Peaks troubleshooting

Beeause the study of rotor dynamies and vibration analysis is eontained in numerous texts only some basie troubleshooting tables and guidelines are presented. They deseribe the most eommon peaks in a typieal vibration analysis speetrum and how these symptoms might be mitigated. 

Discuss troubleshooting procedures for spectrophotometers for 1) failure of electrical components, 2) unexpectedly high absorbance readings, and 3) an unexpected peak in an absorption spectrum. 

Suggested changes are to increase the percentage A at the beginning if the retention time for early peaks are considerably longer than that shown in Figure FI.3.2 or decrease it at 20 min if the later peaks are not well resolved (see Critical Parameters and Troubleshooting). 

Using this or similar mixtures, inject a sample into an equilibrated column, elute the resolved bands, and record them on the recorder. Calculate plate counts for the first and last peak using the 5 [Pg.38]

HPLC Troubleshooting Technical Notes, 1st Ed. Phenomenex Corp. Torrance, CA, USA. 2 Feb 1993. http //kerouac.pharm.uky.edu/asrg/hplc/troubleshooting.html. McDowall, R.D. Where did that peak come from LC GC Int. 1997, 6, 358-359. 

A new topic is now included Chapter 20 about quahty assurance. Part of it could be found before in chapter 19 but now the subject is presented much broadly and independent of Analytical HPLC . Two chapters in the appendix were updated and expanded by Bruno E. Lendi, namely the ones about the instrument test (now chapter 25) and troubleshooting (now chapter 26). Some new sections were created 1.7, comparison of HPLC with capillary electrophoresis 2.11, how to obtain peak capacity 8.7, van Deemter curves and other coherences 11.3, hydrophilic interaction chromatography 17.2, method transfer 18.4, comprehensive two-dimensional HPLC 23.3, fast separations at 1000 bar 23.5, HPLC with superheated water. In addition, many details were improved and numerous references added. 

In the second scenario shown by the data in Table 10.2, poor precision was encountered in both the retention time and peak area of an analyte. Scrutiny of the data showed that both retention time and peak area tended to trend upward. Troubleshooting the autosampler by replacing the sampling syringe yielded no improvements. The poor precision of retention time hinted to possible column problems. The column was therefore replaced and acceptable precision was restored. 

Cameras ensure that boilers operate at peak efficiency. They also help reduce NO emissions. By monitoring burners, they enable operators to quickly confirm proper ignition, and identify flame instability, incomplete combustion, or poor flame distribution. This can shorten troubleshooting and start-up time by several... 

Troubleshooting of Column Problems 17.2.1 Peak-Shape Problems... 

We divided this section into two major subsections peak-shape problems and retention-time problems. The last section then covers problems that do not fit into the first two categories, such as pressure problems. This structure should allow you to quickly move to the chapter that covers the problem that you are trying to solve. In the section of peak-shape problems, example chromatograms should also help to point you to the most appropriate section. While this structure is good for rapid troubleshooting, it also makes repetition unavoidable. Therefore, we would like to remind the reader that this part of the book is not designed to be read as a consecutive text. 

The most common cause of extra peaks in the chromatogram is the sample itself. The source of the sample may be different, it may have decomposed or aged otherwise. It should be easy to verify whether a particular sample is the source of the extra peak by comparison with samples from other sources or the injection of standards or blanks. If the injection of standards or blanks results in extra peaks, we should next troubleshoot the injector and the mobile phase. 

HPLC Instrumentation Troubleshooting Table 1 Peak shape problems and remedies. 

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