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Diagnostic: Gradient garbage
In the case of gradient separations, extra peaks that show up in standards, samples, and blank gradients are usually caused by contamination of the weak solvent. This can be confirmed by running a series of blank gradients with increasing equilibration times between gradients. For example, equilibrate the column for the usual time, then run a gradient (this is simply to clean off the column); equilibrate again for the usual time, then run a second gradient; equilibrate the column for three times the usual time and run a third gradient. Compare the size of the extra peaks in the second and third gradients. If the heights/areas of the extra peaks increase with increasing equilibration time, this confirms weak solvent contamination as the cause.
 
Possible sources include:
  • the water system
  • buffers/salts/additives
  • dirty glassware
  • contaminated pH electrodes, etc.
  • contaminated or impure sparging gas
  • contaminated organic solvent (if the "A" reservoir contains organic)
     
    Ref: LC-GC 16(11) 992 (1998)



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