ASTM_D_5504_-_12.pdf

Designation:D550412Standard Test Method forDetermination of Sulfur Compounds in Natural Gas andGaseous Fuels by Gas Chromatography andChemiluminescence1This standard is issued under the fixed designation D5504;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method is primarily for the determination ofspeciated volatile sulfur-containing compounds in high meth-ane content gaseous fuels such as natural gas.It has beensuccessfully applied to other types of gaseous samples includ-ing air,digester,landfill,and refinery fuel gas.The detectionrange for sulfur compounds,reported as picograms sulfur,isten(10)to one million(1 000 000).This is equivalent to 0.01to 1 000 mg/m3,based upon the analysis of a 1 cc sample.1.2 The range of this test method may be extended to higherconcentration by dilution or by selection of a smaller sampleloop.NOTE1 Dilution will reduce method precision.1.3 This test method does not purport to identify all sulfurspecies in a sample.Only compounds that are eluted throughthe selected column under the chromatographic conditionschosen are determined.The detector response to sulfur isequimolar for all sulfur compounds within the scope(1.1)ofthis test method.Thus,unidentified compounds are determinedwith equal precision to that of identified substances.Totalsulfur content is determined from the total of individuallyquantified components.1.4 The values stated in SI units are standard.The valuesstated in inch-pound units are for information only.1.5 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1072 Test Method for Total Sulfur in Fuel Gases byCombustion and Barium Chloride TitrationD1945 Test Method for Analysis of Natural Gas by GasChromatographyD3609 Practice for Calibration Techniques Using Perme-ation TubesD4468 Test Method for Total Sulfur in Gaseous Fuels byHydrogenolysis and Rateometric ColorimetryE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Summary of Test Method3.1 The analysis of gaseous sulfur compounds is challeng-ing due to the reactivity of these substances.They are difficultto sample and analyze.Ideally,analysis is performed on-site toeliminate sample deterioration as a factor in analysis.Samplingmust be performed using non-reactive containers,such asSilcosteel3lined vessels,Tedlar4bags with polypropylenefittings or the equivalent.Tedlar4bag samples require protec-tion from light and heat.Laboratory equipment must be inert orpassivated to ensure reliable results.3.2 A one cc(mL)sample is injected into a gas chromato-graph where it is eluted through a megabore,thick film,methylsilicone liquid phase,open tubular partitioning column or othersuitable column,and separated into its individual constituents.1This test method is under the jurisdiction ofASTM Committee D03 on GaseousFuels and is the direct responsibility of Subcommittee D03.05 on Determination ofSpecial Constituents of Gaseous Fuels.Current edition approved June 1,2012.Published November 2012.Originallyapproved in 1994.Last previous edition approved in 2008 as D5504 08.DOI:10.1520/D5504-12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Silcosteel is a trademark of Restek Corporation,110 Benner Circle Bellefonte,PA,16823.4Tedlar is a trademark of DuPont.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.3 Sulfur Chemiluminescence DetectionAs sulfur com-pounds elute from the gas chromatographic column,they areprocessed in a flame ionization detector(FID)or a heatedcombustion zone.The products are collected and transferred toa sulfur chemiluminescence detector(SCD).This techniqueprovides a sensitive,selective,linear response to volatile sulfurcompounds and may be used while collecting hydrocarbon andfixed gas data from a FID.3.3.1 Detectors in Series with a SCDA SCD can fre-quently be used in series with other fixed gas and hydrocarbondetectors.However,regulatory bodies may question detectorcompatibility and require demonstration of equivalence be-tween a SCD in a multi-detector system and a SCD operatedusing a FID or combustion z