Many elemental analysis techniques can accurately produce and process a large volume of data in a relatively short time. However, many techniques require that the sample be in the form of a solution. The preparation to meet this requirement often involves a significant degree of time and knowledge from a chemist. Sample preparation automation can be developed to eliminate or reduce these time and knowledge requirements. A flow-through digestion device and an expert system were developed as part of an automation approach for sample preparation prior to inductively coupled plasma atomic emission spectometry (ICP-AES) analysis. The flow-through device was developed for on-line stopped-flow microwave heated digestions of organic biological material. Milk, whole blood, and urine were digested with concentrated nitric acid, concentrated sulfuric acid, and 30% hydrogen peroxide. Digestion of a sample occurs within the device when the sample and reagents are exposed to microwave energy from a commercial apparatus. The physical and chemical characteristics of the digestions dictated the device design. The expert system was designed to perform open-vessel sample digestion method development. After an initial sample digestion was attempted, and the expert system used its modification rules to develop a successful digestion procedure. The expert system then accessed a simplex program to optimize key parameters. The expert system was capable of developing accurate digestion procedures for whole milk, whole blood, and urine. Accurate results were obtained from the analysis, minimal analyte loss and contamination occurred.
| Identifer | oai:union.ndltd.org:UMASS/oai:scholarworks.umass.edu:dissertations-8555 |
| Date | 01 January 1993 |
| Creators | Martines, Laura Jean |
| Publisher | ScholarWorks@UMass Amherst |
| Source Sets | University of Massachusetts, Amherst |
| Language | English |
| Detected Language | English |
| Type | text |
| Source | Doctoral Dissertations Available from Proquest |
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