7.4
Section 7
TroubleshooTing
Pinnacle Operators Manual
Pickering Laboratories Inc.
COMMON SYSTEM PROBLEMS continued
continued
OBSERVED PROBLEM COMMON CAUSE ACTION TO TAKE NOTES
Over-pressure relief valve is opened There is a blockage in the system Determine the exact location of the
blockage.
Disconnect one fitting at a time,
moving backward from the back-
pressure regulator end, until the
pressure drops
Flush the system with solvent/water
until pressure drops, or replace
appropriate part
Blocked Heated Reactor reactor Improper Shutdown
Dissolved silica precipitating in the
reactor
Contaminated reagents
Mineral deposits from hard-water
samples or reagents
Greasy samples
Use of calcium hypochlorite
Home-made reagents
Hydrindantin deposits from Expired
TRIONE
Follow the procedure for removing
mineral deposits on Page 7.8
Follow the procedure for removing
Silica deposits on Page 7.8
Replace heated reactor if flushing does
not help
Silica from NaOH backflow onto
column
Use of calcium hypochlorite as the
oxidant in glyphosate determination
Preparing your own reagents with
poor quality chemicals
COMMON CHROMATOGRAPHY PROBLEMS
When having chromatography problems collect 2-3 chromatograms that show the problem. Fax these and most
recent normal one to Pickering Laboratories at (650) 968-0749.
OBSERVED PROBLEM COMMON CAUSE ACTION TO TAKE NOTES
High Background Signal Contaminated Eluant
Bacterial Growth
Fingerprints
Contaminated Reagent(s)
Defective chemicals
Flush HPLC system and Pinnacle PCX
with 80/20 Water/MeOH
Put new eluants on HPLC, make new
reagents
Noisy Baseline Worn pump seal
Detector noise
Chemical contamination
Reagent too old
Check for pattern in the noise.
If the background signal is also
elevated, check for chemical
contamination, or an error in
formulation
Match the frequency of the noise to
one of the pumps.
If the noise is random, check the
detector
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