Instrumental Analysis ACHM 522
Spring 2008, 4 credit hours Dr. C. L. Leverette
Department of Chemistry and Physics SBDG 305, 803-641-3291
Lecture:
MWF
Lab: T
Th
Office Hours: MWF
and by appointment.*
*Please feel free to call or e-mail me when needed. In addition, my appointment schedule is very flexible. Therefore, if the office hours stated above do not fit into your schedule, we can set up a time that is convenient for you.
Prerequisite: ACHM 542 or consent of Department
Text and required materials:
· Principles of Instrumental Analysis, Sixth Edition, Skoog, Holler, Crouch.(required)
· Supplemental handouts as necessary.
· The lab procedures will be provided prior to each lab period.
· Scientific calculator
Rules for each class period:
1) Be in class on time.
2) Turn off cell phones. (unless you ask
for me for special permission before class)
3) Bring your own calculator to class. You cannot share calculators.
Cell Phone Policy: The use of cell phones
during class for any reason is not allowed unless prior approval has been given
to a student from the instructor. If you are planning to have a cell phone in
class, please turn the cell phone off. If a student is seen touching,
holding, or using a cell phone during a test period, the instructor will assume
that the student is cheating and the test will be recovered and a 0 will be
given to that student for the assignment.
Course Objectives: Analytical methods are often divided into two classifications: classical and instrumental. Classical methods include the “wet-chemistry methods” introduced in ACHM 321 Quantitative Analysis. These methods represent the earliest forms of quantitative analysis and are still used in many labs throughout the country. As technology and chemical instrumentation continue to progress, many of these classical methods are being replaced by more rapid and sensitive instrumental methods. Today’s analytical chemist can be classified as a problem solver that uses cutting edge scientific technology pulled from a variety of fields to qualitatively and quantitatively analyze complex systems in an attempt to better understand a given sample’s chemical composition and structural characteristics that give rise to its unique functionality.
The purpose of this course is to introduce chemists to the ever-changing world of chemical instrumentation. This class is a survey of the theory and practice of modern analytical instrumentation. Some topics covered will include: ultraviolet-visible spectroscopy, infrared and Raman spectroscopy, nuclear magnetic resonance spectroscopy, mass spectrometry, gas and liquid chromatographic techniques, atomic absorption spectroscopy, atomic force microscopy, scanning electron microscopy, and electrochemical methods of analysis. Examinations testing a general understanding of these topics will be given at the end of each organized section.
The goal of this class is to familiarize chemists with the theory and practice of available chemical instrumentation that can be utilized to solve challenging chemical problems.
Tentative Course Schedule:
|
No |
Day |
Lecture Topics |
Day |
Lab Topics |
|
1 |
1/14,M |
**Read |
1/15,T |
No lab |
|
2 |
1/16,W |
|
1/17,Th |
No Lab |
|
3 |
1/18,F |
Finish |
|
|
|
|
1/21,M |
|
1/22,T |
No Lab |
|
4 |
1/23,W |
|
1/24,Th |
Lab Check-In,
Linear Regression/Calibrations Exercise |
|
5 |
1/25,F |
|
|
|
|
6 |
1/28,M |
|
1/29,T |
Lab #1: The
Analysis of Soil Samples for Iron using Atomic Absorption Spectroscopy |
|
7 |
1/30,W |
Finish |
1/31,Th |
Lab #1 continued |
|
8 |
2/1,F |
Finish |
|
|
|
9 |
2/4,M |
|
2/5,T |
Lab #2: Verifying
Optimum Instrument Parameters for Flame AA |
|
10 |
2/6,W |
Finish |
2/7,Th |
Lab #2 continued |
|
11 |
2/8,F |
Finish (Lab #1 Due) |
|
|
|
12 |
2/11, M |
Finish |
2/12,T |
Exam #1 Lab #3: Colormetric
Analysis of Real Water Samples for Iron |
|
13 |
2/13,W |
Finish |
2/14,Th |
Lab #3 continued |
|
14 |
2/15,F |
Finish (Lab #2 Due) |
|
|
|
15 |
2/18,M |
|
2/19,T |
Lab #4: ATR
Analysis of a Complex Mixture |
|
16 |
2/20, W |
|
2/21,Th |
Lab #4 continued |
|
17 |
2/22,F |
(Lab #3 due) |
|
|
|
18 |
2/25,M |
Finish |
2/26,T |
Lab #5: Determination
of Conformational Order of Thin Films Using Infrared Spectroscopy |
|
19 |
2/27,W |
|
2/28,Th |
Lab #5 continued |
|
20 |
2/29,F |
(Lab #4 Due) |
|
|
|
21 |
3/3,M |
Finish |
3/4,T |
Exam #2 No Lab-Pittcon 2008 |
|
22 |
3/5,W |
No Class-Pittcon
2008 |
3/6,Th |
No Lab-Pittcon 2008 |
|
23 |
3/7,F |
(Lab #5 Due) |
|
Presentation topic
due date. (10 pts off presentation if topic not selected by this date) |
|
|
3/10-3/14 |
Spring Break-NO
CLASSES |
|
|
|
24 |
3/17,M |
|
3/18,T |
Lab #6: Introduction
to Surface-Enhanced Infrared Absorption (SEIRA) Spectroscopy |
|
25 |
3/19, W |
|
3/20, Th |
Lab #6 continued |
|
26 |
3/21,F |
Finish |
|
|
|
27 |
3/24,M |
|
3/25,T |
Lab #7: Exploring
Experimental Variables for Raman Spectroscopy |
|
28 |
3/26,W |
|
3/27, Th |
Lab #7 continued |
|
29 |
3/28,F |
Finish (Lab #6 Due) |
|
|
|
30 |
3/31,M |
|
4/1, T |
Lab #8: Quantitative
Analysis of Aspirin, Phenacetin, and Caffeine Mixtures by Nuclear Magnetic
Resonance Spectrometry |
|
31 |
4/2,W |
|
4/3,Th |
Lab #8 continued |
|
32 |
4/4, F |
(Lab #7 Due) |
|
|
|
33 |
4/7,M |
|
4/8,T |
Lab #9 A Study of
the Effect of the Changing of GC Instrument Parameters on Resolution |
|
34 |
4/9,W |
|
4/10,Th |
Lab #9 continued |
|
35 |
4/11, F |
(Lab #8 Due) |
|
|
|
36 |
4/14,M |
|
4/15,T |
Test #3 19, 20, 26-28, 30 Lab #10: HPLC TBD |
|
37 |
4/16, W |
Finish |
4/17,Th |
Lab #10 continued |
|
38 |
4/18, F |
(Lab #9 Due) |
|
|
|
39 |
4/21, M |
|
4/22,T |
Student
Presentations |
|
40 |
4/23,W |
|
4/24,Th |
Check-out of lab Senior Exit Exam |
|
41 |
4/25, F |
(Lab #10 Due) |
|
|
|
42 |
4/28,M |
Review for Final |
|
|
|
|
5/7 |
FINAL EXAM - |
|
|
Student Presentations: I feel very strongly that graduates in any discipline must be able to write coherently and give presentations about their discipline. These intangible skills represent the difference between graduates during the interview process for employment. The only way that these skills can be obtained is through practice. Therefore, in an effort to expand your own understanding about instrumental techniques while giving you an opportunity to speak on the subject, I expect each student to give a presentation on an instrumental method of their choosing to the class during assigned lab periods. The presentation should include some theory for the class to explain the technique (pulled from a selected book from the library or some other source that is approved by me -no wikipedia or google searches), modern experimental details (instrumentation required, various designs of the technique, uses of this technique, etc), and a review of 2 modern applications obtained from scientific literature (Analytical Chemistry, Journal of Physical Chemistry, Langmuir, Journal of Chromatography, Spectrochimica Acta, etc.). I want your articles found using the search engine Web of Science. I will teach you how to use this search engine and will help you retrieve the articles. The presentation should be made in PowerPoint and should be 15 minutes long. At the end of the presentation, anyone in the class may ask questions regarding the presentation. You will turn in your presentation in electronic form to me to be evaluated.
The topics should be selected early in the semester and approved by me before working on the project. Your topic must be approved by March 7, 2007. Failure to meet this date will result in 10 points being deducted from your presentation grade. This opportunity coupled with the conclusion of your 499 will begin to prepare you for the job market by refining your communication skills. If your path is graduate school, literature seminars (which are what these types of presentations are called) are required and the length of the presentation will be 60 minutes! So….this represents an opportunity for you to become more prepared before beginning the next chapter in your professional life!
The assigned grade will be based on the following criteria:
Content: (60 pts) 1) Detailed, accurate theory
2) Modern experimental designs
3) 2 relevant applications
Delivery: (20 pts) 1) Organized format
2) Neat presentation
3) Practiced delivery
Lab Report Guidelines: The labs chosen are designed to reinforce the key concepts learned in the lecture. In addition, the lab is designed to allow us to practice what we are learning. Chemistry is an experimental science and the lab is an integral part of your study in Chemistry. We will be doing labs that incorporate instrumental methods typically utilized by analytical chemists. As in Quant, accuracy and precision are still very important, so your attention to detail is very important for you to be successful.
Each written lab, provided by me
to you before each lab session, will outline the objectives and the procedures
for each lab. You are expected to study this write-up prior to coming to lab.
Tuesday lab time should be used to prepare samples for analysis. Thursday lab
time will allow for the instrumental analysis. You will sign up for time on the
instrument during the Tuesday lab section. You should arrive promptly at
Each written lab report, worth 15 pts, will be awarded the following points for each section.
Correct lab format 10 pts
and calculations
Accuracy of answer 5 pts (when applicable)
Total pts for each lab 15 pts
The tolerance for accuracy for a given lab will be determined by the how well the class does as a whole. This is completely at my discretion. For labs that do not require an accurate answer to a known amount, all 5 points will be given if the lab is done properly.
Lab write-ups for a given lab that was completed on a Thursday are due on the following Friday. These labs can be turned in anytime on Friday. Your class schedule has the days marked when you are to turn in a lab. If lab write-ups are not turned in by Friday, 1.5 pts will be deducted from that lab’s grade for each workday it is late. For instance, if a lab is 2 days late and the lab report initially earned all 15 points, the final points for that lab would be 12.
The following example (mock lab write-up, handout) of a correct lab write up must be copied to receive full credit (10 pts) for the lab format and calculations sections of the lab. I do not care how you collect the raw data from the lab. I recommend using a dedicated notebook that you can bring each week. I will not be grading this notebook. I have designed a lab write-up format that mimics what is often used in industry. The goal is to give you experience using this format that is required of analytical chemists in a “real world” setting. This is very similar to the format I used when working in global R&D for Cargill, Incorporated. In industry, you would have a dedicated notebook for data collection, but your “deliverable” to your client would be a written report. You may be the brightest chemist ever, but if you cannot communicate through presentation and writing then you are ineffective and will have a hard time finding a job. I want you to treat me as your client. You