CHE 3211 and 3281

CHEMISTRY 3211 and 3281

INSTRUMENTAL ANALYSIS

SYLLABUS --

Spring 2002

2001-2002 Catalog:3211 - CREDIT (3-5-5) Introduction to the theory and practice of modern chemical analysis
3281 - CREDIT (3-3-4) Provides a background to modern analytical chemistry and to chemical instrumentation methods of analysis with applications to engineering and other areas.

Text:Skoog, Holler and Nieman: Principles of Instrumental Analysis 5th edition, Saunders 1998

Instructor:Dr. Boris Mizaikoff

Web Site: then select 3211 or 3281

Detailed Description:The Course is designed to cover the theoretical principles and practical operation of a variety of instrumental analytical techniques. The topics include: atomic and molecular spectroscopies, mass spectrometry, electroanalytical techniques, chromatographic separations and thermal analysis. The lecture part of the course is common for 3211 and 3281. The differentiation is in laboratory section and in grading.

Educational Objectives:This course provides students with the theoretical background necessary for understanding the principles behind selected modern analytical instrumentation. Students gain practical experience in the laboratory equipped with modern instrumentation (similar to that employed by practicing scientists and engineers in industry or graduate school) used to solve current analytical problems.

Midterm Exam Dates:M1: 2/1; M2: 3/1; M3: 4/5; Final (in the week of 4/29-5/3)

Review Classes:4/3 and 4/26

Grading:32113281

Lab35 points30 points

Homework15 points15 points

I Midterm10 points10 points

II Midterm10 points10 points

III Midterm10 points10 points

Final Exam20 points25 points

Total100 points100 points

Grading Key:A: 100-85; B: 84-70; C: 69-55; D: 54-40; F: 39-0

Lecture Contents:(Book Chapter)Date

Overview (1 hr).(Chapter 1)1/4

Course objectives and mechanics

Analytical strategy

Classification and selection of analytical methods

Figures of merit (1 hr)(Chapter 1)1/7

Types of instrumental methods

Precision, accuracy, LOD, etc.

Properties of Electromagnetic Radiation (2 hrs)(Chapter 6)1/9-1/11

Types of Electromagnetic Radiation

Nature of Light

Basic Optical Parameters

Quantum Mechanical Basis of Radiation

Term Diagrams

Instruments for Optical Spectroscopy (3 hrs)(Chapter 7)1/14-1/18

Fundamental Components of Optical Instruments

Gratings, Slits, Dispersion, Resolving Power

Radiation Sources

Continuum, Line sources

Wavelength detectors

Photomultipliers, Photodiode Arrays, Charge Coupled Detectors

Signal Processors and Readout

Fiber Optics

FT instrumentation

School Holiday1/21

Atomic Spectrometry - Flame and Electrothermal (3 hrs)(Chapter 8,9)1/23-1/28

Atom Formation in Flames

Nebulizers, Flame Types

Chemical Equilibria in Flame (Element Ionization and Oxidation Equilibria)

Atomic Radiation Sources

Hollow Cathode Lamps and RF Electrodeless Discharge Lamps

Spectral, Matrix, and Ionization Interferences

Atom Formation in Electrothermal Vaporizer

Interferences: Scatter, Matrix Interactions

Emission Spectroscopy Based on RF Plasma Excitation (1 hr)(Chapter 10)1/30

RF Inductively Coupled Plasma

Simultaneous Multielement Analysis

Midterm 12/1

UV/Visible And Near Infrared Spectroscopy (2 hrs)(Chapter 13)2/4-2/6

Beer-Lambert Law, Basics of Absorption Spectroscopy

Quantitative Aspects of Absorption Spectroscopy

Chemical and Physical Errors in Beer-Lambert Law

Instrumentation for UV, Visible and Infrared Spectroscopy

Instruments for Separation in Space, Separation in Time

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CHE 3211 and 3281

Applications of Molecular Spectroscopy (2 hrs)(Chapter 14)2/8-2/11

Molecular Absorption Spectroscopy - Quantitative Aspects

Application to Non-absorbing Species, Standard Additions Method, Analysis of Mixtures

Dual-wavelength Measurements, Photoacoustic Spectroscopy

Luminescence Spectroscopy (2 hrs)(Chapter 15)2/13-2/15

Theory of fluorescence and phosphorescence

Instrumentation

Chemi- and bioluminescence

Applications

Introduction to Infrared Spectrometry (2 hrs)(Chapter 16)2/18-2/20

Theory

Instrumentation

Applications

Introduction to X-Ray Spectrometry (1 hr)(Chapter 12)2/22

Theory

Instrumentation

Applications

Introduction to Chromatographic Separations (2 hrs)(Chapter 26)2/25-2/27

General Concepts

Species Migration Rates

Band Broadening and Column Efficiency

Column Performance Optimization

Midterm 23/1

Spring Break3/4-3/8

Gas Chromatography (2 hrs)(Chapter 27)3/11-3/13

Principles of Gas-Liquid Chromatography

Column Efficiency in Gas-Liquid Chromatography

Instrumentation for Gas-Liquid Chromatography

Columns and Stationary Phases

Applications

High Performance Liquid Chromatography (4 hrs)(Chapter 28)3/15-3/22

Relationship of HPLC to GC

Column Efficiency in Liquid Chromatography

Instruments for High Performance Liquid Chromatography

Types of Liquid High Performance Chromatography

Partition, Adsorption, Ion, and Size-Exclusion Chromatography

Other Separation Methods (1 hr)(Chapter 29,30)3/25

Supercritical Fluid Chromatography

Capillary Electrophoresis

Mass Spectrometry (2 hrs)(Chapter 20)3/27-3/29

Mass Spectrometer Design and Features

Gas Chromatography/Mass Spectrometry, Liquid Chromatography/Mass Spectrometry

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CHE 3211 and 3281

Thermal Methods (1 hr)(Chapter 31)4/1

Thermogravimetric Methods

Differential Thermal Analysis

Differential Scanning Calorimetry

Review Class4/3

Midterm 34/5

Electroanalytical Chemistry (2 hrs)(Chapter 22)4/8-4/10

Types of electroanalytical techniques

Currents in electrochemical cells

Potentiometry (3 hrs)(Chapter 23)4/12-4/17

Reference electrodes

Indicator electrodes

Instrumentation

Voltammetry (3 hrs)(Chapter 24)4/19-4/24

Excitation signals

Instrumentation

Cyclic voltammetry

Polarography

Stripping methods

Microelectrodes

Review Class4/26

Finals4/29-5/3

LABORATORY:

3211: Coordinator Dr. Mira Josowicz (Dr. Christine Kranz)

TAs:Nick Menegazzo, Jamie Maddox, Isao Sasaki, Arteum Bochevarov,
George Lountos, Christine Nolan

Lab Manual:Chem 3211 Instrumental Analysis (handouts)

3281: Coordinator Dr. Christine Kranz

TAsAlexandra Molinelli, Christy Charlton, Tiffany Cao, Neil Pennington,
Manfred Karlowatz

Lab Manual:Chem 3281 Instrumental Analysis for Engineers

LIST OF HOMEWORKS:

January:7., 14., 21., 28.

February:4., 11., 18., 25.

March:11., 18., 25.

April:1., 8., 15., 22.

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