New to GC-FID

Hello,

I’m new to GC machine and I have some issues. We have GC-FID 7890A and using ChemStation G1701EA E.02.01.1177.

Method:

Method: inlet: 250°C, Split: 1:50 with a column: HP-Plot/Q (19095P-QO4) 30m x 0.530mm

Helium is carrier gas

Oven starts at 100°C with a hold time of 0.5min, goes to 200°C in 3min. I also tried isothermal at 150°C

Detector is at 350°C

Sample: 0.1 – 1 µl methanol (tried mixing with heptane as well )

 

First, the GC software (which I believe only control the GC machine) shows me an unusual plot whenever I run a test (Test plot) as shown in image_1. I see those almost consistent peaks all the time whenever I run a sample (in this case methanol) and even when I have no sample!!. I don’t think those peaks are related to the retention time of my sample at all.

When I tried to look at the data using “Data Analysis” software, I was able to see the response vs retention time, but again I also have a problem here. Every time I inject the sample, I’m only seeing noise. Today, I was luck to inject methanol ~1 µl using a syringe and got a peak at retention time ~ 1.2 mint as shown in image_3. After that, every time I inject the sample, I’m only getting noise (image_4).

I tried to change some of the parameters as follows:

Sample volume : 1 -5 µl (tried ethanol, methanol)

Injection temperature: 250 °C split mode (varied split ratio from 2:1 all the way to 50:1)

Overn temperature: 50 – 150 °C isothermal (tried to vary temperature from 50 to 150 °C )

Detector temperature: 350 °C (kept constant )

I don’t understand why I got one good data set (image_3) after that regardless of what I did, all what I’m getting is just noise.  If you could provide some guidance, I would really apricate it.

Parents
  • Also, the machine was shut down for more than 5 years and now I’m working on getting it up and running. During the shutdown, the column was left in the oven (ends were not sealed) with no gas flow of any kind. Upon start up, I cleaned the FID and conditioned the column (also, I trimmed ~10 cm of the column ends). I cleaned and maintained the inlet port as well (replaced the injection septum, O-ring, liner. I checked for leakage and then I lit the FID with no issues.

Reply
  • Also, the machine was shut down for more than 5 years and now I’m working on getting it up and running. During the shutdown, the column was left in the oven (ends were not sealed) with no gas flow of any kind. Upon start up, I cleaned the FID and conditioned the column (also, I trimmed ~10 cm of the column ends). I cleaned and maintained the inlet port as well (replaced the injection septum, O-ring, liner. I checked for leakage and then I lit the FID with no issues.

Children
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