摘要
加氢裂化尾油是蒸汽裂解乙烯装置的主要原料之一,其中的某些痕量有害元素如Na,Ni,V,Pb,As,Hg的含量对裂解炉的安全稳定运行至关重要。筛选了合适的有机溶剂,最大程度溶解加氢裂化尾油实际试样,采用直接有机进样-电感耦合等离子体串联质谱(ICP-MS/MS)技术,在简化试样预处理流程的基础上,提高方法的重复性和准确性,开发了满足需求的加氢裂化尾油中痕量有害元素Na,Ni,V,Pb,As,Hg的定量分析方法。测试结果表明,该方法测定实际试样中Na,Ni,V,Pb,As,Hg的最低检测限分别为21.0,13.0,0.3,0.1,0.3,0.2μg/kg;当各元素含量低于10μg/kg,相对偏差控制在20%以内,含量高于10μg/kg,相对偏差控制在10%以内,对于痕量元素的测定重复性好;六种元素的试样加标回收率在84.6%~117.9%之间,测试方法准确可靠。
Hydrocracking tail oil is one of the main feedstocks in steam cracking ethylene plant.The quality of hydrocracking tail oil,especially trace amounts of Na,Ni,V,Pb,As and Hg,plays an important role in the safe and stable operation of the cracking furnace.Suitable organic solvent which can dissolve actual hydrocracking tail oil samples in a best dilution level was investigated.Direct organic sampling-inductively coupled plasma series mass spectrometry(ICP-MS/MS)technology was developed to analyze trace amounts of harmful elements,such as Na,Ni,V,Pb,As and Hg in hydrocracking tail oil on the basis of a simple pretreatment process and keeping improvement of accuracy and repeatability of the method.The results show that the method detection limit of Na,Ni,V,Pb,As and Hg are 21.0,13.0,0.3,0.1,0.3,0.2μg/kg,respectively.When the content of each element is lower or higher than 10μg/kg,the relative deviation can be controlled within 20%and 10%,respectively,which presents quite good repeatability for the determination of trace amount of such elements.The recovery of the mentioned six elements ranges from 84.6%to 117.9%,which also indicate that the method established herein is quite accurate and reliable.
作者
王小雨
姜丽燕
李继文
王川
Wang Xiaoyu;Jiang Liyan;Li Jiwen;Wang Chuan(Sinopec Shanghai Research Institute of Petrochemical Technology,Shanghai 201208,China)
出处
《石油化工》
CAS
CSCD
北大核心
2021年第10期1075-1080,共6页
Petrochemical Technology
关键词
加氢裂化尾油
电感耦合等离子体串联质谱
痕量元素
hydrocracking tail oil
inductively coupled plasma series mass spectrometry
trace elements
