快速谱线自动拟合技术(FACT)-电感耦合等离子体原子发射光谱法测定烷基铝催化剂中铁铜镍钒  

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)

作　　者：张岩 王磊[1] 陈斯佳 ZHANG Yan;WANG Lei;CHEN Sijia(PetroChina Petrochemical Research Institute,Daqing Chemical Engineering Research Center,Daqing 163714,China)

机构地区：[1]中国石油石油化工研究院大庆化工研究中心,黑龙江大庆163714

出　　处：《冶金分析》2023年第11期70-74,共5页Metallurgical Analysis

摘　　要：烷基铝是乙烯齐聚合成α-烯烃的主要助催化剂,通过它对主催化剂中金属进行还原,将催化剂中的金属还原成低价态,乙烯对中心金属的络合才能发生反应。烷基铝催化剂的含量是促使乙烯齐聚合成α-烯烃的反应顺利进行的先决条件,因此准确测定烷基铝催化剂中Fe、Cu、Ni、V杂质含量至关重要。采用环己烷、乙醇稀释,稀硫酸萃取烷基铝催化剂,采用快速谱线自动拟合技术(FACT)消除Al对Fe的光谱干扰,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定烷基铝催化剂中Fe、Cu、Ni、V含量。方法中Fe、Cu、Ni、V的校准曲线线性相关系数均大于0.999;检出限分别为0.000 96、0.002 41、0.001 65、0.002 01μg/mL。按照实验方法测定烷基铝催化剂中Fe、Cu、Ni、V,结果的相对标准偏差(RSD,n=6)小于3%;回收率为98%~103%。Alkyl aluminum is the main cocatalyst for the synthesis ofα-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 ofα-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 0.00096μg/mL,0.00241μg/mL,0.00165μg/mL,and 0.00201μg/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%.

关 键 词：烷基铝催化剂 电感耦合等离子体原子发射光谱法(ICP-AES) 快速谱线自动拟合技术(FACT) 光谱干扰 萃取 铁 铜 镍 钒 

分 类 号：O657.31[理学—分析化学]