气相色谱用户培训教材.ppt

* * * * * * 17 Sulfur emission occurs around 400 nm wavelength. Therefore we can use an optical filter to eliminate most HC interferences. This figure shows PFPD emission spectra of 0.1% dimethyl sulfoxide-cyclohexane solution viewed through a scanning monochromator. The upper trace was obtained with a short undelayed gated integration. The lower trace was obtained under the same conditions but with a long and delayed gated integration of the pulsed flame emission. The observed S2* emission is independent of any hydrocarbon or flame background emission. The use of wide band-pass optical filters can further isolate the S-emission. The BG-12 colored glass filter that Varian uses for the PFPD S-mode allows passage of light between 340-460 nm. * 16 Emphasize that S emission occurs after HC emission is complete. Correct gating excludes HC interferences. This figure shows the characteristic temporal light emission behavior in the S-detection mode (using a scanning monochromator). At 0-4 ms, you get the pulsed hydrocarbon-related emission of 2 ms duration, and at over 5 ms, you get the S-related emission which lasts 16 ms and is delayed in time, maximizing 5-6 ms after HC-related emission. Therefore sulfur emission can easily be separated in time from any residual hydrocarbon emission. To take advantage of the discreet emissions that occur with each pulse, the detector electronics view the emission only during the delayed sulfur emission, after the flame background and hydrocarbon emissions have decayed away. A gated integrator is used in this way to increase (by 3-orders of magnitude) the S-selectivity of the PFPD versus the FPD. 响应 离子数目正比于碳原子数目(C-H键). 一些官能团如羰基(CO=)、羟基(－OH）、卤素（－X）、胺（NH4+）则很少或根本不会离子化。 对无机气体如H2O, CO2, SO2, 和Nox不灵敏。 火焰 以氢气和空气作为燃气。 在控制的流速下进行电子点火。 火焰无色－除非受到污染。 FID工作原理 燃烧气 H2与载气（或载气＋尾吹气）的流速一般为1:1 。 空气一般为氢气的10倍。。 大的空气流速和热检测器可以赶走大量的水蒸气。 FID燃烧气流速对信号的影响 FID工作原理 FID注意事项 正确设置H2、空气和尾吹气的流量 检测器温度应比柱温箱设定的最高温度高30?C，且大于150?C以防止水凝结在检测器上 FID在电路打开后，会自动点火。在3800报告熄火以