Peak area variability in DMSO analysis

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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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slucas Author
2 Answers
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0
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 ?
0
I think first you should lower your Column flow according to your Column ID, and need to check the glass wool in your linear.