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建立了以镓为内标,经甲苯稀释后直接测定润滑油中Ca,Ti,V,Cr,Mn,Fe,Ni,Cu,Zn,Pb等10种微量金属元素的全反射X射线荧光(TXRF)光谱法检测方法。方法检出限从Pb的0.18 mg/kg到Ca的1.6 mg/kg,相对标准偏差均小于8%,回收率为90%~120%。通过TXRF法与电感耦合等离子体发射光谱法分别对润滑油标准样品和实际样品的测定,发现两种方法所得结果在95%的置信区间内无显著性差异。方法可用于直接测定润滑油中的微量金属元素。
The gallium was used as the internal standard to directly determine the total reflection X-ray fluorescence (TXRF) of 10 trace metal elements such as Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Spectrometric detection method. The detection limits of this method ranged from 0.18 mg / kg Pb to 1.6 mg / kg Ca, with relative standard deviations less than 8% and recoveries between 90% and 120%. By the TXRF method and inductively coupled plasma emission spectrometry, respectively, the determination of the standard and actual samples of lubricating oil found no significant difference between the two methods in the 95% confidence interval. The method can be used for direct determination of trace metal elements in lubricating oils.