Che380 - Instrumental Methods of Analysis
Dr. Dwight R. Stoll
Department of Chemistry
Gustavus Adolphus College
Fall 2009


Table of Contents
Course Materials
Feedback
Paper Discussion Topics
Problem Sets
Recommended Reading
Websites
Writing in this Class



Course Materials (top)
09/09 - Syllabus
09/16 - Tentative Lab Schedule
09/11 - Week 1 slides, Week 1 notes
09/18 - Triclosan data
09/18 - Week 2 slides, Week 2 notes
09/20 - Solvent calibration data
09/21 - Solutions to quiz-1
09/25 - Week 3 slides, Week 3 notes
10/02 - Week 4 slides
10/09 - Solutions to Exam-1
10/09 - Week 5 slides
10/15 - Solutions to quiz-2
10/16 - Week 6 slides
10/23 - Week 7 slides
10/30 - Week 8 slides
10/30 - Solutions to quiz-3
11/05 - Solutions to Exam-2
11/06 - Week 9 slides
11/13 - Week 10 slides
11/14 - Laboratory project Guidelines and Rubric


Feedback (top)
Feedback #1 - Please complete by 9 AM Friday 09/11
Feedback #2 - Please complete by 9 AM Friday 09/18
Feedback #3 (Knowledge Survey #1) - Please complete by class time Monday 09/28
Feedback #4 - Please complete this by 9 AM Wednesday 10/14
Feedback #5 - (Knowledge Survey #2) - Please complete this by 9 AM Friday 10/16
Feedback #6 - Please complete this by 9 AM Monday 10/19
Feedback #7 - Please complete this by 9 AM Thursday 10/29, but earlier is better
Feedback #8 - (Knowledge Survey #3) - Please complete by Midnight Monday 11/02
Feedback #9 - Please complete this survey by midnight Tuesday 11/17


Paper Discussion Topics (top)
Topic
 Citation
 Target Date for Discussion
Solid-Phase Microextraction
 Arthur, C. L. and J. Pawliszyn (1990). "Solid phase microextraction with thermal desorption using fused silica optical fibers." Analytical Chemistry 62(19): 2145-2148. 09/14-09/16
Capillary Gas Chromatography
 Dandeneau, R. D. and E. H. Zerenner (1979). "An investigation of glasses for capillary chromatography." HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun. 2(6): 351-6.
 09-30 (Scott)
(slides)
Gas Chromatography-Electron Ionization Mass Spectrometry
 Gohlke, R. S. (1959). "Time-of-Flight Mass Spectrometry and Gas-Liquid Partition Chromatography." Analytical Chemistry 31(4): 535-541.
 10-08 (Jonna)
(slides)
Electrospray Ionization Mass Spectrometry
 Smith, R. D., J. A. Loo, et al. (1990). "New developments in biochemical mass spectrometry: electrospray ionization." Anal. Chem. 62(9): 882-99.
 Mid Oct.. (Siu On)
(slides)
Triple Quadrupole Mass Spectrometry
 Yost, R. A. and C. G. Enke (1979). "Triple quadrupole mass spectrometry for direct mixture analysis and structure elucidation." Anal. Chem. 51(12): 1251A-1252A, 1256A, 1258A, 1260A, 1262A.
 Mid Oct. (Jason)
(slides)
Matrix Assisted Laser Desorption Mass Spectrometry Karas, M. and F. Hillenkamp (1988). "Laser desorption ionization of proteins with molecular masses exceeding 10,000 daltons." Anal. Chem. 60(20): 2299-301. Mid Oct.
Inductively Coupled Plasma Mass Spectrometry
 Houk, R. S., V. A. Fassel, et al. (1980). "Inductively coupled argon plasma as an ion source for mass spectrometric determination of trace elements." Anal. Chem. 52(14): 2283-9.
Surface Enhanced Raman Spectroscopy
 Haynes, C. L., A. D. McFarland, et al. (2005). "Surface-Enhanced Raman Spectroscopy." Analytical Chemistry 77(17): 338 A-346 A.
 Alice
Cyclic Voltammetry

Anodic Stripping Voltammetry

Capillary Electrophoresis
 Jorgenson, J. W. and K. D. Lukacs (1981). "Zone electrophoresis in open-tubular glass capillaries." Anal. Chem. 53(8): 1298-302.
 Early Dec. (Anne)







Problem Sets (top)
PSet #1 - Due Monday September 21st in class, drug extraction method
Solutions to PSet #1
PSet #2A - Due Monday September 28th in class
Solutions to PSet #2A
PSet #2B - Due Monday October 12th in class (HPLC Simulator)
Solutions to PSet #2B
PSet #3 - Due Monday November 2nd in class
Solutions to PSet #3, two-solute Excel model
PSet #4 - Due Wednesday November 25th

Recommended Reading (top)
Week 1
For 09/11 - Handout on SPE

Week 2
For 09/14 - Paper on pipette tip extraction (link to web article)
For 09/16 - Paper on LLE (link to web article), original paper on SPME, overview of SPME
For 09/17 - Paper on SBSE (link to web article)
For 09/18 - Skoog text, section 1D, text excerpt from Rubinson and Rubinson (Contemporary Instrumental Analysis), article on the use of blanks and controls from JCE

Week 3
For 09/21 - Same as 09/18, article on system suitability from LCGC (link to web article)
For 09/23 - Same as 09/21
For 09/24 - Sections 1.1, 2.1, 2.2, 2.4, 2.5 from Modern HPLC for Practicing Scientists, by Michael Dong; Use Skoog text as a reference, sections A-E, chapter 26
For 09/25 - Skoog sections 27A

Week 4
For 09/28 - Skoog sections 27A, 27B1-B3, 27C
For 09/30 - Skoog sections 27A, 27B1-B3, 27C-E
For 10/01 - None, Exam-1
For 10/02 - Dong book, sections 1.2.2, 2.3, 2.6

Week 5
For 10/05 - Dong book, sections 1.2.2, 2.3, 2.6, and Chapter 3
For 10/07 - None, Nobel Conference 45
For 10/08 - Same as 10/05, Mass Spectrometry Primer Part I, by Michael Balogh (print version from LCGC, current electronic version (see 'How Does It Work', and 'Common Ionization' sections));  see Chapter 20 of Skoog text for reference
For 10/09 - Same as MS Primer material from 10/08

Week 6
For 10/12 - Same as MS Primer from 10/08, also, see MS Primer Part IV for Glossary of MS terms
For 10/14 - MS Primer Part II, or the 'What Types of Instruments are Used?' section of the electronic version
For 10/15 - MS Primer Parts II and III
For 10/16 - Same as 10/15

Week 7
For 10/19 - Article on the use of accurate mass measurements in forensic analysis; Chapter 1 from Random Walks in Biology, by Howard Berg
For 10/21 - Berg chapter on diffusion; review chapter 2 from Dong book, especially section 2.5; sections C and D of chapter 26 in the Skoog text (Note the Skoog sections only apply to packed beds!)
For 10/22 - Same as 10/21
For 10/23 - Same as 10/21

Week 8
For 10/28 - Skoog section 27B-4 (GC Detectors), and 28C-6 (LC Detectors)
For 10/29 - Sections 4.4-4.8 from the Dong book (but focus especially on the detectors we discuss in class), Skoog section 28C-6 (LC Detectors) for reference
For 10/30 - Tour of St. Peter WWTP

Week 9
For 11/02 - Same as 10/29
For 11/04 - Skoog Chapter 6
For 11/06 - Skoog Chapter 7, sections A-F, Chapter 13, sections A and B, and Chapter 14, sections A and B

Week 10
For 11/09 - Same as 11/06
For 11/11 - Skoog Chapter 13, Chapter 14 for reference
For 11/12 - Skoog Chapter 15
For 11/13 - Skoog Chapter 16, and 17, particularly sections 16A,B

Week 11
For 11/16 - Skoog Chapter 18, Chapter 1, sections B and C, Chapter 2 sections A-C
For 11/18 - None - lecture by PChem Candidate
For 11/19 - Skoog Chapter 1, sections B and C, Chapter 2 sections A-C
For 11/20 - Skoog Chapter 3, sections A-C, E-F

Week 12
For 11/23 - Skoog Chapter 4, sections A-C, and Chapter 5

Week 13
For 11/30 - Skoog Chapter 5

Week 14
For 12/7 -

Week 15
For 12/14 -

Week 16
Monday 12/21 - Final Exam at 3:30 PM in NHS 305


Websites/Videos (top)
Chronological
09/09 - U.S. Customs Laboratory Methods
09/16 - SPME Introduction Video
09/19 - Agilent Technologies Guide to Capillary GC
10/08 - Spectral Database for Organic Compounds
10/11 - Introductory video on the manufacture of fused-silica capillaries for analytical puposes (Polymicro)
10/11 - NIST Webbook
10/22 -

By Subject (top)
General
Sample Preparation
Gas Chromatography
Liquid Chromatography
Mass Spectrometry
Spectroscopy


Writing in this Class (top)

Things to remember...
  1. 'Spectra' is the plural of 'spectrum', and 'data' is the plural of 'datum'.  So, we say 'the data analyzed using the linear regression toolpak in Excel...', and 'the mass spectra for benzene and toluene are shown in Figure 3...', and 'four significant peaks are observed in the mass spectrum of xylene...'.
  2. The use of verbs to describe analytical chemical work is usually pretty clear; we say: