Chemistry 3410: Instrumental Methods of Analysis Lab Outline
Spring 2008
Time and Place: Wednesday 1:00 – 3:50pm, D770.
Instructor: Kris Fischer Office: E-830
Email: fiscke@uleth.ca
Office Hours: Whenever I am in my office and not too busy.
Phone ext: 2343
Overview:
As the title suggests, this course is about using instruments to analyze things in a systematic and scientifically sound
manner. We will be using a wide variety of instruments available in the Chemistry department instrument cluster, including
but not limited to Fluorescence, UV/Visible, Atomic Absorption and FT-IR spectroscopy, Gas Chromatography and
Electrochemical analysis.
This laboratory will also put some focus on scientific report writing. By the end of the semester, students will (hopefully!)
be able to produce a paper which would not seem too out of place in a scientific journal.
Instructional Materials:
A lab manual will be distributed in .pdf format. This gives several examples of experiments which can be carried out using
our instrumentation, although it is by no means an exhaustive list of what can be done. You are encouraged to research and
devise your own experiments, and carry them out with guidance from your supervisor.
Relevant material will be distributed by email, class website (if I manage to get it up-and-running), or by physical hand-out
prior to the lab period. Students are expected to have read and understood any materials distributed before coming to lab.
Pre-Lab Meetings:
The lab will be meeting periodically to discuss both past and future lab work performed by the students. This will be
mandatory, but informal. The exact timing will depend on everyone's schedule.
Laboratory Evaluation:
The lab counts as 30% of your final course grade. Students must pass the laboratory with a minimum of 15 out of 30 to pass
the course. All assignments are weighted equally, with each being 5 of 30. Lab reports will be graded in accordance with
guidelines set forth by the instructor.
Laboratory Reports:
Each student is required to hand in a typed formal report after the completion of each experiment, as detailed in the
schedule. Any relevant data collected must accompany the report, and if the experiment was completed with a partner, that
partner's name must be on the report. The grade of any late report will be reduced by 10% for each full day it is late.
Missed Labs:
As there is only one meeting per week, make-up labs will be nearly impossible. Any missed experiments will be given a
mark of zero unless you have a valid excuse, in which case the lab will be pro-rated. If you are sick, please don't come to the
lab and spread your illness; a doctor's note may be required, although I probably won't ask for one (at least for the first
time).
Safety Stuff:
All students are required to wear eye protection and lab coats while any lab work is being done. Closed-toed shoes and long
pants are also necessary in the lab. Any extra safety precautions will be specified by your instructor.
The Schedule:
Week 1: January 9th (today).
Instrument:
No labs on reading week
Week
Week
Week
4&5
6&7
8&9
Week
1
Week
2&3
Week
10&11
Week
12&13
Atomic Absorption
intro
A
E
D
C
B
***
Fluorescence
intro
B
A
E
D
C
***
FT-IR
intro
C
B
A
E
D
***
UV/Visible
intro
D
C
B
A
E
***
Gas Chromatography
intro
E
D
C
B
A
***
Electrochemistry***
***Time permitting, we will be having a one-lab electrochemistry demo.
How the lab will work:
Each group will have two weeks to perform an experiment analyzing something using the instruments detailed in the
schedule. You get to come up with your own experiments, using whatever resources you can find. I will be providing
“expert advice” as needed. There will be a few limitations on what chemicals can be used, depending on our current stock,
and price and availability of any required chemicals – be sure to check with me to see if we have the chemicals you need!
Some Helpful Information to Get You Started
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Get yourself a lab notebook (I have a bunch in my office that you can have for free if you need one), and keep
detailed notes before, during and after any experiment you perform.
Check the Journal of Chemical Education. There is a lot of useful information there.
Find some information about the capabilities and limitations of the instrument you are using.
Make sure your sample actually contains (or has a reasonable possibility of containing) the analyte in question.
Check your textbook for any advice on interpreting data, handling experimental error and statistical analysis, as
well as sample preparation. Chapters 1-5 and chapter 28 of your textbook are particularly relevant.
Come see me in my office a week or so ahead of the lab to go over your experiment with me.
Fischer's Basic Lab Report Ingredients
In order to get full marks for a report, it must include some form of each of the following. Some of these sections will be
quite long; others need only be only a sentence or two. Some sections can even be combined into one.
Abstract: This summarizes the report, usually in 200 words or less, to allow readers to determine whether or not they want
to read the whole report. An abstract must, at the very least, state the purpose of the experiment, any key results, and any
major points of discussion or conclusions. In addition, an abstract may or may not include a brief discussion of important
methods & theories behind the report.
Introduction: Prepares the reader for the rest of the report. It should include the purpose of the experiment (in more detail
than the abstract), as well as any necessary background, such as previously published work or experiments. “Background”
in this case may refer to any equipment used (particularly if the equipment is specialized or unique), and also a justification
of the experiment's importance.
Methods & Materials: This is a brief description of the materials and/or methods used in the experiment. Exact types &
model numbers of equipment, experiment parameters, software, types of glassware, solvents, and reagents (including
suppliers) would all be appropriate for materials, while methods should cover the theory and practice behind the use of
materials.
Procedure: The procedure allows another chemist to retrace your steps and repeat your experiment. It should contain
enough detail that anyone with basic knowledge of chemistry can achieve the same results presented in the paper. A
procedure does NOT need to give every minute detail; for example, a solvent extraction only needs to state “A was
extracted from B with solvent C”, and NOT “X amount of A dissolved in B was added to a separatory funnel containing
solvent C, the mixture was shaken, vented and C was isolated using the tap at the bottom of the funnel”. ANY competent
chemist should know how to perform an extraction, just as he or she should be able to make up NMR samples, put samples
on salt plates, make KBr pellets, and so on...
Results: These are usually best depicted by graphics (charts, graphs, chemical structures, etc). Graphics must be labeled &
titled clearly and consistently. They may of course be elaborated upon using words.
Discussion: Often intertwined with results (as in the “Results & Discussion” section seen in many scientific journals), the
discussion should allow a reader to follow the reasoning behind a set of results. It should analyze those results, and make
rational & logical deductions from that analysis.
For the purposes of this course, your results & discussions should explain to me in plain English what reasoning was used to
obtain your results.
Conclusion: This states what is known as a result of an experiment, and a justification for why it is known. It may also state
the significance of the results, and may suggest further avenues of research for the future.
References: References give the reader somewhere to go for more information on a subject. Any important topic which is
not novel (ie, you did not invent it) and not common knowledge (like the fact that water consists of two hydrogen atoms and
one oxygen atom) should be given a reference. For this course, no more than 50% of your references may be electronic, and
you should have more than two references per paper (as an example, your textbook and an electronic spectrum database
from the Internet could be two commonly used references).
Appendices: Anything else which is important, but does not warrant discussion in any of the previous sections, should go
into an appendix. This must include original spectra, and may include sample calculations or anything else you may want to
bring to my attention.
Some Guidelines for Writing
Write in the Past Tense, and Avoid Using the First Person: Scientific writing focuses on events which have already
happened, data which has already been collected, and results which have already been determined. As such, reports are to be
written “X was determined from Y”, rather than “I determined X using Y”. This emphasizes the importance of the
information being presented, rather than the person presenting the information.
Be Concise: The record for longest report I have ever marked is currently set at no less than 37 pages, not counting spectra
and appendices. While the information presented in that report was accurate and well presented, it was also massive overkill
compared to what could have been written. Remember that you have other courses to study for, and do not write too much.
Your reports should contain facts, results and supporting information, no more and no less.
Read Other Papers: Go to the U of L library website, and find the on-line journal articles. Read a few of the American
Chemical Society (ACS) or Royal Chemical Society (RCS) journal entries, and use those as a guideline when writing your
papers. There is more information at your fingertips now than at any other time in human history; it would be foolish not to
make use of it!
Be Precise; Avoid Ambiguity: Make sure that anything written in a lab report is free from any possible ambiguities. For
example “A minus B plus C” could refer to just A, or it could be A and C. Likewise, the phrase “protection from cancer by
antioxidants” is imprecise, as it does not state whether cancer is being caused by antioxidants, or whether the antioxidants
are protecting from cancer.
Use English: This may sound silly, but your reports should make proper use of the English language. This includes
spelling, grammar, and all that stuff you learned in grade school and wish you could forget. An author will not be taken
seriously if he or she cannot write. Your reports do not need to be the equal of Shakespeare, but should be in correct English
nonetheless.
How I Mark Papers
The “A” Paper – Perfection:
 The Paper is written perfectly. All of the necessary references are there, there are no errors in grammar or spelling
(the occasional error is fine – everybody's fingers slip on the keyboard at some time). Everything makes sense.
 The Experiment is well thought-out, well-researched, and neither too ambitious nor too simple. The experiment
makes proper use of the equipment at hand.
 Interpretation of data is correct.
The “B” Paper – Pretty Darn Good:
 The Paper is written well. There may be a few minor errors here and there, but nothing serious.
 The Experiment is good. Still well planned, but maybe a little too ambitious or simple. The experiment still makes
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proper use of the equipment.
Interpretation is correct, although it may be a lacking in some way – making an incorrect assumption or two, or
perhaps missing some key point.
The “C” Paper – Average:
 This is your average paper. Some mistakes are expected, as are some errors in grammar or spelling. While the
paper makes sense, there is nothing particularly good nor bad about it. It is an average paper.
 The experiment may or may not have worked, but at least it was a good idea. The equipment was properly used,
but may have been lacking in some way or another.
 Interpretation may or may not be correct, but is at least mostly logical and makes sense.
The “D” Paper – Not So Good:
 A below-average paper. Quite a few mistakes, or maybe not enough information. Lots of things written do not
make any sense.
 The experiment had some major flaws in it – either not well-researched, not executed correctly, too simple or too
complex for a two-week experiment. In general, the experiment was probably not a good idea in the first place.
 Interpretation has some major flaws in it.
The “F” Paper – Complete Failure (I have yet to give one of these out in chem 3410):
 The paper was not written in the first place, or not even written in English. You would have to work really hard (or
not work at all) to make this happen.
 The experiment was something which would never work in the first place, and didn't.
 Interpretation is nonexistent or completely incorrect.