Elemental speciation and coupled techniques—towards faster and reliable analyses

Various procedures for accelerated and simplified sample preparation and analyte introduction into a plasma source spectrometer are developed and evaluated for speciation analysis of organometallic compounds using the example of alkyl and arylmetals and cyanocobalamin analogues. The topics discussed include microwave-assisted chemistry in three phase systems (solid–liquid–liquid and solid–liquid–gas), purge and capillary trap sample preparation and fast chromatography (multicapillary GC and microparticulate stationary phase reversed-phase LC) as a sample introduction technique for MIP-AES and ICP-MS, respectively. Integration of the sample preparation and of the chromatographic separation steps into a single instrumental module (as an accessory for atomic spectrometry) is evaluated. Attention is given to the reliability of information obtained in the case when standards are not available and when the target analytes are poorly defined (speciation of Cd bound to metallothionein isoforms). The utility of a dual orthogonal approach (complementary separation and complementary detection techniques) is demonstrated.