Retention time shift for one analyte

071619

Hi,

 

This question is related to my previous question about method development. The method I devised seems to work well, in that a calibration standard run after my curve is set up yields results that I expected. There is virtually no interferences from the new solvent chosen other than having to monitor solvent levels on the GC/FID because of hot weather and evaporation. When I run samples, which are prepared the same way that my calibration standards are prepared, there is a distinct retention time shift with only one of the compounds in the group of analytes. 1,2 trans dichloroethylene shows the retention time shift when it is run as a component of the sample. In calibration standards the retention time is 1.746 min and when it is part of a sample, the retention time is 1.726 min. The other component analytes all retain their retention times that match the calibration standards with no variation. I dont understand why first there is a shift and second, the other analytes in the sample show no retention time shift. I would appreciate any helpful insights or suggestions for resolving this. Also, I am rather a novice when manipulating integration parameters, and that makes me think that that has something to do with my dilemma. Thanks!!

Parents
  • Thank you for your reply Ron. The standard matrix is a solvent, diethyl ether. My sample matrix may have dirt particles or flux, and if it does, it does not appear in the chromatography. Do you think that ambient temperature in the lab would affect the chromatography? My recommended operating temperature range is 68F-80F. My instrument is not fitted with an exhaust flue to move hot exhaust from the lab area, also, my lab is not temperature controlled. There are hot days when my lab heats up to about 92F. Just curious. Also to remember that all of the compounds save one or two have very high vapor pressures and so low boiling points. Would elevated ambient temperature wreak havoc with my chromatography? Any additional insight is helpful.

Reply
  • Thank you for your reply Ron. The standard matrix is a solvent, diethyl ether. My sample matrix may have dirt particles or flux, and if it does, it does not appear in the chromatography. Do you think that ambient temperature in the lab would affect the chromatography? My recommended operating temperature range is 68F-80F. My instrument is not fitted with an exhaust flue to move hot exhaust from the lab area, also, my lab is not temperature controlled. There are hot days when my lab heats up to about 92F. Just curious. Also to remember that all of the compounds save one or two have very high vapor pressures and so low boiling points. Would elevated ambient temperature wreak havoc with my chromatography? Any additional insight is helpful.

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