Course Syllabus for English-Taught Majors

‘Analytical Chemistry Part II’Course Syllabus

 

Course Code09041036

Course CategoryMajor Basic

MajorsChemistry

SemesterSpring

Total Hours72 Hours         Credit3

Lecture Hours72 Hours        

InstructorsJilin Yan

Textbooks

Douglas A. Skoog, F. James Holler, Stanley R. Crouch, Principles of Instrumental Analysis, Cengage Learning, 2006, 6th edition

 

References

Douglas A. Skoog, Donald M. West, F. James Holler, Stanley R. CrouchFundamentals of Analytical ChemistryBrooks 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

 

 

Teaching Aim

         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

课时:2周,共6课时

Content

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

Problems

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

课时:2周,共6课时

Content

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

Problems

1. Compare the advantages and disadvantages of different types of detectors in gas chromatography.

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

课时:2周,共8课时

Content

15.1 mobile and stationary phase in liquid 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

Problems

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

课时:2周,共6课时

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

Problems

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

课时:2周,共8课时

Content

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

Problems

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

课时:2周,共8课时

Content

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

Problems

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

课时:2周,共6课时

Content

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

19.3 Instrumentation

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

Problems

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

课时:1周,共4课时

Content

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

Problems

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

课时:2周,共8课时

Content

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

Problems

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

课时:2周,共6课时

Content

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

Problem

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

课时:2周,共6课时

Content

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

Problems

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?

 

Assessment Methods

Exams (final 50%, mid 20%), Quizzes (20%), Assignments (10%)

 

 

                                Made by Jilin Yan

                       Date 10.28. 2016