Simultaneous determination of bromine and chlorine in coal using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis

• Published in: Analytica chimica acta 2014-12, Vol.852, p.82-87
• Main Authors: de Gois, Jefferson S., Pereira, Éderson R., Welz, Bernhard, Borges, Daniel L.G.
• Format: Article
• Language: English
• Subjects: Bromine - analysis; Calibration; Chlorine; Chlorine - analysis; Coal; Coal - analysis; Direct solid sample analysis; Electrothermal vaporization; Halogen determination; Inductively coupled plasma; Limit of Detection; Mass spectrometry; Mass Spectrometry - methods; Palladium; Temperature; Vaporization; Volatilization
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2014.09.019

[Display omitted] •Direct analysis of coal samples is proposed for the first time for halogens determination using ICP-MS.•Simultaneous determination of Br and Cl can be carried out.•Sample treatment protocols are avoided, adding simplicity to the analytical procedure. A new method for the direct analysis of coal using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis was developed, aiming at the determination of Br and Cl. The procedure does not require any significant sample pretreatment and allows simultaneous determination of both elements to be carried out, requiring small mass aliquots of sample (about 0.5mg). All operating parameters, including carrier gas flow-rate and RF power, were optimized for maximum sensitivity. The use of modifiers/aerosol carriers (Pd, Pd+Al and Pd+Ca) was evaluated, and the mixture of Pd and Ca was chosen, allowing pyrolysis and vaporization temperatures of 700°C and 1900°C, respectively. Chlorine was accurately determined using calibration against solid standards, whereas Br could also be determined using calibration against aqueous standard solutions. The limits of quantification were 0.03μgg−1 for Br and 7μgg−1 for Cl, and no spectral interferences were observed.