首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Feasibility of filter atomization in high-resolution continuum source atomic absorption spectrometry
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Feasibility of filter atomization in high-resolution continuum source atomic absorption spectrometry

机译:高分辨率连续谱源原子吸收光谱法中过滤器雾化的可行性

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A prototype spectrometer for high-resolution continuum source atomic absorption spectrometry(HR-CS AAS),built at ISAS Berlin,Germany,was combined with a graphite filter atomizer(GFA),earlier developed at TUT,Pretoria,South Africa.The furnace and auto-sampler units from a commercial AA spectrometer,model AAS vario 6(Analytik Jena AG,Jena,Germany),were employed in the instrument.Instead of conventional platform tube,the GFA was used to provide low measurement susceptibility to interferences and short determination cycle.The GFA was modified according to the design of the furnace unit and optimal physical parameters of its components(filter and collector)found.Afterwards,optimal GFA was replicated and tested to outline analytical performances of the HR-CS GFA AA spectrometer in view of prospects of multi-element analysis.In particular,reproducibility of performances,repeatability of analytical signals,lifetime,temperature limit and duration of the measurement cycle were examined,and elements available for determination justified.The results show that the peak area of the atomic absorption signal is reproduced in various GFA copies within +-4% deviation range.The GFA can stand temperatures of 2800 deg C with 6 s hold time for 55 temperature cycles,and 2700 deg C(8 s)for about 200 cycles.Only the external tube is prone to destruction while the filter and collector do not show any sign of erosion caused by temperature or aggressive matrix.Analytical signals are affected insignificantly by tube aging.Repeatability of the peak area remains within 1.1-1.7% RSD over more than hundred determination cycles.Peak areas are proportional to the sample volume of injected organic and inorganic liquids up to at least 50 mu L.The drying stage is combined with hot sampling and cut down to 15-20 s.The list of metals available for determination with full vapor release includes Al,Co,Cr,Ni,Pt as well as more volatile metals.Characteristic masses at optimal atomization temperature are close to or slightly better than those found in HR-CS AAS with PIN-platform tubes.In addition,fast sequential determination of multiple elements and truly simultaneous determination of Cd,Fe and Ni using nearby analytical lines were performed with the GFA controlled by a single temperature program and an atomization temperature of 2700 deg C.
机译:在德国ISAS柏林制造的用于高分辨率连续谱源原子吸收光谱仪的原型光谱仪(HR-CS AAS)与早期在南非比勒陀利亚TUT研发的石墨过滤器雾化器(GFA)结合使用。仪器使用了商用AA光谱仪AAS vario 6(Analytik Jena AG,Jena,德国)的自动进样器单元。使用GFA代替传统的平台管,可降低对干扰的测量敏感性,并能快速确定根据炉单元的设计和其组件(过滤器和收集器)的最佳物理参数对GFA进行了修改。然后,复制并测试了最佳GFA,以概述HR-CS GFA AA光谱仪的分析性能。尤其是性能的可重复性,分析信号的可重复性,寿命,温度极限和测量周期的持续时间,以及要素结果表明,原子吸收信号的峰面积在+ -4%偏差范围内的各种GFA副本中均得以再现.GFA可以在2800摄氏度的温度下保持6秒的保持时间,可进行55个温度循环,并在2700摄氏度(8 s)的温度下进行约200个循环。只有外管易于损坏,而过滤器和收集器没有显示出因温度或侵蚀性基质引起的腐蚀迹象。分析信号不受管老化的影响很小。在超过一百个测定周期内,峰面积的可重复性保持在RSD的1.1-1.7%之内。峰面积与注入的有机和无机液体的样品体积成正比,至多为50μL,干燥阶段与热采样和减少至15-20 s。可用于全蒸气释放测定的金属包括Al,Co,Cr,Ni,Pt以及易挥发的金属。最佳雾化温度下的特征质量接近与使用PIN平台管的HR-CS AAS相比要稍好一些。此外,使用单个分析仪控制的GFA可以快速顺序测定多个元素,并使用附近的分析线同时真正测定Cd,Fe和Ni温度程序和2700摄氏度的雾化温度。

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