ASTM_D_5547_-_95_2009.pdf

Designation:D554795(Reapproved 2009)Standard Test Method forClay and Zeolite in Powdered Laundry Detergents by AtomicAbsorption1This standard is issued under the fixed designation D5547;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 covers atomic absorption tests appli-cable to powdered laundry detergents containing clay andzeolite.21.2 The values stated in SI units are to be regarded as thestandard.1.3 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:3E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)43.Summary of Test Method3.1 The test sample is fused with lithium metaborate,dissolved in acid,its silicon and aluminum content measuredby atomic absorption,and the silicon/aluminum(Si/Al)ratiocalculated.The clay and zeolite content of the test sample iscalculated from the Si/Al ratio of the test sample and the Si/Alratio of the clay and zeolite expected in the test sample.4.Interferences4.1 Materials other than clay and zeolite that contain siliconor aluminum,or both,will interfere.5.Principle5.1 Clay and zeolite contain silicon and aluminum at differ-ent relative levels.5The silicon/aluminum ratio is then ameasure of the relative level of clay and zeolite in detergentpowders.That is,detergent powders with a Si/Al ratio match-ing clay or zeolite contain only clay or zeolite,respectively.Detergent powders with Si/Al ratio falling between the Si/Alratio of clay and zeolite contain both clay and zeolite.5.2 This test method is based on the linear relationshipbetween the relative composition(or ratio)of clay/zeolite indetergent powders and the Si/Al ratio of such detergents.5.3 A calibration equation is derivable,therefore,from justtwo experimental points:the Si/Al ratio of the zeolite standard(100 zeolite,0%clay)and the Si/Al ratio of the clay standard(0%zeolite,100%clay).6.Apparatus6.1 Suitable Atomic Absorption Spectrophotometers,fittedwith a nitrous oxide-acetylene burner and aluminum andsilicon hollow cathode source lamps.6.2 Nitrous Oxide and Acetylene Tanks,with suitable regu-lators.6.3 Muffle Furnace,capable of reaching 1000C.6.4 Analytical Balance.6.5 Fisher Burner or Equivalent.6.6 20-mL or Larger Platinum Crucibles.6.7 Platinum-tip Tongs.6.8 25-mL Buret.6.9 100-mL and 200-mL Polypropylene Volumetric Flasks.6.10 10-mL and 25-mL Graduated Cylinders.6.11 150-mL Plastic Beakers.6.12 Magnetic Stirrer and Magnetic Stirring Bars.6.13 Blender,such as Waring6or Osterizer7or an industriallab model,or a mortar and pestle,if a blender is not available.1This test method is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents and is the direct responsibility of Subcommittee D12.12 onAnalysis and Specifications of Soaps,Synthetics,Detergents and their Components.Current edition approved Oct.1,2009.Published March 2010.Originallyapproved in 1994.Last previous edition approved in 2003 as D5547 95(2003).DOI:10.1520/D5547-95R09.2Silicon and aluminum measurements are by atomic absorption in this testmethod.ICP can be used to make such measurements as well.3For 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.4The last approved version of this historical standard is referenced onwww.astm.org.5The Si/Al ratio is usually about 1 in zeolites and about 3 in clays.6Waring blenders are available commercially.7Osterizer blenders are widely available commercially.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Reagents7.1 Purity of ReagentsReagents grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,wheresuch specifications are available.8Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterUnless otherwise indicated,referenceto water shall be understood to mean distilled water or water ofequal purity.7.3 Aluminum Standard,1000 g Al/mL9or equivalent.7.4 Silicon Standard,1000 g Si/mL.97.5 Potassium Chloride,Baker-analyzed reagent or equiva-lent.7.6 Potassium Chlorid