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GC/MS/MS Varian: Autotuning problems!!!

Discussions about GC-MS, LC-MS, LC-FTIR, and other "coupled" analytical techniques.

2 posts Page 1 of 1
Hi everybody

We're having several issues with the GC/MS/MS in our lab. We have a Varian 1200 Quadrupole MS/MS. Initially we had a communication issue between the computer and the MS (I already opened other post about this). We managed to sort this out in the end. We had this issue in the power supply...We measured the volts between two specific test points (TP 2 and TP 27, on communication side). It should be 5 V (or a close value), but the real one was 4.55 V. (Values below 4.65 indicates a problem in the power supply). We managed to re-adjust the voltage in the power board, and the communication was restored. Anyway, a new issue has appeared, since now we're not able to carry out a succesful auto-tune...The instrument passess the coarse tune with no apparent problems! Does anyone have experienced similuar issues with the autotuning? We need some clues, please! Hope anyone who has experienced similar issues will know...

I will detail here the steps we've been following lately + some pics from the software:

1. Run a coarse tune and then autotune. There is a red warning on the readback window as to the 5V. At this time, the detector has not passed the calibration and this autotune was done under a fixed detector voltage. In fact, at first, the peaks were really bad. We even could not see the 18, 28. I kept on doing the autotune, and the results improved.

http://imageshack.us/a/img542/3038/clipimage002pf.jpg

Hardware diagnostics report for Varian Quadrupole Mass Spec

Time: 10:56:56

No errors detected. Proceeding with autotune.

Tune report for Varian Quadrupole Mass Spec

Time: 11:11:04 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (2)

Ionization mode:EI Scan Optimization: Standard GC (Fixed detector)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 18.0 8.691 42.998 0.68 100 27
28.0 27.9 3.550 17.562 0.76 100 37
69.0 69.0 20.213 100.000 0.64 100 107
219.0 219.0 12.250 60.603 0.97 65 226
502.0 502.6 7.134 35.296 4.00 15 126
Warning: the peak is very wide and mass shifted!

(Detector = 1660 V)

Tuning of quad 1 in positive mode had the following error(s):
Problem with fine resolution of m/z 502.0 (Time limit exceeded.)

-----------------------------------------------------------------------------------------------

Tune report for Varian Quadrupole Mass Spec

Time: 11:16:45 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (2)

Ionization mode:EI Scan Optimization: Standard GC (Fixed detector)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 18.0 12.248 78.869 0.68 100 27
28.0 28.0 4.173 26.872 0.80 52 35
69.0 69.0 15.529 100.000 0.75 93 93
219.0 219.0 9.579 61.685 0.97 25 226
502.0 502.4 3.140 20.223 2.67 2 188
Warning: the peak is very wide and mass shifted!

(Detector = 1660 V)

Tuning of quad 3 in positive mode completed.

28 absolute size (mV - EDR on)
- Limit 20.0 - Measured 0.0
- OK!
28/32 Ratio
- Air 3.5:1 - Measured 2.8:1
- OK! - Not indicative of Air
28/18 Ratio
- Limit 1.2:1 - Measured 0.3 :1
- OK!

- No significant leak detected -
- OK –


2. Then the detector has passed the calibration. Using the extended dynamic range of the detector, the autotune gave bad results.


http://imageshack.us/a/img850/2893/clipimage003h.jpg

Hardware diagnostics report for Varian Quadrupole Mass Spec

Time: 11:19:39

No errors detected. Proceeding with autotune.

Tune report for Varian Quadrupole Mass Spec

Time: 11:41:56 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (3)

Ionization mode:EI Scan Optimization: Standard GC (EDR)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 19.0 0.003 53.559 0.68 100 28
Warning: the peak is mass shifted!
28.0 28.9 0.001 16.111 0.88 83 33
Warning: the peak is mass shifted!
69.0 69.6 0.003 47.734 0.69 100 101
Warning: the peak is mass shifted!
219.0 219.0 0.005 100.000 1.68 0 130
Warning: the peak is very wide!
502.0 501.0 0.001 12.649 2.28 16 220
Warning: the peak is very wide and mass shifted!

(Detector = 1560 V)

Tuning of quad 1 in positive mode had the following error(s):
Problem with fine resolution of m/z 502.0 (Time limit exceeded.)
Problem with fine resolution of m/z 219.0 (Time limit exceeded.)
Problem tuning m/z 69.0
Problem tuning m/z 28.0
Problem tuning m/z 18.0

-----------------------------------------------------------------------------------------------

Tune report for Varian Quadrupole Mass Spec

Time: 11:54:49 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (3)

Ionization mode:EI Scan Optimization: Standard GC (EDR)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 18.0 0.006 100.000 0.67 100 27
28.0 28.0 0.002 29.840 0.71 75 39
69.0 69.0 0.003 47.843 0.78 69 88
219.0 218.9 0.002 27.128 0.72 38 303
502.0 502.6 0.001 11.732 4.00 8 126
Warning: the peak is very wide and mass shifted!

(Detector = 1560 V)

Tuning of quad 3 in positive mode completed.

28 absolute size (mV - EDR on)
- Limit 20.0 - Measured 0.0
- OK!
28/32 Ratio
- Air 3.5:1 - Measured 0.0:1
- OK! - Not indicative of Air
28/18 Ratio
- Limit 1.2:1 - Measured 0.0 :1
- OK!

- No significant leak detected -
- OK -


3. But a following autotune tried to improve.


http://imageshack.us/a/img819/1789/clipimage004wv.jpg

Hardware diagnostics report for Varian Quadrupole Mass Spec

Time: 11:57:27

No errors detected. Proceeding with autotune.

Tune report for Varian Quadrupole Mass Spec

Time: 12:20:41 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (4)

Ionization mode:EI Scan Optimization: Standard GC (EDR)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 18.2 0.002 67.355 0.62 96 29
28.0 28.0 0.001 39.577 0.65 71 43
69.0 68.9 0.003 100.000 0.73 92 95
219.0 219.0 0.001 45.948 0.96 32 228
502.0 503.2 0.001 30.810 4.00 11 126
Warning: the peak is very wide and mass shifted!

(Detector = 1560 V)

Tuning of quad 1 in positive mode had the following error(s):
Problem tuning m/z 28.0
Problem tuning m/z 18.0

-----------------------------------------------------------------------------------------------

Tune report for Varian Quadrupole Mass Spec

Time: 12:32:24 Tune file: FC-43 EI (Tuned on 1 Apr 2013) (4)

Ionization mode:EI Scan Optimization: Standard GC (EDR)

Exact Measured Peak Relative Peak Valley Resolution
mass mass height height width
(amu) (amu) (mV) (%) (amu @ 50%) (% of iso) (m/delta-m)
18.0 18.1 0.002 67.243 0.73 57 25
28.0 28.0 0.002 61.757 0.69 95 41
69.0 68.9 0.003 100.000 0.70 85 99
219.0 219.0 0.001 37.811 0.71 37 307
502.0 503.3 0.001 24.405 4.00 19 126
Warning: the peak is very wide and mass shifted!

(Detector = 1560 V)

Tuning of quad 3 in positive mode had the following error(s):
Problem with coarse resolution of m/z 502.0

28 absolute size (mV - EDR on)
- Limit 20.0 - Measured 0.0
- OK!
28/32 Ratio
- Air 3.5:1 - Measured 7.8:1
- OK! - Not indicative of Air
28/18 Ratio
- Limit 1.2:1 - Measured 0.0 :1
- OK!

- No significant leak detected -
- OK -

4. Then the ion source assembly and the hexapole, and the lens 4 have been cleaned, hoping to improve the response of the instrument. However, the results did not improve, but it is even worse. There were almost no peaks for all of the ions.

http://imageshack.us/a/img819/4435/clipimage005k.jpg
What is the main vacuum reading?
Do you have cal gas in the vial?
Does the system pass electronic diagnostics?
Bruker (and Varian) Engineer happy to give advice on GC, GCMS and LCMS products.
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