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Dissertation
Application of supercritical fluid extraction in the isolation of hydrophobic organic compounds from aquatic suspended sediments
Doctor of Philosophy (Ph.D.), Drexel University
Sep 1996
DOI:
https://doi.org/10.17918/00000516
Abstract
Many hydrophobic organic compounds (HOCs) demonstrate a high affinity for fine particles such as suspended sediments (SS), and supercritical fluid extraction (SFE) has the potential to be the most suitable method for the extraction of HOCs from SS. The high diffusivity, low viscosity. and zero surface tension of supercritical fluids allow them to penetrate microporous materials easily. The overall objective of this thesis was to develop an analytical protocol for the isolation of HOCs from SS using SFE for subsequent chromatographic analysis. In achieving this overall objective. a series of evaluation, optimization. validation, and application studies had been successfully conducted, resulting in findings and conclusions which contributed to the development of a protocol for analysis of SS collected from aquatic environments. Evaluation of different filters showed that membrane filters and glass fiber filters with binder are generally sorbing filters. A glass fiber filter with no binder (MSI TCLP) was shown to be the optimum filter for the collection of SS for subsequent SFE. A filter cleanup procedure prior to SFE was developed. Optimization of drying method specific for filtered SS resulted in the development of a closed-jar drying method, which was shown to be more efficient than air drying and freeze drying. Optimization of SFE conditions identified a pressure of 355 atm, a temperature of 120[degrees]C, and a modifier mixture of 250 [mu]l each of water, methanol, and methylene chloride, as the best combination for the extraction of HOCs from SS. The analyte collection technique was also optimized. Validation of the developed method using a standard reference material showed an overall accuracy of 91% and a precision of 7.7% relative standard deviation (RSD) for polynuclear aromatic hydrocarbons (PAHs), which are better than those of EPA Method 3561. Application of the developed method on natural aquatic samples of SS obtained during rain events further confirmed its acceptability, as shown by a precision of 10.9% RSD for all detected organic compounds, and 9.2% for all detected PAHs. Thus, the new method is a quick and reliable SFE analytical protocol for the isolation of HOCs from aquatic SS.
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Details
- Title
- Application of supercritical fluid extraction in the isolation of hydrophobic organic compounds from aquatic suspended sediments
- Creators
- Mario Borinaga Capangpangan
- Contributors
- Nicholas Peter Cernansky (Advisor) - Drexel University, Mechanical Engineering and MechanicsIrwin H. Suffet (Advisor)
- Awarding Institution
- Drexel University
- Degree Awarded
- Doctor of Philosophy (Ph.D.)
- Publisher
- Drexel University; Philadelphia, Pennsylvania
- Number of pages
- xix, 309 pages
- Resource Type
- Dissertation
- Language
- English
- Academic Unit
- Environmental Studies Institute (1970-1997); Drexel University
- Other Identifier
- 991014970189404721