| 摘要: |
| 采用微波消解和微波赶酸处理样品,通过氢化物-原子荧光光谱法对天然气处理厂产出硫磺中微量砷进行测定。基于建立的有效数学模型,开发了微波消解-原子荧光光谱法测定硫磺中微量砷的不确定度评定方法。结果 表明:天然气处理厂产出硫磺中砷含量均小于1 μg /g,达到工业硫磺GB/T 2449.1-2014规定的优级品的要求；消解回收率、标准曲线拟合和测量重复性是影响微波消解-原子荧光光谱法不确定度的主要因素,其中对高、中浓度段不确定度贡献最大是消解回收率,而对低浓度段不确定度贡献最大的是标准曲线拟合。 |
| 关键词: 不确定度 砷 硫磺 微波消解 原子荧光光谱法 |
| DOI：10.3969/j.issn.1007-3426.2020.01.018 |
| 分类号: |
| 基金项目:中国石油西南油气田公司科研项目“硫磺中微量铁、砷含量测定方法推广应用”(20180308-05) |
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| Evaluating uncertainty of determining trace As in sulfur by microwave digestion and atomic fluorescence spectrometry |
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Tu Zhenquan1,2, Wang Yujie1,2, Ouyang Qinghua1,2, Lu Chun1,2
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1. Research Institute of Natural Gas Technology, PetroChina Southwest Oil & Gasfield Company, Chengdu, Sichuan, China;2. Key Laboratory of Natural Gas Quality Control and Energy Measurement, CNPC, Chengdu, Sichuan, China
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| Abstract: |
| Trace As in sulfur produced from the natural gas processing plant was detected by hydride-atomic fluorescence spectrometry after treating with microwave digestion and acid-driving. Based on the established effective mathematical model, an uncertainty evaluation method for determining trace As in sulfur by microwave digestion and atomic fluorescence spectrometry was developed. The results show that all the contents of As in sulfur are lower than 1 μg/g, meeting the superior-quality requirement of industrial sulphur of China national standard GB/T 2449.1-2014. The main factors for affecting the uncertainty of this method are the digestion recovery rate, standard curve fitting and measurement repeatability, of which the greatest contribution of the uncertainty with regard to the high and medium concentrations is the digestion recovery rate while that is the standard curve fitting for the low concentration. |
| Key words: uncertainty As sulfur microwave digestion atomic fluorescence spectrometry |
