‘Analytical Chemistry Part I’Course Syllabus
Course Category：Major Basic
Total Hours：72 Hours Credit：3
Lecture Hours：72 Hours
Na Li, John J. Hefferren. Ke'an Li《Quantitative Chemical Analysis》,Beijing University Press, 2009, 1st edition
Douglas A. Skoog, F. James Holler, Stanley R. Crouch, Principle 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 1 Introduction on Analytical Chemistry
1.1 The definition of analytical chemistry, function
Teaching Outline: Classification and Nomenclature, the aim, the function of analytical chemistry
1.1 The history and recent development
Teaching Outline: recent development; definition of on-line, real-time and in-vivo; gravimetry, titrimetry
1.2 Quantitative and qualitative analysis
Teaching Outline: Quantitative analysis; qualitative analysis; macro, micro, trace, and ultra-trace analysis
1.3 Introduction on titration analysis
Teaching Outline: titrimetry; standard solution; stoichiometric point, end point; classification of titrimetry; direct titration, back titration, replacement titration, indirect titration; calculations in titrimetry
1.4 Sample collection and pretreatment
Teaching Outline: preparation of inorganic samples; sample collection; dry ashing, wet ashing, microwave digestion
1. What does a primary substance mean? What are the general requirements on primary substances?
2. List at least three examples of application of analytical techniques you have used.
2.1 Errors in analytical chemistry
Teaching Outline: Systematic errors, random errors, precision and accuracy, deviation and error, average deviation and standard deviation, mean,
2.2 Distribution of random errors
Teaching Outline: distribution of random error, the Gaussian curves, areas under a Gaussian curve, standard error of the mean, confidence intervals,
2.3 Statistic of limited data
Teaching Outline: T distribution; compare a mean with a true value (t test); compare two precisions (F test); comparing two means (u test)
2.4 Methods for the improvement of accuracy
Teaching Outline: selection of analytical methods, elimination of systematic errors
2.5 Regression equation
Teaching Outline: regression equation, correlation coefficient
2.6 significant figures
Teaching Outline: significant figures, rounding rules
1. What do accuracy and precision mean?
2. How to tell whether a suspicious data in a data set should be retained or rejected?
3. Does a high confidence level always favorable in the determination a confidence interval, why?
Chapter 3 Acid-base Equilibriums and Acid-Base Titrations
3.1 Acid-base titration in aqueous solutions
Teaching Outline: Acid-base theories, dissociation constant, concentration, activity and activity coefficient
3.2 Distribution of various forms in acid-base solution
Teaching Outline: analytical concentration and equilibrium concentration, influence of acidity on the forms in acid-base solution , distribution fractions
3.3 calculation of pH
Teaching Outline: proton balance equation, calculation of various solutions, strong acids or bases, weak acids or bases, monoprotic acid, polyprotic acid
3.4 Buffer solution for acid-base pairs
Teaching Outline: buffer capacity, calculation of pH value of buffer solutions, common buffer solutions and their preparations
3.5 Acid-base indicators
Teaching Outline: working mechanism of indicators, common indicators and their transition range, mixed indicators
3.6 acid-base titration
Teaching Outline: titration curves; the end point break; titration in strong acid (base), polyprotic acids and mixtures; selection of indicators; titration error and the calculations
3.7 application of acid-base titration
Teaching Outline: preparation of standard solutions and their calibration; influence of carbon dioxide in titration; application of acid-base titration: titration of boric acid, Kjeldahl method for nitrogen determination
1. What does a dissociation constant mean?
2. What does a buffer solution mean? Give the details on how to prepare a pH 7.0 phosphate buffer (100mM).
3. How does a titration error occur in an acid-base titration? How can we calculate this error?
Chapter 4 Complexometric Titration
4.1 Introduction on complexometric titration
Teaching Outline: complexometry in analytical chemistry, property of EDTA and its application in complexometric titration
4.2 Complexometric equilibriums
Teaching Outline: stability (formation) constant, dissociation constant; distribution of various formations in aqueous solution; metal ion buffers
4.3 Conditional formation constant
Teaching Outline: side reactions; side reaction coefficient; conditional formation constant, acidic effect coefficient
4.4 Metal ion indicators,
Teaching Outline: working principle of metal ion indicators; transition point, selection of metal ion indicators; commonly used metal ion indicators
4.5 Basic principles for complexometric titration
Teaching Outline: titration curve and change of concentration during the titration process; factors influence the end point break; the titration error and its calculations
4.6 Acidity control in complexometric titration
Teaching Outline: feasibility of titration in a single metal ion solution; control of acidity single metal ion titration; the highest, the lowest and the best acidity; feasibility of titration test in multi-ion solutions
4.7 Methods for the improvement of selectivity in complexometric titration
Teaching Outline: control the acidity; masking agent and demasking agent
4.8 Application of complexometric titration
Teaching Outline: direct titration, indirect titration, back titration and displacement titration; masking; preparation and calibration of EDTA standard
1. What does conditional formation constant mean?
2. Why sometimes back titrations or indirect titrations should be used in complexometric titrations. Give at least one on each type.
3. How does an indicator work in a complexometric titration?
Chapter 5 Oxidation-reduction Titration
5.1 Redox equilibriums
Teaching Outline: formal potentials; ionic strength effect, side reaction effect; acidity effect; rate of redox reactions, self-catalyzed reaction and induced reaction
5.2 Redox titration
Teaching Outline: redox titration curve; end-point potential; redox indicators; commonly used indicators; pre-adjustment: pre-oxidation
5.3 Application of redox titration
Teaching Outline: potassium permanganate method; potassium dichromate; starch-iodine method, iodimetry (direct) and iodometry (indirect), use of starch indicator
1. What does formal potential mean?
2. What is a self-indicator? Given one example.
3. How to prepare standard solutions of KMnO4 and Na2S2O3?
4. What are the differences between iodometry and iodimetry?
Chapter 6 Precipitation titration
Teaching Outline: Precipitation reaction, principles and applications of Mohr titration, Volhard titration and Fajans titration
1. List the typical examples of argentometry. What are the indicators used in these methods?
2. Why sometimes a blank titration is required? Give one example.
Chapter 7 Gravimetry
Teaching Outline: classification of gravimetry, procedure of gravimetric analysis; requirement on the precipitation form
7.2 solubility of precipitation
Teaching Outline: solubility and intrinsic solubility; activity product, solubility product and conditional solubility product; common ion effect, salt effect, acid effect, complexometric effect and other factors influence the solubility
7.3 formation of precipitations
Teaching Outline: Classification of precipitations, crystalline precipitation and amorphous precipitation; Homogeneous and heterogeneous nucleation
7.4 Main factors influence the purity of precipitation
Teaching Outline: Coprecipitation, adsorption co precipitation, occlusion and inclusion; post precipitation
7.5 Conditions for precipitation and post treatment
Teaching Outline: Requirements for crystalline precipitation, amorphous precipitation; aging; homogeneous precipitation
7.6 Organic precipitation agents
Teaching Outline: Classification and commonly used organic precipitation agents
1. With continuous introduction of chloride into an AgNO3 solution, a U-shaped solubility curve is obtained toward silver, try explain this.
2. Why controlling pH sometimes is important for obtaining a good precipitate?
3. What is a homogeneous precipitation and what are the advantages of this method?
Chapter 8 Separation Techniques in Analytical Chemistry
Teaching Outline: Separation and classification, recovery
Teaching Outline: Inorganic precipitate, organic precipitate; separation and enrichment of co-precipitation
8.3 Liquid-liquid extraction
Teaching Outline: Essence of extraction, distribution constant and distribution ratio; efficiency of extraction, classification of extraction; requirements
8.4 Ion-exchange for separation
Teaching Outline: ion-exchange resin, properties and ion-exchange reactions; affinity; operations in ion-exchange; ion-exchange chromatography
8.5 chromatographic methods
Teaching Outline: Principle on chromatographic separation, classification; paper, thin-layer and column chromatography
8.6 other techniques for separation
1. List at least three methods for separation based on the differences on sizes.
2. Why continuous extraction is more powerful as compared with regular one?
3. How does a TLC work?
Chapter 9 introduction on Electrochemical Analysis
Teaching Outline: Classification of electrochemical methods, their applications
Electrochemical cells, potential, classification of cells, Cottrell equation, Farady’s law
Introduction on conductivity analysis
1. What do static methods and dynamic methods mean in electrochemical analyses?
2. What are the differences between an electrolytical cell and a galvanic cell?
Chapter 10 Pontentiometry
10.1 Basic principles
Teaching Outline: Electrode potential and its relation with concentration, calomel electrode, electrodes of the first, second and third kind
10.2 ion-selective electrodes
Teaching Outline: Glass electrode, single crystal electrode, polycrystalline or mixed crystal electrode, membrane electrode, membrane potentials and boundary potentials; Nernst equation; selectivity coefficients
10.3 Application of ion-selective electrodes
Teaching Outline: Method for the detection of ion activity; definition and measurement of pH
10.4 Potentiometric titrations
Teaching Outline: Types of potentiometric titration, working electrode; automatic potentiometric titrator
1. What is a potentiometric titration? What are differences between a potentiometric titration and a regular one?
2. What do SHE and SCE mean in electrochemical analysis? Which one is more popular in these two?
Chapter 11 Coulometry
11.1 Basic principles
Teaching Outline: Applied potential and overpontential, influence of the solution component on electrolysis potential
11.2 Electricity gravimetric method
Teaching Outline: Potentiostats; requirement for a quantitative electrolysis; application of Electricity gravimetric method
Teaching Outline: Farady’s law, controlled-potential Coulometry; controlled-potential Coulometric titration; Automatic Coulometer
1. What does coulometric titration mean?
2. What does electrogravimetry mean?
Chapter 12 Polarography and Voltammetry
12.1 basic principles
Teaching Outline: Basic process of polarography and the setup; dropping mercury electrodes and solid electrodes; E-i curve;
12.2 Polarographic current
Teaching Outline: Diffusion current and diffusion current equation; half-wave potential
12.3 Application of polarography
Teaching Outline: quantitative and qualitative method for polarography, application of polarography
Teaching Outline: excitation signals in voltammetry; voltammetric instrumentation; hydrodynamic voltametry; cyclic and pulse voltammetry; application of voltametry and the stripping methods
1. What does the half-wave potential mean in the voltammogram? What is its relationship with the redox reaction
2. What does the limiting current mean in the voltammogram? How is this one related to the quantity of the species.
3. What does amperometry mean?
Exams (final 50%, mid 20%), Quizzes (20%), Assignments (10%)
Made by Jilin Yan
Date 10.28. 2016