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Trace water vapor determination in corrosive gases by infrared spectroscopy

Technical Report ·
DOI:https://doi.org/10.2172/10181950· OSTI ID:10181950
; ; ;  [1]; ;  [2]
  1. Sandia National Labs., Albuquerque, NM (United States)
  2. New Mexico Univ., Albuquerque, NM (United States). Dept. of Chemistry

To extend the life of gas delivery systems and improve wafer yields, there is a need for an in-line monitor of H{sub 2}O contamination. Goal of this project is to develop such an instrument, based on infrared spectroscopy, that has a detection limit of 30 ppB or better and costs $$50K or less. This year`s work considered the application of Fourier transform infrared (FTIR) spectroscopy to H{sub 2}O detection in N{sub 2} and HCl. Using a modified commercial FTIR spectrometer and a long-path gas cell, a detection limit of about 10 ppB was demonstrated for H{sub 2}O in N{sub 2} and HCl. This includes about a factor of three improvement achieved by applying quantitative multivariate calibration methods to the problem. Absolute calibration of the instrument was established from absorptivities of prominent H{sub 2}O bands between 3600 and 3910 cm{sup {minus}1}. Methods are described to minimize background moisture in the beam path. Spectral region, detector type, resolution, cell type, and path length were optimized. Resolving the narrow H{sub 2}O bands (FWHM {approx} 0.20 cm{sup {minus}1}) is not necessary to achieve optimal sensitivity. In fact, optimal sensitivity is achieved at 2 to 4 cm{sup {minus}1} resolution, allowing the use of an inexpensive interferometer. A much smaller, second generation instrument is described that will have a conservatively estimated detection limit of 1 ppB. Since the present laboratory instrument can be duplicated in its essential parts for about $$90K, it is realistic to project a cost of $50K for the new instrument. An accessory for existing FTIR spectrometers was designed that may be marketed for as little as $10K.

Research Organization:
Sandia National Labs., Albuquerque, NM (United States)
Sponsoring Organization:
USDOE, Washington, DC (United States)
DOE Contract Number:
AC04-94AL85000
OSTI ID:
10181950
Report Number(s):
SAND--93-4026; ON: DE94018496; BR: GB0103012
Country of Publication:
United States
Language:
English