Harper Martin, Pacolay Bruce, Hintz Patrick, Bartley David L, Slaven James E, Andrew Michael E
Exposure Assessment Branch, Health Effects Laboratory Division, National Institute for Occupational Safety and Health, 1095 Willowdale Rd., MS-3030, Morgantown, WV 26505, USA.
J Environ Monit. 2007 Nov;9(11):1263-70. doi: 10.1039/b710591f. Epub 2007 Aug 21.
This paper concludes a five-year program on research into the use of a portable X-ray fluorescence (XRF) analyzer for analyzing lead in air sampling filters from different industrial environments, including mining, manufacturing and recycling. The results from four of these environments have already been reported. The results from two additional metal processes are presented here. At both of these sites, lead was a minor component of the total airborne metals and interferences from other elements were minimal. Nevertheless, only results from the three sites where lead was the most abundant metal were used in the overall calculation of method accuracy. The XRF analyzer was used to interrogate the filters, which were then subjected to acid digestion and analysis by inductively-coupled plasma optical-emission spectroscopy (ICP-OES). The filter samples were collected using different filter-holders or "samplers" where the size (diameter), depth and homogeneity of aerosol deposit varied from sampler to sampler. The aerosol collection efficiencies of the samplers were expected to differ, especially for larger particles. The distribution of particles once having entered the sampler was also expected to differ between samplers. Samplers were paired to allow the between-sampler variability to be addressed, and, in some cases, internal sampler wall deposits were evaluated and compared to the filter catch. It was found, rather surprisingly, that analysis of the filter deposits (by ICP-OES) of all the samplers gave equivalent results. It was also found that deposits on some of the sampler walls, which in some protocols are considered part of the sample, could be significant in comparison to the filter deposit. If it is concluded that wall-deposits should be analyzed, then XRF analysis of the filter can only give a minimum estimate of the concentration. Techniques for the statistical analysis of field data were also developed as part of this program and have been reported elsewhere. The results, based on data from the three workplaces where lead was the major element present in the samples, are summarized here. A limit of detection and a limit of quantitation are provided. Analysis of some samples using a second analyzer with a different X-ray source technology indicated reasonable agreement for some metals (but this was not evaluated for lead). Provided it is only necessary to analyze the filters, most personal samplers will provide acceptable results when used with portable XRF analysis for lead around applicable limit values.
本文总结了一项为期五年的研究计划,该计划旨在研究使用便携式X射线荧光(XRF)分析仪分析来自不同工业环境(包括采矿、制造和回收)的空气采样滤膜中的铅。其中四个环境的结果已经报告。这里展示了另外两个金属加工过程的结果。在这两个场所,铅都是空气中总金属的次要成分,其他元素的干扰最小。然而,只有铅是最丰富金属的三个场所的结果被用于方法准确性的总体计算。使用XRF分析仪对滤膜进行检测,然后对其进行酸消解,并通过电感耦合等离子体发射光谱法(ICP - OES)进行分析。滤膜样品使用不同的滤膜夹或“采样器”收集,其中气溶胶沉积物的尺寸(直径)、深度和均匀性因采样器而异。预计采样器的气溶胶收集效率会有所不同,尤其是对于较大颗粒。一旦颗粒进入采样器,其分布在不同采样器之间也预计会有所不同。将采样器配对以解决采样器之间的变异性问题,并且在某些情况下,对采样器内部壁上的沉积物进行评估并与滤膜捕获物进行比较。相当令人惊讶的是,发现所有采样器的滤膜沉积物(通过ICP - OES分析)给出了等效结果。还发现,在某些规程中被视为样品一部分的一些采样器壁上的沉积物,与滤膜沉积物相比可能相当可观。如果得出应分析壁上沉积物的结论,那么对滤膜的XRF分析只能给出浓度的最低估计值。作为该计划的一部分,还开发了现场数据统计分析技术,并已在其他地方报告。这里总结了基于来自样品中铅是主要元素的三个工作场所的数据得出的结果。给出了检测限和定量限。使用具有不同X射线源技术的第二台分析仪对一些样品进行分析表明,对于某些金属有合理的一致性(但未对铅进行评估)。如果只需要分析滤膜,那么大多数个人采样器在与便携式XRF分析一起用于铅含量在适用限值附近时将提供可接受的结果。