Troubleshooting

ChromatographyTroubleshooting Manual

Work back from the symptom: first establish whether the problem lies with the sample, the mobile phase, the column or the instrument, then work through the listed order — rather than replacing the column first.

Ten Common Chromatography Problems · Causes and Fixes

Possible cause
  • A dry or voided bed head (most common)
  • A blocked frit causing uneven flow distribution
  • Overloading (beyond column capacity)
  • Injection solvent mismatched to the mobile phase
  • Excessive extra-column dead volume (fitting problem)
Fix
  • Replace the guard cartridge and see whether it improves
  • Regenerate by flushing with a strong solvent (isopropanol) to clear the blockage
  • Reduce the load (usually < 10 μg on an analytical column)
  • Switch to a weaker injection solvent (the initial mobile phase)
  • Check every fitting and minimize dead volume
Possible cause
  • Basic compounds interacting with residual silanols
  • Mobile phase pH not suppressing ionization of the basic compound
  • A contaminated or damaged bed head
  • Injection solvent too strong
Fix
  • Add 0.1% triethylamine (TEA) to the mobile phase to mask silanols
  • Lower the mobile phase pH (pH < pKa – 2) to suppress protonation of the basic group
  • Switch to a more completely endcapped column (HPLCONE is fully endcapped)
  • Dissolve the sample in a weaker solvent
Possible cause
  • A void at the bed head (bed collapse)
  • Injection solvent far stronger than the mobile phase
  • Cracking within the packed bed
Fix
  • Inspect the bed head: remove the end fitting and look for a void; a void means the bed head is damaged and the column must be replaced
  • Dissolve the sample in a weaker solvent (similar to or weaker than the initial mobile phase)
  • If the bed has cracked, the column must be replaced
Possible cause
  • The inlet frit blocked by particulates
  • Buffer salt crystallizing out
  • Protein or lipid deposited at the bed head
  • Mobile phase too viscous (neat methanol at low temperature)
  • Blocked tubing (not the column itself)
Fix
  • Remove the column first and see whether system backpressure drops; if it does, the problem is in the column
  • Flush with isopropanol at high flow for 20 min
  • Replace the guard cartridge or the inlet frit
  • Review sample preparation and ensure 0.22 μm filtration
  • Raise the temperature (40 °C) to reduce methanol viscosity
Possible cause
  • A loose or cracked fitting leaking
  • A pump problem (failed check valve)
  • Loss of packing from the column (broken frit)
Fix
  • Check every fitting for leakage
  • Check that pump pressure is stable (replace the check valve ball)
  • If packing has been lost, check whether the outlet frit is intact
Possible cause
  • Bubbles in the mobile phase
  • An aged detector lamp (deuterium lamp at end of life)
  • Mobile phase not adequately degassed
  • Changing organic proportion during gradient elution
  • Column not adequately equilibrated
Fix
  • Degas the mobile phase by sonication for 15 min, or use in-line degassing
  • Check the deuterium lamp energy and replace it when below threshold (our compatible lamps can be used)
  • For gradient methods, run a blank gradient first and record the baseline background
  • Extend equilibration to 20–30 column volumes
Possible cause
  • Carryover from the previous injection (cross-contamination)
  • Impurities in the sample solvent
  • Trace UV-absorbing impurities in the mobile phase
  • A contaminated injection valve
Fix
  • Extend the wash time, or flush the injection valve with a strong solvent
  • Check that the sample solvent blank is clean
  • Switch to HPLC-grade reagents for the mobile phase
  • Flush the injection valve with isopropanol
Possible cause
  • Unstable column temperature
  • Inconsistent mobile phase composition
  • Column not adequately equilibrated
  • Unstable pump flow rate
Fix
  • Use a column oven and fix the temperature
  • Prepare the mobile phase accurately, making up to volume in a volumetric flask
  • Equilibrate with at least 10 column volumes before each injection
  • Calibrate the pump flow rate
Possible cause
  • Inaccurate injection volume (autosampler problem)
  • Insufficient detector lamp energy
  • Sample lost in the autosampler (adsorption)
  • Sample concentration miscalculated
Fix
  • Verify the injection volume with a standard of known concentration
  • Check and replace the detector deuterium lamp
  • Switch to PEEK sample tubing to reduce adsorption
  • Prepare a fresh standard to verify the concentration
Possible cause
  • Sample solvent absorbs less than the mobile phase (negative peak)
  • Refractive index mismatch (RI detector)
  • Overloading producing a system peak
Fix
  • Dissolve the sample in a solvent close to the mobile phase
  • Reduce the injection volume
  • On an RI detector, refill the reference cell with the same mobile phase as the sample side