Chromatography Forum

in my varian saturn 2200 ms unit when i start to run a sample list it indicates a fault and says mass calibratioin required. Then when i press the reset the fault will change to nofault state and samples start to run. I did several mass calibrations but the problem remains. in the electron multiplier settings it says peak threshold not met and also it says final setting is marginal in electron multiplier tuning. Please help me to solve the problem

First optimise rf tune under Manual control section.Then you perform mass and electron multiplier autotune.

Hi thanks david
I did the rf optimization and the counts were around 800 and I couldn't go below that level. Should i be able to go below that level to get rid of this problem.

Your rf setting ok.What is your EM voltage.You have to also ensure that the FC-43 calibration mix in the glass bottle.

I am not sure which voltage you reffering as EM voltage. So I have attached the results I am getting after the EM tuning which includes all upper and lower limits as well. Below is the results of EM tuning.
Electron Multiplier: Started
Electron Multiplier: Offset Determined (Offset: 1 Count(s))
Electron Multiplier: Pre-Adjustment Successful (EM Voltage: 1400)
Electron Multiplier: Low Voltage End Found (EM Voltage: 1300)
Electron Multiplier: High Voltage Start Found (EM Voltage: 1500)
Electron Multiplier: Space Charge Adjusted (Target: 20000, Val/Iso: 0.25)
Electron Multiplier: Peak Threshold Not Met (Inten: 168 counts)
Electron Multiplier: 10^5 Gain setting is OK (EM Voltage: 1400)
Electron Multiplier: Final Gain setting is Marginal (EM Voltage: 1700)
Electron Multiplier: Completed

I hope this details would help you.
Also I have recently changed the cal gas mixture as well
Thank you

Hi Shanika
from your log I can see an EM problem: "final setting is marginal"
So, because your EM voltage is relatively low, may be a ion trap cleaning problem or something related to calgas setting.

Have you checked calgas flow? There is an adjustment procedure.
And if you can post all log from autotune (em and mass cal)
Hope this help

hi
hope dani is right. it may be your ion trap is not clean.
you can verifies on manual control modes in control and status.
click on EM,Filament & rf icon and verified mass abundance in trap if trap in contaminated it show high or lower mass in profile spectrum.
during verification you assure your cal gas is off.

and also post your full auto tune report so we can understand better.

Thank you danny and david,
I also did the cal gas adjustment and made the cal gas pressure to the middle range. Any how I will try to arrange a ion trap cleaning
Below are the full details I got from the auto tunning. Hope this will help you to get an idea about the problems. Again thanks soo much for the great help ..
10:05:04 Auto Tune: Started
10:05:05 Air/Water Check: Started
10:05:31 Air Check: Acceptable Level Found (28 Width: 0.6 m/z)
10:05:32 Water Check: Acceptable Level Found (19/18 Ratio: 8.5 %)
10:05:32 Air/Water Check: Completed - No Problems Found
10:05:33 Integrator Zero Set: Started
10:05:41 Integrator Zero Set: Setting is OK (Setting: 130, Average Counts: 0.50)
10:05:42 Integrator Zero Set: Completed
10:05:42 Electron Multiplier: Started
10:05:44 Electron Multiplier: Offset Determined (Offset: 1 Count(s))
10:05:59 Electron Multiplier: Pre-Adjustment Successful (EM Voltage: 1400)
10:09:54 Electron Multiplier: Low Voltage End Found (EM Voltage: 1300)
10:11:03 Electron Multiplier: High Voltage Start Found (EM Voltage: 1500)
10:11:12 Electron Multiplier: Space Charge Adjusted (Target: 20000, Val/Iso: 0.25)
10:11:52 Electron Multiplier: Peak Threshold Not Met (Inten: 168 counts)
10:11:53 Electron Multiplier: 10^5 Gain setting is OK (EM Voltage: 1400)
10:11:53 Electron Multiplier: Final Gain setting is Marginal (EM Voltage: 1700)
10:11:54 Electron Multiplier: Completed
10:11:54 RF Full Scale Adj: Started
10:12:02 RF Full Scale Adj: Centered on Mass 69 at 69.91 (Setting: 60)
10:12:07 RF Full Scale Adj: Centered on Mass 414 at 416.19 (Setting: 33)
10:12:11 RF Full Scale Adj: Centered on Mass 614 at 642.55 (Setting: 1)
10:12:12 RF Full Scale Adj: Setting is High (Setting: 1, Mass: 614, Apex: 643.
10:12:12 RF Full Scale Adj: Completed
10:12:13 Multi-Point Mass Cal: Started
10:12:19 Multi-Point Mass Cal: Found Calibration Mass 28 at 27.63
10:12:26 Multi-Point Mass Cal: Found Calibration Mass 69 at 68.25
10:12:31 Multi-Point Mass Cal: Found Calibration Mass 131 at 129.79
10:12:42 Multi-Point Mass Cal: Found Calibration Mass 264 at 262.07
10:13:44 Multi-Point Mass Cal: Found Calibration Mass 502 at 499.03
10:14:11 Multi-Point Mass Cal: Found Calibration Mass 614 at 622.54
10:14:12 Multi-Point Mass Cal: Calibration is OK (Slope: 6.243, Std Dev: 0.063)
10:14:12 Multi-Point Mass Cal: Completed
10:14:13 Trap Function Calib: Started
10:14:16 Trap Function Calib: Calibrating at Mass 69
10:15:21 Trap Function Calib: Calibrating at Mass 131
10:15:22 Trap Function Calib: No Reference Peak Located
10:15:22 Trap Function Calib: Failed
10:15:23 Auto Tune: Terminated
10:28:20 Auto Tune: Started
10:28:21 RF Full Scale Adj: Started
10:28:30 RF Full Scale Adj: Centered on Mass 69 at 69.92 (Setting: 59)
10:28:35 RF Full Scale Adj: Centered on Mass 414 at 416.05 (Setting: 34)
10:28:39 RF Full Scale Adj: Centered on Mass 614 at 643.67 (Setting: 1)
10:28:40 RF Full Scale Adj: Setting is High (Setting: 1, Mass: 614, Apex: 644.0)
10:28:40 RF Full Scale Adj: Completed
10:28:41 Multi-Point Mass Cal: Started
10:28:47 Multi-Point Mass Cal: Found Calibration Mass 28 at 27.63
10:28:55 Multi-Point Mass Cal: Found Calibration Mass 69 at 68.25
10:29:00 Multi-Point Mass Cal: Found Calibration Mass 131 at 129.79
10:29:11 Multi-Point Mass Cal: Found Calibration Mass 264 at 262.08
10:29:30 Multi-Point Mass Cal: Found Calibration Mass 414 at 411.42
10:30:13 Multi-Point Mass Cal: Found Calibration Mass 502 at 498.98
10:30:40 Multi-Point Mass Cal: Found Calibration Mass 614 at 622.62
10:30:41 Multi-Point Mass Cal: Calibration is OK (Slope: 6.243, Std Dev: 0.063)
10:30:41 Multi-Point Mass Cal: Completed
10:30:42 Auto Tune: Completed
10:31:41 Auto Tune: Started
10:31:42 Trap Function Calib: Started
10:31:47 Trap Function Calib: Calibrating at Mass 69
10:32:44 Trap Function Calib: Calibrating at Mass 131
10:33:46 Trap Function Calib: Mass 69 Calibrated (Freq: 262.800 kHz)
10:33:46 Trap Function Calib: Mass 131 Calibrated (Freq: 259.900 kHz)
10:33:47 Trap Function Calib: Completed
10:33:47 Auto Tune: Completed

IMHO is a trap cleanliness problem. Your system can't locate a high mass

"10:12:11 RF Full Scale Adj: Centered on Mass 614 at 642.55 (Setting: 1)
10:12:12 RF Full Scale Adj: Setting is High (Setting: 1, Mass: 614, Apex: 643"

so mass adj fail.

Try a long bakeout or -better - a full ion trap cleaning procedure

Thanks dani ,
I'll go for bake out and if couldn't solve will try a cleaning as well and will update the state

Reference data after reinstalling and cleaning.

For the cleaning i just used a neutral soap, water, IPA, ultrasonic.
When reinstalling the coloumn make sure it sticks out 3mm.

Bakeout for 12h

First i adjusted the cal gas flow in the "manual control"
After that, just a general Autotune and it worked just fine for my purposes. A better cleaning could result in a better tuning, but could also make it worse if polished to much.



09:24:37 Auto Tune: Started
09:24:37 Air/Water Check: Started
09:25:32 Air Check: Acceptable Level Found (28 Width: 0.8 m/z)
09:25:32 Water Check: Acceptable Level Found (19/18 Ratio: 0.2 %)
09:25:32 Air/Water Check: Completed - No Problems Found
09:25:32 Integrator Zero Set: Started
09:25:44 Integrator Zero Set: Setting is OK (Setting: 110, Average Counts: 0.52)
09:25:44 Integrator Zero Set: Completed
09:25:44 Electron Multiplier: Started
09:25:46 Electron Multiplier: Offset Determined (Offset: 1 Count(s))
09:25:57 Electron Multiplier: Pre-Adjustment Successful (EM Voltage: 1200)
09:32:05 Electron Multiplier: Low Voltage End Found (EM Voltage: 1200)
09:33:47 Electron Multiplier: High Voltage Start Found (EM Voltage: 1500)
09:33:56 Electron Multiplier: 10^5 Gain setting is OK (EM Voltage: 1350)
09:33:56 Electron Multiplier: Final Gain setting is OK (EM Voltage: 1350)
09:33:56 Electron Multiplier: Completed
09:33:56 RF Full Scale Adj: Started
09:34:00 RF Full Scale Adj: Centered on Mass 69 at 69.09 (Setting: 122)
09:34:03 RF Full Scale Adj: Centered on Mass 414 at 415.05 (Setting: 109)
09:34:06 RF Full Scale Adj: Centered on Mass 614 at 614.11 (Setting: 109)
09:34:06 RF Full Scale Adj: Setting is OK (Setting: 109, Mass: 614, Apex: 614.1)
09:34:07 RF Full Scale Adj: Completed
09:34:07 Multi-Point Mass Cal: Started
09:34:08 Multi-Point Mass Cal: Found Calibration Mass 28 at 28.88
09:34:14 Multi-Point Mass Cal: Found Calibration Mass 69 at 68.80
09:34:20 Multi-Point Mass Cal: Found Calibration Mass 131 at 130.73
09:34:35 Multi-Point Mass Cal: Found Calibration Mass 264 at 263.76
09:34:59 Multi-Point Mass Cal: Found Calibration Mass 414 at 413.96
09:35:26 Multi-Point Mass Cal: Found Calibration Mass 464 at 463.96
09:35:56 Multi-Point Mass Cal: Found Calibration Mass 502 at 501.83
09:36:32 Multi-Point Mass Cal: Found Calibration Mass 614 at 614.10
09:36:32 Multi-Point Mass Cal: Calibration is OK (Slope: 6.279, Std Dev: 0.020)
09:36:32 Multi-Point Mass Cal: Completed
09:36:32 Trap Function Calib: Started
09:36:36 Trap Function Calib: Calibrating at Mass 69
09:36:47 Trap Function Calib: Expanding Search Window to 240.00 - 270.00 kHz
09:38:49 Trap Function Calib: Calibrating at Mass 131
09:38:59 Trap Function Calib: Expanding Search Window to 240.00 - 270.00 kHz
09:40:32 Trap Function Calib: Mass 69 Calibrated (Freq: 260.300 kHz)
09:40:32 Trap Function Calib: Mass 131 Calibrated (Freq: 258.000 kHz)
09:40:32 Trap Function Calib: Completed
09:40:32 Auto Tune: Completed