Optimization of fluorine determination via the molecular absorption of gallium mono-fluoride in a graphite furnace using a high-resolution continuum source spectrometer

被引:78
作者
Gleisner, Heike [1 ]
Welz, Bernhard [2 ,3 ]
Einax, Juergen W. [4 ]
机构
[1] Anal Jena AG, D-07745 Jena, Germany
[2] Univ Fed Santa Catarina, Dept Quim, BR-88040900 Florianopolis, SC, Brazil
[3] Univ Fed Bahia, Inst Nacl Ciencia & Tecnol, CNPq INCT Energia & Ambiente, BR-40170 Salvador, BA, Brazil
[4] Univ Jena, Dept Environm Anal, Inst Inorgan & Analyt Chem, D-07743 Jena, Germany
关键词
High-resolution continuum source AAS (HR-CS AAS); Molecular absorption spectrometry (MAS); Fluorine determination; Gallium mono-fluoride; Graphite furnace; ELECTROTHERMAL VOLATILIZATION; PYROHYDROLYSIS; HALOGENS; SAMPLES; INDIUM; TRACES;
D O I
10.1016/j.sab.2010.08.003
中图分类号
O433 [光谱学];
学科分类号
0703 ; 070302 ;
摘要
The determination of fluorine using the molecular absorption of gallium mono-fluoride (GaF) at the 211.248 nm rotational line has been optimized using a commercially available high-resolution continuum source atomic absorption spectrometer with a transversely heated graphite tube furnace. The electron excitation spectrum of GaF was generated by adding 500 mu g Ga per injection into the graphite tube as molecule forming reagent. Best results were obtained by applying Zr as a permanent modifier and a mixed Pd/Zr modifier, thermally pretreated before each sample injection together with the Ga reagent at 1100 degrees C. The use of sodium acetate and Ru(III) nitrosyl nitrate as additional modifiers injected together with the sample further improved the performance. This way a maximum pyrolysis temperature of 550 degrees C could be used, and the optimum molecule forming temperature was 1550 degrees C. Several drinking water samples, a mineral water sample, and two certified reference materials were analyzed using the standard calibration technique: the absence of potential matrix effects was verified by measuring different dilutions and spiking with known fluorine mass. The results were in good agreement with the certified values and those measured by ion selective electrode; the recovery rate for the spiking experiments was between 97% and 106%. The results show that there was no matrix influence for that kind of samples containing relatively high concentrations of Ca, Mg and chloride, which are known to cause interference in GaF molecule absorption. The limit of detection and the characteristic mass of the method were 5.2 and 7.4 pg F. respectively, and were both about a factor of two better than recently published values. (C) 2010 Elsevier B.V. All rights reserved.
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页码:864 / 869
页数:6
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