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ASTM D7166-05

(Practice)

Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels

Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels

SIGNIFICANCE AND USE
On-line, at-line, in-line and other near-real time monitoring systems that measure fuel gas characteristics such as the total sulfur content are prevalent in the natural gas and fuel gas industries. The installation and operation of particular systems vary on the specific objectives, contractual obligations, process type, regulatory requirements, and internal performance requirements needed by the user. This protocol is intended to provide guidelines for standardized start-up procedures, operating procedures, and quality assurance practices for on-line, at-line, in-line and other near-real time total sulfur monitoring systems.
SCOPE
1.1 This practice is for the determination of total sulfur from volatile sulfur-containing compounds in high methane or hydrogen content gaseous fuels using on-line/at-line instrumentation.
1.2 The values stated in SI units are standard. Values stated in other units 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

Status
Historical
Publication Date
14-Jun-2005
ICS
75.160.30 - Gaseous fuels
Technical Committee
D03 - Gaseous Fuels
Drafting Committee
D03.12 - On-Line/At-Line Analysis of Gaseous Fuels
Current Stage
Ref Project

Relations

Replaced By
ASTM D7166-10 - Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels
Effective Date
01-Jan-2010
Referred By
ASTM D7551-10(2015) - Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases and Natural Gas by Ultraviolet Fluorescence
Effective Date
15-Jun-2005
Referred By
ASTM D4084-23 - Standard Test Method for Analysis of Hydrogen Sulfide in Gaseous Fuels (Lead Acetate Reaction Rate Method)
Effective Date
15-Jun-2005
Referred By
ASTM D7493-22 - Standard Test Method for Online Measurement of Sulfur Compounds in Natural Gas and Gaseous Fuels by Gas Chromatograph and Electrochemical Detection
Effective Date
15-Jun-2005
Referred By
ASTM D7800/D7800M-23 - Standard Test Method for Determination of Elemental Sulfur in Natural Gas
Effective Date
15-Jun-2005

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ASTM D7166-05 - Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous FuelsASTM D7166-05 - Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels
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ASTM D7166-05 - Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels
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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:D7166–05
Standard Practice for
Total Sulfur Analyzer Based On-line/At-line for Sulfur
1
Content of Gaseous Fuels
This standard is issued under the fixed designation D7166; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D5503 PracticeforNaturalGasSample-HandlingandCon-
ditioning Systems for Pipeline Instrumentation
1.1 Thispracticeisforthedeterminationoftotalsulfurfrom
D5504 Test Method for Determination of Sulfur Com-
volatile sulfur-containing compounds in high methane or
pounds in Natural Gas and Gaseous Fuels by Gas Chro-
hydrogen content gaseous fuels using on-line/at-line instru-
matography and Chemiluminescence
mentation.
D6122 Practice for Validation of the Performance of Mul-
1.2 The values stated in SI units are standard. Values stated
tivariate Process Infrared Spectrophotometer Based Ana-
in other units are for information only.
lyzer Systems
1.3 This standard does not purport to address all of the
D6299 Practice for Applying Statistical Quality Assurance
safety concerns, if any, associated with its use. It is the
and Control Charting Techniques to Evaluate Analytical
responsibility of the user of this standard to establish appro-
Measurement System Performance
priate safety and health practices and determine the applica-
D6621 PracticeforPerformanceTestingofProcessAnalyz-
bility of regulatory limitations prior to use.
ers for Aromatic Hydrocarbon Materials
2. Referenced Documents D6667 Test Method for Determination of Total Volatile
2
Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum
2.1 ASTM Standards:
Gases by Ultraviolet Fluorescence
D1070 TestMethodsforRelativeDensityofGaseousFuels
D6920 Test Method for Total Sulfur in Naphthas, Distil-
D1072 Test Method for Total Sulfur in Fuel Gases by
lates, Reformulated Gasolines, Diesels, Biodiesels, and
Combustion and Barium Chloride Titration
Motor Fuels by Oxidative Combustion and Electrochemi-
D3246 Test Method for Sulfur in Petroleum Gas by Oxida-
cal Detection
tive Microcoulometry
D3609 Practice for Calibration Techniques Using Perme-
3. Terminology
ation Tubes
3.1 Definitions:
D3764 Practice for Validation of the Performance of Pro-
3.1.1 direct sampling—sampling where there is no direct
cess Stream Analyzer Systems
connection between the medium to be sampled and the
D4298 Guide for Intercomparing Permeation Tubes to Es-
analytical unit.
tablish Traceability
3.1.2 in-line instrument—instrumentwithanactiveelement
D4468 Test Method for Total Sulfur in Gaseous Fuels by
installed in a pipeline, which is used to measure pipeline
Hydrogenolysis and Rateometric Colorimetry
contents or conditions.
D5287 Practice for Automatic Sampling of Gaseous Fuels
3.1.3 on-line instrument—instrument that samples gas di-
D5453 Test Method for Determination of Total Sulfur in
rectly from a pipeline, but is installed externally.
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel
3.1.4 at-line instrument—instrumentation requiring opera-
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
tor interaction that samples gas directly from the pipeline.
3.1.5 continuous fuel monitor—instrument that samples gas
directly from the pipeline on a continuous or semi-continuous
1
This practice is under the jurisdiction of ASTM Committee D03 on Gaseous
basis.
Fuels and is the direct responsibility of Subcommittee D03.12 on On-Line/At-Line
3.1.6 total reduced sulfur (TRS)—concentration summation
Analysis of Gaseous Fuels.
ofallvolatilesulfurspecieswitha−2sulfuroxidationnumber,
Current edition approved June 15, 2005. Published June 2005. DOI: 10.1520/
D7166-05.
excluding sulfur dioxide, sulfones and other inorganic sulfur
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
compounds.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3.1.7 total sulfur—concentration summation of all volatile
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sulfur species in a sample.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D7166–05
3.1.8 volatile—molecular characteristic wherein the sulfur suitable inert, or passivated, materials to ensure constituents in
specieexistsinthegasphaseattheoperatingconditionsofthe the fuel stream do not degrade these components or alter the
process or pipeline. composition of the sampled gas.
6.2 Sample Probes/Sample Extraction—The location and
4. Summary of Practice
orientation of sampling components are cri
...

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ASTM D7800/D7800M-23(Test Method)
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SIGNIFICANCE AND USE
5.1 Elemental sulfur impacts the quality of pipeline natural gas and deposits on pipeline flanges, fittings and valves, thereby impacting their performance. Natural gas suppliers and distributers require a standardized test method for measuring elemental sulfur. Some government regulators are also interested in measuring elemental sulfur since it would provide a means for assessing the contribution of elemental sulfur in pipelines to the SOx emission inventory from burning of gaseous fuels. Use of this method in concert with sulfur gas laboratory test methods such as Test Methods D4084, D4468, D5504, and D6228 or on-line methods such as D7165 or D7166 can provide users with a comprehensive sulfur compound profile for natural gas or other gaseous fuels. Other applications may include elemental sulfur in particulate deposits such as diesel exhausts.
SCOPE
1.1 This test method is primarily for the determination of elemental sulfur in natural gas pipelines, but it may be applied to other gaseous fuel pipelines and applications provided the user has validated its suitability for use. The detection range for elemental sulfur, reported as sulfur, is 0.0018 mg/L to 30 mg/L. The results may also be reported in units of mg/kg or ppm.  
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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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ASTM D4468-23(Test Method)
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SIGNIFICANCE AND USE
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.
SCOPE
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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.
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ASTM D7166-23(Practice)
Standard Practice for Total Sulfur Analyzer Based On-line/At-line for Sulfur Content of Gaseous Fuels

SIGNIFICANCE AND USE
5.1 On-line, at-line, in-line and other near-real time monitoring systems that measure fuel gas characteristics such as the total sulfur content are prevalent in the natural gas and fuel gas industries. The installation and operation of particular systems vary on the specific objectives, contractual obligations, process type, regulatory requirements, and internal performance requirements needed by the user. This protocol is intended to provide guidelines for standardized start-up procedures, operating procedures, and quality assurance practices for on-line, at-line, in-line and other near-real time total sulfur monitoring systems.
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1.1 This practice is for the determination of total sulfur from gas phase sulfur-containing compounds in high methane or hydrogen content gaseous fuels using on-line/at-line instrumentation.  
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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.
SCOPE
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1.3 The calculation method within this practice is based on the MWM Method as defined in EN 16726, Annex A.2 The calculation method is an optimization algorithm that uses varying sequences of ternary and binary gas component tables generated from the composition of a gaseous fuel sample.3 Both the source code and a Microsoft Excel-based calculator are available for this method.  
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1.5 Units—The values stated in SI units are to be regarded as standard. Other units of measurement included in this standard are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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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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