CHEM 322
INSTRUMENTAL ANALYSIS
SYLLABUS
Dr. DiLella
Spring 2011
COURSE DESCRIPTION
Instrumental Analysis is a three-credit hour course covering both the theoretical and the practical
aspects of modern chemical instrumentation. The course is designed to expose students to the wide variety of
instrumentation and techniques available for chemical analysis. The primary goal of the course is to provide
students with a thorough introduction to instrumental methods so that they will be able to intelligently select and
use the appropriate techniques for a particular analysis.
Most important types of analytical methods are covered, including atomic and molecular spectroscopy,
mass spectroscopy, chromatography, electrophoresis, electrochemistry and surface analysis. Each
instrumental method will be discussed in terms of instrument design, sampling techniques, sensitivity,
specificity, detection limits, and other analytical strengths and weaknesses. The student will learn how to select
an appropriate method for a problem and how to use the information available from the method. Special
emphasis is placed on the fundamentals of spectroscopy, chromatography and electrochemistry. Many
advanced techniques will be discussed in less detail but the student will be aware of how they are used.
Instrument design, sample preparation methods, precision, detection limits and sensitivity are examined for
each technique. Specific applications are discussed for chemical, biochemical and environmental analyses.
PREREQUISITES
CHEM 321 and CHEM 321L are highly recommended
CHEM 322L should be taken concurrently
Computer skills are not a prerequisite but students who do not know basic computer spreadsheet
operations should see the instructor as soon as possible to get special tutoring in these skills.
TEXT
J. R. Robinson, E. M. Skelly Frame, and G. M. Frame II, “Undergraduate Instrumental Analysis”, 6th
ed., Marcel Dekker (2005) ISBN 0-8247-5359-3. Most of chapters of the text will be covered but not all at
the same level of detail. See the list of topics outlined below. Several handouts that summarize important
material will be provided in class.
CLASS HOURS
MWF 11:10 – 12:00
OFFICE HOURS
MWF 10:10-11:00, MW 3:10-4:00, R 1:10-2:00, F 12:10 – 1:00 or by appointment
Office : Byrd Center 315
304-876-5430
ddilella@shepherd.edu
web page: http://WEBPAGES.SHEPHERD.EDU/DDILELLA/
ATTENDANCE POLICY
Students are expected to attend all classes. There are many topics covered in this course and, by
necessity, many will be covered at a lower level than is presented in the text. Class attendance is essential if a
student wants to know what is expected on a given topic.
ACADEMIC HONESTY
Cheating in all its forms, including plagiarism and cheating on visual work, is considered an
academic matter and will result in automatic dismissal from the course and will be recorded on the official
transcript.
TESTS
1
CHEM 322
INSTRUMENTAL ANALYSIS
SYLLABUS
Dr. DiLella
Spring 2011
There will be three term tests and a comprehensive final. There will be several in class quizzes and
graded take-home assignments. Makeup exams will not be administered without a valid written excuse.
Term exams that are missed with a valid excuse may be made up during finals week.
GRADING
Mid-term tests (3)
Take Home Assignments and Quizzes
Comprehensive Final
50%
25%
25%
FINAL GRADE
The final grade will be based on the following scale
A
B
C
D
89 %
77 %
65 %
50 %
to 100 %
to 88+ %
to 76+ %
to 64+ %
TOPICS AND ORDER OF PRESENTATION
For some chapters not all sections will be covered. For those chapters, the sections to be covered are
given in parentheses after the chapter title.
Chapter 1 (1.1 – 1.3, 1.5 – 1.6) – Concepts of Instrumental Analysis
Qualitative analysis, quantitative analysis, sampling, accuracy, precision, systematic and random error,
trace and ultra trace analyses, mean, absolute error, relative error, sample standard deviation, standard
deviation of the mean, variance. confidence level, outliers, signal, noise, signal-to-noise ratio, calibration
curves, sensitivity, detection limits, quantitation limits. Problems: 1.1, 1.4, 1.7, 1.11, 1.19, 1.30
Chapter 2 (2.1 – 2.7) – Introduction to Spectroscopy
Electromagnetic radiation, Interaction of radiation with matter, absorption, emission, scattering,
transmission, reflection, luminescence, fluorescence, phosphorescence, ground state, excited state, electronic
transitions, vibrational transitions, rotational transitions, Beer Lambert Law, absorbance, absorptivity,
transmittance, deviations from Beer’s law, stray light, calibration curve method, standard addition method,
internal standard, spectrometer, continuum and line sources, filters, monochromators, prisms, gratings,
resolution, resolution of prisms and gratings, optical slits, single-beam and double-beam optics, Fourier
Transform spectrometers, interferometer. Problems: 2.7, 2.8, 2.14, 2.15, 2.18, 2.25, 2.26, 2.27, 2.31, 2.34,
2.38, 2.41
Chapter 5 (5.1 – 5.3, 5.5, 5.8 – 5.10) – Visible and Ultraviolet Molecular Spectroscopy
Electronic transitions in molecules, absorption by molecules, molar absorptivity, shape of absorption
bands, solvents for UV-vis spectroscopy, UV-vis instrumentation, UV and visible sources, UV-vis
monochromators, UV-vis detectors, phototube, photomultiplier tube, diode array detectors, sample holders for
UV, quantitative analysis in UV-vis, fluorescence and phosphorescence spectroscopy, instrumentation for
luminescence, arc lamps, applications of fluorescence. Problems: 5.1, 5.2, 5.3, 5.4, 5.6 ,5.10 ,5.12, 5.16, 5.17,
5.18, 5.19, 5.20, 5.42, 5.43
Chapter 4 (4.1 – 4.8) – Infrared Spectroscopy
IR absorption in molecules, dipole moment, stretching and bending vibrations, windows for IR, IR
sources, IR monochromators and interferometers, IR detectors, sampling techniques for IR spectroscopy, IR
reflectance and emission measurements, attenuated total reflection, quantitative analysis with IR spectroscopy,
near IR spectroscopy, instrumentation for near IR, applications of NIR Raman spectroscopy, Raman
instrumentation, applications of Raman. Problems: 4.1, 4.2, 4.8, 4.11 ,4.12 ,4.15 ,4.16 ,4.19 ,4.21 ,4.22
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CHEM 322
INSTRUMENTAL ANALYSIS
SYLLABUS
Dr. DiLella
Spring 2011
Chapter 3 (3.1 – 3.6) – Nuclear Magnetic Resonance Spectroscopy
magnetic nuclei, nuclear spin, saturation, line widths, longitudinal and transverse relaxation time, magic
angle spinning, FTNMR, chemical shift, shielding, spin-spin coupling, coupling constant, NMR instrumentation,
magnet, probe, RF generation and detection, sample preparation, molecular structural determination in NMR,
equivalent nuclei, chemical exchange, 1H NMR, 13C NMR, 2D NMR, COSY, HETCOR, quantitative analysis in
NMR. Problems: 3.1, 3.2, 3.3, 3.4, 3.5 , 3.8, 3.10, 3.15, 3.16, 3.19
TEST 1
Chapter 11 (11.1 – 11.12) – Principles of Chromatography
Equilibrium ratio, capacity factor, retention time, adjusted retention time, selectivity factor, theoretical
plate, resolution, HETP, Van Deemter Equation, longitudinal diffusion, eddy diffusion, mass transfer, extracolumn band broadening, peak shape, normal and reverse phase chromatography, mass and concentration
detectors, Problems: 11.1, 11.2, 11.5, 11.7, 11.8, 11.9, 11.14
Chapter 12 (12.1 – 12.8) - Gas Chromatography
Carrier gas, packed column, split-splitless injection, TCD detector, FID detector, ECD detector, SPFPD, NPD, GC-MS, GC-IR Problems: 12.1, 12.2, 12.6, 12.9
Chapter 13 – (13.1 – 13.6) Chromatography with Liquid and Mobile Phases
Column efficiency in liquid chromatography. Instrumentation, pumping systems, sample injection,
detectors (UV, fluorescence, refractive index, electrochemical). Partition chromatography, reverse-phase and
normal phase packings, selection of column and mobile phase. Adsorption chromatography. Ion exchange
chromatography. Size exclusion chromatography. Thin layer chromatography, Electrophoresis, electroosmotic flow, capillary zone electrophoresis (CZE), detectors, capillary gel electrophoresis (CGE), micellar
electrokinetic chromatography (MEKC). Problems: 13.1, 13.6, 13.9, 13.11, 13.13, 13.20, 13.23
Chapter 9 - Mass Spectroscopy I: Principles and Instrumentation
Sample input systems, ionization sources (EI, CI, ESI, MALDI, FAB). Mass analyzers (magnetic
sector, double-focussing, quadrupole, time-of-flight, ion trap, FTICR), ion detectors (electron multiplier, faraday
cup), Problems: 9.1, 9.2, 9.3, 9.8, 9.10, 9.11, 9.12, 9.13, 9.14, 9.15, 9.16, 9.20
Chapter 10 - Mass Spectroscopy II: Spectral Interpretation and Applications (10.1-10.4)
Base peak, molecular ion, fragmentation, nitrogen rule, isotopic abundance, heteroatoms, halogen
isotopes, rings plus double bonds, mass spectra of common classes of organic compounds, atomic MS, ICPMS) Problems: 10.1, 10.2, 10.3, 10.15, 10.17, 10.21, 10.23, 10.29, 10.33
TEST 2
Chapter 6 - Atomic Absorption Spectroscopy (6.1 – 6.5)
Atomic energy levels, atomic absorption, atomic emission, atomic fluorescence, atomic line widths,
effect of temperature on atomic spectra, spectral linewidth, hollow cathode lamps, electrode-less discharge
lamp, flame atomization, electrothermal atomization, AA optics and spectrometer, modulation, interferences in
AAS, chemical interference, matrix interference, ionization interference, spectral interference, background
correction, Problems: 6.1, 6.3, 6.5, 6.6, 6.17, 6.20, 6.28, 6.29, 6.30, 6.32
Chapter 7 Atomic Emission Spectroscopy (7.1 - 7.3, 7.7, 7.9)
Flame atomization, flame absorption profiles, types of flames, flame structure. Electrothermal
atomization, Atomic spectral sources, source modulation, spectrophotometers, Spectral interferences,
background correction. Chemical interferences, compound formation, ionization. Sample preparation, solvent
effects, calibration curves, standard addition, detection limits, and accuracy. Problems: 7.1, 7.2, 7.4, 7.7, 7.10,
7.11, 7.19, 7.24, 7.27
Chapter 8 - Atomic X - Ray Spectroscopy (8.1 – 8.3)
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CHEM 322
INSTRUMENTAL ANALYSIS
SYLLABUS
Dr. DiLella
Spring 2011
Emission of X-Rays, absorption of X-Rays, X-Ray fluorescence, X-Ray sources, X-Ray Detectors and
signal processors, wavelength dispersive instruments, energy dispersive instruments, Problems: 8.2, 8.6, 8.9,
8.10
Chapter 14 - Surface Analysis (14.1 – 14.2, 14.4 - 5)
Principles of electron spectroscopy, ESCA, instrumentation for electron spectroscopy, Auger electron
spectroscopy, depth profiling, SIMS, electron microprobe Problems: 14.1, 14.4, 14.5, 14.7, 14.9, 14.12, 14.15,
14.18
Chapter 15 - Electroanalytical Chemistry (15.1 – 15.4)
Some of this material is covered in CHEM 321 and it is assumed that the student is familiar with
potentiometry and columetry methods. This material will be reviewed briefly in class. Problems: 15.2, 15.4,
15.10, 15.11, 15.12, 15.13, 15.18
TEST 3 –
COMPREHENSIVE FINAL – Wed. May 4, 2011 - 12:00 noon
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