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ASTM_D_6248_-_98_2012e1.pdf

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1、Designation:D624898(Reapproved 2012)1Standard Test Method forVinyl and Trans Unsaturation in Polyethylene by InfraredSpectrophotometry1This standard is issued under the fixed designation D6248;the number immediately following the designation indicates the year oforiginal adoption or,in the case of r

2、evision,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.1NOTEReapproved with editorial changes in May 2012.1.Scope1.1 This test method covers most types of polyethylene,t

3、hose ethylene plastics consisting of ethylene and-olefincomonomers longer than propylene,and blends of the above inany ratio.1.2 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 i

4、s 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.Specific hazardsstatements are given in Section 8.NOTE1There is no known ISO equivalent for this standard.2.Referenced Docume

5、nts2.1 ASTM Standards:2D792 Test Methods for Density and Specific Gravity(Rela-tive Density)of Plastics by DisplacementD1505 Test Method for Density of Plastics by the Density-Gradient TechniqueD3124 Test Method for Vinylidene Unsaturation in Polyeth-ylene by Infrared SpectrophotometryE131 Terminolo

6、gy Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE275 Practice for Describing and Measuring Performance ofUltraviolet and Visible Spectrophotometers3.Terminology3.1 Ge

7、neralThe units,symbols,and abbreviations used inthis test method appear in Terminology E131.4.Summary of Test Method4.1 The band at 965 cm1is characteristic of the trans-vinylene substituted group.The band at 908 cm1is character-istic of the terminal vinyl group.4.2 These bands are not seriously ove

8、rlapped by interferinggroups from the polymer.The vinyl absorbance at 908 cm1isclose to the absorbance band from terminal methyl groups onchains longer than ethyl,at 895 cm1.This interference isminimal for most products.Inclusion of the bromination andspectral subtraction step from Test Method D3124

9、 has beenfound to improve the results for some very low densityproducts.4.3 Integrated absorbance is used in this test method.Integrated absorbance is found by integrating the spectrumover the absorbance band when the spectrum is plotted asabsorbance versus frequency,in cm1.Most spectral manipu-lati

10、on software contains algorithms for adequately determiningbaseline corrected integrated absorbencies.4.4 Calibration is performed using a solution of 1-octene fornormal vinyl groups,and trans-3-hexene for trans-vinylenegroups.5.Significance and Use5.1 There are three types of olefinic groups present

11、 insufficient concentrations to warrant consideration,one or moreof that can normally be found in any polyethylene.The threetypes are trans-vinylene,R-CH=CH-R,sometimes referred toastrans-internalunsaturation;vinylideneorpendentmethylene,RRC-CH2;and vinyl unsaturation,R-CH=CH2,also referred to as te

12、rminal unsaturation.5.2 The type and quantity of these groups can influence thechemical and physical properties of the resin.Informationconcerning their presence can also be used to characterize oridentify unknown resins or blends of resins.1This test method is under the jurisdiction of ASTM Committ

13、ee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved May 1,2012.Published July 2012.Originally approvedin 1998.Last previous edition approved in 2004 as D6248-98(2004).DOI:10.1520/D6248-98R12E01.2For referenced ASTM standards,visit

14、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 S

15、tates1 5.3 Additives can interfere with unsaturation measurements.The use is cautioned to determine which additives are presentand if there any absorbance bands caused by additive presencethat overlap or interfere with unsaturation absorbance bandsused in this test method in the range of 1050 to 850

16、 cm1.Ifoverlapping bands occur,the method is not applicable.5.4 Interference fringes resulting from smooth sample sur-faces can cause measurement errors.This test method requiresthe use of aluminum foil in the compression molding ofsamples to provide an adequately rough surface to minimizeinterference fringes.6.Apparatus6.1 Infrared Spectrophotometer,either double-beam,or aFourier transform(FTIR).6.1.1 Double-Beam Infrared Spectrophotometer,capable ofspectral resolution as defined in Condition C

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