1、Designation: D7650 13Standard Test Method forSampling of Particulate Matter in High Pressure Hydrogenused as a Gaseous Fuel with an In-Stream Filter1This standard is issued under the fixed designation D7650; the number immediately following the designation indicates the year oforiginal adoption or,
2、in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is primarily for sampling particulatesin hydrogen fuel used in h
3、ydrogen fuel cell vehicles or gaseoushydrogen powered internal combustion vehicle engines up topressures of 70 MPa (700 bars) using an in-stream filter. Thistest method describes sampling apparatus design, operatingprocedures, and quality control procedures required to obtainthe stated levels of pre
4、cision and accuracy.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.2.1 ExceptionIn 7.1 and 10.1.1 the values stated in psiare for information only.1.3 This standard does not purport to address all of thesafety concerns, i
5、f any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D7651 Test Method for Gravimetric Measurement
6、of Par-ticulate Concentration of Hydrogen Fuel2.2 SAE Standards:3SAE J2719 Hydrogen Fuel Quality for Fuel Cell VehiclesSAE J2600 Compressed Hydrogen Surface Vehicle Refuel-ing Connection Devices2.3 ISO Standard:4ISO/CD 146872 Hydrogen fuel Product Specification Part 2: Proton exchange membrane (PEM)
7、 fuel cellapplications for road vehicles.2.4 EU Standard:597/23/EC Pressure Equipment Directive of the EU set outthe standards for the design and fabrication of pressureequipment2.5 DIN Standard:6DIN EN 12266-1 Industrial valves-Testing of metallicvalves-Part 1: Pressure test, test procedures and ac
8、cep-tance criteria Mandatory Requirements2.6 API Standard:7API 598 Valve Inspection and Testing3. Terminology3.1 Acronyms:3.1.1 FCVHydrogen Fuel Cell Vehicle.3.1.2 HQSAHydrogen quality sampling assembly forsampling gaseous hydrogen fuel.3.1.3 PEMPolymer Electrolyte Membrane or Proton Ex-change Membr
9、ane3.1.4 PSA-H70Particulate sampling adapter for samplingparticulate in hydrogen fuel up to pressures of 70 MPa.3.1.5 SAE InternationalSociety of Automotive Engineer-ing3.2 Definitions:3.2.1 pinholea small hole generated during sampling ofparticulate in hydrogen that can be identified by microscope.
10、3.3 SAE J2719 Hydrogen Fuel Quality for Fuel CellVehiclesThis document specifies allowable levels of constitu-ents in the hydrogen fuel at the vehicle/station interface.3.4 SAE J2600Compressed Hydrogen Surface VehicleRefueling Connection DevicesThis document specifies thedesign requirements for nozz
11、les and receptacles used in highpressure hydrogen applications such as delivery from a fuelingstation to a FCV.1This test method is under the jurisdiction ofASTM Committee D03 on GaseousFuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen andFuel Cells.Current edition approved M
12、ay 1, 2013. Published June 2013. Originallyapproved in 2010. Last previous edition approved in 2010 as D765010. DOI:10.1520/D765013.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
13、ation, refer to the standards Document Summary page onthe ASTM website.3Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,PA 15096-0001, http:/www.sae.org.4Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, CP 56, CH-1211 Geneva 20, S
14、witzerland, http:/www.iso.org.5Available from European Committee for Standardization (CEN), AvenueMarnix 17, B-1000, Brussels, Belgium, http:/www.cen.eu.6Available from Deutsches Institut fur Normung e.V.(DIN), Burggrafenstrasse 6,10787 Berlin, Germany, http:/www.din.de.7Available from American Petr
15、oleum Institute (API), 1220 L. St., NW,Washington, DC 20005-4070, http:/www.api.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 This test method provides a procedure for the samplingof particulate matt
16、er contained in hydrogen used as a FCV fuel.It is designed to collect all particulates 0.2 m or largercontained in a known amount of hydrogen at a stationdispenser nozzle in a way that simulates a FCV or a gaseoushydrogen powered internal combustion vehicle engine fuelingevent. The adapter used for
17、sampling particulates in hydrogenfuel is called a Particulate Sampling Adapter for pressures upto 70 MPa (PSA-H70) and is described in Section 7. Great careshould be taken to avoid contamination and exposure of thePSA-H70, filters, and other equipment with particles sized 10m or larger prior to use.
18、5. Significance and Use5.1 Fuel cells such as proton exchange membrane fuel cellsrequire high purity hydrogen for maximum material perfor-mance and lifetime. Collection and measurement of particulatematter 0.2 m or larger is necessary for assuring a feed gas ofsufficient quality to satisfy fuel cell
19、 system needs. In addition,internal combustion engines using high pressure hydrogen fuelalso require low particulate levels. Specifically, particulatematter has been implicated in the premature failure of pneu-matic control components, such as valves within vehicles. Thissampling procedure is used t
20、o collect and measure samplescontaining particles 0.2 m or larger in size.5.2 Although not intended for application to gases otherthan hydrogen and related fuel cell supply gases, the tech-niques within this sampling procedure can be applied to otherhigh pressure gaseous samples requiring particulat
21、e collectionand measurement.6. Interferences6.1 Dust and other environmental particulate matter willinterfere with the accurate measurement of particulates con-tained in FCV quality hydrogen; therefore, every measureshould be taken according to Section 14 to avoid contaminationof the apparatus and a
22、ll equipment, supplies and gases used inthese procedures.7. Apparatus DesignNOTE 1The use of trade names in this section are not intended as anendorsement for use.7.1 The PSA-H70 has a design pressure of 800 Bar (11600psi) and is certified after 97/23/EC and API 598 (conform toDIN EN 12266-1) up to
23、1200 bar (17400 psi) shell testpressures with appropriate safety factors built in. It is designedfor a flow rate of 60 g per second of hydrogen without damageto the filter or leakage from the PSA-H70. The PSA-H70possesses a receptacle as per SAE J2600 followed by a rotaryvalve which is directly inte
24、grated to the filter housing inlet. Therotary valve provides the possibility to switch the innerdiameter of the filter housing inlet from 4 mm to 1 mm. Thatprevents the filter element from high pressure pulse damage.The filter holder contains a standard 47 mm diameter filterelement ( 0.2 m pore size
25、) for particle collection, supportedby a sinter metal frit with a pore size of 150 m. Downstreamthe sinter metal frit a high pressure bleed plug is integrated intothe filter holder followed by a standard hydrogen refuelinghose and nozzle as per SAE J2600 to be connected to a FCVduring sample collect
26、ion. In summary, the configuration of thePSA-H70, as shown in Fig. 1, is:A SAE J2600 compliant Receptacle Filter Holder withintegrated rotary valve, the Filter Element supported by aSinter Metal Frit and a an integrated high pressure BleedPlugRefueling Hose a SAE J2600 compliant FuelingNozzle.Fig. 1
27、 illustrates a PSA-H70 design that has been success-fully used to collect particulate samples from 875 bar (12691psi) fuel cell quality hydrogen. The PSA-H70 should be ratedabove the operating pressure, and all materials used must berated for high pressure hydrogen applications at a 1.5 timesminimum
28、 margin of safety at the maximum operating pressure.The recommended working pressure of the PSA-H70 andassociated materials is 80 MPa. Contamination from lubrica-tion or other sources must be avoided and the apparatus mustbe cleaned prior to use using appropriate cleaning techniquesfor high pressure
29、 hydrogen applications. The design of thePSA-H70 should include minimizing the distance and surfacearea between the nozzle and filter to minimize the particulatesgenerated from the surface of this area by fast flow and highpressure hydrogen7.1.1 High Pressure Filter HolderThe high pressure filterhol
30、der is a 47 mm, stainless steel housing with maximum inletpressure of 120 MPa a polytetrafluoroethylene (PTFE) inner40.94 mm diameter PTFE-O ring and a hydrogenated acrylni-trilbutadiene caoutchouc as high pressure sealing. The filterholder must be equivalent, similar or exceed performancecharacteri
31、stics of the filter holder described in this test method,that is burst strength.7.1.2 FilterA polytetrafluoroethylene (PTFE) filter thattolerates flow rates of up to 60 g per s without damage andcollects particulates with a minimum size of 0.2 m.NOTE 2Hydrogen back flow must be avoided since the bac
32、kflow ofhydrogen can cause pinhole formation or other damage to filters. Thedesign of the apparatus and sampling procedures must prevent fuelbackflow.7.1.3 PSA-H70 SupportThe mechanical PSA-H70 supportmust be designed to securely hold the PSA-H70 and a J2600nozzle. The nozzle should be held firmly a
33、nd not move orshake during particulate sampling.7.1.4 PSA-H70 design for flowing hydrogen to gaseoushydrogen vehicle tankAs sampling during refueling into avehicle tank collects a sample most representative of theparticulates seen by vehicles in service, the PSA-H70 isdesigned for this purpose. Ther
34、efore, for particulates collectionthe refueling nozzle of the station is connected to the SAEJ2600 receptacle of the PSA-H70 and the SAE J2600 nozzle ofthe PSA-H70 is attached to the FCV receptacle. Whilesampling, the hydrogen fuel flows from station SAE J2600nozzle (1st nozzle) PSA-H70 with hose an
35、d a 2nd SAEJ2600 nozzle receptacle of FCV tank.8. Additional Equipment Needed8.1 Glove boxA glove box is a sealed container that isdesigned to assemble PSA-H70 without particulate contamina-tion from ambient air. Two gloves are built into the sides of theD7650 132glove box with entry arranged in suc
36、h a way that the user canplace hands into the gloves to install the filter and assemble thefilter holder inside the box. The glove box must be maintainedparticulate free at all times. Any visual particulate materialmust be removed prior to working with the PSA-H70 or filters.A HEPA8,9vacuum can be u
37、sed to remove particles from theglove bag and other equipment.8.2 Relative Moisture/Temperature Data LoggerA datalogger is placed inside the glove box to measure both moistureand temperature continuously at pre-defined intervals such asonce every two to five minutes. Moisture in the glove box iskept
38、 between 15 to 30% using reagent grade nitrogen. Alltemperature and moisture data are stored in a data logger,which are downloaded into a Microsoft Excel10,9, or a similarprogram, sheet after completion of measurements.8.3 Mini-Clean RoomA small clean room with HEPA airfiltration must be used to sto
39、re unused polytetrafluoroethylene(PTFE) filters, filter holders, and sampled filters at moisturecontent less than 30%.8.4 Ultrasonic CleanerEither an ultrasonic bath or probeis used in lab to shake off particulates on parts of PSA-H70 intoreagent grade water.8.5 Hydrogen Leak DetectorA hydrogen leak
40、 detector is arequired safety device needed to detect small hydrogen gas8HEPA is a trademark of the HEPA Corporation, 3071 East Coronado StreetAnaheim, CA 92806.9The mention of trade names in this test method does not constitute endorsementor recommendation. Other manufacturers of equipment or equip
41、ment models can beused.10Microsoft Excel is a trademark of the Microsoft Corporation, One MicrosoftWay Redmond, WA 98052-6399.Item Description1 SAE J2600 hydrogen receptacle without filter2 Rotary valve DN04 (1 mm and 4 mm diameter)3 Hydac PSA-H70 DN04 PN800 SO 1257 Filter Housing4 Bleed plug5 High
42、pressure hydrogen fueling hose6 SAE 2600 hydrogen fueling nozzleFIG. 1 PSA-H70 ComponentsD7650 133leaks in particular when the PSA-H70 is pressurized prior toparticulate collection. The diluted soap bubble should not beused to detect hydrogen leak from PSA-H70.8.6 HEPA Filter Horizontal Flow HoodA H
43、EPA filterhorizontal flow hood blows filtered air through a HEPA filterhorizontally, providing for an environment with minimal sus-pended particulates. The air velocity measured by an air flowmeter (8.8) within the hood should be over 30 m/min. If belowthis velocity, the air velocity meter should tr
44、igger an alarmnotifying the operator about a low air velocity.8.7 Plastic tweezersUsed to manipulate filters withoutcontamination.8.8 Air Flow MeterA meter to measure the air velocitygoing through the HEPA Filter Horizontal Flow Hood. The airflow meter can trigger alarm when the air flow rate is low
45、erthan 30 m/min.8.9 Clean Room Air Filter FanA fan that blows airthrough a HEPA filter to improve particulate removal effi-ciency.8.10 HEPA VacuumA vacuum with a HEPA filter that isused to remove dust from a glove box or general filters storageor work environments.9. Reagents and Materials9.1 Filter
46、sA 47mm diameter polytetrafluoroethylene(PTFE) filter (PTFE Membrane Disc Filters). For example, aPall TF-200 47mm 0.2 m (P/N 66143) with a pore size of 0.2m, as described in 7.1.2, has been used. This type filter hastwo sides: one is PTFE and the other is polypropylene. Onlythe PTFE side faces inco
47、ming hydrogen fuel and collectsparticulates in hydrogen. New filters must be demonstrated tobe particle free. Filters must be inspected and conditionedbefore use. Inspection and conditioning must be performed ina temperature and humidity controlled environment free ofsuspended particulate matter, su
48、ch as glove box (8.1).9.2 De-Ionized or Regent Grade WaterPurified water withresistivity 18 megohms-cm at room temperature for ultrasoniccleaner (8.4).10. Hazards10.1 High Pressure Hydrogen:10.1.1 Hydrogen fuel pressure can approach 875 bar (12691psi). All PSA-H70 components must be constructed from
49、 316stainless steel, or better, and rated for this application.10.1.2 The total mass of hydrogen passing through thePSA-H70 during a sampling depends on how many FCVs arerefueled over one filter element. Smoking, camera flashes, ormobile phones usage are an ignition hazard and are not allowedwithin 7.6 m hydrogen fueling station itself. Additional safetyprecautions must be taken as necessary to prevent fire orexplosion.10.2 Static ChargesDuring particulate sampling, the ex-tremely high speed of hydrogen flow may generate a
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