ASTM D7606-11
(Practice)Standard Practice for Sampling of High Pressure Hydrogen and Related Fuel Cell Feed Gases
Standard Practice for Sampling of High Pressure Hydrogen and Related Fuel Cell Feed Gases
SIGNIFICANCE AND USE
Hydrogen is delivered to fuel cell powered automotive vehicles and stationary appliances at pressures up to 87.5 MPa. The quality of hydrogen delivered is a significant factor in maximizing fuel cell efficiency and life span. Contamination can arise during the production of fuel cell feed gases, storage containers, station tubing and fuel lines up to the nozzle used for fuel delivery. Collection of a representative fuel sample without the introduction of contamination even as low as parts-per-billion (ppb) per contaminant during collection is crucial for assessing the quality of fuel in real world applications.
This practice is intended for application to high pressure, high purity hydrogen; however, the apparatus design and sampling techniques may be applicable to collection of other fuel cell supply gases. Many of the techniques used in this practice can be applied to lower pressure/lower purity gas streams.
SCOPE
1.1 This practice describes a hydrogen quality sampling apparatus (HQSA) and a procedure for the sampling of high pressure hydrogen at fueling nozzles of 35 or 70 Mega Pascal (MPa) fueling stations.
1.2 This practice does not include the analysis of the acquired sample. Applicable ASTM standards include but are not limited to test methods referenced in Section 2 of this practice.
1.3 This practice is not intended for sampling and measuring particulate matter in high pressure hydrogen. For procedures on sampling and measuring particulate matter see ASTM D7650 and D7651.
1.4 The values stated in SI units are standard. The values stated in inch-pounds are for information only.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
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Designation: D7606 − 11
Standard Practice for
Sampling of High Pressure Hydrogen and Related Fuel Cell
Feed Gases
This standard is issued under the fixed designation D7606; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope SAE J2799 70 MPa Compressed Hydrogen Surface Vehicle
Fuelling Connection Device and Optional Vehicle to
1.1 This practice describes a hydrogen quality sampling
Station Communications
apparatus (HQSA) and a procedure for the sampling of high
SAETIR J2719 Information Report of the Development of a
pressure hydrogen at fueling nozzles of 35 or 70 Mega Pascal
Hydrogen Quality Guideline for Fuel Cell Vehicles
(MPa) fueling stations.
2.3 California Code of Regulations:
1.2 This practice does not include the analysis of the
California Code of Regulations Title 4, Division 9, Chapter
acquired sample. Applicable ASTM standards include but are
6, Article 8, Sections 4180 – 4181
not limited to test methods referenced in Section 2 of this
3. Terminology
practice.
3.1 Definitions:
1.3 This practice is not intended for sampling and measur-
3.1.1 absolute pressure—Pressure measured with reference
ing particulate matter in high pressure hydrogen. For proce-
to absolute zero pressure, usually expressed in MPa, mm Hg,
dures on sampling and measuring particulate matter seeASTM
or pound per square inch (psi).
D7650 and D7651.
3.1.2 contaminant—impurity that adversely affects the com-
1.4 The values stated in SI units are standard. The values
ponents within fuel cell or hydrogen storage systems
stated in inch-pounds are for information only.
3.1.3 gauge pressure—Pressure measured above ambient
1.5 This standard does not purport to address all of the
atmospheric pressure. Zero gauge pressure is equal to ambient
safety concerns, if any, associated with its use. It is the
atmospheric (barometric) pressure.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1.4 gaseous fuel—Material to be tested, as sampled, with-
bility of regulatory limitations prior to use. out change of composition by drying or otherwise.
3.1.5 hydrogen quality sampling apparatus (HQSA)—an
2. Referenced Documents
apparatus used to collect hydrogen from a 35 or 70 MPa
2.1 ASTM Standards:
hydrogen fueling nozzle (SAE J2600 and SAE J2799) into a
D7650 Test Method for Sampling of Particulate Matter in
sample container.
High Pressure Hydrogen used as a Gaseous Fuel with an
3.2 Definitions of Terms Specific to This Standard:
In-Stream Filter
3.2.1 high pressure hydrogen—For the purposes of this
D7651 Test Method for Gravimetric Measurement of Par-
practice, high pressure hydrogen is hydrogen defined as hydro-
ticulate Concentration of Hydrogen Fuel
gen pressurized to 35 or 70MPa.
2.2 SAE Standards
SAE J2600 Compressed Hydrogen Surface Vehicle Refuel-
4. Summary of Practice
ing Connection Devices
4.1 This practice describes an apparatus and procedure for
the sampling of high pressure hydrogen from fueling nozzles
This practice is under the jurisdiction of ASTM Committee D03 on Gaseous
conforming to SAE J2600 or SAE J2799. This practice is
Fuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen and
intended as a guideline for ensuring collection of a represen-
Fuel Cells.
tative sample without introducing trace levels of contaminants.
Current edition approved March 1, 2011. Published April 2011. DOI: 10.1520/
Samples collected using this practice should be suitable for
D7606–11.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
trace analysis of contaminants, utilizing a variety of analytical
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
techniques.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Available from SAE International (SAE), 400 Commonwealth Dr.,Warrendale, Available from Office of Administrative Law, 300 Capitol Mall Suite 1250,
PA 15096-0001, http://www.sae.org. Sacramento, CA 95814–4339.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7606 − 11
5. Significance and Use 6.2 HQSA Metal Support Plate ( 1, Fig. 1)—The HQSA
metal support plate is utilized to mitigate damage during
5.1 Hydrogen is delivered to fuel cell powered automotive
transportation and support the apparatus. The HQSA is firmly
vehicles and stationary appliances at pressures up to 87.5 MPa.
fixed to a metal support plate by tube supports (2, Fig. 1.).
The quality of hydrogen delivered is a significant factor in
6.3 Movable Adjustable Platform—Before sampling, the
maximizing fuel cell efficiency and life span. Contamination
metal plate holding the HQSAis firmly clamped onto a height
can arise during the production of fuel cell feed gases, storage
adjustable and movable platform, such as a heavy duty cart
containers, station tubing and fuel lines up to the nozzle used
with a hydraulic adjustable horizontal platform and brakes on
for fuel delivery. Collection of a representative fuel sample
its wheels. The cart is moved to a position close to the fueling
without the introduction of contamination even as low as
station and the height of platform is adjusted so that the fueling
parts-per-billion (ppb) per contaminant during collection is
nozzle attaches easily to the receptacle of HQSA.The platform
crucial for assessing the quality of fuel in real world applica-
height is adjusted to provide a safe and comfortable work
tions.
space. The cart is then locked into place using the cart wheel
5.2 This practice is intended for application to high
brakes.
pressure, high purity hydrogen; however, the apparatus design
6.4 SAE J2799 Receptacle (3, Fig. 1) – This receptacle can
and sampling techniques may be applicable to collection of
other fuel cell supply gases. Many of the techniques used in adapt to both 35 and 70MPa hydrogen fueling nozzles. For
safety reason, the receptacle must be positioned vertically so
this practice can be applied to lower pressure/lower purity gas
streams. that the fueling nozzle attaches to the receptacle from the top.
Tosupporttheweightofthefuelingnozzle,thereceptaclemust
6. Apparatus Design
have an additional support (3.1, Fig. 1), which is fixed to the
metal support plate (1, Fig. 1).
6.1 The general design of the HQSA is shown in Fig. 1,
which is a depiction of the apparatus with the nozzle hydrogen 6.5 Main Valve (4, Fig. 1)—The functions of the main valve
pressure regulated to approximate 6.9 MPa (1000 psi) before are explained as follows:
sampling. The pressure of 6.9 MPa (1000 psi) is selected as an 6.5.1 Station and HQSA leak test—The station leak test is
example since it is, generally, the lowest pressure tolerated by performed before hydrogen fuel sampling to ensure there are
hydrogen station safety shutoff systems while still providing a
noleaksinthehydrogenfueldeliverysystem.Forsamplingthe
sample that analytical laboratories can safely handle routinely. station personnel must attach the fueling nozzle to the SAE
All HQSA parts, including the ventilation tubes, are made of
J2799 receptacle (3, Fig. 1) first while the main valve is closed.
316 grade stainless steel (SS). The station leak test procedure is then initiated. A hand held
FIG. 1 Hydrogen Quality Sampling Apparatus
D7606 − 11
hydrogen leak detector is used to check for leaks around all the 6.11 Check Valve—The check valve (16, Fig. 1) with 69
connections from nozzle to the main valve as in 10.7. There is KiloPascal(KPa)(10psi)crackpressureisinstalledatthevent
oftheHQSA(Fig.1)topreventairfrombackdiffusionintothe
residual high pressure hydrogen left in the station hose when
HQSA.
the station is not fueling. The residual high pressure hydrogen
can be used for checking the leakage in the complete HQSA
6.12 Ventilation Assembly (17, Fig. 1)—The ventilation
system, including the sample container, as shown in 10.8.
assembly contains a 3 meter (m) (10 ft) long SS braided tubing
6.5.2 Prevention of High Pressure Hydrogen Passing interfaced to a dual 2.4 m (8 ft) long 1.27 cm ( ⁄2 in.) Outside
through the Regulator—If the main valve (4, Fig. 1)isnot Diameter (OD) SS tubing which is kept vertical to the ground.
During sampling, the hydrogen fuel flows through HQSA, then
installed and station fueling starts, the diaphragm of the
regulator (5, Fig. 1) may fail due to rapid hydrogen pressur- the check valve (16, Fig. 1), through thea3m long SS braided
tubing (17.1, Fig. 1) and dual 2.4 m long 1.27 cm ( ⁄2 in.) OD
ization. In this case, pressure relief valve (PRV) 15, (Fig. 1)
SS tubing (17.2, Fig. 1), before venting to atmosphere at
will open to release hydrogen pressure above 10.3 MPa (1500
approximately 2.4 m (8 ft) above ground.
psi). The main valve (4, Fig. 1) when closed is designed to
contain high pressure hydrogen when the station sampling
7. Additional Equipment Needed
starts.The main valve is slowly turned to the open position and
7.1 Hydrogen Leak Detector—Ahydrogen leak detector is a
the high pressure hydrogen is regulated to 6.9 MPa (1000 psi).
required as a safety device needed to detect hydrogen gas leaks
6.6 Regulator 5 (Fig. 1) and all connections from the SAE
when the HQSA is pressurized. Leak detection using soap
J2799 Receptacle to Regulator—The regulator and all the
bubbles must not be used due to possible moisture contamina-
connections, including tubing, tubing fittings, adapter fittings
tion.
and unions from the SAE J2799 receptacle to the main valve
and main valve to regulator must have a pressure rating of 103
8. Hazards
Mpa (15,000 psi) or higher. The regulator should have two
8.1 High hydrogen pressure—The hydrogen pressure can be
gauges, 5.1 and 5.2 in Fig. 1, to monitor both inlet and outlet
as high as 87.5MPa and constitutes both an explosion and fire
pressures.
hazard.
6.7 Inlet and Outlet Valves (6 and 12, Fig. 1, respectively)—
8.2 The total mass of hydrogen passing through the HQSA
The valves should be easily opened and closed, such as ball
during a sampling event is approximately 1 kilogram (kg).
valves. The HQSA and sample container are cleaned by
Smoking, camera flashes, or mobile phone usage is unsafe
pressurizing and, releasing hydrogen from the HQSA and
within 7.6 m (25 ft) of either the ventilation tubing (6.12)or
sample container (10.11) using these valves. This cleaning
hydrogen fueling station itself. Additional safety precautions
procedure can be repeated many times (10.11) but must be
mustbetakenasnecessarytopreventfireorexplosion,orboth.
performedatleast10timestoensureavalidsampleundermost
8.3 Static Charges—During gaseous sampling, the ex-
sampling conditions.
tremely high-speed hydrogen flow rate may generate a static
charge on HQSAcomponents. The static charge is removed by
6.8 Sample Containers—The pressure rating of the sample
groundingtheHQSAwithawirefromhydrogenfuelingstation
containers is 12.4 MPa (1800 psi). The sample containers and
or other available grounding wire(s).
both inlet and outlet valves (8 and 10, Fig. 1, respectively) are
internally coated with silicon (Si) since sulfur gas analysis to
9. HQSA Cleaning
low ppb is required under SAE TIR J2719 and other hydrogen
9.1 Do not clean the HQSAwith water, iso-propanol or any
fuel quality specifications. To avoid air contamination during
other solvent.
sampling, both inlet and outlet valves of sample containers are
equipped with quick connects – one end of the container has a
9.2 The HQSA must be cleaned by purging during sam-
quick-connect stem and the other end a quick-connect body.
pling. This is done by flowing one kilogram hydrogen fuel
These two quick-connections (7 and 11, Fig. 1) and the inlet
through the HQSAafter the nozzle pressure is regulated to 6.9
and outlet valves provide a double seal on both ends of the
MPa (1000 psi). The hydrogen flow rate at 1000 psi is
sample container.
approximately 33.3 grams per second for a total sampling time
of around 30 s. At this flow rate, SAE TIR J2719 targeted
6.9 HQSA Pressure Release Valve (14, Fig. 1)—The valve is
constituents will be removed from within the HQSA and
always closed before and during sampling.After collection, the
sampling lines. This procedure is the best way to conveniently
pressure release valve is opened before removal of the pres-
dehydrate and remove residual sulfur gases from the HQSA,
surized and sealed sample container to release the hydrogen
sampling line, and sample container. Dehydration of the
pressure in the HQSA through a check valve (16, Fig. 1).
apparatus cannot be safely achieved at the station through
Hydrogen at 6.9 MPa (1000 psi) contained inside the HQSA
evacuation or heating, or both.
must be released before next sample container can be safely
connected to the inlet quick-connection (7, Fig. 1).
10. Sampling Procedures
6.10 Proportional Release Valve (PRV, 15, Fig. 1)—The 10.1 Safety Precaution—During gaseous sampling, person-
PRVissetat10.3MPa(1500psi)toprotectthe12.4MPa(1800
nel must wear goggles, safety shoes and a flame resistant lab
psi) pressure proof sample container. coat or other industrial flame resistant clothing. Personnel not
D7606 − 11
directly involved in sampling should beat least 5 m away from sample container outlet valve and record the ending sampling
the HQSA during sampling. time once 1 kg of hydrogen has flowed through the HQSAand
sample container. The regulated hydrogen pressure should be
10.2 Attach a ground wire to the station ground.
back to 1000 psi. Close the sample container inlet valve. In
10.3 Fix the HQSA onto a platform of a hydraulic cart
general, the station fueling process will be shut down when
(6.3).
closing the sample container outlet valve. If not, shut down the
station fueling process.
10.4 Connect HQSA to the ventilation system (6.12).
10.5 Attach a 1-L 1800 psi stainless steel sample container 10.12 If additional sampling is to be performed, do not
to HQSA through quick connections (7 and 11, Fig. 1).
remove the fueling nozzle. Instead, close the main valve. Open
the HQSA pressure release valve (14, Fig. 1) to release the
10.6 Make sure all the valves of HQSA (Fig. 1) are closed
pressure inside the HQSA to atmospheric pressure, excepting
and attach the station 35 or 70 MPa nozzle to the SAE J2799
the pressure remaining between the receptacle and main valve
receptacle (3, Fig. 1).
(3 to 4, Fig. 1). The check valve (16, F
...
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