压力消解ICP-AES法对润滑油异构脱蜡催化剂中铂、钯含量的测试

采用高压消解技术,使用盐酸、硝酸和氢氟酸对润滑油异构脱蜡催化剂进行处理,制备测定样品水溶液,选择Pt波长214.423 nm和Pd波长340.458 nm作分析线,电感耦合等离子体原子发射光谱仪(ICP-AES)进行测定,对压力消解条件进行确定,对待测元素的分析谱线选择进行分析。结果表明,各元素校准曲线线性相关系数均不小于0.999 00,检出限Pt为0.030 12 mg·L^-1,Pd为0.015 21 mg·L^-1。按照实验方法测定润滑油异构脱蜡催化剂样品中Pt、Pd结果的相对标准偏差(RSD,n=6)均小于1%,回收率98.0%~103.0%,测试方法准确可靠。

Determination of platinum and palladium in lubricating oil isodewaxing catalyst by ICP-AES after pressure digestion

Catalyst for isomeric dewaxing of lubricating oil was treated using HCl,HNO₃ and HF by pressure digestion technique to prepare water solution sample. Pt 214.423 nm and Pd 340.458 nm were selected as the analytical lines using determination method of inductively coupled plasma atom emission spectrometry(ICP-AES).Test conditions were determined and selection of spectral lines for the measured elements was analyzed.According to results,the linear correlation coefficient of the calibration curve of each element was not less than 0.99900.The detection limits of Pt and Pd were 0.03012 mg·L^-1 and 0.01521 mg·L^-1, respectively.According to the method of this experiment,the test was conducted using a lubricating oil isodewaxing catalyst sample and the relative standard deviations(RSD,n=6)of found results were less than 1%.Recoveries were between 98.00% and 103.0%.The test method was accurate and reliable.