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ASTM D4084-07

(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)

SIGNIFICANCE AND USE
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 D 7166 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.
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-May-2007
ICS
75.160.30 - Gaseous fuels
Technical Committee
D03 - Gaseous Fuels
Current Stage
Ref Project

Relations

Replaces
ASTM D4084-06 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
Effective Date
01-Jun-2007
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-Jun-2007
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-Jun-2007
Referred By
ASTM D7800/D7800M-23 - Standard Test Method for Determination of Elemental Sulfur in Natural Gas
Effective Date
01-Jun-2007
Referred By
ASTM D4323-21 - Standard Test Method for Hydrogen Sulfide in the Atmosphere by Rate of Change of Reflectance
Effective Date
01-Jun-2007

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ASTM D4084-07 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)ASTM D4084-07 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
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ASTM D4084-07 - 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:D4084 −07
StandardTest Method for
Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead
1
Acetate Reaction Rate Method)
This standard is issued under the fixed designation D4084; 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 3. Summary of Test Method
1.1 This test method covers the determination of hydrogen
3.1 Measurement of H S is accomplished by ratiometrically
2
sulfide (H S) in gaseous fuels. It is applicable to the measure-
comparing a reading of an unknown sample with that of a
2
ment of H S in natural gas, liquefied petroleum gas (LPG),
known standard using a differential colorimetric detection.
2
substitute natural gas, landfill gas, sewage treatment off gasses,
Pure H S is used as a primary standard and mixed volumetri-
2
recycle gas, flare gasses, and mixtures of fuel gases. This
cally with a sulfur free matrix gas that is ideally similar in
method can also be used to measure the hydrogen sulfide
composition to the sample gas. A gaseous sample at constant
concentration in carbon dioxide. Air does not interfere. The
flow is humidified and passed over lead-acetate-impregnated
applicable range is 0.1 to 16 parts per million by volume
paper.H Sreactswithleadacetatetoformabrownstainonthe
2
3
(ppm/v)(approximately0.1to22mg/m )andmaybeextended
paper. The rate of reaction and resulting rate of color change is
to 100 % H S by manual or automatic volumetric dilution.
proportional to the concentration of H S in the sample. The
2
2
analyzer is comprised of an optical system, a photon detection
1.2 This standard does not purport to address all of the
system, a signal differentiation system of first order, and a
safety concerns, if any, associated with its use. It is the
signal output system. When there is no change in the color of
responsibility of the user of this standard to establish appro-
the tape, and no resulting change in photodetector output, E,
priate safety and health practices and determine the applica-
the first derivative, dE/dt, is zero. This results in an analyzer
bility of regulatory limitations prior to use.
that automatically zeroes when there is no H S.
2
2. Referenced Documents
2
4. Significance and Use
2.1 ASTM Standards:
D1193 Specification for Reagent Water
4.1 This test method is useful in determining the concentra-
D1914 PracticeforConversionUnitsandFactorsRelatingto
tion of hydrogen sulfide in gaseous samples and in verifying
Sampling and Analysis of Atmospheres
compliance with operational needs and/or environmental limi-
D2420 Test Method for Hydrogen Sulfide in Liquefied
tations for H S content. The automated performance operation
2
Petroleum (LP) Gases (Lead Acetate Method)
of this method allows unattended measurement of H S con-
2
D3609 Practice for Calibration Techniques Using Perme-
centration. The user is referred to Practice D7166 for unat-
ation Tubes
tended on-line use of instrumentation based upon the lead
D7166 Practice for Total SulfurAnalyzer Based On-line/At-
acetate reaction rate method.
line for Sulfur Content of Gaseous Fuels
E2165 Practice for Establishing an Uncertainty Budget for
5. Apparatus
the Chemical Analysis of Metals, Ores, and Related
3
5.1 Volumetric Measuring Devices—A graduated 10-L cyl-
Materials (Withdrawn 2007)
inder (see Fig. 1) having a movable piston for volumetrically
measuring test gas. Gastight syringes of 0.1 and 0.5-mL
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD03onGaseous
volume for volumetrically measuring 100 % H S. Gas tight
2
Fuels and is the direct responsibility of Subcommittee D03.05 on Determination of
syringes of other volumes can be used. These graduated
Special Constituents of Gaseous Fuels.
devices are not needed when the permeation tube method of
Current edition approved June 1, 2007. Published June 2007. Originally
approved in 1981. Last previous edition approved in 2006 as D4084 – 06. DOI: dynamic mixing is used to prepare the reference sample since
10.1520/D4084-07.
this method will generate a reference mixture.
2
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
5.2 Sample Pump—Apump capable of providing more than
Standards volume information, refer to the standard’s Document Summary page on 3
8 mL/s (approximately 1 ft /h) or less than 1 mL/s at 70 kPa
the ASTM website.
3
(approximately 10.15 psig). Gas-wetted parts are ideally con-
The last approved version of this historical standard is referenced on
www.astm.org. structed from either aluminum or polytetrafluorethylene
Copyright © ASTM International,
...

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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.
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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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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.  
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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.
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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.  
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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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