MS731M: Chemical Analysis of Materials
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1 (Revised) Course Code and Title Course Coordinator Details of Course MS731M: Chemical Analysis of Materials Dr. Eileen Fong (Course Coordinator) Dr. Thresen Matthew Rationale for introducing this course This course will cover the subject of chemical analysis of materials. Chemical analysis of materials is wherein the composition and chemical information of various materials and properties are probed and measured. It is a fundamental process in the field of materials science, without which no scientific understanding of engineering materials could be ascertained. This course will focus specifically on different spectroscopic and spectrometric analytical techniques for chemical analysis of materials It will cover surface chemical analysis to bulk chemical analysis of materials. Aims and objectives At the end of this course the students will be able to Describe the working principles of UV-VIS, IR, XRF, XPS and MS, Analyse data acquired from each of the analytical techniques Recommend suitable techniques for evaluating material properties with clear justifications. Integrate information from multiple datasets to make deductions about material properties Course Syllabus Refer to page 3 to 5 Assessment (Individual Assessment) Assessment Points 7 Mode of Assessments and weighting 3 x Tutorials CA1: MCQs CA2: MCQs CA3: Final Quiz (Written) Research paper critique: peer review 15% 25% 100% 1
2 Mapping of assessment to course objectives LO1. Describe the working principles of UV-VIS, IR, XRF, XPS and MS LO2. Analyse data acquired from each of the analytical techniques LO3. Recommend suitable techniques for evaluating material properties with clear justifications. LO4. Integrate information from multiple datasets to make deductions about material properties CA1 : LO1, LO2, LO3, LO4 CA2 : LO1, LO2, LO3, LO4 Final Quiz : LO1, LO2, LO3, LO4 Peer review: LO2, LO3 and LO4 To be offered with effect from (state Academic Year and Semester) Cross Listing (if Prerequisites (if Preclusions (if Mode of Teaching & Learning (Lectures, regular tests, Q&A, problembased learning) Basic Reading List Compulsory Reading - NIL Supplementary Reading Hours of Contact/Academic Units AY2018/19 Semester 1 Lectures, Regular tests, Q&A Supplementary Reading 1. Foundations of Spectroscopy, Duckett and Gilbert (Oxford Science Publications) 2. Organic Spectroscopic Analysis, Anderson, Bendell and Groundwater (Royal Society of Chemistry) 3. Mass Spectrometry A text book 2017 by Jürgen H. Gross Cham, Switzerland: Springer, (Ebook from NTU Library) 4. A beginner s guide to Mass Spectral Interpretation by Terrence A. Lee, 2003 John Wiley & Sons, Ltd 5. MASS SPECTROMETRY: Instrumentation, Interpretation, and Applications by Rolf Ekman, Jerzy Silberring, Ann Westman- Brinkmalm and Agnieszka Kraj, 2009 John Wiley & Sons, Ltd 39 hours/ 3 AUs 2
3 Course Syllabus The following topics will be covered: MODULE 1: Infrared and UV Vis Spectroscopy 1. Introduction to Spectroscopy -Electromagnetic waves and their use in spectroscopy. -Types of Spectroscopy. 2. Introduction to Infrared Spectroscopy -Infrared spectrometry -Infrared spectrometer -infrared spectrum. 3. Molecular Vibrations due to IR -Absorption of IR -Possible types of vibration motion due to increased energy. -Degrees of freedom, -Bands in IR Spectra 4. Characteristics of an IR Spectrum -Motions detectable by IR Spectroscopy, -Characteristics of IR Spectra 5. Applications of IR Spectroscopy -How to analyse IR spectra. -Applications of IR Spectroscopy in food science, -Pharmaceuticals -Agricultural and environmental studies. 6. Principles of UV-Vis Spectroscopy -Electronic Transitions, -Absorbance -UV-Vis Spectrometers. 7. Electronic transitions in molecules -Absorption of UV-Vis -Transition metals and their electronic configurations, -Ligand field theory, -d-d transitions. 8. Analysis of UV-Vis Spectrum -UV-Vis Spectra -Qualitative analysis of UV-Vis Spectra. 9. Applications of UV-Vis -Food safety -Healthcare -Chemistry -Materials science -Manufacturing MODULE 2: X-ray Fluorescence and Photoelectron Spectroscopy 1. Introduction to XRF -Principles of X-ray fluorescence, -Uses of X-rays 3
4 -X-ray Sources -Detectors and collimators. 2. Fluorescence due to X-rays. -Electron shells -Binding energy versus potential energy -Emission of K and L lines -Auger Emissions -Fluorescent yield. 3. Analysis applications of XRF -Bremsstrahlung -Rayleigh Scattering -Compton scattering -Industries that use XRF 4. Introduction to X-ray Photoelectron Spectroscopy (XPS) -Discovery of XPS -X-ray Sources -Electron energy Analyser -Ultra high vacuum. 5. Photoemission Process in XPS -Energy level diagram, -Factors influencing binding energy -Attraction of electrons to nucleus 6. Characteristics of XPS Spectra Part 1 -Photoelectron peaks -Auger peaks -Auger process -Spin orbital splitting 7. Characteristics of XPS Spectra Part 2 -Background of XPS -Adventitious Carbon -Surface charging 8. Data analysis in XPS. -Quantitative analysis -Chemical analysis -Examples of data analysis 9. Applications of XPS -Biological analysis -Materials synthesis and characterization -Composition and failure analysis -Depth profiling 10. Multi-technique Analyses: Examples -Summary and Case studies MODULE 3: Mass Spectrometry 1. Overview -What is Mass Spectrometry? -A brief history of Mass Spectrometry 4
5 -When to use Mass spectrometry 2. Key concepts of Mass Spectrometry -Molecular mass -Isotopes and isotopic distribution -Mass resolution -The nitrogen rule 3. Principles of Hard Ionisation -Electron ionisation (EI) -Fragmentations in MS -α-bond cleavage -double α-bond cleavage -Benzylic bond cleavage -Allylic bond cleavage -McLafferty rearrangement -Double Bond Equivalents 4. Principles of Soft Ionisation Part 1 -Vacuum Chemical Ionisation (CI) -Atmospheric Pressure Chemical Ionisation (APCI) -Atmospheric Pressure Photoionisation (APPI) 5. Principles of Soft Ionization Part 2 -Electrospray Ionisation (ESI) -Multiple charge states and Charge deconvolution -Analyte Acceptance of ESI 6. Principles of Soft Ionisation Part 3 -Matrix Assisted Laser Desorption Ionisation (MALDI) -Sample Target and Sample Spot -Matrix selection -Fast Atom Bombardment (FAB) ionisation 7. Instrumentation of Mass Spectrometry Basic Components of Modern MS Working principles of major Mass Analysers -Magnetic Sector Mass Analyser -Quadrupole Mass Analyser -Time of Flight Mass Analyser -Ion trap Mass Analyser -Tandem (Hybrid) Mass Spectrometry 8. Applications of MS -Qualitative MS Analysis in Proteomics -Qualitative analysis of Polymers -Quantitative Applications of MS -MRM file and calibration curve generation -Imaging Applications of MS -Case study 9. Summary 5
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