GCMS sampler LCTOF

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Content & What to Expect

Material Covered & Syllabus

Textbook & Materials Required

Analytical Chemistry (Chem 333, 3 credits) is typically taught in a fall semester and requires lab Chem 333L (1 credit) as a co-requisite. The value of analytical chemistry is in a wide range of applications. Various disciplines require information on the composition of the samples. This knowledge is for example needed in medical, environmental, forensic sciences as well as engineering fields. Even though, students who are taking this course will not perform the analysis in the future profession herself/himself. The understanding of the analytical methods is mandatory for the data interpretation, and the evaluation of the error of the method.

Who cares about data interpretation and errors? Imagine in medical field, the doctor will receive two lab results of 0.31 and 0.29, knowing that 0.30 is the threshold value. Thus, the doctor may conclude that patient with 0.31 has problem and needs a treatment while the second patient does not. However with analytical knowledge, the doctor also knows that error of the particular methods is 0.03. Therefore, he or she knows there is not really difference between results of those two patients and further follow-ups or tests are required.

In order to get strong understanding of analytical methods used, student will first review some sections of general chemistry such as stochiometry, units of concentrations, titration, pH determination, equilibria. Students will also learn basics of statistical data evaluation, determination of error, and use of significant figures. This will be followed by specialized topics on electrochemistry, spectroscopy, chromatography and mass spectrometry, and also including sample preparation. It is important to understand that this class covers wide variety topics within one semester. To accomplish this course student need to take lab Chem 333L simultaneously. As this course is a junior (advanced) level, students need to expect that this implies also higher expectation in the laboratory. This may be seen in requirements on the accuracy and precision of the results as well as writing the reports.

Why accuracy? Consider the importance of accuracy on the following example: Analytical chemist would tell you that concentration of fluoride in your drinking water is 1 ppm (parts per million) which is currently level of fluoride recommended by EPA helping to prevent tooth decay. After few years you will find out there was an error in the accuracy and that actual concentration was 3 ppm (seemingly still very low), but causing particularly for children fluorosis – permanent alterations in teeth coloring.

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Analytical terminology - qualitative, quantitative, units

Measurements tools & Statistics – accuracy, precision, error, deviation, significant digits, t-test, outliers, confidence int., P value

Chemical equilibrium - review of general chemistry & constants K, Ksp, Ka, Kb, Kw, pH, solubility, neutralization, pKa, buffers

Titration & Acid-base equilibrium, indicators

Electrochemistry fundamentals – Oxidation/reduction, Nernst equation, potentials, pH electrode, electrodes, instrumental methods

Spectrophotometry – molecular, absorption/emission AAS, AES, instruments

Chromatography – separation, quantification, GC - injectors, columns, detectors, HPLC, IC

Sample Preparation

Mass Spectrometry – ionization, analyzer, instrumentation, interpretation

 

Syllabus

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Quantitative Chemical Analysis textbook 8th edition By Daniel C. Harris

ISBN: 1-4292-1815-0, ISBN-13: 978-1-429-21815-3

RF Turning Point Clicker

Calculator (capable of exponential function, none programmable) will be required for lecture, assignments and exams.

Materials for Chem 333L:

Laboratory Exercise Chemistry 333, 2010 edition A. Kubatova, UND

Safety goggles, paper towels, calculator, laboratory notebook

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Chromatography and Mass spectrometry are considered to be most frequently used analytical techniques. However, as a number of users increases the quality and understanding may decline. This course will cover theory as well as the practical training in chromatographic techniques including also fundamentals of mass spectrometric detection. This course is taught in two levels for undergraduate (Chem 443) and graduate (Chem 543) students in biannual bases (Fall 2011). In both levels fundamentals will be covered/reviewed and expanded with the instrumental details. The graduate level will be significantly extended with regards to the depth of topics covered and theoretical background. To enhance interaction and active learning there will be special assignments within this class including article presentations. Since the analytical chemistry is a practical science requiring hands on experience, there will also be two lab assignments, in which students will individually perform practical measurements and demonstrate their understanding on applied examples.

Fundamental concepts and theory of chromatography

Achieving optimal separation - Rate theory

Gas Chromatography

Liquid Chromatography

Quantitation & Detectors

Mass spectrometry: Ionization sources, Mass Analyzers, Basics of MS interpretation

Hyphenated techniques GC/MS, LC/MS

Sample preparation - Extraction

Undergraduate Instrumental Analysis, Sixth Ed.by James W. Robinson, Eileen M. Skelly Frame, George M. Frame II, CRC press, ISBN-10: 0824753593, ISBN-13: 978-0824753597

Practical HPLC method development by L.R. Snyder, J.J. Kirkland, J.L. Glajch, Wiley Interscience, ISBN 0-471-00703-X

Modern Practice of Gas Chromatography R.L. Grob, E.F Barry, Wiley Interscience, ISBN 0417-22983-0

Split and splitless injection for quantitative gas chromatography concepts, processes, practical guidelines, sources of error, K. Grob, Weinheim, New York : Wiley-VCH, 2001, 4th ed., ISBN 3527298797

Interpretation of mass spectra, F.W. McLafferty, František Tureček, 4th ed, Mill Valley, Calif. : University Science Books, IBSN 0935702253

Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent Stroobant, 2nd ed, Chichester, England ; Hoboken, NJ : J. Wiley, IBSN 0471485659.

Mass spectrometry : principles and applications, Edmond de Hoffmann, Vincent Stroobant, 3rd ed, Chichester, England ; Hoboken, NJ : J. Wiley, IBSN 9780470033104.

Sampling and sample preparation for field and laboratory, ed. J. Pawliszyn, Comprehensive Analytical Chemistry ed. D. Barcelo, Elsevier, ISBN: 0-444-50511-3

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Last updated February 2012 | Chemistry Department | University of North Dakota |