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Gas Sorption Measurement Techniques

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Book cover Hydrogen Storage Materials

Part of the book series: Green Energy and Technology ((GREEN))

Abstract

In this chapter we introduce the main gas sorption techniques applied to the characterisation of the hydrogen sorption properties of potential hydrogen storage materials. We begin with volumetric techniques, with a focus on the commonly used manometric (Sieverts’) method, but also cover some of the alternative approaches, such as the flowing and differential volumetric methods. We then describe the gravimetric technique, including a discussion of vacuum microbalances and the requirements for high pressure hydrogen operation. Thermal desorption techniques are then covered, including Thermogravimetric Analysis (TGA) and Thermal Desorption Spectroscopy (TDS), in which the temperature-programmed desorption of hydrogen can be detected in a number of ways, including quadrupole mass spectrometry. The chapter concludes with a practical comparison of the different gas sorption measurement techniques.

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Notes

  1. 1.

    There are some variations and inconsistencies in the terminology used for the measurements described in this section. The measurement type used often in metal hydride research is essentially the same as the method used by adsorption equipment for the determination of the BET surface area and pore size distribution of porous solids. It is widely called the volumetric technique, although the measurement parameter that determines the sorbed quantity is principally the pressure and therefore it should be termed manometry [1] or the manometric technique or method [4, 9]. The equipment is also sometimes referred to as PCT apparatus, because the measured data determine the Pressure–Composition–Temperature (PCT) properties of a metal hydride system. This is a particularly imprecise term because these properties can be determined in a number of ways. Here we use the term volumetric to encompass all techniques that use the measurement of the volume of hydrogen, as opposed to a change in the sample mass, to determine hydrogen uptake because this is common terminology, but acknowledge that for manometric apparatus this is, strictly speaking, incorrect.

  2. 2.

    The high vacuum regime can be defined as the range ~10−3 to 10−8 mbar (10−1 to 10−6 Pa). Either side of this regime is ultra-high vacuum in the range 10−8 to 10−12 mbar (10−6 to 10−10 Pa), medium vacuum in the range 1 to 10−3 mbar (102 to 10−1 Pa) and low vacuum in the range atmospheric pressure to 1 mbar (105 to 102 Pa) [11].

  3. 3.

    Providing the empty cell volume is known this is also a helium pycnometry measurement of the sample volume and hence its density. For adsorption measurement, this defines the position of the Gibbs dividing surface.

  4. 4.

    Empty in the sense of unloaded, unhydrogenated, or at the hydrogen loading required at the start of the measurement, including any trapped residual hydrogen.

  5. 5.

    The (m s /ρ s ) term therefore simply represents the volume occupied by the sample.

  6. 6.

    This is also the method of determining technical equilibrium described by Keller and Staudt [4].

  7. 7.

    A greater uptake and higher pressure allows a smaller sample size.

  8. 8.

    Careful calculations would be required before this was attempted because the resultant pressure rise due to an increase from 77 to 300 K, for example, is nearly fourfold ignoring any desorption from the sample. However, this might only limit the upper pressure of the measurement because 2–3 MPa would seem to be feasible, whereas 20 MPa would not because a 77 K measurement could potentially result in pressures approaching a kbar (100 MPa).

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  1. Hiden Isochema Ltd, Europa Boulevard 231, Warrington, WA5 7TN, UK

    Darren P. Broom

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Broom, D.P. (2011). Gas Sorption Measurement Techniques. In: Hydrogen Storage Materials. Green Energy and Technology. Springer, London. https://doi.org/10.1007/978-0-85729-221-6_4

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  • DOI: https://doi.org/10.1007/978-0-85729-221-6_4

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