Solà Vázquez Auristela, Martín Antonio, Costa-Fernandez José M, Ruiz Encinar Jorge, Bordel Nerea, Pereiro Rosario, Sanz-Medel Alfredo
Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Clavería 8, 33006 Oviedo, Spain.
Anal Bioanal Chem. 2007 Oct;389(3):683-90. doi: 10.1007/s00216-007-1372-2. Epub 2007 Jun 13.
There is an increasing concern regarding the toxicity and environmental distribution and impact of brominated organic compounds employed as flame retardants. Thus, present interest in searching for new analytical techniques and methods allowing a rapid, simple and reliable detection of those compounds in materials and wastes potentially containing such flame retardants is not surprising. The feasibility of using radiofrequency glow discharge plasma spectrometry coupled with optical emission spectrometry (rf-GD-OES) as a rapid and simple tool to directly analyse bromine-containing flame-retardant polymeric layers is investigated here. Polymeric layers for calibration were made by mixing appropriate amounts of tetrabromobisphenol A, bisphenol A, phloroglucinol and diphenylmethane-4,4'-diisocyanate in tetrahydrofuran. The corresponding blanks (polymers without tetrabromobisphenol A) were also prepared. Detection of bromine was investigated both in the visible (at 470.48 nm) and in the near-infrared (at 827.24 nm) regions, using a charge-coupled device for detection. Discharge parameters affecting the emission intensity of bromine were first optimized (in argon and helium as possible plasma gases) and the analytical performance characteristics were then evaluated. The best detection limit (0.044% Br) was achieved measuring Br I 827.24 nm in a He discharge, using a forward power of 70 W and a pressure of 45 Torr. The linearity range extended up to 27% Br. Finally, the applicability of the rf-GD-OES method proposed to the quantitative analysis of bromine in solid materials coated with flame-retardant commercial paints was successfully demonstrated.
作为阻燃剂使用的溴化有机化合物的毒性、环境分布及影响日益受到关注。因此,当下对寻找新的分析技术和方法以快速、简便且可靠地检测材料及可能含有此类阻燃剂的废物中的这些化合物感兴趣也就不足为奇了。本文研究了将射频辉光放电等离子体光谱法与光发射光谱法(rf-GD-OES)联用作为一种快速简便的工具直接分析含溴阻燃聚合物层的可行性。通过在四氢呋喃中混合适量的四溴双酚A、双酚A、间苯三酚和二苯基甲烷-4,4'-二异氰酸酯来制备用于校准的聚合物层。还制备了相应的空白样(不含四溴双酚A的聚合物)。使用电荷耦合器件进行检测,研究了在可见光区(470.48 nm)和近红外区(827.24 nm)对溴的检测情况。首先优化影响溴发射强度的放电参数(以氩气和氦气作为可能的等离子体气体),然后评估分析性能特征。在氦气放电中,使用70 W的正向功率和45 Torr的压力,测量Br I 827.24 nm时获得了最佳检测限(0.044% Br)。线性范围扩展至27% Br。最后,成功证明了所提出的rf-GD-OES方法在定量分析涂有商用阻燃涂料的固体材料中溴含量方面的适用性。