High-resolution gas chromatography and high-resolution gas chromatography/mass spectrometry study of the volatile fraction obtained from high-inertinite Brazilian coal by supercritical fluid extraction

Autor: Livia Mari Assis, Fernando Mauro Lanças
Rok vydání: 1999
Předmět:
Zdroj: Journal of Microcolumn Separations. 11:501-512
ISSN: 1520-667X
1040-7685
DOI: 10.1002/(sici)1520-667x(1999)11:7<501::aid-mcs2>3.0.co;2-v
Popis: This work presents the results of a study involving a high-inertinite coal from Amando Simoes Mine, located in Parana state (Brazil). The organic matter was extracted in a supercritical fluid (static mode) apparatus using toluene as the extraction fluid in the presence of hydrogen. The variables were studied using a 23 factorial design (two levels for three variables: temperature, reaction time, and pressure) with three center points. The liquid coal extracts obtained were fractionated by preparative liquid chromatography into eight fractions (PLC-8) by using an adequate series of eluents. Each eluted fraction was collected and quantified by gravimetry. The relative fraction yields were used to calculate the influence of the variables and their interaction in the factorial design. All hydrocarbon-rich fractions were analyzed by high-resolution gas chromatography (HRGC)-fluid ionization detection and HRGC-mass selective detection (MSD). The characterization of chemical classes of interest in the collected fractions was carried out using HRGC-MSD in the extracted ion mode. This approach allowed fine monitoring of compounds of interest by their characteristic m/z values and was a fast and very selective setup for detection of specific compounds in a very complex matrix. ©1999 John Wiley & Sons, Inc. J Micro Sep 11: 501–512, 1999
Databáze: OpenAIRE