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

            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)                                             50%

                        Take Home Assignments and Quizzes               25%

                        Comprehensive Final                                        25%

 

FINAL GRADE

 

            The final grade will be based on the following scale

 

                        A          89 %  to 100 %

                        B          77 %  to 88+ %

                        C          65 %  to 76+ %

                        D          50 %  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

 

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, extra-column 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, SP-FPD, 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, electro-osmotic 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, ICP-MS)  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)

            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