Direct determination of nickel in xylene solutions of raw material for catalytic cracking with application of graphite furnace atomic absorption spectrometry

Zofia Kowalewska


Nickel is a severe poison to cracking catalysts, therefore its content in raw material for cracking (which is a mixture of heavier oils boiling in the range 330–550 °C) has to be controlled at levels below mg kg-1. A reliable, simple and fast method of Ni determination in this kind of material is proposed with a detection limit of 1.2 mg kg-1 in the initial sample at 1 : 5 dilution m/v. The method relies just on sample dilution in xylene and Ni determination using graphite furnace atomic absorption spectrometry, with palladium acetylacetonate and air ashing as a double modifier. The method was successfully validated using mineralization as an alternative sample preparation procedure. The following commonly used methods failed as tools for verification of analysis accuracy: Ni in the investigated cracking feed behaved completely differently than in the available certified reference materials; recovery of standard added to samples was close to 100%, while results were up to 10 times too low; pyrolysis curves did not reveal a decrease of integrated absorbance appearing in the entire investigated temperature range. Decreased evaporation of Ni porphyrins due to interaction with graphite, and increased Ni binding in the solid phase in the presence of asphaltenic matrix, should be taken into account in interpretation of technologically important information on speciation of Ni (volatile and non-volatile Ni forms).
Author Zofia Kowalewska (FCEMP / ICEn)
Zofia Kowalewska,,
- Insitute of Civil Engineering
Journal seriesAnalytical Methods, ISSN 1759-9660
Issue year2013
Publication size in sheets0.5
Keywords in EnglishNickel determination, Atomic absorption spektrometry, Graphite furnace, Catalytic cracking, Xylene
ASJC Classification2200 General Engineering; 1500 General Chemical Engineering; 1602 Analytical Chemistry
Languageen angielski
Not used for evaluationyes
Score (nominal)0
Publication indicators Scopus Citations = 1; WoS Citations = 1; Scopus SNIP (Source Normalised Impact per Paper): 2013 = 0.691; WoS Impact Factor: 2013 = 1.938 (2) - 2013=1.913 (5)
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