ASTM_D_2929_-_89_2019e1.pdf

Designation:D292989(Reapproved 2019)1Standard Test Method forSulfur Content of Cellulosic Materials by X-RayFluorescence1This standard is issued under the fixed designation D2929;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.1NOTESection 6.3 primary standard name was updated in October 2019.1.Scope1.1 This test method covers determination of sulfur contentof cellulosic materials by X-ray fluorescence.1.2 Using appropriate standards,the range of the procedureis from approximately 10 ppm to 20%sulfur.1.3 This test method is proposed specifically as an alterna-tive to Test Methods D871,sections on Significance and Use,Apparatus,Reagents,Procedure and Calculation of HydroxylContent,and Test Methods D817,sections on Summary of TestMethod,Significance and Use,Apparatus,Reagents,andProcedure of Hydroxyl Content.As applied to cellulose estersit measures the combined sulfur and sulfur in the accompany-ing inorganic salts.1.4 To determine combined sulfur,the sample,whensoluble,must first be reprecipitated into dilute acid to removethe noncombined sulfur compounds.1.5 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.6 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For a specific hazard statement,see 7.2.1.1.7 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D817 Test Methods of Testing Cellulose Acetate Propionateand Cellulose Acetate ButyrateD871 Test Methods of Testing Cellulose Acetate3.Summary of Test Method3.1 The sulfur content of cellulose,cellulose modification,or cellulose derivative is determined by measuring the intensityof the secondary sulfur K X rays emitted on irradiation of thesample with primary X rays of higher energy from an X-raytube with a target of tungsten or chromium.The sulfur Kradiation is diffracted with a suitable analyzing crystal anddetected with a flow-proportional counter.The entire path ofthe secondary radiation is purged with hydrogen or helium,orevacuated to a pressure of 0.5 mm Hg or less.The intensity ofthe sulfur K rays,as established by a standard counting periodand corrected for background radiation,is then converted topercent sulfur from calibration data.34.Significance and Use4.1 This procedure provides a method for determiningsulfur content in cellulosic materials by nondestructive means.Sulfur may be in the form of sulfate esters that may contributeto thermal instability.Sulfur can also be present as salts thatcan cause haze in solutions.5.Apparatus5.1 Wiley Mill,equipped with 60-mesh screen.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved Oct.1,2019.Published October 2019.Originallyapproved in 1970.Last previous edition approved in 2011 as D2929 89(2011).DOI:10.1520/D2929-89R19E01.2For 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.3This test method is compiled from four techniques,by incorporating certainfeatures of each,as follows:“Sulfur in Cellulose Esters by X-ray EmissionSpectroscopy,”Eastman Kodak Co.;“Sulfur in Cellulose Acetate by X-rayFluorescence,”Tennessee Eastman Co.;“X-ray Fluorescence Analysis of ModifiedCottons”by Tripp,Piccolo,Mitcham and OConnor.Textile Research Journal,Vol34,1964,p.773,and FMC Corp.,American Viscose Div.information furnished byL.H.Phifer and W.B.Swann.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 5.2 Sample MoldChrome steel die of a size depending onthe sample holder to be used.5.3 Laboratory Press,capable of exerting at least 5000 psi.5.4 X-Ra