1、Designation: D 3594 93 (Reapproved 2006)Standard Test Method forCopolymerized Ethyl Acrylate In Ethylene-Ethyl AcrylateCopolymers1This standard is issued under the fixed designation D 3594; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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 test method covers ethylene-ethyl acrylate copoly-mers containing from 1 to 25 % ethyl acryla
3、te comonomer.1.2 The values stated in SI units are to be regarded asstandard. (See IEEE/ASTM SI-10.)1.3 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and heal
4、th practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1There is no similar or equivalent ISO standard.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1898 Practice for Sampling of Plastics3E 131 Terminology Relating to Molecular
5、SpectroscopyE 168 Practices for General Techniques of Infrared Quanti-tative AnalysisE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near-Infrared Spectrophotom-etersIEEE/ASTM SI-10 Standard
6、 for Use of the InternationalSystem of Units (SI): The Modern Metric System3. Terminology3.1 See Terminology D 883.4. Summary of Test Method4.1 The infrared absorption band at 11.60 m responds toincreases in comonomer content. There is no absorption at thiswavelength when there is no comonomer prese
7、nt. It apparentlyis unique and characteristic of the copolymer. There is nointerference from the monomer at this wavelength.4.2 The infrared absorption band at 11.60 m is of mediumintensity; consequently, fairly thick films are employed. This isan advantage in that errors in measurements of the thic
8、knessesof films have minimal influence on the analytical result. Filmthickness is selected so that not more than 80 % of the infraredenergy is absorbed at the analytical wavelength. The approxi-mate thicknesses found to be satisfactory for different concen-trations of comonomer are as follows: (1) l
9、ess than 5 weight %ethyl acrylate = 0.5 mm, ( 2) 5 to 15 weight % ethyl acry-late = 0.25 mm, and (3) 15 to 25 weight % ethyl acry-late = 0.18 mm. It is necessary first to press a film approxi-mately 0.25 mm in thickness and scan it to observe theabsorption intensity unless the approximate ethyl acry
10、latecontent is known.4.3 For the highest precision, the test method requires thatthe thickness of the sample film be determined accurately.4.4 The general procedure is to scan the absorption bandfrom 10.50 to 12.50 m, although a single-point measurementmay also be used. This test method describes th
11、e use of a scanand employs the base-line method as outlined in 7.2 and thefigure illustrating the Base-Line Method for Measuring Absor-bance of Practices E 168. A calibration curve is prepared byplotting absorbance per millimetre values versus weight per-cent ethyl acrylate for several copolymers wh
12、ich have hadethyl acrylate contents established by a fast neutron activationanalysis of oxygen content. The ethyl acrylate content of anunknown sample is then obtained by referring the absorbanceper millimetre value to the calibration curve.5. Significance and Use5.1 Ethyl acrylate is copolymerized
13、with ethylene to pro-duce film, molding, and wire coating resins with improvedphysical properties. Ethyl acrylate comonomer increases flex-ibility, stress cracking resistance, toughness, and clarity. Arapid quantitative technique is needed for the evaluation of theamount of ethyl acrylate in a resin
14、 for specification purposesbecause physical properties change rapidly with increasingcomonomer content.1This test method is under the jurisdiction ofASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.08).Current edition approved
15、 Sept. 1, 2006. Published September 2006. Originallyapproved in 1977. Last previous edition approved in 2000 as D 3594 - 93(2000).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informat
16、ion, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Infrared spectrophotometric analysis, when suitablycalibrated, can be used for the measurement of the
17、 concentra-tion of comonomer present. Calibration is performed withsamples that have been analyzed for oxygen content by fastneutron activation analysis. Oxygen content is converted toethyl acrylate comonomer content by a simple calculation.5.3 A purpose of the infrared method of analysis is toprovi
18、de a procedure for use in quality control analysis. It is arapid, secondary method of analysis as contrasted with themore expensive and time-consuming fast neutron activationanalysis which is the primary, calibrating method.6. Apparatus6.1 Infrared Spectrophotometer,4capable of spectral resolu-tion4
19、equivalent to that defined by Practice E 275 and exhibitedin Fig. 7 of that practice. The instrument should be capable ofscale expansion along the wavelength (or wave number) axis.6.1.1 Fourier Transform Infrared Spectrophotometer (FT-IR), with nominal 4 cm1resolution.6.2 Compression-Molding Press,
20、small, with platens ca-pable of being heated to 150C.6.3 Metal Plates, two, 150 by 150 mm or larger, of 0.5-mmthickness with smooth surfaces, chromium plated preferably.6.4 Brass Shims, three, approximately 75 by 75 mm andthicknesses of 0.50 mm, 0.25 mm, and 0.18 mm, with anaperture in the center at
21、 least 25 by 38 mm.6.5 Micrometer Calipers, with thimble graduations of 0.001mm.6.6 Film Mounts, with apertures at least 6 by 27 mm to holdthe specimens in the spectrophotometer.7. Material7.1 Polyethylene Terephthalate or Aluminum Sheets, 80 by80-mm, or slightly larger, to cover brass shims.8. Haza
22、rds8.1 Use gloves when plaques are prepared using a heatedpress. Take care to avoid burns when handling microscopicslides with the hot plate.8.2 The optical bench of the FT-IR spectrophotometercontains a laser. To avoid eye injury, do not stare directly intothe laser beam.9. Sampling9.1 The copolyme
23、r shall be sampled in accordance withPractice D 1898.10. Calibration10.1 It is necessary to establish the ethyl acrylate comono-mer content of at least eight calibration samples by anindependent method. The samples should vary in ethyl acrylatecontent over the range from near zero to about 25 %.Amet
24、hodthat has been found to give high precision and accuracy foroxygen content is fast neutron activation analysis.5The ethylacrylate comonomer content, E, is calculated from the oxygenanalysis, assuming that all oxygen present is due to ethylacrylate, as follows:E, wt % 5100 3 X31.5(1)where:X = oxyge
25、n content of unknown copolymers, weight %.10.2 Set the controls of the infrared spectrometer for quan-titative conditions with a good signal-to-noise ratio and satis-factory reproducibility. Use a sufficiently expanded chart scalesuch that line width can be measured accurately. Use ascanning speed s
26、ufficiently slow to give good reproducibility ofband shape. Set the slit width narrow enough that there is littledistortion of the true band shape. Record the instrumentconditions used.NOTE 2For the Perkin-Elmer Model 221 Spectrophotometer thefollowing settings are satisfactory: Prism NaCl, slits 23
27、, slit program 927,attenuator speed 600, amplifier gain adjusted to give good response, chartscale 0.01 m/mm, chart speed 0.5 m/min, electrical balance andsuppression adjusted to specifications in instrument manual. Comparableoperating conditions should be used when other instruments are em-ployed.1
28、0.3 Scan the films from 10.50 to 12.50 m.NOTE 3Films having high gloss may exhibit interference fringes inthe infrared spectrum. These fringes make it difficult to establish a baseline. In such cases, the film should be abraded slightly to reduce the gloss.This can be performed by lightly rubbing wi
29、th a clean pencil eraser.10.4 Measure the baseline absorbance (see TerminologyE 131) of each film using a procedure similar to that shown inFig. 1 of this test method and outlined in 7.2 and the figureillustrating the Base-Line Method for Measuring Absorbanceof Practices E 168.10.5 Measure the thick
30、ness of the scanned portion of thefilms with the micrometer to the nearest 0.005 mm byaveraging at least five readings over the area.10.5.1 Care should be taken in making the micrometerreadings not to indent the surfaces of the film by over-tightening the micrometer. The films of high ethyl acrylate
31、 aresofter and more prone to indention.10.6 Calculate the absorbance per millimetre, A, as follows:A 5 Ab/t (2)where:Ab= baseline absorbance, andt = thickness, mm.10.7 Prepare a calibration graph similar to that shown inFig. 2 from the values of absorbance per millimetre and weightpercent ethyl acry
32、late comonomer.11. Procedure11.1 Sample Preparation:11.1.1 Preheat the press to 140 to 150C.4The Perkin-Elmer Model 221 Spectrophotometer, or equivalent, has been foundsatisfactory for this purpose.5Neutron activation analyses are available from Gulf Science and TechnologyCo., Product Evaluation Dep
33、t., P. O. Drawer 2038, Pittsburgh, PA15230, and UnionCarbide Corp., Nuclear Products and Services, P. O. Box 324, Tuxedo, NY 10987.D 3594 93 (2006)2NOTE 1Example illustrates baseline location, baseline wavelengths, and calculation absorbance per millimetre.NOTE 2The absorbance per millimetre value,
34、A, is applied to the calibration curve to obtain the concentration of ethyl acrylate comonomer.A 5log10T0/Itwhere:t = thickness, mm.FIG. 1 Typical Spectrophotometer Scan of Ethylene-Ethyl Acrylate CopolymerFIG. 2 Example of Typical Calibration Curve for Ethyl Acrylate Comonomer in Ethylene-Ethyl Acr
35、ylate Copolymer at 11.6 mD 3594 93 (2006)311.1.2 Place a brass shim on a polyethylene terephthalate orcleaned aluminum sheet, which in turn covers a metal plate.11.1.3 Add polymer in sufficient quantity to completely fillthe shim aperture during pressing.11.1.4 Cover with another sheet of polyethyle
36、ne terephtha-late or aluminum and another metal plate.11.1.5 Insert the mold assembly between the press platensand apply a slight pressure.11.1.6 Allow the sample to preheat for 30 s. Apply the fullpress pressure at 140 to 150C for 1 min or until all exudationceases.11.1.7 Turn off the heat, turn on
37、 the cooling water, and allowthe sample to press quench at full pressure until the tempera-ture drops below 50C (or cool enough to remove the moldassembly by hand).11.1.8 Release the pressure and remove the sample.11.1.9 Using the micrometer, measure the thickness of thesample to 6 0.01 mm at three
38、or more places within the samplebeam area. Calculate an average of the three measurements andrecord in millimetres.11.2 Spectral Measurements:11.2.1 Mount the films on the film mounts so that thethickness measured portion is centered in the infrared beam.11.2.2 Scan the samples slowly from 10.50 to
39、12.50 m.11.2.3 Draw a base line in the manner shown in Fig. 1.11.2.4 Measure the absorbance at maximum intensity.12. Calculation12.1 Calculate the absorbance per millimetre, A, as follows:A 5 log10Io/I!/t (3)where:t = thickness, mm.12.2 Refer the absorbance per millimetre of each sample tothe calibr
40、ation curve to find the value of weight percent ethylacrylate comonomer.13. Report13.1 Report the following information:13.1.1 Complete identification of the material tested includ-ing name, manufacturer, lot code number, and physical formwhen sampled,13.1.2 Date of test,13.1.3 Weight percent ethyl
41、acrylate comonomer,13.1.4 Any sample or spectral anomalies observed duringthe measurements, and13.1.5 Any deviation in procedure from this test method.14. Precision and Bias (See Practice E 177)614.1 The following values were determined for the coeffi-cient of variation of this test method, on the b
42、asis of aninterlaboratory test program involving five laboratories andthree materials and assuming duplicate analyses to report anaverage value. Based on these interlaboratory tests, the dataappear to be linear between 1 and 25 %:Interlaboratory Coefficient of Variation:1.70 % of mean valueInterlabo
43、ratory Coefficient of Variation:Sample A (19.2 % ethyl acrylate by neutron activationanalysis): 3.3 % of mean valueSamples B and C (6.8 % and 3.2 % ethyl acrylate byneutron activation analysis): 2.3 % of mean value14.2 Precision and Mean Bias (versus neutron activationanalysis):Sample A + 13.0 % of
44、reference value.Sample B + 8.8 % of reference value.Sample C + 3.1 % of reference value.15. Keywords15.1 ethyl acrylate; ethylene copolymer; infrared absorptionASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this stan
45、dard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be revie
46、wed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsibl
47、e technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con
48、shohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).6Supporting data are available from ASTM Headquarters. Request RR: D20-1063.D 3594 93 (2006)4
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