Improving Reproducibility in Hydrogen Storage Material Research

Broom, Darren P.; Hirscher, Michael

doi:10.1002/cphc.202100508

Cited by 25 publications

(26 citation statements)

References 126 publications

(206 reference statements)

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“…A relevant issue in assessing experimental data from a diverse array of sources is to understand what level of reproducibility is obtained among distinct measurements. This issue is of course important in many areas of materials chemistry and engineering. − Several recent efforts have been coordinated to examine this issue for measurements of adsorption equilibrium. Gasparik et al performed an interlaboratory study for methane, CO 2 , and ethane isotherms in shales, highlighting the importance of standardized calibration and measurement protocols as well as a precise control of the experimental conditions.…”

Section: Introductionmentioning

confidence: 99%

Experimentally Verified Alkane Adsorption Isotherms in Nanoporous Materials from Literature Meta-Analysis

2022

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Identification of independent experimental replicate measurements of well-defined physical properties provides a useful way to assess the reproducibility of literature reports of these properties. Prior meta-analysis of this kind for single-component adsorption of CO2 and alcohols in nanoporous materials showed that ∼20% of reported isotherms for these molecules were inconsistent with available replicate measurements. In this paper, we extend this analysis to the single-component adsorption of alkanes in nanoporous materials using a collection of 2998 experimental isotherms. Among these isotherms, 846 replicates were identified and analyzed. Many more replicates are available for CH4 adsorption than for any other alkane. Our analysis finds that 15% of the replicate alkane isotherms are inconsistent with other replicate measurements. After discarding these outlier isotherms we report graphical and numerical consensus isotherms for 93 independent combinations of adsorbate, adsorbent, and temperature as well as an assessment of another 124 independent systems for which two replicate isotherms are available.

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Section: Introductionmentioning

confidence: 99%

Experimentally Verified Alkane Adsorption Isotherms in Nanoporous Materials from Literature Meta-Analysis

2022

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“…In line with the issues raised above, Broom and Hirscher discussed the necessary steps for reproducible results in hydrogen storage research [15].…”

Section: Characterization Methods: Old New and Their Pitfallsmentioning

confidence: 97%

“…However, analysis of the literature data also points out to several weaknesses in applying traditional characterization methods that have not yet been tuned for current nanosized materials [15,34,37,38]. For instance, AB (ammonia borane) hydrogenation studies showed many inconsistencies [38].…”

Section: Characterization Methods: Old New and Their Pitfallsmentioning

confidence: 99%

“…12 Al + 17MgH ⟹ Al Mg + 17 H ↑ (15) The reactions involved in the mechanistic proposal of the authors also allowed computation of the apparent activation energies (by Kissinger plot), which were of 97.3 kJ mol −1 for MgH2 and 61.4 kJ mol −1 for AlH3 (Figure 16c). [44].…”

Section: Alhmentioning

confidence: 99%

“…The state-of-the-art of boron-nitrogen compounds for energy storage was reviewed by Kumar et al [11] and Hagemann [12]. The solid-state materials used for hydrogen storage have been addressed by Lee et al [13], Hadjixenophontos et al [14], Broom and Hirscher [15], Comanescu [16], Kharbachi et al [17], Zheng et al [18] and He et al [19], among others. The role of highly dispersed catalysts on hydrogen storage materials [20] and the topologically engineered materials serving for energy conversion and storage [21] have also been very recently reviewed, while the critical issue of accurately describing hydrogen sorption properties of materials has been highlighted by Broom et al [15].…”

Section: Introductionmentioning

confidence: 99%

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Recent Development in Nanoconfined Hydrides for Energy Storage

Comănescu

2022

IJMS

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Hydrogen is the ultimate vector for a carbon-free, sustainable green-energy. While being the most promising candidate to serve this purpose, hydrogen inherits a series of characteristics making it particularly difficult to handle, store, transport and use in a safe manner. The researchers’ attention has thus shifted to storing hydrogen in its more manageable forms: the light metal hydrides and related derivatives (ammonia-borane, tetrahydridoborates/borohydrides, tetrahydridoaluminates/alanates or reactive hydride composites). Even then, the thermodynamic and kinetic behavior faces either too high energy barriers or sluggish kinetics (or both), and an efficient tool to overcome these issues is through nanoconfinement. Nanoconfined energy storage materials are the current state-of-the-art approach regarding hydrogen storage field, and the current review aims to summarize the most recent progress in this intriguing field. The latest reviews concerning H2 production and storage are discussed, and the shift from bulk to nanomaterials is described in the context of physical and chemical aspects of nanoconfinement effects in the obtained nanocomposites. The types of hosts used for hydrogen materials are divided in classes of substances, the mean of hydride inclusion in said hosts and the classes of hydrogen storage materials are presented with their most recent trends and future prospects.

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Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study

Villajos,

Balderas‐Xicohténcatl,

Al Shakhs

et al. 2024

ChemPhysChem

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Hydrogen storage by cryoadsorption on porous materials has the advantages of low material cost, safety, fast kinetics, and high cyclic stability. The further development of this technology requires reliable data on the H2 uptake of the adsorbents, however, even for activated carbons the values between different laboratories show sometimes large discrepancies. So far no reference material for hydrogen cryoadsorption is available. The metal‐organic framework ZIF‐8 is an ideal material possessing high thermal, chemical, and mechanical stability that reduces degradation during handling and activation. Here, we distributed ZIF‐8 pellets synthesized by extrusion to 9 laboratories equipped with 15 different experimental setups including gravimetric and volumetric analyzers. The gravimetric H2 uptake of the pellets was measured at 77 K and up to 100 bar showing a high reproducibility between the different laboratories, with a small relative standard deviation of 3 — 4 between pressures of 10 — 100 bar. The effect of operating variables like the amount of sample or analysis temperature was evaluated, remarking the calibration of devices and other correction procedures as the most significant deviation sources. Overall, the reproducible hydrogen cryoadsorption measurements indicate the robustness of the ZIF‐8 pellets, which we want to propose as a reference material.

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Improving Reproducibility in Hydrogen Storage Material Research

Abstract: This article therefore describes the measurement of hydrogen sorption and covers the required experimental procedures, aspects of troubleshooting and recommended reporting guidelines, with a view of helping improve reproducibility in experimental hydrogen storage material research.

Cited by 25 publications

References 126 publications

Experimentally Verified Alkane Adsorption Isotherms in Nanoporous Materials from Literature Meta-Analysis

Experimentally Verified Alkane Adsorption Isotherms in Nanoporous Materials from Literature Meta-Analysis

Recent Development in Nanoconfined Hydrides for Energy Storage

Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study

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