ICP-OES测定选择性加氢催化剂中的铂、钯含量
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摘要
选择使用微波消解仪法消解选择性加氢催化剂样品,结合电感耦合等离子体収射光谱仪(ICP-OES)测定选择性加氢催化剂中的Pt、Pd元素含量。系统考察了微波消解法消解样品条件,优化了电感耦合等离子体収射光谱仪(ICP-OES)的工作条件,采用内标校正标准工作曲线法,建立了ICP-OES法测定选择性催化剂中Pt、Pd元素含量的分析方法。结果表明,以8 mL硝酸和2 mL氢氟酸体系混合酸体系,微波消解法能够充分消解选择性加氢催化剂样品;测定选择性加氢催化剂中Pt含量:6.489～6.703 mg/L、Pd含量:14.85～15.31mg/L;相对标准偏差(RSD)分别为铂:1.216%、钯:1.217%;样品加标回收率分别为Pt:99.25%～101.26%、Pd:99.58%～102.24%。ICP-OES测定方法用于可以应用于选择性加氢催化剂中Pt、Pd元素含量的测定,分析快速,结果准确,已应用于生产分析中。
The sample of selective hydrogenation catalyst was digested by microwave digestion, and the content of Pt and Pd in the selective hydrogenation catalyst was measured by inductively coupled plasma emission spectrometry(ICP-OES). The microwave digestion conditions of the sample was investigated, and the working conditions of the inductively coupled plasma emission spectrometer(ICP-OES) were optimized. The internal standard method was used to calibrate the standard working curve, an analytical method for the determination of Pt and Pd elements in selective catalysts by ICP-OES was established. The results showed that the microwave digestion method fully digested the selective hydrogenation catalyst sample by the mixed acid system of 8 mL nitric acid and 2 mL hydrofluoric acid; The determination result of Pt content was 6.489～6.703 mg/L, that of Pd content was 14.85～15.31 mg/L; The relative standard deviation(RSDs) were 1.216% for Pt,1.217% for Pd;recoveries of samples were 99.25%～101.26% for Pt,99.58～102.24% for Pd, respectively. ICP-OES method for determination of Pt and Pd in the selective hydrogenation catalyst is rapid, easy to master, so it can be used in production analysis.
The sample of selective hydrogenation catalyst was digested by microwave digestion, and the content of Pt and Pd in the selective hydrogenation catalyst was measured by inductively coupled plasma emission spectrometry(ICP-OES). The microwave digestion conditions of the sample was investigated, and the working conditions of the inductively coupled plasma emission spectrometer(ICP-OES) were optimized. The internal standard method was used to calibrate the standard working curve, an analytical method for the determination of Pt and Pd elements in selective catalysts by ICP-OES was established. The results showed that the microwave digestion method fully digested the selective hydrogenation catalyst sample by the mixed acid system of 8 mL nitric acid and 2 mL hydrofluoric acid; The determination result of Pt content was 6.489～6.703 mg/L, that of Pd content was 14.85～15.31 mg/L; The relative standard deviation(RSDs) were 1.216% for Pt,1.217% for Pd;recoveries of samples were 99.25%～101.26% for Pt,99.58～102.24% for Pd, respectively. ICP-OES method for determination of Pt and Pd in the selective hydrogenation catalyst is rapid, easy to master, so it can be used in production analysis.
引文
[1]樊红青.HDO-18催化剂在芳烃抽提装置中的应用[J].当代化工,2009,38(3):233-236.
[2]李莉.选择性加氢催化剂在碳九加氢装置中的应用[D].上海师范大学,2017.
[3]陈玉琢,徐远国.HDO-18选择性加氢脱烯烃催化剂的反应性能及应用[J].炼油技术与工程,2005,35(11):49-54.
[4]张丼娟.催化重整生成油选择性加氢催化剂和工艺技术研究.2002年加氢技术年会论文集[C].抚顺:抚顺石油化工研究院,2002:56-64.
[5]叶小舟,顾国璋,徐柏福,等.HDO-18选择性加氢催化剂的工业应用[J].石油炼制与化工,2004,35(8):26-29.
[6]刘诗成,李巨峰,郭绪强,等.土壤中重金属检测样品前处理技术现状分析[J].油气田环境保护,2012,22(4):61-64.
[7]李秀丼,万福成.微波消解ICP-AES法测定铁中硅、锰、磷的研究[J].煤炭技术,2011,30(2):197-198.
[8]杨晓慧,霍燕燕,王转莉,等.2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究及其应用[J].冶金分析,2013,33(6):47-51.
[9]孙宝莲,周恺,李波,等.分光光度法测定铼回收溶液中的铼含量[J].光谱实验室,2012,29(6):003922-3926.
[10]郑文英,李君,房勇,等.硫氰酸钾光度法测定铜精矿冶炼污酸中铼[J].冶金分析,2015,35(9):68-72.
[11]郑文英,李君,房勇,等.硫氰酸钾光度法测定铜精矿冶炼污酸中铼[J].冶金分析,2015,35(9):68-72.
[12]沙娇,杨冬霞,徐莲,等.密闭消解-光度法测定乙醇胺羟基铂中的铂含量[J].贵金属,2016,37(1):47-50.
[13]林海山.微波消解-原子吸收法测定氧化铝为载体的钯催化剂中钯[J].分析试验室,2006,25(6):75-77.
[14]季海冰,潘荷芳,金鑫,等.塞曼效应背景校正-石墨炉原子吸收光谱法测定天然水中微量钡[J].理化检验(化学分册),2008,44(11):1091-1093.
[15]Polák J,Mestek O,Suchánek M.Uncertainty of determination of palladium in road dust sample by inductively coupled plasma mass spectrometry[J].Accreditation&Quality Assurance,2006,10(11):627-632.
[16]梁淑轩,王欣,吴虹,等.微波消解/ICP-MS测定水系沉积物中的9种重金属元素[J].光谱学与光谱分析,2012,32(3):809-812.
[17]李业军,张青,李永太.电感耦合等离子体质谱法测定土壤中重金属元素[J].当代化工,2015(4):864-867.
[18]张金龙.ICP及ICP-MS在石油及其产品金属元素分析中的应用研究[D].石河子大学,2016.
[19]单红飞,廖奕鸥,倪雪梅,等.微波消解/ICP-OES测定重整催化剂中的铂金属元素[J].沈阳师范大学学报(自然科学版),2017(4):405-408.
[2]李莉.选择性加氢催化剂在碳九加氢装置中的应用[D].上海师范大学,2017.
[3]陈玉琢,徐远国.HDO-18选择性加氢脱烯烃催化剂的反应性能及应用[J].炼油技术与工程,2005,35(11):49-54.
[4]张丼娟.催化重整生成油选择性加氢催化剂和工艺技术研究.2002年加氢技术年会论文集[C].抚顺:抚顺石油化工研究院,2002:56-64.
[5]叶小舟,顾国璋,徐柏福,等.HDO-18选择性加氢催化剂的工业应用[J].石油炼制与化工,2004,35(8):26-29.
[6]刘诗成,李巨峰,郭绪强,等.土壤中重金属检测样品前处理技术现状分析[J].油气田环境保护,2012,22(4):61-64.
[7]李秀丼,万福成.微波消解ICP-AES法测定铁中硅、锰、磷的研究[J].煤炭技术,2011,30(2):197-198.
[8]杨晓慧,霍燕燕,王转莉,等.2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺与钯显色反应的研究及其应用[J].冶金分析,2013,33(6):47-51.
[9]孙宝莲,周恺,李波,等.分光光度法测定铼回收溶液中的铼含量[J].光谱实验室,2012,29(6):003922-3926.
[10]郑文英,李君,房勇,等.硫氰酸钾光度法测定铜精矿冶炼污酸中铼[J].冶金分析,2015,35(9):68-72.
[11]郑文英,李君,房勇,等.硫氰酸钾光度法测定铜精矿冶炼污酸中铼[J].冶金分析,2015,35(9):68-72.
[12]沙娇,杨冬霞,徐莲,等.密闭消解-光度法测定乙醇胺羟基铂中的铂含量[J].贵金属,2016,37(1):47-50.
[13]林海山.微波消解-原子吸收法测定氧化铝为载体的钯催化剂中钯[J].分析试验室,2006,25(6):75-77.
[14]季海冰,潘荷芳,金鑫,等.塞曼效应背景校正-石墨炉原子吸收光谱法测定天然水中微量钡[J].理化检验(化学分册),2008,44(11):1091-1093.
[15]Polák J,Mestek O,Suchánek M.Uncertainty of determination of palladium in road dust sample by inductively coupled plasma mass spectrometry[J].Accreditation&Quality Assurance,2006,10(11):627-632.
[16]梁淑轩,王欣,吴虹,等.微波消解/ICP-MS测定水系沉积物中的9种重金属元素[J].光谱学与光谱分析,2012,32(3):809-812.
[17]李业军,张青,李永太.电感耦合等离子体质谱法测定土壤中重金属元素[J].当代化工,2015(4):864-867.
[18]张金龙.ICP及ICP-MS在石油及其产品金属元素分析中的应用研究[D].石河子大学,2016.
[19]单红飞,廖奕鸥,倪雪梅,等.微波消解/ICP-OES测定重整催化剂中的铂金属元素[J].沈阳师范大学学报(自然科学版),2017(4):405-408.