Analytical Chemistry for Technicians 3 ed.

Kenkel John. Analytical Chemistry for Technicians 3 ed. 2002 [pdf 558sc 545c. 13,77mb] Surpassing its bestselling predecessors, this thoroughly updated third edition is designed to be a powerful training tool for entry-level chemistry technicians. Analytical Chemistry for Technicians, Third Edition explains analytical chemistry and instrumental analysis principles and how to apply them in the real world. A unique feature of this edition is that it brings the workplace of the chemical technician into the classroom. With over 50 workplace scene sidebars, it offers stories and photographs of technicians and chemists working with the equipment or performing the techniques discussed in the text. It includes a supplemental CD that enhances training activities. A CD containing a sample LIMS system is also available to professors who adopt this book.The author incorporates knowledge gained from a number of American Chemical Society and PITTCON short courses and from personal visits to several laboratories at major chemical plants, where he determined firsthand what is important in the modern analytical laboratory. The book includes more than sixty experiments specifically relevant to the laboratory technician, along with a Questions and Problems section in each chapter. Analytical Chemistry for Technicians, Third Edition continues to offer the nuts and bolts of analytical chemistry while focusing on the practical aspects of training. Analytical Chemistry for Technicians, Third Edition......Page 2 Dedication......Page 4 Preface......Page 5 Acknowledgments......Page 6 The Author......Page 8 Safety in the Analytical Laboratory......Page 9 Contents......Page 11 Table of Contents......Page 0 1.1 Analytical Science Defined......Page 25 1.2 Classifications of Analysis......Page 26 1.3 The Sample......Page 27 1.5 Analytical Technique and Skills......Page 28 1.6 The Laboratory Notebook......Page 31 1.7.1 Errors......Page 33 1.7.2 Elementary Statistics......Page 34 1.7.3 Normal Distribution......Page 35 1.7.4 Precision, Accuracy, and Calibration......Page 36 1.7.5 Statistical Control......Page 37 Experiment 1: Assuring the Quality of Weight Measurements......Page 38 Questions and Problems......Page 39 2.2 Obtaining the Sample......Page 41 2.3 Statistics of Sampling......Page 43 2.4.2 Maintaining Sample Integrity......Page 44 2.5 Sample Preparation: Solid Materials......Page 46 2.5.3 Solid–Liquid Extraction......Page 47 2.5.4 Other Extractions from Solids......Page 48 2.5.5 Total Dissolution......Page 49 2.6.1 Extraction from Liquid Solutions......Page 52 2.6.2 Dilution, Concentration, and Solvent Exchange......Page 53 2.7 Reagents Used in Sample Preparation......Page 54 Experiment 3: A Study of the Dissolving Properties of Water, Some Common Organic Liquids, and Laboratory Acids......Page 55 Questions and Problems......Page 57 3.3 The Balance......Page 60 3.4 Calibration and Care of Balances......Page 62 3.6.1 Physical Separation Methods and Calculations......Page 63 3.6.1.1 Loss on Drying......Page 64 3.6.1.3 Residue on Ignition......Page 66 3.6.1.4 Insoluble Matter in Reagents......Page 67 3.6.1.5 Solids in Water and Wastewater......Page 68 3.6.1.6 Particle Size by Analytical Sieving......Page 69 3.6.3 Gravimetric Factors......Page 71 3.6.4 Using Gravimetric Factors......Page 73 3.7.1 Weighing Bottles......Page 74 3.7.3 Isolating and Weighing Precipitates......Page 75 Experiment 4: Practice of Gravimetric Analysis Using Physical Separation Methods......Page 77 Experiment 5: The Percent of Water in Hydrated Barium Chloride......Page 79 Experiment 6: The Gravimetric Determination of Sulfate in a Commercial Unknown......Page 80 Experiment 7: The Gravimetric Determination of Iron in a Commercial Unknown......Page 82 Questions and Problems......Page 84 4.2 Terminology......Page 88 4.3.1 Molarity......Page 90 4.3.2 Normality......Page 91 4.4.1 Solid Solute and Molarity......Page 93 4.4.2 Solid Solute and Normality......Page 94 4.5 Stoichiometry of Titration Reactions......Page 95 4.6.1 Standardization Using a Standard Solution......Page 96 4.6.2 Standardization Using a Primary Standard......Page 98 4.7 Percent Analyte Calculations......Page 100 4.8.1 The Volumetric Flask......Page 102 4.8.2 The Pipet......Page 105 4.8.3 The Buret......Page 109 4.8.4 Cleaning and Storing Procedures......Page 110 4.9.2 Pipetters......Page 111 4.9.4 Digital Burets and Automatic Titrators......Page 112 4.11 Analytical Technique......Page 113 Experiment 8: Preparation and Standardization of HCl and NaOH Solutions......Page 115 Questions and Problems......Page 116 5.2 Acid–Base Titrations and Titration Curves......Page 121 5.2.2 Titration of Weak Monoprotic Acids......Page 122 5.2.4 Equivalence Point Detection......Page 123 5.2.5 Titration of Polyprotic Acids: Sulfuric Acid and Phosphoric Acid......Page 125 5.2.7 Titration of Tris-(hydroxymethyl)amino Methane......Page 127 5.2.8 Titration of Sodium Carbonate......Page 128 5.2.9 Alkalinity......Page 129 5.2.10 Back Titrations......Page 130 5.2.11 The Kjeldahl Method for Protein......Page 131 5.2.12 Buffering Effects and Buffer Solutions......Page 135 5.3.2 Complex Ion Terminology......Page 139 5.3.3 EDTA and Water Hardness......Page 142 5.3.4.1 Solution Preparation......Page 145 5.3.5 Water Hardness Calculations......Page 146 5.4.1 Review of Basic Concepts and Terminology......Page 149 5.4.2 The Ion-Electron Method for Balancing Equations......Page 152 5.4.3 Analytical Calculations......Page 153 5.4.4.1 Potassium Permanganate......Page 154 5.4.4.2 Iodometry: An Indirect Method......Page 155 5.5 Other Examples......Page 156 Experiment 11: Titrimetric Analysis of a Commercial Soda Ash Unknown for Sodium Carbonate......Page 157 Experiment 12: Determination of Protein in Macaroni by the Kjeldahl Method......Page 158 Experiment 13: Analysis of Antacid Tablets......Page 159 Experiment 14: Determination of Water Hardness......Page 160 Questions and Problems......Page 161 6.1 Review of the Analytical Strategy......Page 170 6.2 Instrumental Analysis Methods......Page 172 6.3.1 Sensors, Signal Processors, Readouts, and Power Supplies......Page 174 6.3.2 Some Basic Principles of Electronics......Page 175 6.4 Details of Calibration......Page 178 6.4.1 Thermocouples: An Example of a Calibration......Page 179 6.4.2 Calibration of an Analytical Instrument......Page 180 6.4.3 Mathematics of Linear Relationships......Page 181 6.4.4 Method of Least Squares......Page 182 6.5 Preparation of Standards......Page 183 6.6.2 Sample Blanks......Page 184 6.7 Effects of Sample Pretreatment on Calculations......Page 185 6.8.1 Data Acquisition......Page 187 Experiment 15: Voltage, Current, and Resistance......Page 188 Experiment 16: Checking the Calibration of a Temperature Sensor......Page 191 Experiment 17: Working with an Instrumentation Amplifier......Page 192 Experiment 18: Use of a Computer in Laboratory Analysis......Page 195 Questions and Problems......Page 196 7.2 Characterizing Light......Page 200 7.2.1 Wavelength, Speed, Frequency, Energy, and Wavenumber......Page 201 7.3 The Electromagnetic Spectrum......Page 205 7.4.1 Brief Summary......Page 206 7.4.2 Atoms vs. Molecules and Complex Ions......Page 208 7.4.3 Absorption Spectra......Page 209 7.4.4 Light Emission......Page 212 7.5 Absorbance, Transmittance, and Beer’s Law......Page 214 7.6 Effect of Concentration on Spectra......Page 217 Experiment 19: Colorimetric Analysis of Prepared and Real Water Samples for Iron......Page 218 Experiment 21: The Determination of Phosphorus in Environmental Water......Page 219 Questions and Problems......Page 220 8.2.1 Sources......Page 225 8.2.2 Wavelength Selection......Page 226 8.2.2.2 Monochromators......Page 227 8.2.3 Sample Compartment......Page 229 8.2.3.2 Beamsplitting and Chopping......Page 230 8.2.3.3 Double-Beam Designs......Page 231 8.2.5 Diode Array Instruments......Page 232 8.3 Cuvette Selection and Handling......Page 233 8.4.2 Deviations......Page 234 8.4.4 Troubleshooting......Page 235 8.5 Fluorometry......Page 236 8.6 Introduction to IR Spectrometry......Page 238 8.7 IR Instrumentation......Page 239 8.8.1 Liquid Sampling......Page 240 8.9.2 Thin Film Formed by Solvent Evaporation......Page 245 8.9.4 Nujol Mull......Page 246 8.9.5.2 Internal Reflectance......Page 248 8.9.6 Gas Sampling......Page 249 8.10 Basic IR Spectra Interpretation......Page 250 8.11 Quantitative Analysis......Page 253 Experiment 23: Determination of Nitrate in Drinking Water by UV Spectrophotometry......Page 254 Experiment 25: Qualitative Analysis by Infrared Spectrometry......Page 255 Experiment 27: Identifying Minor Components of Commercial Solvents......Page 256 Questions and Problems......Page 257 9.1 Review and Comparisons......Page 264 9.2 Brief Summary of Techniques and Instrument Designs......Page 265 9.3.1 Flames and Flame Processes......Page 267 9.3.2 Spectral Line Sources......Page 268 9.3.2.1 Hollow Cathode Lamp......Page 269 9.3.3 Premix Burner......Page 270 9.3.4 Optical Path......Page 272 9.3.5.1 Slits and Spectral Lines......Page 273 9.3.5.3 Lamp Alignment......Page 274 9.3.6.1 Chemical Interferences......Page 275 9.4.1 General Description......Page 277 9.5 Inductively Coupled Plasma......Page 280 9.6.1 Flame Photometry......Page 284 9.6.5 Atomic Fluorescence......Page 285 9.7 Summary of Atomic Techniques......Page 286 Experiment 30: Verifying Optimum Instrument Parameters for Flame AA......Page 287 Experiment 32: The Analysis of Snack Chips for Sodium by Atomic Absorption......Page 289 Experiment 34: The Determination of Sodium in Soda Pop......Page 290 Questions and Problems......Page 291 10.1 Introduction to X-Ray Methods......Page 294 10.2 X-Ray Diffraction Spectroscopy......Page 295 10.3.2 Applications......Page 299 10.4.1 Introduction......Page 300 10.4.2 Instrumentation......Page 301 10.4.3 The NMR Spectrum......Page 303 10.4.3.1 Chemical Shifts......Page 304 10.4.3.2 Peak Splitting and Integration......Page 305 10.5.3 The Magnetic Sector Mass Spectrometer......Page 306 10.5.5 The Time-of-Flight Mass Spectrometer......Page 307 10.5.6 Mass Spectra......Page 308 10.5.7 Mass Spectrometry Combined with Inductively Coupled Plasma......Page 309 10.5.8 Mass Spectrometry Combined with Instrumental Chromatography......Page 311 Questions and Problems......Page 313 11.2 Recrystallization......Page 318 11.3 Distillation......Page 319 11.4.2 The Separatory Funnel......Page 321 11.4.3 Theory......Page 323 11.4.4 Percent Extracted......Page 324 11.4.6 Evaporators......Page 325 11.5 Solid–Liquid Extraction......Page 326 11.6 Chromatography......Page 329 11.7.1 Partition Chromatography......Page 330 11.7.2 Adsorption Chromatography......Page 331 11.7.4 Size Exclusion Chromatography......Page 332 11.8.1 Paper and Thin-Layer Chromatography......Page 334 11.8.2 Classical Open-Column Chromatography......Page 336 11.8.3 Instrumental Chromatography......Page 337 11.8.4 The Instrumental Chromatogram......Page 338 11.8.5 Quantitative Analysis with GC and HPLC......Page 343 11.9.1 Introduction......Page 344 11.9.2 Paper Electrophoresis......Page 345 11.9.3 Gel Electrophoresis......Page 346 Experiment 35: Extraction of Iodine with Heptane......Page 347 Experiment 37: Solid–Liquid Extraction: Determination of Nitrite in Hot Dogs......Page 348 Experiment 38: The Thin-Layer Chromatography Analysis of Cough Syrups for Dyes......Page 349 Questions and Problems......Page 350 12.1 Introduction......Page 355 12.3 Sample Injection......Page 357 12.4.1 Instrument Logistics......Page 359 12.4.2 Packed, Open-Tubular, and Preparative Columns......Page 360 12.4.3 The Nature and Selection of the Stationary Phase......Page 362 12.5.1 Column Temperature......Page 363 12.6 Detectors......Page 365 12.6.1 Thermal Conductivity......Page 366 12.6.2 Flame Ionization Detector......Page 367 12.6.3 Electron Capture Detector......Page 368 12.6.7 GC-MS and GC-IR......Page 369 12.7 Qualitative Analysis......Page 370 12.8.2 The Response Factor Method......Page 371 12.8.3 Internal Standard Method......Page 372 12.9.1 Diminished Peak Size......Page 373 12.9.3 Altered Retention Times......Page 374 12.9.6 Appearance of Unexpected Peaks......Page 375 Experiment 40: A Qualitative Gas Chromatographic Analysis of a Prepared Sample......Page 376 Experiment 42: The Determination of Ethanol in Wine by Gas Chromatography and the Internal Standard Method......Page 377 Experiment 44: A Study of the Effect of the Changing of GC Instrument Parameters on Resolution......Page 378 Questions and Problems......Page 379 13.1.2 Comparisons with GC......Page 385 13.2 Mobile Phase Considerations......Page 386 13.3.1 Pumps......Page 389 13.3.2 Gradient vs. Isocratic Elution......Page 390 13.4 Sample Injection......Page 391 13.5.1 Normal Phase Columns......Page 392 13.5.3 Adsorption Columns......Page 393 13.5.4 Ion Exchange and Size Exclusion Columns......Page 394 13.5.5 Column Selection......Page 395 13.6.1 UV Absorption......Page 396 13.6.3 Fluorescence......Page 397 13.6.4 Refractive Index......Page 398 13.6.5.1 Conductivity......Page 399 13.6.5.2 Amperometric......Page 400 13.6.6 LC-MS and LC-IR......Page 401 13.7 Qualitative and Quantitative Analyses......Page 402 13.8.4 Air Bubbles......Page 403 Experiment 46: The Quantitative Determination of Methyl Paraben in a Prepared Sample by HPLC......Page 404 Experiment 48: Designing an Experiment for Determining Caffeine in Coffee and Tea......Page 406 Questions and Problems......Page 407 14.1 Introduction......Page 411 14.2 Transfer Tendencies: Standard Reduction Potentials......Page 412 14.4 The Nernst Equation......Page 415 14.5.1.1 The Saturated Calomel Reference Electrode......Page 417 14.5.2.1 The pH Electrode......Page 419 14.5.2.2 The Combination pH Electrode......Page 420 14.5.2.3 Ion-Selective Electrodes......Page 421 14.5.3 Other Details of Electrode Design......Page 422 14.5.5 Potentiometric Titrations......Page 423 14.6.2 Amperometry......Page 425 14.7 Karl Fischer Titration......Page 426 14.7.3 The Volumetric Method......Page 427 Experiment 50: Determination of the pH of Soil Samples......Page 429 Experiment 51: Red Cabbage Extract, the pH Electrode, and PowerPoint: A Group Project and Oral Presentation......Page 430 Experiment 52: Potentiometric Titration of Phosphoric Acid in Soda Pop......Page 431 Experiment 53: Operation of Metrohm Model 701 Karl Fischer Titrator (for Liquid Samples)......Page 432 Questions and Problems......Page 433 15.2.1 Introduction......Page 436 15.2.4 Capillary Viscometry......Page 437 15.2.5 Rotational Viscometry......Page 439 15.3.2 DTA and DSC......Page 441 15.3.3 DSC Instrumentation......Page 443 15.4 Refractive Index......Page 444 15.5 Optical Rotation......Page 447 15.6.1 Introduction to Density......Page 449 15.6.3 The Density of Irregularly Shaped Solids......Page 450 15.6.4 The Density of Liquids......Page 451 15.6.6 Specific Gravity......Page 453 15.6.7 Hydrometers......Page 454 15.6.9 Density Gradient Columns......Page 455 15.7.2 Sieves and Screen Analysis......Page 456 15.7.3 Data Handling and Analysis......Page 457 15.7.4 Histogram Representation......Page 458 15.7.5 Fractional and Cumulative Representations......Page 459 15.7.7 Electrozone Sensing......Page 462 15.8.1 Impact Testing......Page 464 15.9.1 Introduction......Page 467 15.9.2 The Stress–Strain Diagram......Page 468 15.10.1 Introduction......Page 469 15.10.2 Simple Hardness Tests......Page 470 15.10.3 Indentation Hardness Tests......Page 471 15.10.6 The Knoop Microhardness Test......Page 472 Experiment 54: Capillary Viscometry......Page 473 Experiment 56: Measuring Refractive Index......Page 474 Experiment 57: Particle Size Analysis......Page 475 Experiment 58: Tensile Testing of Polymers Using a Homemade Tester......Page 477 Questions and Problems......Page 478 16.2.1 Carbohydrates......Page 481 16.2.2 Lipids......Page 483 16.2.3.2 Peptides......Page 485 16.2.3.3 Proteins: Primary Structure......Page 486 16.2.3.5 Proteins: Tertiary Structure......Page 487 16.2.4 Nucleic Acids......Page 488 16.3.2 Electrophoresis......Page 491 16.3.3 Chromatography......Page 492 16.3.3.3.1 Columns......Page 493 16.3.3.3.3 Other Considerations......Page 495 Experiment 59: Qualitative Testing of Food Products for Carbohydrates......Page 496 Experiment 60: Fat Extraction and Determination......Page 497 Experiment 61: Identification of Amino Acids in Food by Paper Chromatography......Page 498 Experiment 63: HPLC Separation of Nucleotides......Page 499 Experiment 65: Restriction Endonuclease Cleavage of DNA......Page 500 Experiment 66: Separation of Restriction Enzyme Digestion Fragments via Horizontal Agarose Gel Electrophoresis......Page 501 Questions and Problems......Page 502 A1.1 General Provisions......Page 503 A1.3 Facilities......Page 505 A1.6 Test, Control, and Reference Substances......Page 506 A1.9 Disqualification of Testing Facilities......Page 507 Appendix 2: Significant Figure Rules......Page 508 Appendix 3: Stoichiometric Basis for Gravimetric Factors......Page 510 Appendix 4: Solution and Titrimetric Analysis Calculation Formulas......Page 511 Appendix 5: Answers to Questions and Problems......Page 514

Surpassing its bestselling predecessors, this thoroughly updated third edition is designed to be a powerful training tool for entry-level chemistry technicians. Analytical Chemistry for Technicians, Third Edition explains analytical chemistry and instrumental analysis principles and how to apply them in the real world. A unique feature of this edition is that it brings the workplace of the chemical technician into the classroom.

With over 50 workplace scene sidebars, it offers stories and photographs of technicians and chemists working with the equipment or performing the techniques discussed in the text. It includes a supplemental CD that enhances training activities. The author incorporates knowledge gained from a number of American Chemical Society and PITTCON short courses and from personal visits to several laboratories at major chemical plants, where he determined firsthand what is important in the modern analytical laboratory.

The book includes more than sixty experiments specifically relevant to the laboratory technician, along with a Questions and Problems section in each chapter. Analytical Chemistry for Technicians, Third Edition continues to offer the nuts and bolts of analytical chemistry while focusing on the practical aspects of training.

Surpassing its bestselling predecessors, this thoroughly updated third edition, along with its unique ancillaries, is designed to be a powerful training tool for entry-level chemistry technicians. Now even more than ever, Analytical Chemistry for Technicians explains analytical chemistry and instrumental analysis principles and how to apply them in the real world. A unique feature of this edition is that it brings the workplace of the chemical technician into the classroom. With over 50 workplace scene side boxes, it offers stories and photographs of technicians and chemists working with the equipment or performing the techniques discussed in the text. Also, an accompanying CD enhances training activities that use the text, and a working LIMS system can be used in training programs for chemical technicians. The author also incorporates knowledge gained from a number of American Chemical Society and PITTCON short courses and from personal visits to several laboratories at major chemical plants, where he determined firsthand what is important in the modern analytical laboratory. Most importantly, the author uses the recently published Voluntary Industry Standards for chemical process industry technicians.Analytical Chemistry for Technicians, Third Edition includes over sixty experiments specifically relevant to the laboratory technician, along with a Questions and Problems section in each chapter. By continuing to provide the fundamentals of analytical chemistry while focusing on the practical aspects of training, this new edition will be an invaluable tool to technicians and chemists.