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Title: On-line sample pretreatment of environmental samples for use with atomic spectrometry
Author: Murphy, James Robert
Awarding Body: University of Plymouth
Current Institution: University of Plymouth
Date of Award: 1998
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The objective of this study was to develop novel techniques for on-line sample pre-treatment for use with atomic spectroscopy. Preconcentration of the analytes using either complexation of the analyte(s) on an analytical column or by in-situ (in atomiser) trapping on a pre-coated graphite tube has been used. The samples were manipulated using flow injection analysis and detection achieved in most cases by ETAAS. All aspects of the study are supported by reference to the literature. Using the above approach, a new method has been developed to determine mercury in environmental (sediment) and biological (tuna fish) samples. This approach successfully achieved a sample throughput of 20-30 sample per hour, with a method detection limit of 0.2 ng g*^ (3a) and a precision of less than 10% at the 0.1 ug g"^ level. An interference study was conducted and seven elements ( As\, Cd", Cu", Ni", Pb". Sb'' and Se"") shown to give less than a 5% interference when the interferent concentration was 2 orders of magnitude greater than the Hg. Silver showed a 9% interference when one order of magnitude greater than the Hg. The technique of "in atomiser trapping" was applied to the determination of As, Bi, Sb and Se, in lake water samples. The hydrides were sequestrated upon an Ir coated graphite tube and the instrumental and chemical parameters optimised for multi-element determinations. Iridium has been identified as the best trapping material (coating) for multi-element determinations. The final method gave detection limits of 0.82, 0.04, 0,26 and 0.29 ug 1'^ (500 ul sample loop) for As, Bi, Sb and Se respectively. A characteristic mass of 177 pg for As, 91 pg for Bi, 107 pg for Sb and 90 pg for Se was achieved. Good agreement was obtained with certified and standard reference materials and the method was successfully applied to the determination of As, Bi, Sb and Se in lake water samples. Six elements (Cd, Cu, Fe, Mn, Ni and Pb) were selected for determination in seawater samples by multi-element on-line column preconcentration. The sample stream was mixed on-line with a buffered solution of diethylammonium dithiocarbamate (DDDC). and the metal-DDC complex retained upon a Cie RP silica column. Ethanol was then used to elute the metals from the column directly into the graphite tube. Disappointing results, were obtained due to interference problems, and although more work is required before this approach may be routinely used, it is shown to have potential for the future. Overall, this study has shown that novel methods employing flow injection methodologies for separation and preconcentration are a viable way to prepare environmental sample for analysis by ETAAS. Further it has demonstrated that multi-element analysis is possible for low levels of analyte despite the presence of troublesome matrices, although further work is required to achieve the ultimate goal of a universal method suitable for all analytes irrespective of the sample type.
Supervisor: Not available Sponsor: Bodenseewerk Perkin Elmer GmbH
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: Water pollution & oil pollution