ASTM_D_4085_-_93_2013.pdf

Designation:D408593(Reapproved 2013)Standard Test Method forMetals in Cellulose by Atomic AbsorptionSpectrophotometry1This standard is issued under the fixed designation D4085;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 the determination of the iron,copper,manganese,and calcium content of cellulose pulp fromwood or cotton.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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:2D1193 Specification for Reagent WaterD1348 Test Methods for Moisture in CelluloseD3516 Test Methods for Ashing CelluloseE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Summary of Test Method3.1 The sample is ashed in accordance with Test MethodsD3516.3.2 This test method is dependent on the fact that metallicelements in the ground state will absorb light of the samewavelength they emit when excited.When radiation from agiven excited element is passed through a flame containingground-state atoms of that element,the intensity of the trans-mitted radiation will decrease in proportion to the amount ofthe ground-state element in the flame.A hollow cathode lampwhose cathode is made of the element to be determinedprovides the radiation.The metal atoms to be measured areplaced in the beam of radiation by aspirating the specimen intoan oxidant-fuel flame.A monochromator isolates the charac-teristic radiation from the hollow cathode lamp and a photo-sensitive device measures the attenuated transmitted radiation.4.Significance and Use4.1 Manganese in pulp acts as a catalyst in oxidizingcellulose.4.2 Iron in pulp can cause yellowness in rayon fibers andinfluence cellulose acetate plastics color.Iron also causesproblems in photographic and blueprint papers.4.3 Copper in pulp can act as a retardant in oxidizingcellulose and can affect viscose ripening.Copper interfereswith the dye level of rayon fibers and influences celluloseacetate plastics color.4.4 Calcium in pulps can cause problems in processing intoacetate,rayon,cellophane,etc.Calcium can create undesirabledeposits in viscose spinning and film casting operation.Cal-cium can influence viscosity control during cellulose acetatemanufacture.5.Apparatus5.1 Atomic Absorption Spectrophotometer,consisting of anatomizer and burner,suitable pressure-regulating devices ca-pable of maintaining constant oxidant and fuel pressure for theduration of the test,a hollow cathode lamp for each metal to betested,an optical system capable of isolating the desired line ofradiation,an adjustable slit,a photomultiplier tube or otherphotosensitive device,and a read-out mechanism for indicatingthe amount of absorbed radiation.5.2 OxidantAir,which has been cleaned and driedthrough a suitable filter to remove oil,water,and other foreignsubstances,is the usual oxidant.5.3 FuelAcetylene,commercially available,is the usualfuel.Acetone,always present in acetylene cylinders,can beprevented from entering and damaging the burner head byreplacing a cylinder that has a gage pressure of only 3.5 kPa(50 psi)remaining.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 June 1,2013.Published June 2013.Originallyapproved in 1981.Last previous edition approved in 2008 as D4085 93(2008).DOI:10.1520/D4085-93R13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.4 Volumetric Flasks,25,100,and 1000-mL.NOTE1In listing the apparatus for this method,the items required forthe ashing step are not listed.For these items refer to Test Methods D3516.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.6.2 Purity of WaterUnless otherwise indicated,reference