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Culture Documents
by Yama Tomonaga
Extraction line
Facts
SF6 – 0.42 min retention time of peak.
CFC-12 – 1.4 min retention time.
Detection limit: 0.07 fmol/kg SF6, 2x10-15 mol/kg CFC-12.
Getting started
Check if the GC is more or less clean (overnight heating up to 300°C). Set the GC to
40°C (holding the button “SB & ISO1”, type the temperature with the keypad and
confirm with “enter”).
Check if you have enough liquid N2 in the big container (the one you cannot hold
over your head). If that’s the case, then mount T4 and refill it with LN.
Bring the rotary vacuum pump back to life (put the power cable in the appropriate
plug).
Turn on the computer. Double click the “Wccman” link on the Desktop.
Pump the line: close (CL) V1 and V3, open (OP) V6, V5, V4 and V2. Check the
pressure on channel B4: if it reaches the 5x10-2 mbar, then you are ready to attach
your sample to the line.
Standard
- CL V1, V2 (pumps), LN to T4 (if needed)
- CL V3 (separate extraction vessel)
- LN to T3 (liquid) (P ~ 5E-3?)
- LN to T2 (liquid)
- Check: GC to 40°C and ~5-8 kHz?
- Check: V7 & V8 closed? (with torque key)
- OP V8 (standard bottle)
- Wait 10” and update laboratory journal
- CL V8 (standard bottle)
- OP V7 (standard in line!)
- Wait 10’
- CL V7 (isolate bottle volume from extraction line)
- VB1 from “Open” to “Close” (this closes trap T2)
- H2O to T2 (get gases back to gaseous form)
- Prepare computer program to measure: activate menu “Run” with mouse
- VB2 from “Load” to “Inject” (gas injected to GC)
- Start measurement: press “S”
- Wait ~6’ (until measurement done)
- VB2 back to “Load” position
- VB1 back to “Open” position
- Pump out extraction line
- Evaluate measurement
Sample
- Check: OP V1, V2, V3, V4, V5, V6; CL V7, V8; VB1 = “Open”; VB2 = “Load”
- Check: P ~4E-2 mbar (P <1E-1 mbar: line is pumped)
- LN to T4 (if needed)
- CL V1, V2 (pumps)
- LN to T3, T2, T1
- Check: P ~5E-3 mbar
- OP SC, move ½ of sample over TU in EX
- Shake SC+TU+EX for 8’
- CL V3
- Start countdown: 10’00” – refill LN to T1, T2, T3 – close and remove bottle
sample – pump head vessel with membrane pump and heat it with “hair dryer”
- @ 08’30”: CL V4, H2O to T1 (P increases)
- @ 00’00”: CL V5, remove H2O from T1
- VB1 to “Close” (close trap circulation), H2O to T2
- GC to 40°C?
- Prepare computer program to measure (activate menu “Run” with mouse)
- VB2 to “Inject” (gas injected to GC)
- Start measurement: press “S”
- Wait ~6’ (until measurement done)
- VB2 back to “Load” position
- VB1 back to “Open” position (open trap circulation)
- Start pumping line as follows:
- T1: remove, dry and mount
- CL V6; OP V2, V4
- Wait: until air is evacuated (hear the sound of the pump decreasing)
- OP V6, V5
- Remove LN from T3 and heat with “hair dryer”
- Warm GC for 30’ with 300°C (holding “SB & ISO1”, type “300” and hit the
enter button)
- Check: CL V1, V3
- Change sample
- CL V2, V6 (isolate purification line)
- OP V1
- OP V2, V3, V6
- Dryer to DR (until P ok)
- After 30’ cool GC (SB &ISO1, 40, enter button), open GC door, frequency
down to ~5-8 kHz
- Check: GC temperature, if OK close GC door
- Restart
STOP
- Vacuum in the system
- CL all pumps and valves
- Shut down oil pump and remove the trap from LN bottle and open and clean
the trap if necessary
- Warm GC to 300 °C