Course Code: B53004H
Course Name: Analytical Chemistry and Experiments
Pre-requisite: Inorganic Chemistry, Organic Chemistry, Physical Chemistry, General Physics, Advanced Mathematics
Through this course, students should a) master basic theories, concepts, analytical methods, calculation, design of routine analysis experiments and operation of instrument and equipment; b) master the method of analysis samples’ collection and preparation, learn the error types, source and lower ways, master the basic concepts of accuracy and precision and relationships between them, as well as the calculation of various types of errors and deviations, be familiar with the method of quality assurance and control during the whole experiment process; c) understand the related theories, concepts and calculation of four volumetric analysis methods, i.e. acid-base titration,complexometric titration, redox titration and precipitation titration. d) learn the process of modern analytical chemistry, and use conventional optical analysis methods skillfully based on light absorption or emission, and conventional electrochemical analysis methods based on conductance, potential and electrolytic current; learn the basic structures, fundamentals and characteristics of analytical instruments, grasp operation of several conventional analytical instruments. e) form serious, careful, tidy experiment habits and strict quantitative concepts; observe and record experimental phenomena and data and write an accurate experimental report. With this course, students will enhance the ability of analyzing and solving problems and grasp the fundamentals of new technology and methods quickly, which will lay a good foundation for their future work and learning.
Topics and Schedule
Chemical Analysis Part (10 hrs total)
1. Description of Analytical Chemistry (0.25 hr)
Students should know: definition, classification, task and functions of analytical chemistry, and its evolution, present situation and perspectives.
2. Sample Collection and Preparation (0.25 hrs)
With this part, students should learn: collection methods and principles of solid/liquid/gaseous state samples, and their decomposition and dissolution ways, as well as the solution pretreatment before measurement.
3. Processing of Error and Analytical Data (8 hrs)
Students will learn: accuracy and precision, error and deviation, systemic error and random error, range/mean variation/standard deviation/standard deviation of average value, significant figure’ digit/rounding rules/operational rules, distribution regularity and interval probability of random error, confidence interval of average value, significance testing: U-test/t-test/F-test, test and choice of dubious value, reducing methods of measuring error: discovery and elimination of systemic error (control test, blank test, recovery test etc.) reduction of random error, introduction of unitary linear recursive analysis.
4. Quality control and Assurance of Analysis (0.5 hrs)
The significance of quality control and assurance as well as the principles and methods of it during the whole experiment process will be discussed.
5. Acid-base Equilibrium and Acid-base Titration (2 hrs)
5.1. Acid-base equilibrium
From this part, we will learn: activity and concentration, analytical concentration and equilibrium concentration, distribution fraction/diagram and predominance-area diagram of unitary/multiple acid-base, computing method of solution pH value, other important equilibrium in solution (mass balance, charge balance, proton condition). Buffering capacity and range of buffer solution, common buffer solution preparation, pH calculation of standard buffer solution.
5.2. Acid-base titration
We can know: the principle and range of indicator color change, influence factors of indicator color change range, common acid-base titration indicators and mixed acid-base indicators;
Strong/weak acid-base titration curve, criterion of unitary weak acid/base titration possibility, criterion of unitary strong acid/base and weak acid/base respective titration possibility, criterion of polybasic acid/base step-by-step titration possibility, select of kinds of indicators.
End point error calculation of strong/weak acid/base and polybasic acid/base titration, error function and its application.
Preparation and standardization of acid/base standard solution, influence of CO2 in acid/base titration, non-aqueous titration.
6. Complexometric Titration (2 hrs)
This part is mainly about: application of complexation in analytical chemistry, characteristics of EDTA and its application in titrimetric analysis.
Stability constant of complex, distribution of each complex existence forms in solution, side reaction coefficient of complexation, condition stability constant of complex.
Complexometric titration curve, metal indicator color change principle and color-turning point influence factors, common metal indicators, end point error function and its application.
The possibility of a single metal ion titration and the suitable pH range, Selective titration of mixed metal ions, the possibility of respective titration and acidity control, as well as the selective titration by masking agent.
Preparation and standardization of EDTA solution.
7. Redox Titration (1 hrs)
Students should learn: the conditional potential of redox reaction and the influencing factors of the conditional potential (effect of salt, acid, complexation and precipitation), the reaction constants and the extent of the reaction, the redox reaction process and the reaction rate, the affecting factors of the redox reaction rate.
Redox titration curves (stoichiometric point and titration jump); redox titration indicator (the type of indicator, the principle of color change and common indicator), calculation of the results of redox titration.
The principle, characteristics and application of typical redox titration: potassium permanganate method, potassium dichromate method, iodometry, acid potassium method, cerimetry.
8. Precipitation Titration and Gravimetric Analysis (1 hrs)
8.1. Precipitation titration
Argentometry titration curve, principles, characteristics and application of common precipitation titration, i.e. Mohr test, Volhard test, Fajans test, will be discussed.
Students will learn: the process, requirements of sediment types and weigh types, calculation of weigh coefficient and gravimetric analysis results.
Sediment solubility and intrinsic solubility, solubility product and conditional solubility product, influence factor of sediment solubility.
Sediment formation and types: sediment types, the formation of sediment (homogeneous nucleation and heterogeneous nucleation), Von Weimarn function and its application.
Influence factors of sediment purity: coprecipitation (adsorption coprecipitation, occlusional coprecipitation, mixed crystal), post-precipitation, influence of coprecipitation on analysis results, methods of reducing coprecipitation.
9. Absorption Spectrophotometry (2 hrs)
This part is about: basic properties of light and its application in analytical chemistry, generation and characteristics of visible light absorption spectrum. Basic theory of absorption spectrophotometry: Lambert-Beer law, additivity of absorbancy, definition and significance of absorptivity Sandell sensitivity, the cause of the deviation of Beer’s law.
Principles and structure of colorimetric and spectrophotometry instrument: visual colorimetric test, photoelectric colorimetry, and spectrophotometer. Measuring conditions selection measuring error of spectrophotometry: the influence of instrument measuring error on analysis results, the control of suitable adsorption range, the selection of incident wavelength and reference solution.
Chromogenic reaction and its influence factor: requirement of adsorption photometry on chromogenic reaction, the main influence factor of chromogenic reaction, the important chromogenic agent, multiple complex chromogenic system.
Absorption spectrophotometry in the application of quantitative analysis: working curve method, differential spectrophotometry method, multicomponent analysis, photometric titration method, the determination of complex composition and acid-base dissociation constants of organic reagents, the introduction of dual-wavelength spectrophotometry and derivative spectrophotometry.
10. Common Separation and Enrichment Methods in Analytical Chemistry （0.5 hrs）
We will talk about: the meaning of separation, the degree of separation and recovery, the classification of the separation method.
Precipitation separation: separation with inorganic precipitant, separation with organic precipitant, the separation and enrichment of coprecipitation.
Liquid-liquid extraction separation method: the nature of the solvent extraction, distribution coefficient and the ratio, the extracting rate and the extracting curve, chelate extraction equilibrium constant Kc and conditional extraction constant Kc.
The characteristics and the types of ion exchange separation, structure and performance of ion exchange resin, cation exchange separation, anion exchange separation, the affinity of ion exchange resin, a brief introduction of ion exchange chromatography.
The principle and classification of chromatography, paper chromatography, thin layer chromatography and column chromatography.
Other commonly used separation methods: liquid film method, flotation method, electrophoresis method, volatilization method and distillation etc.
Instrument Analysis Part (21 hrs total)
1. Introduction (0.5 hrs)
This part will talk about: the content, classification, characteristics, application scope and the status, function and development trend of the instrument analysis in the production and scientific research, instrumental analysis methods overview, analytical instruments overview, structural units, main performance indicators, analytical instruments and methods of calibration.
2. Introduction to Spectral Analysis (0.5 hrs)
Students will know: the basic characteristics of electromagnetic radiation, the mode of action between light and matter, the classification of the optical methods, the composition of the spectral method instrument.
3. Atomic Emission Spectrometry (1 hrs)
We will talk about: generation of atomic spectra, spectral properties and atomic structure, the light source, monochromator and detector of analysis instrument, the qualitative and quantitative methods.
4. Atomic Absorption and Atomic Fluorescence Spectrometry (0.5 hrs)
This part is about: absorption law, peak absorption coefficient and its measurement, quantitative method, atomic absorption spectrometer, interference and elimination method, advantages and disadvantages of atomic absorption spectrometry, atomic fluorescence spectrometry
5. X-ray Spectrometry (1 hrs)
Basic principle of X-ray, composition and working principle of analytical instrument, typical analysis method and its application will be discussed.
6. Mass Spectrometry (1 hrs)
This part is about: the principle of mass spectrometry, the main parts of the mass spectrometer, the main types of the sub peak, the important fragmentation rules, the pattern analysis rules, a brief introduction to the combination of chromatography and mass spectrometry, principle, structure and characteristic of atomic mass spectrometer, a brief introduction to ICPMS.
7. Surface Analysis Method (1 hrs)
In this part, we will talk about: principles, types and instruments of photoelectron spectroscopy; principles, instruments and application of the secondary ion mass spectrometry; a brief introduction to STM and AFM; the principle and application of near-field optics; principles, instruments and application of laser scanning confocal microscope.
8. Molecular Luminescence Analysis (2 hrs)
Students will learn: the generation of molecular fluorescence and phosphorescence, molecular de-excitation process, fluorescence quantum efficiency, fluorescence excitation spectrum, emission spectrum, Synchronous fluorescence spectra, three-dimensional fluorescence spectra, molecular fluorescence spectrometer, the application of molecular fluorescence spectroscopy, phosphorescence spectroscopy, the principle and application of chemiluminescence analysis.
10. Infrared Absorption Spectroscopy (1 hrs)
This part is about: the basic principle of infrared absorption, dispersive infrared spectrophotometer, Fourier transform infrared spectrometer, spectral characteristic absorption frequency and its relationship with molecular structure, Sample treatment, spectrum analysis method, quantitative analysis.
11. Laser Raman Spectroscopy (1 hrs)
Raman scattering, Raman shift, Raman spectrum, principle and application of Fourier transform Raman spectrometer will be introduced.
12. Nuclear Magnetic Resonance Spectroscopy (2 hrs)
In this part, we will learn: the spin and resonance of nucleus, relaxation phenomenon, nuclear magnetic resonance spectroscopy, the relationship between proton nuclear magnetic resonance spectroscopy and organic compound structure, analysis and application of nuclear magnetic resonance spectrum, 13C-nuclear magnetic resonance spectroscopy.
13. Introduction to electrical analysis （0.5 hrs）
This part is about: primary cell and electrolytic cell, electrode solution interface, the Nernst equation, the standard electrode potential and the condition potential， electrode type, Faraday's law and electrolysis current controlled by diffusion.
14. Potential Analysis Method (2 hrs)
We will know: the relationship between electrode potential and concentration, the response mechanism of glass electrode, the method of measuring pH value, ion selective electrode type and its characteristic parameter, quantitative method, ion meter, and potentiometric titration method.
15. Voltammetry and Polarography (2 hrs)
This part is about: voltammetry and polarography, polarography instruments, the particularity of electrode and electrolysis condition, the formation of the polarography wave, the polarography wave equation, diffusion current and interference current, quantitative method, brief introduction of modern methods such as single sweep polarography, cyclic voltammetry, stripping voltammetry, pulse polarography.
16. Electrolysis and Coulometry (0.5 hrs)
With this part, we will know: decomposition voltage and overvoltage, ion p order and complete degree, constant current and constant potential electrolysis and their device, Faraday's law,Constant potential coulometry analysis and coulometer, constant current coulometric titration and end-point indication method, characteristics and applications of Coulometry analysis.
17. New Method of Electro-analysis (0.5 hrs)
Students will learn: principles, types and applications of chemically modified electrodes, microelectrode properties and applications, brief introduction of typical nano electro-analytical chemistry, a brief introduction of combined electrochemical analysis technology.
18. An Introduction to Chromatography (0.5 hrs)
Basic concepts of chromatographic separation, plate theory, rate theory, separation degree and basic separation equation, qualitative analysis, quantitative analysis method will be introduced.
19. Gas Chromatography (2 hrs)
We will learn the structure and working principle of gas chromatograph, classification and characteristics of the detector, stationary phase and its selection, selection and optimization of separation conditions, typical analysis methods and applications.
20. High Performance Liquid Chromatography (1 hrs)
This introduces the production, development and characteristics of high performance liquid chromatography, the composition and working principle of the instrument, stationary phase and mobile phase, column effect, adsorption chromatography, partition chromatography, liquid solid chromatography, ion exchange chromatography and ion chromatography, size exclusion chromatography, micro diameter chromatography.
21. Capillary Electrophoresis and Capillary Electrochromatography (0.5 hrs)
The principle of electroosmotic flow, the influence factors of separation, the basic structure and working principle of the instrument, the principle of micellar electrokinetic capillary chromatography will be talked about.
22. Other Methods of Separation and Analysis (0.25 hrs)
We will introduce the principle of supercritical fluid chromatography and its characteristics, supercritical extraction, solid phase micro extraction, countercurrent chromatography, field flow chromatography, multidimensional chromatography.
24. Thermal Analysis (0.5 hrs)
Differential thermal analysis, differential scanning calorimetry, thermal gravimetric analysis, other thermal analysis will be introduced.
25. Flow Injection Analysis and Microfluidics Technology (0.5 hrs)
Students will learn the composition, principle and application of flow injection instrument; fabrication, drive and control of microfluidic chip; separation, mixing and reaction system; detector selection.
26. Analysis Instrument Measurement Circuit, Signal Processing and Computer Application Foundation (0.25 hrs)
Signal amplification and measurement, the application of computer in analytical instruments, the introduction of commonly used signal processing methods will be introduced,
Experimental Lessons Part
|No.||Content of courses||Hours Allocation||Distribution of class hours|
|Exp. 1||Simultaneous determination of chromium and cobalt in aqueous solution by UV Vis absorption spectroscopy||3||0.5||0.5||2|
|Exp. 2||Determination of ortho-hydroxybenzoic acid and ofm-hydroxybenzoic acid by fluorescence analysis||3||0.5||0.5||2|
|Exp. 3||The infrared absorption spectrum of benzoic acid||3||0.5||0.5||2|
Exp. 1 will be carried out after chapter 9 of chemistry analysis part, Exp. 2 will be after chapter 8 of instrumental analysis part, Exp. 3 will be after chapter 10 of instrumental analysis part.
|Content of courses||Class hours /hrs|
|Chemical Analysis Part||Total: 10|
|1. Description of Analytical Chemistry||0.25|
|2. Sample Collection and Preparation||0.25|
|3. Processing of Error and Analytical Data||8|
|4. Quality Control and Assurance of Analysis||0.5|
|5. Acid-base Equilibrium and Acid-base Titration||2|
|6. Complexometric Titration||2|
|7. Redox Titration||1|
|8. Precipitation Titration and Gravimetric Analysis||1|
|9. Absorption Spectrophotometry||2|
|10. Common Separation and Enrichment Methods in Analytical Chemistry||0.5|
|Instrument Analysis Part||Total: 21|
|2. Introduction to spectral analysis||0.5|
|3. Atomic Emission Spectrometry||1|
|4. Atomic Absorption and Atomic Fluorescence Spectrometry||0.5|
|5. X-ray Spectrometry||1|
|6. Mass Spectrometry||1|
|7. Surface Analysis Method||1|
|8. Molecular Luminescence Analysis||2|
|10. Infrared Absorption Spectroscopy||1|
|11. Laser Raman Spectroscopy||1|
|12. Nuclear Magnetic Resonance Spectroscopy||2|
|13. Introduction to Electrical Analysis||0.5|
|14. Potential Analysis Method||2|
|15. Voltammetry and Polarography||2|
|16. Electrolysis and Coulometry||0.5|
|17. New Method of Electro-analysis||0.5|
|18. An Introduction to Chromatography||0.5|
|19. Gas Chromatography||2|
|20. High Performance Liquid Chromatography||1|
|21. Capillary Electrophoresis and Capillary Electrochromatography||0.5|
|22. Other Methods of Separation and Analysis||0.25|
|24. Thermal Analysis||0.5|
|25. Flow Injection Analysis and Microfluidics Technology||0.5|
|26. Analysis Instrument Measurement Circuit, Signal Processing and Computer Application Foundation||0.25|
|Experiment Lessons Part||Total: 9|
|Exp. 1. Simultaneous determination of chromium and cobalt in aqueous solution by UV Vis absorption spectroscopy||3|
|Exp. 2. Determination of ortho-hydroxybenzoic acid and ofm-hydroxybenzoic acid by fluorescence analysis||3|
|Exp. 3. The infrared absorption spectrum of benzoic acid||3|
The homework and daily performance will be graded and the scores will count for 10% of the total, the experiment class will be graded and the scores will count for 10%, and the final examination will count for 80%.
The homework will be arranged every 4 hrs, 4 questions each at least. After each experiment, the experimental report should be handed in the next week, 3 copies in all. The final examination includes multiple-choice questions (40 points), short-answer questions (20 points), calculation questions (20 points), comprehensive analysis questions (20 points).
Wuhan University, Analytical Chemistry, Fifth Edition, 2 Volumes, Beijing: Higher Education Press (Chinese Version).
 Li Kean. Analytical chemistry course. Beijing: Peking University press, 2005 (Chinese version)
 Lin Shuchang, Hu. Analytical chemistry: chemical analysis part [M]. higher education press, 1993
 Shengcaikaoyan, Notes and Exercises Detailed Explanation of Wuhan University (5th edition), 2 Volumes, China Petrochemical Press.