Chemistry 407
Instrumental Analysis Laboratory
Spring 2008
Instructor: April Dupre Office: 107 Peltier Hall
Phone: (985) 448-4503 Email:
Office Hours: MW 8 – 12:00, TR 8:30-10:30 or by appointment
Catalog Description:
Chemistry 407. Instrumental Analysis Laboratory. 2-0-6. Prerequisite or Co-requisite: Chemistry 405. A laboratory course involving modern instrumental methods of analysis including absorption, emission, and fluorescence spectrophotometry; chromatographic methods and electrochemical analysis.
Prerequisites or Co-requisite:
Chemistry 405.
Required Texts and Other Materials:
1. Sawyer, Heineman, Beebe; Chemistry Experiments for Instrumental Methods, John Wiley and Sons, 1984. (Lab Manual)
2. Lab Notebook
3. Safety Goggles
Supplemental Readings:
A. D. A. Skoog, F.J. Holler, and T. A. Nieman, Principles of Instrumental Analysis, 5th ed., Saunders College Publishing, 1998. (Text)
B. Kanare, H. M., Keeping the Laboratory Notebook, American Chemical Society (ACS), 1985.
C. Dodd, J.S. ed., The ACS Style Guide, A Manual for Authors and Editors.
D. Dodd, Janet S. Ed. The ACS Style Guide ACS: Washington, DC, 1997, p 3. Chemistry Laboratory Report Format
E. Guidelines for Writing a Research Report, ACS http://portal.acs.org/portal/fileFetch/C/CTP_005606/pdf/CTP_005606.pdf
F. Aldrich Library of Infared Spectra, Aldrich Library of NMR Spectra, CRC Press
G. Microcomputer Software
1. JChemEd Software
a. GC, HPLC, NMR, MS, IR simulation
2. Microsoft Word, Excel, Powerpoint
Course Goals:
The student should learn the principles and operations of the following instruments: UV-vis spectrophotometer (diode array and traditional), AA, GC, GC-MS, HPLC; IR, NMR.
Student Outcome Objectives:
The student should emerge from this instrumental analysis laboratory 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 laboratory 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."
Course Content and Experimental Goals:
1. AA (if possible) FORMAL REPORT REQUIRED
a. Experimental protocol 9-1 p. 244
b. Quantitation of Cu content in a German silver alloy using BOTH a calibration curve and the method of standard additions
c. Comparison of calculated values in terms of method and in terms of the true Cu content. An explanation of this difference will be required with necessary references
d. Quantitation of Cu content along with the identification of the other metals present in the alloy will be done using ICP-AE
e. All methods of analysis will be compared and contrasted and the benefits and disadvantages of each must be discussed in the formal report
2. UV-vis and HPLC (if possible) FORMAL REPORT REQUIRED
a. Experimental protocol from handout for UV-vis
b. Experimental protocol 13-1 for HPLC p. 347
c. The caffeine and sodium benzoate content in various commercially available bevarages (mountain dew, mello yello, sprite, coke, pepsi, and red bull) will be determined through both methods
d. The methods will be compared and contrasted and the inherent advantages and disadvantages of each will be discussed, along with the rationale used to determine which method should be chosen for specific analyses
3. GC and IR (if possible) FORMAL REPORT REQUIRED
a. Experimental protocol 12-3 p. 336
b. The exact nature of the sample, experiment and information that must be obtained will be given at the time of the experiment. The goal may be different for each student/team of students. Students will choose and optimize experimental parameters for the analysis.
c. In the formal report, students must discuss the specific results obtained and the rationale for the parameters they chose and why.
4. AA
a. Experimental Protocol 9-3 p. 258
b. Determination of Fe and Ca content in commercially available food products
c. Students may choose between a calibration curve method and the method of standard additions for the analysis, but must justify their choice
d. Comparison of experimentally determined values with those reported on packages
5. UV-vis
a. Experimental protocol 6-4 p. 193
b. Spectrophotometric determination of the pKa of an indicator
c. Students will be given an unknown indicator which they must identify based on the pKa value obtained
6. MS, NMR, and IR Simulator
a. JCE software will be used to generate spectra of compounds.
b. It is crucial that students understand the types of information that can be obtained using different instrumental methods so that they may determine a suitable method to choose based on the specifications of the analysis. In the case of these 3 techniques, they must be used in conjunction with one another to unambiguously identify the sample compound.
c. Focus with these 3 simulators will be based on compound identification and structural elucidation through spectral interpretation.
Course Requirements:
Required reading: Assigned readings in lab manual, textbook and supplements.
Required written work: A laboratory notebook must be maintained on a daily basis Lab reports/write-ups are required for all experiments.
Required oral presentation: 20-minute in-class group power point presentation on selected topics from literature
Method of Evaluation:
Formal lab reports - 3 x 100 pts each 200 pts
Short lab reports - up to 5 x (up to 50 pts each) 150
Group Presentation 50
Final Exam 200
A modified 10 pt scale is used: A 100-90%, B 89-80 %, C 79-65%, D 64-55%.
Make-up Policy:
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 dishonesty will not be tolerated. The University’s cheating and plagiarism policy as stated in the Code of Student Conduct will be followed. Some of your work may be performed in teams. Each team member plays a vital role and is expected to cooperate and help others WITHOUT copying.
Semester Withdrawals:
The last day to withdraw form the class with a “W” is Friday, April 3, 2008.
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)
CLASS DISRUPTIONS: Are not tolerated. The use of cell phones, pagers and/or any other electronic personal devices in class is prohibited. Any infractions will result in the dismissal of the student(s) in violation of this policy and a score of 0 on the lab being conducted that day.
ACADEMIC GRIEVANCES - The proper procedure for filing grade appeals or grievances related to academic matters is listed in Section 5 of the Code of Student Conduct and at the following link: http://www.nicholls.edu/documents/student_life/code_of_conduct.pdf.
CONTINUED LEARNING FOLLOWING AN EXTREME EMERGENCY
In order to make continued learning possible following an extreme emergency:
Students are responsible for:
• Reading regular emergency notifications on the NSU website;
• Knowing how to use and access Blackboard (or university designated electronic delivery system);
• Being familiar with emergency guidelines;
• Evacuating textbooks and other course materials;
• Knowing their Blackboard (or designated system) student login and password;
• Contacting faculty regarding their intentions for completing the course.
Faculty is responsible for:
• Their development in the use of the Blackboard (or designated) software;
• Having a plan for continuing their courses using only Blackboard and email;
• Continuing their course in whatever way suits the completion of the course best, and being creative in the continuation of these courses;
• Making adjustments or compensations to a student’s progress in special programs with labs, clinical sequences or the like only in the immediate semester following the emergency.
***THIS SYLLABUS IS NOT A CONTRACT AND IS SUBJECT TO CHANGE.***
TENTATIVE SCHEDULE
M / T / W / Th / F
14
Classes Begin / 15
CHECK-IN / 16 / 17
UV/vis sodas / 18
21 MLK / 22
UV/vis sodas / 22 / 23
HPLC sodas / 24
28 / 29
AA Food / 30 / 31
AA Food / 1
4 Mardi Gras / 5 Mardi Gras / 6 Mardi Gras / 7
GC Simulator / 8
11 / 12
Team GC / 13 / 14
Team GC / 15
18 / 19
Team GC / 20 / 21
Team GC-MS / 22
25 / 26
HPLC simulator / 27 / 28
Presentations / 29
3
PITTCON / 4
PITTCON / 5
PITTCON / 6
PITTCON / 7 REGION X
SCI FAIR
10 / 11
pKa Indicator / 12 / 13
pKa Indicator / 14
17 / 18
IR / 19 / 20
Spring Break / 21
Spring Break
24
Spring Break / 25
Spring Break / 26
Spring Break / 27
Spring Break / 28
Spring Break
31 / 1
AA Alloy / 2 / 3
AA Alloy / 4
7
ACS MTG / 8
ACS MTG
AE Alloy / 9
ACS MTG / 10
ACS MTG
AE Alloy / 11
14 / 15
Simulations / 16 / 17
Simulations / 18
22 / 22
Simulations / 23 / 24
Simulations / 25
28 / 29 CHEM 407
FINAL EXAM / 30 / 1 STUDY DAY
NO CLASSES / 2 STUDY DAY
NO CLASSES
5
FINAL EXAMS / 6
FINAL EXAMS / 7
FINAL EXAMS / 8 CHEM 405
FINAL 8-10 / 9
FINAL EXAMS
12
GRADES DUE