ASTM D7650-10
(Test Method)Standard Test Method for Test Method for Sampling of Particulate Matter in High Pressure Hydrogen used as a Gaseous Fuel with an In-Stream Filter
Standard Test Method for Test Method for Sampling of Particulate Matter in High Pressure Hydrogen used as a Gaseous Fuel with an In-Stream Filter
SIGNIFICANCE AND USE
Fuel cells such as proton exchange membrane fuel cells require high purity hydrogen for maximum material performance and lifetime. Collection and measurement of particulate matter 0.2 µm or larger is necessary for assuring a feed gas of sufficient purity to satisfy fuel cell system needs. In addition, internal combustion engines using high pressure hydrogen fuel also require low particulate containing fuel. Specifically, particulate matter has been implicated in the premature failure of pneumatic control components, such as valves within vehicles. This sampling procedure is used to collect and measure samples containing particles 0.2 µm or larger in size as specified in ISO/CD 14687–2, SAE J2719, and other hydrogen fuel quality specifications.
Although not intended for application to gases other than hydrogen and related fuel cell supply gases, the techniques within this sampling procedure can be applied to other high pressure gaseous samples requiring particulate collection and measurement.
SCOPE
1.1 This test method is primarily for sampling particulates in hydrogen fuel used in hydrogen fuel cell vehicles or gaseous hydrogen powered internal combustion vehicle engines up to pressures of 35 MPa (350 Bars) using an in-stream filter. This test method describes sampling apparatus design, operating procedures, and quality control procedures required to obtain the stated levels of precision and accuracy.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 The values stated in Bars in 1.1, 7.1 and 10.1.1 are for information only.
1.3 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7650 − 10
StandardTest Method for
Test Method for Sampling of Particulate Matter in High
Pressure Hydrogen used as a Gaseous Fuel with an In-
Stream Filter
This standard is issued under the fixed designation D7650; 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 2.3 ISO Standard:
ISO/CD14687–2 Hydrogenfuel—ProductSpecification—
1.1 This test method is primarily for sampling particulates
Part 2: Proton exchange membrane (PEM) fuel cell
in hydrogen fuel used in hydrogen fuel cell vehicles or gaseous
applications for road vehicles.
hydrogen powered internal combustion vehicle engines up to
pressures of 35 MPa (350 Bars) using an in-stream filter. This
3. Terminology
test method describes sampling apparatus design, operating
3.1 Acronyms:
procedures, and quality control procedures required to obtain
3.1.1 FCV—Hydrogen Fuel Cell Vehicle.
the stated levels of precision and accuracy.
3.1.2 HQSA—Hydrogen quality sampling assembly for
1.2 The values stated in SI units are to be regarded as
sampling gaseous hydrogen fuel.
standard. No other units of measurement are included in this
3.1.3 PEM—Polymer Electrolyte Membrane also called a
standard.
Proton Exchange Membrane
1.2.1 The values stated in Bars in 1.1, 7.1 and 10.1.1 are for
3.1.4 PSA—Particulate sampling adapter for sampling par-
information only.
ticulate in hydrogen fuel.
1.3 This standard does not purport to address all of the
3.1.5 SAE—Society of Automotive Engineering
safety concerns, if any, associated with its use. It is the
3.2 Definitions:
responsibility of the user of this standard to establish appro-
3.2.1 pinhole—a small hole generated during sampling of
priate safety and health practices and determine the applica-
particulate in hydrogen that can be identified by microscope.
bility of regulatory limitations prior to use.
3.3 SAE J2719—Informational Report on the development
of a hydrogen quality guideline for fuel cell vehicles. This
2. Referenced Documents
report specifies PEM FCV hydrogen fuel quality from the
2.1 ASTM Standards:
fueling nozzle.
D7651 Test Method for Gravimetric Measurement of Par-
3.4 SAE J2600 Compressed Hydrogen Surface Vehicle
ticulate Concentration of Hydrogen Fuel
Refueling Connection Devices.—This document specifies the
2.2 SAE Standards:
design requirements for nozzles and receptacles used in high
SAE J2719 Information Report on the development of a
pressure hydrogen applications such as delivery from a fueling
hydrogen quality guideline for fuel cell vehicles.
station to a FCV
SAE J2600 Compressed Hydrogen Surface Vehicle Refuel-
4. Summary of Test Method
ing Connection Devices
4.1 This test method provides a procedure for the sampling
ofparticulatemattercontainedinhydrogenusedasaFCVfuel.
1 It is designed to collect all particulates 0.2 µm or larger
ThistestmethodisunderthejurisdictionofASTMCommitteeD03onGaseous
Fuels and is the direct responsibility of Subcommittee D03.14 on Hydrogen and
contained in a known amount of hydrogen at a station
Fuel Cells.
dispenser nozzle in a way that simulates a FCV or a gaseous
Current edition approved July 1, 2010. Published August 2010.DOI: 10.1520/
hydrogen powered internal combustion vehicle engine fueling
D7650–10.
event. The adapter used for sampling particulates in hydrogen
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
fuel is called a Particulate Sampling Adapter (PSA) and is
Standards volume information, refer to the standard’s Document Summary page on
described in 7. Great care should be taken to avoid contami-
the ASTM website.
nation and exposure of the PSA, filters, and other equipment
Available from SAE International (SAE), 400 Commonwealth Dr.,Warrendale,
PA 15096-0001, http://www.sae.org. with particles sized 10 µm or larger prior to use.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7650 − 10
5. Significance and Use minimize the particulates generated from the surface of this
area by fast flow and high pressure hydrogen
5.1 Fuel cells such as proton exchange membrane fuel cells
7.1.1 High Pressure Filter Holder—The high pressure filter
require high purity hydrogen for maximum material perfor-
holder is a 47 mm, stainless steel housing with maximum inlet
mance and lifetime. Collection and measurement of particulate
pressure 70 Mpa and a polytetrafluoroethylene (PTFE) inner
matter 0.2 µm or larger is necessary for assuring a feed gas of
47mm diameter PTFE-O ring. The filter holder must be
sufficient purity to satisfy fuel cell system needs. In addition,
equivalent,similarorexceedperformancecharacteristicsofthe
internal combustion engines using high pressure hydrogen fuel
filter holder shown in Fig. 1.
also require low particulate containing fuel. Specifically, par-
7.1.2 Filter—A polytetrafluoroethylene (PTFE) filter that
ticulate matter has been implicated in the premature failure of
tolerates flow rates of up to 38 g per s without damage and
pneumatic control components, such as valves within vehicles.
collects particulates with a minimum size of 0.2 µm.
This sampling procedure is used to collect and measure
samples containing particles 0.2 µm or larger in size as NOTE 2—Hydrogen back flow must be avoided since the backflow of
hydrogen can cause pinhole formation or other damage to filters. The
specified in ISO/CD 14687–2, SAE J2719, and other hydrogen
design of the apparatus and sampling procedures must prevent fuel
fuel quality specifications.
backflow, such as implementing the use of a check valve as shown in Fig.
1, Item 6.
5.2 Although not intended for application to gases other
than hydrogen and related fuel cell supply gases, the tech-
7.1.3 PSA Support—The mechanical PSA support must be
niques within this sampling procedure can be applied to other designed to securely hold the PSA and a station nozzle. The
high pressure gaseous samples requiring particulate collection
nozzle should be held firmly and not move or shake during
and measurement. particulate sampling.
7.1.4 PSA Design variations—The design of the PSAdown-
4,5
6. Interferences stream of the stainless steel Swagelok fitting (union 7 in Fig.
1) will vary with the sampling procedure. The procedure
6.1 Dust and other environmental particulate matter will
variations include:
interfere with the accurate measurement of particulates con-
(1) Sampling while the hydrogen is venting to atmosphere,
tained in FCV quality hydrogen; therefore, every measure
(2) Sampling while fueling a vehicle.
should be taken to avoid contamination of the apparatus and all
Sampling when fueling into a vehicle tank collects a sample
equipment, supplies and gases used in these procedures.
more representative of the particulates seen by vehicles in
service since the flow rate is much higher when fueling into a
7. Apparatus Design
vehicle tank than when venting to atmosphere. The following
NOTE 1—The use of trade names in this section are not intended as an
sections describes the post Swagelok fitting designs in detail.
endorsement for use.
7.1.4.1 PSA design for venting to atmosphere—For applica-
7.1 ThePSAisdesignedforpressuresatleastupto6000psi
tion to systems requiring venting hydrogen through the PSAto
(420 Bar) with appropriate safety factors built in and is
atmosphere, a ventilation assembly containsa3m long SS
designedforaflowrateof38gpersecondofhydrogenwithout
braidedtubingconnectsItem7ofFig.1inoneendandanother
damage to the filter or leakage from the PSA. The PSA
to a dual 2.4 m long 1.27cm OD SS tubing vertical to the
possesses a receptacle as per SAE J2600 which is connected
ground. During sampling, the hydrogen fuel flows through
directly to the filter housing.Ahigh pressure needle valve with
PSA, then the ventilation assembly, before venting to air at 8ft
working pressure at 42 Mpa is attached downstream of the
above ground.
filter holder to stop the hydrogen flow when leak testing the
7.1.4.2 PSA design for flowing hydrogen to gaseous hydro-
PSA. Downstream of the needle valve, a check valve is
gen vehicle tank—The configuration is the same as 7.1.4.1,
attachedtopreventthebackflowofhydrogenduringsampling.
except the downstream of the PSA at the elbow of the PSA
In summary, the configuration of the PSA, as shown in Fig. 1,
(Item 7, Fig. 1) connects the inlet hose of a 2nd nozzle
is:
assembly. The 2nd SAE J2600 nozzle is then attached to the
ASAEJ2600compliantReceptacle→FilterHolderwithFilter
receptacle on a vehicle. While sampling, the hydrogen fuel
→Needle Valve→ Check Valve.
flows from station SAE J2600 nozzle (1st nozzle)→ PSA→
Fig. 1 illustrates a PSA design that has been successfully
inlet hose of a 2nd SAE J2600 nozzle assembly→ receptacle
usedtocollectparticulatesamplesfrom5075psi(350Bar)fuel
of FCV tank.
cell quality hydrogen. The PSA should be rated above the
8. Additional Equipment Needed
operating pressure, and all materials used must be rated for
high pressure hydrogen applications at a 1.5 times minimum
8.1 Glove box—A glove box is a sealed container that is
margin of safety at the maximum operating pressure. The
designed to assemble PSA without particulate contamination
recommended working pressure of the PSA and associated
from ambient air. Two gloves are built into the sides of the
materials is 42 Mpa. Contamination from polytetrafluoroeth-
glove box with entry arranged in such a way that the user can
ylene (PTFE) tape, lubrication or other sources must be
avoided and the apparatus must be cleaned prior to use using
appropriate cleaning techniques for high pressure hydrogen
Thementionoftradenamesinthistestmethoddoesnotconstituteendorsement
applications.The design of the PSAshould include minimizing
or recommendation. Other manufacturers of equipment or equipment models can be
the distance and surface area between the nozzle and filter to used.
D7650 − 10
Item Description
1 SAE J2600 hydrogen receptacle without filter
4 TH
2 Swagelok High pressure SS-6–SAEH-1–4 (Pressure rating 9,000 psi)
3 Millipore High Pressure 316 SS Filter Housing (47mm, 02.µm) P/N XX4504700
1 7
4 3–O Outlet ⁄4 in. FNPT-SAE ⁄16-20 union
5 High pressure needle valve
6 Check valve
3 1
7 SS Swagelok Tube fitting, female elbow, ⁄8 in. tube OD × ⁄4 MNPT, P/N SS-600–2–4
FIG. 1 PSA Components
place hands into the gloves to install the filter and assemble the 8.2 Moisture/Temperature Data Logger—A data logger is
filter holder inside the box. The glove box must be maintained placed inside the glove box to measure both moisture and
particulate free at all times. Any visual particulate material temperature continuously at pre-defined intervals such as once
must be removed prior to working with the PSA or filters. A every two to five minutes. Moisture in the glove box is kept
6,5
HEPA vacuum can be used to remove particles from the between 15 to 30% using reagent grade nitrogen.All tempera-
glove bag and other equipment. ture and moisture data are stored in a data logger, which are
HEPA is a trademark of the HEPA Corporation, 3071 East Coronado Street
Anaheim, CA 92806.
D7650 − 10
7,5
downloaded into a Microsoft Excel , or a similar program, 10.1.1 Hydrogen fuel pressure can approach 6000 psi (414
sheet after completion of measurements. Bar). All PSA components must be constructed from 316
stainless steel, or better, and rated for this application.
8.3 Mini-Clean Room—A small clean room with HEPA air
10.1.2 The total mass of hydrogen passing through the PSA
filtration must be used to store unused polytetrafluoroethylene
during a sampling event is approximately 2 kg. Smoking,
(PTFE) filters, filter holders, and sampled filters at moisture
camera flashes, or mobile phones usage are an ignition hazard
content less than 30%.
and are not allowed within 7.6 m from the both ventilation
8.4 Ultrasonic Cleaner—Either an ultrasonic bath or probe
tubing (7.1.4.1) and hydrogen fueling station itself. Additional
is used in lab to shake off particulates on parts of PSA into
safety precautions must be taken as necessary to prevent fire or
reagent grade water.
explosion.
8.5 Hydrogen Leak Detector—Ahydrogen leak detector is a
10.2 Static Charges—During particulate sampling, the ex-
required safety device needed to detect small hydrogen gas
tremely high speed of hydrogen flow may generate a static
leaks in particular when the PSA is pressurized prior to
charge on PSA components. The static charge is removed by
particulate collection. The diluted soap bubble should not be
grounding the PSA with a wire from hydrogen fueling station
used to detect hydrogen leak from PSA.
or other available grounding wire(s).
8.6 HEPA Filter Horizontal Flow Hood—A HEPA filter
10.3 Hydrogen Embrittlement—Highpressurehydrogencan
horizontal flow hood blows filtered air through a HEPA filter
cause embrittlement of contacting metal surfaces or may cause
horizontally, providing for an environment with minimal sus-
metal hydride formation on metal surfaces. This can lead to
pended particulates. The air velocity measured by an air flow
catastrophic PSA failure, hydrogen leaks or generation of
meter (8.8) within the hood should be over 100 ft/minute. If
pyrophoric particulates. The PSA and all equipment used
below this velocity, the air velocity meter should trigger an
according to this standard must be closely inspected for signs
alarm notifying the operator about a low air velocity.
of cracks, metal oxide dust from metal hydride oxidation or
8.7 Plastic tweezers—Used to manipulate filters without any other combination of signs of wear and damage.
contamination.
11. Sampling, Test Specimens, and Test Units
8.8 Air Flow Meter—A meter to measure the air velocity
11.1 Sampling—Samplingofparticulatematterinhighpres-
going through the HEPAFilter Horizontal Flow Hood. The air
flow meter can trigger alarm when the air flow rate is lower surehydrogenfuelisatthedeliverynozzlewithoutusingeither
a regulator or pressure reducing orifice to lower the pressure.
than 30 m/min.
The pressure usage range is generally from 14 Mpa to 42Mpa.
8.9 Clean Room Air Filter Fan—A fan that blows air
11.2 Test Specimens—Particulate matter 0.2 µm or larger.
through a HEPA filter to improve particulate removal effi-
ciency.
11.3 Test Units—µg/L or mg/kg.
8.10 HEPA Vacuum—A vacuum with a HEPA filter that is
used to remove dust from a glove box or general filters storage 12. Preparation of Apparatus
or wor
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