Course Syllabus

Chemistry 405 Instrumental Analysis Spring 2007

TTH (10:30-11:50 am) Beauregard 237 Dr. Jim Baker 112 Beauregard Hall
Phone: (985) 448-4576 Email: jim.baker@nicholls.edu
Office Hours: WF 2:00 4:00, Th, F 8:30-10, 2-3 Other times by mutual arrangement

Catalog Description:
Chemistry 405. Instrumental Analysis. 3-3-0 Prerequisite or co-requisite: Chemistry 306, co-requisite: Chemistry
407. A course in the theory and practice of modern instrumental methods of analysis, with emphasis on
spectrophotometric, chromatographic, mass spectrometric, and electrochemical methods of analysis. (40.0502)

Prerequisite: Chemistry 306 Co-requisite: Chemistry 407.

Required Texts/Materials: D.A. Skoog, F.J. Holler, and T.A. Nieman, Principles of Instrumental
Analysis, 5th ed., Saunders College Publishing, 1998.
Supplemental Readings:
D. A. Skoog, F.J. Holler, and T. A. Nieman, Principles of Instrumental Analysis, 5th ed., Saunders College
Publishing, 1998. (Text)
Kanare, H. M., Keeping the Laboratory Notebook, American Chemical Society (ACS), 1985.
Dodd, J.S. ed., The ACS Style Guide, A Manual for Authors and Editors. ACS 1986. Figures and Tables
Handout (posted to Blackboard (Bb)
Dodd, Janet S. Ed. The ACS Style Guide ACS: Washington, DC, 1997, p 3. Chemistry Laboratory
Report Format (Bb)

Guidelines for Writing a Research Report, ACS

http://www.chemistry.org/portal/a/c/s/1/acsdisplay.html?DOC=education%5Ccpt%5Cts_rrguide.html
Calibrated Peer Review (CPR) Instructions
Molecular Science, http://cpr.molsci.ucla.edu/
then follow the links to the login page.
G. Aldrich Library of Infared Spectra, Aldrich Library of NMR Spectra, CRC Press

H. Microcomputer Software

Notebook, MS Simulator, HPLC Simulator JCE: Software

Graphical Analysis for Windows, Vernier Software
Microsoft Word, Excel, Powerpoint
Savant, Atomic Spectroscopy and Chromatography Training
Programs accessible in 245 Beauregard

WEB SITES
http://www.cem.msu.edu/~cem333/LectureMenu.html SIMON GARRETT, MICHIGAN STATE USES OUR
TEXT BOOK. MANY OF SKOOG'S DIAGRAMS, ORGANIZED BY CHAPTER IN OUR BOOK, 2000
http://www.chemistry.msu.edu/courses/cem333/ GREAT SITE, USES OUR TEXT, HAS REVIEW SHEETS FOR
TESTS, NOTES ON EACH CHAPTER MICHIGAN STATE, PDF FILES Dr. Greg M. Swain, 2004
4. http://science.widener.edu/~svanbram/chem366/chem366.html GREAT SITE, WIDENER STATE, GREAT
LINKS i.e. S/N, T.C. O' HAVER, Problem Sets Sample Abstracts, Writing Guides, more
http://www.chemguide.co.uk/analysismenu.html#top EXCELLENT FOR ALL CHEMISTRY, 405 NMR, IR, MS

Course Goals:
The student should demonstrate knowledge of the basic concepts involved in the theory and practice of modern
instrumental analysis.

Student Outcome Objectives:

Student outcome objectives are derived from the American Chemical Society (ACS) Division of Analytical
Chemistry, found at:
ANALYTICAL CHEMISTRY STANDARDS ACS accessed Dec. 27, 2004

http://www.chemistry.org/portal/a/c/s/1/acsdisplay.html?DOC=education%5Ccpt%5Cts_anlchem.html

"This instrumental analysis course is part of a sequence of courses that also includes modern quantitative analytical
chemistry and presents an integrated view of the theories, chemical methods, and instrumental techniques for
solving a variety of real problems in chemical analysis. Students receive a coherent and progressive treatment of the
various aspects of problem definition, selection of analytical method, experimental design, and data collection and
evaluation. The problem-oriented role of chemical analysis is emphasized throughout the student's experience.

The student should emerge from this instrumental analysis course with the following competencies:

1 Understand the distinction between qualitative and quantitative goals of determinations

2 Understand comparison and critical selection of methods for elemental and molecular analyses

3 Knowledge of sampling methods for all states of matter

4 Understand statistical methods for evaluating and interpreting data

5 Understand concepts of validation of data and experimental design

6 Understand sources of error in chemical and instrumental analysis

7 Understand interferences in chemical and instrumental analysis

8 Understand theory and operational principles of analytical instruments including electronic components

9 Exposure to computer-based data acquisition systems for analytical instruments

10 Understand the concept of instrument calibration

11 Fundamental understanding of the principles of and instrumentation for atomic, molecular, and mass
spectrometry, magnetic resonance spectrometry, chromatography and other methods of separation, electroanalytical
methods, and thermal methods

12 Understand basic concepts of stoichiometry and basic chemical reactions involving analytes and ordinary
reagents

13 Understand the importance to quantitation of equilibrium and kinetic aspects of chemistry

14 Understand concepts of availability and evaluation of analytical standards

15 Understand standardization methodology

Individual topics in this instrumental analysis course are presented in the framework of a systematic approach which
emphasizes functional roles, facilitates comparison of performance characteristics, and provides a pattern the student
can use to understand related topics not included in the formal course work. This course includes discussion of
approaches to optimize performance characteristics such as selectivity, sensitivity, uncertainty, and limit of
detection. Examples are drawn from modern biological materials and environmental chemistry."

The La. State Grade Level Expectations (GLE) for Chemistry (Grades 11/12) covered in this course can be
found at http://www.doe.state.la.us/lde/ssa/1842.html#Chemistry

Course Content
The student is expected to master and apply the following concepts to problem solving:

Ch 1 Introduction, pg 1 Instruments for analysis, selecting an analytical method, calibration of instrumental

methods;
ATOMIC SPECTROSCOPY pg 115
Ch. 6. An Introduction to Spectrometric Methods, pg 116 General properties of electromagnetic radiation, wave
properties of electromagnetic radiation, quantum-mechanical properties of radiation, Beers Law;
Ch 7. Components of Optical Instruments, pg 143 General designs of optical instruments for absorption, emission
and fluorescence, sources of radiation, wavelengths selectors, sample containers, radiation transducers, signal
processors and readouts, types of optical instruments;
Ch 8. An Introduction to Optical Atomic Spectrometry, pg 192 Optical atomic spectra, atomization methods,
sample introduction methods
Ch 9. Atomic Absorption and Atomic Fluorescence Spectrometry, pg 206 Atomic Absorption, sample atomization
techniques, atomic absorption instrumentation, interferences in atomic absorption spectroscopy, atomic
absorption analytical techniques;
Ch 10. Atomic Emission Spectrometry, pg 230 Emission spectroscopy based on plasma sources, flame emission
spectrometry, direct intensity and internal standard methods;
Ch 12. Atomic X-Ray Spectrometry, pg 272 X-ray fluorescence

TEST 1 Thursday, Feb. 15, 2007

SEPARATION METHODS
Ch. 26. An Introduction to Chromatographic Separations, pg. 673 General description of chromatography,
migration rates of solutes, zone broadening and column efficiency, the van Deemter equation, optimization
of column performance;
Ch. 27. Gas Chromatography, pg. 701 Principles of gas-liquid chromatography (GLC), instruments for gas-liquid
chromatography, columns and stationary phases, applications of, gas-solid chromatography,
Ch. 28. High-Performance Liquid Chromatography (HPLC), pg. 725, scope of HPLC, column efficiency,
instrumentation, partition chromatography, adsorption chromatography, ion-exchange chromatography,
size-exclusion chromatography;

TEST 2 Tuesday, March 19, 2007

MOLECULAR SPECTROSCOPY, pg 299
Ch. 13. Introduction to UV/Vis Molecular Absorption Spectrometry, pg. 300 Measurement of transmittance and
Absorbance, Beer's Law, effects of noise, instrumentation, single beam, double beam, photodiode array;
Ch. 14. Applications of Molecular Absorption Spectrometry, pg 329 Spectrometry, Molar absorptivities,
absorbing species, organic (MO description), inorganic (ligand field model) application of absorption
measurement to qualitative and quantitative analysis, photometric titrations;
Ch. 15. Molecular Luminescence Spectrometry, pg 355 Molecular Theory of fluorescence. Instruments for
measuring fluorescence and phosphorescence, applications and photoluminescence methods.
Ch 11. & Ch. 20.Atomic Mass Spectrometry & Molecular Mass Spectrometry, pg. 253 Molecular mass spectra, ion
sources, electron impact, chemical ionization, mass spectrometers, applications of molecular mass
spectrometry;
Ch. 16. Introduction to Infrared (IR) Spectrometry, pg. 380
Ch. 17. Applications of Infrared Spectrometry, pg. 404 Theory of infrared absorption spectrometry, infrared
sources and transducers, infrared instruments, dispersive and Fourier Transform; applications of infrared
spectrometry, mid-Infrared absorption spectrometry, mid-infrared reflection spectrometry;
Ch. 18. Nuclear Magnetic Resonance Spectroscopy, pg. 445 Nuclear Magnetic Resonance spectroscopy, theory of
nuclear magnetic resonance, environmental effects on NMR spectra, NMR spectrometers, applications of
proton NMR, Carbon-13 NMR;

TEST 3, Tuesday, April 26, 2007

ELECTROCHEMISTRY, pg. 563

Ch. 22. Introduction, pg. 564 Electroanalytical chemistry, electrochemical cells, cell potentials, electrode
potentials, calculation of cell potentials from electrode potentials, currents in electrochemical cells, types
of electroanalytical methods;
Ch. 23. Potentiometry, pg. 23 Reference electrodes, metallic indicator electrodes, membrane indicator electrodes,
ion-selective electrodes, instruments for measuring cell potentials, direct potentiometric measurements,
potentiometric titrations;
Ch 24. Coulometry, pg. 622 Current-voltage relationships during an electrolysis, Faraday;s Law, coulometric
methods, potentiostatic coulometry, coulometric titrations (amperostatic coulometry);
Ch. 25. Voltammetry, pg. 639 Voltammetric instrumentation; hydrodynamic voltammetry, cyclic voltammetry,
polarography, stripping methods.

FINAL EXAM - Friday, May 6, 2007 8-10 am

Course Requirements:
Required reading: Assigned readings in textbooks and supplements
Graduate students taking this course for graduate credit are also required to do an oral presentation and write a
comprehensive paper (approximately 10 pages) based on an independent study.

Methods of Evaluation

Tests- Three (3) 80 minute tests - approximately every 5-6 weeks. 300 pts
Daily work (in class activities and writing assignments) 50 pts
Paper (graduate students only) 100 pts
Final exam, comprehensive standardized test 200 pts
Grading Scale: A 90-100%, B 90-80%, C 80-65%, D 65-50%, F below 50%

Late/Missed Assignments: No makeup exams. Late assignments are penalized one letter grade/day late.
Attendance Policy: Regular attendance is required.

Academic Honesty Policy:

Academic misconduct will not be tolerated. The Universitys cheating and plagiarism policy as stated in the
Students Code of Conduct will be followed. The first incident will result in all guilty parties receiving a grade of 0
on the entire assignment. The second will result in a grade of F in the course. Some of your work will be performed
in teams. Each team member is plays a vital role and you are expected to co-operate and help each other without
copying.
"By taking this course, students agree that all assignments are subject to submission to Turnitin.com, an online
plagiarism prevention and detection service. All work submitted to Turnitin.com will be added to its database of
papers. Turnitin's privacy policy and a description of the service are available at http://www.turnitin.com.
Specifically, this service compares your paper with Internet webpages, articles in databases, and all papers
previously submitted from this university or any other. Turnitin then either confirms the originality of your work or
gives the source of plagiarism. In cases of detected plagiarism, the paper and supporting evidence will be handled in
compliance with the Student Code of Conduct (http://www.nicholls.edu/life/policy/code_of_conduct.pdf)."

Semester Withdrawls: The last day to withdraw form the class with a W is Friday March 30th, 2007.

16. Academic Disabilities Policy:

If you have a documented disability that requires assistance, you will need to register with the Office of Disability
Services for coordination of your academic accommodations. The Office of Disability Services is located in Peltier
Hall, Room 100-A. The phone number is (985) 448-4430 (TDD 449-7002)
NOTE: All parts of this syllabus are tentative and therefore should not be construed as a contract. Students will be
duly notified of any changes.

NOTE This syllabus is not a contract and no part of it should be construed as such. The syllabus is subject to
change. Students will be notified of these changes in a timely manner.
Attachment: Scoring Rubric for Discussion Questions, Calendar
Scoring Rubric for Discussion Questions
Level of Achievement General Approach
1. Addresses the question.
Exemplary
2. States a correct,
(3 pts)
relevant, justifiable
answer.
3. Presents arguments in a
logical order.
4. Uses acceptable style
and grammar (no errors)
Adequate 5. Does not address the
(2 pts) question explicitly,
although does so
tangentially.
6. States a correct,
relevant and justifiable
answer.
7. Presents arguments in a
logical order.
8. Uses acceptable style
and grammar (one error).
Needs Improvement 9. Does not address the
(1 pt) question.
10. States no correct,
relevant answers
11. Indicates
misconceptions.
12. Is not clearly or
logically organized.
13. Fails to use acceptable
style and grammar (2 or
more errors).
No answer (0 pts) 14. No answer OR
illegible
Reproduced with permission: Ecology, BIO 226, Spring 1998, D. Ebert-May
OLD OLD FOR REFERENCE ONLY HOMEWORK ASSIGNMENTS FROM OLD (4TH ED.)
SPRING 97, 98
Comprehension
15. Demonstrates a clear
and complete
understanding of the
question.
16. Backs conclusions
with data and warrants
(justification).
17. Uses 2 or more ideas,
examples and/or arguments
that support the answer.
18. Demonstrates only
adequate understanding of
question because does not
back conclusions with
warrants and data.
19. Uses only one idea to
support the answer.
20. Less thorough than
above.
21. Does not demonstrate
understanding of the
question.
22. Does not provide
evidence to support their
answer to the question.
CHEM 405/407 SPRING 2007
Faculty Ins. 11 12 13 14
Jan 10
17 MLK 18 Classes 19 X1 20 Ch 6 21
begin CH 1
24 X1 25 26 X2 27 CH 8 28
Ch 7
31 X2 FIELD 1 CH 9 2 X2 3 CH 10 4
TRIP FIELD TRIP
7 Mardi Gras 8 Mardi Gras 9 Mardi 10 TEST 11
Gras 1
14 15 2/16/2004 17 CH 18
X3 CH 13 X3 13

21 X3 22 CH 14 23 X4 24 CH 11, 20 25

28 X4 3/1/2004 CH 2 X4 3 CH 20 4
20
7 Midsem (MS) 8 MS 3T MS 9 MS 6M MS 10 MS Ch 26 11 MS
4M MS X5 TEST 2 LAB MID
SEM

14 MS grades due 15 ch 26 15 x6 17 ch 27 18
X5

21 x7 22 ch 28 23 x7 24 ch 28 25
Easter
Break
28 29 30 31 1-Apr

4 Classes resume 5 6 X8 7 W DAY CH 8

x8 TEST 3 16

11 X9 12 CH 17 13 X9 14 CH 19 15

18 X10 19 CH 19 20 X 11 21 EC 22
25 EC 26 TEST 4 27 LAB 28 Last Class 29
FINAL Day REVIEW

May 2 3 4 4M 5 6 3T
Finals begin Final 8-10 Final
am 8-10
9 Final 10 11 12 13
grades due

16 Spring
Semester
Ends

405 Ch
1 Intro
SECT II AT. SPEC.
6. Intro. Spec.
7. Comp. Opt. Inst.
8. Intro. Opt. At. Spec.
9. At. Abs.& At. Fluor.
10.At. Em.
12.At. X-Ray
TEST 1
SECT. III MOL. SPEC.
13. Intro. uv/vis Mol.Abs.
14. Ap. uv/vis Mol. Abs.
15. Mol. Luminescence
20&11 Mass Spec.
TEST 2
SECT. V SEP.METH.
26. Intro. Chrom. Sep.
27. GC
28. HPLC
TEST 3
16.Intro. Infrared (IR)
17. Appl. IR
19. NMR
SECT. IV EL.CHEM
22.
Intro
23. Potentiometry
24. Coulometry
25. Voltammetry
TEST 4

407 EXP. (X)

X1 AA **
X2 AE
X3 KaIn- vis**
X4 MS Sim
X5 GC-MS (Team)
X6 HPLC Sim
X7 HPLC BB (Team)
X8 IR
X9 NMR (Team)
X10 ISE (Team)
X11 EC (Team)
** formal report