THE SCIENTIFIC FOUNDATIONS OF ANALYTICAL CHEMISTRY
1 QR Codes 1 Objectives and Scope 1 1 Why are There QR Codes in this Book? 1 11 Applications 2 2 The Origin: Barcodes 3 21 Symbology 4 3 The Present: QR Codes 5 31 TheQR code structure 6 32 QR code types 8 33 QR code styles 9 34 How are QR codes read? 11 References 12 2 Fundamental Calculations in Analytical Chemistry 13 Objectives and Scope 13 1 Introduction 13 11 Relevant units and expressions of concentration 14 111 Units 15 112 Some important terminologies 17 113 Specifying the concentrations of solutions 19 12 Preparing solutions from solids or liquids 23 13 General operational treatments before the analysis 25 131 Drying 26 132 Dissolution, digestion, and extraction 27 133 Dilution and concentration of test solutions 29 References 31 Worked Exercises 31 Exercises Proposed for the Student 49 Exercise References 52 3 Basic Data Analysis 53 Objectives and Scope 53 1 Introduction 53 2 How to Describe a Series of Data 57 21 Central trend of data: the average 57 22 Central trend of the data: themedian 59 23 Measuring the dispersion: range or interval 59 24 Measuring the dispersion: standard deviation 59 25 Measuring the dispersion: relative standard deviation 61 26 Measuring the symmetry: skewness 61 27 Measuring the shape: kurtosis 61 3 Are There Outliers? 62 31 Dixon’s test 64 32 Grubbs’s test 65 33 Calculate once you have eliminated outliers 67 4 Practical Applications of Student’s t-Test 69 41 Does my result coincide with a given result? 71 42 Comparing two series of data 71 5 Calibration 74 51 Basic calibration calculi 77 52 Validate your model 80 53 The standard addition method 82 54 The addition calibration method 84 55 Comparing calibration lines 85 56 Limits of detection and quantitation 86 561 Traditional superseded definitions 87 562 Rationale for the modern definitions, a bit of history 90 563 Calculations and current agreed definitions 95 564 Additional practical issues for calculations 100 References 106 Worked Exercises 108 Exercises Proposed for the Student 131 4 Ultraviolet and Visible Spectroscopy 141 Objectives and Scope 141 1 Introduction 141 11 Basic concepts 141 12 Quantitative applications of Bouguer–Lambert–Beer’s law 144 121 Calculating the concentration of the analyte 144 122 Multicomponent analysis 144 123 Derivative spectroscopy 145 124 Determination of the stoichiometry of a complex 145 References 149 Worked Exercises 149 Exercises Proposed for the Student 173 Exercise Reference 181 5 Infrared Spectrometry 183 Objectives and Scope 183 1 Introduction 183 11 Basic concepts 183 12 Spectral interpretation 186 13 Characteristic typical vibrations in the mid-IR region 188 14 Prediction of the position of the bands in infrared spectrometry 194 15 Quantitation in IR spectrometry 195 16 First approach to the exercises 196 References 198 Worked Exercises 200 Exercises Proposed for the Student 229 6 Atomic Spectrometry 247 Objectives and Scope 247 1 Introduction 247 2 Optical Atomic Spectrometry 248 21 Atomic absorption spectrometry (AAS) 248 211 Instrumentation 249 212 Interferences 251 213 Applications 252 22 Atomic emission spectrometry (AES) 253 221 Instrumentation 253 222 Interferences 255 223 Applications 255 3 Inductively Coupled Plasma Mass Spectrometry (ICP-MS) 256 31 Instrumentation 256 311 Ion source 256 312 Mass spectrometer 256 32 Interferences 258 33 Applications 258 References 259 Worked Exercises 259 Exercises Proposed for the Student 307 7 Chromatographic Techniques 317 Objectives and Scope 317 1 Introduction 318 2 Chromatographic Parameters 321 3 Optimization of the Chromatographic Separations 324 4 Qualitative Analysis: Identifying Compounds 325 5 Quantitative Analysis 328 51 External calibration, internal standard calibration, and normalization 328 52 Multistage sample treatment in combination with chromatographic methods 330 References 331 Worked Exercises 331 Exercises Proposed for the Student 353 Exercise References 356 8 Nuclear Magnetic Resonance and Mass Spectrometry 359 Objectives and Scope 359 Part A: Nuclear Magnetic Resonance Spectrometry 360 1 Introduction to Nuclear Magnetic Resonance 360 11 Basic principles 360 12 Basic concepts of the NMR spectrometers 364 13 Hands-on: Acquisition of an NMR spectrum 365 14 The chemical shift 366 141 Characteristic chemical shifts of some selected functional groups 368 15 Integration 370 16 Spin–spin coupling 370 161 Spin–spin coupling: Problems of interpretation 373 2 Carbon-13 NMR Spectrometry (13C-NMR) 374 3 Other Advanced Techniques 375 Part B:Mass Spectrometry 376 4 Introduction toMass Spectrometry 376 41 Basic instrumentation forMS 376 411 Introduction systems 376 412 Ionization systems 377 413 Ion analyzer systems 377 414 Detectors 378 5 Interpreting aMass Spectrum 379 51 Types of characteristic ions 379 511 Themolecular ion 379 512 Isotopic ions 380 513 Fragments 384 52 Determination of the molecular formula of a molecule by high resolution mass spectrometry 384 References 389 Worked Exercises 389 Exercises Proposed for the Student 415 Solutions to the Exercises Proposed for the Student 423 9 Electroanalytical Techniques 425 Objectives and Scope 425 1 Introduction 425 11 Basic concepts 426 12 Balancing redox equations 429 121 Half-reaction method 430 13 Redox equilibrium and potentials 430 2 Electrochemical Cells 435 21 Standard electrode potentials 436 22 Galvanic cells 439 23 Electrolytic cells 441 3 The Relation Between Potential and Concentration 443 31 Faraday’s laws and electrolytic cells 445 4 Potentiometric Measurements 446 41 Reference electrodes 447 42 Indicator electrodes 448 References 449 Worked Exercises 449 Exercises Proposed for the Student 468