Simultaneous determination of fluorine, chlorine and sulfur in incinerator residues by oxidative high pressure digestion and ion chromatography

Abstract

Abstract. An oxidative high pressure digestion method is presented to dissolve fluorine, chlorine and sulfur components of municipal solid waste incinerator residues. It is a combination of the classical high pressure digestion technique with the combustion in a closed system. The concentration determination is carried out by ion chromatography. The results are compared with those obtained by other digestion and extraction methods combined also with ion chromatography. A CNS-analyzer is used as a further method to compare the sulfur concentrations. Based on the obtained data, the accuracy of the fluorine, chlorine and sulfur concentrations is estimated as better than 85 %. It is concluded, that the oxidative high pressure digestion combined with ion chromatography is an appropriate method to determine fluorine, chlorine and sulfur concentrations in incinerator residues. Its main advantage is the simultaneous analysis of these three elements. However, it is a time consuming method.

Experimental Design Optimization of the Determination of Total Halogens in Coal by Combustion–Ion Chromatography

“…Combustion of an organic substance is a complex and exothermic reaction that results largely in CO2 and H2O production. The ignition process occurs when the oxidation reaction is accelerated and reagents are quickly consumed and is commonly accompanied by light emission (Barnard and Bradley 1985). For closed vessels, if the rate of energy released by chemical reaction exceeds the rate at which it is lost to the vessel walls, the temperature increases, causing the reaction rate and the rate of energy release to increase rapidly (Razus et al 2006;Razus, Movileanu, and Oancea 2007).…”

“…Problems involving combustion followed by chromatographic detection were discussed and solutions were evaluated. Fluorine, Cl, and S determination in solid waste incinerator residues using oxidative high pressure digestion was carried out in a special bomb with the inner surface coated by an auto-regenerating catalysts (Belavi and Mönch 2000). For fluorine determination in coal, oxygen flask combustion with WO3/Sn as a catalyst was developed (Geng et al 2007).…”

“…For fluorine determination in coal, oxygen flask combustion with WO3/Sn as a catalyst was developed (Geng et al 2007). Determination of halogens has been performed using ion-selective electrodes (ISE) by direct detection (Dressler et al 2002;Geng et al 2007) and standard addition (Wood, Dale, and Riley 2003;Sredović and Rajaković 2010), non-suppressed ion chromatography (IC) Dao 1995, 1996), IC with conductivity detection (Belavi and Mönch 2000;Cortes-Pena et al 2002;Flores et al 2008), and inductively coupled plasma mass spectrometry (ICP-MS) (Gao et al 2007;Sun et al 2010).…”

“…Although the combustion bomb may be considered as an old technique, it is still in use and recent applications (after 2000) have been described in the literature showing its suitability, especially as pretreatment for halogen and sulfur determination (Belavi and Mönch 2000;CortesPena et al 2002;Souza et al 2002). Organic halogen group parameters, such total organic halogens, absorbable organic halogens, volatile organic halogens, and extractable organic halogens, are well known and used for monitoring drinking water (Kristiana et al 2009), surface water (Putschew, Mania, and Jekel 2003), wastewater (Vinder and Simonič 2012), soil (Pereira et al 2011), and sediments (Niemirycz, Kaczwarzyk, and Blazejowski 2005).…”

sulphur and chlorine contents of grass and maize silage

“…The sulphur and chlorine contents of a sample can be determined by various analytical techniques. These include neutron activation analysis (NAA; Kump et al, 1996), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma emission-mass spectrometry (ICP-MS; Pöykiö et al, 2000), energy dispersive X-ray fluorescence spectrometry (EDXRF; Kump et al, 1996), wavelength dispersive X-ray fluorescence spectrometry (WDXRFS; Ruiz et al, 1991), ion chromatography (IC; Belevi and Monch, 2000), and coulometric titration by Volhard (Atkin and Somerfield, 1994). In our work EDXRF (to be referred as XRF), ICP-AES and the titrimetric technique for chlorine determination were selected according to the facilities available.…”