Novel silver-tubing method for quantitative introduction of water into high-temperature conversion systems for stable...

A new method to seal water in silver tubes for use in a TC/EA (thermal conversion/elemental analyzer) reduction unit using a semi-automated sealing apparatus can yield reproducibilities (1 standard deviation) of delta(2)H and delta(18)O measurements of 1.0 per thousand and 0.06 per thousand, respectively. These silver tubes containing reference waters may be preferred for the calibration of H- and O-bearing materials analyzed with a TC/EA reduction unit. The new sealing apparatus employs a computer-controlled stepping motor to produce silver tubes identical in length. The reproducibility of the mass of water sealed in tubes (in a range of 200-400 microg) can be as good as 1%. Approximately 99% of the sealed silver tubes are satisfactory (leak free). Although silver tubes sealed with reference waters are robust and can be shaken or heated to 110 degrees C with no loss of integrity, they should not be frozen because the expansion during the phase transition of water to ice will break the cold seals and all the water will be lost. The tubes should be shipped in insulated containers. This new method eliminates air inclusions and isotopic fractionation of water associated with the loading of water into capsules using a syringe. The method is also more than an order of magnitude faster than preparing water samples in ordinary Ag capsules. Nevertheless, some laboratories may prefer loading water into silver capsules because expensive equipment is not needed, but users of this method are cautioned to apply the necessary corrections for evaporation, back exchange with laboratory atmospheric moisture, and blanks.