Development of a vaporization system for direct determination of chlorine in petroleum coke by ICP-MS

作者：Antes Fabiane Goldschmidt; Dullius Eduardo; Ben da Costa Adilson; Molz Rolf Fredi; Gottfried Paniz Jose Neri; Moraes Flores Erico Marlon; Dressler Valderi L^*

来源：Microchemical Journal, 2013, 109: 117-121.

DOI：10.1016/j.microc.2012.03.027

• Electrothermal vaporization
• ICP-MS
• Chlorine
• Petroleum coke

An electrothermal vaporization system (ETV) was developed for direct chlorine (Cl) determination in petroleum coke by inductively coupled plasma mass spectrometry (ICP-MS). The ETV system consists of a high power lamp enclosed in glass chamber equipped with solenoid valves. The system is controlled by a printed circuit board and software developed in LabVIEW environment. The temperature and heating time were optimized. Solenoid valves were used to control the flow of Ar (carrier gas) during pyrolysis and vaporization steps. Pyrolysis and vaporization temperatures were set at 350 degrees C and 900 degrees C, respectively; while the Ar flow rate was 1.201 min(-1) and the plasma power 1300 W. Up to 5 mg of petroleum coke sample can be analyzed. Calibration was carried out by standard addition whereas a certified reference material of coal (SARM 19) was used for that purpose. The relative standard deviation was lower than 9% (n = 4) and the limit of quantification (10s) of Cl was 3.5 mu g g(-1). Results obtained for chlorine in petroleum coke sample were in agreement with those obtained using other validated methods for Cl determination. The time of analysis (approximately 2 min per sample), risk of contamination, analyte losses and waste generation are drastically reduced in comparison with techniques that require sample digestion for chlorine determination.

• 出版日期2013-7