Thermogravimetric desorption and de novo tests I: Method development and validation

Tsytsik, Palina; Czech, Jan; Carleer, Robert; Reggers, Guy; Buekens, Alfons

doi:10.1016/j.chemosphere.2008.04.085

Cited by 10 publications

(4 citation statements)

References 30 publications

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“…Former DTE experiments for 4, 8, 16, and 32 min at 300 C on an iron ore sintering sample (filter dust) showed that PCBz already attain full desorption after 8 min (Tsytsik et al, 2008b). Here, the DTE test time again was set at 4, 8, 16, and 32 min; total output increased from 85 mg/g after 4 min to 210, 220, and 240 mg/g after 8, 16, and 32 min, respectively (Tables 7-9).…”

Section: Effects Of Timementioning

confidence: 98%

“…Quality control procedures, including sorbent blanks and TGA blanks, as well as the optimization and validation of TD-GC/MS for semiquantifying analytes of interest were discussed elsewhere (Tsytsik et al, 2007(Tsytsik et al, , 2008a(Tsytsik et al, , 2008b.…”

Section: Indirect Thermal Extractionmentioning

confidence: 99%

“…The sample is rapidly heated to the temperature desired and thermally desorbed for the programmed time period in a continuous flow of helium carrier gas (70 mL/min); the resulting effluent is cryofocused at À 8 C on graphitized carbon (cold trap) before subsequent GC/MS analysis. Operating conditions and validation of the TE technique have been described elsewhere (Tsytsik et al, 2008a(Tsytsik et al, , 2008b.…”

Section: Direct Thermal Extractionmentioning

confidence: 99%

“…They do not pretend to explain the formation of TE products in detail, rather only to observe such formation under various experimental conditions. Laboratory scale de novo tests were earlier developed for evaluating dioxin formation from filter dust samples by monitoring carbon oxidation and the accompanying dioxin formation (Tsytsik et al, 2008a(Tsytsik et al, , 2008b.…”

Section: Introductionmentioning

confidence: 99%

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Thermal Extraction of Dioxin Surrogates and Precursors from Filter Dust: Effects of Temperature, Time, and Matrix

Tsytsik

Czech

Carleer

et al. 2010

Environmental Engineering Science

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This study identified potential precursors and surrogates of dioxins during thermal extraction (TE) of a sooty filter dust in a wide range of operating conditions, mainly temperature (120 C-540 C) and time, during direct thermal extraction (DTE) in a dedicated commercial analyzer and indirect thermal extraction (ITE) in a thermobalance used as desorber. Using identical analytical techniques, DTE products were monitored in the range of 120 C-320 C, and ITE products were monitored in the range of 300 C-540 C. Emphasis was on polychlorinated dibenzo-p-dioxins/furans potential precursors and surrogates: aromatic hydrocarbons as well as O, Cl, N, and S compounds. Aliphatic compounds were not monitored. Product distributions differ markedly between both TE techniques: matrix effects eliminate heteroatoms O, Cl, and N, rendering especially DTE less suitable for characterizing a complex sample. Effects of temperature and time were specific for each compound and tentatively explained by low-temperature desorption (up to 240 C) and progressive evolution of volatiles and their eventual decomposition on the matrix at higher temperature. The particular filter dust sample was selected due to its amount of volatiles and fixed carbon; it derived from a baghouse filter, cleaning off-gas from a clean aluminum scrap-melting furnace. TE results strongly diverged from those obtained by solvent-extractionbased analysis. Hence, TE cannot be recommended for analyzing complex samples. A second article compared de novo formation from samples precleaned by TE with raw samples. Such tests may differentiate between dioxin formation and carbonaceous matter (de novo route) from the precursor route involving sorbed organics. Results suggest that there is little or no resemblance between TE and de novo products. The novelty of these articles resides in monitoring numerous dioxin structurally related compounds during (1) TE under reducing conditions and (2) de novo tests in an airflow. The scope of these tests is exploratory and the results suggested strong influence of the matrix on the products evolved.

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Section: Effects Of Timementioning

confidence: 98%

Section: Indirect Thermal Extractionmentioning

confidence: 99%

Section: Direct Thermal Extractionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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