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ASTM D4084-05

(Test Method)

Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)

Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)

SCOPE
1.1 This test method covers the determination of hydrogen sulfide (H2S) in gaseous fuels. It is applicable to the measurement of H2S in natural gas, liquefied petroleum gas (LPG), substitute natural gas, and mixtures of fuel gases. Air does not interfere. The applicable range is 0.1 to 16 parts per million by volume (ppm/v) (approximately 0.1 to 22 mg/m3) and may be extended to 100 % H2S by manual or automatic volumetric dilution.
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

Status
Historical
Publication Date
31-Jan-2005
ICS
75.160.30 - Gaseous fuels
Technical Committee
D03 - Gaseous Fuels
Current Stage
Ref Project

Relations

Replaces
ASTM D4084-94(1999) - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
Effective Date
01-Feb-2005
Replaced By
ASTM D4084-06 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
Effective Date
01-Dec-2006
Referred By
ASTM D7165-22 - Standard Practice for Gas Chromatograph Based On-line/At-line Analysis for Sulfur Content of Gaseous Fuels
Effective Date
01-Feb-2005
Referred By
ASTM D7800/D7800M-23 - Standard Test Method for Determination of Elemental Sulfur in Natural Gas
Effective Date
01-Feb-2005
Referred By
ASTM D4323-21 - Standard Test Method for Hydrogen Sulfide in the Atmosphere by Rate of Change of Reflectance
Effective Date
01-Feb-2005
Referred By
ASTM D6021-22 - Standard Test Method for Measurement of Total Hydrogen Sulfide in Residual Fuels by Multiple Headspace Extraction and Sulfur Specific Detection
Effective Date
01-Feb-2005

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ASTM D4084-05 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)ASTM D4084-05 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
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ASTM D4084-05 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 4084 – 05
Standard Test Method for
Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead
1
Acetate Reaction Rate Method)
This standard is issued under the fixed designation D 4084; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Pure H S is used as a primary standard and mixed volumetri-
2
callywithasulfurfreecarriergasthatisofthesametypeasthe
1.1 This test method covers the determination of hydrogen
gas to be analyzed. A gaseous sample at constant flow is
sulfide (H S) in gaseous fuels. It is applicable to the measure-
2
humidified and passed over lead-acetate-impregnated paper.
ment of H S in natural gas, liquefied petroleum gas (LPG),
2
H Sreactswithleadacetatetoformabrownstainonthepaper.
2
substitute natural gas, and mixtures of fuel gases.Air does not
The rate of reaction and resulting rate of color change is
interfere. The applicable range is 0.1 to 16 parts per million by
3
proportional to the concentration of H S in the sample. An
2
volume (ppm/v) (approximately 0.1 to 22 mg/m ) and may be
optical system, photodetectors, a means to obtain the first
extended to 100 % H S by manual or automatic volumetric
2
derivativeofthephotodetectorsignal,andameanstoobtainan
dilution.
output from the differentiation process comprises the analyzer.
1.2 This standard does not purport to address all of the
When there is no change in the color of the tape, and no
safety concerns, if any, associated with its use. It is the
resultingchangeinphotodetectoroutput, E,thefirstderivative,
responsibility of the user of this standard to establish appro-
dE/dt, is zero. This results in an analyzer that automatically
priate safety and health practices and determine the applica-
zeroes when there is no H S.
2
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents
2
4.1 This test method is useful in determining the concentra-
2.1 ASTM Standards:
tionofhydrogensulfideingaseoussamplestoverifythatlimits
D 1193 Specification for Reagent Water
setforH Sintheproductgasarecompliedwith.Theautomatic
2
D 1914 Practice for Conversion Units and Factors Relating
operation of this method allows unattended measurement of
to Sampling and Analysis of Atmospheres
H S concentration.
2
D 2420 Test Method for Hydrogen Sulfide in Liquefied
Petroleum (LP) Gases (Lead Acetate Method)
5. Apparatus
D 3609 Practice for Calibration Techniques Using Perme-
5.1 Volumetric Measuring Devices—a graduated 10-L cyl-
ation Tubes
inder (see Fig. 1) having a movable piston for volumetrically
D 5504 Test Method for Determination of Sulfur Com-
measuring test gas. Gastight syringes of 0.1- and 0.5-mL
pounds in Natural Gas and Gaseous Fuels by Gas Chro-
volume for volumetrically measuring 100 % H S. Gas tight
2
matography and Chemiluminescence
syringes of other volumes can be used. These graduated
3. Summary of Test Method devices are not needed if the permeation tube method of
dynamic mixing is used to prepare the reference sample as this
3.1 Measurement of H S is accomplished by ratiometrically
2
method may be used to generate reference mixture.
comparing a reading of an unknown sample with that of a
5.2 Sample Pump—a pump capable of providing more than
known standard sample using a colorimetric analysis method.
3
8 mL/s (approximately 1 ft /h) or less than 1 mL/s at 70 kPa
(approximately 10.15 psig). Gas-wetted parts are to be either
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD03onGaseous aluminum or polytetrafluorethylene (PTFE). Stainless steel is
Fuels and is the direct responsibility of Subcommittee D03.05 on Determination of
less preferable but may be used for the purpose of improving
Special Constituents of Gaseous Fuels.
safety if applicable.
Current edition approved Feb. 1, 2005. Published February 2005. Originally
5.3 Colorimetric Rate of Reaction Sensor—select a device
approved in 1981. Last previous editionapproved in 1999 as D 4084 – 94 (1999).
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
of sufficient sensitivity to measure a minimum rate of change
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
of color density corresponding to 0.1-ppm H S by volume in
2
Standards volume information, refer to the standard’s Document Summary page on
the sample gas. (See Fig. 2.)
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4084–05
be properly stored and used only within the stated validity
period. In the
...

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1.1 This terminology standard covers the compilation of terminology developed by Committee D03 on Gaseous Fuels. It does not include terms, definitions, abbreviations, acronyms, and symbols specific to only a single D03 standard in which they appear. These terms, definitions, abbreviations, acronyms, and symbols are used in:  
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5.1 This test method can be used to determine specification, or regulatory compliance to requirements, for total sulfur in gaseous fuels. In gas processing plants, sulfur can be a contaminant and must be removed before gas is introduced into gas pipelines. In petrochemical plants, sulfur is a poison for many catalysts and must be reduced to acceptable levels, usually in the range from 0.01 ppm/v to 1 ppm/v. This test method may also be used as a quality-control tool for sulfur determination in finished products, such as propane, butane, ethane, and ethylene.
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ASTM D4084-23(Test Method)
Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)

SIGNIFICANCE AND USE
5.1 This test method is useful in determining the concentration of hydrogen sulfide in gaseous samples and in verifying compliance with operational needs and/or environmental limitations for H2S content. The automated performance operation of this method allows unattended measurement of H2S concentration. The user is referred to Practice D7166 for unattended on-line use of instrumentation based upon the lead acetate reaction rate method.
SCOPE
1.1 This test method covers the determination of hydrogen sulfide (H2S) in gaseous fuels. It is applicable to the measurement of H2S in natural gas, liquefied petroleum gas (LPG), substitute natural gas, landfill gas, sewage treatment off gasses, recycle gas, flare gasses, and mixtures of fuel gases. This method can also be used to measure the hydrogen sulfide concentration in carbon dioxide. Air does not interfere. The applicable range is 0.1 to 16 parts per million by volume (ppm/v) (approximately 0.1 to 22 mg/m3) and may be extended to 100 % H2S by manual or automatic volumetric dilution.  
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ASTM D8487-23(Specification)
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1.1 This specification defines the minimum fuel quality requirements for gaseous fuels consisting primarily of methane blended with volume fraction of up to 10 % hydrogen (H2) when used as an internal combustion engine fuel.  
1.2 This specification defines the criteria for blending hydrogen with natural gas, biogas, or renewable natural gas (RNG) and then compressed into compressed natural gas (CNG) for use as a fuel for internal combustion engines in motor vehicles.  
1.3 The total volume fraction of hydrogen within the fuel shall consist of hydrogen contained in the natural gas, biogas, or renewable gas and any additional hydrogen blended into the fuel mixture.  
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1.5 This specification applies to the fuel as delivered into the on-board fuel tanks of a motor vehicle as a compressed gas.  
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1.7 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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ASTM D1072-23(Test Method)
Standard Test Method for Total Sulfur in Fuel Gases by Combustion and Barium Chloride Titration

ABSTRACT
This test method is for the determination of total sulfur in combustible fuel gases and is applicable to natural gases, manufactured gases, mixed gases, and other miscellaneous gaseous fuels. For the use of barium chloride titration following collection of sulfur dioxide by alternative procedures, ammonia, amines, substances producing water soluble cations, and fluorides will interfere with the titration. The apparatus includes the following: (1) burner, (2) chimneys, absorbers, and spray traps, (3) flow meter, (4) vacuum system, (5) air-purifying system, and (6) monometer. The schematic diagrams of the gas burner, combustion and absorption apparatus, suction system, and purified air system are provided. Reagent grade chemicals shall be used in all tests and include: (1) water, (2) denatured ethyl or isopropyl alcohol, (3) barium chloride, standard solution, (4) hydrochloric acid, (5) hydrogen peroxide, (6) iso-propanol, (7) potassium hydrogen phthalate, (8) phenolphthalein, (9) methyl orange indicator solution, (10) silver nitrate solution, (11) sodium carbonate solution, (12) sodium hydroxide solution, (13) sulfuric acid, (14) tetrahydroxyquinone indicator, and (15) thorin indicator. The procedure for the following are detailed: (1) calibration and standardization of sodium hydroxide, sulfuric acid, and barium chloride solutions, (2) preparation of apparatus, (3) sulfur determination, (4) analysis of absorbent, and (5) quality assurance. The formula of calculating the volume of gas in standard cubic feet burned during the determination and the concentration of sulfur from the results of titration are given.
SCOPE
1.1 This test method is for the determination of total sulfur in combustible fuel gases, when present in sulfur concentrations between approximately 25 and 700 mg/m3 (1 to 30 grains per 100 cubic feet). It is applicable to natural gases, manufactured gases, mixed gases, and other miscellaneous gaseous fuels.  
1.2 The values stated in inch-pound units are to be regarded as standard.  
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SIGNIFICANCE AND USE
5.1 The methane number (MN) is a measure of the resistance of the gaseous fuel to autoignition (knock) when used in an internal combustion engine. The relative merits of gaseous fuels from different sources and having different compositions can be compared readily on the basis of their methane numbers. Therefore, the calculated methane number (MNC) is used as a parameter for determining the suitability of a gaseous fuel for internal combustion engines in both mobile and stationary applications.
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Standard Test Method for Hydrogen Purity Analysis Using a Continuous Wave Cavity Ring-Down Spectroscopy Analyzer

SIGNIFICANCE AND USE
5.1 Proton exchange membranes (PEM) used in fuel cells are susceptible to contamination from a number of species that can be found in hydrogen. It is critical that these contaminants be measured and verified to be present at or below the amounts stated in SAE J2719 and ISO 14687 to ensure both fuel cell longevity and optimum efficiency. Contaminant concentrations as low as single-figure ppb(v) for some species can seriously compromise the life span and efficiency of PEM fuel cells. The presence of contaminants in fuel-cell-grade hydrogen can, in some cases, have a permanent adverse impact on fuel cell efficiency and usability. It is critical to monitor the concentration of key contaminants in hydrogen during the production phase through to delivery of the fuel to a fuel cell vehicle or other PEM fuel cell application. In ISO 14687, the upper limits for the contaminants are specified. Refer to SAE J2719 (see 2.3) for specific national and regional requirements. For hydrogen fuel that is transported and delivered as a cryogenic liquid, there is additional risk of introducing impurities during transport and delivery operations. For instance, moisture can build up over time in liquid transfer lines, critical control components, and long-term storage facilities, which can lead to ice buildup within the system and subsequent blockages that pose a safety risk or the introduction of contaminants into the gas stream upon evaporation of the liquid. Users are reminded to consult Practice D7265 for critical thermophysical properties such as the ortho/para hydrogen spin isomer inversion that can lead to additional hazards in liquid hydrogen usage.
SCOPE
1.1 This test method describes contaminant determination in fuel cell grade hydrogen as specified in relevant ASTM and ISO standards using cavity ring-down spectroscopy (CRDS). This standard test method is for the measurement of one or multiple contaminants including, but not limited to, water (H2O), oxygen (O2), methane (CH4), carbon dioxide (CO2), carbon monoxide (CO), ammonia (NH3), and formaldehyde (H2CO), henceforth referred to as “analyte.”  
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1.3 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM D7493-22(Test Method)
Standard Test Method for Online Measurement of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatograph and Electrochemical Detection

SIGNIFICANCE AND USE
5.1 Gaseous fuels, such as natural gas, petroleum gases and bio-gases, contain sulfur compounds that are naturally occurring or that are added as odorants for safety purposes. These sulfur compounds are odorous, toxic, corrosive to equipment, and can inhibit or destroy catalysts employed in gas processing and other end uses. Their accurate continuous measurement is important to gas processing, operation and use, and is frequently of regulatory interest.  
5.2 Small amounts (typically, total of 4 to 6 ppm(v)) of sulfur odorants are added to natural gas and other fuel gases for safety purposes. Some sulfur odorants are reactive and may be oxidized to form more stable sulfur compounds having higher odor thresholds which adversely impact the potential safety of the gas delivery systems and gas users. Gaseous fuels are analyzed for sulfur compounds and odorant levels to assist in pipeline integrity surveillance and to ensure appropriate odorant levels for public safety.  
5.3 This method offers an on-line method to continuously identify and quantify individual target sulfur species in gaseous fuel with automatic calibration and validation.
SCOPE
1.1 This test method is for on-line measurement of gas phase sulfur-containing compounds in gaseous fuels by gas chromatography (GC) and electrochemical (EC) detection. This test method is applicable to hydrogen sulfide, C1 to C4 mercaptans, sulfides, and tetrahydrothiophene (THT).  
1.1.1 Carbonyl sulfide (COS) is not measured according to this test method.  
1.1.2 The detection range for sulfur compounds is approximately from 0.1 to 100 ppm(v) (mL/m3) or 0.1 to 100 mg/m3 at 25 °C, 101.3 kPa. The detection range will vary depending on the sample injection volume, chromatographic peak separation, and the sensitivity of the specific EC detector.  
1.2 This test method describes a GC-EC method using capillary GC columns and a specific detector for natural gas and other gaseous fuels composed of mainly light (C4 and smaller) hydrocarbons. Alternative GC columns including packed columns, detector designs, and instrument parameters may be used, provided that chromatographic separation, quality control, and measurement objectives needed to comply with user or regulator needs, or both, are achieved.  
1.3 This test method does not intend to identify and measure all individual sulfur species and is mainly employed for monitoring naturally occurring reduced sulfur compounds commonly found in natural gas and fuel gases or employed as an odorant in these gases.  
1.4 This test method is typically employed in repetitive or continuous on-line monitoring of sulfur components in natural gas and fuel gases using a single sulfur calibration standard. Guidance for producing calibration curves specific to particular analytes or enhanced quality control procedures can be found in Test Methods D5504, D5623, D6228, D6968, ISO 19739, or GPA 2199.  
1.5 The test method can be used for measuring sulfur compounds listed in Table 1 in air or other gaseous matrices, provided that compounds that can interfere with the GC separation and electrochemical detection are not present.  
1.6 This test method is written as a companion to Practices D5287, D7165 and D7166.  
1.7 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Tec...

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