Handbook of Inductively Coupled Plasma Spectrometry

Transcription

1 Handbook of Inductively Coupled Plasma Spectrometry Second Edition MICHAEL THOMPSON, BSc, PhD, ARCS, CChem., FRSC Department of Chemistry Birkbeck College University of London J. NICHOLAS WALSH, BSc, PhD Department of Geology Royal Holloway and Bedford New College University of London with additional invited chapters from S.J. Walton and G.E.M. Hall m BLACKIE ACADEMIC & PROFESSIONAL An Imprint of Chapman & Hall London Glasgow New York Tokyo Melbourne Madras

2 Contents 1 Introduction Preliminary-purpose and scope of book The ICP as a spectroscopic source Applications of the ICP Simplicity of the ICP technique The literature of ICP-AES Historie development of ICP spectrometry Background to quantitative ICP analysis Sample introduction (nebulization) Sample excitation System Analysis and quantification of emission spectrum Range of determinable elements in geological materials 14 2 Analytical characteristics Introduction Simultaneous analysis Compromise operating conditions Sequential analysis ICP System Detection limits Calibration ränge of ICP-AES Interferences Spectral overlaps Stray light interference Matrix effect Precision and aecuraey Chemometric improvements to data quality Experimental considerations Solution volumes and sample weights Number of elements determined in liquid samples Number of elements determined in solid samples The injeetion of organic liquids into an ICP 40 3 Instrumentation for ICP-AES Introduction Spectrometers General requirements Simultaneous spectrometers Sequential spectrometers Combined simultaneous/sequential spectrometers Plasma torches Nomenclature The Greenfield torch The Fassel torch The Minitorch Torch maintenance Nebulizer Systems Introduction Concentric pneumatic nebulizers 66 vii

3 Vlll CONTENTS Cross-flow nebulizers Babington-type nebulizers Frit-type nebulizers Ultrasonic nebulizers Direct nebulization Spray Chambers Radiofrequency generators and source Electronics, Computers and Software Software requirements Trends Fourier transform spectrometers ICP-atomic fluorescence spectrometry Direct current plasmas (DCP) Microwave plasmas (MIP) Choice of an ICP System ICP-AES in relation to AAS ICP-AES and X-ray fluorescence ICP-AES and DCP emission spectrometry ICP-AES and ICP-mass spectrometry ICP-AES and other excitation methods Evaluation of an ICP A ES System 92 4 Silicate rock analysis Dissolution methods for Silicates Introduction Fusion dissolution methods Hydrofluoric acid dissolution methods open evaporation Hydrofluoric acid dissolution methods closed digestion Instrument calibration Major dement determinations Trace dement analysis Rare earth dement determinations Introduction Dissolution procedure REE Separation REE spectral lines Evaluation of results Multielement applications of ICPS in applied geochemistry The nature and evolution of applied geochemistry Introduction General aspects of applied geochemical analysis Analytical requirements in applied geochemistry Analytical quality control procedures ICP Instrumentation in relation to the requirements of applied geochemistry Introduction Translational interference effects Rotational interference effects Other instrumental constraints in multielement analysis Decomposition procedures in applied geochemical analysis Introduction General aspects of large-batch analysis Decomposition with nitric acid and perchloric acid Decomposition with hydrofluoric acid, nitric acid and perchloric acid (test tube Version) 156

4 CONTENTS 6 Gas phase sample injection The development of gas phase injection methods Methodology of the hydride injection System Equipment Operating conditions Performance of the hydride generation/icp System Interference effects and their avoidance Arsenic speciation methods Applications of the hydride injection System General introduction Traces of arsenic, antimony and bismuth in soils and Sediments Traces of arsenic, antimony and bismuth in plant materials Trace concentrations of selenium in soils and Sediments The determination of trace concentrations of arsenic, antimony, bismuth, selenium and tellurium in waters The determination of tin in rock, soils and Sediments Injection methods for solid samples Introduction to solid sample injection methods Sample injection following electrothermal vaporization Direct sample injection from a graphite rod Discrete sample injection by means of laser ablation General introduction The Lasertrace System The LMA10 laser-icp microprobe System Nebulization of slurries Water analysis by ICP-AES Introduction General aspects of water analysis Sampling Filtration Storage Stabilization Avoidance of contamination Direct water analysis by ICP-AES Pneumatic nebulizers Alternative nebulizers Gas phase injection Electrothermal vaporization and other discrete methods Water analysis with preconcentration Evaporation methods Mixed-bed ion exchange method Selective ion exchange methods Solvent extraction methods A chelation solvent extraction procedure Coprecipitation methods The analysis of environmental materials by ICP-AES Introduction Air analysis Volatile contaminants Particle contaminants Sewage Sludge 219 ix

5 X CONTENTS 9.4 Domestic dust, road dust and industrial dust Domestic dusts Road dusts Industrial dusts Domestic and industrial refuse The analysis of animal and plant tissues General introduction Sample decomposition of biological materials Destruction of organic matter in plant and animal tissue with perchloric acid-nitric acid mixtures The analysis of archaeological materials by ICP-AES Introduction Archaeological materials Analysis of flints Pottery and clay analysis Analysis of bricks, tiles, glazes, etc Analysis of metals Analysis of slags and ores Inductively coupled plasma mass spectrometry Instrumentation Optimization Interferences Spectral interferences Non-spectral interferences Calibration strategies Externa! Isotope dilution Standard additions Applications of ICP MS with sample introduction by nebulization Elemental analysis of solubilized geological samples Isotope ratio measurements Analysis of waters Other modes of sample introduction Electrothermal vaporization (ETV) Direct sample insertion device (DSID) Laser ablation of solids Are nebulization (solid sampling) Slurry nebulization (solid sampling) Future directions Analysis of metals by ICP-AES Introduction Instrument calibration Internal Standards Sample preparation and dissolution Analysis of iron and steel Spectral lines Sample dissolution Analysis of other metals Virgin aluminium program Titanium-boron-aluminium program Zirconium-aluminium program Chromium program Chrome carbon program 281

6 CONTENTS XI Nickel-cobalt alloy program Ferro-boron program Nickel-boron program Copper base program Stellite program Manganese tablet program Ferro-aluminium program 285 Appendix 1 Safety 287 Appendix 2 Manufacturers of ICP Systems and accessories 291 References 294 Index 311