Speciation and elemental analysis employing a custom designed echelle spectrometer and a charge injection device array detector.

Abstract

A custom designed echelle spectrometer coupled with a charge injection device (CID) detector was applied to a series of analytical challenges in atomic emission spectroscopy (AES). By taking advantage of the two dimensional spectral format of an echelle/CID spectrometer, simultaneous, multi-elemental atomic spectroscopic information can be directly obtained. A direct current plasma (DCP) was utilized as the AES excitation source. The echelle/CID system has a large spectral elemental database. Through the utilization of vast amounts of spectral information and the application of fundamental spectroscopic principles, an intelligent analytical system was designed to make certain routine and non-routine decisions with minimal intervention by the analyst. The utility of the echelle/CID system is investigated through its application to several analytical challenges. These challenges include automated-qualitative analysis, quantitative analysis for samples of limited size (microgram quantities) and qualitative and quantitative chromatographic analysis of various metal species. The results of an analyses generated by an automated-qualitative routine for the determination of elemental constituents in environmental contaminants, unknown particulate from a hospital air delivery system and laboratory waste samples are presented. The ability to simultaneously integrate multi-elemental information makes the echelle/CID system well suited for the quantitative analysis of trace sample quantities. The echelle/CID system was employed in the trace determination of 1000, 400 and 40 micrograms/ml NBS standard reference material 1633a, coal fly ash, samples. Finally, the echelle/CID AES system is utilized as an element selective detector for high performance liquid chromatography (HPLC). HPLC separation methods were developed for the quantitative analysis of iron and copper oxidation states. The results of the HPLC separation of iron(II) and iron(III) through their interactions with the mobile phase modifier, 8-hydroxyquinoline are presented. The results of the HPLC separation of copper(I) and copper(II) are in an mobile phase containing 2,9 dimethyl 1,10 phenanthroline are presented. A novel solid phase extraction (SPE) method for Cu(I) was also developed. The results of the SPE method used to monitor the Cu(I) concentration in a series of electroless copper plating baths are presented.