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5 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.

103 views
Avatar youhana Hosny 5 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 5 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.
Avatar Pathan Sohil 11h ago

I think first you should lower your Column flow according to your Column ID, and need to check the glass wool in your linear.

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Author avatar
22 d ago

I was running a sequence of product samples and decided to inject a methanol blank in between. To my surprise, I saw unexpected peaks—some of which matched my analytes.

Gas Chromatography (GC) gc
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Avatar youhana Hosny 17 d ago

good info :)

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Author avatar
22 d ago

In a long GC run (about 30 samples), I noticed that retention times started shifting gradually. Early samples were fine, but later ones drifted.

Gas Chromatography (GC) gc
91 views
Avatar youhana Hosny 17 d ago

good info :)

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Avatar youhana Hosny 17 d ago

:)

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