Dugheri Stefano, Bonari Alessandro, Pompilio Ilenia, Monti Alessandro, Mucci Nicola, Arcangeli Giulio
Laboratorio di Igiene e Tossicologia Industriale, Azienda Ospedaliero-Universitaria Careggi, Largo P. Palagi 1, 50100 Firenze, Italy.
Dipartimento di Medicina Sperimentale e Clinica, University of Florence, Largo G.A. Brambilla 3, 50139 Firenze, Italy.
Int J Anal Chem. 2016;2016:2129053. doi: 10.1155/2016/2129053. Epub 2016 Oct 13.
Hydrogen fluoride (HF) is a basic raw material for a wide variety of industrial products, with a worldwide production capacity of more than three million metric tonnes. A novel method for determining particulate fluoride and gaseous hydrogen fluoride in air is presented herewith. Air was sampled using miniaturised 13 mm Swinnex two-stage filter holders in a medium-flow pumping system and through the absorption of particulate fluoride and HF vapours on cellulose ester filters uncoated or impregnated with sodium carbonate. Furthermore, filter desorption from the holders and the extraction of the pentafluorobenzyl ester derivative based on solid-phase microextraction were performed using an innovative robotic system installed on an autosampler on-line with gas chromatography (GC)/mass spectrometry (MS). After generating atmospheres of a known concentration of gaseous HF, we evaluated the agreement between the results of our sampling method and those of the conventional preassembled 37 mm cassette (±8.10%; correlation coefficient: 0.90). In addition, precision (relative standard deviation for = 10, 4.3%), sensitivity (0.2 g/filter), and linearity (2.0-4000 g/filter; correlation coefficient: 0.9913) were also evaluated. This procedure combines the efficiency of GC/MS systems with the high throughput (96 samples/day) and the quantitative accuracy of pentafluorobenzyl bromide on-sample derivatisation.
氟化氢(HF)是多种工业产品的基础原料,全球产能超过300万吨公吨。本文介绍了一种测定空气中颗粒态氟化物和气态氟化氢的新方法。空气采样采用小型化的13毫米Swinnex两级过滤器支架,置于中流量抽气系统中,颗粒态氟化物和HF蒸汽通过吸附在未涂层或浸渍碳酸钠的纤维素酯滤膜上进行采集。此外,使用安装在自动进样器上的创新机器人系统在线连接气相色谱(GC)/质谱(MS),进行滤膜从支架上的解吸以及基于固相微萃取的五氟苄基酯衍生物的萃取。在生成已知浓度气态HF的大气环境后,我们评估了我们的采样方法与传统预组装37毫米采样盒的结果之间的一致性(±8.10%;相关系数:0.90)。此外,还评估了精密度(n = 10时的相对标准偏差为4.3%)、灵敏度(0.2微克/滤膜)和线性度(2.0 - 4000微克/滤膜;相关系数:0.9913)。该方法将GC/MS系统的效率与高通量(每天96个样品)以及五氟苄基溴样品上衍生化的定量准确性相结合。