6
Analytical Troubleshooting
General Points Regarding Chromatographic Effects
Thermo Scientific
TriPlus RSH User Guide
229
Sample peaks/responses are not
reproducible.
Dirty syringe.
Increase
PstClnSlv1/Slv2
values in method.
Use
PreClnSlv1/Slv2
and
Pre Cln Spl
.
Syringe pressure difference.
Increase
Def Aspirate Delay (
Pull-up Delay)
value.
Vacuum created in sample vial.
Reduce Sample volume in sample vial.
Use Pre Pressure Vial mode.
Highly volatile solvent.
Use gas-tight syringe and sample tray cooling.
Improperly crimped vials.
Check vial cap by attempting to rotate by
hand. Loose caps might cause selective loss of
volatile compounds from the sample. Adjust
crimping tool correctly.
Method Parameters.
Check recommended Method Parameters.The
following parameters are crucial and must be
verified first:
•
Def Aspirate Flow Rate
(Fill Speed)
•
Def Aspirate Delay
(Pull-up Delay)
•
Def Dispense Flow Rate
(Injection
speed)
•
Def Dispense Delay
(Post Inj Delay)
Note that for dedicated cycles, certain
parameters are locked.
Excessive carryover between samples.
Dirty syringe.
Increase
Pst InjSlv1/2
values in method.
Use
PreClnSlv1/Slv2
and
PrClnSpl
.
Check and, if necessary, replace vial septa
from
Wash/Waste
vials.
Inappropriate wash solvent.
Use appropriate wash solvent.
Wash Solvent and Waste vial septa too
tight.
Check if the syringe fills completely when
washing.
If several cleaning cycles are programmed and
many samples are processed, then vacuum in
the Wash Solvent vials and overpressure in the
Waste vials might build up.
Cut away a segment of the solvent and Waste
septa to ensure equalization of pressure.
Wash solvent level too low.
Check the solvent volume in the
Wash Vial
and the syringe needle penetration in the vial.
Solvent level in Waste vial to high.
Check the volume of the solvent in the
Waste
Vial
. Check also the needle penetration into
the waste vial.
The needle must not touch the liquid at all.
Table 96.
General Points Regarding GC Effects - Troubleshooting Guideline (Sheet 2 of 3)
Symptom or Error Message
Possible Cause
Recommended Action
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