Analytical Atomic Spectrometry with Flames and Plasmas

Born in 1948, José Broekaert studied chemistry at the University of Gent, Belgium, graduating in 1970. After receiving his PhD from the University of Gent in 1976 and a stay in Germany as Alexander-von-Humboldt postdoctoral fellow the following year, he was a scientist at the ISAS, Dortmund from 1978 to 1991 and obtained the degree of "Geaggregeerde voor het hoger onderwijs" from the University of Antwerp, Belgium in 1985. He became associate professor at the University of Dortmund in 1991, full professor at the University of Leipzig in 1998 and, in 2002, joined the University of Hamburg. In 1998 he was a visiting Fulbright research scholar at Indiana University, Bloomington, USA. His main research interests include the development of plasma optical emission, atomic absorption and inorganic mass spectrometry methods and their application in solving analytical problems.

• Preface xiIntroduction 11 Basic Principles 41.1 Atomic structure 41.2 Plasmas 81.3 Emission and absorption of radiation 91.4 Ionization 181.5 Dissociation 231.6 Sources for atomic spectrometry 261.7 Analytical atomic spectrometry 312 Spectrometric Instrumentation 342.1 Figures of merit of an analytical method 342.2 Optical spectrometers 512.2.1 Optical systems 522.2.2 Radiation detectors 612.2.3 Miniaturized spectrometers 702.2.4 Non-dispersive spectrometers 732.3 Mass spectrometers 752.3.1 Types of mass spectrometers 762.3.2 Ion detection 842.3.3 Ion extraction 872.3.4 Ion optics and transmission 882.4 Data acquisition and treatment 892.5 Traceability 923 Sample Introduction Devices 943.1 Sample introduction by pneumatic nebulization 963.2 Ultrasonic nebulization 1133.3 Hydride and other volatile species generation 1143.4 Electrothermal vaporization 1203.4.1 The volatilization process 1213.4.2 Types of electrothermal devices 1223.4.3 Temperature programming 1253.4.4 Analytical performance 1273.5 Direct solids sampling 1283.5.1 Thermal methods 1283.5.2 Slurry atomization 1313.5.3 Arc and spark ablation 1363.5.4 Laser ablation 1423.6 Cathodic sputtering 1474 Atomic Absorption Spectrometry 1594.1 Principles 1594.2 Atomic absorption spectrometers 1614.2.1 Spectrometers 1614.2.2 Primary radiation sources 1634.3 Flame atomic absorption 1714.3.1 Flames and burners 1724.3.2 Nebulizers 1744.3.3 Figures of merit 1754.4 Electrothermal atomic absorption 1774.4.1 Atomizers 1784.4.2 Thermochemistry 1814.4.3 Figures of merit 1824.5 Special techniques 1874.5.1 Hydride and cold-vapor techniques 1874.5.2 Direct solids sampling 1894.5.3 Indirect determinations 1904.5.4 Flow injection analysis 1904.5.5 Diode laser atomic absorption spectrometry 1914.6 Background correction techniques 1924.6.1 Correction for background absorption with the deuterium lamp technique 1924.6.2 Background correction with the aid of the Zeeman effect 1944.6.3 The Smith–Hieftje technique 1974.6.4 Coherent forward scattering 1974.7 Fields of application 1994.8 Outlook 2055 Optical Emission Spectrometry 2075.1 Principles 2075.2 Atomic emission spectrometers 2175.3 Flame emission 2255.4 Arcs and sparks 2255.4.1 Arc emission spectrometry 2255.4.1.1 Arc characteristics 2255.4.1.2 DC arc spectrometry 2265.4.1.3 AC arc spectrometry 2285.4.2 Spark emission spectrometry 2285.4.2.1 Sparks 2285.4.2.2 Analytical features 2305.5 Plasma source OES 2325.5.1 DC plasma-jet OES 2325.5.1.1 Types of plasma jets 2325.5.1.2 Three-electrode plasma jet 2335.5.2 Inductively coupled plasma OES 2345.5.2.1 The inductively coupled plasma 2345.5.2.2 Instrumentation 2365.5.2.3 Analytical performance 2385.5.2.4 Applications 2475.5.3 Low-power high-frequency plasmas 2495.5.4 Microwave plasmas 2535.6 Glow discharge OES 2655.6.1 Hollow cathodes for OES 2665.6.2 Furnace emission spectrometry 2675.6.3 DC glow discharges with a flat cathode 2685.6.4 RF glow discharges 2725.6.5 New developments 2735.7 Laser sources 2796 Plasma Mass Spectrometry 2846.1 ICP mass spectrometry 2856.1.1 Instrumentation 2856.1.2 Analytical features 2876.1.3 Applications 3046.1.4 Outlook 3116.2 Glow discharge mass spectrometry 3146.2.1 Instrumentation 3166.2.2 Analytical performance 3236.2.3 Analytical applications 3237 Atomic Fluorescence Spectrometry 3327.1 Principles 3327.2 Instrumentation 3357.3 Analytical performance 3378 Laser-Enhanced Ionization Spectrometry 3398.1 Principles 3398.2 Figues of merit 3428.3 Analytical applications 3439 Sample Preparation for Atomic Spectrometry 3459.1 Sample preparation in direct compact sample analysis 3459.2 Grinding, sieving, and compaction of powders 3459.3 Sample dissolution 3479.3.1 Wet chemical methods 3479.3.2 Fusion procedures 3479.3.3 Microwave-assisted methods 3489.3.4 Combustion techniques 3489.4 Flow injection analysis 3489.5 Leaching sample preparation methods 34910 Comparison with Other Methods 35010.1 Power of detection 35010.2 Analytical accuracy 35210.3 Economic aspects 353Literature 355Index 402