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

Persistent Link:
http://hdl.handle.net/10150/186754
Title:
Speciation and elemental analysis employing a custom designed echelle spectrometer and a charge injection device array detector.
Author:
Kolczynski, Jeffrey Daniel.
Issue Date:
1994
Publisher:
The University of Arizona.
Rights:
Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author.
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.
Type:
text; Dissertation-Reproduction (electronic)
Degree Name:
Ph.D.
Degree Level:
doctoral
Degree Program:
Chemistry; Graduate College
Degree Grantor:
University of Arizona
Committee Chair:
Denton, M. Bonner

Full metadata record

DC FieldValue Language
dc.language.isoenen_US
dc.titleSpeciation and elemental analysis employing a custom designed echelle spectrometer and a charge injection device array detector.en_US
dc.creatorKolczynski, Jeffrey Daniel.en_US
dc.contributor.authorKolczynski, Jeffrey Daniel.en_US
dc.date.issued1994en_US
dc.publisherThe University of Arizona.en_US
dc.rightsCopyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author.en_US
dc.description.abstractA 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.en_US
dc.typetexten_US
dc.typeDissertation-Reproduction (electronic)en_US
thesis.degree.namePh.D.en_US
thesis.degree.leveldoctoralen_US
thesis.degree.disciplineChemistryen_US
thesis.degree.disciplineGraduate Collegeen_US
thesis.degree.grantorUniversity of Arizonaen_US
dc.contributor.chairDenton, M. Bonneren_US
dc.contributor.committeememberBurke, Michael F.en_US
dc.contributor.committeememberFernando, Quintusen_US
dc.contributor.committeememberBarfield, Michaelen_US
dc.contributor.committeememberMiller, Walteren_US
dc.identifier.proquest9426582en_US
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