing the 0.2 M
NaOH solution. Start gently rotating the stir bar. Record the initial
buret reading and pH meter reading.
c. Add NaOH in 1 mL increments to the buffer until the pH of the
solution has increased by 3.0 pH units. Record the buret reading
and the pH reading after each addition.
d. When you have completed this titration, dispose of this solution
down the sink with copious amount of water.

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 ൌ ߛு௚మమశ 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.

Table 1. Activity Coefficients for Aqueous Solution at 25˚C


Ionic Strength (μ, M)
Ion 0.001 0.005 0.01 0.05 0.1 0.15
H +
0.967 0.933 0.914 0.86 0.83 0.81
Li +
0.965 0.929 0.907 0.835 0.80 0.77
Na , IO , HCO , H2PO
+
3
-
3
-
4
-
0.964 0.928 0.902 0.82 0.775 0.76
OH-, F-, SCN-, MnO4-, ClO4- 0.964 0.926 0.900 0.81 0.76 0.73
K , Cl , Br , I , CN , NO3
+ - - - - -
0.964 0.925 0.899 0.805 0.755 0.72
Rb , Cs , NH , Ag
+ +
4
+ +
0.964 0.924 0.898 0.80 0.75 0.71
Mg , Be 2+ 2+
0.872 0.755 0.69 0.52 0.45 0.41
Ca , Cu , Zn , Mn
2+ 2+ 2+ 2+
0.870 0.749 0.675 0.485 0.405 0.36
Sr , Ba , Cd , Hg , S
2+ 2+ 2+ 2+ 2-
0.868 0.744 0.67 0.465 0.38 0.33
Pb , CO , SO
2+
3
2-
3
2-
0.867 0.742 0.665 0.455 0.37 0.31
Hg , SO , CrO , HPO
2
2+
4
2-
4
2-
4
2-
0.867 0.740 0.660 0.445 0.355 0.30
Al3+, Fe3+, Cr3+ 0.738 0.54 0.445 0.245 0.18 0.15
PO 4
3-
0.725 0.505 0.395 0.16 0.095 0.066
Sn 4+
0.588 0.35 0.255 0.10 0.065 0.048
Source: Data from J. Kielland, J. Amer. Chem. Soc., 59, 1675 (1937)

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

CaF2(s) ⇌ Ca2+(aq) + 2F−(aq) K = 3.9 × 10-11

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

The Solvay Process


Sodium carbonate, commonly known as soda ash or washing soda, is a chemical used in many
products, ranging from glass to toothpaste to moon cakes. The majority of sodium carbonate
produced today comes from the Solvay process, which was developed by the Belgian chemist
Ernest Solvay in the 1860s. The Solvay process takes advantage of the common ion effect to
precipitate sodium bicarbonate (NaHCO3) from a saturated solution of sodium chloride (NaCl),
ammonia (NH3), and carbon dioxide (CO2). The sodium bicarbonate can then be heated to form
sodium carbonate (Na2CO`). The Solvay process is cheaper and less environmentally harmful than
older practices, which involved burning plants or producing toxic byproducts such as HCl gas.
Comparatively, the Solvay process commonly uses ocean brine as a source of NaCl, limestone as a
source of CO2, and the ammonia can be recycled back into production.

Learning Goals
The following is a list of skills that you will use in this experiment.

• Planning and implementing a titration procedure


Laboratory
• Using a starch indicator
• Solubility product constant (Ksp)
• Solubility (x)
Conceptual • Activity coefficients (γ)
• Ionic strength (μ)
• Common Ion Effect
• Calculating solubility product constants using concentration
Data Analysis
• Calculating solubility product constants using activity

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.

Stock Chemicals Used


Chemical Maximum Amount Used
Potassium Iodate, (s) According to calculation (< 1 g) Safety First
Potassium Iodide, (s) According to calculation (< 7 g) Remember to always
1 M Sodium Thiosulfate According to calculation (< 15 mL) wear gloves when
handling all solids.
Saturated Calcium Iodate, (aq) < 10 mL
0.1 M Potassium Iodate in Saturated Wear your goggles!
< 10 mL
Calcium Iodate, (aq)
Starch Indicator Small amounts (< 10 mL)
6 M Hydrochloric Acid < 6 mL

Part I. Preparation of a Potassium Iodate Solution Safety First


In this procedure you will prepare a standard potassium iodate solution

The potassium iodate
for use in standardizing a sodium thiosulfate solution. primary standard is being
dried in the oven. Be
Using a volumetric flask, accurately prepare 250 mL of a solution of careful! The container
is extremely hot.

approximately 0.01 M KIO3. Note that this will need to be made as


accurately as possible since this solution will serve as the primary standard Always use crucible
tongs to manipulate
for the experiment. The solid will take a few moments to dissolve. While
the container.
you are waiting, go on to Part II.
Part II. Preparation of a Sodium Thiosulfate Solution
In this procedure you will prepare and standardize a sodium thiosulfate

Hint
solution. You will use the standard KIO3 solution prepared in Part I Using M1V1=M2V2,
to standardize the sodium thiosulfate solution. The sodium thiosulfate calculate the volume
of 1.0 M sodium
solution will then become a secondary standard. thiosulfate solution
needed to prepare
Using your clean 1 L plastic bottle, prepare about 250 mL of a
your dilute solution.

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

Part III. Standardization of the Sodium Thiosulfate Solution


1. Standardize the sodium thiosulfate solution with the potassium iodate
solution you have prepared. You should use the iodate-to-iodine and
iodine-to-iodide reactions given in the introduction of the experiment.
You will have to plan how to best perform this experiment.
Green Chem
2. For the first reaction you will need excess potassium iodide and
Do not waste chemicals. hydrochloric acid. If you were using a 5 mL sample of the standard
You should be using
no more than a
potassium iodate solution it would require about 1 g of potassium iodide
couple of grams of and about 1 mL of 6 M hydrochloric acid.
potassium iodide and
a few milliliters of acid a. Begin by dissolving the potassium iodide (KI) in about 50 mL of water
in each titration. in your titration flask. Next, accurately add 5.00 mL of potassium
iodate using volumetric glassware. Finally, add the hydrochloric
acid. The solution will turn brown due to the formation of iodine.
Tip b. Immediately titrate the solution with the sodium thiosulfate solution
Do not add the starch
until the solution in the titration flask becomes a pale yellow color
indicator until the brown indicating only a limited amount of iodine present. At this point
solution has lightened add 1 mL of the starch indicator. The starch will react with the I3- to
to a pale yellow. form a complex that is dark blue in color. Continue the titration
until the dark blue color disappears. This is the end point.
3. When you have completed each titration, pour the solution in the
titration flask into an 800 mL beaker.
4. Do at least three acceptable titrations so that you can calculate a
meaningful average sodium thiosulfate concentration, standard deviation
and 90% confidence limit for your data. An acceptable trial is one that
passes the Q-test.

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

Part IV. Solubility and Solubility Product from a Saturated


Calcium Iodate Solution
1. Determine the iodate concentration in a saturated solution of calcium
iodate using your standard sodium thiosulfate solution. You should use
the same procedure you developed for the thiosulfate standardization,
but this time you will use a saturated calcium iodate solution instead of
a potassium iodate solution when performing the first reaction.
The saturated calcium iodate solution will be provided by the stockroom.

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

the 5.00 mL of saturated Ca(IO3)2 in 0.010 M KIO3 solution for the


titration.
3. When you have completed this titration, pour the solution in the
titration flask into an 800 mL beaker.

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

Calculating solubility product (Ksp) of Ca(IO3)2 in pure water based on


concentration
You will start your analysis of solubility product constants by calculating Ksp of Ca(IO3)2 using only
concentration. As you read in the Introduction, this method of calculating Ksp assumes that the
activity coefficients (γ) of each ion is equal to 1.
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.
3. Use the solubility (x) of Ca(IO3)2 that you determined in step 5 of "Calculating solubility (x)
of Ca(IO3)2 in pure water" to solve for the solubility product, Ksp, of Ca(IO3)2.
Calculating solubility product (Ksp) of Ca(IO3)2 in pure water based on activity
Now you will do a more in-depth calculation of solubility product constants by calculating Ksp of
Ca(IO3)2 using both concentration and activity. This method of calculating Ksp takes into account
interactions between ions in solution.
1. Use equation (4) from the Introduction to write out an equation calculating the ionic strength
(μ) of Ca(IO3)2 in pure water using the concentration (ci) and charge (Zi) of each ion.
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.
3. Use the solubility (x) of Ca(IO3)2 you previously calculated to solve for the ionic strength (μ)
of Ca(IO3)2 in pure water.
4. Use Table 1 in the Introduction and your calculated ionic strength (μ) to find the activity
coefficients (γ) for Ca2+ and Ca(IO3)2.
5. Write an equation that describes the solubility product, Ksp, of Ca(IO3)2 in pure water 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.
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 pure water.
Determining solubility (x) of Ca(IO3)2 in 0.01 M KIO3
You will now study the Common Ion Effect by calculating the solubility of Ca(IO3)2 in a solution
already containing 0.01 M KIO3. When you do this calculation, make sure that you account for
the fact that 0.010 M of IO3- does not come from the dissolved Ca(IO3)2, but the KIO3 instead.
1. In your titration of saturated Ca(IO3)2 solution in 0.01 M KIO3, what volume of standardized
Na2SO3 was required to reach the endpoint?

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

Revision Date: June 2023


Appendix Table of Contents
General Experimental Guidelines A-5
1. Pre-Laboratory Preparation
2. Data Collection
3. Unknowns
4. Writing A Laboratory Report

Laboratory Work Grading Policies A-7


Late Reports & Make-Up Policy A-8
1. Late Reports
2. Laboratory Make-Up Policy
3. Laboratory Make-up Procedure
4. Plagiarism and Unauthorized Collaboration

Chemistry Department Safety Policy A-9


Safety in the Chemistry 2 Laboratories A-11
Safe Laboratory Practices A-11
1. Work Under Supervision
2. Follow Instructions
3. Safety Equipment
4. Practice Good Housekeeping
5. Avoid Chemical Contamination
Personal Protective Equipment (PPE)  A-13
1. Dress Code
2. Goggles
3. Lab Coat
4. Gloves

Maps and Emergency Evacuation Procedures A-15


1. Prior to Exiting
2. Evacuation Routes/Exiting the Building
3. Assembly Area

General Emergency Procedures A-19


1. Medical Emergency
2. Major Incident
3. Fire Alarm

Dispensary Procedures A-20


Safety Data Sheet A-21
Hazardous Chemicals A-30
Hazardous Chemicals A-30
Hazardous Waste A-31
Statistical Treatment of Data A-33
1. Average and Standard Deviation
2. Confidence Limits
3. Relative Deviation
4. Analysis of Poor Data: Q-test

An Introduction to Excel A-37


Excel Basics A-38
Calculations in Excel A-42
Graphing in Excel A-45
Common Laboratory Procedures A-49
Handling Solids A-49
1. General Guidelines for Handling Solids
2. Quantitative Transfer
3. Using the Desiccator
Handling Liquids A-51
1. Drawing Solutions from a Reagent Bottle
2. Estimating Volume with a Dispo Pipet
3. Transferring Liquid
4. Capping a Flask with Parafilm
5. Measuring Liquid Volumes
Common Glassware in the Laboratory A-54
1. Care and Maintenance of Laboratory Glassware
2. Beakers
3. Erlenmeyer Flasks
4. Graduated Cylinder
5. Volumetric Flasks
6. Burets
7. Volumetric Pipet
Using the Balance A-60
1. On/Off Switching
2. Simple Weighing
3. Taring
4. Weighing by Difference
Using the Centrifuge A-62
1. Procedure
2. Safety Precautions
Using the Hot Plate A-63
1. Features
2. Safety Precautions
Heating with a Bunsen Burner A-65
Filtration A-66
Setting up a Titration Apparatus A-67
pH Meter Operating Instructions A-68
1. Preparing the pH meter
2. Calibrating the pH meter
3. Measure the pH of sample
Fume Hood Use and Safety A-71
1. Features of the Fume Hood
2. Before using the fume hood
3. Guidelines for working with the fume hood
4. Using the fume hoods in the Chemistry 2 Laboratories
5. Fume Hood Emissions

Locker Inventory A-75


Start of Quarter Check-In A-75
End of Quarter Check-Out A-76
General Experimental Guidelines

General Experimental Guidelines


The laboratory is a critical component of your study of chemistry. Therefore, a student must
complete all of the assigned laboratory work, including all on- & off-line post-laboratory
exercises, in order to pass this course.
1. Pre-Laboratory Preparation
• You are required to prepare for each experiment by doing the following:
• Carefully read the experiment and write a Title, Purpose, Procedure (brief outline), and
Data (outline) section before arriving at the laboratory. A detailed description of each
section is described below under, “Writing a Laboratory Report”.
• You must complete the on-line pre-laboratory presentation and must pass the pre-
laboratory quiz.
If you have not completed the pre-lab preparation at the beginning of the laboratory period,

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.

4. Writing A Laboratory Report


Below is the suggested format that your report should follow. Portions of the report should be

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.

• Questions: All assigned questions are answered in this section.

• Results & Conclusions: Report the outcome of the experiment.

A-6
Laboratory Work Grading Policies

Laboratory Work Grading Policies


1. Pre-lab lab notebook preparation incomplete:
• 30% of post-lab score deduction for first offense.
• 70% of post lab score deduction for subsequent offenses.
• No extra time or make-up
2. Online Pre-lab quiz failed or incomplete 1 hour before lab begins:
• 0/2 points for the pre-lab quiz
3. Late reports
• 5-point deduction for every calendar day the report is late

A-7
Late Reports & Make-Up Policy

Late Reports & Make-Up Policy


1. Late Reports
Laboratory reports are due at the beginning of the period after the one allocated for the

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.

2. Laboratory Make-Up Policy


You must attend the laboratory class for the section in which you are enrolled. If you miss

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.

3. Laboratory Make-up Procedure


If you miss a lab, you must make it up by attending another scheduled laboratory section. It is

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.

4. Plagiarism and Unauthorized Collaboration


Some of your experiments will be done with lab partners. You are encouraged to discuss your

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

Chemistry Department Safety Policy


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.
5. 100% cotton lab coats are REQUIRED.
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.
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.
9. Confine long hair while in the laboratory.
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.

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

Safety in the Chemistry 2 Laboratories


Students are an integral part of accident and injury prevention effort. The laboratory safety rules
require the students to follow Safe Laboratory Practices and wear the proper Personal Protective
Equipment (PPE).

Safe Laboratory Practices


Using safe laboratory practices prevents most accidents and injuries from occurring. Remember
that you are sharing the same work area with 23 other students. Any unsafe practices on the part of
your fellow students may end up injuring you or others. Courteously correct unsafe lab practices
you may encounter or report them to your TA. Laboratory safety is a communal effort.
1. Work Under Supervision
Your TA must be present to supervise all experiments. If your TA is incapacitated, contact dispensary
staff immediately.
Report all accidents and injuries to your TA, no matter how small.

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.

4. Practice Good Housekeeping


•Keep work area organized. Don’t put glassware on edges where they may fall off.
•Cap all bottles and close all drawers immediately.
•Clean up all spills and broken glassware immediately.

5. Avoid Chemical Contamination


•Do not bring food and drinks into labs.
Do not consume or use food, beverage, medicine, chewing gum, or tobacco, apply makeup or

contact lenses in the laboratory.


Take off one glove when leaving the laboratory. Do not touch anything outside the laboratory

with your laboratory gloves.


•Wash your hands thoroughly before leaving the lab.

A-12
Safety in the Chemistry 2 Laboratories

Personal Protective Equipment (PPE)


Students must come to the laboratory section with the appropriate personal protective equipment.
The PPE is the last line of defense against chemical hazards in the laboratory. Failure to don the
appropriate PPE will result in your removal from the laboratory. Many students may find it helpful
to keep a bag dedicated to chemistry lab courses with the proper clothing and PPE and change into
them before class.
1. Dress Code
Clothing worn in the laboratory should be able to protect you from small splashes and spills

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

Maps and Emergency Evacuation Procedures


1. Prior to Exiting
•After being notified to evacuate, cease all work activities and evacuate immediately.
•Stop all reactions and turn off all sources of ignition.
Close, but do not lock, the doors. Take your purse, briefcase, backpack and keys with you if

possible. Remember that you may not be allowed back into the building for an extended time.

2. Evacuation Routes/Exiting the Building


During an emergency evacuation, use the nearest door or stairway if available to exit the

building. Do not use elevators for fire/earthquake evacuations.


•Be aware of at least two exit routes in the event one is compromised.

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

roll to ensure all occupants have safely evacuated the building.

A-15
Maps and Emergency Evacuation Procedures

Figure 1. Evacuation routes for the 1st floor SLB rooms.

A-16
Maps and Emergency Evacuation Procedures

Figure 2. Evacuation routes for the 2nd floor SLB rooms.

A-17
Maps and Emergency Evacuation Procedures

Figure 3. The assembly area for Chemistry 2 students and personnel.

A-18
General Emergency Procedures

General Emergency Procedures


The following are some general instructions for actions to take in case of an emergency:
1. Medical Emergency
1) Remain calm.
2) Initiate lifesaving measures if required.
3) TA will call for the dispensary supervisor and/or for Emergency Response—CALL 911.
4) Do not move injured persons unless it is necessary to prevent further harm.
5) Keep injured person warm.
2. Major Incident
1) Alert TA to injured or contaminates persons.
2) Alert people to evacuate the area.
3) TA will call for the dispensary supervisor and/or Emergency Response—CALL 911.
•Fire 911
•Chemical, radiation, biological spill 911
•(Evenings and Weekends) 911
4) Close doors to affected areas.
5) Have person knowledgeable of incident inform the TA.
3. Fire Alarm
1) When fire alarm sounds, evacuate the room and follow evacuation plan to the Assembly
Area. The Assembly Area is on the south side of the large tree, which is on the west side of
the Sciences Lab Building.
2) TAs must take roll to ensure all students are accounted for.
3) If the building is cleared, you will return to continue your lab.

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

Safety Data Sheet


The Safety Data Sheet (SDS) is a document that provides information to enable users of a
substance or mixture to take the necessary measures relating to protection of health and safety
at the workplace, and the protection of the environment. A Safety Data Sheet has the following
sections:
1. Identification:
2. Hazard identification;
3. Composition/information on ingredients;
4. First-aid measures;
5. Fire-fighting measures;
6. Accidental release measures;
7. Handling and storage;
8. Exposure controls/personal protection;
9. Physical and chemical properties;
10. Stability and reactivity;
11. Toxicological information;
12. Ecological information;
13. Disposal considerations;
14. Transport information;
15. Regulatory information;
16. Other information.
A list of SDS resources may be found at: http://ehs.ucop.edu/sds
The following pages show a sample SDS for the 6 M Hydrochloric Acid commonly used in the
CHE2 laboratory courses.

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)

Cat No. : SA56-1; SA56-4; SA56-200; SA56-500


Synonyms Chlorohydric acid; Hydrogen chloride solution.; Muriatic acid

Recommended Use Laboratory chemicals.

Uses advised against No Information available


Details of the supplier of the safety data sheet

Company Emergency Telephone Number


Fisher Scientific CHEMTREC“, Inside the USA: 800-424-9300
One Reagent Lane CHEMTREC“, Outside the USA: 001-703-527-3887
Fair Lawn, NJ 07410
Tel: (201) 796-7100

2. Hazard(s) identification
Classification
This chemical is considered hazardous by the 2012 OSHA Hazard Communication Standard (29 CFR 1910.1200)

Corrosive to metals Category 1


Skin Corrosion/irritation Category 1 B
Serious Eye Damage/Eye Irritation Category 1
Specific target organ toxicity (single exposure) Category 3
Target Organs - Respiratory system.

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

3. Composition / information on ingredients


Component CAS-No Weight %
Water 7732-18-5 >78
Hydrochloric acid 7647-01-0 22

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
______________________________________________________________________________________________

medical attention is required.

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.

Unsuitable Extinguishing Media No information available

Flash Point No information available


Method - No information available

Autoignition Temperature No information available


Explosion Limits
Upper No data available
Lower No data available
Sensitivity to Mechanical Impact No information available
Sensitivity to Static Discharge No information available

Specific Hazards Arising from the Chemical


Non-combustible, substance itself does not burn but may decompose upon heating to produce corrosive and/or toxic fumes.

Hazardous Combustion Products


Hydrogen chloride gas Carbon monoxide (CO) Carbon dioxide (CO2) Hydrogen
Protective Equipment and Precautions for Firefighters
As in any fire, wear self-contained breathing apparatus pressure-demand, MSHA/NIOSH (approved or equivalent) and full
protective gear.

NFPA
Health Flammability Instability Physical hazards
3 0 1 N/A

6. Accidental release measures


Personal Precautions Use personal protective equipment. Ensure adequate ventilation. Evacuate personnel to
safe areas.
Environmental Precautions Should not be released into the environment. See Section 12 for additional ecological
information.

Methods for Containment and Clean Soak up with inert absorbent material. Keep in suitable, closed containers for disposal.
Up

7. Handling and storage


Handling Use only under a chemical fume hood. Ensure adequate ventilation. Wear personal
protective equipment. Do not get in eyes, on skin, or on clothing. Do not breathe vapors or
spray mist. Do not ingest.

Storage Keep containers tightly closed in a dry, cool and well-ventilated place.

8. Exposure controls / personal protection


Exposure Guidelines

______________________________________________________________________________________________

Page 3 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________

Component ACGIH TLV OSHA PEL NIOSH IDLH


Hydrochloric acid Ceiling: 2 ppm Ceiling: 5 ppm IDLH: 50 ppm
Ceiling: 7 mg/m3 Ceiling: 5 ppm
(Vacated) Ceiling: 5 ppm Ceiling: 7 mg/m3
(Vacated) Ceiling: 7 mg/m3

Component Quebec Mexico OEL (TWA) Ontario TWAEV


Hydrochloric acid Ceiling: 5 ppm Ceiling: 5 ppm CEV: 2 ppm
Ceiling: 7.5 mg/m3 Ceiling: 7 mg/m3
Legend

ACGIH - American Conference of Governmental Industrial Hygienists


OSHA - Occupational Safety and Health Administration
NIOSH IDLH: The National Institute for Occupational Safety and Health Immediately Dangerous to Life or Health

Engineering Measures Use only under a chemical fume hood. Ensure that eyewash stations and safety showers
are close to the workstation location.

Personal Protective Equipment

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.

9. Physical and chemical properties


Physical State Liquid
Appearance Clear
Odor pungent
Odor Threshold No information available
pH 1
Melting Point/Range -74 °C / -101.2 °F
Boiling Point/Range 81.5 - 110 °C / 178.7 230 °F @ 760 mmHg
Flash Point No information available
Evaporation Rate > 1.00 (Butyl Acetate = 1.0)
Flammability (solid,gas) Not applicable
Flammability or explosive limits
Upper No data available
Lower No data available
Vapor Pressure 5.7 mmHg @ 0 °C
Vapor Density 1.26
Specific Gravity 1.0 - 1.2
Solubility Miscible with water
Partition coefficient; n-octanol/water No data available
Autoignition Temperature No information available
Decomposition Temperature No information available
Viscosity No information available

10. Stability and reactivity

______________________________________________________________________________________________

Page 4 / 8
Hydrochloric Acid Solution, 6N (Certified) Revision Date 24-Feb-2014
______________________________________________________________________________________________

Reactive Hazard None known, based on information available

Stability Stable under normal conditions. Water reactive.

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 Polymerization Hazardous polymerization does not occur.

Hazardous Reactions May react with metals and lead to the formation of flammable hydrogen gas. Corrosive to
metals.

11. Toxicological information


Acute Toxicity

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

Toxicologically Synergistic No information available


Products
Delayed and immediate effects as well as chronic effects from short and long-term exposure

Irritation Causes burns by all exposure routes

Sensitization No information available

Carcinogenicity The table below indicates whether each agency has listed any ingredient as a carcinogen.

Component CAS-No IARC NTP ACGIH OSHA Mexico


Water 7732-18-5 Not listed Not listed Not listed Not listed Not listed
Hydrochloric acid 7647-01-0 Not listed Not listed Not listed Not listed Not listed
Mutagenic Effects No information available

Reproductive Effects No information available.

Developmental Effects No information available.

Teratogenicity No information available.

STOT - single exposure Respiratory system


STOT - repeated exposure None known

Aspiration hazard No information available

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
______________________________________________________________________________________________

12. Ecological information


Ecotoxicity
Do not empty into drains.

Component Freshwater Algae Freshwater Fish Microtox Water Flea


Hydrochloric acid - 282 mg/L LC50 96 h - -
Persistence and Degradability Persistence is unlikely based on information available.
Bioaccumulation/ Accumulation No information available.

Mobility No information available.

13. Disposal considerations


Waste Disposal Methods Chemical waste generators must determine whether a discarded chemical is classified as a
hazardous waste. Chemical waste generators must also consult local, regional, and
national hazardous waste regulations to ensure complete and accurate classification.

14. Transport information


DOT
UN-No UN1789
Proper Shipping Name HYDROCHLORIC ACID SOLUTION
Hazard Class 8
Packing Group II
TDG
UN-No UN1789
Proper Shipping Name HYDROCHLORIC ACID SOLUTION
Hazard Class 8
Packing Group II
IATA
UN-No UN1789
Proper Shipping Name HYDROCHLORIC ACID SOLUTION
Hazard Class 8
Packing Group II
IMDG/IMO
UN-No UN1789
Proper Shipping Name HYDROCHLORIC ACID, SOLUTION
Hazard Class 8
Packing Group II
15. Regulatory information
International Inventories

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
______________________________________________________________________________________________

U.S. Federal Regulations

TSCA 12(b) Not applicable

SARA 313
Component CAS-No Weight % SARA 313 - Threshold
Values %
Hydrochloric acid 7647-01-0 22 1.0

SARA 311/312 Hazard Categories


Acute Health Hazard Yes
Chronic Health Hazard No
Fire Hazard No
Sudden Release of Pressure Hazard No
Reactive Hazard No

CWA (Clean Water Act)


Component CWA - Hazardous CWA - Reportable CWA - Toxic Pollutants CWA - Priority Pollutants
Substances Quantities
Hydrochloric acid X 5000 lb - -

Clean Air Act


Component HAPS Data Class 1 Ozone Depletors Class 2 Ozone Depletors
Hydrochloric acid X -

OSHA Occupational Safety and Health Administration


Not applicable

Component Specifically Regulated Chemicals Highly Hazardous Chemicals


Hydrochloric acid - TQ: 5000 lb
CERCLA

Component Hazardous Substances RQs CERCLA EHS RQs


Hydrochloric acid 5000 lb 5000 lb
California Proposition 65 This product does not contain any Proposition 65 chemicals

U.S. State Right-to-Know


Regulations
Component Massachusetts New Jersey Pennsylvania Illinois Rhode Island
Water - - X - -
Hydrochloric acid X X X X X

U.S. Department of Transportation

Reportable Quantity (RQ): N


DOT Marine Pollutant N
DOT Severe Marine Pollutant N

U.S. Department of Homeland Security


This product contains the following DHS chemicals:

Component DHS Chemical Facility Anti-Terrorism Standard


Hydrochloric acid 0 lb STQ (anhydrous); 11250 lb STQ (37% concentration or
greater)
Other International Regulations

Mexico - Grade No information available

______________________________________________________________________________________________

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

WHMIS Hazard Class E Corrosive material

16. Other information


Prepared By Regulatory Affairs
Thermo Fisher Scientific
Email: [email protected]

Creation Date 24-Aug-2009


Revision Date 24-Feb-2014
Print Date 24-Feb-2014
Revision Summary This document has been updated to comply with the US OSHA HazCom 2012 Standard
replacing the current legislation under 29 CFR 1910.1200 to align with the Globally
Harmonized System of Classification and Labeling of Chemicals (GHS)
Disclaimer
The information provided in this Safety Data Sheet is correct to the best of our knowledge, information and belief at the
date of its publication. The information given is designed only as a guidance for safe handling, use, processing, storage,
transportation, disposal and release and is not to be considered a warranty or quality specification. The information
relates only to the specific material designated and may not be valid for such material used in combination with any other
materials or in any process, unless specified in the text

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.

DO NOT FILL ABOVE THIS LINE

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

FOR Chemical Waste


Composition:
WASTE Aluminum, Bismuth, Chromium,

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.

KEEP BOTTLE UNCAPPED


DO NOT REMOVE FROM FUMEHOOD DO N
CALL DISPENSARY WHEN FULL CA
HAZARDOUS WASTE H
Chem 2C Experiment C
Qualitative Analysis Q
Chemical Waste Composition:
Chloroform, Acetone,
Dithizone,

WASTE ONLY
DO NOT LEAVE BOTTLE UNCAPPED DO
-Flammable-
Toxic

A-32
Statistical Treatment of Data

Statistical Treatment of Data


Every measurement made in the laboratory is subject to error. Although you should try to minimize
error, two types of errors will occur. Systematic or Determinate Errors are those errors which are
reproducible and which can be corrected. Examples are errors due to a miscalibrated piece of
glassware or a balance that consistently weighs light. Random or Indeterminate Errors are due
to limitations of measurement that are beyond the experimenter’s control. These errors cannot
be eliminated and lead to both positive and negative fluctuations in successive measurements.
Examples are a difference in readings by different observers, or the fluctuations in equipment due
to electrical noise.
You will be graded by your ability to obtain accurate results. Accuracy describes how close your
result is to the true value. Another related term is precision. Precision describes how close your
results from different trials are to each other. Data of high precision indicates small random errors
and leads experimenters to have confidence in their results. Data that is highly accurate suggests
that there is little systematic error. A well-designed experiment (and a well-trained experimenter)
should yield data that is both precise and accurate.
In an effort to describe and quantify the random errors which will occur during the course of
the Chemistry 2 laboratory you will be asked to report an average, a standard deviation, a 90%
confidence limit, and a relative deviation. You may also have to analyze multiple trials to decide
whether or not a certain piece of data should be discarded. The following sections describe these
procedures.
1. Average and Standard Deviation
The average or mean, 𝑥𝑥̅ , is defined by

∑ 𝑥𝑥�
𝑥𝑥̅ �
𝑛𝑛

where each xi is one measurement and n is the number of trials.


The standard deviation, s, measures how close values are clustered about the mean. The standard
deviation for small samples is defined by

∑��� � �̅ ��
���
��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:

Number of Trials tcritical


(n)
2 6.314
3 2.920
4 2.353
5 2.132
6 2.015

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 2.920 4.303 9.925

4 2.353 3.182 5.841

5 2.132 2.776 4.604

6 2.015 2.571 4.032

∞ 1.645 1.960 2.576

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.

4. Analysis of Poor Data: Q-test


Sometimes a single piece of data is inconsistent with other data. You need a method to determine,
or test, if the data in question is so poor that it should be excluded from your calculations. Many
tests have been developed for this purpose. One of the most common is what is known as the
Q-test. To determine if a data should be discarded by this test you first need to calculate the
difference of the data in question from the data closest in value (this is called the “gap”). Next,
you calculate the magnitude of the total spread of the data by calculating the difference between
the data in question and the data furthest away in value (this is called the “range”). You will then
calculate the QData, given by
𝑔𝑔𝑔𝑔𝑔𝑔
𝑄𝑄���� �
𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟

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).

Number of Trials QCritical


3 0.94

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

Figure 3. A blank spreadsheet in Excel 2016.


The gray rectangles that make up the spreadsheet are called cells, and the active cell, or the cell

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

cell, the formula bar displays the text in the cell.


The ribbon menu contains a variety of commands to edit and manipulate the data in the

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

from the same trial are in the same row.


In this example, we also include a header row to help keep track of the data columns, although

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

Figure 4. Sample data from 2A, Volumetric Analysis.


3. If we need to enter a series of equal intervals, such as a set of increasing wavelengths or time
intervals, we can take advantage of Excel’s auto-fill feature by using the fill handle at the
bottom of an active area to quickly enter that series.
Enter the first few values from your series. Then, click on the top-most cell containing data to

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.

Figure 5. Using the Fill Handle to expand a series of increasing wavelengths.


The fill handle can be used across columns or rows, and can also be used to expand calculations,

as you will see in the next section.

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.

Figure 6. Select Format Cells... from the context menu.


A-40
An Introduction to Excel

The default category for a cell is General. Change the category to Number and set the number

of decimal places as dictated by the experiment.


However, keep in mind that Excel does not allow you to set the number of significant figures, so

you will still need to remember the rules for rounding significant figures in order to determine
the number of decimal places to use.

Figure 7. The Format Cells window showing the Number formatting.

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.

Common math functions for Excel


Finds the sum of all the cells between cell
=SUM(A1:A5)
A1 and cell A5.
Finds the average of the values between
=AVERAGE(A1:A5)
cell A1 and cell A5.
Finds the standard deviation of all the
=STDEV(A1:A5)
cells between cell A1 and cell A5.

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:

1 𝑟𝑟𝑟𝑟𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾 1 𝑟𝑟𝑟𝑟𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝑁𝑁𝑁𝑁𝑟𝑟𝑟𝑟𝑁𝑁𝑁𝑁𝐾𝐾𝐾𝐾


𝑔𝑔𝑔𝑔𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾 × 204.2 𝑔𝑔𝑔𝑔 𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾 ×
1 𝑟𝑟𝑟𝑟𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚 𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾𝐾
= 𝑀𝑀𝑀𝑀𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 (𝑀𝑀𝑀𝑀)𝑁𝑁𝑁𝑁𝑟𝑟𝑟𝑟𝑁𝑁𝑁𝑁𝐾𝐾𝐾𝐾
𝑣𝑣𝑣𝑣𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑚𝑣𝑣𝑣𝑣𝑟𝑟𝑟𝑟𝑣𝑣𝑣𝑣 𝑁𝑁𝑁𝑁𝑟𝑟𝑟𝑟𝑁𝑁𝑁𝑁𝐾𝐾𝐾𝐾 𝑟𝑟𝑟𝑟𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑎𝑣𝑣𝑣𝑣𝑎𝑎𝑎𝑎 (𝐿𝐿𝐿𝐿)

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

Figure 8. The equation typed into cell D2 as an Excel formula.


Hit the enter key, and the formula will switch to the calculated value. You can double click on

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

the fill handle down to the bottom-most row of data.

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 -

Strong Base Titration experiment to create a titration curve.


Enter the data in 2 columns, and click on the top leftmost cell containing data. Then, while

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

will most commonly use the scatter chart to create graphs.


With the data range selected, click on the Insert Scatter (X, Y) Chart button to plot the

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.

Figure 14. The titration curve with connecting lines added.

A-46
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.

Figure 15. The Chart Elements menu.


Double click on each of the text fields to enable editing. Be sure to include your units in the

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

Common Laboratory Procedures


Handling Solids
1. General Guidelines for Handling Solids
1. Use a clean spatula or scoopula to transfer solid from bottles. Never use a contaminated
spatula.
2. Never return unused solid to the reagent bottle. To eliminate waste, avoid removing more
solid from a bottle than is necessary.
3. Never discard chemicals in the trashcan. Follow waste disposal procedures outlined in the
Laboratory Manual.
2. Quantitative Transfer
Quantitative transfer refers to the moving of all the contents to be transferred from one container
to another. Below is an illustration of how to properly weigh and transfer a solid using weighing
paper. You will be using weighing boats rather than weighing paper, but the procedure is essentially
the same.

Figure 1. Quantitative Transfer of Solids

A-49
Common Laboratory Procedures

3. Using the Desiccator


You will occasionally be asked to use the desiccator during the laboratory course to dry some
reagents. The desiccator contains some amount of desiccant, which absorbs moisture from air.

a. Keep the desiccator closed at all times.


The desiccant will absorb moisture in the air extremely rapidly.
b. Keep the desiccator tightly sealed with some vacuum grease.
To apply vacuum grease, put a pea-sized amount of grease on a paper towel and wipe it
along the rim of the transparent cover. Make sure you do not use too much grease. Place the
cover on top of the base and twist the cover 30 degrees to ensure a tight seal.
Desiccator Care
In the Chemistry 2 lab, we use Calcium Chloride as the desiccant. If water is found in the
desiccator, discard the desiccant in the sink and rinse with copious amount of water until all solids
are dissolved. Wipe the desiccator dry with a paper towel. Make sure all traces of water are removed
before refilling from the 10 kg bucket of Calcium Chloride in your lab.
Hard to Open Desiccator
Do not try to force open a desiccator. You may accidentally shatter the glassware stored inside. Use
an aluminum scoopula as a wedge and push it slowly into the space between the covers.

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.

2. Estimating Volume with a Dispo Pipet


The dispo pipette may be used to transfer an estimated amount of solution. This is useful when
working with non-limiting reagents or quickly making a solution that will be titrated later.
To draw 1mL of solution into an empty dispo pipet:
a. Squeeze the bulb to remove some air from the dispo pipet.
b. Submerge the tip of the dispo pipet in the solution.
c. Slowly release the pressure on the bulb and draw solution to the 1mL mark.
d. Without releasing pressure on the bulb, steadily remove the dispo pipet from the solution.

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.

Figure 2. Liquid Transfer with Glass Stir Rod


b. With the exception of beakers, you should always use a funnel when transferring liquids
from a container with a large opening to a container with a small opening.
4. Capping a Flask with Parafilm
During many experiments you will have to cap a flask to protect the contents from contamination.
Figure 3. illustrates the proper method using Parafilm.

Figure 3. Capping A Flask

A-52
Common Laboratory Procedures

5. Measuring Liquid Volumes


Many glassware items have volume marks printed on them. Before using a piece of glassware to
make a volume measurement, you should take a moment to study its calibrations to insure that
you know how to read them properly.
• A beaker or Erlenmeyer flask can be used for rather rough measurements.

• A graduated cylinder can be used for measurements of moderate accuracy.

• A pipet is commonly used to transfer an accurately known volume of a liquid.

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. Reading the Meniscus

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.

A-53
Common Laboratory Procedures

Common Glassware in the Laboratory


Almost all of the glassware used in the Chemistry 2 laboratories are made with borosilicate glass,
which is able to resist high temperatures and most chemicals.
1. Care and Maintenance of Laboratory Glassware
a. Always examine the glassware for chips and scratches before use. Damaged glassware may
break during normal usage or cause bodily injuries.
b. Never place glassware near the edge of lab bench. Keep the work area clean and organized
to prevent accidents and chemical spills.
c. Clean broken glassware must be disposed of inside the designated Glass Disposal Box. If
box is full, ask the dispensary for a new one.
d. Clean all glassware with water. Make sure to rinse the glassware with DI water as a final step.
e. Never heat glassware to dryness. Add cold water with your 250 mL water squeeze bottle
when needed.
f. Never place a heated beaker in an ice bath, or vice versa. Allow the glassware to warm up or
cool down gradually.
g. Never carry lab ware by the neck or cap. Always hold lab ware from the bottom and the side.
h. Never use tape or sticky labels on laboratory glassware. Always write on the white or blue
label area with graphite pencil (a.k.a. “lead pencil”).

A-54
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

for estimating the volume. As noted on the glassware, Volume


mark
there is a ±5% error for the largest volume mark.
d. Place a 100 mm watch glass on top of beaker when
boiling water to speed up the process.
e. If needed, write labels in the frosted areas on the beaker
with graphite pencils (a.k.a. “lead” pencils). Do not
use wax pencil or pen!
3. Erlenmeyer Flasks
Erlenmeyer flasks can be used in the laboratory to estimate volume, storing liquids temporarily,
and carry out certain reactions.
a. All Erlenmeyer flasks in the Chemistry 2 laboratories have
marks for estimating the volume. As noted on the glassware,
there is a ±5% error for the largest volume mark.
b. If needed, write labels in the frosted areas on the beaker with Volume
marks
graphite pencils (a.k.a. “lead” pencils). Do not use wax pencil
or pen!
4. Graduated Cylinder
Graduated cylinders are used to measure a small volume of liquid with more precision than beakers
and Erlenmeyer flasks.
a. The graduated cylinders in the Chemistry 2 laboratories
Plastic ring
include a plastic base and a plastic ring. The plastic ring (keep above
0 mL mark)
is to protect the glass cylinder from shattering when
the glassware is knocked over. Make sure the plastic
ring is placed near the top of the cylinder. Graduation
marks
b. To quickly measure out a specific amount of water, fill
your 250 mL water squeeze bottle with DI water and
squeeze the desired amount of water into the graduated
cylinder.
Plastic base

A-55
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

A-56
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.

A-57
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.

A-58
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.

A-59
Common Laboratory Procedures

Using the Balance


A balance is used to measure the mass of an object. There are 4 balances assigned to your laboratory
section for use in the adjoining balance room. These balances measure the mass to the nearest
milligram. You will use these balances for most mass measurements in the Chemistry 2 lab
experiments.
There is also a less precise “quick” balance in your lab room, between the fume hoods. You may
use this balance to make rough measurements of non-limiting reagents quickly and speed up your
experiment without compromising the experiment results.
1. On/Off Switching
a. To turn on the balance, remove all load from the weighing pan and press the On button.
b. To turn off the balance, press and hold the Off key for 2 seconds.
2. Simple Weighing
Open one of the draft shield sliding doors. Make sure the balance pan and surrounding area is
clean. You can clean it with a balance brush or Kimwipe.
Next, shut the doors and press the 0/T button to set the balance at zero.
Now, simply place the object to be weighed on the weighing pan and measure the mass to 0.001
grams.

Draft Shield

Weighing Pan

LCD Display
Keys

Figure 5. The Analytical Balance

A-60
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.

A-61
Common Laboratory Procedures

Using the Centrifuge


A centrifuge machine is used to separate the different constituents of a solution by their density.
In many experiments, you will be required to separate precipitation products from solution using
the centrifuge machine.
Centrifuge Cover
Rotor with
Aluminum Shields

Cover Latches
(one on each side)
On/off Switch

Figure 7. The Centrifuge


1. Procedure
a. Always load centrifuge tubes of about equal weight. Fill another centrifuge tube with water
to equal weight to balance.
b. To balance the tubes, place a small beaker on the “quick” balance in your lab room. Weigh
your sample tube. Fill another centrifuge tube with water to equal weight (to the nearest
1g).
c. Place the centrifuge tubes in the aluminum shields on opposite sides. The centrifuge tubes
should fit inside the aluminum shield snugly. Use a different tube if more than 1/8 inch of
the glass is exposed.
d. Close the cover. Lock both sides securely into the latches.
e. Press the On/Off switch to turn on the unit. Press the switch again to turn it off.

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.

A-62
Common Laboratory Procedures

Using the Hot Plate


The hot plate is used to heat solutions in nearly all experiments performed in the Chemistry
2 laboratory. However, improper use of the hot plate may result in serious injury. Follow all
instructions and exercise caution when using the hot plate.
There are a variety of hot plates used in the Chemistry 2 labs, but they all have the same essential
features.

Ceramic Top
Indicator Light
Heating/Stirring
Control Knobs

Figure 8. The Hot Plate/Stirrer


1. Features
a. The Ceramic Top: The heating surface. The temperature may reach a maximum of over
400 °C. Do not touch the ceramic top. It may cause serious burns. The ceramic top is also
very delicate. Clean up spills immediately and avoid hitting the surface with heavy objects.
b. There are four common indicating lights on all models used in the Chemistry 2 laboratories.
They are: the Power Indicator, the Heat Indicator, the Stir Indicator, and the Hot Top
indicator.
• Power Indicator: On if the unit is plugged in to a power source. Check power cord
connection if not on.
• Heat Indicator: On if the heat is turned on.
• Stir Indicator: On if the magnetic stirrer is turned on.
• Hot Top Indicator: On if the top has a temperature of over 60°C. Do not unplug the unit
if the top plate is still hot.

Warning
• The hot plate may cause serious burns. Avoid touching the top plate and follow all safety
precautions.

A-63
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.

A-64
Common Laboratory Procedures

Heating with a Bunsen Burner


In using a Bunsen burner, always use a tight blue flame as shown in the illustration below. Always
estimate the appropriate height for the iron support ring before turning on the Bunsen burner.
Control the heat transfer by adjusting the distance from the burner to the object. Note that the
distances suggested in the manual are measured from the hottest part of the flame to the object.

Figure 9. The Bunsen Burner

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!

A-65
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.

A-66
Common Laboratory Procedures

Setting up a Titration Apparatus

buret clamp

buret

stopcock
(open position)

flask

stir bar

stir plate

Figure 10. Titration Setup


Titrations often involve the use of strong acids and bases, and properly setting up your titration
apparatus can reduce the risk of spills or accidents. Reference Figure 10 and the instructions below
to properly set up your titration apparatus.
1. Obtain a stir plate, buret, stir bar, and titration flask. Place the stir plate below the buret clamp
located at your lab bench. If applicable, make sure the heating element is turned off.
2. After conditioning and filling the buret, place it securely in the buret clamp. Make sure there is
enough room between the buret and stir plate to place the titration flask. Adjust the stir plate
so that it is centered underneath the tip of the buret.
3. Use a laboratory tissue to wipe down the tip of the buret. Make one quick stroke downward
beginning at the closed stopcock and ending in the air beyond the buret tip. Dispose of the
tissue as it may now be contaminated.
4. Add your stir bar, solution, and indicator to the titration flask, and place the flask underneath
the tip of the buret. Turn on the stirrer and slowly increase the stirring speed.
5. Lower the buret tip into flask without touching the flask sides. You are now ready to titrate!

A-67
Common Laboratory Procedures

pH Meter Operating Instructions

1. Preparing the pH meter


1. Turn on the pH meter.
2. Meter must be in pH mode. If in mV mode, press the
pH/mV button.
3. Make sure pH meter is showing /Ā. If not shown, press and
hold Read button for 2 seconds.
4. Lower left window must show B1 7.00 4.00 10.01 1.68.
If not, ask your TA to adjust the setting.
5. You may adjust the electrode stand to secure the electrode.
Loosen the tension knob to adjust arm position and tighten
the tension knob before use.

Caution: Do NOT place test tubes on electrode stand!

6. Do NOT let electrode dry out. Always store electrode in saturated KCl solution when
not in use.

A-68
Common Laboratory Procedures

2. Calibrating the pH meter


Note: You only need to calibrate the pH meter once per lab period.

1. Rinse the electrode with DI water.


2. Blot dry with Kimwipe.
WARNING: Do NOT rub the electrode with Kimwipe. Rubbing the electrode may build up
static charge and damage the electrode.

3. Place electrode in pH 7 buffer standard (yellow).


4. Press the Cal button.
5. Wait for the display to stop blinking.

6. Repeat step B-1 to B-5 with the pH 4 buffer standard (red) and then with the pH 10 buffer
standard (blue).

A-69
Common Laboratory Procedures

3. Measure the pH of sample

1. After calibration, place the electrode in sample solution and press Read.
2. Wait for the reading to stabilize.

A-70
Common Laboratory Procedures

Fume Hood Use and Safety


The fume hoods in the laboratory protect personnel from hazardous materials and inhalation of
toxic materials.
1. Features of the Fume Hood

 Flow Monitor
with Emergency button
and Mute button
 Light Switch
 Certification Sticker
 Sash
 Sash Stop
 Work Surface
 Airfoil

2. Before using the fume hood


1. Check the certification sticker (). The Fume Hood is tested and certified every year.
2. Check the flow monitor ().
Laboratory fume hood should have 100 ft/min face velocity or more. Lower the sash if
to increase airflow. If airflow does not reach 100 ft/min, stop work in the fume hood and
contact safety personnel immediately.
3. Turn on light switch ().
3. Guidelines for working with the fume hood
1. Lift the sash up slowly about 12 inches. Never raise the sash above the sash stop ().
2. Always place lab equipment at least six inches away from the edge and inside the fume hood
as much as possible.
3. Do not rest body parts on the edge or the Airfoil ().
4. Do not place glassware or chemicals on the Airfoil ().
5. Move unused equipment and chemicals away. Remove your glassware when done.
Remember, you are sharing the fume hood with 23 other students. Remove your glassware as soon
as possible and clean your glassware. Do NOT abandon your lab ware in the fume hood!

A-71
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.

A-72
THIS PAGE IS INTENTIONALLY LEFT BLANK.

A-73
Locker Inventory

Centrifuge Tube
Casserole Dish

Crucible
(with Cover)

Test Tube
Beaker
Erlenmeyer Flask
Evaporating Dish

Test Tube
Brush

Stir Rod with


Policeman

Volumetric Graduated Wire Gauze


Flask Cylinder
Funnel Watch Glass

Volumetric Pipet

Crucible
Tongs
Washing Bottle
Scoopula

Beaker Tongs

Test Tube Pipet Bulb


Clamp Desiccator
with Tip
A-74
Locker Inventory

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.

CHEMISTRY 2 LOCKER LIST


Glassware Porcelain
# present # total Description # present # total Description

1 100 mL Beaker 1 150 mL Casserole Dish


1 150 mL Beaker 1 Evaporating Dish
1 250 mL Beaker 2 Crucible
1 400 mL Beaker 2 Crucible Cover
1 800 mL Beaker Plastic Ware
2 50 mL Erlenmeyer Flask # present # total Description

2 125 mL Erlenmeyer Flask 1 250 mL Washing Bottle


2 250 or 500 mL Erlenmeyer Flask 1 Short Stem Funnel
1 100 mm Watch Glass 2 1 L Bottle, square
2 Glass Stir Rod 1 Desiccator
10 Test Tubes (rounded end) 1 Plastic Test Tube Rack
6 Centrifuge Tubes (pointed end) Other
2 Thermometer, non-mercury # present # total Description

2 25 mL Volumetric Flask 1 Centrifuge Tube Brush (pointed)


1 250 mL Volumetric Flask 1 Test Tube Brush (round)
1 10 mL Graduated Cylinder 1 Vial, Alkacid Test Paper
1 25 mL Graduated Cylinder 1 Sponge
Metal Equipment 2 Rubber Policeman
# present # total Description

1 Wire Gauze Square


1 Scoopula

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

A-75
Locker Inventory

Procedure for end of quarter locker check-out:


1. Clean and dry all equipment.
2. Count the numbers of items currently present in locker.
3. Place excess items from locker into the extra glassware box in the back of lab.
4. Return community supplies to the appropriate storage location.
5. 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)

CHEMISTRY 2 LOCKER LIST


Glassware Porcelain
# present # total Description # present # total Description

1 100 mL Beaker 1 150 mL Casserole Dish


1 150 mL Beaker 1 Evaporating Dish
1 250 mL Beaker 2 Crucible
1 400 mL Beaker 2 Crucible Cover
1 800 mL Beaker Plastic Ware
2 50 mL Erlenmeyer Flask # present # total Description

2 125 mL Erlenmeyer Flask 1 250 mL Washing Bottle


2 250 or 500 mL Erlenmeyer Flask 1 Short Stem Funnel
1 100 mm Watch Glass 2 1 L Bottle, square
2 Glass Stir Rod 1 Desiccator
10 Test Tubes (rounded end) 1 Plastic Test Tube Rack
6 Centrifuge Tubes (pointed end) Other
2 Thermometer, non-mercury # present # total Description

2 25 mL Volumetric Flask 1 Centrifuge Tube Brush (pointed)


1 250 mL Volumetric Flask 1 Test Tube Brush (round)
1 10 mL Graduated Cylinder 1 Vial, Alkacid Test Paper
1 25 mL Graduated Cylinder 1 Sponge
Metal Equipment 2 Rubber Policeman
# present # total Description

1 Wire Gauze Square


1 Scoopula

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

A-76

You might also like