Analytical Chemistry CHEM 2302 1. Course outline Tentative schedule of lectures 2. Introduction What is analytical chemistry? Chemical analysis is concerned with detecting or determining a specific component or the general composition of a sample. Qualitative analysis - to find out what constituents are in the sample. - to see whether the target constituents of interest are present or not in the sample Quantitative analysis - to determine how much of each constituent is in the sample. Analytical data - solving chemical problems. Where is analytical chemistry used? Topical areas of interest How to approach the course Send me your e-mail addresses to: edward_lai@carleton.ca Course Website developed by the Educational Development Centre http://http-server.carleton.ca/~elai/ http://www.carleton.ca/~elai/ CHEM 2302 CHEM 2302* Analytical Chemistry I Course Material 1 Course Marks on WebCT Course Material 1 Course Outline Introduction All files are .PDF 2 Preparation for test on Chapters 1 2 3 3 Preparation for test on Chapters 1 2 3 (5th edition) 4 Lab Manual 2005 2 How to Approach the Course Attend class regularly. Study lecture notes with reference to the textbook after each lecture. Prepare for lab experiments. See me about difficulties/problems. Do all assignments. Study hard for the quizzes and final exam. Where is analytical chemistry used? inorganic, organic, physical and biological chemistry research research in biology, earth sciences, medicine and physics industrial quality control -- relating chemical composition to physical properties - drugs, pharmaceuticals, foods, polymers and plastic materials trouble-shooting in manufacturing industries -- solving problems with the aid of chemical data forensic chemistry environmental chemistry -- making precise measurements that are required for the determination of trace amounts of pollutants Analytical chemists in industry are problem solvers who use their chemical skills and analytical thinking to solve problems : They gather relevant background information, think through what steps should be taken, and develop a plan (including available resources) before going to the lab. 3 Objectives in Analytical Chemistry Technician level -- methods, principles, instruments (lab) Chemistry 65.2302* and 65.2303* Chemist level -- method selection, parameter optimization, data evaluation, results interpretation Chemistry 65.3305* and 65.4301* Scientist level -- development of new techniques and methods, publication of scientific papers Graduate studies and research (M.Sc. and Ph.D.) 4 3. Nomenclature (or terminology) Sample a fraction of the material whose chemical composition is of interest Chemical analysis is usually performed on a sample Analyte element / ion / compound, the concentration of which is to be determined Analysis only samples are analyzed elements, ions and compounds are identified or determined (detected) When the sample is nominally an element or compound, "analysis of an element or compound" must be understood to mean the identification or determination of impurities. Sample matrix the medium containing the analyte the part of the sample material that is not of interest in an analysis Interferences other chemicals present in the sample that produce an effect upon the measurement and change the signal when the analyte concentration remains unchanged. 5 Send me your e-mail addresses to: edward_lai@carleton.ca 6 Advanced Photo-Oxidation Process for Ammonia Removal from Industrial Wastewater 7 8 Standard Methods http://www.AOAC.org Groundwater and Wastewater Analyses HYPERLINK TO METHOD METHOD TITLE EPA Method 601 PURGABLE HALOCARBONS EPA Method 602 PURGABLE AROMATICS EPA Method 603 ACROLEIN AND ACRYLONITRILE EPA Method 604 PHENOLS EPA Method 604.1 DETERMINATION OF HEXACHLOROPHENE AND DICHLOROPHEN IN INDUSTRIAL AND MUNICIPAL WASTEWATERS EPA Method 605 BENZIDINES EPA Method 606 PHTHALATE ESTERS EPA Method 607 NITROSAMINES EPA Method 608 ORGANOCHLORINE PESTICIDES AND PCB'S EPA Method 608.2 ANALYSIS OF CERTAIN ORGANOCHLORINE PESTICIDES IN WASTEWATER BY GAS CHROMATOGRAPHY EPA Method 609 NITROAROMATICS AND ISOPHORONE EPA Method 610 POLYNUCLEAR AROMATIC HYDROCARBONS EPA Method 611 HALOETHERS EPA Method 612 CHLORINATED HYDROCARBONS EPA Method 613 DIOXIN EPA Method 615 THE DETERMINATION OF CHLORONATED HERBICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 616 C, H, AND O COMPOUNDS EPA Method 617 THE DETERMINATION OF ORGANOHALIDE PESTICIDES AND PCBS IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 618 DETERMINATION OF VOLATILE PESTICIDES IN MUNICIPAL AND INDUSTRIAL WASTEWATERS BY GAS CHROMATOGRAPHY EPA Method 619 DETERMINATION OF TRIAZINE PESTICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 620 DETERMINATION OF DIPHENYLAMINE IN MUNICIPAL AND INDUSTRIAL WASTEWATERS EPA Method 622.1 THIOPHOSPHATE PESTICIDES EPA Method 624 PURGABLE ORGANICS IN WATERS EPA Method 625 SEMIVOLATILE ORGANICS IN WATERS EPA Method 627 THE DETERMINATION OF DINITROANILINE PESTICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 629 THE DETERMINATION OF CYANAZINE IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 631 THE DETERMINATION OF BENOMYL AND CARBENDAZIM IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 632 THE DETERMINATION OF CARBAMATE AND UREA PESTICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 632.1 ANALYSIS OF CARBAMATE AND AMIDE PESTICIDES IN WASTEWATER BY LIQUID CHROMATOGRAPHY EPA Method 633 THE DETERMINATION OF ORGANONITROGEN PESTICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATER EPA Method 634 DETERMINATION OF THIOCARBAMATE PESTICIDES IN INDUSTRIAL AND MUNICIPAL WASTEWATERS BY GAS CHROMATOGRAPHY EPA Method 635 DETERMINATION OF ROTENONE IN INDUSTRIAL AND MUNICIPAL WASTEWATERS BY LIQUID CHROMATOGRAPHY 9 EPA Method 636 DETERMINATION OF BENSULIDE IN INDUSTRIAL AND MUNICIPAL WASTEWATERS BY LIQUID CHROMATOGRAPHY EPA Method 637 DETERMINATION OF MBTS AND TCMTB IN MUNICIPAL AND INDUSTRIAL WASTEWATERS BY LIQUID CHROMATOGRAPHY EPA Method 638 DETERMINATION OF ORYZALIN IN INDUSTRIAL AND MUNICIPAL WASTEWATERS EPA Method 639 DETERMINATION OF BENDIOCARB IN MUNICIPAL AND INDUSTRIAL WASTEWATERS BY LIQUID CHROMATOGRAPHY EPA Method 640 DETERMINATION OF MERCAPTOBENZOTHIAZOLE IN WASTEWATERS BY LIQUID CHROMATOGRAPHY EPA Method 641 ANALYSIS OF THIABENDAZOLE IN WASTEWATER BY LIQUID CHROMATOGRAPHY EPA Method 643 ANALYSIS OF BENTAZON IN WASTEWATER BY LIQUID CHROMATOGRAPHY EPA Method 644 ANALYSIS OF PICLORAM IN WASTEWATER BY LIQUID CHROMATOGRAPHY EPA Method 645 ANALYSIS OF CERTAIN AMINE PESTICIDES AND LETHANE IN WASTEWATER BY GAS EPA Method 646 ANALYSIS OF DINITRO AROMATIC PESTICIDES IN WASTEWATER BY GAS CHROMATOGRAPHY 10 What instrumental methods (or analytical techniques) can you use for the following analysis? determination of calcium in Ca3(PO4)2 anions in tap / river water fluoride in drinking water cadmium, copper, lead and zinc in tap / river water polycyclic aromatic hydrocarbons (PAHs) in environmental water samples carbonyls in atmospheric aerosol and vehicle exhaust chemical oxygen demand of ground / river water 11 Chemistry 65.2302* ANALYTICAL CHEMISTRY LABORATORY MANUAL 2006 Fall Page 3 EXPERIMENTS 1. Ion Chromatography of Anions in Tap/River Water with Conductivity Detection. 2. Determination of Fluoride in Drinking Water by Ion-Selective Electrode Potentiometry. 3. Determination of Lead, Cadmium and Copper in Tap/River Water by Differential Pulse Anodic Stripping Voltammetry. 4. Determination of Copper and Zinc in Tap/River Water by Atomic Absorption Spectroscopy. 5. Gas Chromatography of Polycyclic Aromatic Hydrocarbons with Flame Ionization Detection. 6. Monitoring of Carbonyls by 2,4-Dinitrophenylhydrazine Derivatization and Reversed-Phase High Performance Liquid Chromatography. 7. Chemical Oxygen Demand Assay by Standard Method 5200 D. 12 Summary Method Analytes Destructive / Analytical Non-destructive figures of merit EDTA complexometric titration HPLC GC Ion-selective electrodes Anodic stripping voltammetry 13 14 15 16 Standard Calibration Curve A calibration curve is always prepared to establish a working relationship between the analytical signal (that you measure using an instrument) and the analyte concentration (that you prepare in standard solutions). This curve is required for you to determine the unknown analyte concentration in the sample by using the instrument to measure a signal for interpolation. 17