Chemistry 5710 Instrumental Methods of Analysis - Syllabus
Professor Ralph Allen
OBJECTIVES:
The following outlines general objectives of this course:
1. As a result of Chem 5710 students should be able to define a problem where the
determination and/or measurement of some chemical species is required. There
are a long series of questions which must be answered about the desired results
before one can address the question of what instrumental technique should be
utilized.
2. Students should develop sufficient knowledge about the major instrumental
methods of chemical analysis so that they can determine what technique should be
used to solve a particular problem. The knowledge base includes:
A. the chemical and/or physical basis of the measurement (e.g. what is used
to stimulate the sample, how does the sample interact with the stimulus,
how is the interaction detected)
B. the type of information that can be obtained from the measurement
C. the limitation and/or requirements of the method
D. the advances in instrumentation which have been made, especially those
made as a result of problems encountered with the method.
3. The student should be able to address the problems of analyzing complex
samples. This would include defining the problem, determining any constraints,
choosing the best methodology, and determining how to test the methodology to
prove its merits. Where there are alternatives the student should be able to define
the advantages and disadvantages of each.
4. The class will be divided into groups of about four and most of the assignments
will be performed by the group. This exercise in cooperative learning should help
students develop skills in working as a team.
5. To give a better opportunity for the students to understand all aspects of providing
analytical results, a semester long project will focus on the requirements for a
developing and testing methodologies and/or procedures for the rapid analysis of
threat substance in the field, and in the laboratory. This will include the
background necessary for a scientific expert witness to present new techniques in
a court of law.
INSTRUCTOR:
Professor Ralph Allen
Room 234 Chemistry
Phone: 982-4922 or 531-4250
Office Hours: WF 1-2 PM
Other times by appointment
TEXTBOOK:
There is no official textbook but any modern Instrumental Analysis text like Instrumental
Methods of Analysis, 7th ed, Willard, Merritt, Dean, Settle, will be of value as a
reference. You will need an iClicker for this class, you must register you iClicker. You
can purchase one at the bookstore. To register your iClicker click on this link
http://www.iclicker.com/registration/
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Enter your first and last name in the supplied boxes.
Enter your UVA Email ID (e.g. roa2s) in the box labeled “Student ID”
Enter the number on the back of your iClicker unit in the box labeled
“Clicker ID”
GRADING:
Group Presentations 40%
Final Exam 20%
Group Project 30%
Participation 10%
GROUP PROJECT:
Any analytical approach requires that the problem be defined before making decisions
about what type of instrumentation to utilize. The class will be divided into teams that
will work together to define an analytical problem and develop a proposal for the
analysis. The focus will be forensic (especially substances that could be utilized in a
terrorist attack) or environmental or related to an industrial need. The projects may
involve looking at rapid field analysis or accurate laboratory analysis. There will be oral
and written presentations as well as periodic progress reports.
The use of instrumental methods of analysis on evidentiary material from a crime scene
means that the results will be presented in a court of law. Generally a scientist does not
understand the requirements placed on the expert witness (scientist) and the methodology
that generated the results which will be presented (testimony). To give you an example
of the “analytical approach” the various groups will consider some aspect of the
preparation that a scientific expert might have to prepare for and present in a court of law
or before a judge in a “Daubert hearing.” Each group will choose one of the following
aspects and prepare what they believe would be testimony to present to a judge. The idea
is to give a lawyer enough factual information to explain the process or procedure. You
will then be asked the types of questions that you would likely be asked by a judge (or
opposing lawyer). You may need to go back and get new information to support your
claims and add this to you written testimony. Depending upon the time available, some
groups will appear in a mock courtroom setting before a “judge” to answer questions
posed by the court.
1. Use of fluorescence to do “presumptive tests” to identify blood or other body
fluids.
2. Use of “presumptive tests” for anthrax or cocaine
3. The collection, preservation, and control of blood evidence being used for DNA
testing
4. The use of capillary electrophoresis with laser fluorescence detection for nuclear
DNA (Y chromosome only or multiple chromosome)
5. The use of sequencing for the analysis of mitochondrial DNA
6. Laboratory analysis to confirm anthrax or cocaine
7. Detection in the field and confirmation in the laboratory of flammable accelerants
or explosives
8. Detection of illegal drugs or steroids in athletes
9. Detection of pollutants or illegal dumping
10. Fiber analysis
GROUP PRESENTATIONS:
In an effort to be sure that each person is developing an understanding of a technique or
the analytical approach, each group is expected to meet regularly to discuss and prepare
for specific topics which they will be expected to present in class. These topics are
specified below and will be used to supplement presentations made by the instructor. It is
expected that there will be class discussions on the topics so even the groups not actually
making presentations are expected to have investigated the topic and thus be able to
contribute to the discussions. There will be questions asked as a part of the presentation
and you will use iClickers to respond. The iClicker response will also be used to take
attendance. In the following schedule some of the specific topics that will be assigned
are numbered sequentially for reference. PowerPoint presentations on some of these
topics are available on the class web site
(http://ehs.virginia.edu/ralphs_chemistry_courses/5710/).
You will be expected to attend classes and attendance will be recorded using your
iClickers. You will be allowed no more than 3 (three) absences during the semester.
You may be sick or on an interview or whatever reason but if you are absent for more
than 3 class sessions you will have to write a 3 page paper for each class you miss
(beyond the 3).
TENTATIVE SCHEDULE:
I.
Understanding the problem: the analytical approach
A.
knowing the questions to ask and recognizing connections
B.
recognizing strengths and weaknesses of the technique (what results are
expected and where are the errors)
C.
knowing statistics is essential for interpretation (detection limits,
signal/noise)
D.
general philosophy in instrument design
E.
special problems with analysis within the criminal justice system
F.
G.
II.
issues of quality assurance and quality control
special problems for portable instrumentation and rapid detection
Molecular spectroscopy
A.
what are the samples and what results are expected
B.
infrared spectroscopy - most qualitative
1.
what are the interactions with molecules
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absorption
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scattering
2.
means of excitation (light sources)
3.
separation of spectrum (wavelength dispersion, time resolution)
4.
detection of the signal (heat, differential detection)
5.
interpretation of spectrum (qualitative, mixtures, resolution)
6.
advantages of Fourier Transform (FTIR)
C.
UV-Visible - more qualitative.
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emission
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absorption
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fluorescence
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photoacoustic
7. excitation sources (lasers, time resolution)
8. wavelength dispersion (gratings, prisms, interference filters, laser,
placement of sample relative to dispersion, resolution)
9. detection of signal (photocells, photomultipliers, diode arrays,
sensitivity and S/N)
10. interpretation (quantification, mixtures, absorption vs. fluorescence
and the use of time, photoacoustic, fluorescent tags)
III.
Separation techniques
A.
Chromatography
B.
C.
11. gas chromatography, liquid chromatography, supercritical fluids
12. importance of column technology (packing, capillaries)
13. separation based on increasing number of factors (volatility,
solubility, interactions with stationary phase, size, electrical field)
14. detection: simple vs. specific (gas and liquid)
15. detection as a means of further analysis (use of tags and coupling
to IR and MS)
16. electrophoresis (plates and capillary) and use with DNA analysis
Immunoassays and DNA techniques
mass spectroscopy
17. making the gaseous molecule into an ion (electron impact,
chemical ionization)
18. making liquids and solids into ions (electrospray, electrical
discharge, laser desorption, fast atom bombardment)
19. separation of ions on basis of mass to charge ratio
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magnetic
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time of flight
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electric quadrupole
20. resolution, time and multiple separations
21. detection and interpretation (how this is linked to excitation)
IV.
Elemental analysis
A.
mass spectrometry (electrical discharges)
B.
atomic spectroscopy
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atomic absorption
atomic emission
atomic fluorescence
22. excitation and getting sample into gas phase (flames, electrical
discharges, plasmas)
23. wavelength separation and resolution (dependence on technique)
24. detection of radiation (simultaneous/scanning, signal noise)
25. interpretation (errors due to molecular and ionic species, matrix
effects, other interferences)
C.
X-ray analysis and electron spectroscopy (surface analysis)