Syllabus of Advanced Analytical Chemistry
Course Category：Major Core
Majors：Chemistry, Intensified English Class
Total Hours：36 Hours Credit：2
Lecture Hours：2 /week
Textbooks：Skoog Holler Nieman Principles of Instrumental Analysis 2002
Instrumental Analysis (Wuhan University); Instrumental Analysis (Nanjiang University)
Based on the background of the students with the knowledges of chemical analysis and instrumental analysis such as ultraviolet-visible absorption spectroscopy, atomic absorption spectroscopy, pontentiometry, GC and HPLC, etc., the main aim of this course is to further broaden the students’ knowledge in instrumental analysis. Thus some other instrumental techniques including capillary electrophoresis, Raman spectroscopy, thermal methods, and immunoassay, etc. are presented in this course.
Chapter One: Capillary electrophoresis and capillary electrochromatography
4 weeks, 8 hours
1.1. An overview of electrophoresis
1.2. Principle of CE
1.2.1 Migration velocity
1.2.2 Migration rates
1.2.3 Plate hights in capillary electrophoresis
1.2.4 Electroosmotic flow
Main points emphasized: To understand the electronic double lay and electroosmotic flow
1.3. Instrumentation for CE
1.3.1 Sample introduction
1.4. Separation models and application of capillary electrophoresis
1.4.1 Capillary zone electrophoresis (CZE)
1.4.2 Capillary gel electrophoresis
1.4.3 Capillary isotachophoresis (CITP)
1.4.4 Capillary isoelectric focusing (CIEF)
Main points emphasized: To understand the principles of the found kinds of CE and their application
1.5. Capillary electrochromatography
1.5.1 Packed column electrochoromatography
1.5.2 Micellar electrokinetic capillary chromatography (MECC)
Main points emphasized: To understand the principles of MECC and its application
(1) What is electroosmotic flow? Why does is occur?
(2) Suggest a way in which electroosmotic flow might be repressed or reversed?.
(3) Why does pH affect separation of amino acids by electrophoresis?
(4) What is the principle of separation by capillary zone electrophoresis?
(5) What is the principle of separation by capillary isotachophoresis?
(6) What is the principle of separation by capillary isoelectric focusing?
(7) What is the principle of micellar electrokinetic capillary chromatography? How does it differ from capillary zone electrophoresis?
(8) Describe a major advantage of micellar electrokinetic capillary chromatography over conventional liquid chromatography.
Chapter Two: Raman Spectroscopy
4 weeks, 8 hours
2.1. Theory of Raman spectroscopy
2.1.1 Excitation of Raman spectra
2.1.2 Mechanism of Raman and Rayleigh scattering
2.1.3 Wave model of Raman and Rayleigh scattering
2.1.4 Intensity of Normal Raman Peaks
2.1.5 Raman Depolarization Ratios
Main points emphasized: To understand the principles of Raman spectrum and the inference between RS and infrared spectrum.
2.2.1 Laser sources
2.2.2 Sample illumination system
2.2.3 Raman Spectrometers
2.3. Application of Raman spectroscopy
2.3.1 Raman Spectra of Inorganic Species
2.3.2 Raman Spectra of Organic Species
2.3.3 Biological Applications of Raman Spectroscopy
2.3.4 Quantitative Applications
2.4. Other types of Raman spectroscopy
2.4.1 Resonance Raman Spectroscopy
2.4.2 Surface-Enhanced Raman Spectroscopy (SERS)
2.4.3 Nonlinear Raman Spectroscopy
(1) Why does the ratio of anti-Stokes to Stokes intensities increase with sample temperature?
(2) What is a virtual state?
(3) For carbon tetrachloride, the shift pattern is identical regardless of different excitation, why ?
(4) What is the principle of Raman scattering ?
(5) What is the mechanism difference between the Raman spectroscopy and infrared spectroscopy?
(6) Why homonuclear molecule such as nitrogen, chlorine, or hydrogen are Raman active species?
(7) For carbon dioxide molecule, the symmetric vibrational mode is Raman active, while asymmetric vibrational mode is Raman inactive, why?
(8) Give the explanation why sulfer dioxide is both Raman and infrared active species, while water is infrared active but Raman inactive.
(9) What is the difference between the terms of polarizability and polarization?
(10) Why the near-infrared laser sources find more application?.
Chapter Three: Supercritical Fluid Chromatography and Extraction
3 weeks, 6 hours
3.1 Properties of supercritical fluids
Main points emphasized: To understand the properties of supercritical fluids and to compare these properties to those of gaseous and liquid.
3.2 Supercritical fluid chromatography (SFC)
3.2.1 Instrumentation and operating variables
3.2.2 Comparison of supercritical to other types of chromatography
3.3 Supercritical fluid extraction
3.3.1 Advantages of Supercritical Fluid Extraction
3.3.3 Supercritical Fluid Choice
3.3.4 Off-line and On-line Extractions
3.3.5 Typical Applications of SFE
(1) Define (a) critical temperature and critical pressure of a gas.; (b) supercritical fluid
(2) What properties of a supercritical fluid are important in chromatography?
(3) How do instruments for supercritical fluid chromatography differ from those for
(a) HPLC and (b) GC?
(4) Describe the effect of pressure on supercritical fluid chromatography.
(5) List some of the advantageous properties of supercritical CO2 as a mobile phase for chromatographic separations.
(6) Compare supercritical fluid chromatography with other column chromatographic methods.
Chapter Four: Thermal Methods
3 weeks, 6 hours
4.1 Thermogravimetric analysis (TG)
4.2 Differential thermal analysis (DTA)
4.2.1 General Principles
4.3 Differential scanning calorimetry (DSC)
(1) Describe what quantity is measured and how the measurement is performed for each of the following techniques:
(a) thermogravimetric analysis;
(b) differential thermal analysis;
(c) differential scanning calorimetry;
(2) In thermal analysis methods, why is the thermocouple for measuring sample temperature seldom immersed directly into the sample?
(3) List the types of physical changes that can yield exothermic and endothermic peaks in DTA and DSC.
(4) List the types of chemical changes that can yield exothermic and endothermic peaks in DTA and DSC.
(5) Why are the applications of thermal gravimetry more limited than those for DSC and DTA ?
(6) Why does the glass transition for a polymer yield no exothermic or endothermic peak?
(7) Describe the difference between power compensators and heat flux DSC instruments.
Chapter Five: Automated Methods of Analysis
2 weeks, 4 hours
5.1 Flow-injection analysis (FIA)
5.1.2 Principles of Flow-Injection Analysis
5.1.3 Applications of Flow-Injection Analysis
5.2 Discrete automatic systems
5.2.1 Automatic Sampling and Sample Definition of Liquids and Gases
5.2.3 Automatic Organic Elemental Analyzers
Chapter Six: Automated Methods of Analysis
2 weeks, 4 hours
6.1. Iimmunochemical techniques
6.1.1 Immunoge, antigen and antibody
6.1.2 Immunoreaction, labelling technology
6.1.3 Principle of immunoassays
6.2 Applications of immunoassay
6.2.1 Applications of immunoassay in food and environmental analysis
6.2.2 Applications of immunoassay in medicine and biology
Assessment Methods：Examination in the end of the term
Made by ：Anping Deng