Microwave-assisted ultraviolet digestion of petroleum coke for the simultaneous determination of nickel, vanadium and sulfur by ICP-OES
作者： Jussiane SS Oliveira , Rochele S Picoloto , Cezar A Bizzi , Paola A Mello , Juliano S Barin
DOI: 10.1016/J.TALANTA.2015.07.060
关键词: Digestion (alchemy) 、 Certified reference materials 、 Inductively coupled plasma atomic emission spectroscopy 、 Chemistry 、 Nitric acid 、 Inductively coupled plasma 、 Ultraviolet 、 Analytical chemistry 、 Detection limit 、 Petroleum coke
摘要: A method for the simultaneous determination of Ni, V and S in petroleum coke by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted ultraviolet digestion (MW-UV) closed vessels was proposed. Digestion performed using electrodeless discharge lamps positioned inside quartz turned on microwave radiation. The following parameters were evaluated: HNO3 concentration (15 mL 1, 4, 7, 10 or 14.4 mol L(-1)), volume H2O2 (30%, 1 3 mL), sample mass (100, 250 500 mg) heating time (40 60 min) with without use UV lamps. efficiency evaluated residual carbon content (RCC) digests. Using lower RCC obtained combination 4 L(-1) min allowed a suitable up to mg (RCC< 21%). agreement reference values (obtained microwave-induced combustion) certified material between 96 101%. proposed considered as advantageous when compared American Society Testing Materials because it limit detection (0.22, 0.12 8.7 µg g(-1) S, respectively) avoiding concentrated nitric acid providing digests routine analysis ICP-OES.
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