Tritium from Deuterium Lecture Bottle? (Edit: Misattribution of D3+ Factor)
Posted: Tue Jul 23, 2019 7:49 pm
This morning, while I was evacuating my fusor chamber and differentially pumping the RGA for high-pressure measurement, I cracked the needle valve on the still-pressurized deuterium gas line and immediately noticed a large peak at m/z = 6. The pressure in the main chamber was around 10mtorr and that in the RGA chamber was ~1e-5torr, and there were two peaks of roughly equal height (~9e-6) at m/z = 4 (deuterium) and m/z = 6. In less that ten seconds the peak at m/z = 6 shrank to nothing (literally nothing down to even e-11) and the one at m/z = 4 increased to roughly the sum of two initial partial pressures. I guarantee it was no instrumentation fluke as the RGA has been 100% reliable and the peak corresponded perfectly with opening the valve. When no deuterium was in the line nothing happened, so that rules out anything in the construction (drierite, hydrocarbon valve grease, stainless, etc; all are way above m/z = 6). Something new was definitely there at m/z = 6.
I'm reminded of this conversation had on the forums way back in 2004: http://fusor.net/board/viewtopic.php?f= ... ium#p36510. Frank Sans mentions that the ultra-high-purity deuterium he obtained had as much as 0.1mCi/L of tritium. Could this be the source? Some math (order of magnitude, nothing ultra-precise):
0.1mCi tritium (s.a. = 9650Ci/g) corresponds to 1.04-8g, or, at STP, 3.87e-8L. This corresponds to 1.29ppb in a 50L lecture bottle. The deuterium line is 1m of 4.5mm ID stainless tubing at roughly atmosphere, so we have V = 0.0159L of deuterium and thus 1.23e-11L (STP) of tritium. The total chamber volume is ~1.44L, so the expected partial pressure is 760torr * 1.23e-11L/1.44L = 6.5e-9torr. This is easily measurable by the RGA but 1000x the observed value. My deuterium is not UHP, but 99.8% or 99.9% if I remember correctly, so it may be possible that more tritium found it's way past the refinement steps. So... maybe?
All the RGA spectrum tables I have found online yielded nothing but doubly ionized 12C at m/z = 6 (http://ytionline.com/technical-informat ... ion-guide/) which is in no way the culprit. Since the peak disappeared so quickly and I was rushing to get a picture I did not measure the roughing pump exhaust with a Geiger counter.
Thoughts? I'm skeptical, but those far more experienced may have better explanations. The only other isotope would be 3He, but like I mentioned this happened only with deuterium in the line. While I guess 3He in the deuterium is possible, I just don't know. My neutron detector isn't exactly leaking...
The spectrum is clear... Apologies for the poor quality.
I'm reminded of this conversation had on the forums way back in 2004: http://fusor.net/board/viewtopic.php?f= ... ium#p36510. Frank Sans mentions that the ultra-high-purity deuterium he obtained had as much as 0.1mCi/L of tritium. Could this be the source? Some math (order of magnitude, nothing ultra-precise):
0.1mCi tritium (s.a. = 9650Ci/g) corresponds to 1.04-8g, or, at STP, 3.87e-8L. This corresponds to 1.29ppb in a 50L lecture bottle. The deuterium line is 1m of 4.5mm ID stainless tubing at roughly atmosphere, so we have V = 0.0159L of deuterium and thus 1.23e-11L (STP) of tritium. The total chamber volume is ~1.44L, so the expected partial pressure is 760torr * 1.23e-11L/1.44L = 6.5e-9torr. This is easily measurable by the RGA but 1000x the observed value. My deuterium is not UHP, but 99.8% or 99.9% if I remember correctly, so it may be possible that more tritium found it's way past the refinement steps. So... maybe?
All the RGA spectrum tables I have found online yielded nothing but doubly ionized 12C at m/z = 6 (http://ytionline.com/technical-informat ... ion-guide/) which is in no way the culprit. Since the peak disappeared so quickly and I was rushing to get a picture I did not measure the roughing pump exhaust with a Geiger counter.
Thoughts? I'm skeptical, but those far more experienced may have better explanations. The only other isotope would be 3He, but like I mentioned this happened only with deuterium in the line. While I guess 3He in the deuterium is possible, I just don't know. My neutron detector isn't exactly leaking...
The spectrum is clear... Apologies for the poor quality.