Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry

Parkison, Adam J.; Nelson, Andrew Thomas

doi:10.1016/j.measurement.2015.11.043

Title: Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry

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Abstract

An analytical technique is presented with the goal of measuring reaction kinetics during steam oxidation reactions for three cases in which obtaining kinetics information often requires a prohibitive amount of time and cost. The technique presented relies on coupling thermogravimetric analysis (TGA) with a quantitative hydrogen measurement technique using quadrupole mass spectrometry (QMS). The first case considered is in differentiating between the kinetics of steam oxidation reactions and those for simultaneously reacting gaseous impurities such as nitrogen or oxygen. The second case allows one to independently measure the kinetics of oxide and hydride formation for systems in which both of these reactions are known to take place during steam oxidation. The third case deals with measuring the kinetics of formation for competing volatile and non-volatile oxides during certain steam oxidation reactions. In order to meet the requirements of the coupled technique, a methodology is presented which attempts to provide quantitative measurement of hydrogen generation using QMS in the presence of an interfering fragmentation species, namely water vapor. This is achieved such that all calibrations and corrections are performed during the TGA baseline and steam oxidation programs, making system operation virtually identical to standard TGA. Benchmarking results showed a relative errormore »« less

Authors:

Parkison, Adam J. ^[1];

^[1]

Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Publication Date:: Mon Jan 11 00:00:00 EST 2016

Research Org.:: Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Sponsoring Org.:: USDOE

OSTI Identifier:: 1312564

Alternate Identifier(s):: OSTI ID: 1344131

Report Number(s):: LA-UR-14-27905
Journal ID: ISSN 0263-2241

Grant/Contract Number:: AC52-06NA25396

Resource Type:: Accepted Manuscript

Journal Name:: Measurement

Additional Journal Information:: Journal Volume: 82; Journal Issue: C; Journal ID: ISSN 0263-2241

Publisher:: Elsevier

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; material science; steam; oxidation; hydrogen; QMS; nuclear; cladding

Citation Formats


                    Parkison, Adam J., and Nelson, Andrew Thomas. Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry.  United States: N. p., 2016. 
Web.  doi:10.1016/j.measurement.2015.11.043.

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                    Parkison, Adam J., & Nelson, Andrew Thomas. Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry.  United States.  https://doi.org/10.1016/j.measurement.2015.11.043

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                    Parkison, Adam J., and Nelson, Andrew Thomas. Mon .  
"Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry".  United States.  https://doi.org/10.1016/j.measurement.2015.11.043.  https://www.osti.gov/servlets/purl/1312564.

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@article{osti_1312564,

  title        = {Hydrogen measurement during steam oxidation using coupled thermogravimetric analysis and quadrupole mass spectrometry},

  author       = {Parkison, Adam J. and Nelson, Andrew Thomas},

  abstractNote = {An analytical technique is presented with the goal of measuring reaction kinetics during steam oxidation reactions for three cases in which obtaining kinetics information often requires a prohibitive amount of time and cost. The technique presented relies on coupling thermogravimetric analysis (TGA) with a quantitative hydrogen measurement technique using quadrupole mass spectrometry (QMS). The first case considered is in differentiating between the kinetics of steam oxidation reactions and those for simultaneously reacting gaseous impurities such as nitrogen or oxygen. The second case allows one to independently measure the kinetics of oxide and hydride formation for systems in which both of these reactions are known to take place during steam oxidation. The third case deals with measuring the kinetics of formation for competing volatile and non-volatile oxides during certain steam oxidation reactions. In order to meet the requirements of the coupled technique, a methodology is presented which attempts to provide quantitative measurement of hydrogen generation using QMS in the presence of an interfering fragmentation species, namely water vapor. This is achieved such that all calibrations and corrections are performed during the TGA baseline and steam oxidation programs, making system operation virtually identical to standard TGA. Benchmarking results showed a relative error in hydrogen measurement of 5.7–8.4% following the application of a correction factor. Lastly, suggestions are made for possible improvements to the presented technique so that it may be better applied to the three cases presented.},

  doi          = {10.1016/j.measurement.2015.11.043},

  journal      = {Measurement},

  number       = C,

  volume       = 82,

  place        = {United States},

  year         = {Mon Jan 11 00:00:00 EST 2016},

  month        = {Mon Jan 11 00:00:00 EST 2016}

}

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