Tungsten-rhodium permanent chemical modifier for lead determination in sediment slurries by electrothermal atomic absorption spectrometry

被引:58
作者
Lima, EC [1 ]
Barbosa, F [1 ]
Krug, FJ [1 ]
机构
[1] Univ Sao Paulo, Ctr Energia Nucl Agr, BR-13400970 Piracicaba, SP, Brazil
关键词
D O I
10.1039/a904373j
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A tungsten carbide-rhodium coating on the integrated platform of a transversely heated graphite atomiser was used as a permanent chemical modifier for the determination of Pb in sediment slurries by electrothermal atomic absorption spectrometry. Slurries were sonicated for 20 s before being delivered to the previously W-Rh treated platform. The number of sediment particles introduced into the atomiser for delivery of a 20 mu l slurry aliquot ranged from 1300 to 3400. The permanent W-Rh modifier remains stable for approximately 250 firings when 20 mu l of slurry containing up to 0.5% m/v are delivered to the atomiser. In addition, the permanent modifier increases the tube lifetime by 50-95% when compared with untreated integrated platforms. Also, there is less degradation of sensitivity during the atomiser lifetime when compared with conventional modifiers, resulting in a decreased need for re-calibration during routine analysis. Detection limits, based on integrated absorbance for 0.50% m/v slurries, were 61 ng g(-1) Pb for the 250 mu g W + 200 mu g Rh permanent modifier and 125 ng g(-1) Pb for 5 mu g Pd + 3 mu g Mg(NO3)(2). The RSD for 735 consecutive measurements of 20 mu l of a 0.50% m/v sediment slurry was 3.6% for the proposed permanent chemical modifier. Results for the determination of Pb in sediment slurries using the W-Rh permanent modifier were in agreement with those obtained with digested solutions by using Pd + Mg(NO3)(2), since no statistical differences were found by the paired t-test at the 99% level.
引用
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页码:1913 / 1918
页数:6
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