The Determinations of Pb, Cd, Hg, Cr6+, PBBs/PBDEs to Comply with RoHS Directive

L. Hua, Y.P. Wu, B. An, Y. Chan, B.Y. Wu, F.S. Wu
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Abstract

For RoHS compliance, a method coupled inductively coupled plasma-optical emission spectrometry (ICP-OES), gas chromatography-mass spectrometry (GC-MS), and UV-visible spectrophotometry with microwave technology was developed to determine trace Cd, Hg, Pb, Cr6+, PBBs/PBDEs in electronic and electrical products (EEP). Elements were screened by Energy dispersion X-ray fluorescence spectrometry (EDXRF). In order to achieve good performance, other methods such as colorific test, inter-element correction (IEC) and standard addition techniques etc. were performed. By this study, it showed that analyses of Hg, Cd, Pb by ICP-OES and Cr6+ by UV-visible spectrophotometry had a RSD <5%, and a RSD <1% for PBBs/PBDEs by GC-MS analyzer. UV-visible spectrophotometry offered a good alternative for Cr6+ determination with alkali digestion, the inferences from Fe3+, Pb2+ etc. were eliminated by K2HPO4 buffer. The ramifications from monoBB/BDE to DecaBB/BDE were distinctly separated and successfully determined in the optimized condition. Furthermore, microwave system did an excellent job of consistently putting solid samples into solutions and had a moderate compatibility with spectrometric analyzer due to good recoveries. Though RSD of XRF screening was larger than 10%, it proved to be an easier, cheaper, faster technique. Because of the combination of multiple methodologies, the restricted substances can be determined with good precision and high reliability. It provides a prominent project for EE industries to comply with RoHS compliance.
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符合RoHS指令的铅、镉、汞、Cr6+、多溴联苯/多溴二苯醚的测定
为符合RoHS要求,建立了电感耦合等离子体发射光谱法(ICP-OES)、气相色谱-质谱法(GC-MS)和微波紫外可见分光光度法(uv -可见分光光度法)耦合测定电子电气产品(EEP)中痕量Cd、Hg、Pb、Cr6+、PBBs/PBDEs的方法。用能量色散x射线荧光光谱法(EDXRF)筛选元素。为了获得良好的性能,还采用了显色试验、元素间校正(IEC)和标准加法等方法。结果表明,ICP-OES法和Cr6+紫外可见分光光度法测定Hg、Cd、Pb的RSD <5%, GC-MS法测定PBBs/PBDEs的RSD <1%。紫外可见分光光度法可替代碱消解法测定Cr6+, K2HPO4缓冲液可消除Fe3+、Pb2+等的影响。在优化的条件下,从monoBB/BDE到DecaBB/BDE的分支明显分离并成功测定。此外,微波系统在稳定地将固体样品放入溶液中表现出色,并且由于回收率好,与光谱分析仪具有适度的兼容性。虽然XRF筛选的RSD大于10%,但它被证明是一种更简单、更便宜、更快速的技术。由于多种方法的结合,限制物质的测定精度好,可靠性高。为电子电气行业的RoHS合规提供了一个突出的项目。
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