WO2018001907A1 - Apparatus and processes for monitoring the quality of hydrogen - Google Patents

Apparatus and processes for monitoring the quality of hydrogen Download PDF

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Publication number
WO2018001907A1
WO2018001907A1 PCT/EP2017/065586 EP2017065586W WO2018001907A1 WO 2018001907 A1 WO2018001907 A1 WO 2018001907A1 EP 2017065586 W EP2017065586 W EP 2017065586W WO 2018001907 A1 WO2018001907 A1 WO 2018001907A1
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WO
WIPO (PCT)
Prior art keywords
hydrogen
gas composition
flow control
control unit
delivery line
Prior art date
Application number
PCT/EP2017/065586
Other languages
French (fr)
Inventor
Jurgen Johannes Jacobus Louis
Lars Christian ZIMMERMANN
Alice Margaret Sophie Elliott
Original Assignee
Shell Internationale Research Maatschappij B.V.
Shell Oil Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shell Internationale Research Maatschappij B.V., Shell Oil Company filed Critical Shell Internationale Research Maatschappij B.V.
Publication of WO2018001907A1 publication Critical patent/WO2018001907A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0011—Sample conditioning
    • G01N33/0016—Sample conditioning by regulating a physical variable, e.g. pressure or temperature
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C5/00—Methods or apparatus for filling containers with liquefied, solidified, or compressed gases under pressures
    • F17C5/002—Automated filling apparatus
    • F17C5/007—Automated filling apparatus for individual gas tanks or containers, e.g. in vehicles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22—Fuels; Explosives
    • G01N33/225—Gaseous fuels, e.g. natural gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2221/00—Handled fluid, in particular type of fluid
    • F17C2221/01—Pure fluids
    • F17C2221/012—Hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
    • F17C2223/0107—Single phase
    • F17C2223/0123—Single phase gaseous, e.g. CNG, GNC
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/01—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the phase
    • F17C2225/0107—Single phase
    • F17C2225/0123—Single phase gaseous, e.g. CNG, GNC
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2225/00—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel
    • F17C2225/03—Handled fluid after transfer, i.e. state of fluid after transfer from the vessel characterised by the pressure level
    • F17C2225/036—Very high pressure, i.e. above 80 bars
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/03—Control means
    • F17C2250/032—Control means using computers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/04—Indicating or measuring of parameters as input values
    • F17C2250/0404—Parameters indicated or measured
    • F17C2250/0447—Composition; Humidity
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/06—Controlling or regulating of parameters as output values
    • F17C2250/0605—Parameters
    • F17C2250/0626—Pressure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2250/00—Accessories; Control means; Indicating, measuring or monitoring of parameters
    • F17C2250/06—Controlling or regulating of parameters as output values
    • F17C2250/0605—Parameters
    • F17C2250/0636—Flow or movement of content
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2260/00—Purposes of gas storage and gas handling
    • F17C2260/05—Improving chemical properties
    • F17C2260/056—Improving fluid characteristics
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2265/00—Effects achieved by gas storage or gas handling
    • F17C2265/06—Fluid distribution
    • F17C2265/065—Fluid distribution for refueling vehicle fuel tanks
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2270/00—Applications
    • F17C2270/01—Applications for fluid transport or storage
    • F17C2270/0134—Applications for fluid transport or storage placed above the ground
    • F17C2270/0139—Fuel stations
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2270/00—Applications
    • F17C2270/01—Applications for fluid transport or storage
    • F17C2270/0165—Applications for fluid transport or storage on the road
    • F17C2270/0184—Fuel cells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0011—Sample conditioning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004—CO or CO2
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/0054—Ammonia
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/45—Hydrogen technologies in production processes

Definitions

  • This invention relates to an apparatus and one or more processes for monitoring the quality of gaseous hydrogen dispensed to hydrogen users.
  • Hydrogen fuel cells are devices that convert the chemical energy of hydrogen into electrical energy, which then can be used, for example, by electrical motors to drive machinery.
  • Such machinery may include motor vehicles .
  • hydrogen fuel cells have incorporated in them precious and/or rare metals, such as platinum, acting as catalytically active components. These precious and/or rare metals are essential to the fuel cell' s function, however their catalytic activity is susceptible to deactivation by impurities and/or contaminants that may be present in the hydrogen supplied to the fuel cell.
  • impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water. The levels and the nature of these impurities and/or contaminants depend on how the supplied hydrogen was produced, stored, transported and/or conveyed to the fuel cell. Whilst the adverse effect of impurities and/or contaminants such as carbon monoxide may be reversible, the adverse effect of some sulphur compounds is not reversible. Irreversible adverse effects on a fuel cell are cumulative and ultimately detrimental to its
  • Hydrogen may also contain inert impurities and/or contaminants such as nitrogen, and although they do not adversely affect any fuel cell components, they dilute the hydrogen, thereby reducing the amount of electricity that can be generated by the fuel cell from a given volume of gas. Therefore both the retailers of hydrogen as a fuel for fuel cells, and the user of such hydrogen need to know the purity of the supplied hydrogen.
  • the hydrogen produced at a central production facility may comply with ISO 14687-2-2012, impurities may contaminate the hydrogen while it is conveyed into, for example, a distribution truck. It is therefore desirable to know the quality of the gaseous hydrogen supplied to any hydrogen utilising vehicles by assessing it immediately before it enters the vehicle' s storage tank.
  • SAE J2601 a widely accepted standard for hydrogen refuelling, mandates that light-duty vehicles are refuelled to 70 MPa and heavy-duty vehicles are refuelled to 35 MPa, over a time of 3 to 5 minutes.
  • the current practical way of monitoring hydrogen quality is to transfer a hydrogen sample from the dispenser equipment/system into a sample bottle, take the sample bottle to a laboratory and to analyse the sample in the laboratory using techniques such as gas chromatography, mass spectroscopy,
  • GC-MS chromatography mass spectroscopy
  • infrared spectroscopy and/or Fourier transform infrared
  • FTIR spectroscopy
  • Linde have developed a hydrogen gas sampling instrument marketed under the trade mark x 3 ⁇ 4 QUALITIZER' (a trade mark owned by Linde AG) , which is fitted at the downstream end of the dispensing system to enable hydrogen samples to be bled and captured in specially lined sample cylinders.
  • the use of the ⁇ ⁇ 2 QUALITIZER' has been assessed by the partner of the European Union funded 'HyCora' project (made up of the following partners: VTT Technical
  • the present inventors have provided the invention set out herein which enables the quality of a hydrogen sample representative of the dispensed hydrogen to be obtained and analysed within a hydrogen refuelling/retail station's dispenser equipment/system, either during or shortly after, vehicle refuelling.
  • the present invention provides an apparatus for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, comprising a pressurised hydrogen source (1), a first flow control unit (2); a hydrogen delivery line (3), a sample
  • the first flow control unit (2) regulates the pressure and the amount of hydrogen that may flow from the pressurised hydrogen source (1) into the hydrogen delivery line (3); wherein the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5); wherein at the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other; wherein the sampling line (7) supplies at least a quantity of hydrogen from the sample
  • the gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of hydrogen from the gas composition analyser (8); and wherein the downstream end of the lower section of the hydrogen delivery line (5) is connected to and is in fluid communication with the hydrogen dispensing nozzle (9) .
  • the present invention also provides a first process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen: wherein a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2); wherein a second quantity of hydrogen is released by the first flow control unit (2) towards a sample withdrawal zone (6); wherein a third quantity of hydrogen is diverted at the sample withdrawal zone (6) into a sampling line (7), leaving a remainder of the second quantity of hydrogen available for dispensing to a hydrogen user (x) via a lower section of the hydrogen delivery line (5) and via a hydrogen dispensing nozzle (9); and wherein the
  • composition of the third quantity of hydrogen is analysed by a gas composition analyser (8) .
  • the present invention also provides a second process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, wherein a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2); wherein a second quantity of hydrogen is released by the first flow control unit (2) towards a hydrogen dispensing nozzle (9) via a hydrogen delivery line (3); wherein at least a portion of the second quantity of hydrogen is dispensed via the hydrogen dispensing nozzle (9) to a hydrogen user (x) leaving a third quantity of hydrogen retained in the hydrogen delivery line (3); and wherein at least a portion of the third quantity of hydrogen is released into a sampling line (6) and supplied to a gas
  • composition analyser (8) and its composition is analysed by the gas composition analyser (8) .
  • Figure 1 shows a simplified schematic diagram of the apparatus according to the invention.
  • Figure 2 shows a simplified schematic diagram of an embodiment of the apparatus according to the invention, which carries out an embodiment of the process according to the invention.
  • the apparatus of the present invention not only dispenses gaseous hydrogen to hydrogen users such as to hydrogen utilising vehicles, but also enables quality analyses to be carried out on samples of gaseous hydrogen which are representative of the hydrogen that is supplied by the apparatus to each hydrogen user.
  • the apparatus of the present invention comprises a pressurised hydrogen source (1) .
  • the pressurised hydrogen source (1) supplies gaseous hydrogen to a first flow control unit (2) suitably at a pressure of between at least 20 MPa and 107.5 MPa.
  • the pressure of the gaseous hydrogen supplied to the first line for hydrogen flow is at least 20 MPa, more preferably at a pressure of at least 45 MPa and even more preferably at a pressure of at least 90 MPa.
  • the pressurised hydrogen source (1) may be, for example, any hydrogen storage tank of a type known to the skilled person which is capable of storing hydrogen gas preferably at any one of the abovementioned pressures.
  • the pressurised hydrogen source (1) also may be a hydrogen supply line, supplying gaseous hydrogen from a hydrogen distribution network or from a hydrogen production facility, which can deliver gaseous hydrogen preferably at any one of the abovementioned pressures.
  • the pressurised hydrogen source (1) may be also a type of gaseous hydrogen production equipment preferably located at a hydrogen retail site, such as but not limited to, methane steam reformer (s), solid oxide fuel cell(s) with hydrocarbon reforming capability, and/or a water electrolysis unit(s) .
  • the pressurised hydrogen source (1) may comprise, for example, a combination of a hydrogen supply line feeding gaseous hydrogen into a hydrogen storage tank, or a hydrogen production equipment feeding gaseous hydrogen into a hydrogen storage tank.
  • the pressurised hydrogen source (1) may also comprise one or more gaseous hydrogen compressor ( s ) so that the pressurised hydrogen source (1)
  • pressurised hydrogen source (1) is able to provide a gaseous hydrogen output at any one of the abovementioned pressures.
  • the pressurised hydrogen source (1) is not limited to the abovementioned examples, and further may be a mobile gaseous hydrogen transportation unit such as truck- or railway wagon-mounted hydrogen tanks, or a fixed/immobile unit at a distribution/ supply site.
  • the pressurised hydrogen source (1) provides gaseous hydrogen to a first flow control unit (2) .
  • the first flow control unit (2) comprises an inlet in fluid
  • the first flow control unit (2) may be attached directly to the pressurised hydrogen source (1), or may be connected to the pressurised hydrogen source (1) via a hydrogen supply line.
  • a hydrogen supply line suitably an outlet of the pressurised hydrogen source (1), an inlet of the first flow control unit (2) and said hydrogen supply line are in fluid communication with each other to enable the flow of gaseous hydrogen from the pressurised hydrogen source (1) to the first flow control unit (2) .
  • the hydrogen supply line connecting the pressurised hydrogen source (1) to the first flow control unit (2) may be any type of conduit that is suitable for conveying gaseous hydrogen at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
  • the first flow control unit (2) may be any type of flow control unit known to the skilled person that is suitable for regulating the pressure and the amount of gaseous hydrogen at a temperature of as low as at least -
  • the first flow control unit (2) regulates the pressure and the amount of gaseous hydrogen that may flow from the pressurised hydrogen source (1) into a hydrogen delivery line (3) .
  • Such controls may be effected by the user of the apparatus, or by any suitable automated control system.
  • the flow rate and the frequency of such flow are operated by an automated control system, and through such control, suitably the first flow control unit (2) regulates the pressure of the gaseous hydrogen that may flow from the pressurised hydrogen source (1) into a hydrogen delivery line (3), so that, for example, a final gaseous hydrogen refuelling pressure of 70 MPa for light-duty vehicles and 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle (as mandated by hydrogen refuelling standard SAE J2601), or any other hydrogen refuelling pressure (s) mandated by a standard that may be applicable at the location at the time of refuelling.
  • a final gaseous hydrogen refuelling pressure of 70 MPa for light-duty vehicles and 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle (as mandated by hydrogen refuelling standard SAE J2601), or any other hydrogen refuelling pressure (s) mandated by a standard that may be applicable at the location at the time of refuelling.
  • the apparatus of the present invention also relates to the apparatus of the present invention.
  • the hydrogen delivery line comprises an upper section (4) and a lower section (5) .
  • the references used herein to "upper” and “lower”, as well as references to “upstream” and “downstream” are with respect to the general overall hydrogen flow along the apparatus, i.e. "upper” and “upstream” (as the context so requires) refer to the pressurised hydrogen source (1) end of the apparatus, and “lower” and “downstream” (as the context so requires) refer to the hydrogen dispensing nozzle (9) end of the apparatus .
  • the upstream end of the upper section of the hydrogen delivery line (4) is in fluid communication with an outlet of the first flow control unit (2), such that the gaseous hydrogen released by the first flow control unit (2) may flow into, and along, the upper section of the hydrogen delivery line (4), thereby supplying gaseous hydrogen from the first flow control unit (2) to a sample withdrawal zone (6) .
  • the lower section of the hydrogen delivery line (5) supplies gaseous hydrogen from the sample withdrawal zone (6) to a hydrogen dispensing nozzle (9), as the
  • downstream end of the lower section of the hydrogen delivery line (5) is in fluid communication with hydrogen dispensing nozzle (9) .
  • the apparatus of the present invention also relates to the apparatus of the present invention.
  • the sampling line supplies gaseous hydrogen from a sample withdrawal zone (6) to a gas composition analyser (8) .
  • a gas composition analyser (8) At the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line
  • the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other.
  • each of the upper section of the hydrogen delivery line (4), the lower section of the hydrogen delivery line (5) and the sampling line (7) is any type of conduit that is suitable for conveying gaseous hydrogen at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
  • the downstream end of the upper section of the hydrogen delivery line (4) and the upstream end of the lower section of the hydrogen delivery line (5) may each house one or more flow control device (s) that control the direction of gaseous hydrogen flow along said sections of the hydrogen delivery line (4), as well as the amount of gaseous hydrogen flow along and between said sections.
  • the sampling line (7) comprises a second flow control unit (11) that can regulate the flow of gaseous hydrogen from the sample withdrawal zone (6) to the gas composition analyser (8) .
  • the second flow control unit (11) may be an alternative to the flow control device (s) mentioned in the preceding paragraphs, or may be in addition to any one of the flow control device (s) mentioned in the preceding paragraphs.
  • the second flow control unit (11) is any type of flow control system known to the skilled person that is that suitable for controlling gaseous hydrogen flow at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
  • the second flow control unit (11) may comprise a check valve component or a one-way flow regulator component to prevent backflow of gaseous hydrogen into the sample withdrawal zone (6) .
  • the second flow control unit (11) may also be capable of isolating the sampling line (7) from the sample withdrawal zone (6), to enable a gas composition analyser (8) to retain at least a portion of gaseous hydrogen, so that it may carry out an analysis of its composition.
  • isolating the sampling line may also enable maintenance to be carried out on the gas composition analyser (8) without affecting the
  • the second flow control unit controls (11) the amount of gaseous hydrogen and its flow rate along the sampling line (7), as well as the timing and the frequency of such flow.
  • Such controls may be effected by the user of the apparatus, or by any automated control system.
  • the flow rate and the frequency of such flow are operated by an automated control system.
  • the sampling line supplies gaseous hydrogen to a gas composition analyser (8) suitable for detecting
  • the gas composition analyser (8) may be any gas analyser that is capable of detecting and measuring the concentration of any one or more of the impurities and/or contaminants that may be capable of affecting the functioning of hydrogen fuel cells at ppm levels, and more preferably at sub-ppm levels.
  • the x ppm' levels and ⁇ sub-ppm' levels refer to the concentration of such impurities and/or contaminants when the hydrogen gas pressure is about 0.1 MPa.
  • the gas composition analyser may use techniques such as, but not limited to, gas
  • composition analyser (8) may retain a quantity of gaseous hydrogen within it while analysing it, or may also be able to analyse gaseous hydrogen while the hydrogen flows through the gas composition analyser (8) .
  • the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a pressure of below 90 MPa.
  • the gas composition analyser (8) may be also able to analyse gaseous hydrogen
  • composition at a pressure of at least 90 MPa or more.
  • the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of below 90 MPa
  • a gas pressure reduction device (10) will be required to be in place along the sampling line, between downstream of the sample withdrawal zone (6) and upstream of the gas composition analyser (8) .
  • the function of the gas pressure reduction device (10) is to produce a reduced pressure hydrogen sample for the gas composition analyser to analyse.
  • the gas pressure reduction device (10) reduces the pressure of the gaseous hydrogen which it receives from the sample withdrawal zone (6) via the sampling line (7) to a pressure suitable for the gas composition analyser (8) installed as part of the apparatus of the present invention, such as preferably at most 10 MPa, more preferably at most 1 MPa, even more preferably at most 0.5 MPa, and most preferably at most 0.1 MPa.
  • a pressure suitable for the gas composition analyser (8) installed as part of the apparatus of the present invention, such as preferably at most 10 MPa, more preferably at most 1 MPa, even more preferably at most 0.5 MPa, and most preferably at most 0.1 MPa.
  • the gas pressure reduction device (10) may vent a quantity of gaseous hydrogen that it receives without introducing any impurities and/or contaminants into the remaining hydrogen.
  • a one-way flow valve downstream of the gas composition analyser may take part in said venting.
  • the reduced pressure hydrogen sample remaining in the gas composition analyser (8) may be vented without introducing any further impurities and/or contaminants into the gas composition analyser or into the dispenser equipment /system .
  • a one-way flow valve (12) located downstream of the gas composition analyser may be present and suitably prevents the back- flow of any hydrogen destined for venting.
  • the gaseous hydrogen vented either as part of the pressure reduction step(s), or which went through the gas composition analyser may be released to the atmosphere, or used for applications other than for refuelling hydrogen utilizing vehicles, or it may be redirected to the pressurised hydrogen source (1) .
  • the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, suitably no gas pressure reduction device will be required to be in place along the sampling line upstream of the gas composition analyser.
  • the aim of the apparatus of the present invention is not only to dispense gaseous hydrogen to end users, such as hydrogen utilising vehicles, but also to analyse the quality of the dispensed hydrogen which is representative of that supplied to each hydrogen user, so that the supplier and each user of the hydrogen can be informed of its quality.
  • dispenser equipment can be detected by the gas
  • composition analyser just before the gaseous hydrogen is supplied to the hydrogen user.
  • ⁇ (a) ' in Figure 2 may comprise filter (s) to remove particulates, systems to remove water, cooler (s) to cool the gaseous hydrogen that is being dispensed to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, hydrogen flow meter (s) to measure the amount of gaseous hydrogen being dispensed and/or hydrogen compres sor ( s ) to boost the pressure of the gaseous hydrogen being dispensed.
  • said components of the dispenser equipment may also comprise components that measure the temperature of the hydrogen, and ones that regulate the flow of gaseous hydrogen such as, but not limited to, relief valve (s), block valve (s), flow limiter(s), components to induce or inhibit laminar hydrogen flow etc.
  • the apparatus of the present invention not only overcomes the difficulties of analysing the quality of gaseous hydrogen at dispensing pressures of at least 90 MPa, but it also minimises the possibility of
  • the gas composition analyser (8) may be via the gas pressure reduction device depending on whether the gas composition analyser (8) may, or may not, be able to analyse gaseous hydrogen composition at a pressure of below, or above, 90 MPa, as described above.
  • the lower section of the hydrogen delivery line (5) supplies gaseous hydrogen from the sample withdrawal zone (6) to a hydrogen dispensing nozzle (9) .
  • the hydrogen dispensing nozzle (9) can be any nozzle known to the skilled person that is that suitable for conveying gaseous hydrogen at a temperature of as low as at least - 60°C and at a pressure of up to 107.5 MPa to a hydrogen user.
  • the hydrogen dispensing nozzle (9) is suitable for attaching to the fuel storage system of any hydrogen utilizing vehicle, such as to a line (labelled as "(z)" in Figures 1 and 2) for conveying gaseous hydrogen dispensed from the hydrogen dispensing nozzle (9) to a vehicle's hydrogen fuel tank (labelled as " (y) " in
  • the hydrogen dispensing nozzle (9) is capable of regulating the flow rate and the quantity of the gaseous hydrogen supplied to the fuel storage system of the hydrogen utilizing vehicle that is being refueled.
  • such regulation of the flow rate may be effected manually by any operator, or by an automated control system controlled by any such operator .
  • a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2) .
  • the pressure of the gaseous hydrogen in the pressurised hydrogen source (1) provides at least the initial driving force for gaseous hydrogen to flow into the first flow control unit (2) .
  • the pressure within the pressurised hydrogen source (1) may be created and maintained by a hydrogen compressor and/or by the production process that produces such hydrogen.
  • the gaseous hydrogen flow into the first flow control unit (2) may be also assisted by pump(s) capable of supplying gaseous hydrogen at pressure.
  • a second quantity of hydrogen is then released by the first flow control unit (2) towards a sample withdrawal zone (6) along an upper section of a hydrogen delivery line (4) .
  • the second quantity of hydrogen may be equal to, or less than, the first quantity of hydrogen.
  • the first flow control unit (2) regulates the pressure, timing, frequency and the amount of the second quantity of hydrogen supplied towards the sample withdrawal zone (6) .
  • the first flow control unit (2) may regulate the quantity of the second quantity of hydrogen so that it is matched to the quantity of gaseous hydrogen required by a hydrogen user, such as for refuelling a hydrogen utilizing vehicle to its fuel tank' s maximum capacity, or to any percentage of such capacity as may be necessary at the time.
  • the quantity of the second quantity of hydrogen regulated by the first flow control unit (2) so that a hydrogen refuelling pressure of 70 MPa for light- duty vehicles and of 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle as mandated by hydrogen refuelling standard SAE J2601, or any other hydrogen refuelling standard that may be in place at the location and time of refuelling.
  • the flow of the second quantity of gaseous hydrogen into the upper section of a hydrogen delivery line (4), and its frequency of supply may be regulated by the first flow control unit (2) to be continuous or discontinuous depending on the need of the hydrogen user, such as the stage of the refuelling operation, and the flow-rate is regulated to match such stage.
  • the second quantity of hydrogen flows along the upper section of a hydrogen delivery line (4), it may be filtered by filter (s) to remove particulates, its water removed, cooled by cooler (s) to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, its quantity measured by hydrogen flow meter (s) and/or its pressure adjusted to required pressure by hydrogen compressor (s) .
  • additional processes may also take place along the second line for hydrogen flow as necessary for refuelling hydrogen utilising vehicles.
  • such process takes place along the upper section of a hydrogen delivery line (4) between the the first flow control unit (2) and a sample withdrawal zone (6), and its location is suitably depicted in Figure 2 by the section labelled "(a)".
  • the second quantity of hydrogen reaches the downstream end of the upper section of a hydrogen delivery line (4) it reaches a sample withdrawal zone (6) where a third quantity of hydrogen is diverted into a sampling line (7), leaving a remainder of the second quantity of hydrogen available for dispensing to a hydrogen user (x) .
  • the remainder of the second quantity of hydrogen may be dispensed to a hydrogen user (x) by conveying it initially via a lower section of the hydrogen delivery line (5), then via a hydrogen
  • the second flow control unit (11) also regulates the amount of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas composition analyser (8) .
  • the second flow control unit (11) also regulates the frequency of the supply of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas
  • composition analyser (8) composition analyser (8) .
  • Such regulation may be effected by the user of the apparatus, or by any automated control system.
  • the flow rate and the frequency of such flow are operated by an automated control system.
  • one or more other flow control device located at, or in the vicinity of, the sample withdrawal zone (6) (but not along the sampling line (7)), may provide additional means to regulate the amount of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas composition analyser (8) .
  • the sampling line (7) supplies the third quantity of hydrogen diverted from the sample withdrawal zone (6) into the gas composition analyser (8) .
  • the gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of gaseous hydrogen from the gas composition analyser (8) .
  • a gas composition analyser (8) may involve, but is not limited to, techniques such as gas chromatography, mass spectroscopy and/or infrared spectroscopy, or any combination of techniques, to detect and measure the concentrations of any one or more of such impurities and/or contaminants.
  • impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water.
  • results of such analysis may be presented to the operator of the apparatus of the present invention in electronic form via a visual display unit, and/or in a tangible form such as a print out.
  • the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, so suitably no gas pressure reduction device will be required to be in place along the sampling line (7) upstream of the gas composition analyser .
  • the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa. In such
  • the pressure of the third quantity of hydrogen in the sampling line (7) is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
  • the pressure of the third quantity of hydrogen in the sampling line (7) is reduced to a pressure
  • the gas composition analyser that is installed as part of the apparatus of the present invention to carry out the compositional analysis of the gaseous hydrogen it receives, such reduction being preferably to at most 10 MPa, more preferably to at most 1 MPa, even more preferably to at most 0.5 MPa, and most preferably to at most 0.1 MPa.
  • the gas pressure reduction device (10) may vent a quantity of gaseous hydrogen that it receives without introducing any impurity into the remaining third quantity of hydrogen.
  • the third quantity of hydrogen is diverted at the sample withdrawal zone (6) into the sampling line (7), the remaining second quantity of hydrogen in the hydrogen delivery line (3) is available for dispensing to a hydrogen user (x) via a lower section of the hydrogen delivery line (5) and via a hydrogen dispensing nozzle (9) .
  • the third quantity of hydrogen may be diverted into the sampling line (7) at least once, or alternatively more than once, so that the composition of the gaseous hydrogen supplied to the user can be assessed based on more than one sample.
  • Such process enables the operator of the apparatus of the present invention to know whether the dispensed gaseous hydrogen contains any impurities and/or
  • a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2) .
  • the pressure of the gaseous hydrogen in the pressurised hydrogen source (1) provides at least the initial driving force for gaseous hydrogen to flow into the first flow control unit (2) .
  • the pressure within the pressurised hydrogen source (1) may be created and maintained by a hydrogen compressor and/or by the production process that produces such hydrogen.
  • the gaseous hydrogen flow into the first flow control unit (2) may be also assisted by pump(s) capable of supplying gaseous hydrogen at pressure.
  • a second quantity of hydrogen is then released by the first flow control unit (2) towards a sample withdrawal zone (6) along an upper section of a hydrogen delivery line (4) .
  • the first flow control unit (2) regulates the pressure, frequency and the amount of the gaseous hydrogen supplied towards the sample withdrawal zone (6) .
  • the first flow control unit (2) regulates the quantity of the second quantity of hydrogen so that it is matched to the quantity of gaseous hydrogen required by a hydrogen user, such as for refuelling a hydrogen utilizing vehicle to its fuel tank' s maximum capacity, or to any percentage of such capacity as may be necessary at the time.
  • the quantity of the second quantity of hydrogen regulated by the first flow control unit (2) so that a hydrogen refuelling pressure of 70 MPa for light- duty vehicles and of 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle as mandated by hydrogen refuelling standard SAE J2601, or any other hydrogen refuelling standard that may be in place at the location and time of refuelling.
  • the flow of the second quantity of hydrogen into the upper section of a hydrogen delivery line (4), and its frequency of supply may be regulated by the first flow control unit (2) to be continuous or discontinuous depending on the need of the hydrogen user, such as the stage of the refuelling operation, and the flow-rate is regulated to match such stage.
  • the second quantity of hydrogen flows along the upper section of a hydrogen delivery line (4), it may be filtered by filter (s) to remove particulates, its water removed, cooled by cooler (s) to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, its quantity measured by hydrogen flow meter (s) and/or its pressure adjusted to required pressure by hydrogen compressor (s) .
  • additional processes may also take place along the second line for hydrogen flow as necessary for refuelling hydrogen utilising vehicles.
  • such process takes place along the upper section of a hydrogen delivery line (4) between the the first flow control unit (2) and a sample withdrawal zone (6), and its location is suitably depicted in Figure 2 by the section labelled "(a)".
  • the second quantity of hydrogen is conveyed along the entire length of the hydrogen delivery line (3), bypassing the sampling zone (6) without any of the gaseous hydrogen being diverted into the sampling line (7) .
  • the second quantity of hydrogen reaches a hydrogen dispensing nozzle (9) and at least a portion of the second quantity of hydrogen is dispensed via the hydrogen dispensing nozzle (9) to a hydrogen user (x) , such as a hydrogen utilising vehicle, leaving a third quantity of hydrogen retained in hydrogen delivery line (3) .
  • a third quantity of hydrogen is retained in hydrogen delivery line (3), and at least a portion of the third quantity of hydrogen is released into a sampling line (6) and supplied to a gas composition analyser (8) and its composition is analysed by the gas composition analyser (8) to detect the presence of impurities and/or
  • Such analysis may involve, but is not limited to, techniques such as gas chromatography, mass spectroscopy and/or infrared spectroscopy, or any combination of techniques, to detect and measure the concentrations of any one or more of such impurities and/or contaminants.
  • impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water.
  • results of such analysis are presented to the operator of the apparatus of the present invention in electronic form via a visual display unit, or
  • the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, so suitably no gas pressure reduction device will be required to be in place along the sampling line upstream of the gas composition analyser .
  • the gas composition analyser may be able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa.
  • the pressure of the third quantity of hydrogen in the sampling line (7) is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
  • the pressure of the third quantity of hydrogen in the sampling line (7) is reduced to a pressure
  • the gas composition analyser installed to carry out the compositional analysis of the gaseous hydrogen it receives, such reduction being preferably to at most 10 MPa, more preferably to at most 1 MPa, even more preferably to at most 0.5 MPa, and most preferably to at most 0.1 MPa.
  • the gas pressure reduction device may vent a quantity of gaseous hydrogen that it receives without introducing any impurity into the remaining third quantity of hydrogen.
  • Such process enables the operator of the apparatus of the present invention to know whether the dispensed gaseous hydrogen contains any impurities and/or
  • Figure 1 shows a simplified schematic diagram of the apparatus according to the invention, which carries out the process according to the invention.
  • the apparatus comprises a pressurised hydrogen source (1), a first flow control unit (2), a hydrogen delivery line (3), a sampling line (7), a gas composition analyser (8) and a hydrogen dispensing nozzle (9) .
  • the gas composition analyser (8) is also labelled with the letter ⁇ ⁇ ' .
  • the apparatus comprises a sample withdrawal zone (6), and the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5) .
  • the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other.
  • Figure 1 also shows, optionally, a hydrogen utilising vehicle (x) comprising a hydrogen fuel tank (y) and a line (z) for conveying gaseous hydrogen dispensed from the hydrogen dispensing nozzle (9) to the hydrogen fuel tank (y) .
  • a line may be within the hydrogen utilising vehicle (x) , and suitably is
  • Figure 2 shows a simplified schematic diagram of an embodiment of the apparatus according to the invention, which carries out the processes according to the
  • the embodiment depicted in Figure 2 optionally comprises a second flow control unit (11), and/or optionally a gas pressure reduction device (10) and/or optionally a one-way flow valve (12) .
  • the second flow control unit (11) controls the amount and frequency of gaseous hydrogen supplied first to a pressure reduction device (10) and then to a gas composition analyser (8) .
  • the gas composition analyser is able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa.
  • the sampling zone comprises a gas pressure reduction device (10) located upstream of the gas composition analyser to reduce pressure of the diverted third quantity of hydrogen to a pressure appropriate for the gas composition analyser installed in the apparatus to carry out the compositional analysis of the gaseous hydrogen it receives.
  • the gaseous hydrogen remaining in the gas composition analyser may be vented via a one ⁇ way flow valve (12) without the introduction of any impurities and/or contaminants into the gas composition analyser or to the dispenser equipment /system .

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Abstract

The present invention provides an apparatus for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, comprising a pressurised hydrogen source (1), a first flow control unit (2); a hydrogen delivery line (3), a sample withdrawal zone (6), a sampling line (7), a gas composition analyser (8) and a hydrogen dispensing nozzle (9), wherein the first flow control unit (2) comprises an inlet in fluid communication with the pressurised hydrogen source (1) and an outlet in fluid communication with the hydrogen delivery line (3); wherein the first flow control unit (2) regulates the pressure and the amount of hydrogen that may flow from the pressurised hydrogen source (1) into the hydrogen delivery line (3); wherein the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5); wherein at the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other; wherein the sampling line (7) supplies at least a quantity of hydrogen from the sample withdrawal zone (6) into the gas composition analyser (8); wherein the gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of hydrogen from the gas composition analyser (8); and wherein the downstream end of the lower section of the hydrogen delivery line (5) is connected to and is in fluid communication with the hydrogen dispensing nozzle (9).

Description

APPARATUS AND PROCESSES FOR MONITORING THE QUALITY OF
HYDROGEN
Field of the Invention
This invention relates to an apparatus and one or more processes for monitoring the quality of gaseous hydrogen dispensed to hydrogen users.
Background of the Invention
Hydrogen fuel cells are devices that convert the chemical energy of hydrogen into electrical energy, which then can be used, for example, by electrical motors to drive machinery. Such machinery may include motor vehicles .
To carry out such energy conversion, hydrogen fuel cells have incorporated in them precious and/or rare metals, such as platinum, acting as catalytically active components. These precious and/or rare metals are essential to the fuel cell' s function, however their catalytic activity is susceptible to deactivation by impurities and/or contaminants that may be present in the hydrogen supplied to the fuel cell. Such impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water. The levels and the nature of these impurities and/or contaminants depend on how the supplied hydrogen was produced, stored, transported and/or conveyed to the fuel cell. Whilst the adverse effect of impurities and/or contaminants such as carbon monoxide may be reversible, the adverse effect of some sulphur compounds is not reversible. Irreversible adverse effects on a fuel cell are cumulative and ultimately detrimental to its
function. Further, particulate matter may contaminate the hydrogen, and may block the fine channels that comprise hydrogen fuel cells. Hydrogen may also contain inert impurities and/or contaminants such as nitrogen, and although they do not adversely affect any fuel cell components, they dilute the hydrogen, thereby reducing the amount of electricity that can be generated by the fuel cell from a given volume of gas. Therefore both the retailers of hydrogen as a fuel for fuel cells, and the user of such hydrogen need to know the purity of the supplied hydrogen.
Currently ISO 14687-2-2012 provides an objective standard to assess the purity of gaseous hydrogen as a fuel for hydrogen utilising vehicles. However, because hydrogen vehicle refuelling is a multi-stage process, although the hydrogen in the hydrogen storage tank of the hydrogen refuelling/retail station may comply with ISO 14687-2-2012, impurities and/or contaminants and/or particulates may contaminate the hydrogen while it is processed for dispensing and/or while it is conveyed through the station's dispenser equipment/system.
Similarly, although the hydrogen produced at a central production facility may comply with ISO 14687-2-2012, impurities may contaminate the hydrogen while it is conveyed into, for example, a distribution truck. It is therefore desirable to know the quality of the gaseous hydrogen supplied to any hydrogen utilising vehicles by assessing it immediately before it enters the vehicle' s storage tank.
However, measuring the quality of hydrogen during the refuelling of hydrogen utilising vehicles is
challenging primarily due to the pressure and the flow rate at which hydrogen is delivered to such vehicles. SAE J2601, a widely accepted standard for hydrogen refuelling, mandates that light-duty vehicles are refuelled to 70 MPa and heavy-duty vehicles are refuelled to 35 MPa, over a time of 3 to 5 minutes.
It may seem that at least one hydrogen analyser can be incorporated in-line within the dispenser
equipment/system of hydrogen retails/suppliers, however this has proved challenging because such analyser (s) must not only be able to withstand the high pressure at which hydrogen is dispensed to hydrogen utilising vehicles (at about 87.5 MPa), but also the thermodynamic peculiarities of hydrogen, such as Joule-Thomson heating. Further, because many of the impurities and/or contaminants in hydrogen are able to affect fuel cells at ppm and sub-ppm levels, the analyser has to be capable of detecting such low levels accurately and quickly.
For these reasons, the current practical way of monitoring hydrogen quality is to transfer a hydrogen sample from the dispenser equipment/system into a sample bottle, take the sample bottle to a laboratory and to analyse the sample in the laboratory using techniques such as gas chromatography, mass spectroscopy,
chromatography mass spectroscopy (GC-MS) , infrared spectroscopy and/or Fourier transform infrared
spectroscopy (FTIR) . Not only do such processes and analyses take time, but also there is a possibility that other substances may contaminate the sample on its way for analysis. Such contamination may be because of reasons such as, but not limited to, inadequate sealing between the sample bottle and the dispenser
equipment/system and/or the analysis equipment, as well as the reactivity of the hydrogen with the walls and the seal of the sample bottle. Regarding the latter, special hydrogen sample bottles are designed to mitigate this problem, however, such bottles alone do not overcome the challenges of filling them up from a high pressure source .
To reduce the possibility of contaminating a sample while extracting it from a hydrogen station' s dispenser equipment/system under high pressure, Linde have developed a hydrogen gas sampling instrument marketed under the trade mark x¾ QUALITIZER' (a trade mark owned by Linde AG) , which is fitted at the downstream end of the dispensing system to enable hydrogen samples to be bled and captured in specially lined sample cylinders. The use of the λΗ2 QUALITIZER' has been assessed by the partner of the European Union funded 'HyCora' project (made up of the following partners: VTT Technical
Research Centre of Finland, Alternative Energies and
Atomic Energy Commission (CEA) , European Commission Directorate-General Joint Research Centre Institute for Energy and Transport ( JRC) , Protea Limited, Stiftelsen SINTEF and Powercell Sweden AB) . However, such samples still need to be transported to and analysed at a laboratory, and it will take time for the results to be established and communicated to the interested parties.
However, a further problem still remains, which is that numerous samples may need to be taken to be able to obtain a representative measurement of the hydrogen that was dispensed to each user, and the above mentioned process may not be practical for commercial hydrogen retailers with numerous hydrogen user customers .
To overcome these difficulties and limitation, the present inventors have provided the invention set out herein which enables the quality of a hydrogen sample representative of the dispensed hydrogen to be obtained and analysed within a hydrogen refuelling/retail station's dispenser equipment/system, either during or shortly after, vehicle refuelling.
Summary of the Invention
Accordingly, the present invention provides an apparatus for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, comprising a pressurised hydrogen source (1), a first flow control unit (2); a hydrogen delivery line (3), a sample
withdrawal zone (6), a sampling line (7), a gas
composition analyser (8) and a hydrogen dispensing nozzle (9), wherein the first flow control unit (2) comprises an inlet in fluid communication with the pressurised hydrogen source (1) and an outlet in fluid communication with the hydrogen delivery line (3);
wherein the first flow control unit (2) regulates the pressure and the amount of hydrogen that may flow from the pressurised hydrogen source (1) into the hydrogen delivery line (3); wherein the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5); wherein at the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other; wherein the sampling line (7) supplies at least a quantity of hydrogen from the sample
withdrawal zone (6) into the gas composition analyser (8); wherein the gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of hydrogen from the gas composition analyser (8); and wherein the downstream end of the lower section of the hydrogen delivery line (5) is connected to and is in fluid communication with the hydrogen dispensing nozzle (9) .
The present invention also provides a first process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen: wherein a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2); wherein a second quantity of hydrogen is released by the first flow control unit (2) towards a sample withdrawal zone (6); wherein a third quantity of hydrogen is diverted at the sample withdrawal zone (6) into a sampling line (7), leaving a remainder of the second quantity of hydrogen available for dispensing to a hydrogen user (x) via a lower section of the hydrogen delivery line (5) and via a hydrogen dispensing nozzle (9); and wherein the
composition of the third quantity of hydrogen is analysed by a gas composition analyser (8) .
The present invention also provides a second process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, wherein a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2); wherein a second quantity of hydrogen is released by the first flow control unit (2) towards a hydrogen dispensing nozzle (9) via a hydrogen delivery line (3); wherein at least a portion of the second quantity of hydrogen is dispensed via the hydrogen dispensing nozzle (9) to a hydrogen user (x) leaving a third quantity of hydrogen retained in the hydrogen delivery line (3); and wherein at least a portion of the third quantity of hydrogen is released into a sampling line (6) and supplied to a gas
composition analyser (8) and its composition is analysed by the gas composition analyser (8) . Brief Description of the Drawings
Figure 1 shows a simplified schematic diagram of the apparatus according to the invention.
Figure 2 shows a simplified schematic diagram of an embodiment of the apparatus according to the invention, which carries out an embodiment of the process according to the invention.
Detailed Description of the Invention
In the present invention, firstly an apparatus and secondly one or more processes that may be carried out by using the apparatus are provided and described below.
The apparatus of the present invention not only dispenses gaseous hydrogen to hydrogen users such as to hydrogen utilising vehicles, but also enables quality analyses to be carried out on samples of gaseous hydrogen which are representative of the hydrogen that is supplied by the apparatus to each hydrogen user.
The apparatus of the present invention comprises a pressurised hydrogen source (1) . The pressurised hydrogen source (1) supplies gaseous hydrogen to a first flow control unit (2) suitably at a pressure of between at least 20 MPa and 107.5 MPa. Suitably, the pressure of the gaseous hydrogen supplied to the first line for hydrogen flow is at least 20 MPa, more preferably at a pressure of at least 45 MPa and even more preferably at a pressure of at least 90 MPa.
Suitably, the pressurised hydrogen source (1) may be, for example, any hydrogen storage tank of a type known to the skilled person which is capable of storing hydrogen gas preferably at any one of the abovementioned pressures. Suitably, the pressurised hydrogen source (1) also may be a hydrogen supply line, supplying gaseous hydrogen from a hydrogen distribution network or from a hydrogen production facility, which can deliver gaseous hydrogen preferably at any one of the abovementioned pressures. Suitably, the pressurised hydrogen source (1) may be also a type of gaseous hydrogen production equipment preferably located at a hydrogen retail site, such as but not limited to, methane steam reformer (s), solid oxide fuel cell(s) with hydrocarbon reforming capability, and/or a water electrolysis unit(s) .
Suitably, the pressurised hydrogen source (1) may comprise, for example, a combination of a hydrogen supply line feeding gaseous hydrogen into a hydrogen storage tank, or a hydrogen production equipment feeding gaseous hydrogen into a hydrogen storage tank. Suitably, the pressurised hydrogen source (1) may also comprise one or more gaseous hydrogen compressor ( s ) so that the
pressurised hydrogen source (1) is able to provide a gaseous hydrogen output at any one of the abovementioned pressures. The pressurised hydrogen source (1) is not limited to the abovementioned examples, and further may be a mobile gaseous hydrogen transportation unit such as truck- or railway wagon-mounted hydrogen tanks, or a fixed/immobile unit at a distribution/ supply site.
The pressurised hydrogen source (1) provides gaseous hydrogen to a first flow control unit (2) . The first flow control unit (2) comprises an inlet in fluid
communication with the pressurised hydrogen source (1) and an outlet in fluid communication with a hydrogen delivery line (3) .
Suitably, the first flow control unit (2) may be attached directly to the pressurised hydrogen source (1), or may be connected to the pressurised hydrogen source (1) via a hydrogen supply line. In the latter case, suitably an outlet of the pressurised hydrogen source (1), an inlet of the first flow control unit (2) and said hydrogen supply line are in fluid communication with each other to enable the flow of gaseous hydrogen from the pressurised hydrogen source (1) to the first flow control unit (2) .
If present, suitably the hydrogen supply line connecting the pressurised hydrogen source (1) to the first flow control unit (2) may be any type of conduit that is suitable for conveying gaseous hydrogen at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
The first flow control unit (2) may be any type of flow control unit known to the skilled person that is suitable for regulating the pressure and the amount of gaseous hydrogen at a temperature of as low as at least -
60°C and at a pressure of up to 107.5 MPa.
The first flow control unit (2) regulates the pressure and the amount of gaseous hydrogen that may flow from the pressurised hydrogen source (1) into a hydrogen delivery line (3) . Suitably, such controls may be effected by the user of the apparatus, or by any suitable automated control system. Preferably, the flow rate and the frequency of such flow are operated by an automated control system, and through such control, suitably the first flow control unit (2) regulates the pressure of the gaseous hydrogen that may flow from the pressurised hydrogen source (1) into a hydrogen delivery line (3), so that, for example, a final gaseous hydrogen refuelling pressure of 70 MPa for light-duty vehicles and 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle (as mandated by hydrogen refuelling standard SAE J2601), or any other hydrogen refuelling pressure (s) mandated by a standard that may be applicable at the location at the time of refuelling.
The apparatus of the present invention also
comprises a hydrogen delivery line (3) .
The hydrogen delivery line comprises an upper section (4) and a lower section (5) . The references used herein to "upper" and "lower", as well as references to "upstream" and "downstream" are with respect to the general overall hydrogen flow along the apparatus, i.e. "upper" and "upstream" (as the context so requires) refer to the pressurised hydrogen source (1) end of the apparatus, and "lower" and "downstream" (as the context so requires) refer to the hydrogen dispensing nozzle (9) end of the apparatus .
The upstream end of the upper section of the hydrogen delivery line (4) is in fluid communication with an outlet of the first flow control unit (2), such that the gaseous hydrogen released by the first flow control unit (2) may flow into, and along, the upper section of the hydrogen delivery line (4), thereby supplying gaseous hydrogen from the first flow control unit (2) to a sample withdrawal zone (6) .
The lower section of the hydrogen delivery line (5) supplies gaseous hydrogen from the sample withdrawal zone (6) to a hydrogen dispensing nozzle (9), as the
downstream end of the lower section of the hydrogen delivery line (5) is in fluid communication with hydrogen dispensing nozzle (9) .
The apparatus of the present invention also
comprises a sampling line (7) . The sampling line supplies gaseous hydrogen from a sample withdrawal zone (6) to a gas composition analyser (8) . At the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line
(4) , the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other.
Suitably, each of the upper section of the hydrogen delivery line (4), the lower section of the hydrogen delivery line (5) and the sampling line (7) is any type of conduit that is suitable for conveying gaseous hydrogen at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
In an embodiment of the apparatus of the present invention, suitably, the downstream end of the upper section of the hydrogen delivery line (4) and the upstream end of the lower section of the hydrogen delivery line (5) may each house one or more flow control device (s) that control the direction of gaseous hydrogen flow along said sections of the hydrogen delivery line (4), as well as the amount of gaseous hydrogen flow along and between said sections.
In an embodiment of the apparatus of the present invention, suitably, there may be one or more flow control device (s) located at the sample withdrawal zone (6), i.e. the point where the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line
(5) and the upstream end of the sampling line (7) converge. Such flow control device (s) may be alternatives to the flow control device (s) mentioned in the preceding paragraph, or may be in addition to the flow control device (s) mentioned in the preceding paragraph. Suitably, the sampling line (7) comprises a second flow control unit (11) that can regulate the flow of gaseous hydrogen from the sample withdrawal zone (6) to the gas composition analyser (8) . Suitably, the second flow control unit (11) may be an alternative to the flow control device (s) mentioned in the preceding paragraphs, or may be in addition to any one of the flow control device (s) mentioned in the preceding paragraphs.
Suitably, the second flow control unit (11) is any type of flow control system known to the skilled person that is that suitable for controlling gaseous hydrogen flow at a temperature of as low as at least -60°C and at a pressure of up to 107.5 MPa.
Suitably, the second flow control unit (11) may comprise a check valve component or a one-way flow regulator component to prevent backflow of gaseous hydrogen into the sample withdrawal zone (6) .
Suitably, the second flow control unit (11) may also be capable of isolating the sampling line (7) from the sample withdrawal zone (6), to enable a gas composition analyser (8) to retain at least a portion of gaseous hydrogen, so that it may carry out an analysis of its composition. Suitably, isolating the sampling line may also enable maintenance to be carried out on the gas composition analyser (8) without affecting the
apparatus's hydrogen dispensing capability.
Suitably, the second flow control unit controls (11) the amount of gaseous hydrogen and its flow rate along the sampling line (7), as well as the timing and the frequency of such flow. Such controls may be effected by the user of the apparatus, or by any automated control system. Preferably, the flow rate and the frequency of such flow are operated by an automated control system. The sampling line supplies gaseous hydrogen to a gas composition analyser (8) suitable for detecting
impurities and/or contaminants in gaseous hydrogen, as well as being suitable for quantifying the concentrations of such impurities and/or contaminants. Suitably, the gas composition analyser (8) may be any gas analyser that is capable of detecting and measuring the concentration of any one or more of the impurities and/or contaminants that may be capable of affecting the functioning of hydrogen fuel cells at ppm levels, and more preferably at sub-ppm levels. The xppm' levels and λ sub-ppm' levels refer to the concentration of such impurities and/or contaminants when the hydrogen gas pressure is about 0.1 MPa. Suitably, the gas composition analyser may use techniques such as, but not limited to, gas
chromatography, mass spectroscopy and/or infrared spectroscopy, or any combination of techniques, to detect and measure the concentrations of any one or more of such impurities and/or contaminants. Suitably the gas
composition analyser (8) may retain a quantity of gaseous hydrogen within it while analysing it, or may also be able to analyse gaseous hydrogen while the hydrogen flows through the gas composition analyser (8) .
In an embodiment of the apparatus of the present invention, suitably, there may be more than one gas composition analyser to enable different analysis techniques to be carried out on the gaseous hydrogen sample in order to improve the compositional analysis, or widen the gas compositional analysis to detect and measure the levels of a broader range of impurities and/or contaminants.
In an embodiment of the apparatus of the present invention, suitably the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a pressure of below 90 MPa.
In another embodiment of the apparatus of the present invention, suitably the gas composition analyser (8) may be also able to analyse gaseous hydrogen
composition at a pressure of at least 90 MPa or more.
In the abovementioned embodiment where the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of below 90 MPa, suitably a gas pressure reduction device (10) will be required to be in place along the sampling line, between downstream of the sample withdrawal zone (6) and upstream of the gas composition analyser (8) . Suitably, the function of the gas pressure reduction device (10) is to produce a reduced pressure hydrogen sample for the gas composition analyser to analyse. To do this, suitably the gas pressure reduction device (10) reduces the pressure of the gaseous hydrogen which it receives from the sample withdrawal zone (6) via the sampling line (7) to a pressure suitable for the gas composition analyser (8) installed as part of the apparatus of the present invention, such as preferably at most 10 MPa, more preferably at most 1 MPa, even more preferably at most 0.5 MPa, and most preferably at most 0.1 MPa. Suitably, to reduce the pressure of the gaseous hydrogen which it receives from the sample withdrawal zone (6) via the sampling line (7), the gas pressure reduction device (10) may vent a quantity of gaseous hydrogen that it receives without introducing any impurities and/or contaminants into the remaining hydrogen. Suitably, but without limitation, a one-way flow valve downstream of the gas composition analyser may take part in said venting. Following its analysis by the gas composition analyser (8), the reduced pressure hydrogen sample remaining in the gas composition analyser (8) may be vented without introducing any further impurities and/or contaminants into the gas composition analyser or into the dispenser equipment /system . Suitably, a one-way flow valve (12) located downstream of the gas composition analyser may be present and suitably prevents the back- flow of any hydrogen destined for venting.
Suitably, the gaseous hydrogen vented either as part of the pressure reduction step(s), or which went through the gas composition analyser, may be released to the atmosphere, or used for applications other than for refuelling hydrogen utilizing vehicles, or it may be redirected to the pressurised hydrogen source (1) .
In the other abovementioned embodiment where suitably the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, suitably no gas pressure reduction device will be required to be in place along the sampling line upstream of the gas composition analyser.
The aim of the apparatus of the present invention is not only to dispense gaseous hydrogen to end users, such as hydrogen utilising vehicles, but also to analyse the quality of the dispensed hydrogen which is representative of that supplied to each hydrogen user, so that the supplier and each user of the hydrogen can be informed of its quality.
For the hydrogen sample for analysis to be
representative of the gaseous hydrogen that is supplied to the user, with respect to the flow of hydrogen along the apparatus, the sample withdrawal zone (6) is
desirably downstream of all components of the dispenser equipment/system (labelled as λ (a) ' in Figure 2), other than the hydrogen dispensing nozzle (9), so that any impurity or contaminant that may be introduced by any of such components, or even further upstream of the
dispenser equipment, can be detected by the gas
composition analyser just before the gaseous hydrogen is supplied to the hydrogen user.
Suitably, said components of the dispenser
equipment/system (labelled as λ (a) ' in Figure 2) may comprise filter (s) to remove particulates, systems to remove water, cooler (s) to cool the gaseous hydrogen that is being dispensed to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, hydrogen flow meter (s) to measure the amount of gaseous hydrogen being dispensed and/or hydrogen compres sor ( s ) to boost the pressure of the gaseous hydrogen being dispensed.
Suitably, said components of the dispenser equipment may also comprise components that measure the temperature of the hydrogen, and ones that regulate the flow of gaseous hydrogen such as, but not limited to, relief valve (s), block valve (s), flow limiter(s), components to induce or inhibit laminar hydrogen flow etc.
Further, the apparatus of the present invention not only overcomes the difficulties of analysing the quality of gaseous hydrogen at dispensing pressures of at least 90 MPa, but it also minimises the possibility of
contamination of the gaseous hydrogen sample to be analysed by diverting a quantity of gaseous hydrogen to the sampling line (7) and conveying it to the gas composition analyser (8), which may be via the gas pressure reduction device depending on whether the gas composition analyser (8) may, or may not, be able to analyse gaseous hydrogen composition at a pressure of below, or above, 90 MPa, as described above.
The lower section of the hydrogen delivery line (5) supplies gaseous hydrogen from the sample withdrawal zone (6) to a hydrogen dispensing nozzle (9) . Suitably, the hydrogen dispensing nozzle (9) can be any nozzle known to the skilled person that is that suitable for conveying gaseous hydrogen at a temperature of as low as at least - 60°C and at a pressure of up to 107.5 MPa to a hydrogen user. The hydrogen dispensing nozzle (9) is suitable for attaching to the fuel storage system of any hydrogen utilizing vehicle, such as to a line (labelled as "(z)" in Figures 1 and 2) for conveying gaseous hydrogen dispensed from the hydrogen dispensing nozzle (9) to a vehicle's hydrogen fuel tank (labelled as " (y) " in
Figures 1 and 2), and for dispensing a quantity of gaseous hydrogen until the hydrogen fuel tank of the hydrogen utilizing vehicle is filled with gaseous hydrogen to the tank' s maximum capacity, or to any percentage of such capacity mandated by any refuelling protocol. Suitably, the hydrogen dispensing nozzle (9) is capable of regulating the flow rate and the quantity of the gaseous hydrogen supplied to the fuel storage system of the hydrogen utilizing vehicle that is being refueled. Suitably and without limitation, such regulation of the flow rate may be effected manually by any operator, or by an automated control system controlled by any such operator .
In the present invention one or more processes may be carried out by using the above-mentioned apparatus.
In a first aspect of the process according to the present invention, a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2) .
Suitably, the pressure of the gaseous hydrogen in the pressurised hydrogen source (1) provides at least the initial driving force for gaseous hydrogen to flow into the first flow control unit (2) . Suitably, the pressure within the pressurised hydrogen source (1) may be created and maintained by a hydrogen compressor and/or by the production process that produces such hydrogen. Suitably, the gaseous hydrogen flow into the first flow control unit (2) may be also assisted by pump(s) capable of supplying gaseous hydrogen at pressure.
Once the first quantity of hydrogen is received by the first flow control unit (2), a second quantity of hydrogen is then released by the first flow control unit (2) towards a sample withdrawal zone (6) along an upper section of a hydrogen delivery line (4) . The second quantity of hydrogen may be equal to, or less than, the first quantity of hydrogen.
Suitably, the first flow control unit (2) regulates the pressure, timing, frequency and the amount of the second quantity of hydrogen supplied towards the sample withdrawal zone (6) .
With respect to such regulated quantity of gaseous hydrogen, suitably, the first flow control unit (2) may regulate the quantity of the second quantity of hydrogen so that it is matched to the quantity of gaseous hydrogen required by a hydrogen user, such as for refuelling a hydrogen utilizing vehicle to its fuel tank' s maximum capacity, or to any percentage of such capacity as may be necessary at the time.
Similarly, the quantity of the second quantity of hydrogen regulated by the first flow control unit (2) so that a hydrogen refuelling pressure of 70 MPa for light- duty vehicles and of 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle as mandated by hydrogen refuelling standard SAE J2601, or any other hydrogen refuelling standard that may be in place at the location and time of refuelling.
Suitably, the flow of the second quantity of gaseous hydrogen into the upper section of a hydrogen delivery line (4), and its frequency of supply, may be regulated by the first flow control unit (2) to be continuous or discontinuous depending on the need of the hydrogen user, such as the stage of the refuelling operation, and the flow-rate is regulated to match such stage.
Suitably, as the second quantity of hydrogen flows along the upper section of a hydrogen delivery line (4), it may be filtered by filter (s) to remove particulates, its water removed, cooled by cooler (s) to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, its quantity measured by hydrogen flow meter (s) and/or its pressure adjusted to required pressure by hydrogen compressor (s) . Suitably, additional processes may also take place along the second line for hydrogen flow as necessary for refuelling hydrogen utilising vehicles. Suitably, such process takes place along the upper section of a hydrogen delivery line (4) between the the first flow control unit (2) and a sample withdrawal zone (6), and its location is suitably depicted in Figure 2 by the section labelled "(a)".
Once the second quantity of hydrogen reaches the downstream end of the upper section of a hydrogen delivery line (4) it reaches a sample withdrawal zone (6) where a third quantity of hydrogen is diverted into a sampling line (7), leaving a remainder of the second quantity of hydrogen available for dispensing to a hydrogen user (x) . Suitably, the remainder of the second quantity of hydrogen may be dispensed to a hydrogen user (x) by conveying it initially via a lower section of the hydrogen delivery line (5), then via a hydrogen
dispensing nozzle (9) out to the hydrogen user.
Suitably, once the third quantity of hydrogen is diverted into the sampling line (7), its flow back into the sample withdrawal zone (6) may be prevented by a second flow control unit (11) .
Suitably, the second flow control unit (11) also regulates the amount of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas composition analyser (8) . Suitably, the second flow control unit (11) also regulates the frequency of the supply of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas
composition analyser (8) .
Such regulation may be effected by the user of the apparatus, or by any automated control system.
Preferably, the flow rate and the frequency of such flow are operated by an automated control system.
Suitably, one or more other flow control device (s) located at, or in the vicinity of, the sample withdrawal zone (6) (but not along the sampling line (7)), may provide additional means to regulate the amount of gaseous hydrogen that may flow from the sample withdrawal zone (6) into a gas pressure reduction device (10) and/or a gas composition analyser (8) . The sampling line (7) supplies the third quantity of hydrogen diverted from the sample withdrawal zone (6) into the gas composition analyser (8) .
The gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of gaseous hydrogen from the gas composition analyser (8) .
The composition of at least a portion of the third quantity of hydrogen, supplied by the sampling line (7) from the sample withdrawal zone (6), is analysed by a gas composition analyser (8) to detect the presence of any impurities and/or contaminants that may be present in the he third quantity of hydrogen, as well as to quantify their concentration (s) . Suitably, such analysis may involve, but is not limited to, techniques such as gas chromatography, mass spectroscopy and/or infrared spectroscopy, or any combination of techniques, to detect and measure the concentrations of any one or more of such impurities and/or contaminants. Such impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water.
Suitably the results of such analysis may be presented to the operator of the apparatus of the present invention in electronic form via a visual display unit, and/or in a tangible form such as a print out.
In an embodiment of the first aspect of the process, suitably the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, so suitably no gas pressure reduction device will be required to be in place along the sampling line (7) upstream of the gas composition analyser . However, in another embodiment of the first aspect of the process, suitably the gas composition analyser (8) may be able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa. In such
embodiment, suitably the pressure of the third quantity of hydrogen in the sampling line (7) is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
The pressure of the third quantity of hydrogen in the sampling line (7) is reduced to a pressure
appropriate for the gas composition analyser that is installed as part of the apparatus of the present invention to carry out the compositional analysis of the gaseous hydrogen it receives, such reduction being preferably to at most 10 MPa, more preferably to at most 1 MPa, even more preferably to at most 0.5 MPa, and most preferably to at most 0.1 MPa.
Suitably, to reduce the pressure of the diverted third quantity of gaseous hydrogen in the sampling line (7), the gas pressure reduction device (10) may vent a quantity of gaseous hydrogen that it receives without introducing any impurity into the remaining third quantity of hydrogen.
As the third quantity of hydrogen is diverted at the sample withdrawal zone (6) into the sampling line (7), the remaining second quantity of hydrogen in the hydrogen delivery line (3) is available for dispensing to a hydrogen user (x) via a lower section of the hydrogen delivery line (5) and via a hydrogen dispensing nozzle (9) . During the course of supplying gaseous hydrogen to a user, suitably, the third quantity of hydrogen may be diverted into the sampling line (7) at least once, or alternatively more than once, so that the composition of the gaseous hydrogen supplied to the user can be assessed based on more than one sample.
Such process enables the operator of the apparatus of the present invention to know whether the dispensed gaseous hydrogen contains any impurities and/or
contaminants, and whether such hydrogen is deemed acceptable with respect to any applicable quality standard, such as ISO 14687-2-2012.
In a second aspect of the process according to the present invention, a first quantity of hydrogen is supplied from a pressurised hydrogen source (1) into a first flow control unit (2) .
Suitably, the pressure of the gaseous hydrogen in the pressurised hydrogen source (1) provides at least the initial driving force for gaseous hydrogen to flow into the first flow control unit (2) . Suitably, the pressure within the pressurised hydrogen source (1) may be created and maintained by a hydrogen compressor and/or by the production process that produces such hydrogen. Suitably, the gaseous hydrogen flow into the first flow control unit (2) may be also assisted by pump(s) capable of supplying gaseous hydrogen at pressure.
Once the first quantity of hydrogen is received by the first flow control unit (2), a second quantity of hydrogen is then released by the first flow control unit (2) towards a sample withdrawal zone (6) along an upper section of a hydrogen delivery line (4) . Suitably, the first flow control unit (2) regulates the pressure, frequency and the amount of the gaseous hydrogen supplied towards the sample withdrawal zone (6) .
With respect to said regulated quantity of gaseous hydrogen, suitably, the first flow control unit (2) regulates the quantity of the second quantity of hydrogen so that it is matched to the quantity of gaseous hydrogen required by a hydrogen user, such as for refuelling a hydrogen utilizing vehicle to its fuel tank' s maximum capacity, or to any percentage of such capacity as may be necessary at the time.
Similarly, the quantity of the second quantity of hydrogen regulated by the first flow control unit (2) so that a hydrogen refuelling pressure of 70 MPa for light- duty vehicles and of 35 MPa for heavy-duty vehicles are achieved in the fully refuelled vehicle as mandated by hydrogen refuelling standard SAE J2601, or any other hydrogen refuelling standard that may be in place at the location and time of refuelling.
Suitably, the flow of the second quantity of hydrogen into the upper section of a hydrogen delivery line (4), and its frequency of supply, may be regulated by the first flow control unit (2) to be continuous or discontinuous depending on the need of the hydrogen user, such as the stage of the refuelling operation, and the flow-rate is regulated to match such stage.
Suitably, as the second quantity of hydrogen flows along the upper section of a hydrogen delivery line (4), it may be filtered by filter (s) to remove particulates, its water removed, cooled by cooler (s) to compensate for any temperature rise experienced by the dispensed gaseous hydrogen when it reaches the vehicle' s hydrogen fuel tank, its quantity measured by hydrogen flow meter (s) and/or its pressure adjusted to required pressure by hydrogen compressor (s) . Suitably, additional processes may also take place along the second line for hydrogen flow as necessary for refuelling hydrogen utilising vehicles. Suitably, such process takes place along the upper section of a hydrogen delivery line (4) between the the first flow control unit (2) and a sample withdrawal zone (6), and its location is suitably depicted in Figure 2 by the section labelled "(a)".
In this second aspect of the process according to the present invention, the second quantity of hydrogen is conveyed along the entire length of the hydrogen delivery line (3), bypassing the sampling zone (6) without any of the gaseous hydrogen being diverted into the sampling line (7) . At the downstream end of the lower section of the hydrogen delivery line (5), suitably, the second quantity of hydrogen reaches a hydrogen dispensing nozzle (9) and at least a portion of the second quantity of hydrogen is dispensed via the hydrogen dispensing nozzle (9) to a hydrogen user (x) , such as a hydrogen utilising vehicle, leaving a third quantity of hydrogen retained in hydrogen delivery line (3) .
After dispensing to a hydrogen user, a third quantity of hydrogen is retained in hydrogen delivery line (3), and at least a portion of the third quantity of hydrogen is released into a sampling line (6) and supplied to a gas composition analyser (8) and its composition is analysed by the gas composition analyser (8) to detect the presence of impurities and/or
contaminants and to quantify their concentration ( s ) in the hydrogen. Suitably, such analysis may involve, but is not limited to, techniques such as gas chromatography, mass spectroscopy and/or infrared spectroscopy, or any combination of techniques, to detect and measure the concentrations of any one or more of such impurities and/or contaminants. Such impurities and/or contaminants include but are not limited to, carbon monoxide, methane, ammonia, hydrogen sulphide and water.
Suitably the results of such analysis are presented to the operator of the apparatus of the present invention in electronic form via a visual display unit, or
alternatively may be in a tangible form such as a print out.
In an embodiment of the second aspect of the process, suitably the gas composition analyser may be able to analyse gaseous hydrogen composition at a pressure of at least 90 MPa or more, so suitably no gas pressure reduction device will be required to be in place along the sampling line upstream of the gas composition analyser .
However, in another embodiment of the second aspect of the process, suitably the gas composition analyser may be able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa.
In such embodiment, suitably the pressure of the third quantity of hydrogen in the sampling line (7) is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
The pressure of the third quantity of hydrogen in the sampling line (7) is reduced to a pressure
appropriate for the gas composition analyser installed to carry out the compositional analysis of the gaseous hydrogen it receives, such reduction being preferably to at most 10 MPa, more preferably to at most 1 MPa, even more preferably to at most 0.5 MPa, and most preferably to at most 0.1 MPa.
Suitably, to reduce the pressure of the diverted third quantity of hydrogen in the sampling line (7), the gas pressure reduction device may vent a quantity of gaseous hydrogen that it receives without introducing any impurity into the remaining third quantity of hydrogen.
Such process enables the operator of the apparatus of the present invention to know whether the dispensed gaseous hydrogen contains any impurities and/or
contaminants, and whether such hydrogen is deemed acceptable with respect to any applicable quality standard, such as ISO 14687-2-2012.
Detailed Description of the Drawings
Figure 1 shows a simplified schematic diagram of the apparatus according to the invention, which carries out the process according to the invention.
The apparatus comprises a pressurised hydrogen source (1), a first flow control unit (2), a hydrogen delivery line (3), a sampling line (7), a gas composition analyser (8) and a hydrogen dispensing nozzle (9) . For illustrative purposes, the gas composition analyser (8) is also labelled with the letter λΑ' .
Further the apparatus comprises a sample withdrawal zone (6), and the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5) .
At the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid communication with each other.
Figure 1 also shows, optionally, a hydrogen utilising vehicle (x) comprising a hydrogen fuel tank (y) and a line (z) for conveying gaseous hydrogen dispensed from the hydrogen dispensing nozzle (9) to the hydrogen fuel tank (y) . Suitably, such line may be within the hydrogen utilising vehicle (x) , and suitably is
attachable to the hydrogen dispensing nozzle (9) via its upstream end to enable refuelling operations.
Figure 2 shows a simplified schematic diagram of an embodiment of the apparatus according to the invention, which carries out the processes according to the
invention .
Features numbered (1) to (10) (inclusive), and (x) , (y) and (z) (inclusive) are the same as those depicted in Figure 1. For illustrative purposes, the gas composition analyser (8) is also labelled with the letter λΑ' in Figure 2.
The embodiment depicted in Figure 2, optionally comprises a second flow control unit (11), and/or optionally a gas pressure reduction device (10) and/or optionally a one-way flow valve (12) .
In the embodiment shown in Figure 2, the second flow control unit (11) controls the amount and frequency of gaseous hydrogen supplied first to a pressure reduction device (10) and then to a gas composition analyser (8) . In this embodiment, the gas composition analyser is able to analyse gaseous hydrogen composition at a hydrogen pressure of less than 90 MPa. In such embodiment, suitably the sampling zone comprises a gas pressure reduction device (10) located upstream of the gas composition analyser to reduce pressure of the diverted third quantity of hydrogen to a pressure appropriate for the gas composition analyser installed in the apparatus to carry out the compositional analysis of the gaseous hydrogen it receives. Following its analysis by the gas composition analyser (8), the gaseous hydrogen remaining in the gas composition analyser may be vented via a one¬ way flow valve (12) without the introduction of any impurities and/or contaminants into the gas composition analyser or to the dispenser equipment /system .

Claims

C L A I M S
1. An apparatus for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, comprising a pressurised hydrogen source (1), a first flow control unit (2); a hydrogen delivery line (3), a sample
withdrawal zone (6), a sampling line (7), a gas
composition analyser (8) and a hydrogen dispensing nozzle (9) :
wherein the first flow control unit (2) comprises an inlet in fluid communication with the pressurised hydrogen source (1) and an outlet in fluid communication with the hydrogen delivery line (3);
wherein the first flow control unit (2) regulates the pressure and the amount of hydrogen that may flow from the pressurised hydrogen source (1) into the hydrogen delivery line (3);
wherein the hydrogen delivery line (3) comprises an upper section (4) and a lower section (5);
wherein at the sample withdrawal zone (6), the downstream end of the upper section of the hydrogen delivery line (4), the upstream end of the lower section of the hydrogen delivery line (5) and the upstream end of the sampling line (7) converge and are in fluid
communication with each other;
wherein the sampling line (7) supplies at least a quantity of hydrogen from the sample withdrawal zone (6) into the gas composition analyser (8);
wherein the gas composition analyser (8) comprises an inlet in fluid communication with the downstream end of the sampling line (7) and an outlet for the outflow of hydrogen from the gas composition analyser (8); and wherein the downstream end of the lower section of the hydrogen delivery line (5) is connected to and is in fluid communication with the hydrogen dispensing nozzle (9) .
2. An apparatus according to Claim 1, wherein the sampling line (7) comprises a gas pressure reduction device (10) located upstream of the gas composition analyser (8), in fluid communication with the sampling line (7) and in fluid communication with the gas
composition analyser (8) .
3. An apparatus according to Claims 1 or 2 , wherein the sampling line (7) comprises a second flow control unit (11) which regulates the amount of hydrogen that may flow from the sample withdrawal zone (6) into the gas pressure reduction device (10) and/or the gas composition analyser (8) .
4. A process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, wherein:
(a) a first quantity of hydrogen is supplied from a
pressurised hydrogen source (1) into a first flow control unit (2) ;
(b) a second quantity of hydrogen is released by the first flow control unit (2) towards a sample withdrawal zone (6);
(c) a third quantity of hydrogen is diverted at the
sample withdrawal zone (6) into a sampling line (7), leaving a remainder of the second quantity of hydrogen available for dispensing to a hydrogen user (x) via a lower section of the hydrogen delivery line (5) and via a hydrogen dispensing nozzle (9); and
(d) the composition of the third quantity of hydrogen is analysed by a gas composition analyser (8) .
5. A process according to Claim 4, wherein the pressure of the third quantity of hydrogen in the sampling line is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
6. A process according to Claim 5, wherein the pressure of the reduced pressure hydrogen sample is at most 10 MPa .
7. A process for dispensing hydrogen and monitoring the composition of the dispensed hydrogen, wherein:
(a) a first quantity of hydrogen is supplied from a
pressurised hydrogen source (1) into a first flow control unit (2) ;
(b) a second quantity of hydrogen is released by the first flow control unit (2) towards a hydrogen dispensing nozzle (9) via a hydrogen delivery line (3) ;
(c) at least a portion of the second quantity of
hydrogen is dispensed via the hydrogen dispensing nozzle (9) to a hydrogen user (x) leaving a third quantity of hydrogen retained in the hydrogen delivery line (3); and
(d) at least a portion of the third quantity of hydrogen is released into a sampling line (7) and supplied to a gas composition analyser (8) and its composition is analysed by the gas composition analyser (8) .
8. A process according to Claim 7, wherein during step (d) of Claim 7 the pressure of the third quantity of hydrogen in the sampling line is reduced by a gas pressure reduction device (10) to produce a reduced pressure hydrogen sample prior to the analysis of the reduced pressure hydrogen sample by the gas composition analyser (8) .
9. A process according to Claim 8, wherein the pressure of the reduced pressure hydrogen sample is at most 10 MPa .
PCT/EP2017/065586 2016-06-28 2017-06-23 Apparatus and processes for monitoring the quality of hydrogen WO2018001907A1 (en)

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EP16176748 2016-06-28

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Cited By (2)

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CN114962996A (en) * 2022-05-05 2022-08-30 液空厚普氢能源装备有限公司 Hydrogen quality on-line detection control system of hydrogenation station
WO2022257477A1 (en) * 2021-06-11 2022-12-15 中国石油大学(华东) Experimental system and method for medium-low-pressure hydrogen-containing pipeline

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US20140311220A1 (en) * 2011-12-07 2014-10-23 Peter R. Bossard System and Method of Quantifying Impurities Mixed within a Sample of Hydrogen Gas

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US20110005302A1 (en) * 2009-07-13 2011-01-13 Uchicago Argonne Llc Device and method to sample and enrich impurities in hydrogen
US20130145823A1 (en) * 2011-12-07 2013-06-13 Peter R. Bossard System and Method for Measuring the Concentration of Impurities Mixed with Hydrogen Gas
US20140311220A1 (en) * 2011-12-07 2014-10-23 Peter R. Bossard System and Method of Quantifying Impurities Mixed within a Sample of Hydrogen Gas

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WO2022257477A1 (en) * 2021-06-11 2022-12-15 中国石油大学(华东) Experimental system and method for medium-low-pressure hydrogen-containing pipeline
CN114962996A (en) * 2022-05-05 2022-08-30 液空厚普氢能源装备有限公司 Hydrogen quality on-line detection control system of hydrogenation station
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