Characteristics of atomic absorption calibration curves with the transversely heated graphite furnace

被引:12
作者
Bencs, L [2 ]
Szakács, O
Szoboszlai, N
Ajtony, Z
Bozsai, G
机构
[1] Univ Antwerp, Micro & Trace Anal Ctr, B-2610 Antwerp, Belgium
[2] Hungarian Acad Sci, Res Inst Solid State Phys & Opt, H-1525 Budapest, Hungary
[3] Eotvos Lorand Univ Sci, Dept Inorgan & Analyt Chem, H-1518 Budapest, Hungary
[4] Univ W Hungary, Inst Food Sci, H-9200 Mosonmagyarovar, Hungary
[5] Jozsef Fodor Natl Publ Hlth Ctr, Cent Chem Lab, H-1450 Budapest, Hungary
关键词
D O I
10.1039/b208198a
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Calibration curves with two quasi-linear sections ("double sloping'') were observed for the medium volatile elements, Cr and Cu, with the use of a SIMAA 6000 graphite furnace atomic absorption spectrometer under interrupted internal gas flow conditions. If a standard transversally heated graphite atomizer (THGA) tube was shortened by 0.5 mm at both of its ends, (i.e. the gaps were enlarged between graphite furnace housing and tube ends), a stronger declination of the calibration curves resulted. Elements with fairly high diffusion coefficients (>5.8 cm(2) s(-1)) and with short appearance time of their transients (<0.6 s), such as Cr and Cu, have shown the most characteristic sensitivity drop towards higher concentrations. This anomalous feature could be eliminated in three different ways; (1) by applying end-capped THGA tubes, (2) using mini-flow (50 cm(3) min(-1)) conditions during the atomization stage, and (3) by adding Pd-Mg chemical modifier. For the low volatile Mo and V, the calibration curves had no irregular shape. For Ag, Co, Cr, Cu, Mn and Ni, the mini-flow settings improved the linearity of the calibration curves and extended the upper limit of the linear calibration range by a factor of 1.5-2.0. The irregular characteristic of the analytical curves was interpreted as an increased vapour loss at higher analyte concentrations through the opened ends of the standard THGA tubes. This vapour loss was associated with the significantly diverse expulsion velocities of atoms, caused by the difference in temperature and concentration gradients, when evaporating amounts of analytes with more than one order of magnitude difference.
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页码:105 / 110
页数:6
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