Direct atomic absorption spectrometry determination of tin,lead,cadmium and zinc in high-purity graphite with flame furnace atomizer

摘要

This work described methodology of Sn,Pb,Cd and Zn impurities determination in high-purity graphite at direct atomic absorption spectrometry (AAS) with flame furnace (FF) atomizer.It was evidence that quality of AAS measurements are depended from sample amount,its homogeneity,particle size,as well as calibration procedure and operation parameters of FF atomizer.Prior to analysis the method has been developed and optimized with respect to the furnace heating temperature and flame composition of FF atomizer.Conditions of absorption peak areas (Q_A) formation to each element were studied on the basis of contribution into its value some of individual parameters of analytes,including mass-transporting process from increasing mass of graphite samples into gas phase.Because particle size and homogeneous distribution of analyte in powdered materials has an enormous influence on accuracy and precision of measurement results,graphite as well as appropriate series of powdered reference standards was previously ground and investigated.Graphite samples to be analyzed and standard reference materials with mass from 0.025 to 0.200 g was previously briquetted as pellet and insert on corresponding hole in furnace.The characteristic mass (g0) of Sn,Pb,Cd and Zn were 0.35,0.1,0.008 and 0.025 ng,respectively,and relative standard deviation (S_r) not more than 20%.