ASTM WK5847 - 2009 - Standard Practice for Sampling High Pressure Hydrogen and Related Fuel Cell Feed Gases - Draft

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Designation: X XXXX-XX

Work Item Number: 0

Date: 0

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This document is not an ASTM standard; it is under consideration within an ASTM technical committee but has not received all approvals required to become an ASTM standard. You agree notto reproduce or circulate or quote, in whole or in part, this document outside of ASTM Committee/Society activities, or submit it to any other organization or standards bodies (whether national,international, or other) except with the approval of the Chairman of the Committee having jurisdiction and the written authorization of the President of the Society. If you do not agree with these

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Committee D03 on GASEOUS FUELS

Chairman: R AUL DOMINGUEZ JR., South Coast Air Quality Mgmt, Laboratory, 21865 E Copley Dr, Diamond Bar,CA 91765, United States (909) 396-2225, Fax: (909) 396-2175, e-mail: [email protected]

Vice Chairman: THOMAS F D ANIELS, Agilent Technologies, 2850 Centerville Road, Wilmington, DE 19808, UnitedStates (303) 904-2134, Fax: (720) 981-5030, e-mail: [email protected]

Recording Secretary: JEFFREY J WERNER, DCG Partnership Ltd, 4170A S Main, Pearland, TX 77581

United States (281) 648-1894, Fax: (281) 648-1895, e-mail: [email protected]

Membership Secretary: SHAHID R AZZAK, Southern California Gas Company, 8730 E. Slauson Ave, Pico Rivera, CA

90660, United States (562) 806-4280, Fax: (562) 806-4888, e-mail: [email protected]

Staff Manager: BRYNN MURPHY, (610) 832-9640, Fax: (610) 832-9666, e-mail: [email protected]

THIS NEW STANDARD WAS LAST BALLOTED AS ITEM 1 ON THE

D03.14 (09-03) SUBCOMMITTEE BALLOT AND RECEIVED NO NEGATIVES

REVISION IS NOW SUBMITTED FOR MAIN BALLOT

October 30, 2009

ITEM 8 – WK5847

July 28, 2009

TO: The D03 Membership

FROM: John Mough

SUBJECT: WK5847 Standard Practice for Sampling of High Pressure Hydrogen and Related FuelCell Feed Gases

Following please find WK5847 “Standard Practice for Sampling of High Pressure Hydrogen and RelatedFuel Cell Feed Gases”. This item is submitted for ballot consideration and satisfies the needs ofstakeholders requiring the collection of high pressure and high purity hydrogen from fueling nozzles and

similar interfaces used in automotive vehicles and stationary appliances. The standard will be referenced

in SDO, national, state and regional hydrogen quality standards as the method of choice to draw arepresentative sample from a hydrogen station nozzle.

I thank you for your time.

mailto:[email protected]











http://www.astm.org/




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ITEM 8 – WK5847

Standard Practice for Sampling of High Pressure Hydrogen and Related Fuel

Cell Feed Gases1

This standard is issued under the fixed designation X XXXX; 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

1.1 This practice describes an apparatus and a procedure for the sampling of high

pressure Hydrogen and related fuel cell feed gases from fueling nozzles and similar

interfaces used in automotive vehicles and stationary appliances. Many of the principles

used in this practice can be applied to low pressure sampling applications as well.

1.2 This practice applies only to single phase gas mixtures that may vary in

composition. A representative sample cannot be obtained from a two-phase mixture.

1.3 This practice does not include the actual analysis of the acquired sample.

Applicable ASTM standards including but not limited to test methods are referenced in

Section 2 of this practice.

1.4 This practice is not intended for sampling particulate matter in high pressure

Hydrogen; see ASTM WK9688

1.5 The values stated in SI units are standard. The values stated in inch-pounds are for

information only.

1 This Practice/Guide is under the jurisdiction of ASTM Committee and is the direct responsibility of

Subcommittee .

This document is not an ASTM standard; it is under consideration within an ASTM technical committee but has not received all approvals required to become an ASTMstandard. You agree not to reproduce or circulate or quote, in whole or in part, this document outside of ASTM Committee/Society activities, or submit it to any otherorganization or standards bodies (whether national, international, or other) except with the approval of the Chairman of the Committee having jurisdiction and the writtenauthorization of the President of the Society. If you do not agree with these conditions please immediately destroy all copies of the document. Copyright ASTM International,100 Barr Harbor Drive, West Conshohocken, PA 19428. All Rights Reserved.



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1.6 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.

2. Referenced Documents

2.1 ASTM Standards

2.1.1 D1945 Standard Test Method for Analysis of Natural Gas by Gas Chromatography2

2.1.2 D1946 Standard Practice for Analysis of Reformed Gas by Gas Chromatography2

2.1.3 D4150 Standard Terminology Relating to Gaseous Fuels2

2.1.4 WK24073 Standard Test Method for Determination of Trace Hydrogen Sulfide,

Carbonyl Sulfide, Methyl Mercaptan, and Carbon Disulfide in Hydrogen Fuel by Gas

Chromatography and Sulfur Chemiluminescence Detection. 2,

3

2.1.5 D5287 Standard Practice for Automatic Sampling of Gaseous Fuels2

2.2 Other Documents of Interest

2.2.1 SAE J2600 Compressed Hydrogen Surface Vehicle Refueling Connection Devices

2.2.2 SAE J2719 Information Report of the Development of a Hydrogen Quality Guideline

for Fuel Cell Vehicles

2.2.3 California Code of Regulations, Title 4, Division 9, Chapter 6, Article 8, Sections 4180

– 4181

2.2.4 ISO 14687-2 Hydrogen Fuel- Product Specification- Part 2: Proton Exchange

Membrane (PEM) fuel cell applications for road vehicles.

2.2.5 ISO/TR 15916: 2004 Basic consideration for safety of hydrogen systems

2.2.6 ISO 26142 Hydrogen detection apparatus

Current edition approved XXX. XX, XXXX. Published XX XXXX.2 This Practice/Guide is under the jurisdiction of ASTM Committee and is the direct responsibility of

Subcommittee .



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2.2.7 IEC 60079-29-2: 2007 Selection, installation, use and maintenance of detectors for

flammable gases and oxygen

2.2.8 49 CFR 178 Subpart C- Specifications for Cylinders

2.2.9 CAN/CSA-B339 Cylinders, Spheres, and Tubes for the Transportation of Dangerous

Goods.

3 Terminology

3.2 Definitions

3.2.5 Absolute Pressure- Pressure measured with reference to absolute zero pressure,

usually expressed in MPa, mm Hg, or psia

3.2.6 Contaminant - impurity that adversely affects the components within the fuel cell

system or the hydrogen storage system

3.2.7 Gage Pressure – Pressure measured above ambient atmospheric pressure. Zero gauge

pressure is equal to ambient atmospheric (barometric) pressure (psig).

3.2.8 Gaseous Fuel – Material to be tested, as sampled, without change of composition by

drying or otherwise.

3.2.9 High Pressure Hydrogen – For the purposes of this practice, high pressure Hydrogen

is Hydrogen at 20MPa or higher.

3.2.10 Hydrogen Sampling Apparatus (HSA) – an apparatus used to interface with a

hydrogen delivery nozzle such as a vehicle fueling receptacle and deliver sample to a

collection vessel.

4 Summary of Practice

This practice describes an apparatus and procedure for the sampling of high pressure Hydrogen

and related fuel cell feed gases from fueling nozzles and similar interfaces used in fueling

automotive vehicles and stationary appliances. This practice is intended as a guideline for

ensuring collection of a representative sample without introducing trace levels of contaminants.

Current edition approved XXX. XX, XXXX. Published XX XXXX.



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Samples collected using this practice should be suitable for trace analysis of contaminants,

utilizing a variety of analytical techniques.

5 Significance and Use

5.2 Hydrogen may be delivered to fuel cell powered automotive vehicles and stationaryappliances at pressures up to 70 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, and fuel lines up to and

including the nozzle used for fuel delivery. Collection of a representative sample of fuel

without the introduction of contamination even as low as parts-per-billion (ppb)

concentration during collection is crucial for assessing the quality of fuel in real world

applications.

5.3 This practice is intended for application to high pressure, high purity Hydrogen; however,

the apparatus design and sampling techniques may be valid for other fuel cell supply

gases. Many of the techniques used in this practice could be applied to lower pressure /

lower purity gas streams.

6 Reagents

6.2 Hydrogen- Ultra High Purity (UHP - 99.999%) Hydrogen is required for blank tests

of the apparatus and sampling procedures.

6.3 Nitrogen - High quality Nitrogen may be used in apparatus and sample collection vessel

cleaning. Use of molecular sieves or other suitable agents to remove water, oxygen, and

hydrocarbons is recommended.

7 Procedure

The sampling apparatus must be designed to collect sufficient sample volumes to ensure that the

detection limits for the targeted species can be achieved. The sampling apparatus must be

designed to ensure collection of a sample volume sufficiently large that desired sensitivity is

achieved for analytic test methods employed in measuring trace impurities in the fuel cell feed

gas. A minimum 500 ml volume at 0 psig is suggested. The sampling apparatus design must



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allow for collection of a blank sample. Many designs for apparatus dedicated to collection of

high pressure hydrogen or other fuel cell feed gases are possible. Figure 1 depicts one design

that has been used to sample high pressure hydrogen. Critical features are described below:

Figure 1

7.1 The sampling apparatus shall be designed in accordance with Chapter 5 on the 2006 Edition

of NFPA 52 (55). The sample vessel shall be in compliance with DOT specifications outlined

in 49 CFR 178.

7.2 Safety is a critical factor in the design of an apparatus for sampling high pressure hydrogen

and related fuel cell feed gases from fueling nozzles and similar interfaces used in fueling

automotive vehicles and stationary appliances. For automotive applications, station/HSA

station interface connections must meet SAE Standard J2600 specifications. Figure 1

displays an apparatus that has been successfully employed in collection of high pressure

hydrogen from automotive fueling nozzles. Ideally, all apparatus components are



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constructed of materials inert to common contaminants in fuel cell feed gases including but

not limited to Sulfur compounds, Ammonia, Formaldehyde, Carbon Monoxide, and Water.

Following is a description of the critical components in its construction. Standard Operating

Procedures (SOP) for the equipment must be documented in accordance with Section 10.3

and reviewed regularly by the operator of the sampling apparatus.

7.3 The receptacle interface must be appropriate for the intended use. For example, automotive

fueling facility sampling application will require a SAE J2600 fitting.

7.4 Pressure regulator - A regulator capable of safely accepting hydrogen or other feed gas

at 125% of the maximum anticipated delivery pressure and be capable of delivering at a safe

pressure to the DOT approved sampling vessel.

7.5 Pressure relief valve - A pressure relief valve that will release pressure above 50% of

maximum pressure rating of the DOT approved sample vessel.

7.6 Pressure gauge - A pressure indicator or gauge will measure the pressure of the gas inside

the Hydrogen sampling vessel. The pressure gauge must be capable of measuring

between 0.5 MPa and 21 MPa. The pressure indicator should have an accuracy of 5 %

and resolution of 1%. The pressure indicator should be certified to ensure its accuracy

annually or more frequently as needed, and calibrated per manufacturer's specifications.

7.7 Shutoff valves - Valves must be capable of isolating the various sections of the sampling

apparatus without leakage.

7.8 Sample collection vessel - Vessels must be DOT approved and rated at the appropriate

sampling pressure to at least 12.6 MPa. A higher rated vessel is preferred.

7.9 Check valves - Check valves must be capable of gas release above 1 MPa (150 psig)

without back diffusion of air.

7.10 Vent Stack—A vent stack is required to allow hydrogen to flow safely away from the test

apparatus. A minimum 2.4 m (8’) vent stack is recommended.

8. Sampling Procedures



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Sampling procedures specifics will vary slightly due to sampling adaptor design differences.

General considerations for any sampling procedure are provided in this Section.

NOTE 1 1: It is critical for users of a hydrogen sampling adaptor to develop and maintain a

standard operating procedure for the apparatus. See Section 10.3 for SOP requirements.

9 Sampling Procedure The sample vessel(s) and collection apparatus shall be cleaned and tested

according to section 11.

9.1 Purge the HSA before sampling using ultra-high purity Hydrogen.

9.2 Leak check the HSA. Pressurize slowly and check all connections and valves with an

appropriate monitoring device to ensure that there are no detectable leaks. Acceptable leak

detection methods include but are not limited to an electronic leak detector. SNOOP and

other solvents are not acceptable methods to check for leaks. If a leak is detected, sampling is

terminated and the HSA must be repaired and leak checked again.

9.3 The sampling apparatus will be purged using UHP Hydrogen or other fuel cell feed gas a

minimum of 5 times when determination of impurities at single digit ppbv concentrations is

needed before sampling. Purging the apparatus a minimum of 3 times is suggested for other

applications. Purging will be conducted by pressurizing the sampling apparatus to 25% of

the DOT sample vessel rated pressure and discharging through the vent stack. Care must

be taken to ensure the system is not contaminated with air.

9.4 Hydrogen or other fuel cell feed gas blank sample collection

9.4.1 Purge the HSA and sample vessel with UHP hydrogen or other fuel cell feed gas in

accordance with section 9.1. A minimum of 10 vessel volumes must pass through the HSA.

9.4.2 A sample blank(s) is collected in a DOT approved sample vessel using Hydrogen (UHP) or

other fuel cell feed gas.

9.4.2.1 Mark the blank in accordance with DOT regulations specified in 49 CFR. Sample vessel

labels should be marked with the following information at a minimum: (1) Date, (2) Time, (3)

DOT Tank Identification Number, (4) Tank Pressure, (5) Location, (6) Customer/Owner/Site.

9.4.3 Hydrogen sample collection



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9.4.3.1 Purge the HSA and sample vessel with the fuel cell gas stream in accordance with section

9.1.2.1.

9.4.2.2 After purging the HSA and sample vessel, begin sample collection following the valve

operation sequence as specified in the HSA's SOP. The exact sequence will differ depending on

HSA design. A minimum of 10 vessel volumes should be purged prior to collection of the

analytical sample.

9.4 Mark the samples in accordance with DOT regulations specified in 49 CFR. Sample vessel

labels should be marked with the following information at a minimum: (1) Date, (2) Time,

(3) DOT Tank Identification Number, (4) Tank Pressure, (5) Location, (6)

Customer/Owner/Site.

9.5 Document transfer of the samples from sampler, to third party carrier or to lab through a chain

of custody.

9.6 Ship the sample in accordance with all appropriate regulations including but not limited to

those our lined in 49 CFR.

9.7.1 Shipping containers must use appropriate NFPA labels as specified in 49 CFR. Additional

requirements may be specified by third party carriers.

9.8 Decontaminate the HSA as specified in section 11.

9.9 Store and/or Ship the HSA carefully as to avoid damaging the apparatus. This is critical for

ensuring safe operation of the apparatus.

10. Record Keeping Procedures

10.1 A log containing the usage and history of the HSA and each sample vessel should be kept.

This historical record is valuable in tracking HSA and vessel performance. Vessels containing

samples with unusually high concentrations of fuel cell gas contaminants or that have been used

for purposes other than trace analysis of gas contaminants should be flagged for special cleaning

and subsequent blank analysis or removed from trace analysis service.



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10.2 Analytic reports should include the results from blank sample collection analyses as well as

results from high pressure fuel samples.

10.3 Sampling Apparatus Standard Operating Procedures (SOPs) - SOPs covering activity

associated with use of this standard should be maintained and document for the HSA and each

sample containment vessel the following activities: (1) assembly, calibration, leak check, and

operation of specific sampling systems and equipment used, (2) assembly, leak-check, (3)

sample apparatus storage and cleaning, (4) all aspects of relevant sample collection procedures

including valve operation sequence, (5) emergency shut down and sampling termination

procedures, and (6) preparation, storage, shipment, and handling of samples and/or sampling

apparatus.

11. Cleaning

Sample vessels used in application of this practice must be rigorously free of contaminants.

11.1 Sample Vessel Cleaning

11.1.1 All vessels must be cleaned before sample collection

11.1.2 All vessels are leak tested by pressurizing them to approximately 5 MPa (300 psig) with

UHP Hydrogen. The initial pressure is measured, the vessel valve is closed, and the final pressure

is checked after 24 hours. If leak tight, the pressure will not vary more than 0.5 MPa (30 psig)

over the 24 hours.

11.1.3 A vessel cleaning system may be used. Several manufacturers can supply this equipment.

If a vessel cleaning system is used, after leak checking, the vessels are evacuated to less than 0.5

Pa (0. 5 mm Hg) for at least one hour.

11.1.4 After cleaning, the vessel contents are analyzed according to the same procedure used

for samples. Any vessel that contains more than 0.2 ppbv of targeted substances cannot be used

without re-cleaning and re-analyzing. Any container failing 0.2 ppbv of a targeted substance must

be set aside for a more vigorous cleaning.



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11.1 .5 As a possible option to the vessel cleaning system, heat the vessels in an isothermal

oven to no greater than 100°C.

11.1.6 If a vessel cleaning system is not used, the vessels should be purged a minimum of 5 times

with UHP Hydrogen.

11.1.7 The vessel is now ready for use in sample collection. Attach an identification tag to each

vessel for field notes and chain-of-custody. Retain the vessel in this condition until used.

11.2 Hydrogen Sampling Apparatus (HSA) Cleaning

HSA contamination will impact hydrogen quality sampling results. HSA's must be properly

cleaned to ensure valid hydrogen quality results. Cleaning of low level contamination is

accomplished by a UHP hydrogen purge followed by a UHP hydrogen blank analysis. High level

or particulate contamination requires cleaning with a solvent such as pentane or hexane followed

by heating under vacuum over several hours. Adequate cleaning is verified by a UHP hydrogen

blank analysis. Procedural details are as follows.

Note 2: Do not clean the HQSA with iso-propanol or other low volatility solvent.

11.3 HSA Cleaning - Low contaminant regime < 10 ppmv per component

When contaminant concentration for substances up to CO or similarly volatile species are < 10

ppmv in a UHP hydrogen blank, the assembled HQSA is purged and pressurized with UHP

hydrogen at 4 MPa (600 psi). The pressure is rapidly released through the rear vent line. After

performing the purging and pressurization procedure five times, a lab blank using UHP

hydrogen must be collected and analyzed. Cleaning is confirmed when the concentration for

substances less the detection levels for target analytes.

11.4 HSA Cleaning High contaminant regime > 10 ppmv per component

When contaminant concentration exceeds 10 ppmv per component or when the HSA is

contaminated with oil or high boiling solvents including iso-propanol, the following cleaning

procedure is used.

11.4.1 The HSA exterior is cleaned using a Chem Wipe® or similar low dust hexane or pentane



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soaked material to remove any obvious external oil residue.

11.4.2 Disassemble the HSA and put HSA components in a clean beaker(s).

11.4.3 Ultrasonically clean all HSA components, except the high pressure regulator and check

valves, in reagent grade hexane for 5 minutes. Decant the solvent and replace it with a

new aliquot of reagent grade hexane. Repeat the ultrasonic cleaning procedure. After

this, the hexane is drained and the HSA components are air dried for 30 minutes in a

fume hood with the container of HSA parts covered with clean aluminum foil.

Note 3: In some instances, severe contamination will necessitate replacement of the regulator

and check valves.

11.4.4 Dry hexane cleaned HSA components at 100 °C for 2 hours in a laboratory type oven.

11.4.5 Reassemble the HSA.

11.4.6 If used, connected the J2600 hose assembly to a vacuum system and evacuate the HSA

and J2600 assembly to 0.3 mm Hg (0.006 psia) or better for at least 2 hours. All internal HSA

valves excepting the final exit valve are opened to ensure removal of residual solvent from the

internal surfaces of the HSA under reduced pressure.

11.4.7 The reassembled HSA is leaked check by pressurizing the assembly with UHP

hydrogen at 4 MPa (600 psig) followed by released of the pressure through the rearvent line. This procedure is repeated five times. After performing the purging and

pressurization procedure five times, a lab blank using UHP hydrogen must be collected

and analyzed. Cleaning is confirmed when the concentration for substances less the

detection levels for target analytes.

12. Keywords

12.1 sample containment; representative sampling; hydrogen quality; proton exchange

membrane; fuel cells, gaseous fuels



X XXXX The American Society for Testing Materials takes no position respecting the validity of any patentrights asserted in connection with any item mentioned in this standard. Users of this standard are

expressly advised that determination of the validity of any such patent rights, and the risk ofinfringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be

reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are

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{/FOOT;f1} Footnote 1 This test method is under the jurisdiction of ASTM Committee D-3 onGaseous Fuels and is the direct responsibility of Subcommittee D03.14 on Determination of SpecialConstituents of Gaseous Fuels.

Current edition approved Month day, 2009. Published Month year.

{/FOOT;f2} Footnote2 Annual Book of ASTM Standards, Vol 15.03.

{/FOOT;f4} Footnote3 Test method balloted Month day, 2009.