Ion chromatographic determination of total bromine in electronic devices in conjunction with a catalytic reduction debromination pretreatment
Ion chromatographic determination of total bromine in electronic devices in conjunction with a catalytic reduction debromination pretreatment
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催化还原脱溴预处理电子设备中总溴的离子色谱测定
DOI：
10.1016/j.aca.2019.07.042
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发表时间：
2019-11-15
影响因子：
6.2
通讯作者：
Tang, Heqing
中科院分区：
文献类型：
--
作者：
Dai, Pei;Hou, Dajiao;Tang, Heqing
建立了超声辅助萃取-铜催化还原脱溴-离子色谱法测定电子器件中总溴的新方法。结果表明，添加的溴系阻燃剂（多溴联苯醚、多溴联苯、四溴双酚A和六溴环十二烷）在铜基催化剂和还原剂N_2H_4中心点H_2O的作用下均能完全脱溴。溴化阻燃剂完全脱溴后，溴以溴离子形式释放出来，可用离子色谱法测定。以标准物质GBW（E）082725中的最大离子色谱信号为指标，优化了萃取条件，建立了测定固体样品中总溴的UAE-RD-IC方法。经对标准物质分析，溴含量为695.3 ± 16.0 mg kg（-1），与标准值（694.54 ± 30.63 mg kg（-1））一致。5次平行测定的相对标准偏差（RSD）为1.7%，表明该方法具有良好的重复性。将该方法应用于电缆和鼠标外壳样品的分析。对于所有这些实际样品，由UAE-RD-IC方法得到的溴含量与标准氧弹燃烧-IC方法得到的结果一致。新方法的检出限约为20 mg kg（-1），远低于传统氧弹燃烧-离子色谱法的检出限（75 mg kg（-1））。该方法具有良好的准确度、精密度和灵敏度，可用于实际电子器件中总溴含量的测定。(C)2019 Elsevier B. V.版权所有。
A new determination method for total bromine in electronic devices was developed by using ultrasound assisted extraction, copper-catalyzed reductive debromination and ion chromatography (UAE-RD-IC). It was found that all the added brominated flame retardants (polybrominateddiphenyl ethers, polybrominated biphenyls, tetrabromobisphenol A, and hexabromocyclododecane) could be completely debrominated by using copper-based catalysts and reducing agent N2H4 center dot H2O. The complete debromination of brominated flame retardants released all of their bromine in the form of bromide ions, which could be determined by ion chromatography. After the extraction parameters were optimized by achieving the maximum IC signal in the certified reference material GBW(E) 082725, the UAE-RD-IC method was established for the determination of total bromine in solid samples. By analyzing the certified reference material, the Br content was obtained as 695.3 +/- 16.0 mg kg(-1), being well consistent with its standard value (694.54 +/- 30.63 mg kg(-1)). The relative standard deviation (RSD) of five parallel determinations was 1.7%, indicating the good repeatability of the developed method. The proposed method was further applied to analyze the samples of cables and computer mouse shells. For all these practical samples, the Br contents obtained by the UAE-RD-IC method were in good agreement with that obtained by the standard oxygen bomb combustion-IC method. It was noted that the new method has a detection limit of Br of about 20 mg kg(-1), being much lower than that (75 mg kg(-1)) of the traditional oxygen bomb combustion-IC method for total bromine detection. Therefore, the proposed method was qualified as a practical method to measure total bromine content in actual electronic devices with good analytical performances of accuracy, precision and sensitivity. (C) 2019 Elsevier B.V. All rights reserved.