1、Designation: D7606 11Standard Practice forSampling of High Pressure Hydrogen and Related Fuel CellFeed Gases1This standard is issued under the fixed designation D7606; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t 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 practice describes a hydrogen quality samplingapparatus (HQSA) and a procedure for the sampling of highpressure hydr
3、ogen at fueling nozzles of 35 or 70 Mega Pascal(MPa) fueling stations.1.2 This practice does not include the analysis of theacquired sample. Applicable ASTM standards include but arenot limited to test methods referenced in Section 2 of thispractice.1.3 This practice is not intended for sampling and
4、 measur-ing particulate matter in high pressure hydrogen. For proce-dures on sampling and measuring particulate matter see ASTMD7650 and D7651.1.4 The values stated in SI units are standard. The valuesstated in inch-pounds are for information only.1.5 This standard does not purport to address all of
5、 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 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D7650 Test Method for Te
6、st Method for Sampling ofParticulate Matter in High Pressure Hydrogen used as aGaseous Fuel with an In-Stream FilterD7651 Test Method for Gravimetric Measurement of Par-ticulate Concentration of Hydrogen Fuel2.2 SAE Standards3SAE J2600 Compressed Hydrogen Surface Vehicle Refuel-ing Connection Device
7、sSAE J2799 70 MPa Compressed Hydrogen Surface VehicleFuelling Connection Device and Optional Vehicle toStation CommunicationsSAE TIR J2719 Information Report of the Development ofa Hydrogen Quality Guideline for Fuel Cell Vehicles2.3 California Code of Regulations:4California Code of Regulations Tit
8、le 4, Division 9, Chapter6, Article 8, Sections 4180 41813. Terminology3.1 Definitions:3.1.1 absolute pressurePressure measured with referenceto absolute zero pressure, usually expressed in MPa, mm Hg,or pound per square inch (psi).3.1.2 contaminantimpurity that adversely affects the com-ponents wit
9、hin fuel cell or hydrogen storage systems3.1.3 gauge pressurePressure measured above ambientatmospheric pressure. Zero gauge pressure is equal to ambientatmospheric (barometric) pressure.3.1.4 gaseous fuelMaterial to be tested, as sampled,without change of composition by drying or otherwise.3.1.5 hy
10、drogen quality sampling apparatus (HQSA)anapparatus used to collect hydrogen from a 35 or 70 MPahydrogen fueling nozzle (SAE J2600 and SAE J2799) into asample container.3.2 Definitions of Terms Specific to This Standard:3.2.1 high pressure hydrogenFor the purposes of thispractice, high pressure hydr
11、ogen is hydrogen defined as hydro-gen pressurized to 35 or 70MPa.4. Summary of Practice4.1 This practice describes an apparatus and procedure forthe sampling of high pressure hydrogen from fueling nozzlesconforming to SAE J2600 or SAE J2799. This practice isintended as a guideline for ensuring colle
12、ction of a represen-tative sample without introducing trace levels of contaminants.Samples collected using this practice should be suitable fortrace analysis of contaminants, utilizing a variety of analyticaltechniques.1This practice is under the jurisdiction of ASTM Committee D03 on GaseousFuels an
13、d is the direct responsibility of Subcommittee D03.14 on Hydrogen andFuel Cells.Current edition approved March 1, 2011. Published March 2011. DOI: 10.1520/D760611.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book
14、 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 Administrative Law, 300 Capitol Mall Suite 1250,Sacramento, CA 95
15、8144339.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Hydrogen is delivered to fuel cell powered automotivevehicles and stationary appliances at pressures up to 87.5 MPa.The quality of hydrogen delivered
16、is a significant factor inmaximizing fuel cell efficiency and life span. Contaminationcan arise during the production of fuel cell feed gases, storagecontainers, station tubing and fuel lines up to the nozzle usedfor fuel delivery. Collection of a representative fuel samplewithout the introduction o
17、f contamination even as low asparts-per-billion (ppb) per contaminant during collection iscrucial for assessing the quality of fuel in real world applica-tions.5.2 This practice is intended for application to high pres-sure, high purity hydrogen; however, the apparatus design andsampling techniques
18、may be applicable to collection of otherfuel cell supply gases. Many of the techniques used in thispractice can be applied to lower pressure/lower purity gasstreams.6. Apparatus Design6.1 The general design of the HQSA is shown in Fig. 1,which is a depiction of the apparatus with the nozzle hydrogen
19、pressure regulated to approximate 6.9 MPa (1000 psi) beforesampling. The pressure of 6.9 MPa (1000 psi) is selected as anexample since it is, generally, the lowest pressure tolerated byhydrogen station safety shutoff systems while still providing asample that analytical laboratories can safely handl
20、e routinely.All HQSA parts, including the ventilation tubes, are made of316 grade stainless steel (SS).6.2 HQSA Metal Support Plate ( 1, Fig. 1)The HQSAmetal support plate is utilized to mitigate damage duringtransportation and support the apparatus. The HQSA is firmlyfixed to a metal support plate
21、by tube supports (2, Fig. 1.).6.3 Movable Adjustable PlatformBefore sampling, themetal plate holding the HQSA is firmly clamped onto a heightadjustable and movable platform, such as a heavy duty cartwith a hydraulic adjustable horizontal platform and brakes onits wheels. The cart is moved to a posit
22、ion close to the fuelingstation and the height of platform is adjusted so that the fuelingnozzle attaches easily to the receptacle of HQSA. The platformheight is adjusted to provide a safe and comfortable workspace. The cart is then locked into place using the cart wheelbrakes.6.4 SAE J2799 Receptac
23、le (3, Fig. 1) This receptacle canadapt to both 35 and 70MPa hydrogen fueling nozzles. Forsafety reason, the receptacle must be positioned vertically sothat the fueling nozzle attaches to the receptacle from the top.To support the weight of the fueling nozzle, the receptacle musthave an additional s
24、upport (3.1, Fig. 1), which is fixed to themetal support plate (1, Fig. 1).6.5 Main Valve (4, Fig. 1)The functions of the main valveare explained as follows:6.5.1 Station and HQSA leak testThe station leak test isperformed before hydrogen fuel sampling to ensure there areFIG. 1 Hydrogen Quality Samp
25、ling ApparatusD7606 112no leaks in the hydrogen fuel delivery system. For sampling thestation personnel must attach the fueling nozzle to theSAE J2799 receptacle (3, Fig. 1) first while the main valve isclosed. The station leak test procedure is then initiated. A handheld hydrogen leak detector is u
26、sed to check for leaks aroundall the connections from nozzle to the main valve as in 10.7.There is residual high pressure hydrogen left in the station hosewhen the station is not fueling. The residual high pressurehydrogen can be used for checking the leakage in the completeHQSA system, including th
27、e sample container, as shown in10.8.6.5.2 Prevention of High Pressure Hydrogen Passingthrough the RegulatorIf the main valve (4, Fig. 1)isnotinstalled and station fueling starts, the diaphragm of theregulator (5, Fig. 1) may fail due to rapid hydrogen pressur-ization. In this case, pressure relief v
28、alve (PRV) 15, (Fig. 1)will open to release hydrogen pressure above 10.3 MPa (1500psi). The main valve (4, Fig. 1) when closed is designed tocontain high pressure hydrogen when the station samplingstarts. The main valve is slowly turned to the open position andthe high pressure hydrogen is regulated
29、 to 6.9 MPa (1000 psi).6.6 Regulator 5 (Fig. 1) and all connections from the SAEJ2799 Receptacle to RegulatorThe regulator and all theconnections, including tubing, tubing fittings, adapter fittingsand unions from the SAE J2799 receptacle to the main valveand main valve to regulator must have a pres
30、sure rating of 103Mpa (15,000 psi) or higher. The regulator should have twogauges, 5.1 and 5.2 in Fig. 1, to monitor both inlet and outletpressures.6.7 Inlet and Outlet Valves (6 and 12, Fig. 1, respectively)The valves should be easily opened and closed, such as ballvalves. The HQSA and sample conta
31、iner are cleaned bypressurizing and, releasing hydrogen from the HQSA andsample container (10.11) using these valves. This cleaningprocedure can be repeated many times (10.11) but must beperformed at least 10 times to ensure a valid sample under mostsampling conditions.6.8 Sample ContainersThe press
32、ure rating of the samplecontainers is 12.4 MPa (1800 psi). The sample containers andboth inlet and outlet valves (8 and 10, Fig. 1, respectively) areinternally coated with silicon (Si) since sulfur gas analysis tolow ppb is required under SAE TIR J2719 and other hydrogenfuel quality specifications.
33、To avoid air contamination duringsampling, both inlet and outlet valves of sample containers areequipped with quick connects one end of the container has aquick-connect stem and the other end a quick-connect body.These two quick-connections (7 and 11, Fig. 1) and the inletand outlet valves provide a
34、 double seal on both ends of thesample container.6.9 HQSA Pressure Release Valve (14, Fig. 1) The valveis always closed before and during sampling. After collection,the pressure release valve is opened before removal of thepressurized and sealed sample container to release the hydro-gen pressure in
35、the HQSA through a check valve (16, Fig. 1).Hydrogen at 6.9 MPa (1000 psi) contained inside the HQSAmust be released before next sample container can be safelyconnected to the inlet quick-connection (7, Fig. 1).6.10 Proportional Release Valve (PRV, 15, Fig. 1)ThePRV is set at 10.3MPa (1500 psi) to p
36、rotect the 12.4 MPa (1800psi) pressure proof sample container.6.11 Check ValveThe check valve (16, Fig. 1) with 69Kilo Pascal (KPa) (10 psi) crack pressure is installed at the ventof the HQSA(Fig. 1) to prevent air from back diffusion into theHQSA.6.12 Ventilation Assembly (17, Fig. 1)The ventilatio
37、nassembly contains a 3 meter (m) (10 ft) long SS braided tubinginterfaced to a dual 2.4 m (8 ft) long 1.27 cm (12 in.) OutsideDiameter (OD) SS tubing which is kept vertical to the ground.During sampling, the hydrogen fuel flows through HQSA, thenthe check valve (16, Fig. 1), through thea3mlong SS br
38、aidedtubing (17.1, Fig. 1) and dual 2.4 m long 1.27 cm (12 in.) ODSS tubing (17.2, Fig. 1), before venting to atmosphere atapproximately 2.4 m (8 ft) above ground.7. Additional Equipment Needed7.1 Hydrogen Leak DetectorAhydrogen leak detector is arequired as a safety device needed to detect hydrogen
39、 gas leakswhen the HQSA is pressurized. Leak detection using soapbubbles must not be used due to possible moisture contamina-tion.8. Hazards8.1 High hydrogen pressureThe hydrogen pressure can beas high as 87.5MPa and constitutes both an explosion and firehazard.8.2 The total mass of hydrogen passing
40、 through the HQSAduring a sampling event is approximately 1 kilogram (kg).Smoking, camera flashes, or mobile phone usage is unsafewithin 7.6 m (25 ft) of either the ventilation tubing (6.12)orhydrogen fueling station itself. Additional safety precautionsmust be taken as necessary to prevent fire or
41、explosion, or both.8.3 Static ChargesDuring gaseous sampling, the ex-tremely high-speed hydrogen flow rate may generate a staticcharge on HQSA components. The static charge is removed bygrounding the HQSAwith a wire from hydrogen fueling stationor other available grounding wire(s).9. HQSA Cleaning9.
42、1 Do not clean the HQSA with water, iso-propanol or anyother solvent.9.2 The HQSA must be cleaned by purging during sam-pling. This is done by flowing one kilogram hydrogen fuelthrough the HQSA after the nozzle pressure is regulated to 6.9MPa (1000 psi). The hydrogen flow rate at 1000 psi isapproxim
43、ately 33.3 grams per second for a total sampling timeof around 30 s. At this flow rate, SAE TIR J2719 targetedconstituents will be removed from within the HQSA andsampling lines. This procedure is the best way to convenientlydehydrate and remove residual sulfur gases from the HQSA,sampling line, and
44、 sample container. Dehydration of theapparatus cannot be safely achieved at the station throughevacuation or heating, or both.10. Sampling Procedures10.1 Safety PrecautionDuring gaseous sampling, person-nel must wear goggles, safety shoes and a flame resistant labD7606 113coat or other industrial fl
45、ame resistant clothing. Personnel notdirectly involved in sampling should beat least 5 m away fromthe HQSA during sampling.10.2 Attach a ground wire to the station ground.10.3 Fix the HQSA onto a platform of a hydraulic cart(6.3).10.4 Connect HQSA to the ventilation system (6.12).10.5 Attach a 1-L 1
46、800 psi stainless steel sample containerto HQSA through quick connections (7 and 11, Fig. 1).10.6 Make sure all the valves of HQSA (Fig. 1) are closedand attach the station 35 or 70 MPa nozzle to the SAE J2799receptacle (3, Fig. 1).10.7 Start the station leak test using a hand held hydrogenleak dete
47、ctor to check leaks around all the connections from thenozzle to the main valve (4, Fig. 1). Any leak must beeliminated before proceeding.10.8 Open the main valve (4, Fig. 1) slowly and regulatethe nozzle pressure (5, Fig. 1) down to 6.9 MPa (1000 psi).10.8.1 Use a hydrogen leak detector to check fo
48、r leaksaround all the connections from the main valve to the inletvalve (6, Fig. 1), including the regulator.10.8.2 If leaks are not present, open the inlet valve andcheck for leaks from the inlet valve to the sample containerinlet valve (8, Fig. 1).10.8.3 If leaks are not present, open the sample c
49、ontainerinlet valve and check for leaks around the sample containerinlet valve, especially at the moving stem of the valve and theconnections between sample container body and both samplecontainer valves.10.8.4 If leaks are not present, open the sample containeroutlet valve (10, Fig. 1) to leak check down to the outlet valve(12, Fig. 1).10.8.5 All the leaks found in this 10.8 must be eliminatedbefore proceeding.10.9 Close the main valve and open the outlet valve (12,Fig. 1) to vent hydrogen to atmosphere. After most of thehydrogen is released, close
