Thurbide Kevin B, Anderson Christine D
Department of Chemistry, University of Calgary, 2500 University Drive, NW, Calgary, Alberta, Canada T2N 1N4.
Analyst. 2003 Jun;128(6):616-22. doi: 10.1039/b212727j.
A novel micro-flame photometric detector (FPD) employing a miniature counter-current flame is described. The micro-FPD flame, encompassing a volume of about 30 nL, is operated inside the end of a capillary gas chromatography column (i.e. on-column) or inside of a quartz capillary after the column (i.e. post-column). Either air or oxygen can support a hydrogen flame in the device, although oxygen is far preferable. The detector can be operated for several hours without any observed degradation in performance or flame stability. The optimal gas flows established for the detection of sulfur and phosphorus are in the range of 4 mL min(-1) of oxygen and 9 to 13 mL min(-1) of hydrogen. The fuel-rich micro-FPD flame generates chemiluminescent blue S2* emission for sulfur and green HPO* emission for phosphorus, similar to a conventional FPD. Sulfur response in the micro-FPD is quadratic over nearly 3 orders of magnitude while that of phosphorus is linear over nearly 5 orders of magnitude. The micro-FPD detection limit for sulfur is 1 x 10(-9) g S s(-1), and that of phosphorus is 2 x 10(-10) g P s(-1). The properties established for the initial prototype of the micro-FPD make this counter-current flame method potentially suitable for integration with on-chip gas chromatography or other micro-analytical devices where flame-based detection methods are desirable.
本文描述了一种采用微型逆流火焰的新型微火焰光度检测器（FPD）。微FPD火焰的体积约为30 nL，在毛细管气相色谱柱末端（即柱上）或柱后石英毛细管内部（即柱后）运行。空气或氧气均可在该装置中支持氢气火焰，但氧气更为理想。该检测器可运行数小时，性能或火焰稳定性未见任何下降。用于检测硫和磷的最佳气体流速范围为氧气4 mL min(-1)和氢气9至13 mL min(-1)。富燃料的微FPD火焰会产生硫的化学发光蓝色S2发射和磷的绿色HPO发射，类似于传统FPD。微FPD中硫的响应在近3个数量级内呈二次方关系，而磷的响应在近5个数量级内呈线性关系。微FPD对硫的检测限为1 x 10(-9) g S s(-1)，对磷的检测限为2 x 10(-10) g P s(-1)。微FPD初始原型所具备的特性使得这种逆流火焰方法有可能适用于与片上气相色谱或其他需要基于火焰检测方法的微分析装置集成。
