Chemistry 321: Instrumental Analytical Chemistry Course Details Professor: Richard Oleschuk Room: Dunning Hall Phone: 533-6704 Email: [email protected] Location: 213 Chernoff Hall Textbook(s): Preferred: Quantitative Chemical Analysis, 8th edition, Daniel C. Harris Also Ok: Quantitative Chemical Analysis, 7th edition, Daniel C. Harris Website: http://www.chem.queensu.ca/Courses/13/CHE M321.asp Evaluation Midterm 30% Report 20% Final Exam 50% Two problem sets: Un-marked but answers provided Practice questions assigned after each chapter Midterm in class: February 12th
Exams will be closed book but equations will be provided! Office Hours: Wednesday 1:00-2:30 PM, others available upon request Dean’s Note: • Students who feel that there are reasons to review their grades should follow the steps set out in Regulation 13, “Review and Appeal of Grades”. • Academic Dishonesty • The Senate document on Academic Dishonesty states that "Plagiarism means presenting work done (in whole or in part) by someone else as if it were one's own." Plagiarized work could result in an automatic failure in any Chemistry course and a subsequent request to withdraw from the program. Students should consult the Senate document (http://www.queensu.ca/secretariat/senate/policies/acaddish.html) or talk to the course instructor when in doubt about how best to refer to the work of others. • For the most recent version of Academic Regulation 12 (Academic Integrity), please check the web at www.queensu.ca/calendars/artsci. • Calculators for exams (Academic Regulation 9): • Calculators acceptable for use during quizzes, tests and examinations are intended to support the basic calculating functions required by most Arts and Science courses. For this purpose, the use of the Casio 991 series calculator is permitted. Students may also use calculators with a Gold Applied Science approval sticker or a Blue Commerce approval sticker as they are considered to be comparable to the Casio 991. Calculators with advanced features or substantial text storage capacity are not permitted unless otherwise approved by the instructor. Communicating calculators are banned. http://www.queensu.ca/calendars/artsci/pg529.html Detailed Course Outline (Topics/Chapters Covered) • 1.) Introduction to Chromatography Liquid-Liquid Extraction, Partition Coefficient TLC, Resolution, Van Deemter Equation, Sources of Band Broadening, Selectivity Factor, Capacity Factor, Theoretical plates, Qualitative and Quantitative Analysis.
• 2.) Gas Chromatography: Injectors, Split, Splitless and on-column injection, Silanization, Columns, Packed vs. Capillary, Common stationary phases, Classification of Stationary Phases, Kovats Retention Index, McReynolds Constants, Temperature Programming, Detectors, ECD, FID, TCD, Mass Spectrometry, Library matching EI spectra. GC sample Prep., Purge and Trap, Solid Phase Micro-extraction, Headspace sampling.
• 3.) HPLC: Instrument Components: injectors, high pressure pumps, solvent gradients, guard columns, analytical columns, common stationary phases (reversed and normal phase, bonded, coated, pellicular), elutropic series, detectors, UV-Vis, Fluorescence, Refractive Index, APCI, Electrospray, Selected Ion Monitoring, Light Scattering, developing and optimizing an HPLC separation. Detailed Course Outline (Topics/Chapters Covered) continued
4.) Ion Chromatography, GPC, Capillary Electrophoresis: Types of exchange resins(anion, cation, cross-linking, functional groups), principals of separation, pH gradients, conductivity detector, suppressor columns. GPC molecular weight determination, size exclusion resins, total inclusion vs. total exclusion. Electrophoresis,Gel, capillary electrophoresis, Electrophoretic Mobility, Electroosmotic Flow, Electrokinetic, injection methods, Detection, MEKC, CEC.
5.) Mass Spectrometry: Ionization Methods, Electron Impact (EI), Chemical Ionization (CI), Atmospheric Chemical Ionization (APCI), Electrospray Ionization(ESI), Matrix Assisted Laser Desorption Ionization (MALDI), Desorption Electrospray Ionization, Magnetic Sector Instruments, Quadrupole Instruments, Ion Trap Instruments, Time of Flight Instruments, Orbitrap Instruments. Ion Detectors
6.) Electrochemical Methods of Analysis: pH electrode, selective ion electrode, Electrogravimetric and Coulometric Analysis, Voltametry, Diffusion Current, Polarography, Anodic Stripping, Chem 321 Report
Guidelines Due Noon Friday March 18th, 2016 • Write a report of no less than 7 and no more than 10 typed pages (figures included). Use 12-point font, 1" margins, and at least 1.5 spacing throughout. The topic of your report can be either one of those listed below or another with my approval. Your report should have a short abstract on the first page, with an absolute upper limit of 75 words. The report should contain a detailed introduction and description of your chosen analytical method or application. Further items to be discussed in your paper may include types of compounds analyzed, detection limits, chemical information obtained, sample preparation, instrument types and parameters etc. References should conform to normal conventions by number markings in the text, thus1; or the author’s name and date of publication in parentheses (SMITH, 2008). Copying the work of another writer into your own work without acknowledgment constitutes plagiarism and will not be tolerated (see course details). Please turn in your completed report to my office, 305 Chernoff Hall (under door if I am not there) by noon Friday March 18th, 2016. (You can hand it in early, but you cannot be late). Late reports are subject to a 15 % /day late penalty. Student is required to submit both a paper and electronic version of their report.
• Detailed list of topics and more complete instructions will be posted on Moodle. Some Examples of Report Topics…
Porous polymer monoliths stationary phases for biomolecular Detection and Analysis of Pharmaceuticals in Drinking separation Water in Canada Superparamagentic particle based-cell sorting Single DNA Molecule Sequencing DESI-mass spectrometry for imaging (tissue?) High Throughput Screening of Pharmaceutical NextGen DNA Sequencing Compounds Ultra fast separations using microfluidic devices Authenticity Analysis of Scotch, Whiskey or Wine Immunoassay for low cost environmental analysis Molecularly Imprinted Polymers for Chemical Analytical Chemistry: Challenges for Personalized Medicine Separation DESI – a Star Trek Tricorder? Magnetic Methods for Chemical Fluorescence Resonance Energy Transfer (FRET) in Sensing Separation/Identification Applications “Greener” Analytical Chemistry Methods Detecting Circulating Tumor Cells using microfluidic devices and Single Molecule Detection methods other traditional techniques Single Cell Analysis- Is it useful? X-ray fluorescence for the detection of fine art forgeries Nanopore Sensing Applications Analytical instrumentation on the Mars Landers Surface Plasmon Resonance for Examining Detecting Ecoli O157 Biomolecular Interactions Digital Microfluidics for Multiplexed Analytical Chemistry Microfluidic methods employing magnetic beads Applications Mass Spectrometry methods for metabolomics and Nanoelectrospray Ionization- benefits and challenges lipidomics The analysis of asphaltenes in crude oil using high res chromatography, mass spectrometry and NMR Paper based microfluidic devices as low cost analytical Effectiveness of online products to beat drug tests platforms Gold Nanoparticles in Analytical Chemistry Chiral Separations Large and Small Scale for Patient Health Assessment through Saliva Analysis Pharmaceutical purification Gold Nanoparticles in Analytical Chemistry Patient Health Assessment through Saliva Analysis Chapter 22: Introduction to Chemical Separations
IUPAC Definition of Separation: Separation is the hypothetical condition where there is complete isolation, by m separate macroscopic regions, of each of the m chemical components which comprise a mixture. In other words, the goal of any separation process is to isolate the m chemical components, in their pure forms, into m separate vessels, such as glass vials or polyethylene bottles. Summer Research in Chemistry (3 ways)
• NSERC USRA (14 positions) ($6500-7500) – http://www.nserc-crsng.gc.ca/Students- Etudiants/UG-PC/USRA-BRPC_eng.asp • Student Workplace Exchange Program ($6000- 7000) – http://careers.queensu.ca/faculty-staff/hire- student/summer-work-experience-program-swep • Hired Outright- less common