Shimadzu GCMS-QP2010 Series, Service Manual, Page: 114 / 168

114
2. Adjustment in the high mass-number range
This instrument incorporates an auto-tuning function that conducts mass-number calibration
at m/z614. Mass-number displacement is rare in the normal range of operation (up to
approximately m/z700.)
However, displacement from the calibration at m/z is possible in the high mass-number
range.
Ensuring accurate calibration in the range m/z700 to m/z1000 requires manual calibration
by injecting a triazine (Tris(perfluoroheptyi)-S-triazine) high-mass-number standard sample
into the column.
Procedure
Instrument conditions
Sample: triazine 1% solution in acetone, ultrasonically mixed
INJ: 250
M
C
COL: 50
M
C (1 min.)-5
M
C /min-100
M
C (1min)-30
M
C /min-250
M
C (10min)
I/F: 250
M
C Ion source: 200
M
C
Column head pressure: 100kPa Total flow rate: 30mL/minute
Splitless injection (1 min. sampling)
Triazine flow time is approximately 3 minutes between minute 11 and minute 15
c Take 1
µ
L triazine sample into a syringe and inject it into INJ. Wipe any sample from
the syringe tip before injecting the sample.
d Monitor m/z771, 886, and 1016 on the Peak Monitor window. Leave the filament off
for the first five minutes after sample injection, turn the filament on, and wait for the
peaks to appear.
e The triazine peak can be seen for the three minutes between minute 11 and minute 15.
Check the mass number (within
C
0.3 mass) and resolution (FWHM resolution 0.1M
max.). Conduct manual compensation, if necessary.
f After making this check, increase the column temperature to 250
M
C to drive out the
triazine. Ten minutes at 250
M
C is insufficient, conduct this process for 1 hour at
250
M
C.
Caution) Traces of the injected triazine may remain in the sample lines and
hinder subsequent analysis. Allow the column to age overnight at
250
M
C before conducting ultramicroanalysis.