电热原子吸收光谱法测定铁的最佳化方法

Analusis Pub Date : 2000-09-01 DOI:10.1051/ANALUSIS:2000133
S. Salomon, P. Giamarchi, A. Bihan
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引用次数: 7

摘要

本文报道了电热原子吸收光谱法测定海洋基质中的硫化氢。我们优化了光谱因素,即入口单色器狭缝高度、狭缝宽度和灯电流,以及电热因素,即煅烧温度、煅烧时间、雾化温度和注入体积的实验条件,因为这两组是独立的。由于我们的实验研究领域存在技术限制,我们建立了一个d -最优实验设计来进行这些优化。我们监测了瞬时比吸光度、比积分吸光度和非比积分吸光度的标准差三种实验响应。在三种相反的实验条件下,它们都清楚地显示出最优。因此,实验反应的可取性转换使我们能够获得更好的折衷方案。最后,我们计算了一个新的实验响应,该响应考虑了原始测量值,以直接估计检测限。该计算响应的优化表明,在相同的实验妥协下获得的最低检测限比可取性研究建议的最低检测限。这一结果使我们能够验证计算响应作为电热原子吸收光谱的一个有趣的优化准则。
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Desirability approach for optimisation of electrothermal atomic absorption spectrometry factors in iron determinations
We report here on from determination in sea matrix by electrothermal atomic absorption spectrometry. We optimised the experimental conditions of the spectroscopic factors, i.e. entrance monochromator slit height, slit width and lamp current, and of the electrothermal factors, i.e. calcination temperature, calcination duration, atomisation temperature and injected volume, since these two groups are independent. Because of the technical constraints occuring on our experimental domain of study we built a D-optimal experimental design to conduct these optimisations. We monitored three experimental responses, i.e. the standard deviation of the instantaneous specific absorbance, the specific integrated absorbance and the non-specific integrated absorbance. The three of them clearly showed an optimum in three opposed experimental conditions. Consequently, a desirability transformation of the experimental responses permitted us to obtain a better compromise. We, finally, computed a new experimental response which took the raw measurements into account to directly estimate the limits of detection. The optimisation of this computed response showed us that the lowest detection limit was obtained under the same experimental compromise than the one suggested by the desirability study. This result allowed us to validate the computed response as an interesting optimisation criterion in electrothermal atomic absorption spectrometry.
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