ASTM_D_3324_-_01.pdf

Designation:D 3324 01Standard Practice forCarbon BlackImproving Test Reproducibility Using ASTMReference Blacks1This standard is issued under the fixed designation D 3324;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice provides a statistical procedure for im-proving test reproducibility when a laboratory cannot physi-cally calibrate its apparatus to obtain the standard values of theASTM reference blacks,within the ranges given in theprecision statement of the test method concerned.1.2 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:D 1510 Test Method for Carbon BlackIodine AdsorptionNumber2D 2414 Test Method for Carbon BlackOil AbsorptionNumber2D 3037 Test Methods for Carbon BlackSurface Area byNitrogen Adsorption2D 3265 Test Method for Carbon BlackTint Strength2D 3493 Test Method for Carbon BlackOil AbsorptionNumber of Compressed Sample2D 3765 Test Method for Carbon BlackCTAB(Cetyltrim-ethylammonium Bromide)Surface Area2D 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black Industries2D 4820 Test Methods for Carbon BlackSurface Area byMultipoint B.E.T.Nitrogen Adsorption3D 5816 Test Methods for Carbon BlackExternal SurfaceArea by Multipoint Nitrogen Adsorption33.Terminology3.1 Definitions:3.1.1 ASTM reference blacks,na set of six blacks thatspan the useful range of the test method for which they arestandards.3.1.2 measured value,nan observed test result as opposedto a standard value.3.1.3 regression of standard values on measured values,nstatistical equation derived by the method of least-squares.3.1.4 standard value,nthe value assigned to a referenceblack by ASTM Committee D-24 on Carbon Black.Usuallythis value is calculated as the average test result of aninterlaboratory testing program.4.Procedure4.1 Physically calibrate the test apparatus using the instruc-tions in the test method or the manufacturers instructions.4.2 Test the ASTM reference blacks a sufficient number oftimes to establish firm measured values.4.3 Calculate the regression of the standard values on themeasured values.This relationship has usually been observedto be linear,although a curvilinear function might conceivablysometimes exist.4.4 Correct the values measured on all subsequent samplesby substituting each measured value into this equation andcalculating the corrected value.4.5 Alternatively,a nomograph or a table of numbers maybe used to find the correspondence between a measured valueand a calibrated value.4.6 Recheck this regression equation whenever replacementapparatus or a new lot of materials is put into use.Also,recheck it periodically to find changes due to wear or aging.4.7 Each laboratory is responsible for establishing andmaintaining the correlation between the ASTM referenceblacks and their measured values.5.ASTM D-24 Standard Reference Blacks45.1 The standard values with their limits of uncertainty5forthe SRB 4 series,and the repeatability precision(as defined in1This practice is under the jurisdiction of ASTM Committee D24 on CarbonBlackand is the direct responsibility of Subcommittee D24.61 on Carbon BlackSampling and Statistical Analysis.Current edition approved May,10,2001.Published July 2001.Originallypublished as D 3324 74.Last previous edition D 3324 99.2Annual Book of ASTM Standards,Vol 09.01.3Discontinued 2000;replaced by Test Method D 6556;see 1999 Annual Book ofASTM Standards,Vol 09.01.4Standard Reference Blacks SRB 4 and SRB 5,are available from TitanSpecialties,P.O.Box 2316,Pampa,TX 790662316.5The standard values and limits of uncertainty were determined in an interlab-oratory study completed in January 1989.“The limits of uncertainty”are shown toindicate ranges within which replicate interlaboratory testing has been able to fix theconcensus standard values;they are not to be confused with or interpreted as therepeatability precision shown for the respective test methods.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.Practice D 4483),to be expected for each test method are givenin Table 1.5.1.1 Precision data on the SRB 5 series,determined duringthe validation of the SRB 5 series,is given in Table 2.6.Keywords6.1 ASTM reference blacks;carbon black;carbon blackstandard values;carbon black test reproducibilityTABLE 1 Precision DataA,BTest PropertyASTMStandardPrecisionSingle TestResultStandard Reference BlacksRepeatabilityA-4 N326B-4 N330C-4 N121D-4 N762E-4 N660F-4 N683Srr