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Laboratory Manual Laboratory Manual to Accompany Quantitative Chemistry and Instrumental Analysis David B. Green Natural Science Division Pepperdine University Copyright 1991, 1995, 1996 by David B. Green. All rights reserved. Except as permitted under the United States Copyright Act of 1976, no part of this publication may be reproduced or distributed in any form or by any means without prior written permission of the author. ii Acknowledgments The author wishes to acknowledge with thanks, the contributions to this laboratory manual by the following people: Brandy Violanti Determination of Caffeine in Beverages by HPLC (July 1995) Isaac Bright & Brian Smart Determination of Doxylamine Succinate and 4-acetamidophenol in an OTC Pharmaceutical by HPLC (July 1996) and to those who have pointed out editorial, content, and accuracy errors in this and prior editions. iii iv Table of Contents Introduction to the Analytical Laboratory ................................... 1 Safety in the Laboratory ....................................................................................... 3 The Laboratory Notebook .................................................................................... 5 The Analysis Report ............................................................................................. 8 Statistical Analysis in Chemistry ................................................. 11 The Lab You Can Eat ......................................................................................... 13 Volumetric Analysis ......................................................................... 15 Acid-Base Titrations .......................................................................................... 17 Determination of %Fe in Iron Ore ..................................................................... 21 Determination of %Cl in a Soluble Chloride by the Mohr Method ................... 25 Determination of Silver in an Alloy or Soluble Salt .......................................... 27 Iodimetric Determination of Ascorbic Acid in Vitamin-C Tablets ................... 29 Gravimetric Analysis ....................................................................... 33 Gravimetric Determination of Chloride in a Soluble Sample ............................ 35 Gravimetric Analysis of Nickel ......................................................................... 37 Determination of the Thermodynamic Ksp of a Sparingly Soluble Salt ............. 41 Electrochemical Methods of Analysis ........................................ 45 The pH Meter: Determination of Apparent pKa and the Molar Mass of a Compound ................................................................................................. 47 Potentiometric Titration of a Bromide-Iodide Mixture ...................................... 51 Fluoride Ion Selective Potentiometry................................................................. 55 Electrochemical Methods of Analysis: Polarography ........................................ 57 Determination of the Formula and Apparent Formation Constant of the Lead-Oxalate Complex Ion by Differential Pulse Polarography ................. 61 Conductimetry: Analysis of Aspirin ................................................................. 67 Spectrophotometric Methods of Analysis................................. 73 Determination of Iron with 1,10-Phenanthroline ............................................... 75 Determination of the Formula of a Complex by the Method of Continuous Variations .................................................................................. 77 Determination of the Manganese in Steel .......................................................... 81 Spectrophotometric Analysis of a Complex Mixture ........................................ 83 Spectrophotometric Determination of the pKa of an Acid-Base Indicator ......... 87 Multicomponent Drug Analysis by UV-Visible Spectroscopy .......................... 91 Determination of the Spectrochemical Series .................................................... 95 Determination of Acetylsalicylic and Salicylic Acid in Aspirin by Fluorescence Spectroscopy .......................................................................... 99 Determination of the Critical Micelle Concentration of Sodium Dodecyl Sulfate Using a Fluorescent Probe ............................................................. 103 Atomic Absorption Spectroscopy .................................................................... 107 Fourier Transform Infrared Spectroscopy - FT-IR .......................................... 113 v Analysis Based on Separation Science ................................... 117 Gas Chromatography: Mechanistic Study of the Dehydration of Butanol ....................................................................................................... 119 Identification of an Unknown Mixture by Gas Chromatography .................... 123 Determination of Caffeine in Beverages by HPLC.......................................... 125 Determination of Doxylamine Succinate and 4-Acetamidophenol in an OTC Pharmaceutical by HPLC .................................................................. 130 Computers in Analytical Chemistry .......................................... 138 Mathcad Problem Session: Equilibrium........................................................... 140 Spreadsheets in Chemistry: An Introduction ................................................... 144 A Problem of the Least-Squares Fit When You Don't Look at Your Data ...... 156 Appendices ...................................................................................... 158 Appendix 1: Formula Weights of Selected Compounds ................................. 160 Appendix 2: Concentrations of Some Common Acids and Bases .................. 161 Appendix 3: Some Important Statistical Tables.............................................. 162 Table 1: Confidence Levels for Various Values of z ........................... 162 Table 2: Critical Values for the Rejection Quotient, Q ........................ 162 Table 3: Values of Student's-t .............................................................. 162 Table 4: Critical Values for the Rejection Quotient, Tn ...................... 163 Table 5: Critical Values for F at the 5% Level .................................... 163 Appendix 4: Acid Dissociation Constants of Some Weak Acids and Bases .......................................................................................................... 164 Acid Dissociation Constants ................................................................ 164 Base Ionization Constants .................................................................... 165 Appendix 5: Solubility Products of Selected Compounds .............................. 166 Appendix 6: Stability Constants for Selected Complex Ions .......................... 168 Appendix 7: Standard Reduction Potentials ................................................... 169 Sorted In Order of Decreasing Potential .............................................. 169 Sorted In Alphabetical Order ............................................................... 171 vi Introduction to the Analytical Laboratory Introduction to the Analytical Laboratory 1 2 Introduction to the Analytical Laboratory Safety in the Laboratory With few exceptions, ANSI approved safety goggles are required at all times in the laboratory when chemical reactions in the area are underway. Prescription glasses are not adequate eye protection. Contact lenses are not recommended in the laboratory unless they must be worn for proper eyesight where prescription glasses would be unsatisfactory, very inconvenient, or unsafe. A lab coat is required and should be worn buttoned. Acids, bases, and other liquid reagents are used frequently. Closed-toe shoes are recommended to protect feet from splashes. Some analyses may require more than the normal lab time to complete (especially when oven drying and some other steps are required). The laboratory is open during many times outside of the scheduled lab time to complete analyses. Goggles and a lab coat must be worn when working outside of normal lab times. Failure to wear personal protection will result in the loss of this privilege. This requirement is not negotiable and no warnings will be given. University Public Safety may ask you to leave a laboratory area if working after normal university hours. This request must be complied with immediately and without argument. Radios and tape or CD players are acceptable in this laboratory if the volume is low enough that a quiet conversation can be heard by everyone in the area. The volume must never be so loud that it can be heard in other laboratory areas, classrooms, etc. Food and drink have no place in the laboratory when chemical reactions, preparations, or transfers are being performed. It is your responsibility to get information about chemicals in use and their safe handling. Much of this aspect is covered in prelaboratory lecture. The Material Safety Data Sheets (MSDS) are available and should be referenced for important chemical information. If in doubt about a safety procedure, find out the appropriate information prior to starting the analysis. Properly dispose of waste materials. Some solids may not be disposed in the trash; some liquids may not be disposed in the sink. Maintain a neat and orderly work area. This is especially important since the laboratory is shared by others. Used glassware must be cleaned and dried on the drying
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