An Evaluation of the Semi-VOST Method for Determining Emissions from Hazardous Waste Incinerators

The Semi-Volatile Organic Sampling Train method was investigated to determine its reliability and to determine the bias and precision of the method when used to determine emissions from hazardous waste incinerators. Experiments showed that the matrix and sampling variables usually involved in sampling emissions from a hazardous waste incinerator had no significant effect on the recovery of 11 different organic compounds. Significant losses of the sampled compounds can occur during sample preparation. The degree of loss appears to be directly related to the compounds, vapor pressure. These losses can be corrected for by adding deuterated surrogates to the sample and analyzing the surrogates along with the native compounds.

The bias determination was based on dynamic spiking of the sampling train with five deuterated organic compounds selected from Appendix VIII of the Resource Conservation and Recovery Act regulations. The results show biases of from -1 ± 8 percent to -18 ± 27 percent for chlorinated and nonchlorinated compounds. Pyridine, a water-soluble compound, showed a larger bias of-29 ± 13 percent. Particular attention to the recovery of water soluble compounds is necessary to minimize bias in their determinations. Further work is needed to determine the reliability of laboratory-determined retention volumes that are used to determine sampling conditions.     

Results of an "emergency quality control study" as confirmation of a PCDD/PCDF-contamination of milk and butter samples

Elevated PCDD/F levels in four butter samples and one milk sample had to be confirmed under considerable time pressure. These samples should demonstrate a raising dioxin contamination in different regions of Germany caused by the use of Brazilian citrus pulp as feedstuff. Above all, the increase of 2,3,7,8-TCDD and 1,2,3,7,8-PeCDD had to be confirmed. Thus, an "emergency quality control study" was performed including five laboratories from the official food control in Germany. The results had to be reported about two to three weeks after the first announcement of the samples (including time for shipment). The five laboratories applied different extraction and clean-up methods, used different GC-columns and GC/MS-equipment and different standard solutions. The results are in a good agreement. Slightly different results for most individual congeners were of minor importance. A difference was observed only in the 2,3,7,8-TCDF content of one laboratory which was not relevant for the evaluation of the increase of the dioxin contamination in milk and dairy products. The laboratory's individual methods proved to give correct results even under a very tight schedule.     

Fluidized-bed-combustion ash for the solidification and stabilization of a metal-hydroxide sludge

Fluidized-bed-combustion (FBC) ash is a by-product from a developing technology for coal-fired power plants that will economically reduce air emissions to meet requirements of the Clean Air Act. FBC ash has physical and chemical properties similar to Portland cement, but only has moderate success as a pozzolan in concrete applications due to low compressive strengths. However, FBC ash has proven effective for use as a binder for the solidification and stabilization (S/S) of metal-bearing sludges. Physical and chemical characterization procedures were used to analyze FBC ash and a metal-bearing sludge obtained from a hazardous waste treatment facility to develop 12 different S/S mix designs. The mix designs consist of four binder designs to evaluate sludge-to-binder ratios of approximately 0, 0.5, and 1. Portland cement is used as a control binder to compare unconfined compressive strengths and Toxicity Characteristic Leaching Procedure (TCLP) analyses from different ratios of the FBC ash streams: fly ash, char, and spent bed material (SBM). Compressive strengths ranging from 84 lbs per square inch (psi) to 298 psi were obtained from various mix designs containing different sludge-to-ash ratios cured for 28 days. All the mix designs passed the TCLP. Recoveries from leaching for each metal were less than 5% for most mix designs. Results of unconfined compressive strengths, TCLP, and percent recovery calculations indicate that the mix design containing approximately a 1:1 ratio of fly ash to char-and-sludge is the best mix design for the S/S of the metal-bearing sludge.     

Validation of a test method for the measurement of methanol emissions from stationary sources

Title III of the 1990 Clean Air Act Amendments designated methanol as a pollutant to be regulated. The U.S. Environmental Protection Agency (EPA), through a contract with Research Triangle Institute, has developed a method for measuring methanol emissions from stationary sources. The methanol sampling train (MST) consists of a glass-lined heated probe, two condensate knockout traps, and three sorbent cartridges packed with Anasorb 747. Samples are desorbed with a 1:1 mixture of carbon disulfide (CS2) and N,N-dimethylformamide (DMF). Condensate water and CS2/ DMF samples are analyzed by gas chromatography with flame ionization detection. The MST has a practical quantitation limit of approximately 3 ppm for a 20-L sample. Samples were shown to be stable for at least two weeks after collection. Field tests of the MST and the National Council of the Paper Industry for Air and Stream Improvement (NCASI) methanol sampling method were conducted at two pulp and paper mills. Sampling and analysis procedures followed EPA Method 301 requirements. The sampling location for the first field test was the inlet vent to a softwood bleach plant scrubber, where the methanol concentration was approximately 30 ppm. The mean recovery of spike was 108.3% for the MST method and 81.6% for the NCASI method. Although neither method showed significant bias at the 95% confidence level, the between-methods bias was significantly different. A second field test was conducted at a vent from a black liquor oxidation tank where the methanol concentration was approximately 350 ppm. Mean spike recoveries were 96.6 and 94.2% for the MST and NCASI methods, respectively. The biases of the two methods and the between-methods bias were not significantly different for the second field test.