Method development and validation for sulfur determination via CS molecule in petroleum green coke by high resolution continuum source molecular absorption spectrometry

作者: Adriana Simane Camera , Patrícia Passos Arcênio , Waldemar de Oliveira Pacheco Filho , Tatiane de Andrade Maranhão , Fernando Jorge Santos de Oliveira

DOI: 10.1016/J.MICROC.2017.06.022

关键词:

摘要: Abstract Development and validation of a method for determination sulfur via CS molecule in petroleum green coke samples by high resolution continuum source molecular absorption spectrometry (HR-CS MAS) is the aim this work. The protocol adopted followed criteria based on international guidelines. Optimizations analyte were carried out at wavelength 258.0330 nm, same spectral interval analytical line Tl. Slurry prepared using Triton X-100 (0.05% v/v) without use HNO 3 , proposed as simple fast sample treatment. Chemical modifier KOH (1.0% m/v) was important to promote formation stabilization molecule. Pyrolysis Vaporization temperatures optimized different compounds, ammonium sulfate, l -cysteine monohydrochloride thiourea aqueous solutions, also certified reference material, NIST 2718, coke. Compromise temperature conditions 1000 °C 2600 °C, pyrolysis vaporization, respectively. Aqueous calibration with presented best condition chosen analyte. obtained concentrations between 6.20 mg g − 1 9.40 mg g . following parameters evaluated protocol: accuracy, precision, linearity, limits detection quantification, sensitivity, selectivity, robustness, working range measurement uncertainty. Weighted least square (WLS) employed estimate LOD LOQ, since it leads lower final evaluation parameters, especially uncertainty, confirmed satisfactory performance method.

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