Che380 - Instrumental Methods of Analysis
Dr. Dwight R. Stoll
Department of Chemistry
Gustavus Adolphus College
Fall 2011


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



Course Materials (top)

09/06 - Syllabus, link to Chromedia
09/08 - Video - SPE Basic Concepts (11 MB)
09/09 - Introductory materials for Che380 laboratory, Handout for Experiment #1 (SPE)
09/09 - Week 1 notes, Week 1 slides
09/14 - Analytical Chemistry 2.0, by David Harvey
09/16 - Week 2 notes, Week 2 slides
09/16 - Solutions to Quiz-1
09/19 - TCS data for regression and internal standards; Video - External calibration and regression (18 MB)
09/28 - Solutions to Quiz-2
09/23 - Week 3 notes, Week 3 slides
09/29 - Video introduction to retention in HPLC (7 MB)
09/30 - Solutions to PS-1
09/30 - Solutions to PS-2
09/30 - Week 4 notes, Week 4 slides
10/07 - Week 5 slides
10/14 - Week 6 slides
10/14 - Weeks 5 and 6 notes
10/21 - Week 7 slides
10/28 - Week 8 notes and slides
11/3 - Solutions to PS-4; my 2-solute model in Excel
11/4 - Week 9 notes, slides
11/7 - Solutions to Quiz-4
11/14 - Evaluation of photometric accuracy using dichromate
11/15 - Solutions to Exam-2
11/11 - Week 10 notes, slides
11/18 - Week 11 notes, slides
11/22 - Week 12 notes, slides
12/2 - Week 13 notes, slides
12/8 - Solutions to Pset-5
12/9 - Week 14 notes, slides


Feedback (top)
09/08 - Feedback #1 - Please complete by 9 AM on Friday
09/28 - Knowledge Survey #1 - Please complete by 5 PM on Saturday
11/04 - Knowledge Survey #2 - Please complete by 7 PM on Sunday
12/12 - Knowledge Survey #3 - Please complete by 11 AM on Thursday


Problem Sets (top)
PS-1, due 09/19 in class - Handout, SPME using graphene article, Thermo glyphosate method
PS-2, due 09/30 in class
PS-3, due on or before 10/12 - Assignments 1-8 from Mark Jensen's LabView page (reading suggestions for Travis book) - Work in pairs, and send me your .VI files as you complete them.
PS-4, due 10/31 in class, link to HPLC simulator
PS-5, due 12/7 at 5 PM, link to data
   

Recommended Reading (top)
Week 1
09/07 - Handout on SPE (I'll handout in class), Trends in Sample Preparation by Ron Majors
09/07 - Chromedia - 'Basic goals' and 'Applying Solid Phase Extraction', under Sample Preparation for LC/MS
09/09 - Not all C18 SPE Phases are Created Equal, by Craig Perman

Week 2
09/12 - Practical aspects of Liquid/Liquid Extraction (LLE), by Ron Majors
09/13 - Overview of Solid Phase Microextraction (SPME), by John Hinshaw; Chromedia section on SPME, original research paper on SPME
09/14 - Recent review of QuECheRS extraction technology, by Ron Majors
09/16 - Article on the basics of quantitation; Chapter 5 from Analytical Chemistry 2.0, particularly sections C and D

Week 3
09/19 - Article on system suitability, by John Dolan
09/20 - Same as 09/19
09/21 - Same as 09/19
09/23 - Sections 1.1, 2.1, 2.2, 2.4, and 2.5 from Modern HPLC for Practicing Scientists, by Michael Dong - check out from reserve desk in library or purchase; see Chapter 12 of Harvey AC 2.0 text for reference

Week 4
09/26 - Same as 09/23; Parts 1, 2, 3, and 5 from Introduction to Open-Tubular Gas Chromatography by Hinshaw and Ettre; see Chapter 12 of Harvey AC 2.0 text for reference
09/27 - Continue with parts 1, 2, 3, and 5 from Hinshaw and Ettre
09/28 - Continue with parts 1, 2, 3, and 5 from Hinshaw and Ettre
09/30 - Dong book, sections 1.2.2, 2.3, 2.6, and Chapter 3

Week 5
10/03 - None, Exam-1
10/04 - None, Nobel Conference
10/05 - None, Nobel Conference
10/07 - Same as 09/30, ChromAcademy Tutorial on Electron Ionization for GC-MS

Week 6
Date/Day
 Topic
 Reading
 Multimedia
10/10 - Monday
 Electron Ionization for GC/MS
 Sections 1 (Who Uses Mass Spectrometry) and 2 (What are Mass Spectrometers) from Mass Spectrometry, by Michael Balogh ChromAcademy Tutorial on Electron Ionization for GC-MS
10/11- Tuesday
 GC Retention/Columns
 Hinshaw and Ettre, sections 3.3, 5.1-5.3, 5.6, 6.3, and 6.6
 ChromAcademy class section on GC Columns
10/12 - Wednesday
 LC Retention/RP Columns
 Dong book, sections 1.2.2, 2.3, 2.6, and Chapter 3 ChromAcademy class section on RPLC
10/14 - Friday
 Electrospray Ionization for LC/MS
 Balogh book, section 5 on Electrospray Ionization
 ChromAcademy class section on Electrospray Ionization


Week 7
Date/Day
 Topic
 Reading
 Multimedia
10/17 - Monday
 Tandem mass spectrometry
 Balogh book, pp. 27-28
 ChromAcademy - LC/MS Intro #15; Mass Spec #'s 28, 29-38
10/18- Tuesday
 Other ionization sources: APCI, APPI, MALDI
 Balogh book, pp. 19, 21
 ChromAcademy - Mass Spec sections on APCI, APPI; Proteomics #'s 9-11
10/19 - Wednesday
 Mass resolution, resolving power, and accurate mass
 Balogh book, pp. 40-48
 ChromAcademy - Mass Spec section on MS Interpretation #'s 2-11
10/21 - Friday
 Other mass analyzers: TOF, Sectors, ICR
 Balogh book, pp. 25, 30
 ChromAcademy - Mass Spec section on Mass Analyzers


Week 8
Date/Day
 Topic
 Reading
 Multimedia
10/26 - Wednesday
 Other mass analyzers: TOF, Sectors, ICR; begin peak broadening in separations Balogh book, pp. 25, 30 ChromAcademy - Mass Spec section on Mass Analyzers
10/28 - Friday
 Peak broadening in separations
 Chapter 1 on diffusion from Random Walks in Biology by Howard Berg; Part IV from Hinshaw and Ettre; In Dong book, review section 2.2 and read section 2.5


Week 9
Date/Day
 Topic
 Reading
 Multimedia
10/31 - Monday
 Peak broadening in separations; UV-Vis Pre-lab Giddings Random Walk paper
11/1- Tuesday
 Peak broadening in separations
 Same as 10/28, 10/31
11/2 - Wednesday
 Peak broadening in separations

11/4 - Friday
 Detectors
 Part VIII in Hinshaw and Ettre, Sections 4.4 through 4.8 in Dong book


Week 10
Date/Day
 Topic
 Reading
 Multimedia
11/7 - Monday
 Detectors; Fluorescence Pre-lab Part VIII in Hinshaw and Ettre, Sections 4.4 through 4.8 in Dong book
11/8- Tuesday
 Introduction to Spectroscopy
 Harvey AC 2.0, section 10A
11/9 - Wednesday
 Exam-2

11/11 - Friday
 UV/Vis Spectroscopy Basics
 Harvey AC 2.0, section 10A


Week 11
Date/Day
 Topic
 Reading
 Pre-Thoughts
 Multimedia
11/14 - Monday
 Spectroscopic Instrument Components
 Harvey AC 2.0, section 10B,C
Spectroscopy NOW Primer on UV-Vis, especially the section on Absorption Intensity
11/15- Tuesday
 UV-Vis Problems and Applications
 Harvey AC 2.0, sections 10C.5 and 10C.3

11/16 - Wednesday
 Fluorescence Spectroscopy
 Harvey AC 2.0, section 10F

11/18 - Friday
 IR Spectroscopy Harvey AC 2.0, section 10C
 IR
 Spectroscopy NOW Primer on IR


Week 12
Date/Day
 Topic
 Reading
 Multimedia
11/21 - Monday
 Raman Spectroscopy
 Chapter from Skoog, Holler, and Crouch
11/22- Tuesday
 Introduction to Electronics and Signal Processing

11/23 - No Class - Thanksgiving


11/25 - No Class - Thanksgiving




Week 13
Date/Day
 Topic
 Pre-Thoughts
 Reading
 Multimedia
11/28 - Monday
 Basic Electronics
 Basic Electronics
 Chapter from Rubinson and Rubinson, Contemporary Instrumental Analysis, sections 6.1-6.4, 6.8
11/29- Tuesday
 No Class


11/30 - Wednesday
 No Class - Analog Filtering
Rubinson sections 6.5, 17.6
 Analog Filtering Video
12/2 - Friday Analog to Digital Conversion
Chapter from Rubinson and Rubinson, Contemporary Instrumental Analysis, section 17.1


Week 14
Date/Day
 Topic
 Pre-Thoughts
 Reading
 Multimedia
12/5 - Monday
 Digital Filtering
Chapter from Rubinson and Rubinson, Contemporary Instrumental Analysis, sections 17.2
12/6- Tuesday
 Fourier Transforms
Chapter from Rubinson and Rubinson, Contemporary Instrumental Analysis, sections 17.4, 17.5, 17.7
12/7 - Wednesday
 Introduction to Electrochemical Methods
Harvey AC 2.0, chapter 11, sections A and B
12/9 - Friday Echem Intro cont.
Harvey AC 2.0, chapter 11, sections A and B


Week 15
Date/Day
 Topic
 Pre-Thoughts
 Reading
 Multimedia
12/5 - Monday
 Potentiometry and Voltammetry
Harvey AC 2.0, chapter 11, sections B and D
12/6- Tuesday
 Capillary Electrophoresis
 CE
 Harvey AC 2.0, chapter 12, section G
12/7 - Wednesday
 Modes of HPLC other than RPLC
Dong book, section 1.2; Harvey AC 2.0, chapter 12, section F



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:
  3. Numbers are always separated from their units.  So, we write 5 mL/min., not 5mL/min.