This course first offers an introduction to sampling, error and statistical analysis as applied to analytical chemistry. Specific analytical techniques or concepts covered are: gravimetric and volumetric analyses, aqueous solution equilibrium principally involving complexation equilibria, spectrophotometric analysis, electrochemical methods, atomic spectroscopy, and chromatographic methods. These topics will be covered from the point of view of theory, the associated analytical instrumentation and relevant computational methods. The experimental application of this material will be covered in the laboratory experiments (see below)
- The concepts of sampling, experimental error, precision, accuracy (introduced in earlier courses) will be expanded upon.
- The concepts of statistical analysis and calibration as applied to analytical chemistry will be introduced.
- Gravimetric and volumetric techniques of analysis will be briefly reviewed.
- The quantitative principles of solution equilibria as applied to metal-ligand complexes will be explored in some detail and applications to complexometric titrations examined.
- The principles of spectrophotometric analysis will be introduced and their practical application explored.
- Electrochemical methods (e.g. potentiometry, coulometry, voltammetry) will be introduced, both from the point of view of theory and the associated instrumentation.
- The principles of atomic spectroscopy will be introduced and the associated instrumentation examined.
- The basic principles of chromatography will be introduced and the associated instrumentation examined; the focus will be on gas-liquid chromatography and high pressure liquid chromatography.
A selection (approximately 10) of the following experiments will be performed in the laboratory period.
- Statistics in Analytical Chemistry
- Aqueous Chemical Equilibria – A Detailed Investigation
- Detection of Fuel Components of Gas Chromatography
- Complexometric Titrations
- Potentiometry – Ion Selective Electrodes
- Spectrophotometric Determination of Maganese and Chromium in a Mixture
- Determination of Copper Using Flame Atomic Absorption Spectrometry
- Separation and Identification of Fatty Acids in Commercial Oil Using Gas Chromatography
- Soil Sample Extraction and Analysis for Magnesium and Calcium
- Separation of compounds using high pressure liquid chromatography (HPLC)
- Caffeine Analysis in Beverages by HPLC
- Determination of Iron in Cereal by Atomic Absorption
- Detection of Petroleum Contaminants by Capillary Gas Chromatography
- Determination of Trace Metals in Human Hair by Atomic Absorption
- Analysis of Capsaicinoids by Reversed Phase HPLC
Methods Of Instruction
Lectures, problem-solving sessions and class discussion will be the major methods of instruction in this course. A variety of audio-visual aids and pre-programmed material (as appropriate) will also be used. Problems will be assigned on a regular basis; these will be handed in and evaluated. The laboratory portion of this course will be closely coordinated with the lecture portion of this course and used to illustrate the theoretical and practical material associated with common analytical chemistry techniques.
Means of Assessment
Lecture Material (70%)
- Two term tests will be given during the semester (20-25%)
- A final comprehensive examination to be given during the final exam period (30%)
- Any or all of the following evaluations, at the discretion of the instructor: problem assignments, quizzes, projects, class participation [5% maximum] (15-20% in total)
- Ten experiments will be performed during the semester and the grade for this portion of the course will be based on (a) the accuracy of the results and/or (b) the written report for each experiment.
A student who misses three or more laboratory experiments will earn a maximum P grade.
A student who achieves less than 50% in either the lecture or laboratory portion of the course will earn a maximum P grade.
Upon completion of this course, the students will:
- Apply the concepts of precision, accuracy and statistical analysis to a variety of chemical analytical techniques
- Understand the concepts of gravimetric and volumetric analysis and apply them to a wide variety of problems in analytical chemistry
- Understand the quantitative principles of aqueous solution equilibria as applied to metal-ligand complexes and carry out detailed calculations on these systems.
- Understand the basic theory behind various spectrophotometric techniques, produce a block diagram of the associated instrumentation for each and discuss the purpose of each block plus describe the practial considerations appropriate for the application of each method to typical chemical analyses (e.g. sensitivity, detection limits, linear response ranges, interferences, etc).
- Understand the basic theory behind various electrochemical techniques, such as potentiometry, coulometry and voltammetry.
- Produce a block diagram of the associated instrumentation for each of these electrochemical techniques and discuss the purpose of each block plus describe the practical considerations appropriate for each method (e.g. sensitivity, detection limits, interferences, etc.).
- Understand the basic theory behind atomic spectroscopy, produce a block diagram of instrumentation for both emission and absorption modes (flame and graphite furnace) and discuss the purpose and important considerations for each block.
- Discuss the practical considerations appropriate for the application of these methods to typical chemical analyses (e.g. sensitivity, detection limits, linear response ranges, interferences, etc.)
- Understand the basic principles associated with chromatography and discuss how these are applied to the various specific applications of chromatography (e.g. solid-liquid, gas-liquid, HPLC, SFC, etc).
- Produce a block diagram of the associated instrumentation for each of these applications and discuss the purpose and limitations associated with each block.
- For each method, describe a typical sample that might be separated by this method and discuss the appropriate practical considerations (sensitivity, detection limits, interferences, band broadening mechanisms, repeatability, etc.)
Textbooks and Materials to be Purchased by Students
Harris, D.C., Quantitative Chemical Analysis, 6th Edition, 2002