ASTM D5594-1998(2004) Standard Test Method for Determination of the Vinyl Acetate Content of Ethylene-Vinyl Acetate (EVA) Copolymers by Fourier Transform Infrared Spectroscopy (FT-.pdf

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1、Designation: D 5594 98 (Reapproved 2004)Standard Test Method forDetermination of the Vinyl Acetate Content of Ethylene-VinylAcetate (EVA) Copolymers by Fourier Transform InfraredSpectroscopy (FT-IR)1This standard is issued under the fixed designation D 5594; the number immediately following the desi

2、gnation 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. Scope*1.1 This test method covers infr

3、ared procedures for deter-mining the vinyl acetate content of EVA copolymers usingpressed films (Procedure A) or molded plaques (Procedure B)and internal corrections for sample thickness.1.2 This test method is applicable to the analysis of EVAcopolymers containing 0.5 to 55 % vinyl acetate except a

4、sspecified in 1.3.1.3 Talc interferes with the 1020 cm1vinyl acetate band.Resins containing SCBfor iii=1 TIL3XSP=620XEP=560PAU.PRESS .THEN ENTER THICKNESS (MILS). PREES AGAINVF0VF1=YEPYSPVF1=VF1/VF0VFW=VF1 * SLOPE VALUEVF2=VF2 + Y-INTERCEPT VALUEPRN VF2VF3=VF2+VF2DSSNXT IIIVF3=VF3/3OMDTHE AVERAGE PE

5、RCENT VA IS.PRN VF3 ENDEVA Copolymers Containing 0.56 Vinyl AcetateCRT LVACR “% VINYL ACETATE RANGE: 06 %”cr “CLEAN BEAM TO TAKE BACKGROUND”PAUSCBFOR IIICR “INSERT SAMPLE”PAUSCS RAS ABS DSSSXP=2100 XEP=1910ASS VF0=YEPYSPXSP=1040 XEP=970ASS VF1=YEPYSPVF2=VF1/VF0VF3=VF2 * 0.3648VF3=VF3+0.048CR “PEAKHE

6、IGHT 1020/PEAK HEIGHT 2019”VF2=CR “PERCENT (%) VINYL ACETATE=”VF3=NXT IIIENDFIG. A1.1 Macros for Calculating Vinyl Acetate Content of EVA Copolymers from FT-IR Spectra Using Molded PlaquesD 5594 98 (2004)5A2. SUMMARY OF PYROLYSIS TITRATION AND SAPONIFICATION DATA FOR EVA COPOLYMER REFERENCEMATERIALS

7、SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue that mayimpact the use of this standard. (November 10, 1998)(1) Extended scope of vinyl acetate polymers covered to 55 %.(2) Added an option to use the 4250 cm1ethylene band forEVA r

8、esins containing 5 to 28 weight percent vinyl acetate.(3) Allowed plaque thickness to vary so long as the absorptionmaxima of the analytical bands does not exceed 1.5 absorbanceunits.(4) Modified plaque preparation procedure for high vinylacetate resins.(5) Eliminated the option to use peak height r

9、atios.(6) Eliminated the option to use the 1465 cm1ethylene band.(7) Revised calculation procedure to use nonlinear regressionanalysis for resins with vinyl acetate content $5%.(8) Eliminated references to specific manufacturers equip-ment and software.ASTM International takes no position respecting

10、 the validity of any patent rights 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 standar

11、d is subject to revision at any time 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

12、 Headquarters. Your comments will 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.Thi

13、s standard is copyrighted by ASTM 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),

14、 or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).TABLE A2.1 Summary of Pyrolysis Titration and Saponification Data for EVA Copolymer Reference MaterialsI II III IV V VI VII VIII IX XLab 1 x 0.68 1.11 2.80 4.15 4.78 5.84 9.34 14.54 18.46 27.62Pyrolysis S 0.038 0.018 0.045 0.115

15、 0.078 0.111 0.140 0.201 0.071 0.088(DuPont) CV 5.59 1.62 1.61 2.77 1.63 1.90 1.50 1.38 0.38 0.32 + +0 Lab 2 x 0.61 0.87 2.72 4.07 4.70 5 9.33 14.86 18.90 28.05Pyrolysis s 0.003 0.022 0.014 0.022 0.042 0 0.024 0.073 0.468 0.060(Toyo Soda) CV 0.49 2.53 0.51 0.54 0.89 1 0.26 0.49 0.25 0.21 + Lab 3 x 0

16、.71 0.97 2.77 4.10 4.73 5.81 9.33 14.91 18.78 28.18Pyrolysis s 0.030 0.133 0.053 0.080 0.127 0.040 0.074 0.233 0.100 0.269(DuPont) CV 4.22 13.71 1.91 1.95 2.68 0.69 0.79 1.56 0.53 0.95+ + 0 +Lab 4 x 0.80 1.02 2.82 4.19 4.81 5.92 9.46 14.98 19.00 28.27Saponification S 0.042 0.046 0.052 0.059 0.049 0.067 0.059 0.061 0.072 0.089CV 5.25 4.51 1.84 1.41 1.02 1.13 0.62 0.41 0.38 0.31+ + + + + +x 0.70 0.99 2.78 4.13 4.76 5.84 9.36 14.82 18.78 28.03sx0.079 0.100 0.043 0.053 0.049 0.052 0.064 0.195 0.235 0.288CVx11.29 10.10 1.55 1.28 1.03 0.89 0.68 1.32 1.25 1.03D 5594 98 (2004)6