色谱柱讲义-雷晓强-色谱世界.ppt

* * * * * This was copied out of the HP 4980, HP 5890 and HP 6890 operating manuals. A sheet of paper with this information is included with every HP column. * * This slide shows three examples of positioning of the column ends in the GC the first two show poor positioning the last shows the proper positioning and the appropriate chromatogram * * * * This was a real example which happened to the speaker of this talk. A new column was installed, and a method (one which had be used many times in the past (it was a simple, robust method). However, when the sample was injected, only a baseline appeared with no peaks. The items listed in the little table actually are printed in the operating manual of the HP 5890 and HP 6890 and probably many others. The operator begin to try each of the items in the list. In one of the next slides, you will see the result of each of the tests. * * This is the same list of tests that we saw in the previous slide. Here we see the result of each of the tests leading to the observation that the sample, although injected into the inlet of the column, it was not coming out of the end of the column into the flame ionization detector. It was found that the soft graphite ferrule had been forced into the bottom of the flame jet and no flow was going up into the detector flame. The interesting thing that was confusing was that the baseline went up with the temperature program although no sample was passing into the flame to make peaks. The FID was dissassembled and cleaned , re-assembled and worked perfectly as seen in the next slide * * This is another common observation, the appearance of a peak that is not symmetrical and also changes in retention time as larger amounts are injected. This is usually an overloaded peak. Sometimes, a peak will be overloaded because it is not well suited for the type of stationary phase. A good example is the injection of benzoic acid on a 5 % phenyl phase. The peak will overload on a normal