Title page for ETD etd-08012012-040502

Type of Document Master's Thesis
Author Alderman, Lori A.
URN etd-08012012-040502
Title The evaluation and comparison of the extraction procedure toxicity test and the toxicity characteristic leaching procedure for the analysis of municipal wastewater sludges
Degree Master of Science
Department Environmental Engineering
Advisory Committee
Advisor Name Title
Dietrich, Andrea M. Committee Chair
Gallagher, Daniel L. Committee Member
Knocke, William R. Committee Member
  • Sewage sludge
Date of Defense 1989-06-05
Availability restricted

A viable sludge management alternative is land application of waste sludge. However, it is necessary to implement efficient monitoring and analysis of land applied sludges in order to assess potential health risks associated with this means of disposal.

The State of Virginia is considering a proposal that requires land-applied wastewater sludges to undergo analysis by EPA’s Toxicity Characteristic Leaching Procedure (TCLP) (EPA, 1986b) to determine if the sludge exhibits hazardous characteristics, which preclude land application as a management alternative. The method currently used for the analysis of hazardous wastes is the Extraction Procedure (EP) Toxicity Test. Both of these test methods analyze for trace organic chemicals and heavy metals. However, the TCLP is designed to analyze for volatile organic chemicals to a greater extent than the EP. Because of the added complexity and the current expense of the TCLP, the State is concerned that the TCLP may not be warranted for the analysis of trace organic chemicals in land-applied sludges.

This research was designed to compare the abilities of the EP and TCLP for the analysis of trace organic chemicals in wastewater sludges. Samples from three municipal wastewater treatment plants that utilize secondary biological treatment, aerobic digestion and land-apply waste sludge were evaluated by both EP and TCLP methods. Both tests utilize a weak acid extraction to remove organic chemicals from the wastewater sample. The weak acid extract was subjected to liquid-liquid extraction (EPA Method 625) to partition and concentrate the organic chemicals into methylene chloride; this methylene chloride extract was then subjected to GC and GC/MS for quantitative analysis and qualitative identification of targeted and nontargeted organic chemicals.

In order to assess recovery and extractability efficiencies of each test, surrogate standards were added prior to the test procedure. These standards were bromoform, 1-chlorooctane, DDT, ethylene dibromide (EDB, a volatile fungicide), fusarex (tetrachloronitrobenzene), and heptachlor. Control samples were run for both EP and TCLP, in addition to a sludge samples with no surrogates added.

Analysis indicated that both the TCLP and EP tests showed high variability for the recovery of the sludge surrogates. The recoveries of the surrogate standards were low and varied between zero and 30 percent depending on the standard and the matrix. Surrogate recoveries were evaluated with respect to various physical/ chemical properties of the individual standard, the sample site, and the test method utilized. Although the TCLP recovered the volatile surrogate standards only slightly better than the EP, there was no statistically significant difference between the TCLP and EP for the recovery of the non- and semi-volatile surrogate standards.

Specific trace organic chemicals identified in the sludges included dimethylpentanol, dichlorodimethoxybenzene, 4-methylphenol, and tetrabutylphenol. Other chemicals, such as contaminants and artifacts resulting from laboratory processing and background contamination in the reagents, were also identified in the blank control samples as well as the sludge samples.

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