Laboratory Syllabus -

Chemistry 421 - Instrumental Analysis

Spring 2007

Prof. Scott Shippy

5417 SES
5-2426
[email protected]

MW Lab T.A.: Kongthong Thongkhao-on

Office: 4323 SES
Office Phone: 3-5082
email: [email protected]

TR Lab T.A.: Miao-Jen Lu

Office: 4323 SES
Office Phone: 3-5082
email: [email protected]
Chem 421

General 1/11/077
The lab portion of Chemistry 421 consists of a rotation session in which there are 7 labs, for
which students are paired into groups of two. Each experiment must be completed in the four lab
periods allotted for each rotation.
Pre-Lab Preparation
Students will unfortunately have to perform many experiments before the related information is
covered in the lecture. Pre-lab preparation, therefore, is very important. Before each lab,
one should read the textbook sections dealing with the relevant instrumentation and theory. Of
course, before each lab, one must also read the experiment he or she will perform and decide
how to use the time in the lab. If the TA determines that students from a particular group are not
prepared for the experiment, they will be asked to leave the lab until such preparation can be
completed. The TA is the final arbiter in this matter.

Lab Report Due Dates

Lab reports are due by the beginning of the lab period one week after your last scheduled
rotation day. Late lab reports will be subject to a 10-point deduction for each day that they are
late. Furthermore, all labs must be turned in by the last day of classes (May 4 at 4:00 pm), or
you will not receive a passing grade in the course. There will be no exceptions to this late
policy.

Grading Laboratory Portion of Course

The lab portion of the course is worth 50% of the final grade. The maximum possible scores are
distributed as follows:
7 experiments @ 100 pts/each
Evaluation of notebook @ 100 pts
Instrumentation Intro @ 100 pts
TA evaluation @ 100 pts
Total 1000 pts.
The TA evaluation is an overall rating including general preparedness, lab technique, and a
bound lab notebook evaluation. Notebooks will be collected for evaluation. Notably, these
should be an accurate reflection of your time spent in the laboratory. Please see comments below
on the proper use of a notebook.

General Rules for Laboratory Work and Behavior

You must provide and wear safety goggles at all times while in the lab. This is state law and
there are no exceptions.
Notify the T.A. immediately about problems with equipment and about shortages of any
materials relevant to your experiment. Many items used by this class must be ordered. Running
out of these supplies may cause experiments to be unavailable for up to 1 week. Also, you must
check out with the T.A. before going to the next experiment.

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Do not store solutions overnight in volumetric flasks. They are in short supply and may be
needed by another section. Solutions stored in volumetric flasks may be thrown out without
warning by the next section.
You must clean the balance area after use. Five technique points will be deducted if you fail to
use the balance carefully and keep the area clean. Return all other chemicals to proper shelves at
the end of each day.
All glassware must be washed at the end of each class. It may be then left on the drying racks to
dry. It is the responsibility of each section to put away all dry glassware to their proper storage
areas at the beginning of each class. You should never leave dirty glassware by the sinks. If you
find any please wash it and place on the rack.
Never eat, drink, or bring food into the lab. Once samples are brought into the lab they are
considered chemicals and will be treated accordingly.
If friends are waiting for you to complete an experiment, please insist that they wait outside the
lab.

The Lab Notebook

Scientists keep careful records of their experiments. This includes observations, data, and
comments on what worked and what didn't work. For this course, you must purchase and use a
bound laboratory notebook (i.e., a composition book) and organize it in such a way that anyone
could easily follow your progress through the assigned experiments. Your lab notebook should
contain:
1. A Table of Contents.
2. Numbered pages.
3. No torn out pages. Instead, neatly cross out any unwanted pages.
4. Write on and number only the right facing page, keeping the back facing page blank for
scratch work.
5. Draw a single line through mistakes or changes in the notebook. All writing should be
clearly legible. The use of white-out or similar is never acceptable.
6. Correct English grammar and spelling throughout.
7. Final analysis of your data, clearly written in blue or black ink.
8. All plots and other computer-generated material neatly glued, taped, or stapled into the
notebook. All fitting of data to straight lines must be done by linear least squares
analysis, with the correlation quoted.
Each student maintains their own lab notebook. These notebooks are reviewed at the end of the
semester. This should be an accurate reflection of what actually happened over the course of the
semester.
Your TA must sign your data pages on the day the data is recorded.

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Guidelines for The Laboratory Report*

• Each student hands must hand in their own lab report for every experiment,
although you are encouraged to work together on these reports.
• Lab Reports are due for only the seven rotation labs (see schedule).

A. Format
One of the aims of this course is to develop the student's ability to formally communicate
scientific information. Students are, therefore, required to present their reports for each
experiment in the form outlined below. Each section's points are approximate and will vary.
1. Abstract (5 points). An abstract is a summary of the salient points that are presented in the
report. Included in the abstract should be the objectives of the experiment, the type of
instrumentation used, and all of the final numerical results with associated errors. Proper
abstract format must be followed.
2. Introduction (10 points). This section briefly introduces the instrumental technique being
used. Included here should be the characteristics of the instrumentation and comparisons with
other techniques for similar determinations.
3. Theory (10 points). Any relevant theories and principles underlying the measurements in the
experiment are presented in this section. An example would be a discussion of the chemical and
physical processes occurring in a flame during an atomic absorption experiment. Important
equations should be explained. This section should be kept short and concise - it should never
exceed 3/4 page in length. There is no need to write a treatise on the subject here or elsewhere in
the report.
4. Experimental (10 points). This should be a brief summary of the procedures used in the
experiment. For example, the model of the instrument, the wavelengths used for a
determination, the concentrations of solutions, and any deviations from the normal procedures
should be included. A carefully hand drawn block diagram of the instrument indicating the basic
components and their function should be presented. There is no need to repeat material already
included in the handouts.
5. Data and Calculations (20 points). This section should contain all the collected data
presented in tabular form, samples of the calculations used in the data workup including
statistical treatment, and all graphs. This section should be clear and organized so the reader can
understand what was done to the data. The original recordings, not copies, should be included
either in the body of the report or as an appendix. All spectra should be completely filed out.

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6. Results and Discussion (25 points). All results, including unknown values, are presented
here in a neat, clearly labeled, tabular form. All numerical results must be accompanied by their
statistical error. This is accompanied by a discussion of the results as well as a discussion of the
various aspects of the instrumental method studied. This will include qualitative and quantitative
comparisons when appropriate, discussions of the sources of error, any chemical, physical, or
instrumental limitations imposed on the analysis, and reasons for deviation from ideality.
Experimental errors such as errors in dilution, weighing chemicals, etc. should not be discussed
qualitatively, but quantitatively. Do not explain away results that deviate from the expected
behavior by stating "I might have made mistakes during the experiment."
7. Questions (15 points). Where applicable, assigned questions associated with the lab should
be answered. Always state the question that you are answering. Note that questions similar to
these will be on the final exam.
8. References (5 points). A bibliography referencing all literature sources used in writing the
report should be presented. In the past, there have been problems associated with students not
adequately referencing sources used in writing their reports. The importance of proper
referencing in scientific reports cannot be overstated. In your reports, the format defined by the
examples given below should be followed.
1. C.I. Miles and G.H. Schenk, Anal. Chem., 42 (1970) 656.
2. J.W. Robinson in “Treatise on Analytical Chemistry”, P.J. Elving, E.J. Meehan, and I.M.
Kolthoff, eds., 2nd ed. Part 1, Vol 7, Interscience, New York, 1981.
3. D.A. Skoog and D.M. West, “Principles of Instrumental Analysis”, 2nd ed., Saunders,
Philadelphia, 1980, Ch. 11.
4. T.S. Bixley (1995), Sentient Microfilaments Home Page. Available:
http://www.microfilaments.com/consciousness/synchronicity/quantum.html.
Be sure to use the correct abbreviations for journal names.

B. Presentation of the Lab Report

The laboratory report must be written on a word processor. It should be submitted as both
hardcopy and electronically via e-mail to [email protected] or with an appropriate transportable
medium. It should have a cover sheet following the format shown on the following page.
Preparation of graphs and tables should use the following guidelines:
1. Graphs and tables must be produced by a spreadsheet, plotting program or equivalent
software. The instructor and TA are not responsible for showing you how to use your
plotting or word processor software.
2. Graphs should follow these guidelines.
a) Graphs should be labeled so that the experiment and the relationships plotted are clear.
b) Choose a scale for each axis so that the plot fills the graph. It is only necessary to have
the plot pass through zero if this is a condition of the experiment.
c) Label each axis and include units (e.g., temperature (EC) or time (min.)).
d) Plot the independent variable on the x-axis and the dependent variable on the y-axis.
e) Each curve on the graph should be plotted in a different color, line style, or symbol.
Include a legend for the graph that explains the symbols used.
f) The points should be plotted with error bars.

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g) Do not connect the 'dots' on your graph unless such a continuous curve is justified. If a
series of points is presumed to fall on a straight line, then a least squares analysis should
be performed, and the correlation should be reported.
3. In the rare instances that chart recordings or printouts cannot be imported into your
document, they should be neatly cut out and taped onto a blank space in your lab report 8.5"
x 11" sheets of paper. Each recording should have a title with axes and all variables clearly
indicated. This includes sensitivity, chart speed, name of experimenter, and the designation
of the experiment.
4. Data and results should be presented in tables with appropriate headings including units.

C. Grading Lab Reports for Quality of Written English

The TA will grade most lab reports. However, the instructor may additionally grade your lab
reports for the quality of your written English. This will allow you to improve your written
English, which is critical to the success of any scientist.

D. Plagiarism
Plagiarism is against UIC's academic policy and will not be tolerated. A general definition of
plagiarism is the appropriation of passages, either word for word or in substance, from the
writing of another and the incorporation of those passages as one’s own in written work offered
for credit. This includes direct quotation of whole sections of textbooks or web pages and
copying of lab reports of other students. Downloading prewritten lab reports from the internet
(either for free or purchased) is plagiarism. Note that the TAs have a CD Rom containing old lab
reports from students who previously enrolled in Chem 421.

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SAMPLE COVER SHEET FOR LAB REPORTS

CHEMISTRY 421

TITLE OF EXPERIMENT

STUDENT’S NAME

TA’S NAME
DATES OF PERFORMANCE OF EXPERIMENT
DATE OF SUBMISSION OF REPORT
DUE DATE OF REPORT
NAME OF LAB PARTNER