1、Designation: D7651 10Standard 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 particulates in hydrogen intended as a fuel f
3、orfuel cell or internal combustion engine powered vehicles. Thistest method describes operating and quality control proceduresrequired to obtain data of known quality satisfying the require-ments of SAE J2719 and the California Code of Regulations,Title 4, Division 9, Chapter 6, Article 8, Sections
4、4180 4181.The levels of precision and accuracy stated. This test methodcan be applied to other gaseous samples requiring determina-tion of particulates provided the users data quality objectivesare satisfied.1.2 The values stated in SI units are to be regarded asstandard. No other units of measureme
5、nt are included in thisstandard.1.3 This standard does not purport to address all of thesafety 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 limitati
6、ons prior to use.2. Referenced Documents2.1 ASTM Standards:2D7650 Test Method for Sampling of Particulate Matter inHigh Pressure Hydrogen used as a Gaseous Fuel with anIn-stream Filter2.2 SAE Standards:3SAE J2719 Hydrogen Quality Guideline for Fuel CellVehicles, April 2008SAE J2600 Compressed Hydrog
7、en Surface Vehicle Refuel-ing Connection Devices2.3 Other Standards:California Code of Regulations , Title 4, Division 9, Chapter6, Article 8, Sections 4180 41814ISO 14687 Hydrogen fuel - Product specification - Part 1:All applications except proton exchange membrane(PEM) fuel cell for road vehicles
8、53. Terminology3.1 Acronyms:3.1.1 FCVHydrogen Fuel Cell Vehicle3.1.2 PSAParticulate sampling adapter for sampling par-ticulate in hydrogen fuel.3.1.3 PEMPolymer Electrolyte Membrane, also calledProton Exchange Membrane3.1.4 SAESociety of Automotive Engineering3.2 Definitions:3.2.1 contaminantimpurit
9、y that adversely affects the com-ponents within the fuel cell system or the hydrogen storagesystem3.2.2 densityMass per unit of volume of the fuel gas or airbeing considered.3.2.3 fuel cell hydrogenhydrogen satisfying the specifica-tions in SAE J2719.3.2.4 weight monitoring filter, WMFThis filter is
10、 putinside the glove box (7.3) with balance (7.1) and not removedfrom the glove box (7.3). The weight of this filter is alwaysmeasured before and after each measurement event.3.3 SAE J2719Informational Report on the developmentof a hydrogen quality guideline for fuel cell vehicles. Thisreport specif
11、ies PEM FCV hydrogen fuel quality from thefueling nozzle.3.4 SAE J2600 Compressed Hydrogen Surface Vehicle Re-fueling Connection DevicesThis document specifies thedesign requirements for nozzles and receptacles used in highpressure hydrogen applications such as delivery from a fuelingstation to a FC
12、V4. Summary of Test Method4.1 This procedure is for the weight determination of filtersbefore and after collection of particulates contained within1This test method is under the jurisdiction ofASTM Committee D03 on GaseousFuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen andF
13、uel Cells.Current edition approved July 1, 2010. Published August 2010. DOI: 10.1520/D765110.2For 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 standards Document
14、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 Administrative Law 300 Capitol Mall, Suite 1250Sacramento, CA 95814-43395Available from International Organization for Standardization
15、(ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.hydrogen fuel or other gaseous streams at fueling stationdispenser nozzles (Test Metho
16、d 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 total volume of hydrogen or other gaseousfuel passing through a fi
17、lter. Every precaution should be takento avoid contamination of particulates 10 m or larger onto thefilter coming from the PSA, the analytical system, ambient air,filter handling or other environmental sources.5. Significance and Use5.1 Low operating temperature fuel cells such as protonexchange mem
18、brane 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 andinternal combustion system needs as defined in SAE J2719.The particulates in hy
19、drogen fuel for FCVs and gaseoushydrogen powered internal combustion engine vehicles mayadversely affect pneumatic control components, such as valves,or other critical system components. Therefore, the concentra-tion of particulates in the hydrogen fuel should be limited asspecified by ISO 14687, SA
20、E J2719, or other hydrogen fuelquality specifications.5.2 Although not intended for application to gases otherthan hydrogen fuel, techniques within this test method can beapplied to gas samples requiring determination of particulatematter.6. Interferences6.1 Particulate matter 10 m or larger origina
21、ting in theenvironment or equipment will interfere with the determinationof total particulate matter collected on the filter. Every precau-tion should be taken to avoid contamination of particulates 10m or larger onto the filter coming from the PSA, the analyticalsystem, ambient air, filter handling
22、, or other environmentalsources.6.2 To minimize contamination of the filters from bodymoisture and oils, wear powder-free gloves while handlingfilters outside of the glove box.6.3 Moisture content may affect polytetrafluoroethylene(PTFE) filter weight, even though the polytetrafluoroethylene(PTFE) f
23、ilter is hydrophobic. Filters should be equilibrated fora minimum of 24 h in a controlled environment prior toweighing. For reference, U.S. EPA filter conditioning require-ments for PM10 samples are a temperature range of 25 C (63 C) and a humidity range of 20 to 30% RH (6 5% RH).7. Apparatus7.1 Bal
24、anceThe balance must measure to 10-5 g. Thebalance should have the capability to download the weightmeasurement into Microsoft Excel6,7, or a similar program, forweight recording and calibration. In order to prevent contami-nation of particulates from ambient air, the balance must beplaced inside a
25、glove box in a small confined room with aHEPA8,7air cleaner.7.2 Calibration weightClass 1 (Class S)category cali-bration weights with a tolerance of 6 0.1 mg. certified astraceable to NIST mass standards. The weights used forcalibration are a 0.05 g and 0.2 g weight, of corrosion-resistantconstructi
26、on. Calibration weight is to be certified on an annualbasis. The weight of the particular 0.2m polytetrafluoroeth-ylene (PTFE) filter used in this method test was around 0.1g.7.3 Glove boxA glove box is a sealed container that, inthis application, is designed to allow weight measurement bybalance wi
27、thout particulate contamination from ambient air.Two gloves are generally built into the front sides of the glovebox with entry arranged in such a way that the user can placetheir hands into the gloves and perform weight measurement,install filters and assemble the filter holder inside the box. Theg
28、love box must be maintained clean at all times and any visualparticulate matter must be removed immediately. A HEPAvacuum can be used for cleaning purposes. A side evacuationport or anti-chamber should also be used to minimize contami-nating the glove box environment. The glove box should beflushed
29、at all times with clean dry N2 maintaining a RH of 30%or less inside the glove box as determined by a data logger orother device installed in the glove box.7.4 Static Charge Removal DeviceA static charge re-moval device, such as an ionization bar, must be placed insidethe glove box (7.3) next to the
30、 balance. Before measurement ofany material, such as standard weights and filters, the staticcharges on the material must be removed using a static chargeremoval device. Alternatively, anti-static strips which consistof radioactive (a - particle) Polonium-210 strips can be used todischarge static fr
31、om weights and filters. Polonium stripsshould be replaced every 6 months (conservatively) or accord-ing to the useful life quoted by the manufacturer.7.5 Moisture/Temperature Data LoggerA data logger isplaced inside the glove box to measure both moisture andtemperature of atmosphere inside the glove
32、 box either continu-ously or at pre-defined intervals. The moisture of the glove boxis kept of 30% or less using reagent grade or better nitrogenflow. All the temperature and moisture information are storedin a data logger, which is downloaded into excel, or a similarprogram after completion of meas
33、urements.7.6 Mini-Clean Room A small clean room with HEPAfilter must be used to store new polytetrafluoroethylene (PTFE)filters, the filter holder, and sampled filters at moisture less than30%.7.7 HEPA VacuumA vacuum with HEPA filter is used toremove dust from the glove box or areas where filters ar
34、estored or manipulated.7.8 Light box (Optional)A light box may be useful forinspection of filters.6Microsoft Excel is a trademark of the Microsoft Corporation, One MicrosoftWay Redmond, WA 98052-63997The mention of trade names in this test method does not constitute endorsementor recommendation. Oth
35、er manufacturers of equipment or equipment models can beused.8HEPA is a trademark of the HEPA Corporation, 3071 East Coronado StreetAnaheim, CA 92806D7651 1028. Reagents and Materials8.1 FilterA 47 mm diameter polytetrafluoroethylene(PTFE) filter (PTFE Membrane Disc Filters) is used. One sideof this
36、 type filter is composed of polytetrafluoroethylene(PTFE) and the reverse side is composed of polypropylene.Installed in the filter holder, the PTFE side should face thehydrogen fuel stream. The polypropylene side of the filter isgenerally shinier than the PTFE side, which is dull whenviewed under a
37、 bright light. When examining, handling, andweighing filters, the side facing the gas stream and collectingparticulates must always face up. Before usage of any newfilter, examine it carefully inside a glove box to ensure the filteris not damaged and that there are no particulates on the filter.Filt
38、ers containing particulates should be discarded as they areunsuitable for usage.9. Sampling, Test Specimens, and Test Units9.1 Test SpecimensParticulates.9.2 Test Unitsg/L, mg/kg.10. Preparation of Balance10.1 BalanceBalance must be put in a glove box de-scribed in 7.3 and remain there throughout th
39、e proceduresdescribed in this standard.11. Calibration and Standardization11.1 Balance CalibrationThe balance is calibrated at thebeginning of a weighing session using a 0.05 and 0.2 gstandard weights.Afilter blank is also weighed. In addition thebalance is internally calibrated with internal standa
40、rd weightsautomatically at pre-determined intervals.11.2 QC weighing of the first filter in a batch of ten filters isrecommended.12. Conditioning12.1 Filter ConditioningNew filters are stored in theiroriginal packaging and are considered ready for use whenstored in mini-clean room as described in 7.
41、6.13. Procedure13.1 Filter Weighing Procedure13.1.1 Transfer new polytetrafluoroethylene (PTFE) filter ina box from a mini clean room (7.6) to a glove box (7.3)containing a balance inside. Turn on the nitrogen flow at theflow rate of 0.5 L per minute for about an h to lower moisturecontent inside th
42、e glove box below 30%. Keep nitrogenflowing throughout the measurement process.13.1.2 The analyst must wear gloves when handling filtersand filter holders. Clean non-powdered plastic gloves withplastic sleeves are used for activity outside the glove box.polytetrafluoroethylene (PTFE) filters must be
43、 handled usingclean plastic or polytetrafluoroethylene (PTFE) coated twee-zers.13.1.3 Inspect the filters:13.1.3.1 Filters must not be contaminated with particulatesas seen by eye under a light box or under a microscope.13.1.3.2 Filter must not be torn or nicked. If damageddiscard filter.13.1.4 Set
44、up the balance so that the output of balance candirectly download to Excel or a similar data logging system.Perform a calibration so that all the calibration data isdownloaded.13.1.4.1 Set up the balance so that the weight number ofeach measurement can be automatically downloaded every twoseconds.13
45、.1.5 Since the weight for each measurement can shiftback and forth at five places after decimal point (10-5 g), a rulemust be set up to determine which weight number should beselected. The rule suggested is that the first value, that persistsfor at least 12 s without change will be selected.13.1.6 T
46、he typical sequence for measurement is as follow-ing:13.1.6.1 Internal Calibration:13.1.6.2 200 mg,13.1.6.3 50 mg,13.1.6.4 WMF,13.1.6.5 Filter#1,13.1.6.6 Filter#2,13.1.6.7 ,13.1.6.8 Repeat weighing all the Filters in the above se-quence nine additional times,13.1.6.9 WMF.13.1.7 The average weight of
47、 the ten measurements of eachfilter is the weight of the filter for particulate concentrationcalculation. The percent relative standard deviation of the tenweights for each filter should be less than 0.02%.13.1.8 The reason to monitoring weight of WMF is to makesure the environment of the glove box
48、(7.3) does not affectweight of the polytetrafluoroethylene (PTFE) filter used forparticulate monitoring in hydrogen fuel.14. Calculation or Interpretation of Results14.1 The polytetrafluoroethylene (PTFE) filter before andafter sampling is weighed according to 13.1. The difference ofthe weight in gr
49、am multiplied by 1000 divided by hydrogenfuel sampled in kg is the particulate concentration in mg per Kgof hydrogen.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 24.4 L at 25 C. Therefore, the totalvolume of hydrogen is hydrogen in kg * 1000/2 * 24.4 L. Theweight of particulate in gram multiplied by 1 000 000 dividedby total volume of
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