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采用激光烧蚀和内标信号归一化的多元素激光增强电离光谱法测定造粒煤中痕量铅。

Multielemental laser-enhanced ionization spectrometry for the determination of lead at the trace level in pelletized coal using laser ablation and internal standard signal normalization.

作者信息

Gravel Jean-François Y, Viger Mathieu L, Nobert Philippe, Boudreau Denis

机构信息

Center for Optics, Photonics and Lasers (COPL) and Department of Chemistry, Université Laval, Quebec City (PQ), Canada G1K 7P4.

出版信息

Appl Spectrosc. 2004 Jun;58(6):727-33. doi: 10.1366/000370204873088.

DOI:10.1366/000370204873088
PMID:18171515
Abstract

Laser ablation laser-enhanced ionization (LA-LEI) was used for the simultaneous measurement of lead and indium in pelletized graphite and coal samples. UV Laser ablation of the solid samples was performed in an ablation cell and the ablated material was carried by a flow of gas to a miniature LEI flame where lead was detected. The influence of parameters such as binder content of the solid pellets and dispersion of the analytes spiked in the sample material, as well as the number of ablation pulses per crater on signal repeatability and on the size and shape of ejected particles was examined. Measurement repeatability values of 2 to 5% of relative standard deviation were obtained using indium as an internal standard to correct for variations in the ablation rate. A limit of detection of 120 nanograms per gram was calculated for the determination of Pb in high-purity graphite. The Pb concentration in the NIST 1632c Bituminous Coal certified reference material was determined to within 1% of its certified value, using graphite as the matrix-matching material and In as the internal standard in pelletized solid samples.

摘要

激光烧蚀激光增强电离(LA-LEI)用于同时测量造粒石墨和煤样品中的铅和铟。在烧蚀池中对固体样品进行紫外激光烧蚀,烧蚀后的物质通过气流输送到微型LEI火焰中,在那里检测铅。研究了诸如固体颗粒的粘合剂含量、样品材料中添加的分析物的分散情况以及每个坑的烧蚀脉冲数等参数对信号重复性以及喷射颗粒的大小和形状的影响。以铟作为内标来校正烧蚀速率的变化,获得了相对标准偏差为2%至5%的测量重复性值。对于高纯度石墨中铅的测定,计算出的检测限为每克120纳克。使用石墨作为基体匹配材料,铟作为造粒固体样品中的内标,测定了NIST 1632c烟煤标准参考物质中的铅浓度,其测定值在认证值的1%以内。

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