1、Designation: D7651 17Standard Test Method forGravimetric Measurement of Particulate Concentration ofHydrogen Fuel1This standard is issued under the fixed designation D7651; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f 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 intended for gravimetricdetermination of particulate concentration in hydrogen in-tend
3、ed as a fuel for fuel cell or internal combustion enginepowered vehicles. This test method describes operating andquality control procedures required to obtain data of knownquality satisfying the requirements of SAE J2719. This testmethod can be applied to other gaseous samples requiringdeterminatio
4、n of particulates provided the users data qualityobjectives are satisfied.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its u
5、se. 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.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-i
6、zation established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4150 Terminology Relating to Gaseous FuelsD7650 Te
7、st Method for Sampling of Particulate Matter inHigh Pressure Hydrogen used as a Gaseous Fuel with anIn-Stream FilterE617 Specification for Laboratory Weights and PrecisionMass Standards2.2 SAE Standards:3SAE J2600 Compressed Hydrogen Surface Vehicle Refuel-ing Connection DevicesSAE J2719 Hydrogen Qu
8、ality Guideline for Fuel Cell Ve-hicles2.3 Other Standards:Code of Federal Regulations, Title 40, Part 50, Appendix L,Section 8.24ISO 146872 Hydrogen fuel - Product specification - Part2: Proton exchange membrane (PEM) fuel cell applica-tions for road vehicles53. Terminology3.1 Acronyms:3.1.1 FCVHyd
9、rogen Fuel Cell Vehicle3.1.2 HEPAHigh Efficiency Particulate Air3.1.3 PEMPolymer Electrolyte Membrane, also calledProton Exchange Membrane3.1.4 PEMFCProton Exchange Membrane Fuel Cell3.1.5 PTFEPolytetrafluoroethylene3.1.6 SAESAE International3.2 Definitions: For definitions of general gaseous fuelte
10、rms used in this practice, refer to D4150.3.2.1 weight monitoring filter, WMFThis filter is putinside the glove box or clean room (7.3) with the balance (7.1)and never removed. The weight of this filter is alwaysmeasured before and after each measurement event.4. Summary of Test Method4.1 This test
11、method is used to determine the concentrationof particulate matter and nonvolatile reside on filters collectedfrom hydrogen fuel or other gaseous streams at fueling station1This test method is under the jurisdiction ofASTM Committee D03 on GaseousFuels and is the direct responsibility of Subcommitte
12、e D03.14 on Hydrogen andFuel Cells.Current edition approved Nov. 1, 2017. Published December 2017. Originallyapproved in 2010. Last previous edition approved in 2010 as D765110. DOI:10.1520/D765117.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
13、at serviceastm.org. For Annual Book of ASTMStandards volume information, 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 Office of the Federal Register, 800 N. C
14、apitol St., NW Suite 700Washington, DC 20001.5Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
15、-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technic
16、al Barriers to Trade (TBT) Committee.1dispenser nozzles (Test Method D7650, SAE J2600) or othergaseous fuel delivery system dispenser interfaces. The particu-late concentration is determined by dividing the particulateweight, which is the difference of filter weights before and aftersampling, by the
17、 total volume of hydrogen or other gaseousfuels passing through the filter. Every precaution should betaken to avoid contamination of particulates onto the filtercoming from the particulate sampling adapter, the analyticalsystem, ambient air, filter handling, or other environmentalsources.5. Signifi
18、cance and Use5.1 Low operating temperature fuel cells such as protonexchange membrane fuel cells (PEMFCs) require high purityhydrogen for maximum material performance and lifetime.Measurement of particulates in hydrogen is necessary forassuring a feed gas of sufficient purity to satisfy fuel cell an
19、dinternal combustion system needs as defined in SAE J2719.The particulates in hydrogen fuel for fuel cell vehicles (FCV)and gaseous hydrogen powered internal combustion enginevehicles may adversely affect pneumatic control components,such as valves, or other critical system components. Therefore,the
20、 concentration of particulates in the hydrogen fuel should belimited as specified by ISO 14687-2, SAE J2719, or otherhydrogen fuel quality specifications.5.2 Although not intended for application to gases otherthan hydrogen fuel, techniques within this test method can beapplied to gas samples requir
21、ing determination of particulateconcentration.6. Interferences6.1 Particulate matter on the filter from sources other thanthe hydrogen fuel will interfere with the determination ofparticulate concentration. Every precaution should be taken toavoid contamination of particulates onto the filter from t
22、heparticulate sampling adapter, the analytical system, ambient air,filter handling, or other environmental sources.6.2 To minimize contamination on the filters from body oilsand moisture, wear powder-free gloves while handling filters.6.3 Humidity may affect polytetrafluoroethylene (PTFE)filter weig
23、ht. Filters should be equilibrated for a minimum of24 hours (h) in a controlled environment prior to weighing. Forreference, U.S. EPA filter conditioning requirements for PM10samples are a temperature range of 21 6 2 C and a humidityrange of 35 6 5% relative humidity (RH).7. Apparatus7.1 BalanceThe
24、balance must have a readability of 0.01milligrams (mg). The balance may have the capability torecord the weight and calibration data into Microsoft Excel,6,7or a similar program. In order to prevent contamination ofparticulates from ambient air, the balance must be placed insidea glove box or clean
25、room with a HEPA8,7air filter.7.2 Calibration WeightASTM Class 1 (E617)Categorycalibration weights with a tolerance of 6 0.01 mg certified astraceable to a national metrology institute (NMI) such as NISTmass standards should be used. The weights used for calibra-tion are 0.05 g and 0.2 g, of corrosi
26、on-resistant construction.Calibration weights are to be certified on an annual basis.7.3 Glove Box (Option A)Aglove box is a sealed chamberthat, in this application, allows weight measurements to betaken without particulate contamination from ambient air. Twogloves are built into the front side of t
27、he glove box so that theuser can place their hands into the gloves and perform weightmeasurements, install filters, and assemble the filter holders. Aside evacuation port or antechamber should also be used tominimize contamination of the glove box environment. Theglove box must be kept clean at all
28、times and any visualparticulate matter must be removed immediately. The glovebox should have a steady flow of clean, dry nitrogen (N2)atalltimes. The temperature and humidity should be kept consistentat 21 6 2 C and 35 6 5% RH and should be monitored by adata logger or other device installed in the
29、glove box.7.4 Clean Room (Option B)Analysis should occur in aclimate-controlled, draft-free room constantly under positivepressure. The relative humidity must be maintained at 35 6 5%and the temperature must be maintained at 21 6 2 C. If thetemperature or humidity falls out of range, no weighing can
30、occur for 24 h. Before entering the clean room, the analystmust step on “sticky” floor mats to remove any particulatematter from the bottoms of shoes. The room must have a HEPAair filter on the inlet air system to remove particulates from theair.7.5 Static Charge Removal DeviceAstatic charge removal
31、device, such as an ionization bar, must be placed inside theglove box or clean room (7.3) next to the balance. The staticcharge on the materials, such as weights and filters, must beremoved before weighing. Alternatively, anti-static stripswhich consist of radioactive ( - particle) Polonium-210 can
32、beused to discharge static from weights and filters. Poloniumstrips should be replaced every 6 months (conservatively) oraccording to the useful life quoted by the manufacturer.7.6 Humidity/Temperature Data LoggerA data logger isplaced inside the glove box or clean room to measure bothhumidity and t
33、emperature of the atmosphere either continu-ously or at pre-defined intervals. The humidity is kept at 35 65% RH. Temperature and humidity information may be storedin a data logger, which can be downloaded into MicrosoftExcel,6,7or a similar program after completion of measure-ments.7.7 StorageA cle
34、an room or a glove box with a HEPAfilter may be used to store new PTFE filters, the filter holder,and sampled filters at 35 6 5% RH and 21 6 2 C.6Microsoft Excel is a trademark of the Microsoft Corporation, One MicrosoftWay Redmond, WA 98052-6399.7The mention of trade names in this test method does
35、not constitute endorsementor recommendation. Other manufacturers of equipment or equipment models can beused.8HEPA is a trademark of the HEPA Corporation, 3071 East Coronado StreetAnaheim, CA 92806.D7651 1727.8 HEPA VacuumA vacuum with a HEPA filter may beused to remove dust from the glove box or ar
36、eas where filtersare stored or handled.7.9 TweezersFilters must be handled using clean plastic orPTFE coated tweezers.7.10 GlovesClean, non-powdered plastic gloves must beworn when handling filters outside of the glove box.7.11 Light Box (Optional)A light box may be useful forinspection of filters.8
37、. Reagents and Materials8.1 FilterA 47 millimeter (mm) diameter PTFE filter(PTFE Membrane Disc Filters) is used. One side of this filteris composed of PTFE and the reverse side is composed ofpolypropylene. When the filter is installed in the filter holder,the PTFE side should face the hydrogen fuel
38、stream. Thepolypropylene side of the filter is generally shinier than thePTFE side. When examining, handling, and weighing filters,the PTFE must always face up. Before using a new filter,examine it carefully to ensure the filter is not damaged and thatthere are no particulates on the filter. Filters
39、 containingparticulates should be discarded as they are unsuitable for use.The weight of the particular 0.2 micrometer (m) PTFE filterused in this test method is approximately 0.1 gram (g).9. Sampling, Test Specimens, and Test Units9.1 Test SpecimensParticulates.9.2 Test Unitsg/L, mg/kg.10. Preparat
40、ion of Balance10.1 BalanceBalance must be placed in a glove box orclean room described in 7.3 and remain there throughout theprocedures described in this standard.11. Calibration and Standardization11.1 Balance CalibrationBefore taking any filtermeasurements, the balance should be internally calibra
41、ted,externally calibrated using the 0.05 g and 0.2 g standardweights, and a filter blank should be weighed.11.2 QC weighing of the first filter in a batch of ten filters isrecommended.11.2.1 Take the average weight of three measurements of afilter. The precision of the mass measurements should begre
42、ater than the balances repeatability.12. Conditioning12.1 Filter ConditioningNew filters are stored in theiroriginal packaging and are considered ready for use whenstored according to 7.7 for 24 h.12.2 Post-Sampling Filter ConditioningFilters should beremoved from the particulate sampling adapter an
43、d placedinside a storage container (7.7) for 24 h.13. Procedure13.1 Filter Inspection:13.1.1 Filters must not be contaminated with particulates asseen by the naked eye, on a light box, or under a microscope.13.1.2 Filter must not be torn or nicked. If damaged discardfilter.13.2 Filter Weighing Proce
44、dure:13.2.1 Perform an internal balance calibration.13.2.2 Perform an external balance calibration using the0.05 g and 0.2 g weights.13.2.2.1 Wait for the balance to stabilize for at least 12 swithout change before taking a reading.13.2.3 Take the weight of the WMF.13.2.4 Take the weight of up to 10
45、 PTFE filters.13.2.5 Weigh the WMF.13.2.6 Continue weighing up to 10 filters and the WMFuntil all filters have been weighed.13.2.7 Perform an external balance calibration using the0.05 g and 0.2 g weights. For a valid analytical sequence, anymeasurement of the 0.05 g and 0.2 g weight must not varymo
46、re than 6 1 mg from the certified weight.14. Calculation or Interpretation of Results14.1 The PTFE filter is weighed before and after samplingaccording to 13.2. The particulate concentration in mg per kgof hydrogen is found by taking the difference of the weight ingrams multiplied by 1000 and divide
47、d by the amount ofhydrogen fuel sampled (kg).Particulate ConcentrationSmgkgD5 (1)Difference in Weight g! of Filter before and after Sampling*100Hydrogen fuel Sampled in kg14.2 The hydrogen in kg multiplied by 1000 and thendivided by 2 gives the moles of hydrogen. The volume of amole of hydrogen is 2
48、4.4 L at 25 C. Therefore, the totalvolume of hydrogen is hydrogen in kg * 1000/2 * 24.4 L. Theweight of particulates in grams multiplied by 1 000 000 dividedby total volume of hydrogen gives the particulate concentrationin g/L.Particulate ConcentrationSgLD5 (2)Difference in Weight g! of Filter befor
49、e and after SamplingHydrogen fuel Sampled in kg*10002*24.4 L15. Report15.1 Report concentration of particulates calculated in 14 inboth g/L and mg/kg.16. Precision and BiasNOTE 1Statements of precision and bias for this method will beprovided as a result of inter-laboratory testing which will be performedwithin five (5) years.16.1 RepeatabilityThe difference between successive testresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materials.16.2 Repeatability1%
