Isotopic hydrogen analysis via conventional and surface-enhanced fiber optic Raman spectroscopy

Abstract

This report describes laboratory development and process plant applications of Raman spectroscopy for detection of hydrogen isotopes in the Tritium Facilities at the Savannah River Site (SRS), a U.S. Department of Energy complex. Raman spectroscopy provides a lower-cost, in situ alternative to mass spectrometry techniques currently employed at SRS. Using conventional Raman and fiber optics, we have measured, in the production facility glove boxes, process mixtures of protium and deuterium at various compositions and total pressures ranging from 1000 -4000 torr, with detection limits ranging from 1-2% for as low as 3-second integration times. We are currently investigating fabrication techniques for SERS surfaces in order to measure trace (0.01-0.1%) amounts of one isotope in the presence of the other. These efforts have concentrated on surfaces containing palladium, which promotes hydrogen dissociation and forms metal hydride bonds, essentially providing a chemical enhancement mechanism.

Geological mechanisms of the accumulation of coalbed methane induced by hydrothermal fluids in the western Guizhou and eastern Yunnan regions

“…All the samples were first ground to 0.2-0.5 mm and both sides were polished under preparation temperatures below 80℃. The measurements were made using the Laser Raman Spectroscopic Analysis Method described by Irmer, 2002 andLascola, 2004. We used a LABHRVIS LABRAM HR800 Micro Laser Raman Spectrometer manufactured in France, which is capable of nondestructive analysis.…”

Dynamic Raman spectroscopy of hydrogen isotopomer mixtures in-line at TILO

“…More "exotic" studies involving Raman spectroscopy of hydrogen isotopomers have been reported sporadically between the late 1970s and the present day. For example, Daigneault et al investigated a means for measuring the partial pressure of deuterium in fusion targets [15], and quite recently Lascola et al applied the technique of Surface Enhanced Raman Spectroscopy (SERS) to isotopic hydrogen analysis of adsorbates on surfaces [16]. While an intriguing approach, in principle, the geometry of SERS in the gas phase only works at relatively high pressures, and does look unsuitable for the low-pressure, fast-flow conditions encountered in our KATRIN set-up.…”