电感耦合等离子体原子发射光谱法测定Ni-Cu-Li/SiO2催化剂中镍铜锂

Determination of nickel,copper and lithium in Ni-Cu-Li/SiO2 catalyst by inductively coupled plasma atomic emission spectrometry

准确测定Ni-Cu-Li/SiO2催化剂中镍、铜、锂含量,对Ni-Cu-Li/SiO2催化剂的催化性能影响因素研究意义重大。试验采用5mL盐酸-3mL硝酸-4mL氢氟酸消解体系,于160℃密闭消解样品100min后,选择Ni231.604nm、Cu327.396nm、Li670.784nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定镍、铜、锂,建立了Ni-Cu-Li/SiO2催化剂中镍、铜、锂的测定方法。各元素校准曲线的相关系数均大于0.999;镍、铜、锂的检出限分别为0.0006%、0.0002%和0.00005%,定量限分别为0.002%、0.0007%和0.0002%。按照实验方法测定两个Ni-Cu-Li/SiO2催化剂样品中镍、铜、锂,测定结果的相对标准偏差(RSD,n=6)均小于4.0%;加标回收率为90%~103%。

The accurate determination of nickel,cooper and lithium in Ni-Cu-Li/SiO2 catalyst is of great significance to investigate the influencing factors on the catalytic performance of Ni-Cu-Li/SiO2 catalyst.The sample was digested in closed system at 160℃for 100 min with 5 mL of hydrochloric acid,3 mL of nitric acid and 4 mL of hydrofluoric acid.Ni 231.604 nm,Cu 327.396 nm and Li 670.784 nm were selected as the analytical lines.The method for determination of nickel,copper and lithium in Ni-Cu-Li/SiO2 catalyst by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The correlation coefficients of calibration curves of elements were all higher than 0.999.The limit of detection of nickel,copper and lithium was 0.0006%,0.0002%and 0.00005%,respectively.The limit of quantification was 0.002%,0.0007%and 0.0002%,respectively.The contents of nickel,copper and lithium in two Ni-Cu-Li/SiO2 catalyst samples were determined according to the experimental method.The relative standard deviations(RSD,n=6)of determination results were all less than 4.0%.The recoveries were between 90%and 103%.