CHE1047L Student Manual

CHE 1047L
General Chemistry Lab

Spring 2014
Text
Yeshiva College
Department of Chemistry
New York, NY 10033
CHE 1047L: General Chemistry Laboratory
Spring 2014
Instructors
Monday (261) Monday (262)
Belfer 1507 Belfer 1513
Dr. Allan Burger Dr. Jacopo Samson

aburger1@yu.edu jsamson1@yu.edu
Office Hours: by appointment Office Hours: by appointment
Tuesday
Belfer 1513
Dr. Wayne Lo
wayne1728@yu.edu
Office Hours: by appointment
Wednesday
Belfer 1513
Dr. Jacopo Samson
jsamson1@yu.edu
Friday
Belfer 1513
Dr. Rosalyn Strauss
straussd@yu.edu
Required Materials
1. Yeshiva College General Chemistry Laboratory Manual (provided)
2. Duplicate Laboratory Notebook. Recommended: Hayden-McNeil "Student Lab Notebook: 100

Top Bound duplicate pages" ISBN:1930882009
3. Laboratory Handbook for General Chemistry, 2nd ed., N.E. Griswold, H. A. Neidig, J. N. Spencer, C.
L. Stanitski. ISBN: 0-534-97694-8,
Grading
Pre-labs: 15% End of Semester Lab Exam: 15%
Lab report sections: 5% total Technique: 10%
Full lab report: 25%
Post-labs: 30%
Academic Integrity
THERE IS A ZERO-TOLERANCE POLICY FOR ACADEMIC DISHONESTY IN THIS COURSE. Each
student is responsible for conducting his own laboratory work and writing up his own unique and
individual laboratory report. Occasionally, students will be asked to pool their data with other
students. In this case, each student must indicate clearly in his laboratory report which data is his
and which is that of another, giving the name of the other student whose data was used.
In addition to the policies outlined in the Academic Integrity Statement of Yeshiva College, the
following activities constitute academic integrity violations:
submitting data or results that are not your own work, regardless of if these data
and results are fictitious or that of another person
having in your possession the laboratory notebook or report of another student
If you are suspected of academic dishonesty, the laboratory coordinator will be notified and the
case submitted to the Dean’s Office for review.
General Course Rules

No student may take this course without the lecture. If you drop the lecture, you must drop
the lab and vice-versa.
Students are expected to attend all laboratory sessions as scheduled and complete all
experimental work.
Attendance at all laboratory meetings is mandatory. Should there be an unavoidable conflict
due to emergency or other suitable circumstance; a make-up lab may be requested.
Students are allowed at most one make-up lab in the course. Make-ups should be pursued
by filling out the “make-up request form” and submitting it to Dr. Camara with supporting
documentation as soon as possible.
Any missed experiment that is not made up will receive a score of zero. Students who miss
two or more experiments will be dropped from the course.
It is expected that you will have read through the experiment before you come to the
recitation section. You are required to complete the pre-laboratory assignment before you
come to the lab. Failure to do so may result in not being permitted to do the laboratory
work that day.
Laboratory reports are due one week after completion of the experiment and should be
uploaded to dropbox. Post-labs are due at the end of each laboratory period and will be
collected on site.
Laboratory Lecture
Understanding the experiments before the lab meets will be vital to your success in this laboratory
course. Laboratory lectures will be available online at the Yeshiva University e-campus
(http://ecampus.yuschoolpartnership.org/) and must be completed a minimum of 1 hour before
your section meets. The online lab lectures each contain short, straightforward quizzes that must
be passed with a grade of 100% before being allowed to attempt the lab. The online content of the
laboratory lecture will be available for your reference throughout the year, so feel free to use the
website to review for more advanced experiments.
Schedule
Week Experiment
1 Check-in, Safety Quiz, Excel Assignment
2 Lab 1: Introduction to Volumetric Glassware
3 Lab 2: Synthesis of Alum
4 Lab 3: Spectrophotometric Analysis of Aluminum in Alum
5 Lab 4: Thermometric and Potentiometric Titration of an Unknown Hydrochloric Acid

Solution
Lab 5: Determination of Heat of Formation of Magnesium Oxide Using Calorimetry and
6 Hess’s Law.
Partial Report: Title and Abstract
7 Lab 6: Kinetics of Decomposition of Crystal Violet Dye,

Partial Report: Introduction and Experimental
Lab 7: Characterization of Complex Ion Equilibria of Co2+
8 Partial Report: Results and Discussion
Determination of Nitrogen in Soil Set-up
9 Lab 8: Determination of Nitrogen Content in Soil

Full Lab Report
Lab 9-10: Titration of Phosphoric Acid and Determination of Phosphoric Acid content
10-11 in Coke™
Full Lab Report
Lab 11-12: Electrochemistry and Measurement of Faraday’s Constant
12-13
Full Lab Report
Monday Tuesday Wednesday Friday
20 January 21 Check-in 22 Check-in 24 Check-in

Excel Assignment Excel Assignment Excel Assignment
27 Check-in 28 Lab 1 29 Lab 1 31 Lab 1

Excel Assignment
3 February 4 Lab 2 5 Lab 2 7 Lab 2

Lab 1
10 Lab 2 11 Lab 3 12 Lab 3 14 Lab 3
17 Lab 3 18 Lab 4 19 Lab 4 21 Lab 4
24 Lab 4 25 Lab 5 26 Lab 5 28 Lab 5
3 March 4 Lab 6 5 Lab 6 7 Lab 6

Lab 5
10 Lab 6 11 Lab 7 12 Lab 7 14 Lab 7
17 Lab 7 18 Lab 8 19 Lab 8 21 Lab 8
24 Lab 8 25 Lab 9 26 Lab 9 28 Lab 9

Lab 8 Report Due Lab 8 Report Due Lab 8 Report Due
31 Lab 9 1 April 2 Lab 10 4 Lab 10

Lab 8 Report Due Lab 10
7 Lab 10 8 Lab 11 9 Lab 11 11 NO LAB
14 15 16 18
21 22 23 25 Lab 11
Lab 10 Report Due
ALL SECTIONS
28 Lab 11 29 Lab 12 30 Lab 12 2 May Lab 12
5 Lab 12 6 7 9
Lab 12 Report Due Lab 12 Report Due Lab 12 Report Due
12 Lab 12 Report Due 13 14 16

Laboratory Notebooks
What to write in your lab notebook before, during and after the experiment
Before the Experiment: Pre-Laboratory Assignments (10% of the final grade)

Before lab, you should view the laboratory lecture video, read the description of the experiment as
well as any background reading materials from the textbook and lab manual. Select a section of
your laboratory notebook and designate it for the experiment. On these pages you should have:
Title: Give the experiment an informative title.
Objective: State in your own words what you will study in the experiment, and what you will learn
from doing the experiment.
Pre –lab questions: You are required to complete any pre-laboratory questions on the first page of
your lab notebook that corresponds to the experiment. The yellow carbon copy of these questions
will be collected by the instructor at the beginning of the session. Make sure the pages are stapled
and include your name, section, title and date.
Procedure: In addition to the pre-lab questions, each pre-lab assignment includes a flow chart
procedure for the experiment to be performed. The procedure should describe in detail every step
of the planned experiment in sufficient detail for you to carry out the experiment in the absence of
the laboratory manual. Be sure to include diagram(s) of any new apparatus being used, write down
any relevant balanced chemical equations, and leave enough space in your procedure for any
observations or experimental notes.
Calculations, Tables and Charts: Set up any calculations that will need to be carried out to complete
the experiment. Draft any charts and/or tables that will be populated during the experiment.
The pre-lab question will be collected by your instructor before lab. The procedure, calculations,
tables and charts will be checked by your instructor before lab. If any portion of your pre-lab
assignment is deemed inadequate, you will not be allowed to carry out the experiment and will
receive a zero for the lab.
During the Experiment

You must always bring your lab notebook to the lab session. Your instructor may check it at any
time. You are responsible for recording, understanding and interpreting all of your experimental
results and keeping your lab notebook neat and up to date.
Observations made during the laboratory should be recorded neatly in the laboratory notebook in
blue or black ink. All measurements taken should be recorded with their appropriate units.
Observations recorded should include physical appearance of reaction mixtures and isolated
material and actual temperatures, reaction times, and any other variables. Another chemist should
be able to reproduce your experiment using only what is written in your notebook.
After the Experiment: Notebook Reports (35% of the final grade)
For the experiments that you will not type a formal lab report, you will handwrite a report in your
notebook and hand in the yellow copy at the end of the same session. The report will have the
record of all your experimental results, interpretation of the experimental data, and the answers to
the discussion questions.
For the experiments that you will type a formal lab report, you will only write down in your
notebook experimental observations and hand in the yellow copy at the end of the session.
Below is a short list of relevant information to be included in your notebook report after you have
completed the experiment:
• Yield of any reactions, if applicable.
• Brief assessment of the purity of any isolated materials, if applicable.
• Identity of any unknown compounds, if applicable.
• Answers to the discussion questions.
• Copies of any spectra (UV-Vis), graphs, tables or plots. Brief interpretation of the results
contained in these items is also required.
• Brief analysis of sources of error.
Formats for Tables and Graphs
Tables: All data tables will be placed directly after the procedure in the lab notebook. Drafting these
tables as part of the pre-lab ensures that you know what data you will be recording during the
experiment.
Each table should have a title indicating the purpose of the measurement.
Tables should be drawn neatly using a ruler, with the required number of columns and
rows.
Each column and/or row should be labeled with the quantity entered and the unit in which
it is measured. For example, mass (g), volume (mL) etc.
If the table includes data for an unknown sample, the unknown number should be clearly
indicated at the top of the table below the table heading.
Any data or results gathered from other students should be clearly labeled crediting the
person(s) who collected that data.
Graphs: All graphs must be included with your post-lab.
Each graph must have a title describing the nature of the graph. A title just listing
what the x and y axis are is not sufficient. Include your name on the same line as
the title.
Axes should be labeled with the quantity being plotted and indicate units.
The experimental data points should not be connected unless it is appropriate for the
nature of the graph.
A best fit line or curve should be drawn, if required, and the equation should be displayed
on the graph.
The font size of the title, axes labels, etc, should be appropriate.
Make sure that you use a scale for both axes so that the graph fills a page, Divisions on the
axes and gridllnes should be such that the data can be read off the graph (without
resorting to using the equation of the line).
While printing the graph, make sure that the background is white.
Ben Goldblatt: Absorbance of Various Concentrations of Cresyl Violet and Neptune Blue
Aqueous Dye Solutions
Dye: Cresyl Violet Neptune Blue(Collected by Josh Levy)
Concentration (M) Absorbance (au) Concentration (M) Absorbance (au)
1.0 x10-6 8.72 x10-2 1.0 x10-6 1.37 x 10-1

2.0 x10-6 1.58 x10-1 2.0 x10-6 2.47 x 10-1
4.0 x10-6 3.32 x10-1 4.0 x10-6 5.20 x 10-1
8.0 x10-6 6.97 x10-1 8.0 x10-6 1.09
Ben Goldblatt: Beer's Law Plot for Aqueous Solutions of

Cresyl Violet Dye
0.80
y = 88016x - 0.0115
0.70
R² = 0.9989
0.60
Absorbance (au)
0.50
0.40
0.30
0.20
0.10
0.00
0.00E+00 2.00E-06 4.00E-06 6.00E-06 8.00E-06 1.00E-05
Concentration (M)
Formal Laboratory Reports
A necessary part of this course is learning to write a scientific laboratory report. For each of the
application labs, you will write 1-2 section(s) of a lab report as indicated on the schedule. These
sections will be graded liberally as “all or nothing” and you will receive ample feedback from your
instructor on them.
You will write a single full-length lab report for each of the final labs as indicated on the schedule.
The full reports will be more rigorously graded and will count for 25% of your final grade.
*All laboratory reports are to be typed and must include the following, at the top of the first page:
Student name, instructor name, lab day, date submitted.
*All lab reports should be uploaded to the turn-it-in dropbox no later than 1 week after the
completion of the experiment.
General (~15 pts)

Laboratory reports must be clear and professional in their presentation, and be typed in 12 point
Times New Roman font with 1.5 line spacing in paragraph form.
Sections must be separated with the headings given below.
Proper spelling and grammar is expected.
All sections must be written in passive third person, with the correct verb tense.
All schemes, figures and tables must be numbered, discussed in the text, and have a brief and
descriptive title.
Excess wordiness will be penalized. Scientist write in short concise sentences without unnecessary
explanations or repetitions.
Balanced chemical equations and chemical formulas should be written with appropriate subscripts
and superscripts.
Calculations should be in typed using equation editing software such as that included with
Microsoft Word. Do not type out calculations across a single line of text such as : mass % = 100 x
(mass element)/(total mass).
1. Title
Give an appropriate title to your laboratory report. It should be different from the title in
the laboratory manual and should be specific to and descriptive of the experiment you are
performing.
2. Abstract (~5 pts)

The abstract concisely expresses what the problem is, how it was addressed, and what was
discovered. It should not be vague and general, but rather should refer to the specific
experiment being conducted and should function as a summary of the information in the
laboratory report. Mention the reaction that was performed, the reagents and product(s),
and the results of the experiment. If the experiment involved any major technique to either
perform the experiment or analyze the product, mention that here as well. The reader
should know what experiment was performed, what the outcome was, and how you
determined the results from reading this section. It might be helpful to wait until you have
answered the discussion questions before composing this section. This section should be
no longer than a paragraph and should not include detailed procedural information.
3. Introduction (~20 pts)
The introduction should explain the background material concerning the problem being
studied. This should be done in sufficient detail for another student at your level who has
not taken the class to understand the purpose of the experiment, the problem being
addressed, any new techniques being used, and how the experiment addresses the stated
problem. Balanced chemical equations and relevant mathematical equation should be
included. In some circumstances you may choose to describe any new instrumentation
such as spectrophotometers in this section to aid in the explanation of the experimental
design. However, typically this information is included in the Experimental Procedure
section.
4. Experimental Procedure (~15 pts)
Describe in detail the experimental procedure that you followed. Do not give a general
procedure from the lab manual. If you are using a particular apparatus, instrument, or
technique for the first time you should describe it’s set up and operation. For the
subsequent experiments, assume that your reader is a chemist who is familiar with the
basic laboratory techniques from previous experiments but is unfamiliar with the
particulars of your experiment. Include those experimental details and observations that
would be necessary for anyone who wished to reproduce the exact experiment you
conducted (in past tense). For example, you should include reagent names, quantities,
temperatures, reaction times, color of the reaction mixture, physical description of the
product, etc. Note that this is a description of what you actually did in the lab, not what you
originally planned to do. Do not include trivial information such as the mass of tared
glassware. Refer to the experimental section of any research publication from the Journal
of the American Chemical Society (JACS), Journal of Organic Chemistry (JOC) or other similar
publication for examples. These journals can be accessed on campus at pubs.acs.org
5. Results and Discussion (~30-35 pts)
Results should be tabulated in a clear and legible format, introduced by and connected to
narrative text. You should work all of your data tables into a brief discussion, which may
include how data was obtained, how charts/graphs were constructed, etc. Results should
always include all physical properties determined in the laboratory (if any), as well as the
theoretical or literature values for comparison. All literature values must be referenced.
Raw values as well as calculated values should both be included. Any relevant calculations
should be shown; if there are multiple calculations that are identical, only one sample
calculation needs to be shown using actual data from the lab. Every quantity and
measurement should include the appropriate units and significant figures.
If applicable, this section should include:
- yields: experimental yield, percent yield, theoretical yield
- expected values for any property you measure
- brief description of any significant potential sources of error, being more specific than
“human error” or “impurities”. Do not speculate on what might have happened, such as
saying that “some solution may have been spilled during transfer”. Concentrate on what
did happen and how it may influence your results. Think about the methods you used to
conduct the experiment, what level of uncertainty is expected from those methods and if
your measured results are consistent with the expected uncertainty from our methods.
- Discussion of any postlab questions or analyses indicated in the experimental
procedure.
Read the discussion questions carefully before answering. Your answers should specifically
address the questions asked in paragraph form (not bulleted or numbered items). Make
sure your answers are clear, well written and easy to follow. All data obtained should be
addressed. Discussion questions are written to ensure that you think about particular
aspects of your experiment, but any conclusions that you draw from your results and any
errors that influenced your results should also be explained.
6. References (~5 pts)
Insert references with a superscript number within the text and list the reference as
endnote at the end of the report. Include the title of the article when citing scientific
journals.
Consult the ACS style guide for the correct format to refer journals, books, online sources,
material safety data sheets, etc.
Coghill, A. M.; Garson, L. R. The ACS Style Guide; Oxford University Press: New York, 2006;
pp 292-293. Chapter 14 of this publication is available for free online at the following link:1
http://pubs.acs.org/userimages/ContentEditor/1246030496632/chapter14.pdf
A copy of The ACS Style Guide is on reserve at the YU library.
The following web sites from UW Madison, Penn State and UCBerkeley libraries also
explain the correct way to cite your sources: 1
http://chemistry.library.wisc.edu/writing/acs-style-guidelines.html#book
http://www.libraries.psu.edu/content/dam/psul/up/pams/documents/QuickGuideACS.pdf
http://www.lib.berkeley.edu/CHEM/acsstyle.html
7. Appendix (~5 pts)
If you generate any graphs, chromatograms, spectra, computer printouts, etc. that are
inappropriate for the results and discussion section they belong in an Appendix. Each item
should have a clear number and a title. All appendices must be discussed at some point in
the text, else they must be omitted
1 Accessed August, 2013

Sample Laboratory Report
Organic Chemistry Lab CHE1215L – Thursday Section

Prof. R. T. Choke
Student: Budd Weisser
Submitted: 11/11/2011
Determination of Melting Point of Pure Solids and
Demonstration of Melting Point Depression of Impure Solids
Abstract
The melting points of samples of pure urea, pure trans-cinnamic acid, along with impure
mixtures of the two were measured. The melting point ranges of the pure solids were
similar to their literature values. The melting point ranges of the impure mixtures were
lower by several degrees. The results are consistent with the phenomenon of melting point
depression of an impure solid.
Introduction
A molecular solid is an orderly arrangement of molecules held together by van der Waals
forces of attraction. As heat is added to the solid, the molecules will vibrate, but still remain
arranged in the solid structure. At a characteristic temperature, the molecules in the solid
will have enough energy to overcome the intermolecular forces and will transition into a
liquid phase, where the molecules are not held as tightly together and lack long-range
order. This characteristic temperature is known as the substance’s melting point. Larger
molecules, more symmetrical molecules, and molecules that form hydrogen bonds tend to
form solids that have higher melting points than their smaller, unsymmetrical, less polar
solid counterparts.1
The melting point value can help to identify an unknown solid or to determine its relative
purity. Any pure solid will typically melt over a narrow range of temperature. Typically,
this range is less than 2 C. An impure solid will melt below the reported literature value
and usually transition to liquid over a much wider range of temperature. This phenomenon
is called melting point depression.
Figure 1 shows a typical phase diagram to illustrate the different melting temperatures of a
mixture of two substances as a function of composition. When two different solids are
combined, the solid mixture will exhibit melting point depression. The lowest possible
temperature at which such a mixture will melt is called the eutectic temperature, labeled TE
in Figure 1. A mixture of solids with a composition that allows it to melt completely at the
eutectic temperature is called a eutectic mixture. The eutectic point, E in Figure 1, marks
the eutectic temperature and molar composition of solid mixture that leads to a eutectic
mixture. When a mixture of 2 solids is not of the eutectic composition, it still begins to melt
at the eutectic temperature. The liquid formed, or “melt”, will have also the eutectic
composition. The system will make melt of eutectic composition at TE until the minor
component of the mixture is used up. Once the minor component of the mixture is used up
to form the melt, the system can continue to heat and the remaining solid of the major
component will melt and dissolve into the liquid phase. The sample becomes a
homogeneous liquid (L) once the melting temperature is reached. The melting point range
starts at the temperature at which liquid phase first begins to form and ends at the
temperature at which the sample is a homogeneous liquid.2, 3
Figure 1. Phase diagram for a two-component mixture (taken from reference 2).
In this experiment, the influence of substance purity upon melting point will be
investigated by measuring the melting points of pure urea, pure trans-cinnamic acid, and
mixtures of the two.
Experimental Procedure
Melting points were determined using a Mel-Temp apparatus. The Mel-Temp apparatus is
shown in Figure 2. It is comprised of an aluminum heating block, a rheostat, a
thermometer and a viewing window. A sample of solid is placed in a capillary tune and
inserted into the sample holes of the heating block. The rheostat controls the heating of the
aluminum heating block, the viewing window allows melting of the sample to be
monitored, and the thermometer allows the determination of the temperature at which
melting begins and ends.
Figure 2: The Mel-Temp Apparatus. (Adapted from reference 3)
Using a metal spatula, 0.060 g (1.0 mmol) of pure urea was crushed to a fine powder on a
watch glass. The open end of a capillary tube was pushed into the powder. The solid
powder was forced down to the bottom of the tube by dropping the tube through a long
plastic tube held vertically atop a hard surface. More solid was added until the tube was
filled to a height of approximately 0.3 cm. A second tube was prepared with 0.15 g (1.0
mmol) of pure trans-cinnamic acid following the same procedure.
Both tubes were placed in a Mel-Temp apparatus. The rheostat was set to heat at a rapid
rate. When the temperature was 20 C below the known melting point of the solids, the
heating rate was reduce to about 1 C per minute. By observing (through the eyepiece of
the apparatus) when liquid began to form in the tube and when the entire solid in the tube
melted, the melting point ranges were obtained.
In the second part of the experiment, three mixtures with different mole ratios of urea and
trans-cinnamic acid were prepared and their melting points were measured. The first
mixture with a 1:4 mole ratio was prepared by adding 0.060 g (1.0 mmol) of urea and 0.59
g (4.0 mmol) of trans-cinnamic acid to a clean watch glass. The solids were crushed and
mixed well to make the mixture homogenous. The solid was placed inside the capillary tube
as described previously. The tube was placed in the Mel-Temp apparatus set at a moderate
heating rate and the melting point range of the mixture was measured. The mixture with a
1:1 mole ratio was prepared with 0.060 g (1.0 mmol) of urea and 0.15 g (1.0 mmol) of
trans-cinnamic acid and the mixture with a 4:1 mole ratio was prepared with 0.24 g (4.0
mmol) of urea and 0.15 g (1.0 mmol) of acid.
Results and Discussion

The identities of the pure solids, although already known, were confirmed by the
experimental melting point ranges. In both cases, the observed melting point was very
similar to the literature melting point values (Table 2). The experimental melting point
ranges of the impure mixture (Table 2) demonstrated the phenomenon of melting point
depression; the melting point ranges were not only much lower than the literature melting
point ranges of the respective pure solids (Table 2), but also melted over a much wider
temperature range, demonstrating the presence of an impurity in the solids.
Table 2. Experimental Melting Point Ranges
Experimental Corrected Literature

Compound/Mixture Melting Point Melting Point Melting
Range ( C) Range ( C)* Point4,5 ( C)
Pure urea3
130.6–133.1 132.1–134.6 132–135
Pure trans-cinnamic acid4
130.3–132.8 131.8–134.3 132–135
1:4 mole urea:trans-cinnamic acid

97.4–111.6 98.9–113.1 --
mixture
96.6–109.4 98.1–110.9 --
mixture
99.7–119.9 101.2–121.4 --
mixture
* Note that the temperatures reported in Table 2 are corrected by addition of 1.5 C to the
experimental values recorded. This adjustment was necessary according with the
calibration of the Mel-Temp apparatus (#7) that was used.
All the results are consistent with melting point depression due to the presence of
impurities; however, there is no clear trend between the mol ratio of the mixtures and the
extent of melting point depression. If we had measured ten or fifteen more mixtures with
different ratios, maybe we could have enough data points and find a clear trend in the
melting point depression or even pinpoint the eutectic point by constructing a plot similar
to Figure 1. Additionally, the melting points of pure urea and pure trans-cinnamic acid were
in good agreement with literature values.
Besides measuring the melting point of even more mixtures, measuring the melting point of
a particular mixture multiple times would decrease measurement error and help provide a
more accurate experimental melting point of the mixture. Entry 5 in the Table 2 shows a
particularly large melting range for the 4:1 mixture of urea:trans-cinnamic acid. This range
may be unusually large due to inhomogeneity of the sample mixture. While melting onset
for this sample was easy to identify, the end of melting was difficult to determine due to a
few small crystals near the top of the sample that persisted even after the majority of the
sample had melted. If the sample solids were inadequately mixed, these crystals may have
been pure crystals of a single substance that were not in contact with the melt. Again,
conducting multiple melting point measurements for each mixture would minimize this
type of error.
References
1. Mohrig, J. R.; Hammond, C. N.; Schatz, P. F. Techniques in Organic Chemistry, 2nd ed.;
W. H. Freeman: New York, 2006; pp 116-117.
2. Redid, R. S. B.; Kumar Satuluri, V. S. A.; Rai, U. S.; Rai, R. N. Thermal, physicochemical
and microstructural studies of binary organic eutectic systems. J. Therm. Anal.
Calorim. 2012, 107, 377-385.
3. LeFevre, J.W; “Measuring the Melting Points of Compounds and Mixtures” in

Modular Laboratory Program in Chemistry; Brooks/Cole Publishing, New York, NY,
2004.
4. Sigma-Aldrich Database. Urea MSDS.

http://www.sigmaaldrich.com/catalog/product/sigma/u5378?lang=en&region=US
(accessed 08/15/12)
5. Sigma-Aldrich Database. trans-cinnamic MSDS.

http://www.sigmaaldrich.com/catalog/product/aldrich/c80857?lang=en&region=
US (accessed 08/15/12)
Laboratory Safety
Don't needlessly endanger yourself or others
Laboratory safety is the single most important aspect of laboratory work. For the health and safety
of yourself and everyone else, it is imperative that you familiarize yourself with the following rules.
Flagrant or excessive violation of these rules may result in a zero for a lab assignment or possible
removal from the course.
1. Eye protection must be worn at all times. As soon as you enter the laboratory, you must put on
your safety goggles and you must wear them at all times during that laboratory period even if
you are not performing an experiment. You may not remove your safety goggles until you are
about to leave the laboratory. If you are caught not wearing safety goggles more than once, you
will be expelled from the laboratory for that entire laboratory period.
2. Do not wear contact lenses in lab. Students who wear glasses must also wear safety goggles
over their glasses.
3. Laboratory aprons must be worn at all times while in the laboratory.
4. You will be required to wear gloves when working with certain chemicals. Follow the
instructions of your instructor as to when gloves are required.
5. No open-toed shoes, sandals, bare feet or shorts are permitted in the laboratory.
6. Hair and loose items of clothing should be secured; otherwise, you'll be asked to leave.
7. No smoking, eating, drinking or chewing gum in the laboratory. Don't bring snacks or drinks to
lab.
8. All book bags and coats should be left outside the laboratory.
9. Do not enter the laboratory unless the instructor is present, even if the door is open.
10. Always follow the procedures given in your laboratory manual or approved by your instructor.
Do not change or modify the procedures or perform unauthorized experiments.
11. Proper handling of equipment and chemicals used in an experiment is your responsibility, if
you do not know how to operate the equipment or handle the chemicals, ask your instructor.
A. Be sure to check glassware for cracks before using it.
B. Acids should always be diluted by adding acid to water and not the reverse.
C. Use only the required chemicals in proper concentrations. Reading labels is your
responsibility,
D. Be sure you are aware of the hazards associated with a chemical before you use it.
Consult your laboratory text and check the Material Safety Data Sheets (MSDS) located
in the laboratory.
12. Keep your work area, including common areas (i.e. front bench, hoods) clean. Notify your
instructor of chemical spills. Your lab bench must be cleaned before leaving the laboratory.
Avoid needless skin contact with any solid or liquid chemical reagents.
13. Report all injuries, however slight, to the instructor.
14. Any special medical conditions (i.e., diabetes, allergies) must be reported to your
instructor at the beginning of the semester.
15. When heating a test tube, point its mouth away from yourself and others.
16. Hot plates, sand baths and heating mantles should not be used in the presence of highly
flammable materials. Organic solvents should be heated using an explosion-proof hotplate.
17. Always extinguish flames when NOT being used. Do not leave an open flame unattended.
18. Never inhale any gas of unknown properties.
19. Never taste anything in the laboratory.
20. Never pipette anything with your mouth. Always use a rubber bulb or pipet pump.
21. Be cautious when working with hot glassware. Hot glassware and cold glassware look the
same.
22. Use the fume hood when toxic or flammable vapors or gases may be released, The hood
sash should be maintained at a height of no more than 12 inches.
23. All waste should be disposed of properly. Nothing except water should go down the sink.
A. No chemicals should go down the drain or into the garbage can. Dispose of waste
chemicals in the waste containers provided.
B. Contaminated paper, plastic and glass (as well as broken glass) should be placed in the
red waste receptacles provided. Only uncontaminated paper or paper towels should go
in the ordinary trash.
C. In the case of broken glassware, notify your instructor.
24. All electrical equipment must be turned off and unplugged before leaving the laboratory.
25. Gas valves must be closed before leaving the laboratory.
26. Never sit on the lab bench where many different types of chemical residues may be present.
27. Your laboratory instructor will point out the following safety features. Be sure you know their
locations:
A. Shower: If you spill a large amount of substance on yourself, stand under the shower
and rinse thoroughly. Contaminated clothing should be removed immediately.
B. Eye wash: If any chemical gets in your eye or eyes, hold your eyes open with your
fingers and rinse them in the eye wash for at least 15 minutes.
C. Fire extinguisher & Fire blanket.
D. First aid kit.
E. All exits.
28. Be sure to wash your hands when you leave the laboratory.
29. Use of cell phones and personal audio equipment is strictly forbidden in the laboratory.
Laboratory Equipment
Check-in/Check-out Rules
Check-in Procedures
1 . Each student will be assigned a numbered drawer containing his laboratory equipment. A list
of the equipment that the drawer contains can be found in section of this manual. Each student
should make sure that all of the equipment on the list is indeed in his drawer and that none of
the glassware is cracked or broken.
2. Each student will be given a combination lock with which to lock his drawer. If the drawer is
left unlocked after the laboratory period is completed, the student will be held responsible for
any missing equipment.
During the Semester
I. If additional equipment, not in the drawer, is required for a particular experiment, each student
must sign out for his equipment and return it clean and in working order at the conclusion of
the laboratory period. If such equipment is not returned, or is returned damaged, the student
will be billed for its cost.
2. The equipment in the drawer is for the assigned student's use only and is not to be loaned to
fellow students.
3. All equipment removed from the drawer during the laboratory must be returned to the
drawer at the end of the day. Any equipment left out at the conclusion of the laboratory will be
confiscated.
4. Students who enroll in one section of laboratory in the fall semester may not switch into
another laboratory section for the spring semester unless a program conflict is demonstrated.
5. At the end of the semester, students will be billed for all broken or missing equipment if their
total bill exceeds $15 USD. The cost of not returning the combination lock is $16 USD. If any
glassware or equipment is broken or lost during the semester, the stockroom supervisor will
replace it and add its cost to the student's tab.
Check-out Procedures
1. All glassware must be returned clean. (Glassware should be washed with soap and
water and any labels must be removed.) If equipment is missing, its cost will be added
to the student's tab. Extra equipment must be returned to the stockroom. One may not
give any equipment to other students.
2. Once the student checks out, he can no longer work in the laboratory.
3. Students must check out on the assigned day: the last lab day of the spring semester as
indicated in the spring syllabus.
4. If a student fails to check out on the specified check-out day, or if a student drops the
course in the middle of the semester he must check out within 30 days of this last day
of attendance in the laboratory. If he fails to check out within 30 days, he will be billed
$50 USD for the necessary lock removal, equipment cleaning and drawer restocking. In
addition, the student will be billed for any missing or broken equipment. Failure to pay
this bill will result in barred registration and transcript service.
5. Any student who checks out on any day other than the specified check-out day must
schedule a check-out appointment in advance with the laboratory technician by calling
960-5494.
Laboratory #1
Introduction to Volumetric Glassware
I. Pre-Laboratory Assignment
Read Chapter III and Chapter IV in “Laboratory Handbook for General Chemistry”, view the pre-
lab video and read the laboratory procedure (below). Write an objective (paragraph form) and
procedure (flowchart) for this lab.
Answer the following questions in your laboratory notebook:

1. Define and explain the differences between TD and TC volumetric glassware. Give examples
of both.
2. In your own words, describe how you might use a volumetric flask to prepare 500 mL of a
1.0M HCl(aq) solution from stock solution of 10M HCl(aq).
3. Explain the distinction between accuracy and precision. How are mathematical quantities like
the mean (average) or standard deviation related to these quantities?
4. If you pipet ten different aliquots of water into a beaker, measuring the change in mass each
time, you might determine the mass of each of the ten aliquots to be similar but slightly
different. Explain how you might use these ten masses and the density of water to compute the
accuracy and precision of the liquid volumes delivered by the pipet.
II. Laboratory Procedure
Part A - Quantitative precision of TD glassware

Execute the following procedure once for each type of TD glassware---a buret, a 10 mL
volumetric pipet, and a 10 mL Mohr or serological pipet. You are given a 100 mL volumetric
flask into which you will deliver the water. Discard the collected water only after each
experiment is complete.
1. Clean and dry your volumetric flask.
2. Measure the mass of the empty volumetric flask.
3. Deliver 10 mL of the water from your TD glassware into your flask. If you are using a buret,
be sure and record the initial and final readings so that you can calculate the dispensed volume
from the difference in the final and initial readings. Always be sure to use the correct
number of decimal places!
4. Record the total mass of the flask after adding a 10 mL aliquot and compute the change in
mass due to adding the water.
5. Repeat the last two steps until you have added a total of 100 mL of water to the flask. (10
aliquots).
6. Use a thermometer to measure the temperature of the water in the flask.
7. Use the below table to determine the density of water at your measured temperature.
Density of Water in g/L at Various Temperatures and 1 atm.

T (°C) xx.0 xx.1 xx.2 xx.3 xx.4 xx.5 xx.6 xx.7 xx.8 xx.9
20 998.23 998.21 998.19 998.17 998.15 998.13 998.11 998.09 998.07 998.04
21 998.02 998.00 997.98 997.96 997.93 997.91 997.89 997.87 997.85 997.82
22 997.80 997.78 997.75 997.73 997.71 997.69 997.66 997.64 997.62 997.59
23 997.57 997.54 997.52 997.50 997.47 997.45 997.42 997.40 997.38 997.35
24 997.33 997.30 997.28 997.25 997.23 997.20 997.18 997.15 997.13 997.10
25 997.08 997.05 997.02 997.00 996.97 996.95 996.92 996.89 996.87 996.84
26 996.81 996.79 996.76 996.73 996.71 996.68 996.65 996.63 996.60 996.57
27 996.54 996.52 996.49 996.46 996.43 996.41 996.38 996.35 996.32 996.29
28 996.26 996.24 996.21 996.18 996.15 996.12 996.09 996.06 996.03 996.00
29 995.98 995.95 995.92 995.89 995.86 995.83 995.80 995.77 995.74 995.71
30 995.68 995.65 995.62 995.59 995.56 995.53 995.50 995.46 995.43 995.40
8. Assuming this density is exact (i.e. contains no uncertainty) convert the mass of each of the
ten aliquots into a corresponding volume and compare these actual volumes with the volumes
you thought you dispensed in order to determine the average deviation in delivered volume
( mL).
9. Design a similar approach to compute the standard deviation of the volumes ( mL).
Part B - Preparation of a solution from a solid and preparation of a solution by

dilution
You are required to make 50.00 mL of an aqueous solution of CuSO4 5H2O whose concentration
is 1.00×10−2 M.
1. Determine the mass of CuSO4 5H2O present in a solution having the concentration specified
above.
2. Measure out this amount of CuSO4 5H2O and dissolve it in approximately 10 mL of distilled
water in a small beaker.
3. Transfer this solution carefully to a 50.00 mL volumetric flask. Rinse out the beaker multiple
times with a small amount of distilled water, transferring the rinse water into the volumetric
flask each time.
4. Add distilled water to the volumetric flask until the lower meniscus of the solution coincides
with the mark in the volumetric flask. You may wish to use a pipet for more control as you
approach the mark.
5. Close the flask with the stopper and invert several times to mix. Note the appearance of this
final stock solution.
6. Calculate the amount of stock solution needed to prepare 10.00 mL of 5.00×10−4 M
aqueous solution of CuSO4 5H2O.
7. Using a pipet, transfer the calculated amount volume into a 10.00 mL volumetric flask.
Prepare the solution by filling the volumetric flask up to the mark with distilled water. Note the
appearance of the solution.
III. Post Laboratory Questions

Answer the following questions in your laboratory notebook. Turn them in at the end of the
laboratory period.
1. What is the accuracy with which volume can be measured using each type of glassware?
What is the precision with which volume can be measured using each type of glassware? Do all
of the types of TD glassware used appear to be equally accurate and precise?
2. Does the uncertainty in your temperature measurement influence your results substantially?
Explain.
3. Describe possible sources of error (systematic and random) in your experiment and rank
them according to which you think would most strongly affect your results. Which of your
measured quantities (mass, volume, temperature) are the least precise?
Laboratory #2
Synthesis of Alum
Read Chapter VII in “Laboratory Handbook for General Chemistry”, view the pre-lab video and
read the laboratory procedure (below). Write an objective (paragraph form) and procedure
(flowchart) for this lab.
Answer the following questions in you laboratory notebook:
1. What is the balanced overall chemical reaction you will be carrying out?
2. How will you isolate the alum from the reaction mixture? What physical property will you
exploit?
3. Explain how recrystallization works. What factors influence your yield from recrystalization?
1. Into a pre-weighed 150 mL beaker, add about 0.5 g of aluminum foil. Be sure to
record the exact mass added.
2. Add a magnetic stir bar to the beaker. Slowly add 25 mL of 1.4M KOH (aq) solution
to the beaker containing the aluminum. CAUTION: KOH (aq) IS CAUSTIC
3. Gently heat the beaker on a warm hotplate (do not boil!) with stirring until all the
aluminum has dissolved. Remove the beaker from the hotplate and set aside while
assembling your filtration apparatus.
4. Support a glass stem funnel on an iron ring attached to a ring stand over a clean 150
mL beaker. Fold a piece of filter paper into quarters by folding it in half twice. Open
one edge of the filter paper into a cone and insert it into the funnel. Wet the filter
paper with a small amount of distilled water.
5. Obtain 10 mL of 9M H2SO4 (aq) and add it carefully but quickly to your beaker of
warm aluminum solution while stirring with a long glass rod. CAUTION: H2SO4 (aq)
is caustic and this reaction is exothermic. If your addition is too slow, you may
see temporary formation of Al(OH)3 precipitate. This should dissolve with additional
stirring.
6. Stir the solution. If after several minutes white crystals persist, heat the solution
gently on a hotplate until all solid is dissolved. DO NOT BOIL. If solid persists, you
may add an additional 1-2 mL of 9M H2SO4 (aq).
7. Allow the solution to cool until it is safe to handle (warm/hot). Using your stirring
rod to direct the flow of fluid, filter the hot solution into the fresh beaker. Do not let
the liquid level in the funnel rise above the level of the filter paper. The filtrate should
be clear.
8. Fill a 600ml beaker about half full of crushed ice. Place the beaker with filtrate in
the ice bath for about 20-30min. Stir the solution frequently as crystals of alum form.
9. While solution is cooling, set up a suction filtration apparatus. Place the circle of #5
filter paper in the Buchner funnel and moisten the filter paper with distilled water to
hold it in place.
10. Once your solution has cooled for about 20 minutes, record the temperature of the
solution using a thermometer. The temperature should be below 6 °C.
11. Turn on the vacuum to your suction filtration apparatus. Swirl your solution in the
beaker to suspend the crystals and pour your solution into the funnel. Be sure to
transfer all of the solid into the funnel using your rubber policeman. Rinse any leftover
crystals stuck to the beaker into the funnel using small portions of methanol.
12. Once filtered, rinse the crystals with two 10 mL portions of methanol to get rid of
residual supernatant and sulfuric acid. Continue to pull air through the funnel for an
additional 10 minutes to dry the crystals.
13. Once dry, turn off the vacuum and transfer the crystals to a pre-weighed 250 mL
beaker. Record the mass of the beaker with crystals in it, and determine the mass of
the crystals by subtraction.
14. Transfer your crystals to a plastic vial. Label them with your name, the mass of the
crystals, and the identity of the substance. Store the crystals in your drawer for the
next laboratory. DO NOT DISCARD YOUR CRYSTALS.
III. Post-Laboratory Questions
Answer the following questions in your laboratory notebook. Turn them in before
leaving the laboratory.
1. What is your theoretical yield (in g) of alum given the amount of aluminum metal
you added to your reaction?
2. What is your experimental yield of alum?
3. Were you expecting to get a near 100% experimental yield of alum from your
synthesis? Why or why not. What was the largest source of error in your
synthesis?
Laboratory #3
Spectrophotometric Analysis of Aluminum in Alum
Read Chapter IX and XIII in “Laboratory Handbook for General Chemistry”, view the pre-lab
video and read the laboratory procedure (below). Write an objective (paragraph form) and
procedure (flowchart) for this lab. Familiarize yourself with how you will calculate the
concentration of Al3+ initially present in each solution form Part A.
1. What is the Beer-Lambert Law? Write it and identify all the variables in the equation as well
as the units they are typically expressed in.
2. Draw an example of what you expect your Beer’s Law Plot will look like. Be sure to label
your axes, the slope and the y-intercept. Indicate what information you can determine from the
slope and what value you expect the y-intercept to be.
3. Assuming a path length of 1.3 cm for your spectrophotometer tube, an extinction coefficient
at λmax of ε = 10,400 M-1cm-1 and an absorbance of 0.24 in Part D, what would be the
concentration of Al3+ in the 100mL solution prepared in Part D, step 4?
Part A. Preparing solutions of known Al3+ concentration.
1. Prepare an Al3+ (aq) stock solution by pipetting 3.00 mL of the aluminum solution into a
25mL volumetric flask. Dilute to the mark and mix thoroughly.
2. Number five 10-mL volumetric flasks 1 to 5.
3. Add the following amounts of aluminum stock solution to each volumetric flask. Use a Mohr
pipet to measure each volume.
Flask #1 #2 #3 #4 #5
Volume Al3+ stock solution (mL) 0 0.10 0.20 0.40 0.60
4. Add 4 mL of the acetate buffer solution and 1 mL of the aluminon solution (in that order!)
to each flask and swirl gently to mix. You may use a graduated cylinder for these
measurements.
5. Dilute the solutions in each flask to the mark by adding distilled water and mix thoroughly.
Allow the solutions to sit for 20 min while monitoring the solutions’ colors. Note any changes in
your notebook.
Part B. Absorbance Spectrum of Al3+-Aluminon complex and determination of λmax
1. Follow the spectrometer's operating instructions to ready the instrument for use.
2. Fill a spectrophotometer tube about 2 cm from the top with the buffer solution to use as a
blank. Only touch the tube at the very top, where this is no solution. Wipe the outside of the
tube with a KimWipe thoroughly before inserting the tube into the spectrophotometer. You
may use this tube and solution as a blank throughout your experiment, so do not discard it.
3. Fill another spectrophotometer tube with solution #4 in similar fashion.
4. Build an absorbance spectrum by taking absorbance measurements of solution #4 in 10nm

increments in the range of 450nm-550nm. You will need to use your blank to zero the
spectrometer each time you change the wavelength. Instructions are printed on the
spectrophotometer. Record and tabulate your data in your notebook. Be sure to record the
path length of spectrophotometer tube. DO NOT DISCARD YOUR SOLUTIONS YET.
5. Transfer your data to Excel and make a scatter plot to generate your absorbance spectrum.
Be sure to label your axes. You may connect the dots with a smoothed line. From your plot,
find λmax of the Al3+-Aluminon complex.
6. Before you proceed, check your results with your instructor to get approval to move on to
Pact C.
Part C. Beer’s Law Plot and Determination of the Extinction Coefficient.
1. Measure the absorbance of solutions #1 -#5 at the λmax you determined from your
absorbance spectrum. Record and tabulate the data in your notebook as below.
Flask Al3+ Concentration (M) Absorbance

Flask #1 0.000 0.000
2. Transfer your data to excel, and create a scatterplot of absorbance as a function of

concentration of Al3+. Be sure to label your axes and title your plot. Fit a linear trendline to
your data, and be sure to check the “display equation” and “display R2” option boxes.
3. From your trendline, determine the extinction coefficient of the Al3+-Aluminon complex.
Part D. Determination of Aluminum Content in Alum
1. Precisely weigh about 0.2 g of your alum. Be sure to record the mass to 3 decimal places.
2. Transfer the alum to a small beaker and add distilled water to bring the volume to about 15
mL. Place the beaker on a hot plate in the hood, cover with a watch glass and heat just to
boiling. Stir the solution occasionally with a glass stirring rod. After you stir, be sure to rinse the
glass rod off into the beaker with a small amount of distilled water from your wash bottle.
3. While the alum mixture is heating, clean and dry (exterior only) a 100 mL volumetric flasks.
Prepare for a gravity filtration directly into the 100-mL volumetric flask using a long-stemmed
glass funnel.
4. Remove the beaker from the hot plate just as the solution starts to boil. CAUTION: The
beaker, watch glass and the hot plate's top are all hot! Immediately pour the hot
solution into the funnel. As the solution is being filtered rinse the beaker, the bottom of the
watch glass and the stirring rod each with several small washes of distilled water into the
funnel. When the solution is completely filtered, remove the funnel from the volumetric and
rinse the volumetric's neck with several small portions of distilled water. DO NOT ADD SO
MUCH WATER THAT YOU COMLETELY FILL THE VOLUMETRIC FLASK. Once the volumetric
flask is cool, dilute the solution in the flask to the mark.
5. Transfer 3.00 mL (use a volumetric pipet or Mohr pipet) of this solution to a 25-mL
volumetric flask and dilute to the line.
6. Pipet 0.60 mL of the alum solution that you just prepared into a 10-mL volumetric flask.
Add 4 mL of acetate buffer and 1 mL of aluminon solution (as you did in Part A) then dilute to
the mark with distilled water. Wait 20 min and measure the absorbance at the λmax you
determined. Record this value in your notebook.
Answer the following questions in your laboratory notebook. Turn them in before leaving the
laboratory. Be sure to turn in plots of your absorbance spectrum and Beer’s law plot.
1. Using your Beer’s Law plot, assess the quality of your determination of the extinction
coefficient. Do you have any reason not to trust the data?
2. Using your absorbance data from Part D, what is concentration of Al3+ you made in Part
D, step 4?
3. What is the mass% of aluminum in your alum sample? Is this what you expected? Why
or why not.
4. What were the significant sources of error in your experiment?

Laboratory #4
Thermometric and Potentiometric Titration of an Unknown Hydrochloric Acid Solution
Read Chapter X in “Laboratory Handbook for General Chemistry”, view the pre-lab video and
read the laboratory procedure (below). Write an objective (paragraph form) and procedure
1. What is the reaction you will study during the thermometric titration and the potentiometric
titration?
2. Explain in your own words how you will determine the equivalence point of the thermometric
titration. Draw a picture to illustrate.
3. What is KHP and how will it be used in this experiment? Include a Lewis structure and
balanced chemical equation.
Part A. Preparation of a standardized NaOH (aq) solution
1. Calculate and weigh out the necessary amount of solid NaOH required to make 150 mL of
1.50M NaOH (aq) solution. When weighing the NaOH, there is no need to strive to perfection
because you will standardize this solution later to determine its exact concentration.
2. Transfer the NaOH to a 250 mL Erlenmeyer flask and add 150 mL of distilled water from a
graduated cylinder. Stir until the NaOH dissolves and be sure to seal the flask whenever it is not
in use. This is your NaOH (aq) stock solution. CAUTION: NaOH (aq) is caustic.
3. Prepare a dilution of your ~1.5M NaOH solution transferring 5.00 mL of the solution with a
volumetric pipet to a 50 mL volumetric flask. THIS MUST BE DONE WITH BOTH ACCURACY
AND PRECISION. Dilute the solution to the line with distilled water and mix well. Repeat this
procedure two additional times so that you have 3 solutions of diluted NaOH (aq) that is
approximately 0.15M.
4. You will standardize your solutions by reaction with Potassium acid phthalate, KHP.
KHP reacts with NaOH in a 1-to-1 fashion according to the following equation.
Calculate and weigh out the correct amount of KHP (mw 204.23 amu) required to react
stoichiometrically with 10.0 mL of your diluted NaOH (aq) solutions that are
approximately 0.15M. Be sure to record the mass of KHP to 3 decimal places. Add the
KHP to a small beaker. Repeat this 2 additional times so that you have 3 beakers with
KHP in them. Label each beaker so you know the mass of KHP in each beaker and
record this in your notebook by setting up a table like the one below.
Beaker Mass KHP (g) Moles KHP Titration Volume True concentration of
~.15M NaOH NaOH (aq)
5. To each beaker containing KHP add 50 mL of distilled water and a stir bar to dissolve
the KHP. Once dissolved, add 2 drops of phenolphthalein indicator to each beaker as
well.
6. After rinsing your buret with a few mL of one of the 50mL NaOH solutions that are
approximately 0.15M, fill the buret with the same NaOH solution.
7. Titrate one of the KHP solutions with the NaOH solution in the buret until the
solution in the beaker turns faint pink. This is the equivalence point, where the moles of
NaOH added are equal to the moles of KHP initially present. Record the volume of
NaOH required for the titration.
8. Repeat this 2 additional times for the 2 remaining beakers. Use a different NaOH
solution for each titration.
9. Determine the average concentration of the NaOH STOCK SOLUTION from your
data. (You may do this at the end of the lab if you are running behind).
Part B. Potentiometric titration of an unknown hydrochloric acid solution
1. Add exactly 20.00 mL of HCl (aq) solution to a 100 mL beaker with stir bar.
2. Fill you buret with your ~1.5M NaOH (aq) stock solution. Be sure to rinse the buret
with a few mL of the solution first.
3. Open Logger Pro. Place the pH electrode into your beaker containing the HCl (aq)
solution. Set up a table in you notebook to record the volume of NaOH (aq) added and
the pH.
4. Titrate the HCl (aq) solution with your NaOH (aq) solution by adding a small amounts
of your NaOH (aq) solution from the buret. Be sure to note initial volume on the buret
and the final volume on the buret after addition of an aliquot. Record the volume
added and the pH both in Logger Pro and in your notebook.
5. Continue to add small aliquots until your pH is over pH = 9.
6. The equivalence point should be around pH=7.0 and reflect a maximum in the d(pH)
plot, and a zero of the d(dpH) plot.
Part C. Thermometric titration of an unknown hydrochloric acid solution
1. Add exactly 20.00 mL of HCl (aq) solution and stir bar to a thermos.
2. Fill you buret with your ~1.5M NaOH (aq) stock solution. Be sure to rinse the buret
with a few mL of the solution first.
3. Unplug the pH electrode from channel 1 on the port hub. Plug in the temperature
probe to channel 1 on the port hub. Open Logger Pro. Insert tip of the buret into one
of the openings on the rubber stopper of the thermos. Insert the thermocouple probe
into another opening so it is immersed into the Hydrochloric Acid solution. Set up a
table in you notebook to record the volume of NaOH (aq) added and the temperature of
solution.
4. Titrate the HCl (aq) solution with your NaOH (aq) solution by adding about 3 mL of
NaOH (aq) solution from the buret at a time. The temperature of the solution will go
up with each addition until the equivalence point is reached. Be sure to note initial
volume on the buret and the final volume on the buret after addition of each aliquot.
Record the volume added and the maximum temperature achieved after each addition
both in Logger Pro and in your notebook.
5. Continue to add small aliquots until you have enough data to determine the
maximum overall maximum temperature achieved by the solution. This means you
must titrate past when the temperature stops increasing.
6. Transfer your data to excel and plot a graph of temperature against the total volume
of base added. Use extrapolation of the two sections of the graph to deduce the
maximum temperature reached without heat loss. This will be your equivalence point.
laboratory. Be sure to also turn in plots of all your experimental data.
1. What is the concentration of your standardized NaOH (aq) stock solution?
2. What is the concentration of the unknown HCl solution as determined by potentiometric

titration?
3. What is the concentration of the unknown HCl solution as determined by thermometric
titration?
4. What are the major sources of error in each part of the experiment? Which method of
titration yielded more accurate results? Which yielded more precise results?
Laboratory #5
Determination of Heat of Formation of Magnesium Oxide Using Calorimetry and Hess’s Law.
View the pre-lab video and read the laboratory procedure (below). Review Hess’s Law and
calorimetry in your text book. Write an objective (paragraph form) and procedure (flowchart)
for this lab.
1. In this lab you will carry out the reactions represented in equations (1) and (2) below and
measure their associated enthalpies. Show how you can determine the enthalpy of formation
of MgO using ΔH3 and the measured quantities ΔH1 and ΔH2.
(1) Mg(s) + 2 H+ (aq) Mg2+(aq) + H2 (g) ΔH1 = ??
(2) MgO(s) + 2 H+(aq) Mg2+(aq) + H2O (l) ΔH2 = ??
(3) H2 (g) + ½ O2 (g) H2O (l) ΔH3 = −285.8 kJ/mol
2. Explain how you will use the ΔT measured in Part A to determine the calorimeter constant.
3. What equations and relationships will you use to determine the enthalpy of reaction from
the change in temperature of the solution during each chemical reaction?
4. What is the literature value of ΔHf of MgO?
Part A. Determination of the Calorimeter Constant
We will use a reaction with a known ΔH to measure the calorimeter constant.
OH−(aq) + H+(aq) H2O (l) ΔH4 = known.
Temperature ΔH4 (kJ/mol)

(°C)
21 -58.01
22 -57.81
23 -57.61
24 -57.41
25 -57.20
1. Assemble the calorimeter as instructed and open Logger Pro.
2. Measure 20.0 mL of the provided standardized 1.0 M HCl(aq) solution using a graduated
cylinder. Be sure to record the exact concentration from the bottle. Using another graduated
cylinder, measure 30.0 mL of the provided standardized 1.0 M NaOH (aq).
3. Using a thermocouple, take the initial temperature of both solutions. Make sure they are
similar temperatures before proceeding.
4. Remove the cover of the calorimeter. Pour the HCl (aq) solution into the calorimeter, start
the data collection, then pour the NaOH (aq) solution into the calorimeter as well. Replace the
cover of the calorimeter. The temperature should begin to rise.
5. Monitor the temperature as the reaction proceeds and note when the temperature begins to
fall. Continue to collect data for 1 minute after the temperature begins to fall. After this point,
you may stop data collection. Be sure to save your file.
6. Empty your calorimeter, rinse it with distilled water, and dry it with paper towels.
7. Determine ΔT for the experiment and the calorimeter constant.
Part B. Measuring ΔH1
1. Measure 50 mL of 2M HCl (aq) in a graduated cylinder and transfer it to the calorimeter.
2. Obtain a strip of Mg(s), lightly scour it with sand paper, wind it into a small coil and then
obtain the mass of the strip of magnesium.
3. Start data collection on Logger Pro.
4. Add the magnesium strip to the calorimeter, making sure the entire strip is submerged.
Quickly note any observations, and replace the calorimeter cover.
5. While the reaction proceeds, you will need to gently swirl the solution occasionally. Monitor
the temperature as the reaction proceeds and note when the temperature begins to fall.
Continue to collect data for 1 minute after the temperature begins to fall. After this point, you
may stop data collection. Be sure to save your file.
7. Determine ΔT and use the calorimeter constant to determine ΔH1.
Part C. Measuring ΔH2
1. Find the mass of a weighing paper. On the weighting paper, weigh about 0.250g of MgO(s).
This does not have to be exact, but be sure to record the mass precisely.
2. Measure 50 mL of 2M HCl (aq) in a graduated cylinder and transfer it to the calorimeter.

3. Start data collection on Logger Pro.
4. Add the MgO to the calorimeter, quickly note any observations, and replace the calorimeter
cover. You do not have to get all of the MgO out of the weighing paper, but be sure to get
most of it.
5. Mass the weighing paper again to determine how much MgO remained on the paper so that
you can calculate how much MgO was delivered into the calorimeter.
6. While the reaction proceeds, you will need to gently swirl the solution occasionally. Monitor
the temperature as the reaction proceeds and note when the temperature begins to fall.
Continue to collect data for 1 minute after the temperature begins to fall. After this point, you
may stop data collection. Be sure to save your file.
8. Determine ΔT and use the calorimeter constant to determine ΔH2.
laboratory. Be sure to print plots of all your titrations, and indicate you’re the maximum T
reached.
1. Use Hess’s Law to determine ΔHf of MgO.
2. What are the principle sources of error in your experiment? To what level of precision
are you confident in your value of ΔHf of MgO?
3. Is your measured value of ΔHf of MgO consistent with the literature value?
Laboratory #6
Kinetics of Decomposition of Crystal Violet Dye
Review the use of the Spec 20 and Laboratory #3. Review Chapter 13 in your text book,
lecture notes and view the pre-lab video. Read the laboratory procedure (below). Write an
objective (paragraph form) and procedure (flowchart) for this lab.
Answer the following questions in your laboratory notebook:
1. Write a generic rate law for the reaction you will be studying.
2. How does the flooding method allow you to determine the rate law of a reaction?
3. What relationship will allow you to change your absorbance data to concentration data?
4. Write an expression for kobs in terms of the true rate constant and the concentration of
flooding reactant for your reaction.
You will work in groups of 2 for this experiment.
Part A. Absorption Spectrum of Crystal Violet
1. Using the supplied stock solution of Crystal Violet (1.0×10-5M), build an absorption spectrum
for crystal violet from 465nm – 605nm. Increments of 25nm will be sufficient. It is okay if your
absorption spectrum has some absorbance values higher than 1.0 as long as the maximum
observed absorbance is less than 1.5.
2. Determine λmax from your spectrum.
Part B. Beer’s Law Plot and Determination of Extinction Coefficient.
1. Build a Beer’s law plot for the absorption at λmax from your stock solution. Be sure to make
and use solutions such that your maximum absorbance is not higher than 1.0 and goes down to
0.1.
2. Determine the extinction coefficient for the absorption at λmax from your plot.
Part C. Kinetics of decomposition of crystal violet by flooding.
1. You will determine the kinetics of crystal violet formation by flooding experiments.
You will need to select a concentration of crystal violet that will have starting
absorbance around 0.75-1.0 AFTER MIXING WITH OTHER REAGENTS. You will need to
make enough of this crystal violet solution to use in all of your experiments below.
2. You will conduct 3 experiments, one using 1000 fold excess of OH−(aq), one using a
2000 fold excess of OH−(aq), and one using a 4000 fold excess of OH−(aq). The
easiest way to conduct the experiment is to mix relatively large volumes of the crystal
violet solution and sodium hydroxide solution in 50ml Erlenmeyer flask, then quickly
transfer a small amount of the reaction solution to your spectrophotometer tube for
analysis. You will be provided 0.10M NaOH (aq). Build a table in your lab notebook like
the one below that lists the amounts of reagents for each experiment.
Experiment Excess Total Volume Volume Volume [CV+]o [OH-]o

of OH− Volume Crystal Violet 0.10M NaOH H2O
(aq) (aq)
1 1000 eg 25 mL 15ml 2ml 8
2 2000 eg 25 mL 15ml 4ml 6
3 4000 eg 25 mL 15ml 8ml 2
3. Have your table checked by your instructor. Then conduct the experiments by first
zeroing the spectrophotometer with a blank at λmax. Create an excel spreadsheet that
has a column for time, and a column for absorbance (or transmittance). Be sure to
populate the time column with 60sec intervals for the “1000 fold” run and 20s intervals
for the 2000 fold and 4000 fold runs BEFORE you start the experiment. Once you
prepare your spread sheet add to a 50ml Erlenmeyer flask required amount of water,
then sodium hydroxide solution, and then the crystal violet solution. Quickly mix, then
transfer to your spectrophotometer tube and begin data collection. Run each
experiment for the following time length.
Excess of OH− Approximate Reaction Time (min) Data Recording Interval (s)
1000-fold 21 60
2000-fold 10 20
4000-fold 5 20
4. Record the absorbance (or transmittance) reading every 60s for the 1000-fold run
and every 20s for the 2000fold and 4000fold runs as above. One partner should
monitor the time and read the absorbance, while the other partner records the data in
excel and a lab notebook. REPEAT EACH EXPERIMENT 2 times. Since for the 1000-fold
experiment you have a minute between each reading, you should be able to run two
trials simultaneously.
Part D. Analysis
1. Convert your absorbance data to concentrations. Determine if the order in crystal

violet is zero-order, 1st-order, or 2nd order by graphical methods as described in your
textbook and the lab lecture.
2. Determine the average observed rate constant (kobs) for each experiment group.
3. Determine the order in [OH−] by comparison of your kobs values from different
experiments.
laboratory. Be sure to turn in your absorption spectrum, Beer’s law plot and plots of all your
kinetic data, as well as those required to determine the true rate constant.
1. What is the rate law for the decomposition of crystal violet?
2. What is the rate constant for the decomposition of crystal violet at room temperature?
3. What are the principle sources of error in your experiment?

Laboratory #7
Characterization of Complex Ion Equilibria of Co2+
Review the use of the Spec 20 and Laboratory #3. Review Chapter 14 in your text book,
lecture notes and view the pre-lab video. Read the laboratory procedure (below). Write an
objective (paragraph form) and procedure (flowchart) for this lab.

1. Write an overall balanced equation for the synthesis of bis(tetraethymammonium)
tetracholorocobaltate in part 1 of this lab.
2. Write an equilibrium constant expression for the below reaction occurring in ethanol solution.
3. Describe how the equilibrium from (1) would respond according to LeChatlier’s principle if:
(a) Chloride ion was removed from the system
(b) Chloride ion was added to the system
(c) the reaction was endothermic (as written) and heat was applied to the system
(d) the reaction was exothermic (as written) and heat was applied to the system

The tetrachlorocobaltate dianion participates in the following equilibrium:
In this experiment you will:
a) Synthesize bis(tetraethymammonium) tetracholorocobaltate
b) Determine the color of each cobalt species in the equilibrium above.
c) Determine the equilibrium constant for the reaction
d) Observe the effect of temperature on the equilibrium, and determine if the reaction is
exothermic or endothermic
Part A. Synthesis of bis(tetraethymammonium) tetracholorocobaltate.
1. Dissolve 1.19g (0.005mol) of cobalt (II) chloride hexahydrate into 5ml of absolute ethanol in
a beaker.
2. Place the beaker on an explosion proof hotplate, and warm to about 70-75°C to dissolve the
solid.
3. Dissolve 1.84g (0.01mol) of tetraethylammonium chloride monohydrate in 5ml of absolute
ethanol in 250ml Erlenmeyer flask. Warm the flask on the explosion proof hotplate.
4. Once all solids are dissolved in both flasks, slowly add cobalt (II) chloride solution to
tetraethylammonium chloride solution.
5. Cover the flask with a small watch glass. Heat the resulting mixture until it starts to boil.
While keeping the solution hot/refluxing, add more ethanol using beral pipette until all solid
dissolves. It will take about 70ml of ethanol to dissolve the solid. Swirl the flask to make sure
that no crystals stick to the walls. Caution: Your flask will be hot! Use your hot hand
protector to handle the flask.
6. Remove the solution from the hotplate, and place the flask on a paper towel on the bench
top to cool. Precipitate should form upon cooling.
7. Add about 75mL of water to a 100mL beaker, and heat it on the hotplate to not more than
60 °C. This bath will be used in part D)
8. After the flask containing your cobalt solution as cooled to about room temperature (~10
minutes), partially submerge the flask in an ice bath to cool the solution further for 10
additional minutes. While mixture is cooling setup a suction filtration apparatus.
9. Filter your cold mixture. Rinse the flask with few ml of cold absolute ethanol to get the
remaining crystals out. Leave your product in the funnel with vacuum on for 5 minutes to let it
dry. Find the mass of your product
Part B. Determination of the color of CoCl42- and Co(H2O)62+
1. Weigh about 185 mg of your product and dissolve it in enough 95% ethanol to make a
25 mL stock solution. You don’t need to be exact when weighing your product, but be sure to
record your mass. Note the color of your solution. DO NOT DISCARD THIS SOLUTION
UNTIL THE END OF THE EXPERIMENT!
2. Remove about 2-5mL of your stock solution and transfer to a test tube. Add 4-8 drops of 1M
Ag(NO3) (aq) to the tube, mix and let settle.
3. Remove another 2-5mL of your stock solution and transfer to another test tube. Add 4-8
drops of 1M Tetraethylammonium chloride in ethanol solution.
4. Using your knowledge or LeChatlier’s principle and the results from the above experiments,
determine which cobalt complex ion is pink, and which is blue.
Part C. Determination of Equilibrium Constant.
1. Transfer about 5-7 mL of your stock solution into a spectrophotometer tube
2. Obtain absorbance readings at 519nm and 656nm. Be sure to blank the spectrophotometer
tube at the appropriate wavelength with your solvent. DO NOT DISCARD YOUR TUBE OR
SOLUTION.
3. Write the law of mass action equilibrium expression for the equation above. Given that 95%
ethanol is 2.8 M in water, 519nm = 7.5 M-1cm-1 and 656nm = 220 M -1cm-1, determine the value
of the equilibrium constant. HINT: set up an ICE table starting with a known initial
concentration of CoCl42-, known initial concentration of H2O, and no Co(H2O)62+ or Cl-. Fill in
the equilibrium values that you know and infer the rest of the table.
Part D. Observation of the effect of temperature on the equilibrium.
1. Place you spectrophotometer tube in an ice-water bath for 5 minutes, then determine the
temperature of the solution. Note any observations.
2. Obtain absorbance readings of your cold solution at 519nm and 656nm. Be sure to place the
solution back in the icebath while you re-zero the spectrophotometer between measurements.
3. Place your spectrophotometer tube in the warm water bath (prepared in part A) for 5
minutes. DO NOT BOIL THE WATER, THE WATER MUST NOT BE HOTTER THAN 60 °C.
4. Obtain absorbance readings of your hot solution at 519nm and 656nm. Be sure to place the
solution back in the warm water bath while you re-zero the spectrophotometer between
measurements.
laboratory.
1. What is the %yield of your synthesis of bis(tetraethymammonium)

tetracholorocobaltate? What are the most significant sources of error in your
synthesis?
2. What is the value of the equilibrium constant for the below reaction?
3. Using your knowledge or LeChatlier’s principle and the results from the part D,
determine if the equilibrium is endothermic or exothermic as written above. Are your
visual observations consistent with your spectrophotometer readings?
4. What are the principle sources of error in your experiment?

Laboratory #8
Determination of Nitrogen Content in Soil
Week 1: Set-up of experiments. Complete at end of Laboratory 7.
Read the laboratory procedure (below). Write an objective (paragraph form) and procedure
(flowchart) for this lab. Copy the following table.
Sample Sample Mass Volume Volume Mass Mass Volume

Cup Name wet boric 2M Devarda’s MgO ammonia
soil (g) acid / KCl(aq) Alloy standard
indicator (mL)
(mL)
A Soil Sample ~15 20 mL 0

A
B Soil Sample ~15 20 mL 0

B
C Control – 0 ~15 20 mL 0
No Soil
D Control – 0 ~15 20 mL 2.00

Known
Ammonia
1. Collect 4 small plastic sample cups. Add about 15mL of boric acid solution with indicator to
each cup. Set aside.
2. Collect 4 large sample cups, label them A-D. To each cup add 20 mL of 2M KCl(aq) solution
using a graduated cylinder.
3. Cup A: Measure about 1 g of soil and add it to sample cup A. Be sure to record the exact
mass of soil you add. Quickly sprinkle about .2g of Devarda’s Alloy and .2g MgO over the soil
mixture and swirl the cup to mix. Immediately after mixing, insert one of the smaller cups
containing boric acid solution into the large cup and seal the large cup with a cover. Place a
sticker on the large cup with your name and “Soil Sample A”.
4. Cup B: Prepare exactly as cup A. Place a sticker on the large cup with your name and “Soil
Sample B”.
5. Cup C: Quickly sprinkle about .2g of Devarda’s Alloy, 0.2g of MgO over the solution in cup
C, and swirl the cup to mix. DO NOT ADD SOIL TO THIS CUP. Quickly place one of the smaller
cups containing boric acid solution into cup C and seal with a lid. Place a sticker on the large
cup with your name and “Control – No Soil”.
6. Cup D: Add exactly 2.00mL of ammonia standard solution to sample cup D using a
volumetric pipet or Mohr pipet. Quickly place one of the smaller cups containing boric acid
solution into cup D and seal with a lid. Place a sticker on the large cup with your name and
“Control – Known Ammonia”. Be sure to record the exact concentration of N in the standard.
7. Place all your sample cups in the designated storage area until next lab period.
8. Weigh a small aluminum boat and record its mass to 3 decimal places. Weigh approximately
1 g of soil onto the boat and record the total mass (wet soil + boat) to 3 decimal places. Label
a small watch glass with your name. Place the boat with the soil on top of the labeled watch
glass and place them in the oven to dry until next lab period.
Week 2: Analysis of Nitrogen content in soil.
View the lab lecture video for this experiment. Read the laboratory procedure (below). Write an
objective (paragraph form) and procedure (flowchart) for this lab. Answer the following
questions:
1. How will the boric acid /indicator solution allow you to determine the amount of nitrogen in
your soil.
2. Briefly explain (max 2 sentences each) the following:

a) What will you learn from the experiment in sample cup “Control – No Soil”?
b) What will you learn from the experiment in sample cup “Control – Known Ammonia”?
c) How will you determine the mass% of water in your soil sample?
3. How will you use the results from the control experiments to increase the accuracy of your
results?
The mineral nitrogen in your soil samples has been converted to ammonia. The ammonia has
been absorbed by the boric acid solution according to the below equation. Note that ammonia
acts a bas in this equation.
(1)
Upon generation of H2BO3 the indicator changes color. In this part of the experiment you will
determine how much H2BO3− was formed by titrating the boric acid indicator solution with acid
to reform H3BO3 (aq) and turn the solution back to its original color.
(2)
Part A. Practice titration
Before titrating the solution from your soil analysis, it will be helpful to practice the titration.
1. Add 15 mL of boric acid/indicator solution to a beaker with stir bar. Note the color.
2. Add exactly 2.00mL of “N standard solution” to the beaker and note any color change. The
“N standard solution” is actually just NaOH (aq), which exactly mimics the base behavior of
ammonia in equation (1). The “N standard” solution” simulates a solution that is 41μg N/mL.
3. Titrate the solution with the standardized acid solution provided. This solution is 2.000 mM
in H+(aq). The titration is complete when the solution returns to the original color of the boric
acid/indicator solution. It will be helpful to also monitor the titration by pH and note at what pH
range the solution starts to change color.
Part B. Titration of soil samples
1. Carefully remove the boric acid /indicator solution from the “Soil Sample A” cup. Note any
observations. Transfer the solution to a small beaker for titration.
2. Titrate the solution with 2.000 mM H+(aq) solution. Monitor the pH as you titrate. Be sure
to slow your titration when you approach the pH at which you expect the indicator to change
color.
3. Repeat the process for the boric acid /indicator solution from the “Soil Sample B” cup.
Part C. Control Experiments
1. Open the sample cup labeled “Control− No Soil”. Note the color of the boric acid/indicator
solution. If it has changed color in any way, titrate it with 2.000 mM H+(aq) solution.
2. Open the sample cup labeled “Control – Known Ammonia”. Carefully remove the boric acid
/indicator solution cup. Note any observations. Transfer the solution to a small beaker for
titration.
3. Titrate the solution with 2.000 mM H+(aq) solution. Monitor the pH as you titrate. Be sure
to slow your titration when you approach the pH at which you expect the indicator to change
color.
Part D. Mass% water in soil.
1. Remove your soil sample from the oven. Measure the mass of the dry soil + boat to three
decimal places.
2. Use this information along with the mass of wet soil + boat from last week to determine the
mass % of water in the soil sample.
You will write a full laboratory report on experiment 8. The report will be due one week after
completion of laboratory 8. Make sure you address the following in your lab report. Be sure to
turn in all data sheet before you leave the lab.
1. With is the mass% of water in your soil samples?
2. Without considering the results of your control experiments, what is the amount of N in
your soil samples in (μg N)/(g dry soil).
3. Does boric acid quantitatively trap all ammonia in your experiment?
4. Taking into account your control experiments, do you think your measure N content is
accurate? If not, can you use the results of your control experiments to correct your
measured nitrogen content? If so, what is the corrected nitrogen content of your soil
samples?
Laboratory #9 and #10
Titration of Phosphoric Acid and Determination of Phosphoric Acid Content in Coke™
Week 1: Laboratory #9 Titration of Phosphoric Acid
Review the titrations and Laboratory #4. Review Chapter 16 in your text book, lecture notes
and view the pre-lab video. Read the laboratory procedure (below). Write an objective
(paragraph form) and procedure (flowchart) for this lab.
1. Write a balanced equation for the reaction of KHP with sodium hydroxide. How will this
reaction allow you to determine the concentration of your NaOH (aq)?
2. What do you expect the pH of your phosphoric acid solution to be when you are half-way to
the first equivalence point?
3. Sketch a rough diagram of what you expect your titration curve to look like.
Part A. Preparation Hydroxide Solution.
1. Make up approximately 100 mL of 1 M NaOH by dissolving an appropriate amount of solid

NaOH in water in an Erlenmeyer flask. Keep the solid and the solution protected from air (by
covering the flask with Parafilm) as much as possible to minimize reaction of the NaOH with
atmospheric CO2. The concentration does not have to be accurate to high precision, since we
will standardize the solution to be used for the final titration in a later.
2. Titrate 100 mL of the unknown phosphoric acid solution with the ~1 M NaOH solution using a
drop of phenolphthalein as the indicator. Upon color change, this gives you the volume of 1 M
NaOH needed to reach the second equivalence point.
The phosphoric acid solution has a concentration similar to that in Coke™. Use the results of
your rough titration to determine the appropriate concentration of NaOH titrant such that 10 mL
of titrant will be required to reach the first equivalence point with 100 mL of phosphoric acid.
3. Dilute the stock (~1 M) NaOH solution to the desired concentration for the analysis. Make
200 mL of diluted solution to allow for multiple titrations. The required volume of NaOH will be
delivered from the buret. The volume of distilled water needed can be measured out using a
graduated cylinder. Store this in the plastic bottle provided. The exact concentration of NaOH
prepared will be determined by the standardization in part B.
Part B. Standardization of Sodium Hydroxide Solution.
NaOH titrant should be standardized against primary-standard potassium hydrogen phthalate

(KHP). Reaction of NaOH (aq) with atmospheric CO2 over several days can change its
concentration, so keep you solution sealed when not in use.
1. Weigh 0.2 to 0.3 g KHP to at least 3 significant figures. Dissolve the KHP in 50 to 75 mL of
distilled water. Add two drops of phenolphthalein.
2. Titrate with your diluted NaOH (aq) until the pink color of the indicator persists for 30
seconds.
3. Repeat the standardization one additional time.
Part C. Titration of Unknown Phosphoric Acid Solution
1. Deliver 100.0 mL of the unknown phosphoric acid solution into a beaker, using a 50 mL
volumetric pipet. The pH will be monitored using a pH probe attached to the computer. Open
Logger Pro and set up the pH probe as instructed.
2. Fill your buret with standardized NaOH (aq) solution. Titrant can be added in larger
increments (~ 1 mL) when not near an equivalence point (e.g. when the pH is not changing
rapidly), but should be added in small increments with frequent pH readings near the
equivalence points (e.g. when the pH is changing rapidly). Closeness to equivalence points can
be estimated by (1) steepness of the pH vs Volume curve (if plotted while titrating), (2) by
approaching a maximum in the derivative curve (ΔpH/ΔVolume vs Volume), or (3) estimated
from the earlier ”quick and dirty“ titration with approximately 1 M base. Alternatively, a fast
titration can be followed with a slower, more careful one.

You will write a full laboratory report on experiments 9 and 10. The report will be due one
week after completion of laboratory 10. Additionally, answer the following questions in your
laboratory notebook. Turn them in before leaving the laboratory. Turn in copies of all your data
before leaving the lab.
1. What was the concentration of your diluted NaOH(aq) solution in Part B?
2. What was the concentration of phosphoric acid determined in Part C?

Titration of Phosphoric Acid and Determination of Phosphoric Acid Content in Coke™
Week 2: Laboratory #10 Determination of Phosphoric Acid Content in Coke™
Review the titrations and Laboratory #4. Review Chapter 16 in your text book, lecture notes
and view the pre-lab video. Read the laboratory procedure (below). Write an objective
(paragraph form) and procedure (flowchart) for this lab.
1. Write balanced chemical reactions that depict reaching the first equivalence point of the
titration and the second equivalence point of the titration.
2. Why must you boil the Coke™?
3. Read Part B carefully. Design the 2 experiments described and write procedures for how
you will conduct the experiments. Additionally, state how you will interpret the results of your
control experiments to answer the 2 questions posed in Part B.
Part A. Titration of Coke™
1. Pour about 125mL of Coca-Cola™ into a pre-weighed beaker, record the mass, and then
calculate the grams of Coke™ added.
2. Bring the Coke™ to a gentle boil for at least 15 minutes to remove the dissolved carbon
dioxide. Allow the Coke™ to cool. Measure the mass and total volume of degassed Coke™.
3. Add 100 mL of degassed and cooled Coke™ to a beaker for titration. Add a stirring bar and
pH meter electrode. Stir the Coke™ on an automatic stirrer, being careful not to damage the
electrode with the stir-bar.
4. Titrate the solution with your standardized, diluted NaOH(aq) solution. The titration should
be continued until you are past the second equivalence point (however the third proton on
H3PO4 is too weakly acidic to be titrated conveniently).
5. Note the volumes of titrant required to reach the first equivalence point and the second
equivalence point.
Part B. Control reactions
When a solution of a diprotic or polyprotic acid is titrated with base, the second equivalence
point should be reached at exactly twice the volume of titrant as the first. This is because the
strong base, NaOH, completely reacts with each acidic proton in turn, in equimolar amounts:
However, when trying the Coke™ titration you may find that the second equivalence point was
not at twice the volume as the first. This deviation from expected behavior could be due to
buffering or other interference with the titration, either caused by residual carbonate or other
ingredients in the Coke™. You are provided with a bottle of seltzer water (carbonated water
without Coke™ syrup). You are also provided with Coke™ syrup which has been diluted so that
the concentration of phosphoric acid is similar to that in Coca-Cola™. Design and carry out
experiments to test the following assumptions: (1) boiling is sufficient to remove all carbonic
acid present in Coke™ and (2) a delayed second equivalence point could be due to the
presence some other acidic ingredient in Coke™.

You will write a full laboratory report on experiments 9 and 10. The report will be due one
week after completion of laboratory 10. Additionally, answer the following questions in your
laboratory notebook. Turn them in before leaving the laboratory. Turn in copies of all your data
before leaving the lab.
1. Calculate the moles of phosphoric acid in the 100 mL sample of degassed Coke from the
first equivalence point and the concentration of your base.
2. From your answer to question 1, calculate the moles of phosphoric acid in the entire
sample. Then calculate the mass % of phosphoric acid in Coke™.
Electrochemistry and measurement of Faraday’s Constant.
Week 1: Effect of concentration and temperature on cell potential.
Review Chapters 17 and 18 in your text book, lecture notes and view the pre-lab video. Read
the laboratory procedure (below). Write an objective (paragraph form) and procedure
1. Write a balanced electrochemical equation for the reactions you will study in Parts A & B.
2. Write a balanced electrochemical equation for the reactions you will study in Part C.
3. How will you determine the enthalpy and entropy of reaction from your data in Part B?
Part A. Effect of Concentration on Cell Potential
1. Obtain a 12-well well plate. Fill two wells on the opposite ends with 1 M zinc sulfate solution.
Fill the adjacent wells with copper sulfate solutions of 1 M, 0.1 M, 0.01 M and 0.001 M.
2. Construct a makeshift salt bridge by wetting a strip of filter paper in a potassium nitrate
solution. Use this salt bridge to connect the zinc sulfate well to one of the copper sulfate wells.
3. Place a copper wire and zinc strip into the corresponding solutions and record the resulting
voltage.
4. Repeat for each combination of zinc/copper cell concentrations. Use a new salt bridge for
each copper sulfate solution.
Part B. Effect of Temperature on Standard Cell Potential
1. Setup an electrochemical cell by adding a small amount of 1M zinc sulfate solution to a test
tube. To a second test tube add a small amount of 1M copper sulfate.
2. Place the half cells inside a water bath in a large beaker. Use the large strips of zinc and
copper as your electrodes. Clamp the cell carefully and heat the bath on a hot plate to a
temperature of approximately 50°C.
3. Construct a salt bridge from a U-shaped test tube filled with electrolyte agar gel and
potassium nitrate soaked cotton. Insert the test salt bridge upside down into both solutions so
that it spans the two beakers. Record the cell potential and the temperature of the solutions.
4. Repeat at 2 additional temperatures. You may pool you data.

5. In your laboratory report you will make a plot of the dependence of the cell potential on the
temperature. Also, you will use a graphical analysis to estimate ΔH and ΔS of the reaction. Be
sure that you have all the necessary data.
Week 2: Electrolysis of acid solution and measurement of Faraday’s constant
Part C. Measurement of Faraday’s Constant
1. Obtain a DC source with an attached ammeter (this will supply the current needed to bring
about the electrolytic process).
2. In a 250 mL beaker, add 100 mL of distilled water and then 50 mL of 3 M sulfuric acid. Stir
the mixture well.
3. Completely fill a 50 mL buret with this solution. Invert it into the beaker holding it in place
with a buret clamp and stand.
4. Measure the mass of a clean, dry Cu strip. Insert the Cu strip (anode) into the beaker and
attach the other end to the positive terminal of the power source. Attach the Cu wire to the
negative terminal of the power source and the other uninsulated end into the inverted mouth of
the buret. Make sure that all the bare part of the wire is wholly inside the buret.
5. Record the initial reading of the buret. Turn on the power source to approximately 0.4 amps
and start the stop watch. Continue the electrolysis until 20 mL of hydrogen gas have been
collected. Note the time when electrolysis is stopped. Measure the volume of hydrogen
collected. Record the average current.
6. Remove the Cu strip. Rinse with distilled water. Dry well. Measure the mass.
7. Measure the height of water column in the buret above the solution in the beaker,
temperature of solution in the beaker, barometric pressure.
8. In your laboratory report you will use these measurements to calculate the pressure of
hydrogen gas and hence the moles of hydrogen gas collected. Be sure you have all the
information you need.
9. In your laboratory report, you will also the Faraday constant form the mass of Cu dissolved
and from the volume of hydrogen collected. Be sure you have all the information you need.
You will write a full laboratory report on this experiment. The report will be due one week after
completion of the laboratory. Be sure to include answers or discussions of the following in your
laboratory report. There are no additional questions to turn in at the end of this lab period.
1. Discuss the effect of concentration on cell potential.
2. Make a plot of the dependence of the cell potential on the temperature.
3. Use a graphical analysis to estimate ΔH and ΔS of the reaction. Be sure to
indicate how precise you think these numbers are.
4. How many moles of hydrogen gas were collected?
5. Calculate the Faraday constant from you experimental data obtained in Part C. Do this
twice, once using the moles of hydrogen produced, and once using the moles of Cu
dissolved.
6. Discuss any significant sources of error in your experiment.

General Chemistry Laboratory Equipment
The following list of equipment has been received and accepted undamaged and in working
order.
Print Name: Signature: _______________________ Date
1 laboratory apron 1 vial of blue litmus paper

1 pair gloves 2 magnetic stir bars, 1 large, 1 small
1 combination lock 1 buret reader card
1 grease pencil
1 beaker, 800 ml
1 plastic ruler (30cm, clear)
1 beaker, 600 ml
1 beaker, 400 ml 3 watch glasses (2 small, one large)
2 beakers, 250 ml
1 graduated cylinder 10 ml
2 beakers, 150 ml
2 beakers, 50 ml
1 beaker, 100 ml
1 rubber policeman
3 Erlenmeyer flasks, 250 ml
1 stirring rod
3 Erlenmeyer flasks, 125 ml
2 spatulas (large, small)
2 Erlenmeyer flask, 50 ml
1 test tube holder
1 buret funnel (small funnel) 1 forceps
1 glass funnel (large) 1 tongs
2 test tube brushes (large, small)
1 hot hand protector
1 test tube racks (metal)
2 utility clamps (1 large, 1 small)
3 medicine droppers
1 pipet bulb 1 well plate
1 vial of red litmus paper 1 wash bottle
Check-in/Checkout Rules
Check-in Procedures
1. Each student will be assigned a numbered drawer containing his laboratory equipment. A list of the
equipment that the drawer contains can be found on page vii of this pamphlet. Each student should
make sure that all of the equipment on the list is indeed in his drawer and that none of the glassware is
cracked or broken.
2. Each student will be given a combination lock with which to lock his drawer. If the drawer if left
unlocked after the laboratory period is completed, the student will be held responsible for any missing
equipment.
During the Semester

1. If additional equipment, not in the drawer, is required for a particular experiment, each student must
sign out for his equipment and return it clean and in working order at the conclusion of the laboratory
period. If such equipment is not returned, or is returned damaged, the student will be billed for its
cost.
2. The equipment in the drawer is for the assigned student’s use only and is not to be loaned to fellow
students.
3. All equipment removed from the drawer during the laboratory must be returned to the drawer at the
end of the day. Any equipment left out at the conclusion of the laboratory will be confiscated.
4. Students who enroll in one section of laboratory in the fall semester may not switch into another
laboratory section for the spring semester unless a program conflict is demonstrated.
5. At the end of the semester, students will be billed for all broken or missing equipment if their total
bill exceeds $15. The cost of not returning the combination lock is $16. If any glassware or
equipment is broken or lost during the semester, the stockroom supervisor will replace it and add its
cost to the student’s tab.
Check-out Procedures
1. All glassware must be returned clean. (Glassware should be washed with soap and water and any
labels must be removed.) If equipment is missing, its cost will be added to the student’s tab. Extra
equipment must be returned to the stockroom. One may not give any equipment to other students.
2. Once the student checks out, he can no longer work in the laboratory.
3. Students who complete both the fall and spring semesters of this course must check-out on check-out
day: the last lab day of the spring semester as indicated in the spring syllabus.
4. If a student attends both semesters and fails to check out on the specified check-out day, or if a
student drops the course in the middle of either semester, or if a the student only completes the fall
semester of the course, in all cases, he must check-out within 30 days of his last day of attendance in
laboratory.
If he fails to check-out within 30 days, he will be billed $50 for the necessary removal of his lock,
cleaning of equipment and restocking of his drawer. In addition, the student will be billed for any
missing or broken equipment. Failure to pay this bill will result in barred registration and transcript
service.
5. Any student who checks out on any day other than the specified check-out day must schedule a
check-out appointment in advance with Arkadiy by calling 960-5494.
-------------------------------------------------------------------------------------------------------------------------------
I have read the check-in/checkout rules listed above and agree to abide by them.
Print Name ______________________________
Signature _______________________________ Date _____________

Laboratory Safety Quiz
CHE 1047L: General Chemistry Lab
Name (Print): Section:
True False Open-toed shoes, sandals or “crocks” are acceptable footwear for the lab.
True False Backpacks, jackets and other items can be stored in the laboratory.
True False Long hair is acceptable in the lab if it is tied back.
True False You should never eat or drink in the laboratory.
It is okay to remove your goggles in the laboratory to defog them while

True False
performing an experiment.
True False Gloves must be worn whenever working with chemicals in the laboratory.
True False Always carry and transport chemicals with both hands
True False You may dispose of chemicals down the drain
True False Cracked or chipped glassware is a safety hazard
When heating a substance in a test tube, you should always point it away
True False
from yourself and others.
True False Use of your cell phone is permitted in the laboratory.
True False Contact lenses may be work in the lab
Hotplates, Bunsen burners and heating mantles may be used in the

True False
presence of flammable materials.
Spending on the experiment, it is okay to leave the lab without washing

True False
your hands.
On the below floor plan, indicate the location of the following items:
a. shower e. nearest exit from 15th floor
b. eyewash f. nearest fire extinguisher
c. first aid station g. fire blanket
d. nearest exit from laboratory h. telephone

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CHE 1047L

General Chemistry Lab

Dr. Allan Burger Dr. Jacopo Samson

2. Duplicate Laboratory Notebook. Recommended: Hayden-McNeil "Student Lab Notebook: 100

General Course Rules

1 Check-in, Safety Quiz, Excel Assignment

2 Lab 1: Introduction to Volumetric Glassware

3 Lab 2: Synthesis of Alum

4 Lab 3: Spectrophotometric Analysis of Aluminum in Alum

5 Lab 4: Thermometric and Potentiometric Titration of an Unknown Hydrochloric Acid

7 Lab 6: Kinetics of Decomposition of Crystal Violet Dye,

9 Lab 8: Determination of Nitrogen Content in Soil

20 January 21 Check-in 22 Check-in 24 Check-in

27 Check-in 28 Lab 1 29 Lab 1 31 Lab 1

3 February 4 Lab 2 5 Lab 2 7 Lab 2

10 Lab 2 11 Lab 3 12 Lab 3 14 Lab 3

17 Lab 3 18 Lab 4 19 Lab 4 21 Lab 4

24 Lab 4 25 Lab 5 26 Lab 5 28 Lab 5

3 March 4 Lab 6 5 Lab 6 7 Lab 6

10 Lab 6 11 Lab 7 12 Lab 7 14 Lab 7

17 Lab 7 18 Lab 8 19 Lab 8 21 Lab 8

24 Lab 8 25 Lab 9 26 Lab 9 28 Lab 9

31 Lab 9 1 April 2 Lab 10 4 Lab 10

7 Lab 10 8 Lab 11 9 Lab 11 11 NO LAB

28 Lab 11 29 Lab 12 30 Lab 12 2 May Lab 12

12 Lab 12 Report Due 13 14 16

Before the Experiment: Pre-Laboratory Assignments (10% of the final grade)

Title: Give the experiment an informative title.

During the Experiment

Formats for Tables and Graphs

Dye: Cresyl Violet Neptune Blue(Collected by Josh Levy)

Concentration (M) Absorbance (au) Concentration (M) Absorbance (au)

1.0 x10-6 8.72 x10-2 1.0 x10-6 1.37 x 10-1

Ben Goldblatt: Beer's Law Plot for Aqueous Solutions of

General (~15 pts)

2. Abstract (~5 pts)

3. Introduction (~20 pts)

4. Experimental Procedure (~15 pts)

5. Results and Discussion (~30-35 pts)

6. References (~5 pts)

7. Appendix (~5 pts)

1 Accessed August, 2013

Organic Chemistry Lab CHE1215L – Thursday Section

Figure 2: The Mel-Temp Apparatus. (Adapted from reference 3)

Results and Discussion

Experimental Corrected Literature

130.6–133.1 132.1–134.6 132–135

Pure trans-cinnamic acid4

130.3–132.8 131.8–134.3 132–135

1:4 mole urea:trans-cinnamic acid

3. LeFevre, J.W; “Measuring the Melting Points of Compounds and Mixtures” in

4. Sigma-Aldrich Database. Urea MSDS.

5. Sigma-Aldrich Database. trans-cinnamic MSDS.

During the Semester

Answer the following questions in your laboratory notebook:

II. Laboratory Procedure

Part A - Quantitative precision of TD glassware

1. Clean and dry your volumetric flask.

2. Measure the mass of the empty volumetric flask.

Density of Water in g/L at Various Temperatures and 1 atm.

Part B - Preparation of a solution from a solid and preparation of a solution by

III. Post Laboratory Questions

Answer the following questions in you laboratory notebook:

II. Laboratory Procedure