GCMS

Wed, 06/05/2013 - 10:47 -- sewm02

GCMS

 

Running a Single Sample

1.) Place GC-MS vials into the sample chamber, starting in the first row #1

2.) Open the Real-Time Analysis Icon (when prompted for password: Username = Admin, and password blank. Select OK)

3.) If starting new method: Click File→ New Method File (name your method file and click OK)

4.) If using previously prepared method: Click File → Load Method File (Select your method and click OK)

5.) Click Method→ Instrument Parameters

6.) Under Sampler Tab (Change ONLY the Viscosity Composition for a VISCOUS SAMPLE from 0.2 sec. to 1.0 sec.) → Click Advanced

  • a. Set pumping times = 5
  • b. Set injection port dwell time = 0.3 sec.
  • c. Set terminal air gap = No
  • d. Plunger washing speed = high.
  • e. Washing volume set = 8 μL
  • f. Syringe suction position = 0 mm for liquid injections (This value will be set higher for head space sampling consult Jim Weekley for head space sampling settings.)
  • g. Syringe injection position = 0 mm
  • h. Solvent selection = any of the settings as long as you have solvent in the sample rack for the vial you have selected.

7.) Click OK

8.) Click on GC Tab (set up GC parameters)

9.) Under MS Tab (set up MS parameters)

10.) Click File→ Save Method File As…..

11.) Click the TOP icon on the left hand side of the screen

12.) Click the TUNING icon on the left hand side of the screen

13.) Click the START AUTO TUNING icon on the left hand side of the screen

14.) Click File→ Save Tuning File As→ Today’s Date→ Close Tuning Window

15.) Take out rinsing rack and fill the vial to the far right with a solvent, preferably one used for the experiment. Push rinsing rack back into place and press the RESET button the front of the auto-injector

16.) At the top of the screen under the GCMS Real Time Analysis window……

17.) Click Acquisition→ download initial parameters

18.) On the left hand side of the screen click the SAMPLE LOGIN icon and fill in the information **Be sure to change the Tuning File to Today’s Date

19.) On the left hand side of the screen click the STAND BY icon and click “Yes”

20.) On the left hand side of the screen click the START icon

21.) Click on the GCMS Postrun Analysis icon on the desktop to view the chromatograms

Running a Batch

1.) Follow steps (1)-(14) above

2.) Click the TOP icon on the left hand side of the screen

3.) Click the BATCH PROCESSING icon on the left hand side of the screen

4.) Click the WIZARD icon on the left hand side of the screen

    a. click the “New” selection and the “Line 1” selection
    b. click what you are analyzing (unknown only, standard only, or both)
    c. Load the method file that was set up
    d. change the average count to however many samples are being analyzed
    e. check mark the “auto-increment” box (if its not already check marked)
    f. click “next”
    g. write in the File Name and then click “done”

5.) In your batch processing table…..

    a. write in the names of the samples and change the Vial # as to where each sample is in the sample chamber
    b. go all the way to the right of the table and under the TUNING tab, open today’s TUNING FILE for each sample

6.) Click the START button on the left hand side of the screen

7.) Click on the GCMS Postrun Analysis icon on the desktop to view the chromatograms

Shutting Down

1.) In the GCMS Real Time Analysis window click on TOOLS on the task bar → Daily Shutdown→Shutdown

2.) DO NOT TURN THE INSTRUMENT OFF!!!

(This idiot sheet was taken from Instrumental Analysis Chem 2215-01 Spring 2009)

Added by Larisa Lynch

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