Tritium and He isotope
samples are prepared for mass spectrometric measurement by using
two vacuum extraction systems. Typically, we receive two types of
water samples: small volume samples sealed in copper tubes (length:
about 1 m; diameter: about 10 mm; volume: about 40 ml) and large
volume samples collected in 1 l glass bottles.
Eight samples are
connected to a vacuum extraction system held at a pressure of about
10E-6 to 10E-5 mbar. The copper tubes are opened and the water is
expanded into a glass bulb. After quantitative transfer of all gases
from the expansion bulb into a glass ampoule, the ampoule is flame
sealed for storage of the samples. At this point, the water contained
in the glass bulb is completely gas-free and can be flame sealed
for 3He ingrowth from the tritium decay (tritiogenic
3He). After a period of typically about 6 months, the
tritiogenic 3He is extracted from the glass bulbs and
measured mass spectrometrically. If the tritium concentrations of
the samples are very low or if a shorter ingrowth time is desired,
we use a second extraction system designed for larger volumes. In
this system, about 400 grams of water are transferred from the 1
l glass bottles into 1 l glass bulbs. After extraction of all gases
under a vacuum of about 10E-3 mbar (3He extraction efficiency:
>99.999 %), the glass bulbs are flame sealed for tritiogenic
3He buildup during storage in a freezer. The measurement
procedure of the large volume samples is very similar to that used
for small volume samples.
The design and performance
of the two extraction systems used in the L-DEO noble gas laboratory
are similar to those described by Bayer et al. (1989).