Thermochemical Reactions Research Articles

Hydrothermal Carbonization of Urban Lignocellulosic Wastes – A Review

Expressional dependence on the consumption of products from fossil sources still prevails in the third decade of this century. Meanwhile, the environmental impacts caused by their excessive use, especially fuel, have been criticized more intensely and compromise the sustainability of the Earth. In addition, it influences the consolidation of new sources and ecological matrices. Therefore, this scenario requires the search for new natural, renewable and sustainable sources. In this context, evidence indicates that biomass is one of the sources with solid foundations to replace fossil sources. Urban lignocellulosic biomass shows various attributes, such as being abundant, low cost, easy to locate, renewable, etc. In this line, thermochemical methods have been cited as the most appropriate and sustainable for their transformation. In this context, this scientific review explored the transformation of urban lignocellulosic biomass into carbon fractions through hydrothermal carbonization. After the components of the urban lignocellulosic biomass were provided, such as the chemical composition, physical-chemical and energetic properties, the general vision of hydrothermal carbonization was introduced, with the temperature and residence time were identified as the parameters with the major influence on the thermochemical reaction. Finally, the authors described the capability of hydrothermal carbonization to yield products in the liquid, gas, and solid states (hydrochar), along with addressing the challenges associated with hydrothermal carbonization of urban lignocellulosic waste.

Development of machine learning-based models for describing processes in a continuous solar-driven biomass gasifier

The synergy of two renewable and efficient sources in producing clean fuels, i.e., solar energy and biomass, can result in high efficiency. In this regard, developing syngas production systems based on solar biomass gasification has attracted much attention. However, experimental setups on solar-driven gasifier processes are costly and time-intensive. In such a situation, an accurate and low-cost alternative is to develop data-driven machine learning (ML) models to predict the processes involved in solar-driven biomass gasifiers. In the present study, several ML models, including random forest (RF), RANdom SAmple Consensus (RANSAC), stochastic gradient descent (SGD), automatic relevance determination (ARD) regression, and elastic net linear (ENL) regression, were developed to accurately predict the various processing of a continuous solar-driven biomass gasifier, including CO production rate and H2 production rate (H2), carbon feeding rate, solar power input, thermochemical reactor efficiency, solar-to-fuel energy conversion efficiency, solar energy input, and carbon consumption rate. Using efficient ML methods, the eight formulas and the eight models for H2, CO production rate, carbon feeding rate, carbon consumption rate, solar energy input, solar power input, thermochemical reactor efficiency, and solar-to-fuel energy conversion efficiency are made in this study. Using the linear form can be reached the best R-Squared (R2) values for all formulas and the model, and the best R2 values are between 0.998 and 0.999 for the formulas by the elastic net and the ARD regression, and also the best R2 values are between 0.998 and 0.999 for the models by the RF and the RANSAC regressor. The R2 values for H2, CO production rate, carbon consumption rate, solar energy input, solar power input, thermochemical reactor efficiency, and solar-to-fuel energy conversion efficiency for formulas, respectively, are 0.998, 0.998, 0.999, 0.999, 0.999, 0.996, and 0.998 by the elastic net. For temperature of the carbon feeding rate, this value is 0.999 by the ARD regressor.

Experimental and simulation study of Mn–Fe particles in a controllable-flow particle solar receiver for high-temperature thermochemical energy storage

CSP systems hold tremendous potential for large-scale and long-duration energy storage. However, their extensive adoption has been impeded by cost constraints. To overcome this hurdle, the development of the next generation CSP systems, focusing on high-temperature heat absorption and storage, is paramount for reducing the LCOE. The integration of TCES technologies shows promise in bolstering energy storage density, stability at high temperatures, and decreasing the LCOE. This study investigates the performance of Mn–Fe particles in a controllable-flow particle receiver operating at high temperatures. Experimental data demonstrate that the particles reach a maximum temperature of 1041.8 °C, resulting in an outstanding outlet particle thermochemical reaction conversion rate of 96.35%. Critical parameters influencing receiver performance were also examined meticulously. It was observed that increased incident flux density significantly enhanced receiver efficiency of 88%. Moreover, effective management of local overheating through the integration of TCES proved indispensable. The outlet particle temperature differential was merely 9.53 °C, and the sudden fluctuations in incident flux led to a limited temperature rise of 4.84 °C, attributing to intensified reaction enthalpy and reaction rate. By optimizing operational stability, continuous operation of CSP systems under high temperatures can be achieved, maximizing efficiency and allowing for greater system flexibility.

Study of Chemical Additives for Optimization of Binary Systems Used for Downhole Thermochemical Treatment of Heavy Oil

Currently, most explored oil fields in Russia are at a late stage of development, and in order to maintain high levels of oil production, it is rational to put into operation fields with hard-to-recover reserves. For complicated oil fields, in particular fields with high-viscosity oil, the known traditional methods of development are ineffective. Therefore, the search for new technologies for the development and operation of such fields to significantly increase oil recovery and intensify production is of fundamental importance. One such method of heat treatment of the bottomhole formation zone is the use of heat and gas generating systems on site. In this work, new results were obtained on physical modeling of thermochemical reaction initiation with delayed-action catalyst (2,2-bis(hydroxymethyl)butanoic acid) filtration tests on composite core models of sandstone and carbonate with foam heat generation and initiating additives of binary type. Using hydrodynamic modelling, the results of laboratory studies were reproduced, and the preliminary efficiency of the developed technology for thermochemical treatment of deposits in the Samara region (Russia) was evaluated.

A review on in-situ process analytical techniques for the thermochemical conversion of coal and biomass

Abstract Coal and biomass are important feedstocks for carbon energy from thermochemical conversion process. Fully understanding the analytical technology that characterizes the changes in physicochemical properties and structural characteristics of coal and biomass during the thermochemical reactions is a key prerequisite for the realization of appropriate utilization of energy fuels. Modern in-situ process analysis technology can accomplish the in-situ detection of the experimental process, and therefore reflect the experimental process more accurately. Moreover, it is developing towards automation, intelligentization, and comprehensive detection. Based on the characteristics of each detection technology, this paper summarizes the basic principles, application scope and performance characteristics of the three advanced in-situ process analysis technologies: hyphenated technology, synchrotron radiation, and online analysis. The practicability and accuracy of each detection technology in coal and biomass research are compared and analyzed, and its latest application and development trend are elucidated. These tools not only make up for the shortcomings of traditional detection techniques in characterizing the in-situ reaction, but also provide complementary information on molecular microscopic changes during fuel thermal conversion. This review paper can provide insights for relevant researchers in the selection of analytical techniques, and promote in-depth study on microcosmic mechanism of fuel conversion.

Solar‐Driven Redox Splitting of CO2 Using 3D‐Printed Hierarchically Channeled Ceria Structures

AbstractFuel produced from CO2 and H2O using solar energy can contribute to making aviation more sustainable. Particularly attractive is the thermochemical production pathway via a ceria‐based redox cycle, which uses the entire solar spectrum as the source of high‐temperature process heat to directly produce a syngas mixture suitable for synthetizing kerosene. However, its solar‐to‐fuel energy efficiency is hindered by the inadequate isotropic topology of the ceria porous structure, which fails to absorb the incident concentrated solar radiation within its entire volume. This study presents the design and 3D‐print of hierarchically channeled structures of pure ceria by direct ink writing (DIW) to enable volumetric radiative absorption while maintaining high effective densities required for maximizing the fuel yield. The complex interplay between radiative heat transfer and thermochemical reaction is investigated in a solar thermogravimetric analyzer with samples exposed to high‐flux irradiation, mimicking realistic operation of solar reactors. Channeled structures with a stepwise optical thickness achieve a higher and more uniform temperature profile compared to that of state‐of‐art isotropic structures, doubling the volume‐specific fuel yield for the same solar flux input. Thermomechanical stability of the ceria graded structures, DIW‐printed using a novel ink formulation with optimal rheological behavior, is validated by performing 100 consecutive redox cycles.

Recent Developments in Ceria-Driven Solar Thermochemical Water and Carbon Dioxide Splitting Redox Cycle

Metal oxide (MO) based solar thermochemical H2O (WS) and CO2 splitting (CDS) is one of the most promising and potential-containing processes that can be used to produce H2 and syngas (liquid fuel precursor). Several non-volatile and volatile MOs were considered redox materials for the solar-driven WS and CDS operation. Among all the examined redox materials, based on their high O2 storage capacity, faster oxidation kinetics, and good stability, ceria and doped ceria materials are deemed to be one of the best alternatives for the operation of the thermochemical redox reactions associated with the WS and CDS. Pure ceria was used for solar fuel production for the first time in 2006. A review paper highlighting the work done on the ceria-based solar thermochemical redox WS and CDS cycle from 2006 until 2016 is already published elsewhere by the author. This review paper presents all the significant findings reported in applying pure ceria and doped ceria materials for the WS and CDS by research teams worldwide.

Optical and thermal analysis of solar parabolic dish cavity receiver system for hydrogen production using deep learning

The solar thermochemical cycle, responsible for converting solar energy to chemical fuel, is an emerging clean hydrogen production technique. The distribution of the concentrated heat flux and temperature on the receiver is crucial in deciding solar-to-fuel conversion efficiency. Thus, the optimum configuration of a solar parabolic dish collector (PDC) is necessary for providing efficient thermal energy. The dish diameter, rim angle, and distance of the receiver aperture from the focal point of the dish characterize the optimization of the PDC. The non-uniform heat flux captured is coupled with a heat transfer model of a solar thermochemical reactor for a thermal dissociation of ZnO involved in a ZnO/Zn thermochemical cycle for hydrogen production. The directly irradiated rotating reactor comprises a cylindrical cavity packed with insulation layers and a quartz glass window. The rotating cavity is loaded with ZnO granular particles held by a centrifugal force. A 3D CFD numerical model is analyzed by coupling the Eulerian multiphase model for ZnO particle dynamics, fluid flow of gaseous mixture, RNG k-ԑ turbulence model, Energy and Discrete Ordinates (DO) radiation model, and Arrhenius reaction rate chemical reaction of ZnO dissociation. A numerical model with non-uniform heat flux input is validated for a cavity temperature, mass fraction of zinc and oxygen, and oxygen molar flow rate at the reactor outlet. An artificial neural network model is adopted to predict the heat flux and uniformity factor values of PDC. Correlation Coefficient (R2), Root Mean Square Error (RMSE), and Mean Absolute Percentage Error (MAPE) error metrices were used to evaluate the model's performance having the receiver diameter (d), the dish diameter (D), the rim angle (φ), and the distance between the focus and receiver (h) as input variables.

Oxidation of Polycyclic Aromatic Hydrocarbons: Evidence of Similarities in Thermochemical Properties and Reaction Paths

ABSTRACT This work elaborates similarities of thermochemical properties and oxidation kinetics among several polycyclic aromatic hydrocarbons. The systems considered are benzene (A1), naphthalene (A2), phenanthrene (A3), pyrene (A4), and the larger ones, benzo[ghi]perylene (A6) and coronene (A7). For each system, thermochemical properties, bond energies and oxidation kinetics are calculated and compared. Interpretation of the results revealed strong similarities and redundancies in behavior among these systems. The results imply that reactions are not dependent on the size of the molecules and, therefore, reaction paths and kinetic barriers determined with high-level calculations for small molecules can be used as estimates in the investigation of larger aromatic hydrocarbons to avoid expensive calculation efforts.

Directional oxygen diffusion in Cu1.5Mn1.5O4 crystals for long reversible thermochemistry

Redox activity of metal oxides are the key to the development of high-temperature thermochemical energy storage. However, few studies have reported that the reactivity of metal oxides as thermochemical energy storage is significantly affected by the changes of crystal structure and morphology during redox, caused by ion diffusion and vacancy formation and migration. In this study, we find a previously unreported high-performance thermochemical energy storage material Cu1.5Mn1.5O4 with special structure. Cu1.5Mn1.5O4 shows high energy densities during reduction and oxidation (−219.852 and 207.618 kJ/kg), and keeps 97.06% and 92.98% reactivity after 600 cycles. Voids on specific surfaces are observed after cycling, but not in the fresh sample. We find the voids provide abundant Cu2+, Mn4+ species and lattice oxygen to promote its reaction performance. Cu ions migrate obviously after oxidation and molecular dynamics simulations reveal that DCu (7.4 × 10−14 cm2 s−1) is higher than DMn (5.1 × 10−14 cm2 s−1) and DO (1.7 × 10−14 cm2 s−1). Cu1.5Mn1.5O4 exhibits voids during oxidation due to ion transport described by the Kirkendall effect. In addition, DFT calculations verify that O2− is more easily to adsorb and diffuse on (111) surface, revealing the optimal transport path and directional diffusion mechanism of O2−. These mechanisms can provide ideas for the reasonable design of materials to improve thermochemical reaction performance.

Reconceptualization of the mechanism of thermal hydrolysis pretreatment to enhance the anaerobic conversion of sludge organic nitrogen: Decisive role of organic nitrogen occurrence

The occurrence state of organic nitrogen (ON) is the key to affect anaerobic biotransformation of sludge. ON in sludge was chemically classified as PA (easily accessible part), PB (moderately accessible) and PC (hardly accessible) according to the modified CNCPS method. The components of them were analyzed by PY-GCMS, and it was identified that PA was extracellular amino acids, peptides and proteins; PB was genetic material, cell wall peptidoglycans and intracellular proteins; PC was ON that cross-linked with complex macromolecules. The conversion characteristics of PA, PB and PC in sludge and their relationship with anaerobic digestion (AD) performance were investigated after thermal hydrolysis pretreatment (THP) at different temperatures (100–180 °C). With the increase of THP temperature, the hydrolysis of PA and the conversion of PB to PA were promoted. At 180-THP, part of PA was converted to PC due to thermochemical reactions. In the fast degradation stage of AD of ON (ON-fast), PA is the main component of degradation; while in the slow degradation stage (ON-slow), the degradation of ON is mainly dominated by PB. Therefore, THP can significantly increase the proportion of ON-fast and reduce the ON fraction in the digestate (ON-hard). Moreover, PA and PB, rather than PC, were identified as dominant in ON-hard with or without THP for the first time, overturning the traditional view (remaining ON after AD was that cross-linked with complex macromolecules). This is due to that PA and PB are the main ON that make up microbial cells. The findings upgraded our perspective on conversion of ON of sludge during AD and inspire the shifted focus from “degrading PC” to “PC accumulation” for later use, through targeted enhanced PA degradation.

Temperature-entropy and energy utilization diagrams for energy, exergy, and energy level analysis in solar water splitting reactions

Solar hydrogen production by water splitting reaction is an important route to realize the storage of solar energy. The involvement of light and chemical energy can reduce the high reaction temperature of direct thermochemical water splitting reactions, but the pivotal issues such as energy, exergy, and energy level relationships behind the temperature reduction remain under-researched. A graphic analysis of water splitting reactions using the temperature-entropy and energy utilization diagrams is proposed to research the energy, exergy, and energy level relationships. The energy composition and conversion mechanisms with the light and chemical energy are presented in the diagrams by comparing with direct thermochemical water splitting reactions. Three cases, including the photocatalytic, photo-thermochemical, and methane steam reforming reactions, are studied to explain the effect of light, the synergistic effect of heat and light, and the effect of chemical energy in reducing the temperature of water splitting reactions. The energy levels of light and methane are higher than those of hydrogen, thus lowering the energy level of heat and reducing reaction temperatures. The discovery of the energy level required for hydrogen production will provide guidance for reducing its temperature.

Research on the chemical barrier and failure behavior of WS2 and WS2/Ti coatings under high-temperature conditions and the effects on the lifespan of diamond-coated cutting tools

With its outstanding performance as a solid lubricant, WS2 has found applications in cutting tools. Diamond-coated tools often experience the formation of a graphite phase during machining of ferrous metals. The WS2 coating effectively hinders the thermochemical reaction between the tool-chip and tool-work, thereby extending the tool's operational lifespan. However, WS2 is susceptible to oxidation at high temperatures, leading to the loss of its lubricating properties. Therefore, improvements in its high-temperature resistance are necessary. This study proposes a WS2/Ti multilayer coating structure, which enables the development of solid lubricating coatings (SLC) that are better suited for high-temperature environments. Through the application of negative bias, Ti atoms are propelled into the gaps within the WS2 dendritic structure at high velocities, thereby forming metallic bonds between the layered structures. This process reduces the transfer film effect and hinders the rapid degradation of the SLC. Additionally, the Ti layer forms a sealing barrier on the surface of WS2, effectively impeding contact between WS2 and O2, minimizing WS2 oxidation, and prolonging the SLC's operational lifespan at elevated temperatures.

The migration and transformation mechanisms of heavy metals during molten salt cyclic thermal treatment of MSWI fly ash

Molten salt thermal treatment has been demonstrated to be effective in dissolving heavy metals in municipal solid waste incineration (MSWI) fly ash. However, the complex thermochemical reactions of various heavy metals during the process remain unclear. This study investigated the migration and transformation mechanisms of typical heavy metals during molten salt (NaCl-CaCl2) cyclic thermal treatment of fly ash at 600–750 °C, as well as the leaching characteristics and recovery methods of heavy metals in the reacted products. Molten chlorides could be recycled to extract heavy metals from fly ash, which reduced the leaching toxicity of heavy metals in the reacted slags. Over 64.3% of Cd, Cu and Pb in fly ash were transferred to molten salt while the migration rate of Zn was restrained to only 32.3% during the cyclic process at 750 °C. Regarding Cd, Cu, and Pb in molten salt, the chlorination and dissolution of their oxides were significant, while the combination of their chlorides with free O2– to form oxides precipitation was weak. However, the above reaction characteristics of Zn were the opposite. Furthermore, Zn2+ could be stabilized into hardystonite (Ca2ZnSi2O7) in molten salt by reacting with Si2O76- generated from the combination of O2– and SiO2. Besides, increasing the reaction temperature facilitated the chlorination and dissolution of heavy metals. For recovery, heavy metals could be concentrated on the insoluble matters of molten salt, with a maximum concentration of approximately 5 times that in fly ash.

Effect of separation wavelength on a novel solar-driven hybrid hydrogen production system (SDHPS) by solar full spectrum energy

Hydrogen energy, with its features of high calorific value, cleanliness and zero-carbon footprint, has been considered an ideal sustainable future energy carrier. Therefore, the identification of a green, efficient and cost-effective hydrogen production method becomes critically important. This paper proposes a novel solar-driven hydrogen production system (SDHPS) by introducing photovoltaic/thermal (PV/T) utilization technology and electrolytic water technology into the photo-thermochemical cycle (includes two processes: photochemical reaction and thermochemical reaction). Among the many parameters that affect the solar energy to hydrogen transformation efficiency, the separation wavelength λligr_pvt decides the energy distribution between photochemical reaction process in the photo-thermochemical cycle and photovoltaic/thermal (PV/T) utilization technology. In order to maximize the harvesting of the solar energy in the proposed SDHPS, this research aims to critically examine how to choose the separation wavelength λligr_pvt's value within the allowed range of 360 nm–400 nm to rationally distribute solar energy. Therefore, the numerical models for the PV/T, the electrochemical water splitting and the photo-thermochemical cycle are established in the paper and combined to examine the efficiency of hydrogen generation for the proposed SDHPS. The influence of separation wavelength λligr_pvt on the hydrogen production efficiency is discussed and analyzed under the variations of four chosen materials of photovoltaic (PV) cell (i.e., Si, GaAs, CIGS, or CdTe). It can be concluded that for the proposed SDHPS, the utilization of GaAs as the photovoltaic material demonstrated the highest solar energy to hydrogen transformation efficiency (i.e., 20.60%) under the separation wavelength λligr_pvt of around 360 nm, in comparison with the rest of the selected PV cell materials (e.g., Si, CdTe and CIGS). It is believed the results could provide guidance for the formulation and construction of higher hydrogen generation effectiveness systems.

Direct Laser Writing of Diffractive Structures on Bi-Layer Si/Ti Films Coated on Fused Silica Substrates

This paper presents the results of an investigation of direct laser writing on a titanium film with an antireflection capping silicon coating. Bi-layer films were deposited on fused silica substrates using an e-beam evaporation system. Modeling predicted that optical absorption for a bi-layer Si/Ti material can be increased by a factor of ~2 compared to a single-layer Ti film at 532 nm laser writing beam wavelength. It is experimentally proved that rate of thermochemical laser writing on Si/Ti films is at least 3 times higher than that on a single-layer Ti film with comparable thickness. The silicon layer was found to participate in the thermochemical reaction (silicide formation) under laser beam heating, which allows one to obtain sufficient position-dependent phase change (PDPC) of light reflected from exposed and unexposed areas. This results in much larger profile depth measured with a white light interferometer (up to 150 nm) than with an atomic force microscope (up to 25 nm). During direct laser writing on Si/Ti films, there is a broad range of writing beam power within which the PDPC and reflection coefficient for the exposed areas change insignificantly. The possibility of selective development of a thermochemically written pattern on a Ti film by removing the capping silicon layer on unexposed areas in a hot KOH solution is shown.

Synergistic Effect of WS2 and Micro-Textures to Inhibit Graphitization and Delamination of Micro-Nano Diamond-Coated Tools

Diamond-coated tools often fail due to coating graphitization and delamination caused by poor coating adhesion, large contact stress, and thermochemical reactions. To address these issues, this research utilized a combination of micro-nano double-layer diamond coating, WS2 coating, and micro-textures. The WS2 coating inhibits the graphitization of the diamond coating through a transfer film mechanism, while the micro-textures and nanocrystalline diamond coating store WS2, resulting in a prolonged lubrication life. Additionally, the influence of micro-texture on coating-substrate residual stress and coating-substrate mechanical interlocking was discussed, and it was proved that proper micro-textures effectively improve the coating adhesion. Under the same cutting flux conditions, taking coating peeling as the judging standard, the cutting distance of textured WS2/Micro-Nano diamond coating tool is more than three times that of ordinary, diamond-coated tools, which greatly improves the service life of the tool.

Engineering thermochemistry to cope with challenges in carbon neutrality

More than 90% of anthropogenic carbon emissions are from uses of organic carbon resources and carbonate minerals that cannot be abandoned any time soon. In this context, we have realized that the most effective strategy to cope with carbon-neutral challenges is to focus on a few super-emitters, which are all associated with heat-induced or heat-driven thermochemical reactions. To assist in reducing CO2 emissions from these super-emitters, we introduce an emerging interdisciplinary Engineering Thermochemistry (ETC) that focuses on heat-induced/driven thermochemical reactions and their engineering. Combined with some exemplary processes, we demonstrate how and why ETC can play a vital role in innovating CO2 super-emitting processes to reduce energy consumption and carbon emissions substantially at the scale of several billion tons. The approaches discussed in this study can help governments and researchers to establish applicable policies and develop practical techniques to meet the challenges of CO2 emission reductions toward a green and carbon-neutral future.

Chemical and thermal performance analysis of a solar thermochemical reactor for hydrogen production via two-step WS cycle

Ceria-based H2O/CO2-splitting solar-driven thermochemical cycle produces hydrogen or syngas. Thermal optimization of solar thermochemical reactor (STCR) improves the solar-to-fuel conversion efficiency. This research presents two conceptual designs and thermal modelling of RPC-ceria-based STCR cavities to attain the optimal operating conditions for CeO2 reduction step. Presented hybrid geometries consisting of cylindrical–hemispherical and conical frustum–hemispherical structures. The focal point was positioned at x = 0, -10 mm, and -20 mm from the aperture to examine the flux distribution in both solar reactor configurations. Case-1 with 2 milliradian S.E (slope error) yields a 27% greater solar flux than case-1 with 4 milliradians S.E, despite the 4 milliradian S.E produces an elevated temperature in the reactor cavity. The mean temperature in the reactive porous region was most significant for case-2 (x = -10 mm) with 4 mrad S.E for model-2, reaching 1966 K and 2008 K radially and axially, respectively. In case-2 (x = -10 mm) for 4 mrad S.E, model-1 attained 1720 K. The efficiency analysis shows that the highest conversion efficiency value was obtained to be 7.95% for case-1 with 4 milliradian S.E.

Novel temperature-driven technique to characterize hydrogen sorption properties under vacuum conditions: Method development, experimental setup, and demonstration on the AB5-type metal hydride LaNi4.1Al0.52Mn0.38

In this study, a modified temperature-controlled sorption characterization technique based on a Sieverts’ apparatus is presented. The main characteristic of the developed method is the hydrogen mass being constant in the system over individual measurement runs while the thermochemical reaction is controlled by the sample temperature. This allows the sorption properties to be measured in vacuum – even down to high vacuum - without the need for large capturing volumes provided. The method itself, the correspondingly built test rig as well as the measurement procedure are discussed in detail. Sources of uncertainty are discussed and evaluated.By performing reference measurements of the absorption and desorption equilibria of the AB5-type alloy LaNi4.1Al0.52Mn0.38, the method is validated and the corresponding results are demonstrated for the first time. Extensive measurements are performed and complete pressure-composition-isotherms are presented along with repeat measurements series to confirm the results of the novel technique. The obtained PCI data are compared with pressure-concentration isotherms from the literature to validate the measurement method and system. The primary equilibrium data in this work are in very good agreement with both the repeat measurements and the comparison with literature data. It can be shown that the method as well as the experimental design are valid and capable of providing accurate measurements of hydrogen sorption behavior.