Trends and applications of integrated automated ultra-trace sample handling and analysis (T9)

Full text: Automated analysis, sub-ppt detection limits, and the trend toward speciated analysis (rather than just elemental analysis) force the innovation of sophisticated and integrated sample preparation and analysis techniques. Traditionally, the ability to handle samples at ppt and sub-ppt levels has been limited to clean laboratories and special sample handling techniques and equipment. The world of sample handling has passed a threshold where older or 'old fashioned' traditional techniques no longer provide the ability to see the sample due to the influence of the analytical blank and the fragile nature of the analyte. When samples require decomposition, extraction, separation and manipulation, application of newer more sophisticated sample handling systems are emerging that enable ultra-trace analysis and species manipulation. In addition, new instrumentation has emerged which integrate sample preparation and analysis to enable on-line near real-time analysis. Examples of those newer sample-handling methods will be discussed and current examples provided as alternatives to traditional sample handling. Two new techniques applying ultra-trace microwave energy enhanced sample handling have been developed that permit sample separation and refinement while performing species manipulation during decomposition. A demonstration, that applies to semiconductor materials, will be presented. Next, a new approach to the old problem of sample evaporation without losses will be demonstrated that is capable of retaining all elements and species tested. Both of those methods require microwave energy manipulation in specialized systems and are not accessible through convection, conduction, or other traditional energy applications. A new automated integrated method for handling samples for ultra-trace analysis has been developed. An on-line near real-time measurement system will be described that enables many new automated sample handling and measurement capabilities. This new approach has been developed for the semiconductor industry; however, as with most new technologies its applicability extends to many other areas as well including environmental, pharmaceutical, clinical and industrial chemical processing. This instrumental system represents a fundamentally new approach. Sample preparation has been integrated as a key system element to enable automation of the instrument system. It has long been believed that an automated fully integrated system was not feasible if a powerful MS system were included. This application demonstrates one of the first fully automated and integrated sample preparation and mass spectrometric instrumental analyses systems applied to practical use. The system is also a broad and ambitious mass based analyzer capable not only for elements but also for direct speciated analysis. The complete analytical suite covering inorganic, organic, organo-metallic and speciated analytes is being applied for critical contamination control of semiconductor processes. As with new paradigms technology it will now extend from its current use into those other applications needing real-time fully automated multi-component analysis. Refs. 4 (author)