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Summary
Summary
Trace element analysis has a key role to play in quality control of food and diet. This timely book introduces the subject in a practical way - from sampling and the techniques available for trace analysis, to procedures for specific elements and data analysis. Beginning with a brief introduction and discussion of statistical evaluation of data, the subsequent chapter looks at trace analysis in general, with its essentials and terminology. Another section introduces sampling and preparation of foodstuffs such as wheat, potato, vegetables and milk. This is followed by descriptions of the various spectrometric techniques (atomic absorption, atomic emission, atomic fluorescence) that are available. Plasma techniques for both optical emission and mass spectrometry are presented, as are nuclear activation analysis and X-ray methods. A comparison of the various analytical techniques is provided, and a separate chapter handles speciation analysis. Finally, procedures for determining essential and toxic elements such as arsenic, iron, selenium and zinc are suggested, using several recent references. Detailed explanations and a simple format will appeal to laboratory technicians and graduate students, as well as more experienced researchers. Comprehensive coverage, coupled with illustrations and a guide to relevant literature and manufacturers, will make Trace Element Analysis of Food and Diet a valuable source of information for anyone working on analysis of trace elements in food, diet or other biological or environmental samples - particularly food engineers, agricultural scientists and government testing agency employees.
Table of Contents
Abbreviations | p. XV |
Chapter 1 Introduction | p. 1 |
1.1 Importance of Trace Elements in Food | p. 1 |
1.1.1 Essential Trace Elements | p. 1 |
1.1.2 Classification of Trace Elements | p. 3 |
1.1.3 Discovery of Essential Trace Elements | p. 3 |
1.1.4 Functions of Trace Elements | p. 5 |
1.2 Trace Element Studies | p. 5 |
References | p. 6 |
Chapter 2 Statistical Evaluation of Data | p. 8 |
2.1 Introduction | p. 8 |
2.2 Analytical Errors | p. 8 |
2.2.1 Accuracy and Precision | p. 8 |
2.2.2 Determinate and Indeterminate Errors | p. 9 |
2.2.3 Significant Figures | p. 9 |
2.3 Mean, Median, Mode, Range and Mean Deviation | p. 10 |
2.3.1 Mean | p. 11 |
2.3.2 Median | p. 11 |
2.3.3 Mode | p. 11 |
2.3.4 Range | p. 11 |
2.3.5 Mean Deviation | p. 11 |
2.4 Normal Distribution of Random Variables: Gaussian Distribution | p. 12 |
2.4.1 Log-Normal Distribution | p. 13 |
2.4.2 Standard Deviation | p. 14 |
2.5 Confidence Limit, Confidence Interval and Confidence Level | p. 15 |
2.6 Student's t Distribution: Confidence Limit for Small Number of Measurements | p. 16 |
2.7 Testing for Statistical Hypothesis | p. 17 |
2.7.1 Comparison of Experimental Means with True Value or with Each Other: Student's t Test | p. 17 |
2.7.2 Comparison of Two Experimental Standard Deviations: The F Test | p. 18 |
2.8 Rejection of Outliers | p. 19 |
2.8.1 Dixon's Q Criterion | p. 19 |
2.8.2 Student's t Criterion | p. 19 |
2.8.3 Gibbs's R Criterion | p. 19 |
2.9 Linear Regression Analysis | p. 22 |
2.9.1 Multiple Linear Regression | p. 25 |
2.10 Receptor Models | p. 26 |
2.10.1 Factor Analysis | p. 27 |
2.10.2 Chemical Mass Balance Method | p. 29 |
2.10.3 Enrichment Factors of the Elements | p. 30 |
References | p. 30 |
Chapter 3 Trace Analysis | p. 32 |
3.1 Scope of Trace Analysis | p. 32 |
3.2 Methodology, Terms and Definitions | p. 33 |
3.2.1 Sample, Analyte, Matrix and Blank | p. 33 |
3.2.2 Qualifications for a Trace Analysis Laboratory | p. 33 |
3.2.2.1 Water Purification | p. 35 |
3.2.3 Precision, Accuracy and Traceability | p. 39 |
3.2.4 Calibration | p. 40 |
3.2.5 Analytical Figures of Merit | p. 41 |
3.2.5.1 Detection Limit and Limit of Quantitation | p. 41 |
3.2.5.2 Analytical Range | p. 42 |
3.2.5.3 Sensitivity | p. 43 |
3.2.5.4 Signal to Noise Ratio | p. 44 |
3.2.5.5 Relations between Precision, Sensitivity, DL and S/N | p. 44 |
3.2.6 Selectivity and Interference | p. 45 |
3.2.7 Legal Importance of Results, Traceability and Other Related Concepts | p. 49 |
References | p. 51 |
Further Reading | p. 52 |
Chapter 4 Sampling and Sample Pre-treatment | p. 53 |
4.1 General Guidelines in Collection and Preparation of Staple Foods and Diets | p. 53 |
4.2 Sampling of Major Staple Foods | p. 54 |
4.2.1 Wheat | p. 54 |
4.2.2 Wheat Flour | p. 55 |
4.2.3 Bread | p. 55 |
4.2.4 Pasta | p. 56 |
4.2.5 Rice | p. 56 |
4.2.6 Potato | p. 56 |
4.2.7 Meat | p. 57 |
4.2.8 Vegetables and Fruits | p. 58 |
4.2.9 Milk | p. 58 |
4.2.10 Fresh Eggs | p. 59 |
4.2.11 Other Staple Foods | p. 59 |
4.3 Collection of Diet Samples | p. 59 |
4.3.1 Collection and Preparation of Foods for Composition of Representative Mixed Total Daily Diets, Market Basket Method | p. 60 |
4.3.2 Collection of Food Samples | p. 62 |
4.3.3 Duplicate Portion Technique | p. 62 |
4.3.4 Homogenization and Freeze Drying | p. 62 |
4.4 Sample Dissolution and Decomposition | p. 63 |
4.4.1 Dry Ashing Techniques | p. 66 |
4.4.2 Wet Ashing Techniques | p. 66 |
4.4.2.1 Open Wet Digestion | p. 69 |
4.4.2.2 Closed Wet Digestion | p. 70 |
References | p. 73 |
Further Reading | p. 74 |
Chapter 5 Spectrochemistry for Trace Analysis | p. 75 |
5.1 Fundamentals, Definitions and Terms | p. 75 |
5.2 Atomic and Molecular Spectrometry | p. 84 |
5.2.1 Molecular Spectrometry | p. 85 |
5.2.2 Luminescence Spectrometry | p. 86 |
5.2.3 Atomic Spectrometry | p. 86 |
5.3 Instrumentation | p. 86 |
5.3.1 Basic Components for Spectrometric Instrumentation | p. 87 |
5.3.1.1 Some Important Optical Units | p. 87 |
5.3.1.2 Wavelength Selectors | p. 89 |
5.3.1.3 Sources | p. 98 |
5.3.1.4 Detectors | p. 101 |
Further Reading | p. 104 |
Chapter 6 Atomic Absorption Spectrometry | p. 105 |
6.1 Introduction, History and Principles | p. 105 |
6.2 Instrumentation | p. 107 |
6.2.1 Sources | p. 107 |
6.2.2 Monochromators | p. 109 |
6.2.3 Atomizers | p. 109 |
6.2.3.1 Flame Atomizers | p. 109 |
6.2.3.2 Furnace Atomizers | p. 111 |
6.2.3.3 Cold Vapour Atomic Absorption Spectrometry (CVAAS) | p. 116 |
6.2.3.4 Hydride Generation Atomic Absorption Spectrometry | p. 117 |
6.2.3.5 Atom Traps for Flame Atomizers | p. 118 |
6.3 Interferences | p. 119 |
6.3.1 Non-spectral Interferences | p. 120 |
6.3.2 Spectral Interferences | p. 122 |
6.4 Analysis of Solid Samples | p. 130 |
6.5 A General Evaluation and Capabilities of AAS Systems | p. 131 |
References | p. 134 |
Further Reading | p. 135 |
Chapter 7 Atomic Emission and Mass Spectrometry using Plasma Techniques | p. 136 |
7.1 Introduction, History and Principles | p. 136 |
7.2 Optical Emission Spectrometry | p. 138 |
7.2.1 Optical Emission Spectrometry with Classical Sources | p. 138 |
7.2.2 Optical Emission Spectrometry with Plasma Sources | p. 140 |
7.2.2.1 Power Supplies for RF Generation | p. 142 |
7.2.2.2 Sample Introduction Systems | p. 143 |
7.2.2.3 Detection Systems and Measurement Modes in ICP-OES | p. 146 |
7.2.2.4 Interferences | p. 148 |
7.3 Inductively Coupled Plasma-Mass Spectrometry | p. 150 |
7.3.1 Instrumentation | p. 152 |
7.3.1.1 Mass Analyzers | p. 152 |
7.3.1.2 Detectors | p. 154 |
7.3.2 Interferences | p. 155 |
7.3.2.1 Spectral Interferences | p. 155 |
7.3.2.2 Non-spectral Interferences | p. 157 |
7.3.2.3 Approaches for Elimination of Interferences | p. 158 |
7.3.3 Isotope Dilution ICP-MS | p. 160 |
7.3.4 Instruments and Applications | p. 162 |
References | p. 163 |
Further Readings | p. 163 |
Chapter 8 Atomic Fluorescence Spectrometry | p. 164 |
8.1 Introduction, History and Principles | p. 164 |
8.2 Instrumentation | p. 167 |
8.2.1 Excitation Sources | p. 168 |
8.2.2 Atomizers | p. 168 |
8.3 Interferences | p. 170 |
8.4 Instrumentation and Applications | p. 170 |
References | p. 171 |
Further Reading | p. 171 |
Chapter 9 Nuclear Activation Analysis | p. 172 |
9.1 Introduction | p. 172 |
9.2 Basic Principles | p. 172 |
9.2.1 Radioactive Decay | p. 173 |
9.2.2 Half-Life | p. 173 |
9.2.3 Irradiation with Neutrons and Charged Particles | p. 174 |
9.3 Neutron Activation Analysis | p. 176 |
9.3.1 Cross Section | p. 177 |
9.3.2 Neutron Sources | p. 177 |
9.3.2.1 Laboratory Neutron Sources | p. 177 |
9.3.2.2 Research Reactors | p. 178 |
9.3.3 Preparation of Samples for Irradiation | p. 178 |
9.3.4 Short Irradiation | p. 179 |
9.3.5 Intermediate and Long-Lived Isotopes, Long Irradiation | p. 180 |
9.3.6 Calculation of Activity Produced after Neutron Irradiation | p. 181 |
9.3.7 Measurement of Gamma Rays | p. 184 |
9.3.7.1 Interaction of Gamma Rays with Matter | p. 184 |
9.4 Other Nuclear Techniques | p. 188 |
9.5 Determination of Trace Elements in Total Diet by Neutron Activation Analysis | p. 189 |
9.6 Present Status of Activation Analysis by Comparison with Other Analytical Techniques | p. 189 |
References | p. 191 |
Chapter 10 X-Ray Methods | p. 192 |
10.1 Introduction | p. 192 |
10.2 Basic Principles | p. 193 |
10.3 X-Ray Fluorescence Spectrometry | p. 194 |
10.3.1 Production of X-Rays | p. 195 |
10.3.2 Wavelength Dispersive X-Ray Fluorescence Spectrometry | p. 197 |
10.3.3 Energy Dispersive X-Ray Fluorescence | p. 198 |
10.3.4 Total Reflection X-Ray Fluorescence Spectrometry | p. 199 |
10.4 Particle-Induced X-Ray Emission Spectrometry | p. 201 |
10.5 Quantitative Determination in XRF Methods | p. 202 |
References | p. 204 |
Chapter 11 Speciation Analysis | p. 205 |
11.1 Importance of Speciation Analysis and Related Terms | p. 205 |
11.2 Chromatography and Electrophoresis | p. 207 |
11.2.1 Common Laws and Properties for Chromatography and Electrophoresis | p. 211 |
11.2.2 Instruments for Chromatography and Electrophoresis | p. 215 |
11.2.2.1 Columns | p. 215 |
11.2.2.2 Detectors | p. 216 |
11.3 Typical Instruments | p. 219 |
References | p. 221 |
Further Reading | p. 221 |
Chapter 12 Comparison of Analytical Techniques | p. 222 |
12.1 General Approaches for Selecting a Technique | p. 222 |
12.2 Criteria for Selecting an Analytical Technique | p. 222 |
12.2.1 Considerations for Sample Preparation | p. 223 |
12.2.2 Sensitivity | p. 224 |
12.2.3 Speed | p. 225 |
12.2.4 Ease of Use | p. 226 |
12.2.5 Cost of Instrumentation and Analysis | p. 228 |
12.3 Evaluation of Individual Analytical Techniques | p. 232 |
Chapter 13 Essentiality and Toxicity of Some Trace Elements and Their Determination | p. 233 |
13.1 Introduction | p. 233 |
13.2 Essential and Probably Essential Trace Elements | p. 233 |
13.2.1 Boron | p. 233 |
13.2.2 Chromium | p. 237 |
13.2.3 Cobalt | p. 237 |
13.2.4 Copper | p. 238 |
13.2.5 Iodine | p. 239 |
13.2.6 Iron | p. 239 |
13.2.7 Manganese | p. 240 |
13.2.8 Molybdenum | p. 240 |
13.2.9 Nickel | p. 241 |
13.2.10 Selenium | p. 242 |
13.2.11 Silicon | p. 244 |
13.2.12 Tin | p. 245 |
13.2.13 Vanadium | p. 245 |
13.2.14 Zinc | p. 246 |
13.3 Potentially Toxic Elements: Some Possibly with Essential Function | p. 248 |
13.3.1 Arsenic | p. 248 |
13.3.2 Fluorine | p. 249 |
13.3.3 Cadmium | p. 250 |
13.3.4 Lead | p. 252 |
13.2.5 Mercury | p. 252 |
13.3.6 Aluminium | p. 253 |
13.4 Literature on Determination of Trace Elements in Food Samples | p. 254 |
References | p. 304 |
Subject Index | p. 336 |