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Design of high pressure differential volumetric adsorption measurements with increased accuracy

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Abstract

High pressure adsorption measurements for light gases on volumetric equipment are prone to error. Differential units reduce the sensitivity to leakage, gas compressibility, and temperature gradients, but remain highly sensitive to volume uncertainties, the calibration of which is difficult in the presence of low-density, microporous samples. Calibration error can be reduced using a high initial pressure differential and large calibration volume; however, systematic error is prevalent in the literature. Using both analytical and multivariate error analysis, we demonstrate that calibration of the differential unit with the differential pressure transducer significantly decreases volume sensitivity. We show that hydrogen adsorption to GX-31 superactivated carbon at 298 K and 80 bar can be measured with a 7 % error in measurement (i.e. within 0.05 wt% for a 100 mg sample), even when experimental volume calibration is determined only within ~1 %. This represents approximately a 2–7 fold increase in sensitivity relative to previous reports using differential measurements. We also provide a framework for optimizing the design of a volumetric adsorption unit. For virtually any system design, the improved differential methods offer a significant increase in precision relative to the conventional volumetric measurement (from 10- to over 250-fold, depending on the precision of the pressure transducer). This improvement further enhances advantages of the differential unit, in addition to advantages that arise for treating gas compressibility and temperature fluctuations.

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Acknowledgments

This work was supported by the U.S. Department of Energy, Energy Efficiency and Renewable Energy program, award DE-FG36-08GO18139. The following people worked with us in the initial design and build of the equipment: Peter Eklund, David Narehood, Kofi Adu. Funding for design and purchase of components was provided by Penn State University and the Materials Research Institute.

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Authors and Affiliations

  1. Department of Energy and Mineral Engineering, EMS Energy Institute, The Pennsylvania State University, 104 Materials Research Laboratory, University Park, PA, 16802, USA

    Sarmishtha Sircar, Cheng-Yu Wang & Angela D. Lueking

  2. Department of Chemical Engineering, EMS Energy Institute, The Pennsylvania State University, University Park, PA, 16802, USA

    Angela D. Lueking

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  1. Sarmishtha Sircar
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  2. Cheng-Yu Wang
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  3. Angela D. Lueking
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Correspondence to Angela D. Lueking.

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Sircar, S., Wang, CY. & Lueking, A.D. Design of high pressure differential volumetric adsorption measurements with increased accuracy. Adsorption 19, 1211–1234 (2013). https://doi.org/10.1007/s10450-013-9558-8

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