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SF6 for dummies

by Yama Tomonaga

Extraction line

T1-T4: empty cold traps cooled to -196°C using liquid nitrogen


V1, V2: separate extraction line from pumping line
V3-V6: divide extraction line
C: capillary prevents back-diffusion of the extracted gases
R: standard reservoir. Calibration: 0.1 ppm +/- 2% SF6 + 1.7 ppm +/- 1.1% CFC-12 dilluted in N2
99.9%, SF6 cc~20pptV, CFC-12 cc~30ppbV
DR: drying column: ¼ AgNO3 powder, ¾ molecular sieve 3A (protects GC from H2O vapour and H2S
that may interfere with SF6 peak)
VAC: rotary vacuum pump
P: Pirani
GC: gas chromatograph
ECD: electron capture detector kept at 350°C

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.

Connecting the sample to the line


Check that V1+V3 are closed. Connect the bottle to the line. If you think that the
bottle is now air-tight sealed to the line, then close V2+V6 and open V1 to evacuate
the air contained in the extraction vessel. You will hear the pump working well. When
the noise from the pump decreases, open V6+V2 and check the pressure.

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

Connect membrane pump to SF6 line


- MacGC in Mac at CFC line
- All valves closed, online, OP 19
- At the and of the day make the opposite

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