Handbook of Inductively Coupled Plasma Spectrometry

1 Introduction.- 1.1 Preliminary-purpose and scope of book.- 1.1.1 The ICP as a spectroscopic source.- 1.1.2 Applications of the ICP.- 1.1.3 Simplicity of the ICP technique.- 1.1.4 The literature of ICP—AES.- 1.2 Historic development of ICP spectrometry.- 1.3 Background to quantitative ICP analysis.- 1.3.1 Sample introduction (nebulization).- 1.3.2 Sample excitation system.- 1.3.3 Analysis and quantification of emission spectrum.- 1.4 Range of determinable elements in geological materials.- 2 Analytical characteristics.- 2.1 Introduction.- 2.2 Simultaneous analysis.- 2.2.1 Compromise operating conditions.- 2.3 Sequential analysis ICP system.- 2.4 Detection limits.- 2.5 Calibration range of ICP—AES.- 2.6 Interferences.- 2.6.1 Spectral overlaps.- 2.6.2 Stray light interference.- 2.6.3 Matrix effect.- 2.7 Precision and accuracy.- 2.7.1 Chemometric improvements to data quality.- 2.8 Experimental considerations.- 2.8.1 Solution volumes and sample weights.- 2.8.2 Number of elements determined in liquid samples.- 2.8.3 Number of elements determined in solid samples.- 2.9 The injection of organic liquids into an ICP.- 3 Instrumentation for ICP—AES.- 3.1 Introduction.- 3.2 Spectrometers.- 3.2.1 General requirements.- 3.2.2 Simultaneous spectrometers.- 3.2.3 Sequential spectrometers.- 3.2.4 Combined simultaneous/sequential spectrometers.- 3.3 Plasma torches.- 3.3.1 Nomenclature.- 3.3.2 The Greenfield torch.- 3.3.3 The Fassel torch.- 3.3.4 The Minitorch™.- 3.3.5 Torch maintenance.- 3.4 Nebulizer systems.- 3.4.1 Introduction.- 3.4.2 Concentric pneumatic nebulizers.- 3.4.3 Cross-flow nebulizers.- 3.4.4 Babington-type nebulizers.- 3.4.5 Frit-type nebulizers.- 3.4.6 Ultrasonic nebulizers.- 3.4.7 Direct nebulization.- 3.4.8 Spray chambers.- 3.5 Radiofrequency generators and source.- 3.6 Electronics, computers and software.- 3.6.1 Software requirements.- 3.6.2 Trends.- 3.7 Fourier transform spectrometers.- 3.8 ICP-atomic fluorescence spectrometry.- 3.9 Direct current plasmas (DCP).- 3.10 Microwave plasmas (MIP).- 3.11 Choice of an ICP system.- 3.11.1 ICP—AES in relation to A AS.- 3.11.2 ICP—AES and X-ray fluorescence.- 3.11.3 ICP—AES and DCP emission spectrometry.- 3.11.4 ICP—AES and ICP-mass spectrometry.- 3.11.5 ICP—AES and other excitation methods.- 3.11.6 Evaluation of an ICP—AES system.- 4 Silicate rock analysis.- 4.1 Dissolution methods for silicates.- 4.1.1 Introduction.- 4.1.2 Fusion dissolution methods.- 4.1.3 Hydrofluoric acid dissolution methods—open evaporation.- 4.1.4 Hydrofluoric acid dissolution methods—closed digestion.- 4.2 Instrument calibration.- 4.3 Major element determinations.- 4.3 Trace element analysis.- 4.4 Rare earth element determinations.- 4.5.1 Introduction.- 4.5.2 Dissolution procedure.- 4.5.3 REE separation.- 4.5.4 REE spectral lines.- 4.5.5 Evaluation of results.- 5 Multielement applications of ICPS in applied geochemistry.- 5.1 The nature and evolution of applied geochemistry.- 5.1.1 Introduction.- 5.2 General aspects of applied geochemical analysis.- 5.2.1 Analytical requirements in applied geochemistry.- 5.2.2 Analytical quality control procedures.- 5.3 ICP instrumentation in relation to the requirements of applied geochemistry.- 5.3.1 Introduction.- 5.3.2 Translational interference effects.- 5.3.3 Rotational interference effects.- 5.3.4 Other instrumental constraints in multielement analysis.- 5.4 Decomposition procedures in applied geochemical analysis.- 5.4.1 Introduction.- 5.4.2 General aspects of large-batch analysis.- 5.4.3 Decomposition with nitric acid and perchloric acid.- 5.4.4 Decomposition with hydrofluoric acid, nitric acid and perchloric acid (test tube version).- 6 Gas phase sample injection.- 6.1 The development of gas phase injection methods.- 6.2 Methodology of the hydride injection system.- 6.2.1 Equipment.- 6.2.2 Operating conditions.- 6.2.3 Performance of the hydride generation/ICP system.- 6.2.4 Interference effects and their avoidance.- 6.2.5 Arsenic speciation methods.- 6.3 Applications of the hydride injection system.- 6.3.1 General introduction.- 6.3.2 Traces of arsenic, antimony and bismuth in soils and sediments.- 6.3.3 Traces of arsenic, antimony and bismuth in plant materials.- 6.3.4 Trace concentrations of selenium in soils and sediments.- 6.3.5 The determination of trace concentrations of arsenic, antimony, bismuth, selenium and tellurium in waters.- 6.3.6 The determination of tin in rock, soils and sediments.- 7 Injection methods for solid samples.- 7.1 Introduction to solid sample injection methods.- 7.2 Sample injection following electrothermal vaporization.- 7.3 Direct sample injection from a graphite rod.- 7.4 Discrete sample injection by means of laser ablation.- 7.4.1 General introduction.- 7.4.2 The Lasertrace system.- 7.4.3 The LMA10 laser-ICP microprobe system.- 7.5 Nebulization of slurries.- 8 Water analysis by ICP—AES.- 8.1 Introduction.- 8.2 General aspects of water analysis.- 8.2.1 Sampling.- 8.2.2 Filtration.- 8.2.3 Storage.- 8.2.4 Stabilization.- 8.2.5 Avoidance of contamination.- 8.3 Direct water analysis by ICP—AES.- 8.3.1 Pneumatic nebulizers.- 8.3.2 Alternative nebulizers.- 8.3.3 Gas phase injection.- 8.3.4 Electrothermal vaporization and other discrete methods.- 8.4 Water analysis with preconcentration.- 8.4.1 Evaporation methods.- 8.4.2 Mixed-bed ion exchange method.- 8.4.3 Selective ion exchange methods.- 8.4.4 Solvent extraction methods.- 8.4.5 A chelation—solvent extraction procedure.- 8.4.6 Coprecipitation methods.- 9 The analysis of environmental materials by ICP—AES.- 9.1 Introduction.- 9.2 Air analysis.- 9.2.1 Volatile contaminants.- 9.2.2 Particle contaminants.- 9.3 Sewage sludge.- 9.4 Domestic dust, road dust and industrial dust.- 9.4.1 Domestic dusts.- 9.4.2 Road dusts.- 9.4.3 Industrial dusts.- 9.5 Domestic and industrial refuse.- 9.6 The analysis of animal and plant tissues.- 9.6.1 General introduction.- 9.6.2 Sample decomposition of biological materials.- 9.6.3 Destruction of organic matter in plant and animal tissue with perchloric acid-nitric acid mixtures.- 10 The analysis of archaeological materials by ICP—AES.- 10.1 Introduction.- 10.2 Archaeological materials.- 10.2.1 Analysis of flints.- 10.2.2 Pottery and clay analysis.- 10.2.3 Analysis of bricks, tiles, glazes, etc.- 10.2.4 Analysis of metals.- 10.2.5 Analysis of slags and ores.- 11 Inductively coupled plasma mass spectrometry.- 11.1 Instrumentation.- 11.2 Optimization.- 11.3 Interferences.- 11.3.1 Spectral interferences.- 11.3.2 Non-spectral interferences.- 11.4 Calibration strategies.- 11.4.1 External.- 11.4.2 Isotope dilution.- 11.4.3 Standard additions.- 11.5 Applications of ICP-MS with sample introduction by nebulization.- 11.5.1 Elemental analysis of solubilized geological samples.- 11.5.2 Isotope ratio measurements.- 11.5.3 Analysis of waters.- 11.6 Other modes of sample introduction.- 11.6.1 Electrothermal vaporization (ETV).- 11.6.2 Direct sample insertion device (DSID).- 11.6.3 Laser ablation of solids.- 11.6.4 Arc nebulization (solid sampling).- 11.6.5 Slurry nebulization (solid sampling).- 11.7 Future directions.- 12 Analysis of metals by ICP—AES.- 12.1 Introduction.- 12.1.1 Instrument calibration.- 12.1.2 Internal standards.- 12.1.3 Sample preparation and dissolution.- 12.2 Analysis of iron and steel.- 12.2.1 Spectral lines.- 12.2.2 Sample dissolution.- 12.3 Analysis of other metals.- 12.3.1 Virgin aluminium program.- 12.3.2 Titanium-boron-aluminium program.- 12.3.3 Zirconium-aluminium program.- 12.3.4 Chromium program.- 12.3.5 Chrome carbon program.- 12.3.6 Nickel-cobalt alloy program.- 12.3.7 Ferro-boron program.- 12.3.8 Nickel-boron program.- 12.3.9 Copper base program.- 12.3.10 Stellite program.- 12.3.11 Manganese tablet program.- 12.3.12 Ferro-aluminium program.- Appendix 1 Safety.- Appendix 2 Manufacturers of ICP systems and accessories.- References.