The bubbling gas was sampled using the replacement method.
The composition of the gas was analyzed by gas chromatography
techniques using thermal conductivity detectors and molecular
sieve columns with He and Ar as carrier gases for the determination
of He, H2, N2, O2, and CH4. A Porapak Q column with He carrier
gas was used for the separation of CO2. A combined CTR-3 Alltech
column was used for the Ar analysis at room temperature with He
as a carrier gas. Detection limits were 0.001 vol.% for He, H2 and
N2, less than 0.001 vol.% for O2 and Ar, 0.001 vol.% for CO2.
CH4 and CO2 gases isotopes ratios (13C/12C) were determined by
isotope-ratio mass spectrometry MAT-253 using Trace-GC gas
chromatograph at the Sapporo University (Japan). The precisions
of the analyses are 0.1‰ for d13C and 1‰ for 2H.
Tritium determinations were performed using electrolytic
enrichment and subsequent measurement of counting rates;
details of sample preparation for 3H analysis are described by
Goriachev (1997). The standard deviation was 0.3–1.1 TU depending
on the 3H concentration.
The bubbling gas was sampled using the replacement method.The composition of the gas was analyzed by gas chromatographytechniques using thermal conductivity detectors and molecularsieve columns with He and Ar as carrier gases for the determinationof He, H2, N2, O2, and CH4. A Porapak Q column with He carriergas was used for the separation of CO2. A combined CTR-3 Alltechcolumn was used for the Ar analysis at room temperature with Heas a carrier gas. Detection limits were 0.001 vol.% for He, H2 andN2, less than 0.001 vol.% for O2 and Ar, 0.001 vol.% for CO2.CH4 and CO2 gases isotopes ratios (13C/12C) were determined byisotope-ratio mass spectrometry MAT-253 using Trace-GC gaschromatograph at the Sapporo University (Japan). The precisionsof the analyses are 0.1‰ for d13C and 1‰ for 2H.Tritium determinations were performed using electrolyticenrichment and subsequent measurement of counting rates;details of sample preparation for 3H analysis are described byGoriachev (1997). The standard deviation was 0.3–1.1 TU dependingon the 3H concentration.
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