High-Sensitive and Nondestractive Determination of Trace Toxic Metals in Brass by Using Energy Dispersive X-ray Fluorescence Spectrometer with 3-Dimentional Polarization Optics

Abstract

A quick, easy and highly sensitive analysis of toxic metals has been required for a purpose of WEEE and RoHS directive. 3 dimensional polarization optics energy dispersive X Ray fluorescence spectrometer (3D EDX, Epsilon5, PANalytical B.V.) has been introduced as a easy and accurate with high sensitive method for bulk samples. To adapt this measurement method to shaped Brass samples, the scatter collection was used. Intensities of each element lines (Ka for Cr, Cd and Lb for Pb) have been collected by Rayleigh scatter of each secondary targets these are used for exciting interesting elements. Calibration curves were created and obtained by CRM's bulk flat Brass standard samples for Cr, Cd, and Pb. Estimated LLD (Lower Limit of Detection) was Cd 3.28 mg/g, Pb 29.0 mg/g, and Cr 6.64 mg/g with 300 seconds measurement time for each condition. Cd and Pb of some shaped and small Brass samples, they have been quantified by ICP AES, were measured and quantified by Rayleigh scatter collection. As a result of this comparison, there are quite good correlation between ICP AES and Epsilon5 with Rayleigh scatter correction. This correlation was also valid for smaller samples (e.g. 5 mg sample weight for Pb measurement). These LLD were kept while measurement was done within Maximum operating power (600 W, 100 kV, 6 mA).

Atomic spectrometry update. X-ray fluorescence spectrometry

“…Since the implementation of the new EU Directives on Restriction on Hazardous Substances (RoHS) and Waste Electrical and Electronic Equipment (WEEE) in July 2006, the development of analytical methods, including new reference materials, to control the level of these hazardous substances is making significant progress. Matsuda et al 253 set up a method for the determination of Cd, Cr and Pb in shaped brass samples using EDXRF with polarisation optics. For each element a calibration curve was set up using bulk CRMs comprising flat brass standard samples and measurements were performed with dedicated secondary targets.…”

Atomic spectrometry update. Industrial analysis: metals, chemicals and advanced materials

“…The authors claim energy dispersive (ED) XRF was comparable to the fire assay cupellation method (Au and Ag) and potentiometric titration (Ag) for a number of samples. Matsuda et al 55 used an EDXRF equipped with 3 dimensional polarization optics to determine toxic metals in brass. Lower limits of detection were estimated to be: 3.3 ppm Cd, 29 ppm Pb, and 6.6 ppm Cr.…”