‘Analytical Chemistry Part II’Course Syllabus
Course Category：Major Basic
Total Hours：72 Hours Credit：3
Lecture Hours：72 Hours
Douglas A. Skoog, F. James Holler, Stanley R. Crouch, Principles of Instrumental Analysis, Cengage Learning, 2006, 6th edition
Douglas A. Skoog, Donald M. West, F. James Holler, Stanley R. Crouch《Fundamentals of Analytical Chemistry》Brooks Cole; 8 edition (August 7, 2003)
Gary D. Christian, Analytical Chemistry, Wiley; 6 edition (March 14, 2003)
Robert Kellner, Jean-Michel Mermet, Matthias Otto, Miguel Valcarcel, H. Michael Widmer Analytical Chemistry: A Modern Approach to Analytical Science, Wiley-VCH; 2 edition (October 8, 2004)
David T. Harvey, Modern Analytical Chemistry, McDraw-Hill, 1999 1st edition
Daniel C. Harris, Quantitative Chemical Analysis, W. H. Freeman, 2015, 9th edition
Analytical chemistry is a discipline that studies and uses instruments and methods to separate, identify, and quantify matter. In practice separation, identification or quantification may constitute the entire analysis or be combined with another method. Separation isolates analytes. Qualitative analysis identifies analytes, while quantitative analysis determines the numerical amount or concentration. Taking this course, the students will develop the basic concepts of quantity in chemistry, and will get a systematic knowledge on the four basic chemical equilibriums and their applications for analyses, such as for titrimetric and gravimetric analyses, working principles of typical analytical instruments, their applicability over different forms of species. Through this course and related training, the students could also develop the ability of resolving related practical problems with suitable analytical strategies and technologies.
Chapter 13 Introduction on chromatography
13.1 chromatographic methods and classification
Teaching Outline: History and development; stationary phase and mobile phase; classification;
13.2 chromatogram and Nomenclature
Teaching Outline: Basic concepts, baseline, dead time, retention time, retention volume, adjusted values, peak width; information obtained from a chromatogram
13.3 basic principles for chromatography
Teaching Outline: Distribution process and distribution constant; capacity factor/retention factor; selectivity factors; related retention value; basic retention equation; plate theory, plate number and plate height; rate theory; separation resolution; basic separation equation
1. What do retention factor and selectivity factor mean in chromatography?
2. How to evaluate the theoretical plate number of a specific chromatographic column?
3. One stated that high theoretical plate number will lead to complete separation of a pair of species, is that correct? Try explain.
Chapter 14 Gas Chromatography
14.1 Instrumentation of gas chromatography
Teaching Outline: The construction, four subsystems: carrier gas, sample injection system, columns and temperature control system; temperature programming
14.2 detectors for gas chromatography
Teaching Outline: ideal properties of a good detector; thermal conductivity detector; flame ionization detector; electrode capture detector and flame photometery detector, their properties and applications
14.3 packed column gas chromatography
Teaching Outline: Classification of stationary phase; Kovats constants; McReynolds constants; widely used stationary phases; bonded and cross-linked stationary phases; basic principle for chiral separation;
14.4 open tubular chromatography
Teaching Outline: The advantages and disadvantages of open tubular columns; classification of open tubular columns; wall-coated open tubular column and porous-layer open tubular column; comparison with packed columns
14.5 qualitative and quantitative analysis
Teaching Outline: Qualitative analysis, by retention value, GC-MS; quantitative analysis, peak area, internal standard; standard calibration curve
14.6 application of gas chromatography
Teaching Outline: Some examples of the application
2. Why are open tubular columns so popular in gas chromatography as compared with packed ones?
3. What is a gas-solid chromatography?
4. How to evaluate the stationary phase of a gas-liquid chromatography?
Chapter 15 High Performance Liquid Chromatography and Supercritical Fluidic Chromatography
Teaching Outline: Effect of particle size of packing; requirement on mobile phases
15.2 instrumentation of liquid chromatography
Teaching Outline: Construction of the instrument; commonly used detectors, ultraviolet detector, fluorescence detector, refractive index detector and electrochemical detector
15.3 liquid-solid chromatography
Teaching Outline: The basic principles; commonly used stationary phase and mobile phase;
15.4 bonded-phase chromatography
Teaching Outline: Preparations of bonded-phase columns; Normal- and reverse-phase packing, properties and applications;
15.5 ion-exchange chromatography
Teaching Outline: Basic principle of ion-exchange chromatography; stationary phase and mobile phase; the instrumentation and the process;
15.6 size-exclusion chromatography
Teaching Outline: Basic principle of size-exclusion chromatography; gel filtration chromatography and gel permeation chromatography; the stationary and mobile phase;
15.7 supercritical fluid chromatography
Teaching Outline: Basic principle of supercritical fluid chromatography; the instrumentation; stationary and mobile phases; commonly used detectors for SFC; applications
1. Why are HPLCs advantageous over traditional low pressure liquid chromatography?
2. Compare the advantages and disadvantages of different types of detectors in HPLCs.
3. How does a size-exclusion chromatography work?
4. What is a reverse-phased liquid chromatography? Explain its popularity.
5. What is a supercritical fluid chromatography?
Chapter 16 introduction on spectroscopy
16.1 basic of electromagnetic radiation
Teaching Outline: Wave properties of electromagnetic radiation; electromagnetic spectrum; quantum-mechanical properties of radiation and photoelectric effect;
16.2 interactions of matter and light
Teaching Outline: Absorption, emission, scattering, refraction, reflection and diffraction;
16.3 Spectroscopic method
Teaching Outline: Absorption and emission spectroscopy; instrumentation for spectroscopy; source of radiation, continuum sources, line sources and laser sources; wave length selectors, filters, prism and grating monochromators, monochromator slits; radiation transducers; barrier-layer photovoltaic cells, vacuum phototubes, photomultiplier tubes; multichannel phototransducers,photodiode arrays, charge-coupled devices, charge-transfer devices; thermal transducers, thermal couples and bolometers
1. Name at least two transducers for visible light and infrared radiation detection respectively.
2. How does an absorption-based instrument differ from an emission-based one?
3. How do filters differ from monochromators differ in applications?
Chapter 17 Atomic Emission Spectroscopy
17.1 basic principles of Atomic emission spectroscopy
Teaching Outline: Origin of the spectrum; intensity of the spectrum lines; atomic line width; line broadening from the uncertainty effect; the effect of temperature
17.2 AES instrument
Teaching Outline: Inductively coupled plasma source, sample introduction, plasma appearance and spectra, analyte atomization and ionization; characteristics of Arc and spark sources; glow-discharge, laser based AES systems, direct plasma and microwave-induced plasma
17.3 Application of AES
Teaching Outline: Qualification with AES, quantitative and semi-quantitative detection with AES; Doppler, pressure, electric and magnetic field, self-absorption broadening; self-reversal
1. What does atomization mean?
2. Why internal standards are usually added in atomic emission measurements?
3. How could a solid sample be introduced for atomic emission measurement?
4. What does ICP-AES mean? List its advantages.
Chapter 18 Atomic Absorption Spectroscopy
18.1 basic principles of Atomic absorption spectroscopy
Teaching Outline: The process of AAS, resonance line and absorption line,; the number of ground atom and temperature of the flame; quantitative analysis with AAS
18.2 instrumentation for AAS
Teaching Outline: Primary radiation source, hollow cathode lamp and electrodeless discharge lamp; flame and electrothermal atomizer; the optical dispersive system; detectors and signal measurements
18.3 measurements and interferences
Teaching Outline: Quantitative measurements; spectral, chemical, and physical interferences; Zeeman effect
18.4 AAS method and its application
Teaching Outline: sensitivity and detection limit; characteristic sensitivity ,characteristic concentration and characteristic mass; standard calibration curve and standard addition;
18.5 atomic fluorescence
Teaching Outline: The process of atomic fluorescence, the intensity of atomic fluorescence; atomic fluorometer
1. How does atomic absorption differ from atomic emission in applications?
2. List at least three methods for background correction in atomic absorption measurement.
3. What do ionization suppressor, protecting agent and releasing agent mean, respectively?
4. How does a graphite furnace tube work in an atomic absorption measurement?
Chapter 19 Ultraviolet-Visible Absorption Spectroscopy
19.1 basic principles of Ultraviolet-visible absorption spectroscopy
Teaching Outline: the process of Ultraviolet-visible absorbance; the magnitude of molar absorptive molecular absorbing species and electron transition; absorbance of organic compound; absorption by inorganic species; the effect of slit width; detection of functional groups
19.2 Law of absorption
Teaching Outline: Lambert-Beer’s law and absorptivity; apparent deviation from Beer’s law
Teaching Outline: Components of the instrument, sources, monochromators, sample containers and photon detectors; types of spectrophotometer, single-beam system, double-beam-in-space and double-beam-in-time spectrometer;diode-array instrument
19.4 application of UV-Vis absorption spectroscopy
Teaching Outline: Application in qualitative analysis; quantitative analysis; application to absorbing and nonabsorbing species; procedural details, selection of wavelength, variables that influences absorbance; analysis of mixtures of absorbing substances; double-wavelength spectroscopic method; standard addition method; derivative spectroscopy
1. In UV-vis absorption , how to control the slit width for quantitative and qualitative analyses, respectively?
2. List possible reasons for deviation from Beer's law.
3. Give a illustrative diagram of a UV-vis spectrometer.
4. What is the advantage of a double-beam UV-vis spectrometer as compared with a single-beam one?
Chapter 20 molecular Luminescence Spectroscopy
20.1 molecular fluorescence and phosphorescence
Teaching Outline: Theory of fluorescence and phosphorescence; excited states producing fluorescence and phosphorescence, electron spin, single and triplet excited states; energy-level for photoluminescence molecules; deactivation processes, vibrational relaxation, internal conversion, external conversion, intersystem crossing, phosphorescence; quantum yield; transition types in fluorescence; quantum efficiency and transition type, fluorescence and structure, effect of structural rigidity; fluoresce spectra, fluorescence excitation spectra, fluorescence emission spectra and three-dimensional fluorescence spectra; characteristic of fluorescence spectra, Stock’s shift; variables affecting fluorescence and phosphorescence;
20.2 fluorescence spectroscopy and application
Teaching Outline: Components of fluorometer and spectrofluorometers, sources, filters and monochromators, cells and cell components, detectors; Quantitative detection, relation between fluorescence intensity and concentration; direct and indirect measurements; fluorescence imaging
20.3 phosphorimetric spectroscopy
Teaching Outline: Low temperature and room temperature phosphorescence; phosphoremeter and applications
20.4 chemiluminescence analysis
Teaching Outline: Principle for chemiluminescence; types of chemiluminescence; measurement of chemiluminescence; application of chemiluminescence
1. How do a fluorescence emission and a fluorescence excitation spectrum differ?
2. Describe the process of generation of fluorescence with a Jabloski diagram.
3. Why does phosphorescence only have a much lower occurrence as compared with fluorescence?
Chapter 21 Infrared Absorption Spectroscopy
21.1 theory of IR absorption spectrometry
Teaching Outline: Dipole moment change during vibrations and rotations; rotation transitions, vibration-rotation transitions; types of molecular vibrations; mechanical model of a stretching vibration in a diatomic molecule; simple harmonic motion and anharmonic oscillator; IR absorption spectra
15.2 IR spectra and molecular structure
Teaching Outline: Group frequencies of functional groups; important spectral region in infrared; the fingerprint region; factors affecting group frequencies, adjacent groups, hydrogen bonding, vibration coupling; inductive and conjugated effect;
15.3 instrument for IR spectroscopy
Teaching Outline: Dispersive IR spectrometer, source, sample cell, monochromator, detectors; Fourier-transform infrared spectrometer and working mechanism; sample handling and pretreatment
15.4 application of IR spectroscopy
Teaching Outline: Qualitative application for structural analysis; calculation of the degree of unsaturation; verification of structural analysis; quantitative analysis
1. What are the requirements for IR absorption? Why are some species IR inactive?
2. What are the advantages of the FT-IR as compared with a dispersive one?
3. Why is IR method mainly adopted for qualitative analysis while UV-vis mainly for quantitative?
4. What does fingerprint region mean in IR? What is the application?
Chapter 22 nuclear Magnetic Resonance Spectroscopy
22.1 theory of NMR
Teaching Outline: Quantum description of NMR; energy level on a magnetic field, relaxation process in NMR, spin-lattice relaxation and spin-spin relaxation,
22.2 NMR instrument
Teaching Outline: Instrumentation, the magnet, the field sweep generator, the radio–frequency source, the signal detector and recorder system; sample handling
22.3 Chemical shift of proton in organic compounds;
Teaching Outline: Source of the chemical shift; environmental effect on the chemical shift of proton NMR, effect of electron, effect of magnetic anisotropy; spin-spin coupling and splitting; coupling constant and its relation with molecular structure; first-order spectra and their interpretation
22.4 application of NMR method
Teaching Outline: Identification of structure of organic compound
1. What does chemical shift mean?
2. How does spin-spin splitting occur? What is its application?
3. Why are high quality and strong magnetic field magnets required for NMR measurements?
4. What are the regular solvents used for NMR measurements?
Chapter 23 mass Spectroscopy
23.1 Principles of mass spectrometer
Teaching Outline: Ion source, electron ionization, chemical ionization, field desorption, laser desorption, electrospary ionization; mass analyzer, double-focusing spectrometer, quadrupole mass spectrometer, time-of-flight analyzer, ion cyclotron resonance mass analyzer; signal detection and data processing; resolution of mass spectrometer
23.2 types of ions
Teaching Outline: The electron impact ionization process; molecular ion; isotope peaks, peaks for collision products, fragmentation patterns
23.3 organic compound structure and mass spectroscopy and application of mass spectroscopy
Teaching Outline: identification of structure of organic compounds; molecular weight determination; compound identification from comparison spectra; quantitative analysis, precision and accuracy; reaction mechanism; computerized library search system; analysis of mixture by hyphenated mass spectral methods
1. What do hard sources and soft sources mean in mass spectrometers?
2. Why is an electron impact ionization useful for the determination of the structure of organic compounds?
3. How does a time-of-flight mass analyzer work?
Exams (final 50%, mid 20%), Quizzes (20%), Assignments (10%)
Made by Jilin Yan
Date 10.28. 2016