<p> Introduction & Figures of Merit</p><p>Suggested Reading  Skoog/Holler/Crouch 6th Edition: Chapter 1A, 1B, 1E, Appendix 1  Harris 7th Edition: Chapters 3&4, mostly same material as Appendix 1 of Skoog, Chapter 5 Sections 3&4, Appendix B&C Some of this material is redundant between the two texts</p><p>Chemical Analysis</p><p>Classical Instrumental "Wet" Chemical</p><p>Qualitative Analysis Quantitative Analysis Qualitative Analysis Quantitative Analysis</p><p>Instrumental Methods</p><p>Thermal Mass/Separations</p><p>Spectroscopic Electrochemical</p><p>1 To perform an analysis, the analyte must often first be separated from a mixture.</p><p>Analytical Separations</p><p>Chromatography Mass Spectrometry GC, LC, SFC Capillary Electrophoresis</p><p>After separation chemical analysis often performed on analyte.</p><p> Preparatory Separations – analysis often performed off-line. (Synthesis, large scale separations)  Analytical Separations – analysis often performed on-line with separation method. This course is concerned with analytical, or very small scale separations. </p><p>Fundamentals are the same for analytical and preparatory separations, technique specifics differ.</p><p>General Course Outline</p><p>1. Fundamentals A. Instrument performance characteristics (Figures of Merit) and statistical background review.</p><p>B. Instrument Calibrations</p><p>2 a. Traditional (Review) b. Standard Additions c. Internal Standards C. Signals, Noise, S/N a. Definitions/Sources b. Methods for S/N enhancement</p><p>2. Separations A. Mass Spectrometry a. Fundamentals b. Instrumentation c. Information</p><p>B. Chromatography a. Fundamentals – Plate and Rate Theories, etc. b. Liquid and Gas chromatography c. Capillary electrophoresis</p><p>3. Analytical Spectroscopy A. Fundamentals of absorption/emission processes a. Line, Band, Continuous spectra b. Measurement basics of absorption and emission spectra & types of instrumentation</p><p>B. Absorption spectroscopy a. Molecular (UV-vis, IR) b. Atomic (AA)</p><p>C. Emission spectroscopy a. Atomic (AES) b. Molecular (Fluorescence)</p><p>General Instrument Performance Characteristics</p><p>3 First define the problem:  What accuracy is required?  What is the analyte concentration range?  What components of the sample might interfere with the analysis?  Etc.</p><p>Tables 1-3, 1-5 (Skoog)</p><p>1. Precision = Measurement Reproducibility Review statistics:</p><p>2. Bias = systematic measurement error</p><p>4 3. Sensitivity = Ability to distinguish between small differences in analyte concentration</p><p>Sensitivity Illustration</p><p>12</p><p>S = mC + SBl</p><p>10</p><p>8 l a n g i S</p><p> t</p><p> n 6 e m u r t s n I</p><p>4</p><p>2</p><p>0 0 1 2 3 4 5 6 Analyte Concentration</p><p>4. Detection Limit = minimum analyte concentration that can be detected with a given confidence level.</p><p>5 SUMMARY OUTPUT Standard Coefficients Error Regression Statistics Intercept 1.517857143 0.294936001 X Variable Multiple R 0.998879565 1 1.930357143 0.040900264 R Square 0.997760386 Adjusted R Square 0.997312463 Standard Error 0.432847713 Observations 7</p><p>Find the detection limit for a fluorescence analysis given the following calibration data. Analyte Conc. (pg/mL) Fluorescence Intensity 0 2.1 2 5.0 4 9.0 6 12.6 8 17.3 10 21 12 24.7</p><p>30</p><p> l y = 1.9304x + 1.5179 a 25 n g i</p><p>S 20</p><p> e c</p><p> n 15 e c s</p><p> e 10 r o u</p><p> l 5 F 0 0 2 4 6 8 10 12 14 pg/mL</p><p>6 5. Linear Dynamic Range = Analyte concentration range from the Limit of Quantification  concentration at which there is a non- linear instrument response.</p><p>7 6. Selectivity = A method’s ability to selectively analyze an analyte in the presence of other chemical species (the sample “matrix”). Signal = maCa + mbCb + Sbl m = analytical sensitivity, c = concentration </p><p>8</p>