Issue 8, 2018

Sample preparation strategies for petroleum coke digestion and further cerium and lanthanum determination by DSN-ICP-OES

Abstract

The determination of cerium and lanthanum in petroleum coke samples by inductively coupled plasma optical emission spectrometry coupled to a desolvating nebulizer system (DSN-ICP-OES) is proposed for the first time after studying the following sample preparation methods: microwave-assisted digestion (MW-AD) in medium and high pressure systems and microwave-induced combustion (MIC). MW-AD in a medium pressure system was not suitable for digestion of petroleum coke even when using a low sample mass (up to 100 mg). Both MIC and MW-AD in a high pressure system were considered suitable for petroleum coke digestion, but MIC was preferable in view of the possibility of using diluted acid (2.5 mol L−1 HNO3) to digest 400 mg of sample and obtaining lower residual carbon content (RCC) values (below 0.1% instead of approximately 25% for MW-AD). The use of MW-AD required a dilution step (with a factor of four) to minimize the interference in analyte determination by DSN-ICP-OES. Accuracy was evaluated by comparing the results with those obtained by neutron activation analysis (an agreement of more than 94% was obtained) and also analyzing spiked samples (recoveries in the range of 88 to 102% were achieved).

Graphical abstract: Sample preparation strategies for petroleum coke digestion and further cerium and lanthanum determination by DSN-ICP-OES

Article information

Article type
Technical Note
Submitted
07 Jun 2018
Accepted
29 Jun 2018
First published
19 Jul 2018

J. Anal. At. Spectrom., 2018,33, 1284-1291

Sample preparation strategies for petroleum coke digestion and further cerium and lanthanum determination by DSN-ICP-OES

J. P. Souza, K. Kellermann, M. S. Camargo, D. P. Moraes, D. Pozebon and J. S. F. Pereira, J. Anal. At. Spectrom., 2018, 33, 1284 DOI: 10.1039/C8JA00192H

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