ADVANCED ANALYTICAL CHEMISTRY Mike Ross Spring 1999 ASC-155
CHEM 336 5482
Wisdom is seeing the pattern which connects one to another.
We will spend this semester trying to see the patterns which connect instrumental analytical techniques together. There are four ways we will do that this semester.
* Introduce and name the essential parts of some new or
widely accepted chemical instruments that are in
routine use in research or production laboratories.
* Illustrate selected ways of applying sets of physical
principles to form an instrumental method of analysis.
* Highlight areas within instrumental methods where
greatest chance for error occurs.
* Present conventional uses of instrumental methods in
research and production applications.
We will study these through;
~ Discussions covering techniques and illustrating above.
~ Skoog/Holler/Nieman's text covering most modern methods of instrumental analysis will parallel and supplement the discussions.
~ Discussion problems to emphasize specific areas of each
technique.
~ Outside Readings: -- to fill in the missing pieces of background relative to discussion material.
Learning is an active process which is accomplished by a variety of different methods. The discussion, laboratory, problem sets, outside readings and formal evaluations are methods to provide a variety of approaches for learning. These provide only the framework, the learner must provide the time and effort.
A series of discussion problem sets containing questions selected from the chapter or other sources will allow you to gain a better understanding of the topics covered. It is felt that if taken seriously, these problems can provide learning by focusing your attention on specific topics. These problems will be used as the catalyst for our discussions.
Evaluation always seems to be required in these kinds of courses. The formal evaluations will take on four different forms:
1) Six, 30-minute problem-solving quizzes related to the discussion and reading materials (maximum of two problems on each quiz). These will be given at the beginning of Day 4, even cycles.
2) Seventeen homework sets collected as specified in the attached schedule.
3) An oral presentation on an instrumental technique of the student's choice. The topic must be approved by Dr. Ross. The presentations will be given during the final exam period to a panel of faculty and interested students.
There are reading assignments associated with each discussion topic. The major assignment is the "textbook", which this semester is Skoog/Holler/Nieman "Principles of Instrumental Analysis, 5th Edition". This material is at just about the same level that the discussion will be conducted, and provides a good indication of the performance level expected by the profession of a bachelor chemist operating in industry in the first year out of school. Clearly, it is a good idea to read these assignments to help with all of the aspects of the course, in addition to sensing this professional level of understanding.
However, there is another reading assignment that requires more professional interest with which to become involved. The primary purpose of these readings is to give each person a way of testing their mastery of the material presented in the course as they move sequentially through it. The articles are taken from several trade magazines and journals, (especially the A - pages of the Journal of Analytical Chemistry) and represent just the kind of reading that crosses a professional's desk on a pretty routine basis. The idea is to stay up on the developments in the field, which, of course, presupposes a general background understanding of the material comprising the field. If, after reading the appropriate text assignment, doing the assigned problem set, attending the discussion, you were to find that you could not comfortably read these articles, flaws in your understanding of the basics of the material should be suspected.
Grading
Methods for learning are designed to encourage you to teach others to enhance your own understanding. The class may move ahead in proportion to the rate at which each person can help others understand the material. This approach has been called non-competitive, although in fact it simply acknowledges that we almost invariably learn at a more meaningful level if we plan on teaching what we wish to know as we work to learn it. Since it is hard to picture teaching an adversary, it follows that we can avoid the competitive effect of having our own advancement dependent upon another's retardation if we simply agree to exchange "student" roles during the semester.
This approach raises the question of how grades can be assigned, if one person cannot succeed at another's expense. The answer lies in the rejection of the class average; and by working toward a point total. Effectively being able to preselect the grade you want for the course.
Grading Point Breakdown:
6 Quizzes 500
(@100 points each, 5 graded)
Final Exam 500
17 Problem Sets 500
(@30 points each)
4 Experiments 400
(@100 points each)
2 Laboratory Write-ups 300
(@150 points each)
Group Designed Experiments 200
Laboratory Handout for Designed Expt. 100
Total 2500
Letter Grade Assigned:
Total Points Letter Grade
2160 A
1920 B These are guaranteed maximum cut-off levels.
1680 C
1440 D
Laboratory
Learning can be accomplished in several ways, but the most effective method is a method which is as concrete as possible. For this reason, the laboratory experience becomes a very important part of our learning process.
Experiments:
The laboratory experiments are of three types. You will start with an experiment in potentiometry. You are to do this experiment on your own and should be completed within the first two cycles. You will also be assigned a lab group to begin the design of an experiment for the rest of the groups to conduct. This experimental design and testing will be completed by the beginning of Cycle 5. At that time, all experiments will be ready to run. These experiments will be run in a round-robin with each group having two cycle to complete each of the remaining experiments. Each lab will have a single page report to be completed by each student group, following the pattern of the first semester of analytical chemistry. In addition, formal lab write-ups similar to the write-ups of first semester will be expected from each student (see below). Lab will be open all six days of the cycle but instructional "staff" will be available only Days 2,3,4 and 5.
Possible Experimental Techniques:
1 Electrochemistry
2 Gas Chromatography
3 HPLC
4 GC/MS
During the first two cycles, you and your lab partner should get together with Dr. Ross and decide the kind of experiment you will develop. You will then have three cycles to develop the experiment and produce an experimental hand-out.
Formal Lab Write-Ups
Formal lab write-ups are required. Everyone is expected to write-up the potentiometry experiment. For the other individual student write-up, the student has a choice as to which laboratory experiment will be the focus for their write-up. The write-up is your choice. These write-ups are to take on the general format of a scientific paper written for "Analytical Chemistry" (manuscript requirements given in each January issue). Expected length of these write-ups are 3-5 typed pages, therefore you must be concise in what is presented. Focus your attention on the results and discussion section, answering any questions posed in the experimental hand-out. The two write-ups require that you submit a rough draft and final draft. The rough draft is not an initial draft, but a draft you feel is ready for publication. It is to be typed (double spaced) and resubmitted with the final draft. All final drafts must be typed. It is expected that you will draw from sources other than your text in writing this paper, therefore be sure to include references and citations.
Each lab group is to submit an experimental procedure similar to the procedures given out during first semester. This procedure will be duplicated and given to all other lab groups. In addition one write-up for the experiment you developed must be submitted by the group. This write-up should represent the work the group did on the experiment therefore should include successes and failures and an explaination for the failures.
ALL DATES ARE ABSOLUTE: Write-ups will not be accepted after these dates.
Potentiometry Experiment - Write-up Rough Draft: Due Feb 22
Final Draft Mar 5
Experimental Procedure
Due March 16
Group Developed Experiment -Write-up Rough Draft:
Due Mar 24
Final Draft Apr 9
Last Formal Report Due at time of Final Presentation
TENTATIVE SCHEDULE
CH 336 Spring 1999
| Cycle | Day | Date | Topic | Assignment |
| 1 | 2 | 2/2 | Introduction | Chapter 1; Problems: Chapt 1 1-11 |
| 1
2 3 |
4
6 2 4 6 2 |
2/4
2/8 2/10 2/12 2/16 2/18 |
Electronic Principles
Analog Components Digital Gates/Microprocessors Noise |
Chapter 2; Problems: Chapt 2 -even
Chapter 3; Problems: Chapt 3-odd Chapter 4; Problems: Chapt 4-even Chapter 5; Problems: Chapt 5-odd |
| 3
4 |
4
6 2 4 6 |
2/22
2/24 2/26 3/2 3/4 |
ElectroAnalytical Chemistry
Potentiometers Titrations Reference Electrodes ISE |
Chapters 22; Problems: Chapt 22-odd
Chapter 23; Problems: Chapt 23- odd |
| 5
|
2
4 6 |
3/9
3/11 3/15 |
Electrolysis
Mass transport Current-Voltage curves Polarization Electrolytic Methods Coulometry |
Chapter 24; Problems: Chapt 24-odd |
| 6
7
|
2
4 6 2 |
3/17
3/19 3/23 3/25
|
Voltammetry
Quantitation Polarography Pulse Techniques Standard Addition |
Chapter 25; Problems: Chapt 25-even |
|
Cycle |
Day | Date | Topic | Assignment |
|
7 8 |
4
6 2 4 |
4/6
4/8 4/12 4/14 |
Spectrophotometry
Properties of EMR Principles of optics Laws of Radiation Absorption Instrument Components Spectroscopic Methods |
Chapter 6; Problems: Chapt 6-even
Chapter 7; Problems: Chapt 7-even |
| 8
9 |
6
2 4 |
4/16
4/20 4/22
|
Molecular Spectroscopy
Theory Instrumentation |
Chapter 13; Problems: Chapt 13-even
|
| 9
10 |
6
2 4 |
4/26
4/28 4/30 |
FT Techniques
IR NMR MS |
Chapters 16,17; Problems: Chapt 17-odd
Chapters 19,20; Problems: Chapt 20-odd |
| 10
11 |
6
2 |
5/4
5/6 |
Separation Theory
Countercurrent Extraction Chromatographic theory |
Chapter 26; Problems: Chapt 26-odd |
| 11
12 |
4
6 2 |
5/10
5/12 5/14 |
Chromatographic Methods
Liquid Chromatography Gas Chromatography |
Chapter 27; Problems: Chapt 27-every
other even starting with 2
Chapter 28; Problems: Chapt 28-every other even starting with 2 |
Note: Final Presentation will be given during Final Exam Week.