Hydrogen in Steel Measurements with the UHV-TPD Workstation

Determination of hydrogen bound in steel is an important factor in developing new steel types for ever more demanding applications.

Temperature Programmed Desorption (TPD), also known as Thermal Desorption Spectrometry (TDS) or Thermal Desorption Analysis (TDA) is a well-established technique for analysing the hydrogen content in such samples. Analysis by TPD involves positioning the sample in an Ultra High Vacuum (UHV) chamber and heating the sample at different linear temperature ramp rates while collecting the desorption spectra using a quadrupole mass spectrometer.

In industries such as oil extraction the steels used in deep reservoir drilling presents significant technical challenges. The deeper the reservoir the greater requirement for materials that can perform at higher operating temperatures and pressures. It is not appropriate to simply increasing steel strength for such sub-sea applications because the accompanying microstructure exacerbates the susceptibility to hydrogen embrittlement. To produce steel suitable for these harsh environments the toughness and ductility are often sacrificed for strength while the different characteristics are balanced. Therefore the challenge is to improve multiple properties without detriment to others. Additionally, the presence of hydrogen that arises through cathodic protection or the transportation of hot fossil fuels is a major concern and its ingress in to the steel can lead to embrittlement. The Hiden TPD Workstation can be used to determine the quantity and binding strength of the hydrogen trapped in steel samples.

UHV-TPD with Hiden Analytical

Hiden Analytical’s complete experimental UHV-TPD Workstation is equipped with a multiport UHV sample chamber and a heated sample stage of up to 1000 °C with integrated PID controls. An optional cooled sample stage with dry atmosphere glove box introduction system allows liquid N2 cooled samples to be inserted into the system and temperature ramps initiated from -60 °C.  This hardware is equipped with a high precision triple filter analyser, for time/temperature-resolved analysis of desorbed species with unmatched sensitivity and is ideal for hydrogen isotope analysis. This equipment has proven successful in numerous areas of product and technology research and development, including:

  • Thin films
  • Photovoltaics
  • Semiconductors
  • Materials characterisation
  • H2/D2/T characterisation in fusion reactor wall tiles
  • Surface science

The UHV-TPD workstation is geared towards the study of hydrogen in metals for research and development purposes.

UHV-TPD studies are also focused on the outgassing properties of high performance materials used in extreme environments, with fully-automated temperature control and analysis enabling high-throughput TPD measurements of coated silicon surfaces.

UHV-TPD Workstation from Hiden Analytical

Hiden Analytical has been developing, manufacturing, and supplying cutting-edge quadrupole mass spectrometers for some of the most advanced forms of material analysis currently performed. Our UHV-TPD workstation provides a unique solution for advanced electronics manufacturing and research and development into novel energy storage materials.

If you would like any more information about any Hiden Analytical instrument, please do not hesitate to contact us directly.

SSITKA study of complete methane oxidation on palladium and platinum catalysts

Authors: Marek Rotko, Andrzej Machocki

The catalytic process of complete methane oxidation is a highly promising alternative to flame combustion, because it makes it possible to reduce the emission of NOX, CO and non-oxidized hydrocarbons into the Earth’s atmosphere. Some of the most active catalytic materials for complete methane oxidation are supported palladium and platinum catalysts. They demonstrate very high activity and selectivity; also, their resistance to high temperature and mechanical damage is acceptable. However, for the wide application of palladium and platinum catalysts in the industry, there is still a need for clear answers to many important questions. One of the most crucial issues is the reaction mechanism of complete methane oxidation over palladium and platinum catalysts. We studied this problem by means of the SSITKA method (Steady State Isotopic Transient Kinetic Analysis).

The SSITKA method enables obtaining much unique and valuable information concerning mechanisms of various heterogeneous catalytic reactions, as well other equally important issues such as: the number of active centres on the catalyst surface, an average surface life-time and surface concentrations of reagents, intermediates and products of the catalytic reaction. However, the SSITKA study needs very high-quality and precise equipment, in particular, a system of dosing and fast switching of reagent streams as well as a mass spectrometer, which makes it possible to investigate even extremely low changes in the concentration of isotopes. In our experiments, the switches between reaction streams including 12CH4/Ar/O2/He and 13CH4/Kr/O2/He as well as between 16O2/Ar/CH4/He and 18O2/Kr/CH4/He were carried out. The examples of results for the Pd-Pt/Al2O3 catalyst are included in Fig. 1.

Fig. 1. Effect of the switching between reaction streams including 16O2/Ar/CH4/He and 18O2/Kr/CH4/He (X is the conversion of methane).
Fig. 1. Effect of the switching between reaction streams including 16O2/Ar/CH4/He and 18O2/Kr/CH4/He (X is the conversion of methane).

On the basis of such results and after a comprehensive analysis (widely described in the reference paper), it has been proposed that two different kinds of active centres (α – more active, but less numerous and β – less active, but more numerous) exist on the catalyst surface and the process of methane oxidation proceeds simultaneously according to two different reaction mechanisms (by Mars-van Krevelen and Langmuir-Hinshelwood). The level of their participation in methane oxidation is different and depends on the reaction temperature. What is more, the process of methane oxidation proceeds not only simultaneously, according to two different reaction mechanisms, but also with different reaction rates determined by the type of active centres.

Project summary by:

ssitka-logoMarek Rotko, Andrzej Machocki
University of Maria Curie-Skłodowska
Faculty of Chemistry
Department of Chemical Technology
3 Maria Curie-Skłodowska Square
20-031 Lublin

Paper Reference:

  1. Rotko, A. Machocki, G. Słowik (2014) “The mechanism of the CH4/O2 reaction on the Pd-Pt/γ-Al2O3 catalyst: A SSITKA study” Applied Catalysis B: Environmental, 160-161 298-306
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Dehydrogenation mechanism of LiBH4 by Poly(methyl methacrylate)

Hydrogen is considered as a promising alternative energy carrier owing to its high-energy density, abundance, light weight and pollution-free burning [1]. Developing a safe and efficient hydrogen storage material is one of the key challenges for the mobile application of hydrogen [2]. Due to the high gravimetric (18.5 wt.%) and volumetric (121 kg H2/m3) hydrogen density, lithium borohydride (LiBH4) has been acknowledged as a potential candidate for hydrogen storage materials [3]. However, due to the unfavorable high thermal stability (e.g. decomposition peak temperature of ~ 470 °C), the practical utilization of LiBH4 as hydrogen storage medium is hampered [4]. Hence, several approaches including reactant destabilization, catalyst/additive introduction, nanostructuring, and anion/cation substitution have been applied to decrease the dehydrogenation temperature and accelerate the kinetics [5].

Nanoengineering had been demonstrated to be a useful method to reduce the dehydriding/rehydriding temperature of LiBH4 by decreasing diffusion path lengths and increasing surface areas [6]. However, nanoscale LiBH4 is too reactive and very sensitive to the water and oxygen in the air, which impede its practical utilization. PMMA ((Poly (methyl methacrylate))), with a high permeability ratio of H2/O2, was reported to have good gas selectivity [7]. Therefore, in this project, PMMA was applied to protect LiBH4 from oxygen and water but let the hydrogen get in or out freely (Scheme 1). Furthermore, the nanoconfinement of LiBH4 in the fine network pore of PMMA and the interaction between the B atom in LiBH4 and the O atom in C=O of PMMA resulted in a much lower hydrogen release temperature of LiBH4. LiBH4 PMMA composite started to dehydrogenate at 53oC and released 5.2 wt.% of hydrogen at 162oC within 1 h. This project provides a general strategy to utilize a gas-selective polymer to protect air-sensitive hydrogen storage compounds and improve their hydrogen storage properties.

Scheme 1. Schematic illustration of LiBH4 protected from oxygen and water by PMMA.
Scheme 1. Schematic illustration of LiBH4 protected from oxygen and water by PMMA.


[1] Jain, I. P. Int J Hydrogen Energ 2009, 34, (17), 7368-7378.

[2] Schlapbach, L.; Zuttel, A. Nature 2001, 414, (6861), 353-358.

[3] Züttel, A.; Wenger, P.; Rentsch, S.; Sudan, P.; Mauron, P.; Emmenegger, C. J Power Sources 2003, 118, (1-2), 1-7.

[4] Saldan, I. Cent Eur J Chem 2011, 9, (5), 761-775.

[5] Li, H.-W.; Yan, Y.; Orimo, S.-i.; Züttel, A.; Jensen, C. M. Energies 2011, 4, (1), 185-214.

[6] Fang, Z. Z.; Wang, P.; Rufford, T. E.; Kang, X. D.; Lu, G. Q.; Cheng, H. M. Acta Mater 2008, 56, (20), 6257-6263.

[7] K. J. Jeon, H. R. Moon, A. M. Ruminski, B. Jiang, C. Kisielowski, R. Bardhan and J. J. Urban, Nat. Mater., 2011, 10, 286.


 Project summary by:

Jianmei Huang, Liuzhang Ouyang, Min ZhuSchool of Materials Science and Engineering

Key Laboratory of Advanced Energy Storage Materials of Guangdong Province,South China University of Technology,

Guangzhou 510641

People’s Republic of China


Paper Reference:

Jianmei Huag et al. (2015) “Dehydrogenation mechanism of LiBH4 by Poly(methyl methacrylate)” Journal of Alloys and Compounds 645 (1), S100-S102


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Multifunctionality of Silver Closo-boranes

As a successor of research based on metal borohydrides, higher boranes are being investigated. Ag2B12H12 and Ag2B10H10 are synthesized and found to possess very high ion conductivities, as well as being semiconducting. In the course of decades, research on borane materials has broadened to embrace many different properties other than hydrogen storage properties. This is an example of unravelling such useful properties, serving as a basis for further property studies of related materials.

Ag2B12H12 reduces to metallic silver, by exposure to an electron beam (TEM), and as such caught attention for further work. Silver boranes are also complexed with AgI in order to access high ion conductivities at room temperature. Synthesis is straight forward, and is achieved in water as a solvent, yielding the desired materials. It is crucial to ensure that residual water is fully removed, to perform reliable quantification of semi-conducting and ion conducting properties. For this purpose, mass spectrometry was employed, analyzing the release of any residual gases, providing assurance of completely dry and water free samples. The gas spectrum was also analyzed to determine the thermal stability of the silver boranes and understand their decomposition mechanism.

The Hiden Analytical HPR-20 quadrupole mass spectrometer was utilized and allowed for unambiguous determination of the water content, as well as ensuring that no undesired impurities are present. At the University of Aarhus, Department of Chemistry and iNANO center, daily investigations of e.g. borane materials are aided by analysis of residual gases released from materials studied as either classical hydrogen storage materials, or as demonstrated here, for other purposes. The information gained is valuable in evaluating synthesis methods, evaluating the purity of materials, and for studies of behavior upon thermal decomposition of materials.

Hydrogen evolution as the silver boranes decompose, is evident from the data presented in the DSC/MS figures. Both compounds decompose above 250oC, releasing an appreciable quantity of hydrogen. Heating to high temperatures for ion conductivity studies it is obvious that no decomposition or release of any gaseous species is observed. Thus, the information from the mass spectroscopy data assures that the samples are pure and that the derived properties are quantified accordingly.

Project Summary by:

Bo Richter and Torben R. Jensen

Department of Chemistry and Interdisciplinary Nanoscience Center (iNANO), Center for Materials Crystallography (CMC), Aarhus University, Denmark.

www.chem.au.dk / www.inano.au.dk




Paper Reference:

“Multifunctionality of silver closo-boranes” Nature Communications 8, Article number: 15136 (2017). doi:10.1038/ncomms15136


Differential scanning calorimetry (DSC) and mass spectroscopy (MS) data of Ag2B10H10 (top) and Ag2B12H12 (bottom). Two DSC measurements are shown for each material, one illustrating decomposition (solid line) and another showing the polymorphic phase transformation (dashed line). The MS trace is shown in the bottom part of the graphs.
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An experimental assessment of the ammonia temperature programmed desorption method for probing the surface acidic properties of heterogeneous catalysts

The aim of this work was to study the surface acidic properties of oxide catalysts and carriers (g-Al2O3, CeO2, ZrO2, SiO2, TiO2, HZSM5 zeolite), comparatively probing their surfaces by ammonia temperature programmed desorption (ATPD) measurements. ATPD is a simple and reliable technique in which a surface, after saturation with ammonia at low temperature, is subject to a temperature ramp, which causes desorption of the probe molecule along with a temperature profile. By qualitatively and/or quantitatively analyzing the desorption pattern, it is possible to obtain information about the adsorption/desorption energy and the quantity of ammonia that has been adsorbed on the surface (ammonia uptake). Since ammonia is a basic molecule, it can be used as a probe to investigate surface acidity. This information can help understand the catalytic behavior of a sample, or even help in fine tuning the synthesis of new systems. Instead of using a traditional TCD Detector for this task, we employed a Quadrupole Mass Spectrometer (Hiden HPR-20 EGA) connected through a heated capillary to our testing apparatus.

The Hiden HPR-20 EGA in the Lab used for characterisation and testing of catalytic samples
The Hiden HPR-20 EGA in the Lab used for characterisation and testing of catalytic samples

The use of a QMS allowed us to easily discriminate between the different species desorbing from our surfaces, without the use of any kind of chemical or physical filter and traps which could negatively affect our analyses. By properly tuning the ionization potential of our instrument, we were also able to avoid water molecule fragmentation and related interference with the ammonia m/z signal. The reliability and accuracy of the ATPD data were assessed by theoretical criteria and experimental tests highlighting the effects of carrier gas, data acquisition mode, catalyst particle size and reactor geometry, remarking the flexibility of the technique employed. All of the studied materials featured complex ATPD patterns spanned in the range 423-873K, except for ceria which showed a narrow and resolved desorption peak, indicative of homogeneous weak acidity. Quantitative data signalled a difference of more than one order of magnitude in ammonia uptake between silica and the other materials. Since the ATPD profiles of ceria match Gaussian curves regardless of heating rate and surface coverage, the patterns of the studied materials are described as linear combinations of four Gaussian functions related to weak, medium, strong and very strong site populations. After collecting all the profiles, we were able to apply ATPD modelling analyses to get information about the energy of adsorption of the probe molecule related to each desorbing temperature. The cumulative energy site distributions indicated the following acidity scale based on the average energy (expressed in kJ/mol) value (e.g., surface coverage q=0.5)

CeO2 (100) <g-Al2O3 (111) » ZrO2 (111) » TiO2 (117) » SiO2 (118) < HZSM5 (135)

In order to acquire additional information on the functionality of the studied materials, we performed dehydration of isopropanol to propylene as a probe reaction. The results obtained matched the ones previously uncovered by ATPD measurements in terms of abundance and strength of surface acid sites, but also let us distinguish between Brønsted and Lewis acidic sites.

Figure 1: (Left) Deconvolution of ATPD profiles by Gaussian functions (dotted yellow lines depict the generated profiles, while black points are the experimental data); (Right) Energy distribution functions of ammonia desorption from the various site populations.
Figure 1: (Left) Deconvolution of ATPD profiles by Gaussian functions (dotted yellow lines depict the generated profiles, while black points are the experimental data); (Right) Energy distribution functions of ammonia desorption from the various site populations.

unime-logoProject Summary By:

Roberto Di Chio

Dipartimento di Ingegneria,

Università degli Studi di Messina,

Contrada Di Dio, Sant’Agata,

I-98166 Messina, Italy

Paper Reference:

Francesco Arena, Roberto Di Chio, Giuseppe Trunfio (2015) “An experimental assessment of the ammonia temperature programmed desorption method for probing the surface acidic properties of heterogeneous catalysts” Applied Catalysis A: General 503, 227-236

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Real-time Human Breath Analysis for Cellular Wellbeing


With the advances in medical science and research, the modern academics are vigorously engaging with the development and discover of new technology which can be imbedded into society, furthering medical care and improving lives. Currently, Hiden along with MIMIT, Manchester University and the Manchester University NHS Foundation Trust (MFT) trust have are in collaboration with the focus of non-invasively measuring biomarker compounds in human breath.  Focusing on monitoring cellular wellbeing for the real time diagnosis of diseases, such as sepsis, and real time feedback for therapeutic guidance.

The biomarker compounds selected to be of most interest are Volatile Organic compounds, or VOC for short, are carbon-based chemicals which are present in blood plasma at concentrations of low % to ppb levels.  VOCs act as biomarkers for cellular events brought on by disease, physiological stress or biological event.

Using a sensitive, real time, mass spectrometry (MS), the end goal of the project is to implement a bedside monitor into every NHS hospital.  This device will be able to provide real time analysis of changes at the cellular level of high-risk patients. With this technology, NHS medical staff will be able to monitor the VOCs contained in exhaled breath of their patients allowing them thoroughly understand the magnitude of the metabolic effects and most importantly receive a warning of any imminent cellular changes such as disease progression, and to guide therapies.

During the first phase of the study, one of Hiden’s keen cyclists and Special Projects Manager, Dane, was invited to participate in the development. In order to mimic the physiological disturbances exhibited in critical illness, pilot investigations will be in healthy volunteers undertaking extreme exercise. It is hoped that a library of candidate biomarkers in exhaled breath will be identified for future use in the clinical setting.

For more information on the research project please click here

For more information on breath analysis please click here

Integrated Gas Phase Reaction Studies with the Hiden Analytical QGA Gas Analysis System and Altamira Instrument’s BenchCAT™ Microreactor

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Hiden Analytical are delighted to partner with Altamira Instruments for the integration of Hiden’s QGA quantitative gas analysis system with Altamira’s range of custom-designed, fully automated, BenchCAT™ microreactors.


Bringing together the latest in custom reactor design and precision gas analysis capability the integrated package provides for sub ppm detection of reagent gases and reaction products in an extensive range of single and multi-reactor applications. Key applications include; catalyst characterization and screening, emissions monitoring, gasification, fuel cell development, bio-gas studies and pyrolysis.

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To configure your ideal reactor and gas analysis package please contact Hiden Analytical at info@hiden.co.uk

What is TPO and Why is it Performed?

Temperature programmed oxidation (TPO) is an analytical technique capable of characterising catalysts and is an important consideration for research and development.

The performance of TPO requires a furnace or microreactor capable of increasing temperatures of a catalyst in precise increments up to extreme conditions, for example in brackets of 1-20°C min-1 up to 1000°C. An integrated mass spectrometer allows for constant real-time analysis of catalytic activity throughout a given thermal reaction, in which a gas mixture will flow over a catalyst throughout an incrementally programmed temperature rise.

Hiden Analytical -TPO

During the experiment’s temperature ramp, various reactions will occur between the gas flowing and the catalyst in the microreactor. For example, coke build-up on the catalyst (blocking reaction sites and reducing efficiency) during pyrolysis reactions can be investigated by using an oxygen flow and TPO experiments. The coke can be characterised by measurement of the carbon monoxide and carbon dioxide and hydrocarbon species on the reactor outlet.

TPO is typically used to provide insights into various catalytic reactions with an array of applications. A popular application is research and development of alternative energy fuels and increased energy efficiency chemical manufacture.

For example, hydrogen (H) based fuel cells have emerged as a highly-efficient, low-pollutant energy source which is gradually being introduced in fuel cell electric vehicles (FCEVs) with a positive yet potentially superficial impact on greenhouse gas emissions. The problem with this exciting process is that the primary method of hydrogen production is natural gas reformation. Steam-hydro carbonation reforming reacts a natural hydrocarbon such as methane (CH4) with high pressure steam at up to 1000°C in the presence of a catalyst. This produces hydrogen for use in various industries, including for implementation in greener energy sources. However, this process has very high energy demands, significantly reducing the environmental benefits of the end-product. TPO is used to characterise coke during this reaction.

Want to learn more? Read about our Tools for Catalysis Research

Researchers have been considering alternatives to natural gas reformation for years, including partial oxidation processes, while improvements to the existing manufacture of hydrogen include looking for ways to augment natural gas reformation processes with production from renewable energy sources. This research requires extensive consideration and analysis of catalytic materials, and TPO is uniquely suited to provide dynamic and accurate data in this field of research.

TPO Mass-Spectrometers from Hiden Analytical

Hiden Analytical has developed and manufactured a modular bench-top analytical system known as CATLAB-PCS, capable of performing TPO with seamless data acquisition from the in-bed thermocouple, allowing researchers to directly monitor catalyst temperature. It is designed to allow for automated and repeatable catalyst characterization studies using TPO principles.


The integrated microreactor CATLAB-PCS module system has already been prepared for the characterization of nickel-based catalysts for partial oxidation of methane. This exothermic reaction is proven to reduce the energy demands of natural gas reformation because it is a relatively exothermic reaction which occurs at an exorbitantly higher rate than high-pressure reformation. Using TPO, researchers hoped to determine the catalytic properties of the low-cost metal nickel (Ni) with methane, which is stable and active enough to partially oxidize with methane, although it exhibits a risk of sintering at high temperatures.

This is just one of the established areas of research of TPO-enabled products from Hiden Analytical, with potential for the further characterization and analysis of reaction mechanisms and oxidation of catalysts for a range of applications. If you would like to find out more about TPO, please contact us.

How Gas Analyzers Can Benefit the Automotive Industry

Emissions standards imposed upon auto engineering firms in the US could be set to change, as the Environmental Protection Agency reviews the current standards which have been in place since 2012. The EPA are considering redressing the greenhouse gas emissions standards for light-duty vehicles due for production in the model years 2022—2025, citing changing economic circumstances as the reason behind the potential shift. Automakers are divided as to the environmental and commercial impact of rolling back these stringent emissions standards, as contemporary gas analyzers are successfully optimizing vehicles in terms of CO2 emissions and fuel efficiency in-line with existing EPA standards.

There is a global trend towards decreasing greenhouse gas emissions in the automotive industry, with increasing numbers of consumers considering reduced emissions as a key performance indicator of a new vehicle. Mass spectrometers, including gas analyzers, for the automotive industry will therefore be of continued importance as American auto manufacturers react to contrasting environmental demands from domestic and global markets.

Gas analyzers are chiefly implemented to monitor the chemical composition of a vehicle’s emissions, yet there increasing applications for such mass spectrometers within the automotive industry:

A laboratory scale fuel cell

Gas Analyzers for Catalyst Characterization

According to the EPA, the transportation sector is responsible for approximately 27% of the US’s total greenhouse gas emissions, and roughly 60% of that figure comes a result of the use of light-duty vehicles. These significant percentages have influenced widespread research into the environmental optimization of essential vehicles, through the introduction of automotive catalysts designed to reduce atmospherically-harmful emissions. Catalytic converters with high geometric surface areas are fitted to exhaust outlets to oxidize pollutant gases, converting carbon monoxide (CO) to carbon dioxide (CO2) for example. This component was made mandatory for any vehicle from the model year 1975.

Vehicle requirements, capabilities, and specifications have changed in the decades since, and continuing innovation in the automotive industry demands improved catalytic materials. Microreactor gas analyzers can perform kinetic and thermodynamic measurements of catalysts to ensure real-world performance of catalytic converters at temperatures up to 1000°C, as well as establishing the agglomeration properties of new catalytic materials which may result in decreased performance after lengthy periods of service due to soot build-up and subsequent surface area degradation.

The CATLAB-PCS combines multiple gas/vapor feeds, a microreactor and mass spectrometer into a single instrument and provides the ideal platform for advanced catalysis research, providing for detailed catalysis reaction analysis combined with TPD/TPR studies.

The CATLAB-PCS system from Hiden Analytical features seamless hardware and software integration with a fast-response time and integrated air-cooling for accurate catalyst characterization.

Gas Analyzers for Advanced Fuel Cell Research

Gasoline is still the primary fuel source used for automobiles across the world, while diesel fuel remains relatively established in the European market. However, enormous improvements in the electric vehicle industry have significantly reduced consumer concerns about the performance qualities of vehicles which run on alternative sources of fuel. This increasing market awareness and favor towards electric vehicles has invigorated research into cheaper and more efficient cars which eschew fossil fuels in favor of battery, motor, and / or fuel cell setups.

Specialist gas analyzers are available for fuel cell research, to monitor the attributes of evolved gases and vapors in a range of conditions. Hydrogen (H2) gas for example has emerged as a potential candidate for use in automotive fuel cells, but viable hydrogen must meet stringent purity requirements to be used in a vehicle’s fuel cell – otherwise the electrodes may become poisoned, rendering the full cell unrepairable.

The QGA compact bench-top system from Hiden Analytical is capable of high-purity gas analysis and is ideally suited for use in fuel cell research, with an internal gas and vapor mass spectral library and an intelligent scan feature.

Gas Analyzers from Hiden Analytical

Hiden Analytical has been developing and manufacturing gas analyzers for real-time gas / vapor analysis and characterization of catalysts for 35 years, with a proven expertise in various industries requiring mass spectrometry equipment.

If you would like any more information on our gas analyzers which are suitable for use in the automotive industry, please do not hesitate to send us a message.