Problems Of Instrumental Analytical Chemistry: A Hands-on Guide

by Jose Manuel Andrade-garda, Alatzne Carlosena-zubieta, Maria Paz Gomez-carracedo, Miguel A Maestro-saavedra, Maria Carmen Prieto-blanco

Overview

The complex field of analytical chemistry requires knowledge and application of the fundamental principles of numerical calculation. Problems of Instrumental Analytical Chemistry provides support and guidance to help students develop these numerical strategies to generate information from experimental results in an efficient and reliable way. Exercises are provided to give standard protocols to follow which address the most common calculations needed in the daily work of a laboratory. Also included are easy to follow diagrams to facilitate understanding and avoid common errors, making it perfect as a hands-on accompaniment to in-class learning.Subjects covered follow a course in analytical chemistry from the initial basics of data analysis, to applications of mass, UV-Vis, infrared and atomic spectrometry, chromatography, and finally concludes with an overview of nuclear magnetic resonance. Intended as a self-training tool for undergraduates in chemistry, analytic chemistry and related subjects, this book is also useful as a reference for scientists looking to brush up on their knowledge of instrumental techniques in laboratories.

Product Details

ISBN-13:	9781786341792
Publisher:	World Scientific Publishing Europe Ltd
Publication date:	05/08/2017
Series:	Essential Textbooks In Chemistry
Pages:	480
Product dimensions:	6.30(w) x 8.80(h) x 1.20(d)

Table of Contents

Preface v

About the Authors ix

Chapter 1 Fundamental Calculations in Analytical Chemistry Alatzne Carlosena-Zubieta José Manuel Andrade-Garda 1

Objectives and Scope 1

1 Introduction 1

1.1 Relevant units and expressions of concentration 2

1.1.1 Units 3

1.1.2 Some important terminologies 5

1.1.3 Specifying the concentrations of solutions 6

1.2 Preparing solutions from solids or liquids 10

1.3 General operational treatments before the analysis 12

1.3.1 Drying 13

1.3.2 Dissolution, digestion and extraction 14

1.3.3 Dilution and concentration of test solutions 16

References 17

Worked Exercises 18

Exercises Proposed to the Student 38

Exercise References 40

Chapter 2 Basic Data Analysis José Manuel Andrade-Garda María Paz Gómez-Carracedo 43

Objectives and Scope 43

1 Introduction 43

2 How to Describe a Series of Data 47

2.1 Central trend of the data: the average 48

2.2 Central trend of the data: the median 49

2.3 Measuring the dispersion: range or interval 49

2.4 Measuring the dispersion: standard deviation 49

2.5 Measuring the dispersion: relative standard deviation 51

2.6 Measuring the symmetry: skewness 51

2.7 Measuring the shape: kurtosis 51

3 Are There Outliers? 52

3.1 Dixon's test 54

3.2 Grubbs's test 55

3.3 Calculate once you have eliminated outliers 59

4 Practical Applications of the Student's t-test 60

4.1 Does my result coincide with a given one? 63

4.2 Comparing two series of data 63

5 Calibration 74

5.1 Basic calibration calculi 77

5.2 Validate your model 80

5.3 The standard addition method (SAM) 82

5.4 The addition calibration method 84

5.5 Comparing calibration lines 85

5.6 Limits of detection and quantitation 86

5.6.1 Traditional superseded definitions 88

5.6.2 Rationale for the modern definitions, a bit of history 91

5.6.3 Calculations and current agreed definitions 95

5.6.4 Additional practical issues for calculations 100

References 106

Worked Exercises 108

Exercises Proposed to the Student 134

Chapter 3 Ultraviolet and Visible Spectroscopy Rosa María Soto-Ferreiro 143

Objectives and Scope 143

1 Introduction 143

1.1 Basic concepts 143

1.2 Quantitative applications of the Bouguer- Lambert-Beer law 146

1.2.1 Calculating the concentration of the analyte 146

1.2.2 Multicomponent analysis 146

1.2.3 Derivative spectroscopy 147

1.2.4 Determination of the stoichiometry of a complex 147

References 151

Worked Exercises 151

Exercises Proposed to the Student 176

Exercise References 188

Chapter 4 Infrared Spectrometry José Manuel Andrade-Garda María Paz Gómez-Carracedo 189

Objectives and Scope 189

1 Introduction 189

1.1 Basic concepts 189

1.2 Spectral interpretation 192

1.3 Characteristic typical vibrations in the mid-IR region 194

1.1 Prediction of the position of the bands in IR spectrometry 197

1.5 Quantitation in IR spectrometry 202

1.6 First approach to the exercises 203

References 204

Worked Exercises 206

Exercises Proposed to the Student 239

Chapter 5 Atomic Spectrometry Rosa María Soto-Ferreiro Alatzne Carlosena-Zubieta 263

Objectives and Scope 263

1 Introduction 263

2 Optical Atomic Spectrometry 264

2.1 Atomic absorption spectrometry (AAS) 264

2.1.1 Instrumentation 265

2.1.2 Interferences 267

2.1.3 Applications 268

2.2 Atomic emission spectrometry (AES) 269

2.2.1 Instrumentation 269

2.2.2 Interferences 270

2.2.3 Applications 271

3 Inductively Coupled Plasma Mass Spectrometry (ICP-MS) 271

3.1 Instrumentation 271

3.1.1 Ion source 272

3.1.2 Mass spectrometer 272

3.2 Interferences 273

3.3 Applications 274

References 274

Worked Exercises 274

Exercises Proposed to the Student 322

Chapter 6 Chromatographic Techniques María del Carmen Prieto-Blanco 333

Objectives and Scope 333

1 Introduction 334

2 Chromatographic Parameters 336

3 Optimization of the Chromatographic Separations 339

4 Qualitative Analysis: Identifying Compounds 340

5 Quantitative Analysis 342

5.1 External calibration, internal standard calibration and normalization 343

5.2 Multistage sample treatment in combination with chromatographic methods 345

Reference 346

Worked Exercises 346

Exercises Proposed to the Student 372

Exercise References 376

Chapter 7 Nuclear Magnetic Resonance and Mass Spectrometries Miguel Angel Maestro-Saavedra 379

Objectives and Scope 379

Part A Nuclear Magnetic Resonance Spectrometry 380

1 Introduction to Nuclear Magnetic Resonance 380

1.1 Basic principles 380

1.2 Basic concepts of the NMR spectrometers 383

1.3 Hands-on: Acquisition of an NMR spectrum 385

1.4 The chemical shift 385

1.4.1 Characteristic chemical shifts of some selected functional groups 388

1.5 Integration 388

1.6 Spin-spin coupling 391

1.6.1 Spin-spin coupling: problems of interpretation 393

2 Carbon-13 NMR Spectrometry (¹³C-NMR) 394

3 Other Advanced Techniques 397

Part B Mass Spectrometry 398

4 Introduction to Mass Spectrometry 398

4.1 Basic instrumentation for MS 398

4.1.1 Introduction systems 399

4.1.2 Ionization systems 399

4.1.3 Ion analyzer systems 399

4.1.4 Detectors 401

5 Interpreting a Mass Spectrum 402

5.1 Types of characteristic ions 402

5.1.1 The molecular ion 402

5.1.2 Isotopic ions 404

5.1.3 Fragments 405

5.2 Determination of the molecular formula of a molecule by high-resolution MS 407

References 411

Worked Exercises 412

Exercises Proposed to the Student 441

Index 451