1、Designation: D7650 10Standard Test Method forTest Method for Sampling of Particulate Matter in HighPressure Hydrogen used 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 oforigin
2、al adoption or, 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 hydroge
3、n fuel used in hydrogen fuel cell vehicles or gaseoushydrogen powered internal combustion vehicle engines up topressures of 35 MPa (350 Bars) using an in-stream filter. Thistest method describes sampling apparatus design, operatingprocedures, and quality control procedures required to obtainthe stat
4、ed levels of precision 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 The values stated in Bars in 1.1, 7.1 and 10.1.1 are forinformation only.1.3 This standard does not purport to address all of thesafet
5、y concerns, if 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
6、 Measurement of Par-ticulate Concentration of Hydrogen Fuel2.2 SAE Standards:3SAE J2719 Information Report on the development of ahydrogen quality guideline for fuel cell vehicles.SAE J2600 Compressed Hydrogen Surface Vehicle Refuel-ing Connection Devices2.3 ISO Standard:ISO/CD 146872 Hydrogen fuel
7、Product Specification Part 2: Proton exchange membrane (PEM) fuel cellapplications for road vehicles.3. 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 also called aProton
8、 Exchange Membrane3.1.4 PSAParticulate sampling adapter for sampling par-ticulate in hydrogen fuel.3.1.5 SAESociety of Automotive Engineering3.2 Definitions:3.2.1 pinholea small hole generated during sampling ofparticulate in hydrogen that can be identified by microscope.3.3 SAE J2719Informational R
9、eport on the developmentof a hydrogen quality guideline for fuel cell vehicles. Thisreport specifies PEM FCV hydrogen fuel quality from thefueling nozzle.3.4 SAE J2600 Compressed Hydrogen Surface VehicleRefueling Connection Devices.This document specifies thedesign requirements for nozzles and recep
10、tacles used in highpressure hydrogen applications such as delivery from a fuelingstation to a FCV4. Summary of Test Method4.1 This test method provides a procedure for the samplingof particulate matter contained in hydrogen used as a FCV fuel.It is designed to collect all particulates 0.2 m or large
11、rcontained 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 sampling particulates in hydrogenfuel is called a Particulate Sampling Adapter (PSA) and isdescribed
12、in 7. Great care should be taken to avoid contami-nation and exposure of the PSA, filters, and other equipmentwith particles sized 10 m or larger prior to use.1This test method is under the jurisdiction ofASTM Committee D03 on GaseousFuels and is the direct responsibility of Subcommittee D03.14 on H
13、ydrogen andFuel Cells.Current edition approved July 1, 2010. Published August 2010.DOI: 10.1520/D765010.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standard
14、s Document Summary page onthe ASTM website.3Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,PA 15096-0001, http:/www.sae.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Fuel cel
15、ls 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 purity to satisfy fuel cell system needs. In addition,internal
16、combustion engines using high pressure hydrogen fuelalso require low particulate containing fuel. Specifically, par-ticulate matter has been implicated in the premature failure ofpneumatic control components, such as valves within vehicles.This sampling procedure is used to collect and measuresample
17、s containing particles 0.2 m or larger in size asspecified in ISO/CD 146872, SAE J2719, and other hydrogenfuel quality specifications.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 applie
18、d to otherhigh pressure gaseous samples requiring particulate 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 to avoid
19、 contamination of the apparatus and allequipment, supplies and gases used in these procedures.7. Apparatus DesignNOTE 1The use of trade names in this section are not intended as anendorsement for use.7.1 The PSAis designed for pressures at least up to 6000 psi(420 Bar) with appropriate safety factor
20、s built in and isdesigned for a flow rate of 38 g per second of hydrogen withoutdamage to the filter or leakage from the PSA. The PSApossesses a receptacle as per SAE J2600 which is connecteddirectly to the filter housing. A high pressure needle valve withworking pressure at 42 Mpa is attached downs
21、tream of thefilter holder to stop the hydrogen flow when leak testing thePSA. Downstream of the needle valve, a check valve isattached to prevent the back flow of hydrogen during sampling.In summary, the configuration of the PSA, as shown in Fig. 1,is:A SAE J2600 compliant Receptacle Filter Holder w
22、ithFilter Needle Valve Check Valve.Fig. 1 illustrates a PSA design that has been successfullyused to collect particulate samples from 5075 psi (350 Bar) fuelcell quality hydrogen. The PSA should be rated above theoperating pressure, and all materials used must be rated forhigh pressure hydrogen appl
23、ications at a 1.5 times minimummargin of safety at the maximum operating pressure. Therecommended working pressure of the PSA and associatedmaterials is 42 Mpa. Contamination from polytetrafluoroeth-ylene (PTFE) tape, lubrication or other sources must beavoided and the apparatus must be cleaned prio
24、r to use usingappropriate cleaning techniques for high pressure hydrogenapplications. The design of the PSAshould include minimizingthe distance and surface area between the nozzle and filter tominimize the particulates generated from the surface of thisarea by fast flow and high pressure hydrogen7.
25、1.1 High Pressure Filter HolderThe high pressure filterholder is a 47 mm, stainless steel housing with maximum inletpressure 70 Mpa and a polytetrafluoroethylene (PTFE) inner47mm diameter PTFE-O ring. The filter holder must beequivalent, similar or exceed performance characteristics of thefilter hol
26、der shown in Fig. 1.7.1.2 FilterA polytetrafluoroethylene (PTFE) filter thattolerates flow rates of up to 38 g per s without damage andcollects particulates with a minimum size of 0.2 m.NOTE 2Hydrogen back flow must be avoided since the backflow ofhydrogen can cause pinhole formation or other damage
27、 to filters. Thedesign of the apparatus and sampling procedures must prevent fuelbackflow, such as implementing the use of a check valve as shown in Fig.1, Item 6.7.1.3 PSA Support The mechanical PSA support must bedesigned to securely hold the PSA and a station nozzle. Thenozzle should be held firm
28、ly and not move or shake duringparticulate sampling.7.1.4 PSA Design variationsThe design of the PSAdown-stream of the stainless steel Swagelok4,5fitting (union 7 in Fig.1) will vary with the sampling procedure. The procedurevariations include:(1) Sampling while the hydrogen is venting to atmosphere
29、,(2) Sampling while fueling a vehicle.Sampling when fueling into a vehicle tank collects a samplemore representative of the particulates seen by vehicles inservice since the flow rate is much higher when fueling into avehicle tank than when venting to atmosphere. The followingsections describes the
30、post Swagelok fitting designs in detail.7.1.4.1 PSA design for venting to atmosphereFor appli-cation to systems requiring venting hydrogen through the PSAto atmosphere, a ventilation assembly containsa3mlong SSbraided tubing connects Item 7 of Fig. 1 in one end and anotherto a dual 2.4 m long 1.27cm
31、 OD SS tubing vertical to theground. During sampling, the hydrogen fuel flows throughPSA, then the ventilation assembly, before venting to air at 8ftabove ground.7.1.4.2 PSA design for flowing hydrogen to gaseous hydro-gen vehicle tankThe configuration is the same as 7.1.4.1,except the downstream of
32、 the PSA at the elbow of the PSA(Item 7, Fig. 1) connects the inlet hose of a 2nd nozzleassembly. The 2nd SAE J2600 nozzle is then attached to thereceptacle on a vehicle. While sampling, the hydrogen fuelflows from station SAE J2600 nozzle (1st nozzle) PSAinlet hose of a 2nd SAE J2600 nozzle assembl
33、y receptacleof FCV tank.8. Additional Equipment Needed8.1 Glove boxA glove box is a sealed container that isdesigned to assemble PSA without particulate contaminationfrom ambient air. Two gloves are built into the sides of the4Swagelok is a trademark of Swagelok Fluid System Technologies, 29500 Solo
34、nRoad, Solon OH 44139.5The mention of trade names in this test method does not constitute endorsementor recommendation. Other manufacturers of equipment or equipment models can beused.D7650 102glove box with entry arranged in such a way that the user canplace hands into the gloves to install the fil
35、ter 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 or filters. AHEPA6,5vacuum can be used to remove particles from theglove bag and other equipment.8.2 Moisture/
36、Temperature Data LoggerA data logger isplaced inside the glove box to measure both moisture andtemperature continuously at pre-defined intervals such as once6HEPA is a trademark of the HEPA Corporation, 3071 East Coronado StreetAnaheim, CA 92806.Item Description1 SAE J2600 hydrogen receptacle withou
37、t filter2 Swagelok4High pressure SS-6SAEH-14TH(Pressure rating 9,000psi)3 Millipore High Pressure 316 SS Filter Housing (47mm, 02.m) P/NXX45047004 3O Outlet14 in. FNPT-SAE716-20 union5 High pressure needle valve6 Check valve7 SS Swagelok Tube fitting, female elbow,38 in. tube OD 314 MNPT,P/N SS-6002
38、4FIG. 1 PSA ComponentsD7650 103every two to five minutes. Moisture in the glove box is keptbetween 15 to 30% using reagent grade nitrogen. All tempera-ture and moisture data are stored in a data logger, which aredownloaded into a Microsoft Excel7,5, or a similar program,sheet after completion of mea
39、surements.8.3 Mini-Clean RoomA small clean room with HEPA airfiltration must be used to store 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 particu
40、lates on parts of PSA intoreagent grade water.8.5 Hydrogen Leak DetectorAhydrogen leak detector is arequired safety device needed to detect small hydrogen gasleaks in particular when the PSA is pressurized prior toparticulate collection. The diluted soap bubble should not beused to detect hydrogen l
41、eak from PSA.8.6 HEPA Filter Horizontal Flow HoodA HEPA 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 100 ft/minute
42、. Ifbelow this velocity, the air velocity meter should trigger analarm notifying 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 airf
43、low meter can trigger alarm when the air flow rate is lowerthan 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 storag
44、eor work environments.9. Reagents and Materials9.1 FiltersA 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
45、 the other is polypropylene. Onlythe PTFE side faces incoming 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 contr
46、olled environment free ofsuspended particulate matter, such 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 6000 psi (
47、414Bar). All PSA components must be constructed from 316stainless steel, or better, and rated for this application.10.1.2 The total mass of hydrogen passing through the PSAduring a sampling event is approximately 2 kg. Smoking,camera flashes, or mobile phones usage are an ignition hazardand are not
48、allowed within 7.6 m from the both ventilationtubing (7.1.4.1) and hydrogen fueling station itself. Additionalsafety precautions 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 staticchar
49、ge on PSA components. The static charge is removed bygrounding the PSA with a wire from hydrogen fueling stationor other available grounding wire(s).10.3 Hydrogen EmbrittlementHigh pressure hydrogencan cause embrittlement of contacting metal surfaces or maycause metal hydride formation on metal surfaces. This can leadto catastrophic PSA failure, hydrogen leaks or generation ofpyrophoric particulates. The PSA and all equipment usedaccording to this standard must be closely inspected for signsof cracks, metal oxide dust f
