Determination of iron,copper,nickel and vanadium in alkyl aluminum catalysts by inductively coupled plasma atomic emission spectrometry with fast automated curve-fitting technique (FACT)
ZHANG Yan, WANG Lei, CHEN Sijia
PetroChina Petrochemical Research Institute,Daqing Chemical Engineering Research Center,Daqing 163714,China
Abstract：Alkyl aluminum is the main cocatalyst for the synthesis of α-olefin via ethylene oligomerization. In presence of alkyl aluminum, the metal in the main catalyst is reduced to a low valency state, and the complex reaction between ethylene and the central metal can occur. The content of alkyl aluminum catalyst is a prerequisite for the synthesis of α-olefin via ethylene oligomerization, so the accurate determination of impurity contents such as iron, copper, nickel and vanadium in alkyl aluminum catalyst is very important. In this study, the alkyl aluminum catalyst was treated by dilution with cyclohexane and ethanol followed by extraction with dilute sulfuric acid. The spectral interference of Al with Fe was eliminated by fast automated curve-fitting technique (FACT). The contents of Fe, Cu, Ni and V in the alkyl aluminum catalyst were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficients of calibration curves for Fe, Cu, Ni and V in this method were all higher than 0.999. The limits of detection were 0.000 96 μg/mL, 0.002 41 μg/mL, 0.001 65 μg/mL, and 0.002 01 μg/mL, respectively. The contents of Fe, Cu, Ni and V in the alkyl aluminum catalyst were determined according to the experimental method, and the relative standard deviations (RSD,n=6) of the measured results were less than 3%. The recoveries were between 98% and 103%.
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