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Analytical Chemistry
for Technicians
Fourth Edition

John Kenkel
Analytical
Chemistry
for
Technicians
Fourth Edition
Analytical
Chemistry
for
Technicians
Fourth Edition

John Kenkel

Boca Raton London New York

CRC Press is an imprint of the

Taylor & Francis Group, an informa business
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 This book is dedicated to the hundreds of hardworking students
that have passed through my classroom and laboratory over
the past 36 years. Without them, the wonderful career that has
defined my professional life would have been a mere dream.
This book is also dedicated to the precious women in my personal life that
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Contents
List of Experiments.........................................................................................................................xvii
Preface.............................................................................................................................................xix
Acknowledgments............................................................................................................................xxi
Author........................................................................................................................................... xxiii
Introduction to Laboratory Work....................................................................................................xxv

Chapter 1 Introduction to Analytical Science................................................................................1

1.1 Analytical Science Defined................................................................................1
1.2 Classifications of Analysis..................................................................................2
1.3 The Sample......................................................................................................... 3
1.4 The Analytical Process......................................................................................3
1.5 Analytical Technique and Skills........................................................................4
1.6 Elementary Statistics.......................................................................................... 5
1.6.1 Errors..................................................................................................... 5
1.6.2 Definitions............................................................................................. 6
1.6.3 Distribution of Measurements............................................................... 8
1.6.4 Student’s t............................................................................................ 10
1.6.5 Rejection of Data................................................................................. 12
1.6.6 Final Comments on Statistics.............................................................. 13
1.7 Precision, Accuracy, and Calibration............................................................... 13

Chapter 2 Sampling and Sample Preparation.............................................................................. 19

2.1 Introduction...................................................................................................... 19
2.2 Obtaining the Sample....................................................................................... 19
2.3 Statistics of Sampling.......................................................................................20
2.4 Sample Handling.............................................................................................. 21
2.4.1 Chain of Custody................................................................................. 21
2.4.2 Maintaining Sample Integrity............................................................. 22
2.5 Sample Preparation—Solid Materials.............................................................. 23
2.5.1 Particle Size Reduction....................................................................... 23
2.5.2 Sample Homogenization and Division................................................ 23
2.5.3 Solid–Liquid Extraction......................................................................24
2.5.4 Other Extractions from Solids.............................................................24
2.6 Water Purification and Use...............................................................................25
2.6.1 Purifying Water by Distillation...........................................................25
2.6.2 Purifying Water by Deionization........................................................26
2.7 Total Sample Dissolution and Other Considerations........................................26
2.7.1 Hydrochloric Acid............................................................................... 27
2.7.2 Sulfuric Acid....................................................................................... 27
2.7.3 Nitric Acid...........................................................................................28
2.7.4 Hydrofluoric Acid................................................................................28
2.7.5 Perchloric Acid....................................................................................28
2.7.6 “Aqua Regia”.......................................................................................28
2.7.7 Acetic Acid..........................................................................................28
2.7.8 Ammonium Hydroxide....................................................................... 29

vii
viii Contents

2.8 Fusion............................................................................................................... 30
2.9 Sample Preparation: Liquid Samples, Extracts, and Solutions of Solids......... 30
2.9.1 Extraction from Liquid Solutions........................................................ 30
2.9.2 Dilution, Concentration, and Solvent Exchange................................. 32
2.9.3 Sample Stability.................................................................................. 32
2.10 Liquid–Liquid Extraction................................................................................. 32
2.10.1 Introduction......................................................................................... 32
2.10.2 The Separatory Funnel........................................................................ 33
2.10.3 Theory.................................................................................................34
2.10.4 Calculations Involving Equation 2.2................................................... 35
2.10.5 Calculations Involving Equation 2.3................................................... 36
2.10.6 Calculations Involving a Combination of Equations 2.3 (or 2.7)
and 2.4................................................................................................. 37
2.10.7 Calculation of Percent Extracted (Equation 2.5)................................ 37
2.10.8 Evaporators.......................................................................................... 38
2.11 Solid–Liquid Extraction................................................................................... 38
2.12 Distillation of a Mixture of Liquids................................................................. 39
2.13 Reagents Used in Sample Preparation.............................................................. 41
2.14 Labeling and Record Keeping.......................................................................... 41

Chapter 3 Gravimetric Analysis.................................................................................................. 49

3.1 Introduction...................................................................................................... 49
3.2 Weight vs. Mass................................................................................................ 49
3.3 The Balance...................................................................................................... 49
3.4 The Desiccator.................................................................................................. 51
3.5 Calibration and Care of Balances..................................................................... 52
3.6 When to Use Which Balance........................................................................... 52
3.7 Details of Gravimetric Methods....................................................................... 53
3.7.1 Physical Separation Methods and Calculations.................................. 53
3.7.1.1 Loss on Drying.................................................................... 55
3.7.1.2 Loss on Ignition................................................................... 55
3.7.1.3 Residue on Ignition.............................................................. 56
3.7.1.4 Insoluble Matter in Reagents............................................... 56
3.7.1.5 Solids in Water and Wastewater.......................................... 56
3.7.1.6 Particle Size by Analytical Sieving..................................... 57
3.7.2 Chemical Alteration/Separation of the Analyte.................................. 58
3.7.3 Gravimetric Factors............................................................................. 59
3.7.4 Using Gravimetric Factors.................................................................. 61
3.8 Experimental Considerations........................................................................... 63
3.8.1 Weighing Bottles................................................................................. 63
3.8.2 Weighing by Difference...................................................................... 63
3.8.3 Isolating and Weighing Precipitates....................................................64

Chapter 4 Introduction to Titrimetric Analysis........................................................................... 73

4.1 Introduction...................................................................................................... 73
4.2 Terminology..................................................................................................... 73
4.3 Review of Solution Concentration.................................................................... 75
4.3.1 Molarity............................................................................................... 75
4.3.2 Normality............................................................................................ 77
Contents ix

4.4 Review of Solution Preparation........................................................................ 79

4.4.1 Solid Solute and Molarity....................................................................80
4.4.2 Solid Solute and Normality................................................................. 81
4.4.3 Solution Preparation by Dilution......................................................... 82
4.5 Stoichiometry of Titration Reactions............................................................... 82
4.6 Standardization.................................................................................................84
4.6.1 Standardization Using a Standard Solution........................................84
4.6.2 Standardization Using a Primary Standard........................................ 86
4.6.3 Titer..................................................................................................... 88
4.7 Percentage Analyte Calculations...................................................................... 88
4.8 Volumetric Glassware....................................................................................... 91
4.8.1 Volumetric Flask................................................................................. 91
4.8.2 Pipet.....................................................................................................94
4.8.3 Buret.................................................................................................... 98
4.8.4 Cleaning and Storing Procedures...................................................... 100
4.9 Pipetters, Automatic Titrators, and Other Devices........................................ 100
4.9.1 Pipetters............................................................................................. 100
4.9.2 Bottle-Top Dispensers....................................................................... 102
4.9.3 Digital Burets and Automatic Titrators............................................. 102
4.10 Calibration of Glassware and Devices........................................................... 103
4.11 Analytical Technique...................................................................................... 103

Chapter 5 Applications of Titrimetric Analysis......................................................................... 113

5.1 Introduction.................................................................................................... 113
5.2 Acid–Base Titrations and Titration Curves.................................................... 113
5.2.1 Titration of Hydrochloric Acid.......................................................... 113
5.2.2 Titration of Weak Monoprotic Acids................................................ 115
5.2.3 Titration of Monobasic Strong and Weak Bases............................... 116
5.2.4 Equivalence Point Detection............................................................. 116
5.2.5 Titration of Polyprotic Acids: Sulfuric Acid and Phosphoric
Acid............................................................................................ 118
5.2.6 Titration of Potassium Biphthalate.................................................... 121
5.2.7 Titration of Tris-(Hydroxymethyl)Amino Methane.......................... 122
5.2.8 Titration of Sodium Carbonate.......................................................... 122
5.3 Examples of Acid/Base Determinations........................................................ 123
5.3.1 Alkalinity of Water or Wastewater.................................................... 124
5.3.2 Back Titration Applications.............................................................. 124
5.3.3 Indirect Titration Applications.......................................................... 126
5.4 Other Acid/Base Applications........................................................................ 127
5.5 Buffer Solution Applications.......................................................................... 127
5.5.1 Conjugate Acids and Bases............................................................... 128
5.5.2 Henderson–Hasselbalch Equation..................................................... 129
5.6 Complex Ion Formation Reactions................................................................. 133
5.6.1 Introduction....................................................................................... 133
5.6.2 Complex Ion Terminology................................................................ 133
5.6.3 EDTA and Water Hardness............................................................... 135
5.6.4 Expressing Concentration Using Parts per Million.......................... 138
5.6.4.1 Solution Preparation.......................................................... 139
5.6.5 Water Hardness Calculations............................................................ 141
5.6.6 Other Uses of EDTA Titrations......................................................... 143
x Contents

5.7 Oxidation–Reduction Reactions..................................................................... 144

5.7.1 Review of Basic Concepts and Terminology.................................... 144
5.7.2 The Ion-Electron Method for Balancing Equations.......................... 147
5.7.3 Analytical Calculations..................................................................... 148
5.7.4 Applications....................................................................................... 150
5.7.4.1 Potassium Permanganate................................................... 150
5.7.4.2 Iodometry: An Indirect Method........................................ 150
5.7.4.3 Prereduction and Preoxidation.......................................... 152
5.8 Other Examples.............................................................................................. 152

Chapter 6 Introduction to Instrumental Analysis...................................................................... 165

6.1 Review of the Analytical Process................................................................... 165
6.2 Instrumental Analysis Methods..................................................................... 166
6.3 Basics of Instrumental Measurement............................................................. 167
6.3.1 Sensors, Signal Processors, Readouts, and Power Supplies.............. 168
6.3.2 Calibration of an Analytical Instrument........................................... 168
6.3.3 Mathematics of Linear Relationships................................................ 170
6.3.4 Method of Least Squares................................................................... 171
6.3.5 The Correlation Coefficient............................................................... 172
6.4 Preparation of Standards................................................................................ 172
6.5 Blanks and Controls....................................................................................... 173
6.5.1 Reagent Blanks.................................................................................. 173
6.5.2 Sample Blanks................................................................................... 174
6.5.3 Controls............................................................................................. 174
6.6 Post-Run Calculations in Instrumental Analysis............................................ 174
6.6.1 Calculation of ppm Analyte in a Solution Given Mass and
Volume Data...................................................................................... 175
6.6.2 Calculation of ppm Analyte in a Solid Sample Given Mass Data......... 175
6.6.3 Calculation of the Mass of Analyte Found in an Extract.................. 175
6.6.4 Calculation of ppm Analyte in a Liquid or Solid That Was
Extracted........................................................................................... 176
6.6.5 Calculation When a Dilution Is Involved.......................................... 176
6.7 Laboratory Data Acquisition and Information Management......................... 178
6.7.1 Data Acquisition................................................................................ 178
6.7.2 Laboratory Information Management............................................... 179

Chapter 7 Introduction to Spectrochemical Methods................................................................ 185

7.1 Introduction.................................................................................................... 185
7.2 Characterizing Light....................................................................................... 185
7.2.1 Wavelength, Speed, Frequency, Energy, and Wavenumber.............. 186
7.3 The Electromagnetic Spectrum...................................................................... 189
7.4 Refractometry................................................................................................. 190
7.5 Absorption and Emission of Light................................................................. 193
7.5.1 Brief Summary.................................................................................. 193
7.5.2 Atoms vs. Molecules and Complex Ions........................................... 196
7.5.3 Absorption Spectra............................................................................ 197
7.5.4 Light Emission.................................................................................. 201
7.6 Absorbance, Transmittance, and Beer’s Law.................................................202
7.7 Effect of Concentration on Spectra................................................................207
Contents xi

Chapter 8 UV-Vis and IR Molecular Spectrometry................................................................... 215

8.1 Review............................................................................................................ 215
8.2 UV-Vis Instrumentation................................................................................. 215
8.2.1 Sources.............................................................................................. 215
8.2.1.1 Tungsten Filament Lamp................................................... 215
8.2.1.2 Deuterium Lamp................................................................ 216
8.2.1.3 Xenon Arc Lamp............................................................... 216
8.2.2 Wavelength Selection........................................................................ 216
8.2.2.1 Absorption Filters.............................................................. 217
8.2.2.2 Monochromators................................................................ 217
8.2.3 Sample Compartment........................................................................ 220
8.2.3.1 Single-Beam Spectrophotometer....................................... 220
8.2.3.2 Beam Splitting and Chopping........................................... 221
8.2.3.3 Double-Beam Designs....................................................... 222
8.2.3.4 Diode Array Design........................................................... 223
8.2.3.5 Summary........................................................................... 225
8.2.4 Detectors........................................................................................... 226
8.2.4.1 Photomultiplier Tube......................................................... 226
8.2.4.2 Photodiodes....................................................................... 228
8.3 Cuvette Selection and Handling..................................................................... 228
8.4 Interferences, Deviations, Maintenance, and Troubleshooting...................... 229
8.4.1 Interferences...................................................................................... 229
8.4.2 Deviations.......................................................................................... 229
8.4.3 Maintenance...................................................................................... 230
8.4.4 Troubleshooting................................................................................. 230
8.5 Fluorometry.................................................................................................... 231
8.6 Introduction to IR Spectrometry.................................................................... 233
8.7 IR Instrumentation......................................................................................... 234
8.8 Sampling......................................................................................................... 235
8.8.1 Liquid Sampling................................................................................ 235
8.9 Solid Sampling...............................................................................................240
8.9.1 Solution Prepared and Placed in a Liquid Sampling Cell.................240
8.9.2 Thin Film Formed by Solvent Evaporation.......................................240
8.9.3 KBr Pellet..........................................................................................240
8.9.4 Nujol Mull......................................................................................... 242
8.9.5 Reflectance Methods......................................................................... 242
8.9.5.1 Specular Reflectance......................................................... 242
8.9.5.2 Internal Reflectance........................................................... 242
8.9.5.3 Diffuse Reflectance...........................................................244
8.9.6 Gas Sampling....................................................................................244
8.10 Basic IR Spectra Interpretation......................................................................244
8.11 Quantitative Analysis..................................................................................... 247

Chapter 9 Atomic Spectroscopy................................................................................................ 259

9.1 Review and Comparisons............................................................................... 259
9.2 Brief Summary of Techniques and Instrument Designs................................260
9.3 Flame Atomic Absorption.............................................................................. 262
9.3.1 Flames and Flame Processes............................................................ 262
9.3.2 Spectral Line Sources....................................................................... 263
xii Contents

9.3.2.1 Hollow Cathode Lamp.......................................................264

9.3.2.2 Electrodeless Discharge Lamp.......................................... 265
9.3.3 Premix Burner................................................................................... 265
9.3.4 Optical Path....................................................................................... 267
9.3.5 Practical Matters and Applications................................................... 268
9.3.5.1 Slits and Spectral Lines..................................................... 268
9.3.5.2 Linear and Nonlinear Standard Curves............................. 269
9.3.5.3 Hollow Cathode Lamp Current......................................... 271
9.3.5.4 Lamp Alignment................................................................ 271
9.3.5.5 Aspiration Rate.................................................................. 271
9.3.5.6 Burner Head Position......................................................... 271
9.3.5.7 Fuel and Oxidant Sources and Flow Rates........................ 271
9.3.6 Interferences...................................................................................... 271
9.3.6.1 Chemical Interferences...................................................... 272
9.3.6.2 Spectral Interferences........................................................ 273
9.3.7 Safety and Maintenance.................................................................... 274
9.4 Graphite Furnace Atomic Absorption............................................................ 275
9.4.1 General Description.......................................................................... 275
9.4.2 Advantages and Disadvantages......................................................... 277
9.5 Inductively Coupled Plasma........................................................................... 278
9.6 Miscellaneous Atomic Techniques................................................................. 281
9.6.1 Flame Photometry............................................................................. 281
9.6.2 Cold Vapor Mercury.......................................................................... 282
9.6.3 Hydride Generation........................................................................... 282
9.6.4 Spark Emission.................................................................................. 282
9.6.5 Atomic Fluorescence......................................................................... 282
9.7 Summary of Atomic Techniques.................................................................... 282

Chapter 10 Introduction to Chromatography............................................................................... 291

10.1 Introduction.................................................................................................... 291
10.2 Chromatography............................................................................................. 291
10.3 “Types” of Chromatography........................................................................... 292
10.3.1 Partition Chromatography................................................................. 292
10.3.2 Adsorption Chromatography............................................................. 293
10.3.3 Ion-Exchange Chromatography........................................................ 294
10.3.4 Size Exclusion Chromatography....................................................... 295
10.4 Chromatography Configurations.................................................................... 295
10.4.1 Paper and Thin-Layer Chromatography........................................... 296
10.4.2 Classical Open-Column Chromatography........................................ 298
10.4.3 Instrumental Chromatography.......................................................... 301
10.4.4 Instrumental Chromatogram............................................................. 301
10.4.5 Quantitative Analysis with GC and HPLC....................................... 305
10.5 Electrophoresis...............................................................................................306

Chapter 11 Gas Chromatography................................................................................................ 311

11.1 Overview........................................................................................................ 311
11.2 Vapor Pressure and Solubility........................................................................ 311
11.3 Instrument Components................................................................................. 312
11.4 Sample Injection............................................................................................. 314
Contents xiii

11.5 Column Details............................................................................................... 316

11.5.1 Instrument Logistics.......................................................................... 316
11.5.2 Packed, Open Tubular, and Preparative Columns............................. 317
11.5.3 The Nature and Selection of the Stationary Phase............................ 318
11.5.4 Column Temperature......................................................................... 319
11.5.5 Carrier Gas Flow Rate...................................................................... 320
11.6 Detectors......................................................................................................... 321
11.6.1 Flame Ionization Detector (FID)...................................................... 321
11.6.2 Thermal Conductivity Detector (TCD)............................................. 322
11.6.3 Electron Capture Detector (ECD)..................................................... 323
11.6.4 Nitrogen/Phosphorus Detector (NPD).............................................. 324
11.6.5 Flame Photometric Detector (FPD).................................................. 324
11.6.6 Electrolytic Conductivity (Hall Detector)......................................... 324
11.6.7 Gas Chromatography–Mass Spectrometry (GC-MS)....................... 324
11.6.8 Photoionization Detector (PID)......................................................... 325
11.7 Qualitative Analysis....................................................................................... 325
11.8 Quantitative Analysis..................................................................................... 326
11.8.1 Quantitation Methods........................................................................ 326
11.8.2 Response Factor Method................................................................... 326
11.8.3 Internal Standard Method................................................................. 327
11.8.4 Standard Additions Method.............................................................. 328
11.9 Troubleshooting.............................................................................................. 329
11.9.1 Diminished Peak Size....................................................................... 329
11.9.2 Unsymmetrical Peak Shapes............................................................. 329
11.9.3 Altered Retention Times................................................................... 330
11.9.4 Baseline Drift.................................................................................... 330
11.9.5 Baseline Perturbations....................................................................... 330
11.9.6 Appearance of Unexpected Peaks..................................................... 330

Chapter 12 High-Performance Liquid Chromatography and Electrophoresis............................ 341

12.1 Introduction.................................................................................................... 341
12.1.1 Summary of Method......................................................................... 341
12.1.2 Comparisons with GC....................................................................... 341
12.2 Mobile Phase Considerations......................................................................... 342
12.3 Solvent Delivery.............................................................................................344
12.3.1 Pumps................................................................................................344
12.3.2 Gradient vs. Isocratic Elution............................................................ 345
12.4 Sample Injection.............................................................................................346
12.5 Column Selection...........................................................................................348
12.5.1 Normal Phase Columns.....................................................................348
12.5.2 Reverse-Phase Columns....................................................................348
12.5.3 Adsorption Columns......................................................................... 349
12.5.4 Ion Exchange and Size Exclusion Columns...................................... 349
12.5.5 The Size of the Stationary Phase Particles........................................ 349
12.5.6 Column Selection.............................................................................. 349
12.6 Detectors......................................................................................................... 350
12.6.1 UV Absorption.................................................................................. 350
12.6.2 Diode Array....................................................................................... 351
12.6.3 Fluorescence...................................................................................... 351
12.6.4 Refractive Index................................................................................ 353
xiv Contents

12.6.5 Electrochemical................................................................................. 354

12.6.5.1 Conductivity....................................................................... 354
12.6.5.2 Amperometric.................................................................... 354
12.7 Qualitative and Quantitative Analysis............................................................ 355
12.8 Troubleshooting.............................................................................................. 356
12.8.1 Unusually High Pressure................................................................... 356
12.8.2 Unusually Low Pressure.................................................................... 356
12.8.2.1 System Leaks..................................................................... 356
12.8.2.2 Air Bubbles........................................................................ 357
12.8.2.3 Column “Channeling”....................................................... 357
12.8.2.4 Decreased Retention Time................................................ 357
12.8.2.5 Baseline Drift.................................................................... 357
12.9 Electrophoresis............................................................................................... 357
12.9.1 Introduction....................................................................................... 357
12.9.2 Capillary Electrophoresis.................................................................. 359
12.9.2.1 Electroosmotic Flow.......................................................... 361
12.9.2.2 Sample Introduction.......................................................... 361
12.9.2.3 Analyte Detection.............................................................. 361

Chapter 13 Mass Spectrometry.................................................................................................... 371

13.1 Basic Principles.............................................................................................. 371
13.2 Sample Inlet Systems and Ion Sources........................................................... 372
13.3 Mass Analyzers.............................................................................................. 373
13.4 The Ion Detector............................................................................................. 376
13.5 Mass Spectra................................................................................................... 377
13.6 ICP-MS........................................................................................................... 378
13.7 GC-MS........................................................................................................... 378
13.8 LC-MS............................................................................................................ 380
13.9 Tandem Mass Spectrometry........................................................................... 381

Chapter 14 Electroanalytical Methods........................................................................................ 387

14.1 Introduction.................................................................................................... 387
14.2 Transfer Tendencies: Standard Reduction Potentials..................................... 391
14.3 Determination of Overall Redox Reaction Tendency: E°cell............................ 393
14.4 The Nernst Equation....................................................................................... 394
14.5 Potentiometry................................................................................................. 396
14.5.1 Reference Electrodes......................................................................... 396
14.5.1.1 The Saturated Calomel Reference Electrode (SCE).......... 396
14.5.1.2 The Silver–Silver Chloride Electrode................................ 398
14.5.2 Indicator Electrodes.......................................................................... 399
14.5.2.1 The pH Electrode............................................................... 399
14.5.3 Combination Electrodes....................................................................400
14.5.3.1 The Combination pH Electrode.........................................400
14.5.3.2 Ion-Selective Electrodes.................................................... 401
14.5.4 Other Details of Electrode Design....................................................403
14.5.5 Care and Maintenance of Electrodes................................................403
14.5.6 Potentiometric Titrations...................................................................404
14.6 Voltammetry and Amperometry....................................................................405
14.6.1 Voltammetry......................................................................................405
Contents xv

14.6.2 Amperometry....................................................................................406
14.7 Karl Fischer Titration.....................................................................................406
14.7.1 End Point Detection..........................................................................406
14.7.2 Elimination of Extraneous Water......................................................407
14.7.3 The Volumetric Method....................................................................407
14.7.4 The Coulometric Method..................................................................409

Chapter 15 Miscellaneous Instrumental Techniques................................................................... 417

15.1 X-Ray Methods............................................................................................... 417
15.1.1 Introduction....................................................................................... 417
15.1.2 X-Ray Diffraction Spectroscopy....................................................... 418
15.1.3 X-Ray Fluorescence Spectroscopy.................................................... 421
15.1.4 Applications....................................................................................... 421
15.1.5 Safety Issues Concerning X-Rays..................................................... 422
15.2 Nuclear Magnetic Resonance Spectroscopy.................................................. 422
15.2.1 Introduction....................................................................................... 422
15.2.2 Instrumentation................................................................................. 423
15.2.3 The NMR Spectrum.......................................................................... 425
15.2.3.1 Chemical Shifts................................................................. 425
15.2.3.2 Peak Splitting and Integration........................................... 427
15.2.4 Solvents and Solution Concentration................................................. 428
15.2.5 Analytical Uses................................................................................. 428
15.3 Viscosity......................................................................................................... 428
15.3.1 Introduction....................................................................................... 428
15.3.2 Definitions......................................................................................... 429
15.3.3 Temperature Dependence.................................................................. 430
15.3.4 Capillary Viscometry........................................................................ 430
15.3.5 Rotational Viscometry...................................................................... 433
15.4 Thermal Analysis........................................................................................... 434
15.4.1 Introduction....................................................................................... 434
15.4.2 DTA and DSC................................................................................... 434
15.4.3 DSC Instrumentation......................................................................... 436
15.4.4 Applications of DSC.......................................................................... 437
15.5 Optical Rotation............................................................................................. 437
Appendix 1: Formulas for Solution Concentration and Preparation Calculations................ 443
Appendix 2: T
 he Language of Quality Assurance and Good Laboratory Practice
(GLP) Laws: A Glossary........................................................................................ 447
Appendix 3: S
 ignificant Figure Rules......................................................................................... 451
Appendix 4: Answers to Questions and Problems..................................................................... 453
List of Experiments
Experiment 1: Assuring the Quality of Weight Measurements...................................................... 14
Experiment 2: Weight Uniformity of Dosing Units....................................................................... 15
Experiment 3: A Study of the Dissolving Properties of Water, Some Common Organic
Liquids, and Laboratory Acids............................................................................... 42
Experiment 4: Loss on Drying....................................................................................................... 64
Experiment 5: Particle Sizing........................................................................................................ 65
Experiment 6: The Determination of Salt in a Salt–Sand Mixture................................................ 65
Experiment 7: The Gravimetric Determination of Sulfate in a Commercial Unknown................ 65
Experiment 8: High-Precision Glassware: A Calibration Experiment........................................ 104
Experiment 9: Preparation and Standardization of HCl and NaOH Solutions............................ 106
Experiment 10: Titrimetric Analysis of a Commercial Soda Ash Unknown for Sodium
Carbonate............................................................................................................. 152
Experiment 11: Titrimetric Analysis of a Commercial KHP Unknown for KHP.......................... 152
Experiment 12: EDTA Titrations................................................................................................... 153
Experiment 13: Plotting a Standard Curve Using Excel Spreadsheet Software (Version 2010)........179
Experiment 14: Percentage of Sugar in Soft Drinks by Refractometry......................................... 207
Experiment 15: Colorimetric Analysis of Prepared and/or Real Water Samples for Iron............. 207
Experiment 16: Design an Experiment: A Study of the Effect of pH on the Analysis of
Water Samples for Iron........................................................................................208
Experiment 17: Design an Experiment: Determining the Concentration at Which a Beer’s
Law Plot Becomes Nonlinear............................................................................... 208
Experiment 18: The Determination of Phosphorus in Environmental Water................................ 208
Experiment 19: Spectrophotometric Analysis of a Prepared Sample for Toluene......................... 248
Experiment 20: Extraction of Iodine with Cyclohexane................................................................ 248
Experiment 21: Determination of Nitrate in Drinking Water by UV Spectrophotometry............. 249
Experiment 22: Fluorometric Analysis of a Prepared Sample for Riboflavin............................... 249
Experiment 23: Design an Experiment: Determination of Riboflavin in a Vitamin Tablet
Using Fluorometry............................................................................................... 250
Experiment 24: Quantitative Infrared Analysis of Isopropyl Alcohol in Toluene......................... 250
Experiment 25: Quantitative Flame Atomic Absorption Analysis of a Prepared Sample............. 284
Experiment 26: The Analysis of Soil Samples for Iron Using Atomic Absorption....................... 284
Experiment 27: Design an Experiment: A Study to Determine the Optimum pH for the
Extraction Solution for Experiment 26................................................................ 285
Experiment 28: The Determination of Sodium in Soda Pop......................................................... 285
Experiment 29: Design an Experiment: Sodium in Soda Pop by the Standard Additions
Method................................................................................................................. 286
Experiment 30: Design an Experiment: Analysis of Fertilizer for Potassium............................... 286
Experiment 31: Thin-Layer Chromatography Analysis of Cough Syrups for Dyes......................306
Experiment 32: Thin-Layer Chromatography Analysis of Jelly Beans for Food Coloring........... 307
Experiment 33: A Qualitative Gas Chromatography Analysis of a Prepared Sample................... 330
Experiment 34: The Quantitative Gas Chromatography Analysis of a Prepared Sample
for Toluene by the Internal Standard Method...................................................... 331
Experiment 35: The Determination of Ethanol in Wine by Gas Chromatography and the
Internal Standard Method..................................................................................... 332

xvii
xviii List of Experiments

Experiment 36: Design an Experiment: Determination of Ethanol in Cough Medicine or

Other Pharmaceutical Preparation........................................................................ 333
Experiment 37: A Study of the Effect of the Changing of GC Instrument Parameters on
Resolution............................................................................................................. 333
Experiment 38: The Quantitative Determination of Methyl Paraben in a Prepared Sample by
HPLC.................................................................................................................... 362
Experiment 39: HPLC Determination of Caffeine in Soda Pop.................................................... 363
Experiment 40: Design an Experiment: Dependence of Caffeine Analysis on the pH of the
Mobile Phase........................................................................................................ 364
Experiment 41: The Analysis of Mouthwash by HPLC: A Research Experiment........................ 364
Experiment 42: The Determination of 4-Hydroxyacetophenone by Capillary Electrophoresis.... 365
Experiment 43: The Quantitative GC-MS Analysis of a Prepared Sample for Chlorobenzene
by the Internal Standard Method.......................................................................... 382
Experiment 44: GC-MS Determination of Ethylbenzene in Gasoline by Combined Internal
Standard and Standard Additions Methods.......................................................... 382
Experiment 45: Determination of the pH of Soil Samples............................................................ 409
Experiment 46: Analysis of a Prepared Unknown for Fluoride Using an Ion-Selective
Electrode............................................................................................................... 409
Experiment 47: Design an Experiment: Determination of Fluoride in Toothpaste Using an
Ion-Selective Electrode........................................................................................ 410
Experiment 48: Operation of Metrohm Model 701 Karl Fischer Titrator (for Liquid
Samples)............................................................................................................... 410
Preface
The primary purpose of this text continues to be as a training manual for chemistry-based labora-
tory technicians. It is designed to emphasize the practical rather than the theorical. The practical
begins with classical quantitative analysis, because this is what instills the mindset of analytical
skill and technique into the students’ psyche, and very practicing scientists should agree that this
is a very important part of a technician’s training. But equally important is what follows this in the
book: a very practical approach to the complex world of the sophisticated electronic instrumenta-
tion that a technician will find in common use in the real-world laboratory. My hope is that labora-
tory supervisors will find that technicians who have utilized this textbook will have an analytical
mindset and a basic understanding of the analytical instrumentation needed for success on the job.
It has been 10 years since the publication of the third edition of Analytical Chemistry for
Technicians. I have taught the sequence of courses that use this text over 20 times since then. Each
time I teach these courses, it seems I have fresh ideas and new developments to discuss with my
students. These have resulted in new drawings for my PowerPoint slides and new (and I hope better)
explanations of what can be complex instrument designs and functions. It is true that my students
have a limited background in chemistry when they come to me, and so I strive to write, draw, and
speak with this in mind.
And now the time has come for the fourth edition. What is new and what has changed? Following
is the list:

• Over 150 new photographs and either new or reworked drawings spanning every chapter
to assist the visual learner.
• A new chapter on mass spectrometry.
• Thirteen new laboratory experiments, including nine “design an experiment” exercises.
• An “Introduction to Laboratory Work” section before Chapter 1 to give students a pre-
view of general laboratory considerations, safety, laboratory notebooks, and instrumental
analysis.
• “Application Notes” in each chapter. A few of these are carryovers of the “Workplace
Scenes” in the third edition, but most are new. The intent is to give students a larger hint of
how specific techniques may be routinely used in the laboratory.
• Calculation summary tables in Chapters 3 and 4.
• Relevant section headings in the end-of-chapter Questions and Problems section to help
better organize the material for students.
• An appendix providing a glossary of quality assurance and good laboratory practice (GLP)
terms.
• More end-of-chapter problems in Chapters 1, 2, 3, 6, and 14 covering statistics, liquid–liquid
extraction, gravimetric analysis, post-run instrumental analysis, and electrode potential.
• More examples of calculations covering liquid–liquid extraction theory and post-run
instrumental analysis in Chapters 2 and 6.
• The topic of refractometry has been moved to Chapter 7 from Chapter 15 since it repre-
sents a basic technique involving light.
• The topics of liquid–liquid extraction, solid–liquid extraction, and distillation–deionization
have been moved to Chapter 2 from Chapter 11 as sample and solution preparation tech-
niques rather than analytical separation techniques. Chapter 11 has become Chapter 10 and
is now dedicated to chromatography, and this is reflected in the chapter title “Introduction
to Chromatography.”

xix
© 2010 Taylor & Francis Group, LLC
xx Preface

• The topic of capillary electrophoresis has been moved from the former Chapter 11 to the
new Chapter 12 and expanded.
• Chapter 1 has been expanded to include more information on statistics.
• Expanded end-of-chapter “report”-type questions have been included in Chapters 5, 7, 8, 9,
11, 12, and 14 to give improved guidance to students as to how to answer these questions.
• De-emphasis of the Kjeldahl method in Chapter 5.
• Appendix 1 has been reworked to include the percent unit and deleting standardization and
percentages of analyte formulas.
• The material from the former Chapter 10 (“Other Spectroscopic Methods”) has been
moved to the new mass spectrometry chapter and to a new Chapter 15, “Miscellaneous
Instrumental Technique.”
• Coverage of the mathematical relationships involving wavelength, frequency, energy, and
wavenumber have been retained, but the calculations involving these relationships have
been deleted.
• The first few sections of Chapter 11, “Gas Chromatography,” have been rewritten to reflect
the popularity of capillary columns and to include more information about injectors.
GC-MS coverage has been moved to Chapter 13, “Mass Spectrometry.”
• The chapters on bioanalysis and physical testing methods have been deleted. Approximately
25% of this latter chapter is in the new Chapter 15, “Miscellaneous Instrumental Technique.”
• Coverage of recrystallization has been deleted.

One of the biggest changes is the introduction of an entirely new chapter on mass spectrometry,
Chapter 13, which includes coverage of GC-MS, LC-MS, LC-MS-MS, and ICP-MS. This chapter
follows other chapters on basic quantitative analysis, atomic and molecular spectroscopy, and gas
and liquid chromatography. It comes in the third course in the analytical chemistry sequence at
Southeast Community College, and while the students’ background is far from advanced at that
point, I find that they are well prepared for an illustrated but limited discussion of this important
topic.
What do I mean by illustrated? Reading this text, students will see dozens of new illustrative
drawings and photographs throughout, not just in Chapter 13. I find that most of my students learn
and I can teach best from illustrations. Whether the topic is laboratory glassware, spectrophotom-
eters, gas chromatographs, mass spectrometers, or electrodes, students are visual learners, and all
the drawings and photographs were created by me. I had no outside artist or photographer for this
text. Over the years, I have learned to use the drawing tools in PowerPoint to great advantage. I have
also learned how to use digital photography to great advantage. The drawings and photographs are
exactly as I intended them to appear because I created them. Some were done over the last 10 years
of teaching and others were done as I sat at my desk or laboratory bench the past 2 years and con-
templated how best to convey the information in this fourth edition.
From monochromators to capillary columns, from absorption spectra to standard curves, from
titration curves to electrodes, from double-beam spectrophotometers to quadrupole mass analyzers,
and from flame atomic absorption to ICP-MS, there are many new and, I trust, improved illustra-
tions and photographs for students to ponder.
Of course, I am anxious for students to get their hands on this fourth edition and to begin to
peruse its contents. It comes to you after 36 years of practice, and it has evolved considerably since
the first edition appeared in 1988. Good luck to you!

John Kenkel
Southeast Community College

© 2010 Taylor & Francis Group, LLC

Acknowledgments
I am very grateful to Southeast Community College for the professional niche they provided me
starting in 1977 and continuing for a full 36 years. In all that time, I have come to know many stu-
dents who are hungry to learn about science and to have a career in the field. They were my primary
inspiration year after year.
As always, I am indebted to a number of people who assisted in some direct way during the
development of the manuscript. My editor at CRC Press, Barbara Glunn, offered me the opportunity
and was very friendly and encouraging at every step along the way, especially when I asked if I
could delay the project six months due to a serious family illness.
A number of my colleagues at institutions across the United States served as reviewers on this
project and I appreciate their work very much. They are:

Tracy Holbrook, Cape Fear Community College

Cynthia Peck, Delta College
Michele Mangels, Cincinnati State Technical and Community College
Susan Marine, Miami University Middletown
Charlie Newman, Mount San Antonio College
Onofrio Gaglione, College of Southern Nevada
Kazumasa Lindley, College of Southern Nevada
Renee Madyun, Los Angeles Trade Tech College

I am indebted to my wife, Lois, for her superior proofreading skills. One thing I have learned
during my various writing projects over the years is that many errors seem to creep in unno-
ticed despite a seemingly thorough review by the author. For this project, Lois’ help was greatly
appreciated.

John Kenkel
Southeast Community College

xxi
© 2010 Taylor & Francis Group, LLC
Author
John Kenkel is a chemistry instructor at Southeast Community College (SCC) in Lincoln,
Nebraska. Throughout his 36-year career at SCC, he has been directly involved in the education of
chemistry-­based laboratory technicians in a vocational program. He has also been heavily involved
in chemistry-based laboratory technician education on a national level, having served on a num-
ber of American Chemical Society (ACS) committees, including the Committee on Technician
Activities and the Coordinating Committee for the Voluntary Industry Standards project. In addi-
tion to these, he has served a 5-year term on the ACS Committee on Chemistry in the Two-Year
College, the committee that administers the Two-Year College Chemistry Consortium (2YC3) con-
ferences. He was the general chair of this committee in 1996. He later served a 3-year term on this
committee as the Industrial Sponsor Chair (2006–2008).
Mr. Kenkel has authored several popular textbooks for chemistry-based technician education.
Three editions of Analytical Chemistry for Technicians preceded the current edition, the first pub-
lished in 1988, the second in 1994, and the third in 2003. In addition, he has authored five other
books: Basic Chemistry Concepts and Exercises, published in 2011, Chemistry: An Industry-Based
Introduction and Chemistry: An Industry-Based Laboratory Manual, both published in 2000–
2001, Analytical Chemistry Refresher Manual, published in 1992, and A Primer on Quality in the
Analytical Laboratory, which was published in 2000. All were published through CRC Press/Lewis
Publishers.
Mr. Kenkel has been the principal investigator for a series of curriculum development project
grants funded by the National Science Foundation’s Advanced Technological Education Program,
from which four of his nine books evolved. He has also authored or coauthored four articles on the
curriculum work in the Journal of Chemical Education and has presented this work at more than
20 conferences.
In 1996, Mr. Kenkel won the prestigious National Responsible Care Catalyst Award for excel-
lence in chemistry teaching sponsored by the Chemical Manufacturer’s Association. He has a mas-
ter’s degree in chemistry from the University of Texas at Austin (1972) and a bachelor’s degree in
chemistry (1970) from Iowa State University. His research at the University of Texas was directed by
Professor Allen Bard. He was employed as a chemist from 1973 to 1977 at Rockwell International’s
Science Center in Thousand Oaks, California.

xxiii
© 2010 Taylor & Francis Group, LLC
Introduction to Laboratory Work
GENERAL CONSIDERATIONS
There is laboratory work, and then there is laboratory work! No doubt you have had a general
chemistry course before enrolling in the course for which this textbook is used. And no doubt there
was a laboratory section included in this general chemistry course. In this general chemistry labo-
ratory section, you paid attention to detail to the extent that you were able to pass the class with a
satisfactory grade. Perhaps you worked as part of a group of other students and never were quite on
your own for any of the tasks involved. You probably used ordinary laboratory balances, prepared
solutions in Erlenmeyer flasks or beakers, and used graduated cylinders to transfer volumes of solu-
tions from one container to another. In short, you did the work, but it was not important to strive for
highly precise measurements or results nor perhaps even highly accurate measurements or results.
All of that is about to change.
Perhaps you wondered about the nature of laboratory work in the real world. Perhaps you thought
about the analysis of pharmaceutical, food, or beverage samples, that is, samples that represent
products consumed by the general public. Or perhaps you thought about the analysis of a hospital
patient’s blood or urine. Would a supervisor demand more careful attention to detail in these situ-
ations? Indeed, the answer is a resounding “yes.” In this textbook, high precision and high accu-
racy are the name of the game. You will usually be working by yourself on a given analysis in the
laboratory and striving to meet the demands of your instructor to develop your analytical skill and
technique so you will be qualified to work in a real-world analytical laboratory. After all, you will
be using balances where the weight of your fingerprint is measureable and where you strive to keep
containers to be weighed free of fingerprints. You will be using glassware where a fraction of a drop
will make a difference in the position of a meniscus on a calibration line and make a difference in
the results. In short, when you complete the class for which this textbook is used and you enter the
real world, you will have the confidence to be successful no matter what demands are thrown at
you. You will be an analytical laboratory technician who works at a high level of analytical skill to
complete the tasks assigned.

SAFETY IN THE ANALYTICAL LABORATORY

The analytical chemistry laboratory is a very safe place to work. However, that is not to say that
the laboratory is free of hazards. The dangers associated with contact with hazardous chemicals,
flames, etc. are very well documented, and as a result, laboratories are constructed and procedures
are carried out with these dangers in mind. Hazardous chemical fumes are, for example, vented
into the outdoor atmosphere with the use of fume hoods. Safety showers for diluting spills of con-
centrated acids on clothing are now commonplace. Eyewash stations are strategically located for
immediately washing one’s eyes in the event of accidental contact with a hazardous chemical. Fire
blankets, extinguishers, and sprinkler systems are also located in and around analytical laboratories
for immediately extinguishing flames and fires. Also, a variety of safety gear, such as safety glasses,
aprons, and shields, is available. There is never a good excuse for personal injury in a well-equipped
laboratory where well-informed analysts are working.
Although the pieces of equipment mentioned above are now commonplace, it remains for the
analysts to be well-informed of potential dangers and of appropriate safety measures. To this end,
we list below some safety tips of which any laboratory worker must be aware. This list should be
studied carefully by all students who have chosen to enroll in an analytical chemistry course. This
is not intended to be a complete list, however. Students should consult with their instructor in order

xxv
© 2010 Taylor & Francis Group, LLC
xxvi Introduction to Laboratory Work

to establish safety ground rules for the particular laboratory in which they will be working. Total
awareness of hazards and dangers and what to do in case of an accident is the responsibility of each
student and the instructor.

1. Safety glasses must be worn at all times by students and instructors. Visitors to the labora-
tory must be appropriately warned and safety glasses made available to them.
2. Fume hoods must be used when working with chemicals that may produce hazardous
fumes.
3. The location of fire extinguishers, safety showers, and eyewash stations must be known.
4. All laboratory workers must know how and when to use the items listed in number 3.
5. There must be no unsupervised or unauthorized work in the laboratory.
6. A laboratory is never a place for practical jokes or pranks.
7. The toxicity of all the chemicals you will be working with must be known. Consult the
instructor, material safety data sheets (MSDSs), safety charts, and container labels for
safety information about specific chemicals. Recently, many common organic chemicals,
such as benzene, carbon tetrachloride, and chloroform, have been deemed unsafe. Eating,
drinking, or smoking in the laboratory is never allowed.
8. Never use laboratory containers (beakers or flasks) to drink beverages.
9. Shoes (not open-toed) must always be worn; hazardous chemicals may be spilled on the
floor or feet.
10. Long hair should always be tied back.
11. Mouth pipetting is never allowed.
12. Cuts and burns must be immediately treated. Use ice on new burns and consult a doctor for
serious cuts.
13. In the event of acid spills on one’s person, flush thoroughly with water immediately. Be
aware that acid–water mixtures will produce heat. Removing clothing from the affected
area while water flushing may be important so as to not trap hot acid–water mixtures
against the skin. Acids or acid–water mixtures can cause very serious burns if left in con-
tact with skin, even if only for a very short time.
14. Weak acids (such as citric acid) should be used to neutralize base spills, and weak bases
(such as sodium carbonate) should be used to neutralize acid spills. Solutions of these
should be readily available in the laboratory in case of emergency.
15. Dispose of all waste chemicals from the experiments according to your instructor’s
directions.
16. In the event of an accident, report immediately to your instructor, regardless of how minor
you perceive it to be.
17. Always be watchful and considerate of others working in the laboratory. It is important not
to jeopardize their safety or yours.
18. Always use equipment that is in good condition. Any piece of glassware that is cracked or
chipped should be discarded and replaced.

It is impossible to foresee all possible hazards that may manifest themselves in an analytical
laboratory. Therefore, it is very important for all students to listen closely to their instructor and
obey the rules of their particular laboratory in order to avoid injury. Neither the author of this text
nor its publisher assumes any responsibility whatsoever in the event of injury.

THE LABORATORY NOTEBOOK

Another item basic to all analytical laboratory work is proper record keeping. In the real world,
laboratory notebooks are considered legal documents. Indeed, good record keeping is central to

© 2010 Taylor & Francis Group, LLC

Introduction to Laboratory Work xxvii

good analytical science. Not only must data obtained from samples and analytes be recorded, but it
must be recorded with diligence and with considerable thought being given to integrity and purpose.
Accordingly, an analytical laboratory will usually have strict guidelines with respect to labora-
tory notebooks. The following typifies what these guidelines might be.

I. General Guidelines
A. All notebooks must begin with a table of contents. All pages must be numbered, and
these numbers must be referenced in the table of contents. The table of contents must
be updated as projects are completed and new projects begun.
B. All notebook entries must be made in ink. Use of graphite pencils or other erasable
writing instruments is strictly prohibited.
C. No data entries will be erased or made illegible. If an error was made, a single line is
drawn through the entry. Do not use correction fluid. Initial and date corrections and
indicate why the correction was necessary.
D. Under no circumstances will the notebook be taken or otherwise leave the laboratory
unless there are data to be recorded at a remote site, such as a remote sampling site, or
unless special permission is granted by the supervisor.
E. The following notebook format should be maintained for each project undertaken:
(1) title and date; (2) purpose or objectives statement; (3) data entries; (4) results;
(5) conclusions. Each of these are explained below. In each case, write out and under-
line the words “title and date,” “objective,” “data,” etc. to clearly identify the beginning
of each section.
F. Make notebook entries for a given project on consecutive pages where practical. Begin
a new project on the front side of a new page. You may skip pages only in order to
comply with this guideline.
G. Draw a single diagonal line through blank spaces that consist of four or more lines
(including any pages skipped according to guideline “F” above). These spaces should
be initialed and dated.
H. Never use a highlighter in a notebook.
I. Each notebook page must be signed, dated, and possibly witnessed.
II. Title and Date
A. All new experiments will begin with the title of the work and the date the work is per-
formed. If the work was continued on another date, that date must be indicated at the
point the work was restarted.
B. The title will reflect the nature of the work or shall be the title given to the project by
the study director.
III. Purpose or Objectives Statement
A. Following the title and date, a statement of the purpose or objective of the work will be
written. This statement should be brief and to the point.
B. If appropriate, the standard operating procedure (SOP) will be referenced in this
statement.
IV. Data Entries
A. Enter data into the notebook as the work is being performed. This means that loose
pieces of paper used for intermediate recordings are prohibited. Entries should be
made in ink only.
B. If there is any deviation from the SOP, permission must be obtained from the study
director, and this must be thoroughly documented by indicating exactly what the devi-
ation is and why it occurred.
C. The samples analyzed must be described in detail. Such descriptions may include the
source of the sample, what steps were taken to ensure that the sample represents the
whole (reference SOP if appropriate), and what special coding may be assigned and

© 2010 Taylor & Francis Group, LLC

Another random document with
no related content on Scribd:
 "You will naturally ask why I am telling these facts now. I have
two reasons. Fortune has deserted me at last. I had intended to
reveal Guy's parentage when he stood in the dock so deeply stained
with crime that part of the odium he incurred would necessarily fall
upon you. More recently I determined that I would refrain from
putting that coping stone on the edifice of my revenge. Not out of any
misplaced tenderness for you. Do not think that. My reason was a
purely selfish one. My adopted son had somehow endeared himself
to me. I foresaw in him an ornament to my own profession. I became
sentimental and so, foolish. I thought he should always remain my
son. I forgot that he had your blood in his veins and I let him fall
under your influence. I forgot too that a girl can shatter the most
complete philosophy with a glance of her eyes. The young fool has
fallen in love with Meriel Challys, and the consequence is that he has
got into his head a ridiculous idea that he must deliver himself up to
justice in order to make amends for his legitimate spoiling of the
Egyptians, Flurscheim and yourself. He is proposing to do so within
the next forty-eight hours, so you may have time to prevent his
voluntary martyrdom—a martyrdom he will certainly regret, judging
from my own experience. Do not think, however, that I am only
animated by Guy's interests. I am still keenly alive to my own safety.
I have had quite enough of prison life, and am well prepared with
means of escape, though I do not desire to end my existence just
yet. Of course, if you care to sacrifice your son in order that I shall
not escape, that is your affair. Guy knows nothing of his parentage,
though I have taken steps to inform him of it should you fail to do so.
I shall not leave him entirely in your hands."
Captain Marven laid the letter down, and, dropping his face in
his hands, he groaned aloud. His heart was sick with anguish. His
long lost son was returned to him, but in what guise? By training, by
profession, he was a thief. Guy Marven, his son, a thief! The horror
of it was almost too great to be borne! It was the bitterest blow of his
life, far more bitter even than the blow which had fallen when his
baby boy had been stolen from him. If Lynton Hora could have
watched the effect produced by his communication, even his thirst
for revenge would have been satisfied. But more bitter even than the
knowledge of what his son had become was the realisation of the
burden of duty which the revelation thrust upon him. As he realised
his duty in the matter, Captain Marven's face was grey with anguish.
He had found his son only to lose him again—to lose him amongst
the yellow-garbed denizens of the convict prison. More, it was he
who must, with his own hand, send him to that outer darkness. God
grant that his son would be a man! God grant it! That was Captain
Marven's earnest prayer.
Then his wife and Meriel? What if they were to learn of Guy's
relationship. Captain Marven could only dimly conceive the effect
upon them.
The servant came again to announce that the cab was awaiting
him. Marven rose, but it was as a man ten years older than the one
who had opened Hora's letter ten minutes before. His face was lined,
and his hand tremulous, but his lips were set firmly. He saw his duty
plainly before him. There was only one path he could tread, even
though every step on that path gave him a fresh pang. But he must
see Guy first, before he took that step.
He entered the cab and was driven to the Albany. He was more
master of himself by the time he arrived. He wondered what he
should do if Guy should be absent from home, for the time at his
command was short. Within an hour he was due at the Foreign
Office.
Guy opened the door, and started with amazement at sight of
his visitor's face.
"Captain Marven!" he exclaimed. Then a great fear took
possession of him. "Meriel?" he gasped.
Marven grasped the intention of the query.
"Meriel was all right when I left her this morning," he replied.
Guy's relief was obvious. "Are you ill? Is anything the matter?"
he asked, as he closed the door behind the Captain, and followed
him into his sitting-room.
Marven was at a loss for words. Hora's letter was in his hand.
He held it out to Guy, and said huskily, "Read this."
 "But——" interrupted Guy.
"No, read this," repeated Marven.
Guy took the letter. He recognised the handwriting, and he
wondered. His wonder gave place to amazement as he read.
Amazement was succeeded by horror, and, when he had finished
reading, the paper dropped from his hands, and he turned his face
away from the man who had brought it, in a vain endeavour to
conceal his emotion. He was hardly aware that a hand was laid on
his arm, until a voice, tremulous with emotion, said, "Guy, my son."
He disdained concealment then. He wheeled round and
clutched blindly at the two hands outstretched to meet his own.
"Father, forgive! forgive!" he muttered brokenly.
 CHAPTER XXVII
DUTY CALLS

All too swiftly speeded the minutes which were at Captain

Marven's disposal. There was so much to be explained, so much to
be learned, and barely an hour to explain everything. Yet, short as
the time, it was broken in upon by the arrival of another visitor. For
the second time that day Mr. Hildebrand Flurscheim found himself
thrusting his company upon persons who had little desire for it.
When he knocked at the door of Guy's chambers Guy at first ignored
the summons. But the knocking persisted. He was forced to open the
door, if only to prevent his neighbours being disturbed, and, when
once the door was open, Flurscheim refused to be excluded.
"I must see you privately at once," declared the connoisseur.
"My business is of the utmost importance."
Guy admitted him into the sitting-room, where the sight of
Captain Marven surprised him into an exclamation.
"I must see you alone—quite alone," he insisted to Guy.
"I would rather you did not," said Guy. "I am afraid there is
nothing you can say which will be news to Captain Marven."
Flurscheim looked from the young man to the elder man, and
his shrewd eyes noted the emotion from which both were obviously
suffering.
"It's my misfortune to have arrived at an inopportune time," he
remarked. "But you shall soon be rid of my presence. I only want to
rid myself of the debt I owe you for preserving my life."
Guy's face flushed. He felt exquisitely uncomfortable.
"You rate my service too highly," he said. "I did nothing which
entailed any risk to myself, and——" Flurscheim interrupted, but Guy
continued hastily, "And yet, perhaps, it is as well that you should
have arrived just now, while Captain Marven is here. I have a
confession to make to you. I should like him to hear what I have to
say and—and, when I have said it, I think you will no longer consider
yourself in my debt."
The connoisseur found it difficult to believe his ears. Guy's
words could only bear one meaning. He glanced at Captain Marven
and saw that a light had come into his face. Marven had grasped
Guy's arm, and Flurscheim heard him say,
"That's right, Guy, get it over."
Guy turned to him. There was a new-born humility in his voice
and manner. "It is really your wish?" he asked.
"My wish is that my son should do his duty," replied Marven
sadly.
Guy threw back his head and faced the Jew.
"Mr. Flurscheim," he said, "I am the thief who stole your picture."
Father and son were astounded at the result of the bold
confession. They had expected amazement, probably immediate
denunciation, but, instead, the Jew threw up his hands deprecatingly,
and fussily remarked: "There, there, there. What if you did? I could
very well afford the loss, couldn't I?"
Guy stared. He thought that he was not believed, that, possibly,
Flurscheim imagined that he had taken leave of his senses.
"But it is true, Mr. Flurscheim. I—Guy Hora—stole your pictures.
See, I can give you proof."
He turned to a little silver-bound casket lying on the table, and
took from it the miniature which was so like Meriel. He cast one
longing glance at the portrait as he handed it to the connoisseur.
"Well, what if you did steal my picture," snapped Flurscheim,
"there is no need to inform the whole world of the fact, is there?"
Guy was bewildered.
 "I shall say no more about it," continued Flurscheim, "except to
advise you to keep that miniature out of the sight of prying eyes, and
to take the earliest opportunity of getting rid of that d——d scoundrel
of a valet of yours."
"But, Mr. Flurscheim," said Guy, "you do not seem to
comprehend, I——"
The situation trembled on the verge of farce. The Jew's eyes
twinkled with amusement, but he grew grave as he saw Captain
Marven's haggard face.
"Let me explain, Mr. Hora," he said. "A few days ago your man
Jessel gave me information of this miniature being in your
possession. That same afternoon while I was planning how to punish
you, I fell overboard and you saved my life. Now, you tell me, you
were the actual robber of the picture and other little articles. Well, in
return you presented me with something I value still more. Shall we
call it a deal, and shake hands on it?"
Guy could barely see the outstretched hand. A mist was before
his eyes.
"Anyhow, I can appreciate your generosity," he said, as he and
the Jew grasped hands, "and perhaps, if I could have restored you
the articles I have stolen, I might have listened. But there is another
concerned. I must share the penalty he will have to pay."
"There may be a hundred concerned. I'll not trouble any of 'em,
if I should hurt you by so doing. Come, Mr. Hora, say it's a deal.
Don't think you're accepting a favour. It's all the other way about, so
you needn't let your pride stand in the way."
"Pride!" remarked Guy. "My pride has gone before my fall." He
was silent. A few hours previously he would eagerly have accepted
Flurscheim's offer, but since he had read Hora's letter to Captain
Marven, the whole position was changed. Lynton Hora was no
longer worthy of consideration. There was no tie of blood between
them. Hora had deliberately deceived him, poisoned his mind,
robbed him of parents and honour and love to gratify the malice in
his heart. Guy could not think of sparing him. There could be no
treachery where so deeply dyed a traitor was concerned.
"You'll say it's a deal?" asked Flurscheim again.
Captain Marven intervened. "Perhaps it will be best to explain
the whole of the circumstances to Mr. Flurscheim," he said quietly. "I
know that he will treat the family matters involved as purely
confidential."
Flurscheim listened while Captain Marven deliberately laid
before him the facts. "You see," he added quietly, when he had
finished the story, "that this matter cannot remain a secret between
us. This letter must be laid before my chief."
"But that is madness," cried Flurscheim. He gesticulated wildly
in his excitement. He protested, he implored, he argued that only an
entirely wrong-headed sense of duty could demand such a course of
action. But Marven remained inflexible, and Guy supported him in his
determination.
He was still arguing when the striking of a clock warned Marven
that he must leave. Already it had been arranged that Guy was to
accompany him to the Foreign Office. "I shall come, too," declared
the Jew. "Sir Everard Markham is an old acquaintance of mine.
Perhaps he will make you listen to reason."
Neither Captain Marven nor Guy believed that he would fulfil his
threat. But they did not know the pertinacity with which Flurscheim
carried out every scheme to which he had once set his hand. They
left him on the pavement, and drove to Whitehall, but Flurscheim
followed them a few minutes later. When he arrived at the Foreign
Office Captain Marven had already been shown to the Permanent
Secretary's room. Flurscheim demanded notepaper, and, scribbling
a hasty note, succeeded in persuading a messenger to deliver it to
Sir Everard Markham at once. Then he sat down, and awaited the
result.
The note was delivered as he desired, but it remained unopened
for a while. The Permanent Secretary was far too deeply immersed
in the business in hand to have a single thought for anything else.
 It was a distasteful task which Sir Everard Markham had
undertaken to perform. Never before, during his tenure of office, had
he been called upon to question the honesty of any of his trusted
officials. That a soldier and a gentleman could be so lost to all sense
of honour as to deliberately steal government secrets for purposes of
private gain was almost unthinkable. Yet the report which Detective
Inspector Kenly had made left very little room for doubt as to Captain
Marven's guilt. And Marven was the last man whom he should have
suspected of such infamy. The Secretary of State, too, was as much
amazed as the Permanent Secretary at Kenly's report. He also knew
Captain Marven personally. He had dined at his house, they
belonged to the same clubs, he would have pledged his whole estate
on Marven's fidelity, and yet—he trusted that the damning facts
might be explained away, though he doubted that it would be
possible to furnish any plausible explanation of the facts save one.
Most damning of all to both their minds was the final item of
information which Inspector Kenly had brought with him shortly
before the hour at which it had been arranged for the King's
Messenger to call. There could only be one explanation of Lynton
Hora's communication with Marven within an hour or two of his
reaching town. The two men must be in close communication with
one another. Kenly himself no longer had any doubts as to Captain
Marven's guilt. He only regretted that the exigencies of the situation
were such that any one of the gang would escape his clutches. Still,
there would be some satisfaction in having assisted to unmask such
a scoundrel. He looked forward to the interview with keen
anticipation. He had advised the course to be adopted, and, with
some alterations of their own, both the Great Man and the
Permanent Secretary had fallen in with his views.
But the interview was not destined to take the lines suggested,
for almost the first words Captain Marven had spoken, when he had
been ushered into the presence of his three judges, had thrown the
carefully discussed plans into confusion. So intent was he on
performing the duty he had laid down for himself, that he observed
nothing out of the way in the presence of Sir Gadsby Dimbleby and
another man, a stranger to him, in the Permanent Secretary's room.
He did not observe that neither the Permanent Secretary nor the
Great Man had offered him a hand, nor that there was a false ring
about the "How d'ye do, Marven," with which Sir Gadsby greeted
him. Trivialities, such as these, were of no importance to the man
who had before him the terrible duty of denouncing the son whom he
had but just found.
Captain Marven had mapped out for himself the course to be
pursued. First he must make amends for his own share in the
disclosure. He had failed in his trust. He had allowed himself to fall
into the trap laid for him. There was only one way in which he could
make amends.
"I suppose, Sir Markham," he said, "you have sent for me in the
ordinary course. I regret that some matters I have to lay before you
will probably lead you to the conclusion that I am no longer fit to be
entrusted with your commands. I think it well to tell you at once, in
case you are in urgent need of a messenger, so that you may
communicate with the next man on the rota."
A dead silence followed his words. The Great Man looked at the
Permanent Secretary and the Permanent Secretary returned the
glance. One thought was common to each of their minds. Was
Marven going to confess? They suddenly became aware that the
Captain had aged considerably since they last saw him, that his face
was worn and lined, his eyes dull. Yet he held himself erect, and his
voice was calm.
He continued, "The matter is of importance. Of course I can
have no objection to the presence of Sir Gadsby, but I do not
recognise this gentleman,"—he indicated Kenly with a gesture—"and
if he would retire——"
Kenly made no movement, and the Permanent Secretary raised
his eyebrows in mute enquiry to the Great Man. Sir Gadsby
coughed. Then he remarked drily, "This gentleman is Detective
Inspector Kenly of Scotland Yard. It is my desire that he should hear
why you consider yourself unfit to be trusted with your duties as a
King's Messenger."
 Captain Marven could not fail to understand the suggestion
which lay behind the Great Man's words. Still more significant was
the cold tone in which the words were spoken. He was himself
suspect. His summons was not in the ordinary course of events. He
was to have been called to account. Well, what did it matter? Yet,
though his cheek flushed, and as suddenly paled, he gave no other
sign of agitation. "He has a soldier's pluck, anyway," muttered Kenly
to himself, as Marven replied calmly, "Certainly, if you wish it, Sir
Gadsby."
Marven turned immediately to the Permanent Secretary. "I
received barely two hours ago a letter from an old brother officer of
mine, named Hartley Ruthven, who is now known by the name of
Lynton Hora. I want you to read that letter first. Afterwards I should
like to add any information which is in my possession to the
disclosures it contains."
The Permanent Secretary took the letter from Marven's hand,
and glanced rapidly over the first page.
"Good God!" he said. He looked up and insensibly his tone
became more kindly. "Won't you sit down, Marven?"
Captain Marven seated himself. The Permanent Secretary read
another page. Then he spoke again.
"Shall I read this letter to Sir Gadsby? I am sure that if I say it is
desirable that Mr. Kenly shall withdraw he will not insist upon his
remaining."
"I should prefer Mr. Kenly should hear the contents," answered
Marven steadily.
The Permanent Secretary read the letter aloud. When he
concluded there was a silence that could be felt.
Marven broke it. "My son is waiting below to give himself up to
justice." His voice quivered for a moment, then became steady
again. "He is ready—even anxious—to pay the penalty."
Sir Gadsby's face became purple. He turned to Kenly. "Here
you, what the devil do you mean by letting this d——d scoundrel
Hora go about kidnapping honest men's sons and bringing 'em up to
break their father's hearts? What is the use of a detective force at
all?"
Kenly nearly fell off his chair at the suddenness of the attack. He
was far too amazed to defend himself. He understood the next
moment that the explosion was only the ebullition of a warm heart
which needed an outlet, for the next moment the Great Man had
taken Captain Marven's hand and was shaking it violently, while he
stuttered out, "By Gad, Marven, I have to apologise to you. I've been
thinking that you peeped into that despatch box yourself. I'll never
forgive myself for doubting you."
Captain Marven smiled sadly. "Though unintentionally, I have
betrayed my trust," he said. "If I had been more careful, my son——"
He could get no further. The Great Man wiped his eyes and blew his
nose violently. He knew Marven's story, knew of his sorrow and his
hopes, and he could appreciate the wonderful devotion to duty which
had led him to so sacrifice his son. He turned to the Permanent
Secretary. "Look here, Markham, we must put our old heads together
and get the boy out of this scrape somehow." He nodded to the
detective. "You ought to be able to suggest something, Kenly."
The Inspector's face was a study. He foresaw all his efforts
being wasted. He set his lips doggedly.
"I am afraid you are asking me to assent in compounding a
felony," he answered sourly.
"Compounding a felony be d——d!" roared the Great Man. "I'll
guarantee it wouldn't be the first time you've compounded."
To this totally undeserved slur, the Inspector was about to make
a heated reply, when the Permanent Secretary intervened. "Sir
Gadsby often says more than he means," he remarked, adding
thoughtfully, "—in private life, of course."
The Great Man laughed, and said, "Yes, you must not take my
last remark to you literally, Inspector."
Kenly's face cleared, but he was still loth to let the victim, about
whom he had wound his net, escape.
 "Do you propose to let this man Lynton Hora go free, then?" he
asked. "What would Mr. Flurscheim say to that?"
A totally unexpected answer came to the enquiry. The
Permanent Secretary had remembered the unopened note which
had been brought to him. He had torn it open, and the signature had
attracted his attention.
"Suppose we ask Mr. Flurscheim," he said. "Listen to this," he
read the note aloud.
"DEAR SIR MARKHAM: A friend of mine, from some pig-
headed notion of duty, is insisting on sending his son to prison. I
want you, before you take any action in the matter, to hear what I
have to say on the question.
"Very sincerely yours,
"HILDEBRAND FLURSCHEIM.
"P. S.—By the time you receive this you will, of course,
understand that I am writing about Captain Marven.
"PP. S.—I shall wait here until I see you."
The Great Man rubbed his hands together and chuckled.
"Let us have Mr. Flurscheim up," he said.
 CHAPTER XXVIII
THE FRUITS OF A CRIMINAL PHILOSOPHY

Lynton Hora was not to be allowed to escape. That was the

decision arrived at, after the prolonged conference at the Foreign
Office, and Detective Inspector Kenly's mind was thereby
disburdened of the fear lest all his efforts should have been wasted.
He would have liked to have made certain of one prisoner there and
then, but this was forbidden him. He had no belief in repentant
offenders, and to him Guy appeared nothing more. Still Flurscheim
refused to charge Guy. Captain Marven undertook to be responsible
for his answering any charge, Sir Everard Markham added his
persuasions, and Sir Gadsby Dimbleby declared that he would take
it as a personal insult if Guy were arrested before the Master
Criminal was laid by the heels. The Great Man was far too great a
man for a detective inspector to offend, and so Guy left the Foreign
Office with Captain Marven to await the summons to surrender
himself, when information of Hora's arrest should reach him.
The Captain was very grateful for the respite, none the less
because he had not personally urged it. For a little while his son
would be with him. As yet the prison stain was not upon him. He was
pathetically anxious to become acquainted with the grown child who
was so soon to be torn away again. Duty may be sometimes an
over-hard task-master, yet he faced it manfully, and could at least
find some small consolation in the fact that his son faced it as
manfully as himself.
Detective Inspector Kenly saw them drive away together, and,
as he caught sight of the look of pleasure on the face of the King's
Messenger, he was not altogether sorry that he had been compelled
to forego the arrest.
 "It's a curious tangle," he muttered. Then he hailed a cab, and
gave the address of a police court. Ten minutes' interview with the
magistrate was all he sought, and, when he re-entered the waiting
cab, he had in his possession two documents—a warrant for Lynton
Hora's arrest, and a search warrant for the flat in Westminster
Mansions.
Thus provided for all emergencies, he drove straight away for
Hora's residence. There was no time to be wasted. From what he
had learned during the afternoon it was clear that Lynton Hora must
be aware that at any moment his deeds might be brought to light, for
Guy had been called in to the conference, and he had revealed all
that had passed between himself and the man he had believed to be
his father.
On arrival at Westminster Mansions Inspector Kenly stamped
his foot with vexation on learning that Lynton Hora had gone out. His
subordinate was absent, too. If flight was in Hora's mind, the
sergeant would obey the instructions and detain him. Kenly
determined to make use of the absence to execute the search
warrant in his possession. But he was not going to leave anything to
chance. He telephoned to Scotland Yard for further assistance, and,
pending its arrival, he chatted with his old friend, the hall porter, and
from him he learned that the other occupant of the flat had also gone
out that morning, and had not returned. This seemed more like
preparation for flight than ever, but Myra's absence also left him a
clear field for his investigations. A very few minutes elapsed before
the assistance he had asked for arrived. He left one of the two plain-
clothes men in the hall and took the other with him upstairs. No one
was aware of the nature of their business, and the two men entered
the flat with the service key. Kenly did not waste time on a careful
examination of the lower rooms. He went directly to the floor leading
to the attics where Hora's "collection" was stored. He only wanted to
verify the information which Guy had given as to the whereabouts of
the Greuze. He had long since provided himself with a key to the
lock of the door so that admission to the attics presented no difficulty.
Guy had spoken truly. Kenly found the Greuze and the snuff-boxes
stolen from Flurscheim's house. He saw also that there was a rich
store of other articles in locked cabinets and cases, for which no
doubt he would be able to find owners. But he did not linger to
examine them. There would be plenty of time for that after Hora had
been apprehended.
After he had been apprehended! Kenly did not allow himself to
consider the possibility that he might escape. Yet as minutes passed
by and the minutes added themselves into hours, he began to be
uneasy in his mind. His uneasiness became acute apprehension
when, as dusk was falling, the subordinate to whom had been
entrusted the duty of shadowing Hora returned to the Mansions
alone.
A rich variety of objurgations rose to the Inspector's tongue, but
there was no time to be lost in uttering them. He enquired where
Hora had been lost sight of. The man explained to the best of his
ability. He had followed Hora to Waterloo railway station, had heard
him take a return ticket to Worcester Park, had himself booked to the
same destination, had taken a seat in the next compartment, had
watched to see whether he alighted at any intermediate station, and
on arrival at Worcester Park had discovered that the compartment in
which Hora had travelled was empty.
Kenly reflected. Worcester Park was two stations further down
the line than Wimbledon. What if Hora had wished to see Jessel
again? He turned to the man. "Was Hora carrying a small black bag
and an overcoat on his arm?"
"Yes," was the reply.
"You idiot," muttered Kenly; then he added, "You will wait here
until Hora returns, or you are relieved. If he comes back, you will
arrest him and take him straight to Bow Street. If the girl returns,
arrest her, too." Then he turned to the other two men. "Go back to
the Yard, and have a full description of him and the girl telegraphed
to every port in the kingdom. Stay, though, you had better wire, also,
particulars of the disguise in which he succeeded in eluding this
dolt."
 The subordinate shivered, and realised that if Hora did not
return it would be advisable for him to retire from the force.
Kenly dictated a description of Hora's clerical disguise. There
was yet a chance that he might get upon his track. He jumped into
the first cab that passed and drove away to Waterloo. He could have
wept with vexation at the thought of his prey escaping so easily,
through the incompetence of his subordinate. He looked at his
watch. A train was timed to start for Wimbledon in two minutes. With
luck he would just catch it. He lifted the trap in the roof of the
hansom, and shouted, "Hurry up, cabby, I have a train to catch."
Luck was apparently against him. Traffic was heavy and the cab
was caught in a block. Kenly writhed with impatience. But a moment
later the traffic block appeared to be a special dispensation of
Providence. Kenly caught sight, in the light of a street lamp, of an old
clergyman, in shabby hat and cloak and carrying a small black bag,
amongst the crowd on the sidewalk. He could have shouted aloud
with delight. He jumped out of the cab, and tossed the driver a half-
crown piece. His first impulse was to dash forward, and there and
then effect the arrest. He had recognised Hora, he could have sworn
to the distinguishing limp. But a second thought restrained him.
Though Guy's statements had been apparently full and frank, Kenly
had not credited him when he had declared that he and Lynton Hora
worked alone. He had thought that there must be other members of
the gang, a supposition which had been fed by the information he
had extracted from Jessel. Hora had worn his clerical disguise when
communicating with Jessel. What more likely than that he should put
it on when communicating with other tools? Kenly determined to
follow him.
Soon he was glad that he had done so. Hora apparently had no
intention of returning to Westminster Mansions. He boarded an
omnibus which took him northwards. Kenly sat behind him while they
drove through the brilliant streets of the West End. He changed the
bus for another travelling westwards, the detective at his heels.
Passengers came and went, but Hora remained until the end of the
journey.
 Kenly knew the district, and he thought that his suppositions
were about to be verified when he observed the direction Hora took
upon alighting. That way led to the quarter where the thieves of the
metropolis had gathered and made themselves a colony when their
old haunts in the centre of the city had been mowed down. He felt in
his pocket for his whistle, and wished that he had slipped a revolver
into his pocket that morning. But he followed, nevertheless, and was
thankful when a couple of uniformed policemen came in sight. As he
passed them he uttered a single word. The constables apparently
took no notice, but when Kenly was half the length of the street
distant they wheeled round and followed him steadily.
Hora pursued his way in a manner that showed that the quarter
was not strange to him. The detective hunched his shoulders, pulled
his cap down over his ears, and turned up his coat collar. Here he
might be recognised any moment. He did not want to alarm his
quarry.
Hora turned into Fancy Lane. He was walking more quickly now.
He disappeared under the archway which led to "Ma" Norton's
disreputable shed. Arriving there Kenly paused. The two policemen
turned into the lane. He held up his hand and plunged into the
blackness. The constables came on, and arriving at the entrance
they stood there chatting quietly. But their eyes were keenly
observant, and each had loosened the truncheon hidden beneath his
tunic. They were in the enemy's country, and at any moment might
be called upon to fight for their lives.
Kenly blundered on through the darkness, guided by the sound
of voices, until he emerged into the yard. There his attention was
attracted by a dull light filtering through dirty panes of glass. It
seemed to him evidence that his objective was attained. Stealthily he
made his way to the window and peeped through.
He had seen many strange tableaux during his career, but none
stranger than that he now looked upon. He saw a dropsical old
woman, with a glass in her hand and a maudlin grin on her bloated
face, balancing herself with difficulty on a rickety chair. He saw
Lynton Hora, with a mocking smile on his face, by no means in
keeping with his clerical garb, pointing to the hideous figure. He saw
another man at Hora's elbow, a bullet-headed man, with closely
cropped red hair and with flushed face, whose eyes never wandered
from the face of the fourth member of the party. Kenly recognised
her, too. Myra's beauty was not easily forgotten, and it peeped out
from beneath the mask of horror which was drawn over her face.
Hora was speaking.
"So you have found your way back to your native slum, Myra.
Do you find it congenial to your dainty spirit? I see your mother is
celebrating your return. One day you will be like her." He wheeled
round rapidly and glanced at the man at his elbow. "You have found
an admirer, too, as well as a mother. You have lost no time."
Myra threw out her hands imploringly.
"Take me away, Commandatore. Take me away," she cried. She
saw that Hora hesitated, and she renewed her appeal.
"Why should I take you away?" he answered. "I offered you a
husband and a home. You let them escape you." He jerked his head
to the man. "Hagan here will supply you with both. Why should I
interfere?"
The hope died out of her face and the fear reappeared as the
man lurched forward.
"'Ear what the Master says; e's a toff at spoutin', is the Master,"
he said, with an ugly leer on his face.
She shrank from his touch, and looked vainly round for a way of
escape. Kenly thought of a hare he had once seen as it doubled
almost at his feet from two pursuing greyhounds. He placed his
whistle between his lips ready.
"Stand back, Hagan," said Hora authoritatively.
The man dropped his hand, but there was a frown on his face.
"Suppose I were to take you away?" he asked.
Hope shone out in her face again.
 "Ask of me anything you will," she cried. "Anything but this."
She had forgotten everything in the supreme horror of the
hideous hole in which she had found herself.
That morning when she had left Lynton Hora's abode she had
thought she had been incapable of further suffering. She had gone
out into the park and sat there hour after hour, conscious at first only
of the one fact that Guy was lost to her forever. She had told herself
that she would never return to Lynton Hora's roof to face his sneers.
He had always hated her. She had no doubt that he was aware all
the time that Guy would never marry her, and that he had only
bidden her try to win his love that she might be humiliated by its
rejection. Perhaps he had lied to her about her mother and her
home, merely that she might not be tempted to escape from him.
The sound of the word mother appealed strongly to her in her dazed
condition. Her mother could not be worse than Hora. She had the
address. One day she had copied it down carefully. The slip of paper
was still in her purse.
She had found her way thither with difficulty. Not until she had
lost herself amongst the streets in the neighbourhood of Fancy Lane
did she begin to regain her senses. Then the words of coarse abuse
from the doors of public houses, the shrill voices of women from
open doors, made her wish for flight. Darkness had fallen on the face
of the town by that time, and she became aware that she was nearly
exhausted. Then a child had led her to Fancy Lane, and another
youngster, for the gift of a sixpence, had acted as guide to her
destination. Everybody in Fancy Lane knew "Ma" Norton.
The bully on his way to his favourite drinking shop had seen her
passing along the street. A flash of the stones set in the bracelet she
still wore on her wrist—the bracelet Guy had given her—attracted his
attention. He had changed his purpose and followed her.
Myra had known that Hora had spoken only too truly the
moment she entered the den, where Mrs. Norton was soaking
herself to death in alcohol. The old woman had been just too tipsy to
comprehend who her visitor was. Myra had soon given up the task of
trying to explain. She had found a lamp, and, after lighting it, had
shuddered with disgust at the filthy surroundings revealed by the
light. She could not stop there. She had risen to leave, but found the
exit blocked by the burly figure of Bully Hagan.
He had heard her attempts to make Mrs. Norton understand
who she was. This was "Ma's" lady daughter. He foresaw profit in the
fact. When his eyes rested on Myra's perfect figure silhouetted
against the lamp she had lighted, another thought entered into his
brain. He did not at first disclose his thought. Myra thought he was
merely intent upon plunder. When she understood, she realised how
the Sabine women must have felt; she experienced the emotions of
the women of a Balkan village when an Albanian regiment was let
loose upon it.
For an hour Myra had kept him at bay, her faculties racked to
the utmost. Then Lynton Hora had come on the scene, and she had
appealed to him.
Now Hora seemed to be considering her appeal, and her face
brightened with hope as she gazed eagerly on his face. He
responded with a smile.
"It is lucky for you that I thought of coming and looking for you
here," he said. "Whatever you have done or left undone would not
deserve such a fate as that."
He indicated the man at his elbow with a gesture of scorn.
"You will take me home again." The relief was so great that she
could scarcely believe it.
"Yes, come along. It is getting late."
An angry growl arrested him.
"No, you don't," said Hagan.
The veins of the bully's forehead were swollen and his fists
clenched.
"Get out of the way," said Hora, in the tone he would have used
to a cur in the street, and, as the man did not stir, he caught him by
the arm and thrust him aside so violently that he crashed against the
opposite wall.
"Come, Myra," said Hora.
Kenly lost nothing of the scene. He saw the look on the bully's
face as he picked himself up. He saw a flash of steel in his hand.
The whistle he held between his teeth shrilled out as he left the
window and dashed to the door. The sound was answered by other
whistles, and he heard the rush of feet towards him down the
passage. He reached the door, but it stuck fast. The sound of the
advancing feet was drowned by a woman's shriek. Kenly hurled his
whole weight against the door. The shriek was repeated. A second
time the detective hurled himself against the door. This time the
catch gave way and he blundered forward into the room.
Two figures lay prone upon the floor, a man stood over them
calmly wiping the blood-stained blade of a knife on his sleeve. A
dropsical old woman sat gazing with a maudlin smile on her face at
the scene.
Kenly's head whirled. He stood still, mechanically, until panting
breath behind him gave warning that assistance had arrived.
Hagan coolly handed him the knife.
"I done it," he said; "I've outed 'em both."
Then he held out his hands for the bracelets.
Kenly stooped to the floor, and laid his finger on Myra's wrist.
The pulse had ceased to beat. He laid her hand down again, and
bent over Lynton Hora. The Master lay perfectly still, and even while
the detective bent over him a glaze spread itself over the open eyes.
Kenly's quarry had escaped him.
 L'ENVOI
Captain Marven never had cause to mourn for a son hidden
behind the bars of a convict prison.
The fate which had fallen upon Lynton Hora was so full of horror
that even Detective Inspector Kenly would have been willing to admit
that a greater power than that of the law he had striven to enforce
had administered justice. When his chief, therefore, told him that he
was expected to keep a discreet silence in regard to the part Guy
had played in the Flurscheim robbery, he could hardly squeeze out a
sigh. Later, he was to win his reward when, by means of the Great
Man's recommendation, he was appointed to the chief constableship
of an important borough where his position was such that Mrs.
Detective Inspector was compelled finally and for all time to
renounce taking in lodgers.
Mr. Hildebrand Flurscheim once again rejoiced in the
possession of his Greuze. It returned to its old place on his wall, so
that morning and night he could feast his eyes upon its beauties.
Jessel never applied for the reward. He returned to the shadows
from which he had emerged. In fact, he felt that he could not be
happy in a land where he was so well known to an important
member of the detective force of the police. But Flurscheim always
lamented that, since the Greuze and other valuables had been
returned to him, it would be impossible for him to liquidate his debt to
Guy, who had insisted even upon returning the miniature which bore
so great a likeness to Meriel.
That miniature, however, came again into Guy's possession in
the form of a wedding gift, when Meriel Challys changed her name to
Meriel Marven. The Jew's words had borne fruit. She found a loving
duty in helping Guy to bury his past, and Captain and Mrs. Marven
found a renewal of their own youth in the happiness which attended
the union. As for Guy—well, he has been heard to declare that the
waters of his life are full of star-dust.
THE END
 Recent Publications of Cupples & Leon Co.
The Powers and Maxine
By C. N. & A. M. Williamson
Authors of

"The Lightning Conductor,"

"Lady Betty Across the Water,"
"The Car of Destiny," etc.

1 vol. 12 mo. cloth, gilt embossing

Illustrated by FRANK T. MERRILL
OPINIONS OF THE PRESS:
The Boston Globe
"When a gifted and beautiful actress, who at the same time is a
secret service agent for the British government, captivates Parisian
society with her histrionic powers and incidentally breaks many
hearts and gets into innumerable tragic situations, the narrative of
her adventures could not possibly be dull. When it is told by C. N. &
A. M. Williamson, those past-masters in the art of fiction, in such a
dramatic book as 'The Powers and Maxine' every page throbs with
interest."
Portland Oregonian
"In reading this romance where sensations are knee deep, it is
well to recall that every recent work of the Williamsons has been so
popular that it has run above the 100,000 mark. Maxine, the heroine
of this novel—which is the best and latest of the Williamsons,—is a
beautiful actress who captures Paris with her art, while privately she
is a secret service agent for the British government. Of course, she
comes out ahead."
Chicago Record-Herald
"A stirring story, written in a manner new to these authors. Deals
with a purloined treaty, lost diamonds, love, mystery and vigorous
plotting, set against a London and Paris background. The double
love episode ends well, despite wicked schemes against both pairs
of lovers."
 Hill Rise
By W. B. Maxwell
Author of

"Vivien,"
"The Guarded Flame," etc.

1 vol. 12 mo. cloth, 320 pp. illustrated

Nor is "Hill Rise" one of those dreary, unpleasant creations
known as a "problem novel." It has a strong, virile, intensely exciting
plot, full of vigorous action, sustained suspense, thrilling episode and
continuous surprises. The character drawing is almost miraculous in
its fidelity to human nature. The whole story is powerful, simple and
intense. The sort of a narrative one cannot lay down unfinished.
 The Man in the Basement
By Baron Palle Rosenkrantz
Author of

"A Confession,"
"The Widow," etc.

1 vol. 12 mo. cloth, illustrated

"The Man in the Basement" is perhaps the strangest story ever
written. Its every situation is out of the common and startlingly
unique. It compares to the average detective or mystery romance as
Sherlock Holmes compares with "Deadwood Dick" or some other
dime novel hero. The characters, most of them are Danes, and the
wild, breezy freedom and charm of the North are strikingly portrayed.
 Graham of Claverhouse
By Ian Maclaren
The Last Great Novel of this Famous Author
Illustrated in Colors by Frank T. Merrill
1 vol. 12 mo. cloth, gilt
"GRAHAM OF CLAVERHOUSE" is a splendid novel of love,
intrigue, and adventure. Through every line breathes the spirit of
vibrant human nature and flashing local color. It is the historical
romance of the century, instinct with poetic feeling and impelling
dramatic charm.
 Caleb Conover, Railroader
By Albert Payson Terhune
1 vol. 12 mo. cloth, gilt
Illustrated in Colors by Frank Parker
"CALEB CONOVER" is truly an original character. His humor is
quaint and contagious and will be remembered long after the book
has been read.—Washington Star.
 Aladdin of London
By Max Pemberton
Author of

"The Lady Evelyn,"

"The Hundred Days," etc.

1 vol. 12 mo. cloth, gilt, illustrated

"Max Pemberton, the popular novelist, sustains his high
reputation in this thrilling tale of European life. Alban Kennedy, the
impoverished son of a British parson, is compelled to take up his
abode in the Whitechapel district of London, and becomes the suitor
of a little Polish maid who is infinitely above her mean environment.
The circumstances which lead to his adoption by a millionaire, the
net of intrigue woven about him, and the efforts to bring about the
death of his little sweetheart for political purposes, using him as the
innocent tool, make an engrossing plot."—Albany Times-Union.