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4 d ago

Hello,
I am running an impurity analysis method for DMSO with the following parameters:

FID Temperature: 250 °C
Injector Temperature: 250 °C
Column: Agilent DB-624
Flow: 5 mL/min (Hydrogen)
Initial temp: 100 °C, hold for 2 min
Ramp from 100 to 200 °C at 10 °C/min
Final temp: 200 °C, hold for 3 min
Injection volume: 0.5 microliters
Injection syringe volume: 1 microliter (auto-injector)
Split: 1:10
Liner: Ultrainert 5190-2295
FID flows:
• Hydrogen: 35 mL/min
• Air: 400 mL/min
• Nitrogen: 35 mL/min

I’m having serious issues with area repeatability when injecting the same vial 6 times in a row. I’m getting %RSD values around 9%, and my requirement is ≤ 5.0%
I’ve tried all kinds of adjustments—changing injection speeds, adding a 3-second viscosity delay… but nothing seems to solve the issue.

Can you help me?

Thank you very much.

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Avatar youhana Hosny 4 d ago

you have to exclude first that the problem is not related to the instrument itself.
is the instrument calibrated?
have you tried another method using the same instrument and the results are good ?

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slucas 4 d ago
Yes, the instrument is fully calibrated and other methods report good results. The only remarkable thing is that this method is the only one I have that use hydrogen as carrier gas.