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LCMS Presentation

1) This document provides troubleshooting tips and preventative maintenance strategies for HPLC systems. 2) It addresses issues like high or low pressure, leaks, irregular chromatograms, and recommends daily flushing, replacing seals and lamps regularly, and using guard columns. 3) The document also provides tips for proper mobile phase, reservoir, pump, fitting, check valve, and column maintenance to minimize problems and extend the life of the system.

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Nur Shahila Ibrahim
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© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PPT, PDF, TXT or read online on Scribd
925 views16 pages

LCMS Presentation

1) This document provides troubleshooting tips and preventative maintenance strategies for HPLC systems. 2) It addresses issues like high or low pressure, leaks, irregular chromatograms, and recommends daily flushing, replacing seals and lamps regularly, and using guard columns. 3) The document also provides tips for proper mobile phase, reservoir, pump, fitting, check valve, and column maintenance to minimize problems and extend the life of the system.

Uploaded by

Nur Shahila Ibrahim
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PPT, PDF, TXT or read online on Scribd

HPLC

TROUBLESHOOTING
TROUBLESHOOTING :
1) Pressure
High: blockage,setting
Low: bubble,check valve,setting
Variable: bubble,check valve
Check chromatogram
2) Leaks
Loose fitting
Overpressure
Failed seal: pump, injector
3) Chromatogram
Constant high or low retention
Variable retention: bubble, check valve
Peak shape: column, mobile phase
Check pressure
MAINTAINING LC SYSTEM WITH
EASE:
1) Clean and degassed solvents.
2) Used guard column.
3) Flush the system daily.
4) Replace the pump seals regularly
(every 3 months).
5) Replace the detector lamp early (6
months to 1 year)
MOBILE PHASE
Never refill the reservoir.
Mobile phase reservoir should be an
inert container.
MP bottle should be covered to prevent
dust from entering.
Do NOT use parafilm to cover bottle
cap.
Change water EVERYDAY.
Prepare enough mobile phase for only
one batch running.
RESERVOIR PREVENTIVE
MAINTENANCE
oFilter mobile phase
oUse inlet-line frit (sinker frit)
oDegas mobile phase
oClean or replace regularly
PUMP PREVENTIVE
MAINTENANCE
1) Flush system daily
2) Use fresh solvents
3) Flush behind heads
4) Scheduled seal replacement
5) Check owner’s manual
6) Other per system log
SOLVE ERRATIC FLOW &
PRESSURE PROBLEMS

1) Check inlet frit and tubing


2) Degas solvents
3) Purge pump
4) Sonicate check valve
5) Replace check valve
CHANGE PUMP SEALS
Leaking
Liquid dripping
Pressure build up
Fluctuation of 2 piston
After 1 yr (Warranty from
manufacture)
After 6 months (suggest)
MINIMIZE CHECK VALVE
FAILURE
1. Filter solvents
2. Degas solvents
3. Use sinker frit
4. Flush system daily
5. Never shut off with buffers in
system (low flow is ok)
FITTING
• Use match parts
• Stay with one brand
• Label connectors
• Don’t over-tighten
• Don’t under-tighten
• Use PEEK
COLUMN DEATH!!!!
• Plugging the frit or column
 Pressure increase
 Peak shape problems

• Mechanical shock (voids)


• Adsorbed sample impurities
• Chemical attack on the silica or
bonded phase
SYMPTOMS???
• Pressure increase
• Tailing peaks
• Loss in plate number
• Loss selectivity
• Decrease in retention
PM
• Use in-line filter
• Use frit or guard column
• Cleaner samples (sample prep.)
• Flush column especially MP that
using buffer
• Use HPLC grade solvent
• Flush system daily
EXTENDING COLUMN LIFE
1) Rugged method
2) Sample preparation
3) In-line filter
4) Guard column
5) Dedicated columns
6) Regular flushing
COLUMN NOT CONTRIBUTE ALL
PROBLEM
• Overload
• Strong sample diluent
• Injection volume
• On-column degradation
• “Extra” peaks
• Mobile phase problems

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