作者：严方1, 谢永杰2
作者单位：1. 中国石油大学化学化工学院, 山东 青岛 266555;
2. 山东石大科技集团有限责任公司, 山东 东营 257061
关键词：化学分析; X射线荧光光谱法; 催化剂; 镍; 钒; 锑
摘要：
针对催化剂中的重金属污染问题,采用X射线荧光光谱法测定催化裂化催化剂中重金属Ni、V、Sb的含量,分析了影响Ni、V、Sb元素测定的各种因素,以未使用过的催化剂为载体配制标准样品,使标准样品与样品的基体基本一致,减少了基体效应的影响。待测元素的线性范围分别:Ni为0.10%~1.20%,V为0.05%~0.30%,Sb为0.02%~0.20%,相关系数均为0.999 9,测定结果的相对标准偏差小于2%。该方法的测定结果与原子吸收法的测定结果相吻合。
Determination of Ni、V、Sb on FCC catalysts
YAN Fang1, XIE Yong-jie2
1. College of Chemistry and Chemical Engineering, China University of Petroleum, Qingdao 266555, China;
2. Shandong Shtar Science & Technology Co., Ltd, Dongying 257061, China
Abstract: In catalysts, heavy metal pollution is a serious problem. The XRF method was introduced in this paper for determining Ni, V, Sb in FCC catalysts. By the establishment of analytical method, the cause and effect of content determination has been discussed. The matrix effect can be overcome by using calibration standards with fresh catalyst as matrix. Linearity window is 0.10%~1.20% for Ni, 0.05%~0.30% for V, 0.02%~0.20% for Sb, the correlative coefficients are larger than 0.999 9 for three metals, and measurement RSDs are less than 2%. Results show that the method is fast, accurate and convenient. The results are generally consistent with those from AAS.
Keywords: Chemical analysis; X-ray fluorescence spectrometry; Catalyst; Ni; V; Sb
2010, 36(1): 46-48 收稿日期: 2009-4-7;收到修改稿日期: 2009-6-15
基金项目:
作者简介: 严方(1970-),女,实验师,主要从事仪器分析工作。
参考文献
[1] 林世雄.石油炼制工程[M].北京:石油工业出版社,2000.
[2] 李豫晨,陆善祥.FCC催化剂失活与再生[J].工业催化,2006,14(11):26-30.
[3] 增田立男,黄木林.重金属对沸石系FCC催化剂的影响[J].石油炼制译丛,1991(8):1-3.
[4] 严 方,高文苗,罗文平,等.原子吸收法测定催化剂中的镧含量[J].中国测试,2009,35(1):81-83.
[5] 高风林.石油化工分析方法汇编[M].北京:石油工业出版社,1998.
[6] 吉 昂.X射线荧光光谱分析[M].北京:科学出版社,2005.
[7] 刘立明.微波消解-ICP-AES测定催化剂中铁、镍、铜、钒、钠、锑、钙的研究[J].安徽化工,2008,34(2):66-68.
[8] 李秀荣,叶江湖.ICP-AES方法测定加氢催化剂中的元素[J].分析测试通报,1988,7(2):37.
[9] 马志军,白吉云.催化裂化催化剂中微量金属元素的测定[J].分析测试技术与仪器,2007,10(1):42-45.
