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Rexer T.F.T.,Northumbria University | Benham M.J.,Hiden Isochema Ltd | Aplin A.C.,Durham University | Thomas K.M.,Northumbria University
Energy and Fuels | Year: 2013

Shale gas is becoming an increasingly important energy resource. In this study, the adsorption of methane on a dry, organic-rich Alum shale sample was studied at pressures up to ∼14 MPa and temperatures in the range 300-473 K, which are relevant to gas storage under geological conditions. Maximum methane excess uptake was 0.176-0.042 mmol g-1 (125-30 scf t-1) for the temperature range of 300-473 K. The decrease in maximum methane surface excess with increasing temperature can be described with a linear model. An isosteric enthalpy of adsorption 19.2 ± 0.1 kJ mol-1 was determined at 0.025 mmol g-1 using the van't Hoff equation. Supercritical adsorption was modeled using the modified Dubinin-Radushkevich and the Langmuir equations. The results are compared with absolute isotherms calculated from surface excess and the pore volumes obtained from subcritical gas adsorption (nitrogen (78 K), carbon dioxide (273 and 195 K), and CH 4 (112 K)). The subcritical adsorption and the surface excess results allow an upper limit to be put on the amount of gas that can be retained by adsorption during gas generation from petroleum source rocks. © 2013 American Chemical Society.


Broom D.P.,Hiden Isochema Ltd. | Thomas K.M.,Newcastle University
MRS Bulletin | Year: 2013

There are numerous applications of nanoporous materials, including gas storage, separation, and purification. In recent years, the number of available nanoporous materials has increased substantially, with new material classes, such as metal-organic frameworks and microporous organic polymers, joining the traditional adsorbents, which include activated carbons, porous silicas, and zeolites. The determination of the gas adsorption properties of these materials is critical to both the development of new materials for targeted applications and the assessment of the suitability of a material for a particular technology. In this article, we provide an overview of nanoporous materials and their gas adsorption properties, existing and future applications for new materials, adsorption measurement methods, and the experimental challenges involved in the determination of gas adsorption both at elevated pressures and from multicomponent mixtures. Copyright © 2013 Materials Research Society.


Tedds S.,University of Birmingham | Walton A.,University of Birmingham | Broom D.P.,Hiden Isochema Ltd. | Book D.,University of Birmingham
Faraday Discussions | Year: 2011

Porous materials adsorb H2 through physisorption, a process which typically has a rather low enthalpy of adsorption (e.g. ca. 4 to 7 kJ mol-1 for MOFs), thus requiring cryogenic temperatures for hydrogen storage. In this paper, we consider some of the issues associated with the accurate characterisation of the hydrogen adsorption properties of microporous materials. We present comparative gravimetric hydrogen sorption data over a range of temperatures for different microporous materials including an activated carbon, a zeolite, two MOFs and a microporous organic polymer. Hydrogen adsorption isotherms were used to calculate the enthalpy of adsorption as a function of hydrogen uptake, and to monitor the temperature dependence of the uptake of hydrogen. Under the conditions investigated, it was found that the Tóth equation provided better fits to the absolute isotherms compared to the Sips (Langmuir-Freundlich) equation at low pressures, whereas it appeared to overestimate the maximum saturation capacity. The isosteric enthalpy of adsorption was calculated by either: fitting the Sips and Tóth equations to the adsorption isotherms and then applying the Clausius-Clapeyron equation; or by using a multiparameter Virial-type adsorption isotherm equation. It was found that the calculated enthalpy of adsorption depended strongly upon the method employed and the temperature and pressure range used. It is shown that a usable capacity can be calculated from the variable temperature isotherms for all materials by defining a working pressure range (e.g. 2 to 15 bar) over which the material will be used. © The Royal Society of Chemistry 2011.


Xiang Z.,Beijing University of Chemical Technology | Cao D.,Beijing University of Chemical Technology | Lan J.,Beijing University of Chemical Technology | Wang W.,Beijing University of Chemical Technology | Broom D.P.,Hiden Isochema Ltd
Energy and Environmental Science | Year: 2010

Computational modelling is a powerful tool for the study of gas-solid interactions, and can be used both to complement experiment and design new materials. For the modelling of gas adsorption by nanoporous media, a multiscale approach can be used, in which the molecular force fields required for Grand Canonical Monte Carlo (GCMC) simulations are derived from first-principles calculations. This can result in significantly enhanced accuracy, in comparison with conventional empirical force field-based GCMC methods. In this article, we review the application of this multiscale approach to the simulation of the adsorption of hydrogen, methane and carbon dioxide in Porous Coordination Frameworks (PCFs) for the purpose of gas storage for energy transportation and Carbon Capture and Storage (CCS) technology. We also define a scheme for the design of new materials with improved adsorption performance for the storage of these gases through the combination of multiscale simulation and experimental work, and discuss some of the issues regarding gas adsorption measurement accuracy in the context of the validation of simulation results using experimental data. © 2010 The Royal Society of Chemistry.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

In this chapter, we discuss many of the practical issues that can affect the accuracy of gas phase hydrogen sorption measurement techniques. We begin with some relevant properties of gaseous hydrogen, such as the description of its compressibility as a function of temperature and pressure, the Joule-Thomson effect, thermal conductivity and the gas purity. We then cover some of the properties of materials that can affect hydrogen sorption measurement, including our knowledge of the sample volume, density and mass, the sensitivity of materials to air and moisture, the history and purity of samples, and gaseous impurity gettering. General instrumentation issues, such as the vacuum and pressure handling capability of apparatus, its thermal stability and homogeneity, and the accuracy of pressure and temperature measurement, are then discussed. Two aspects of experimental measurement methodology, namely sample degassing and activation, and equilibration times, are then covered. The last three sections of the chapter then discuss a series of issues that can affect the volumetric, gravimetric and thermal desorption methods, respectively.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

In this concluding chapter we firstly discuss interlaboratory studies, which can be used to demonstrate the reproducibility of a measurement technique, or to compare the results of different techniques, and hence to assess the accuracy of the characterisation process. In particular, we discuss the results of a recent relevant interlaboratory study on hydrogen adsorption. We then discuss reference materials, which can be used to characterise and corroborate both sorption instrument performance and experimental methodology, before describing some provisional measurement guidelines, which provide both a guide to best practice in hydrogen sorption measurement and serve as a useful practical summary of the discussion of the experimental considerations in Chap. 6 10.1007/978-0-85729-221-6_6. We conclude by emphasising the importance of future research into hydrogen sorption measurement accuracy, in order to aid our understanding of the interaction of hydrogen with matter and to help reduce the variation in the reported hydrogen sorption properties of new materials, as the search for a solution to the hydrogen storage problem continues. © Springer-Verlag London Limited 2011.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

In this chapter we cover some of the common complementary techniques used for hydrogen storage material characterisation. We begin with thermal analysis and calorimetry, which can be used to determine the thermodynamic properties that can also be measured using hydrogen sorption techniques, as well as activation energies and characteristic temperatures of absorption and desorption. Gas adsorption methods, such as BET (Brunauer-Emmett-Teller) surface area measurement and DFT (Density Functional Theory) based pore size distribution determination, are commonly used to characterise the properties of porous hydrogen adsorbents and so these are then covered, with a focus on the data analysis methods used in each case. We then consider neutron and X-ray powder diffraction and small angle scattering, which can complement hydrogen sorption measurements for both hydrides and porous adsorbents. Different types of spectroscopy are then covered including Inelastic Neutron Scattering (INS), proton (1H) Nuclear Magnetic Resonance (NMR) and Variable Temperature Infrared (VTIR) spectroscopy. A number of other techniques that do not fit readily into the above categories are also briefly covered. © Springer-Verlag London Limited 2011.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

In this chapter we examine the hydrogen sorption properties of materials, considering both the parameters that are of prime practical engineering importance, and the thermodynamic and kinetic properties of interest for future materials development. We begin with the practical storage properties, such as the reversible storage capacity, including definitions of the gravimetric and volumetric capacities and the total and excess adsorption for adsorptive hydrogen storage, the long term cycling stability, gaseous impurity resistance, and the ease of activation. The thermodynamic properties, including the enthalpy of molecular hydrogen adsorption and the enthalpy of hydride formation or decomposition are then covered. We then discuss the kinetics of hydrogen adsorption and absorption, including parameters such as the activation energy, hydrogen diffusion coefficient and the apparent rates of absorption or desorption, which can be used to characterise the time-dependent sorption and desorption properties of materials. The latter part of the chapter then considers both equilibrium and kinetic models that can be used to describe experimental data. © Springer-Verlag London Limited 2011.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

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. © Springer-Verlag London Limited 2011.


Broom D.P.,Hiden Isochema Ltd
Green Energy and Technology | Year: 2011

This chapter presents an overview of the various materials that are currently being considered as potential solid state storage media. We concentrate on the physical and chemical properties of the materials relevant for the characterisation of their hydrogen storage properties and their practical use in storage devices, as opposed to the materials synthesis methods. The chapter looks first at microporous materials, including activated and nanostructured carbons, zeolites, organic microporous polymers and metal-organic frameworks. Secondly, we cover the alloys and intermetallic compounds that form interstitial hydrides at practical storage temperatures and hydrogen pressures. The complex hydrides, including alanates and lithium-based materials, such as LiNH2 and LiBH4, are then discussed before concluding with a look at some materials that do not fit readily into the above categories. © Springer-Verlag London Limited 2011.

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