Deuterium/hydrogen isotope ratio measurement of water and organic samples by continuous-flow isotope ratio mass spectrometry using chromium as the reducing agent in an elemental analyser

A rapid continuous-flow technique for quantitative determination of hydrogen isotope ratios in water and organic materials at natural abundance levels is described. Water and organic samples were reduced in a helium stream at temperatures in excess of 1000 degrees C over chromium metal. delta(2)H per thousand values of water and organic samples were determined by calibration against International Atomic Energy Agency reference materials V-SMOW and SLAP water. The accuracy of the method was demonstrated through the analysis of the intermediate water standard GISP and IAEA water intercomparison materials OH-1, OH-2 and OH-3. Values obtained using this technique compared well with reference values (maximum difference 2.2 per thousand). The precision of water analyses was less than 2.3 per thousand (1 sigma or 1 standard deviation) in all cases. No apparent memory effect was observed when measuring samples at the natural abundance level. The application of the technique to organic molecules and the salts of organic acids was successfully demonstrated by measuring the delta(2)H per thousand values of an n-hexadecane laboratory reference and anhydrous calcium formate versus water calibration materials. Copyright Crown copyright 2001. Reproduced with permission of the Controller of Her Majesty's Stationery Office. Published by John Wiley & Sons, Ltd.