Joseph E. Knoll

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 n...

Chromium analysis at a ferrochrome smelter, a chemical plant and a refractory brick plant

Techniques were developed to sample and analyze the Cr content of particulate samples with emphasis on determining the concentration of the carcinogen Cr/sup +6/. Cr/sup +6/ is extracted to alkaline solution and analyzed colorimetrically. Residual particles are extracted with acid solution to remove soluble Cr/sup +3/, which is determined by atomic absorption spectrometry. This methodology was tested on samples from three diverse types of sources: a ferrochrome smelter, a chemical plant, and a refractory brick plant. Identical quadruplicate samples were collected to determine accuracy and precision of the collection and analysis procedures, and extraction of Cr/sup +6/ and Cr/sup +3/. A statistical analysis revealed that the precision of Cr/sup +6/ analysis is comparable to that of the particulate mass determination. The stability of Cr/sup +6/ in particulate form and in solution was determined. Size resolved particulate samples were collected to determine the particle size versus the Cr/sup +6/ content. At the ferrochrome smelter and the chemical plant the majority of the Cr/sup +6/ was contained in the respirable particles. The accuracy and completeness of the chemical methods employed were verified by neutron activation analysis, x-ray photoelectron spectroscopy, and scanning electron microscopy-energy dispersive x-ray analysis.

Determination of high sulfur dioxide concentrations and carbon dioxide in electric utility plants by alkaline permanganate sampling and ion chromatography

A manual 24-h integrated method for determining high concentrations of SO/sub 2/ and CO/sub 2/ in electric utility plants was field-tested upstream from an SO/sub 2/ control system. Samples were collected in an alkaline, potassium-permanganate solution contained in restricted-orifice impingers. Samples were analyzed by ion chromatography. The SO/sub 2/ collection efficiency was 84.6 +/- 4.2 (5.0 percent) relative to an independent continuous monitoring system; the CO/sub 2/ determination was unbiased provided that the sample flow rate was maintained below 40 cm/sup 3//min. The relative standard deviation for the SO/sub 2/ and CO/sub 2/ determinations was 5 and 2 percent, respectively. The method, when combined with earlier work downstream from a flue gas desulfurization systems, can be used for determining the efficiency of a flue gas desulfurization system. However, the upstream method may be biased low by approximately 10 percent.

EPA Reference Method 25 - laboratory evaluation and field testing

EPA Reference Method 25 for measurement of total gaseous nonmethane organics as carbon in source emissions was evaluated in the laboratory and through field testing. Laboratory evaluation included development and testing of a nonmethane organic analyzer. In addition, a series of tests was performed on the condensate trap recovery system. The tests involved evaluation of two different condensate trap recovery system designs. The first design was very similar to the Federal Register design and the second design was a modified system for minimizing interference from trapped carbon dioxide. Field testing of the method was performed at two different printing plants. Both plants used carbon bed adsorption for solvent recovery and control of VOC emissions. Samples were collected from the inlet and outlet streams of adsorption units at both plants. In addition to Method 25 samples, Method 18 samples were collected for analysis by gas chromatography with flame ionization detection. The results of all the laboratory and field test samples are described.

A Manual Method for Measurement of Reduced Sulfur Compounds

A manual method for measuring reduced sulfur compounds in kraft pulp mill and sulfur recovery plant emissions was evaluated. The method involves removing SO/sub 2/ from the gas stream (if present) with a citric acid-potassium citrate buffer that passes reduced sulfur compounds; thermal oxidation of all reduced sulfur compounds to SO/sub 2/; collection of the SO/sub 2/ in H/sub 2/O/sub 2/; and a titrimetric analysis of the H/sub 2/O/sub 2/ for SO/sub 4//sup 2 -/. A heated filter removes alkaline particulate matter that would produce a negative interference if absorbed by the buffer. When used at kraft pulp mills, the method agrees closely with Reference Method 16, provided that nonregulated reduced sulfur compounds, such as carbonyl sulfide, are not present in the emissions. At sulfur recovery plants, nonregulated reduced sulfur compounds, such as thiophene, are likely to be present in the emissions and will produce a positive bias in the results obtained with this method. The precision of the method ranges from 1 to 7% relative standard deviation.

Development of a 24-Hour Method for Analysis of SO2 and CO2 from Electric Utility Units Equipped with Flue Gas Desulfurization Scrubbers

A procedure was developed for the 24-h determination of SO/sub 2/ and CO/sub 2/ in effluent gas from fossil fuel combustion sources. Laboratory experiments were conducted to test absorption of SO/sub 2/ in hydrogen peroxide solution and absorption of CO/sub 2/ by sodium hydroxide on an inert substrate at expected ambient temperatures of 15 to 45/sup 0/C. Isopropyl alcohol cannot be used to trap sulfuric acid and particulates because it permeates the sampling train and prevents complete absorption of CO/sub 2/. Elemental analysis of stack particulates revealed that at least 31 elements were present. Iron and other elements interfered with SO/sub 2/ analysis. These particulates were completely removed by a heated borosilicate glass filter. Both laboratory and field experiments showed that molecular sieves are a promising alternative for CO/sub 2/ absorption. Statistical evaluation of data collected at three units equipped with flue gas desulfurization scrubbers proved that the new procedure is accurate and precise.

The Collaborative Test of Method 6-B: Twenty-Four-Hour Analysis of SO2 and CO2

The results are presented from the collaborative test of EPA Method 6-B for the 24-h analysis of SO2, CO2, and emission rate. Using both the intermittent and continuous options of Method 6-B, nine laboratories simultaneously sampled the stack at a flue gas desulfurizing unit of a coal burning electric power plant. The precision and accuracy of the method was based on results of 145 24-h determinations performed by the collaborators over a five day period. The estimates of repeatability (or within laboratory precision) expressed as a percent of the overall averages were: SO2, 9.8%; CO2, 9.9%; and E.R. (emission rate as lbs SO2/106 Btu), 8.0%. The reproducibility (or between laboratory precision estimates) were: SO2, 12.9%; CO2, 13.2%; and E.R., 11.1 %. The relative accuracy of the collaborative test results was determined by comparing the results obtained by reference methods and the plant continuous monitor. This overall accuracy for SO2, CO2, and E.R. was within 3%. Further tests performed during the sam...