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Multielement trace analysis of pure graphite powders using optical emission spectrometry coupled to a magnetically stabilized DC arc supplied with halogenating gases as chemical modifiers – a rapid and robust methodology†‡
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-02-01 00:00:00 , DOI: 10.1039/c7ja00387k Ralf Matschat 1, 2, 3, 4, 5 , Jürgen Hassler 3, 4, 5 , Silke Richter 1, 2, 3 , Margitta Klewe 2, 3, 6 , Angelika Dette 1, 2, 3
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-02-01 00:00:00 , DOI: 10.1039/c7ja00387k Ralf Matschat 1, 2, 3, 4, 5 , Jürgen Hassler 3, 4, 5 , Silke Richter 1, 2, 3 , Margitta Klewe 2, 3, 6 , Angelika Dette 1, 2, 3
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A magnetically stabilized DC arc device, designed for operation with OES spectrometers was used to determine the elements Ag, Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Si, Sn, Sr, Ti, V, Zr at trace levels of some μg kg−1 up to some 10 mg kg−1 in graphite powders. The coil for the generation of the homogeneous magnetic field was placed outside the closed arc chamber. The time programs of variable current strengths of the magnetic coil (up to 6 A) and of the arc (up to 17 A) which was burning in air were computer controlled. Halogenating gases (mainly CCl2F2, alternatively SF6 and NF3) were used as chemical modifiers to allow an effective release of the carbide forming trace elements. The mass flow controlled modifier gas was led through a special carrier electrode near the arc plasma. The emission radiation was guided by an optical fiber alternatively into two different ICP spectrometers in which the ICP torches were removed. The synergistic interaction of the magnetic field with the halogenating modifier gases resulted in a significant improvement in the analytical performance of the optimized analytical method. All our results for 22 trace elements were in good agreement with the means of an inter-laboratory comparison by BAM for certification of a pure graphite powder material; this holds also for our results for two other graphite materials. The optimized method showed an analytical performance suitable for comprehensive trace analysis of pure graphite. The instrumentation could be integrated into modern DC arc emission spectrometers to improve their analytical capabilities substantially.
中文翻译：
使用光发射光谱法与磁稳定的直流电弧结合卤化气体作为化学改性剂，对纯石墨粉末进行多元素痕量分析–快速而可靠的方法† •
设计用于OES光谱仪的磁稳定直流电弧设备用于确定元素Ag，Al，B，Ba，Be，Ca，Co，Cr，Cu，Fe，Ga，In，K，Li，Mg，Mn在石墨粉中的痕量水平为-，Mo，Na，Nb，Ni，Si，Sn，Sr，Ti，V，Zr，从约μgkg -1到约10 mg kg -1。用于产生均匀磁场的线圈被放置在封闭电弧室的外部。在空气中燃烧的电磁线圈（最高6 A）和电弧（最高17 A）的可变电流强度的时间程序是由计算机控制的。卤化气体（主要是CCl 2 F 2，或者是SF 6和NF 3）用作化学改性剂，以有效释放碳化物形成的痕量元素。质量流控制的改性剂气体被引导通过电弧等离子体附近的特殊载体电极。发射辐射通过光纤引导进入两个不同的ICP光谱仪中，在其中除去了ICP炬管。磁场与卤化改性气体的协同作用导致优化分析方法的分析性能得到显着改善。我们对22种微量元素的所有结果均与BAM在实验室间进行的用于鉴定纯石墨粉末材料的比较方法相吻合；这也适用于我们对其他两种石墨材料的研究结果。优化后的方法显示出适合纯石墨全面痕量分析的分析性能。该仪器可以集成到现代直流电弧发射光谱仪中，以大大提高其分析能力。
更新日期：2018-02-01
中文翻译：
使用光发射光谱法与磁稳定的直流电弧结合卤化气体作为化学改性剂，对纯石墨粉末进行多元素痕量分析–快速而可靠的方法† •
设计用于OES光谱仪的磁稳定直流电弧设备用于确定元素Ag，Al，B，Ba，Be，Ca，Co，Cr，Cu，Fe，Ga，In，K，Li，Mg，Mn在石墨粉中的痕量水平为-，Mo，Na，Nb，Ni，Si，Sn，Sr，Ti，V，Zr，从约μgkg -1到约10 mg kg -1。用于产生均匀磁场的线圈被放置在封闭电弧室的外部。在空气中燃烧的电磁线圈（最高6 A）和电弧（最高17 A）的可变电流强度的时间程序是由计算机控制的。卤化气体（主要是CCl 2 F 2，或者是SF 6和NF 3）用作化学改性剂，以有效释放碳化物形成的痕量元素。质量流控制的改性剂气体被引导通过电弧等离子体附近的特殊载体电极。发射辐射通过光纤引导进入两个不同的ICP光谱仪中，在其中除去了ICP炬管。磁场与卤化改性气体的协同作用导致优化分析方法的分析性能得到显着改善。我们对22种微量元素的所有结果均与BAM在实验室间进行的用于鉴定纯石墨粉末材料的比较方法相吻合；这也适用于我们对其他两种石墨材料的研究结果。优化后的方法显示出适合纯石墨全面痕量分析的分析性能。该仪器可以集成到现代直流电弧发射光谱仪中，以大大提高其分析能力。
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