1、Designation: D3594 93 (Reapproved 2013)Standard Test Method forCopolymerized Ethyl Acrylate In Ethylene-Ethyl AcrylateCopolymers1This standard is issued under the fixed designation D3594; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis
2、ion, 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 ethylene-ethyl acrylate copoly-mers containing from 1 to 25 % ethyl acrylate
3、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 health
4、practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1There is no known ISO equivalent to this standard.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1898 Practice for Sampling of Plastics (Withdrawn 1998)3E131 Terminology Relating
5、 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 SpectrophotometersIEEE/ASTM SI-10 Standard for U
6、se of the InternationalSystem of Units (SI): The Modern Metric System3. Terminology3.1 See Terminology D883.4. 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 present. It
7、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 thicknesses
8、of 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) less tha
9、n 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 acrylatecont
10、ent 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 the use of
11、 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 E168. A calibration curve is prepared byplotting absorbance per millimetre values versus weight per-cent ethyl acrylate for several copolymers which have
12、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 with ethy
13、lene to pro-duce film, molding, and wire coating resins with improvedphysical properties. Ethyl acrylate comonomer increasesflexibility, stress cracking resistance, toughness, and clarity. Arapid quantitative technique is needed for the evaluation of the1This test method is under the jurisdiction of
14、ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Meth-ods.70.08).Current edition approved April 1, 2013. Published April 2013. Originallyapproved in 1977. Last previous edition approved in 2006 as D3594 - 93(2006).DOI: 10.1520/D3594-93R13.2For refer
15、enced 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.3The last approved version of this historical standard is referenced on
16、www.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1amount of ethyl acrylate in a resin for specification purposesbecause physical properties change rapidly with increasingcomonomer content.5.2 Infrared spectrophotometric ana
17、lysis, when suitablycalibrated, can be used for the measurement of the 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 c
18、alculation.5.3 A purpose of the infrared method of analysis is toprovide 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. App
19、aratus6.1 Infrared Spectrophotometer,4capable of spectral resolu-tion4equivalent to that defined by Practice E275 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
20、(FT-IR), with nominal 4 cm1resolution.6.2 Compression-Molding Press, 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 andthickness
21、es of 0.50 mm, 0.25 mm, and 0.18 mm, with anaperture in the center at 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
22、 Sheets, 80 by80-mm, or slightly larger, to cover brass shims.8. Hazards8.1 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,
23、 do not stare directly intothe laser beam.9. Sampling9.1 The copolymer shall be sampled in accordance withPractice D1898.10. 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 et
24、hyl acrylatecontent over the range from near zero to about 25 %.Amethodthat 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
25、 to ethylacrylate, as follows:E, wt% 5100 3X31.5(1)where:X = oxygen 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
26、 that line width can be measured accurately. Use ascanning speed sufficiently 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 Spectrophoto
27、meter thefollowing settings are satisfactory: Prism NaCl, slits 2, 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
28、 conditions should be used when other instruments are em-ployed.10.3 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 slightl
29、y to reduce the gloss.This can be performed by lightly rubbing with a clean pencil eraser.10.4 Measure the baseline absorbance (see TerminologyE131) 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 f
30、or Measuring Absorbanceof Practices E168.10.5 Measure the thickness 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 o
31、ver-tightening the micrometer. The films of high ethyl acrylate 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 v
32、alues of absorbance per millimetre and weightpercent ethyl acrylate comonomer.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 Dept., P. O. Draw
33、er 2038, Pittsburgh, PA15230, and UnionCarbide Corp., Nuclear Products and Services, P. O. Box 324, Tuxedo, NY 10987.D3594 93 (2013)2NOTE 1Example illustrates baseline location, baseline wavelengths, and calculation absorbance per millimetre.NOTE 2The absorbance per millimetre value, A, is applied t
34、o 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 Acrylate Copolymer
35、 at 11.6 mD3594 93 (2013)311. Procedure11.1 Sample Preparation:11.1.1 Preheat the press to 140 to 150C.11.1.2 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
36、during pressing.11.1.4 Cover with another sheet of polyethylene 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 o
37、r until all exudationceases.11.1.7 Turn off the heat, turn on 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 micromet
38、er, measure the thickness of thesample to 6 0.01 mm at three 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 th
39、e infrared beam.11.2.2 Scan the samples slowly from 10.50 to 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 Re
40、fer the absorbance per millimetre of each sample tothe calibration 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 form
41、when sampled,13.1.2 Date of test,13.1.3 Weight percent ethyl 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 E177)614.1 The following values were determined for
42、 the coeffi-cient of variation of this test method, on the basis 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 %:Interlabor
43、atory Coefficient of Variation:1.70 % of mean valueInterlaboratory 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 Bi
44、as (versus neutron activationanalysis):Sample A + 13.0 % of 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 right
45、s asserted in connection with any item mentionedin this standard. 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 t
46、ime by the responsible technical committee and must be reviewed 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
47、 receive careful consideration at a meeting of theresponsible 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
48、 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).6Supporting data are available from ASTM Headquarters. Request RR:D20-1063.D3594 93 (2013)4
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