1、Designation: D 1203 94 (Reapproved 2003)Standard Test Methods forVolatile Loss From Plastics Using Activated CarbonMethods1This standard is issued under the fixed designation D 1203; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 These test methods cove
3、r the determination of volatileloss from a plastic material under defined conditions of timeand temperature, using activated carbon as the immersionmedium.1.2 Two test methods are covered as follows:1.2.1 Test Method A, Direct Contact with ActivatedCarbonIn this test method the plastic material is i
4、n directcontact with the carbon. This test method is particularly usefulin the rapid comparison of a large number of plastic specimens.1.2.2 Test Method B, Wire CageThis test method pre-scribes the use of a wire cage, which prevents direct contactbetween the plastic material and the carbon. By elimi
5、nating thedirect contact, the migration of the volatile components to thesurrounding carbon is minimized and loss by volatilization ismore specifically measured.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety concerns
6、, 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.NOTE 1This standard is similar in content (not technically equivalent)to ISO 176-1976(
7、E).2. Referenced Documents2.1 ASTM Standards:D 618 Practice for Conditioning Plastics for Testing2D 883 Terminology Relating to Plastics2D 1600 Terminology of Abbreviated Terms Relating toPlastics2E 197 Specification for Enclosures and Servicing Units forTests Above and Below Room Temperature3E 691
8、Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method42.2 Other Documents:ISO 176-1976 Determination of the Loss of Plasticizersfrom Plastics by the Activated Carbon Method53. Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nologies D 883 and
9、D 1600 unless otherwise indicated.4. Significance and Use4.1 The test methods are intended to be rapid empirical testswhich may be useful in the relative comparison of materialshaving the same nominal thickness.NOTE 2When the plastic material contains plasticizer, loss from theplastic is assumed to
10、be primarily plasticizer. The effect of moisture isconsidered to be negligible.4.2 Correlation with ultimate application for various plasticmaterials should be determined by the user. To obtain acceler-ated tests that more nearly approach actual service conditions,reference should be made to Specifi
11、cation E 197.5. Apparatus5.1 BalanceAn accurate analytical balance, equippedwith Class S weights or better.5.2 Oven or BathA thermostatically controlled oven orbath capable of maintaining the temperature to within 61C ofthe test temperature, which normally will be in the range from50 to 150C.5.3 Con
12、tainersMetal cans or wide-mouth screw-top jars,of cylindrical form, approximately 100 mm in diameter andapproximately12 L in capacity.5.4 MicrometerA micrometer capable of measuring to thenearest 0.0025 mm for measuring the thickness of the testspecimens.5.5 Metal Cages (for Test Method B)Wire cages
13、 con-structed from approximately 30-mesh bronze gauze, in cylin-drical form, having a diameter of 60 mm and a height of 6 mm,1These test methods are under the jurisdiction of ASTM Committee D20 onPlastics and are the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials (Section D20
14、.15.11 on Plasticizers).Current edition approved July 10, 2003. Published September 2003. Originallyapproved in 1952. Last previous edition approved in 1999 as D 1203 94(99)e1.2Annual Book of ASTM Standards, Vol 08.01.3Discontinued. See 1982 Annual Book of ASTM Standards, Parts 40 and 41.4Annual Boo
15、k of ASTM Standards, Vol 14.02.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
16、959, United States.formed by soldering a strip of gauze at right angles to theperiphery of a disk of bronze gauze. One of the bases acts as alid.6. Material6.1 Activated Carbon,614 MeshIt has been found thatdifferent types and grades of activated carbon give differingresults, thus making it necessar
17、y for the purchaser and theseller to agree on the same type and grade in order to obtainconcordant results. Care should be taken that an airtight storagecontainer is used for the activated carbon and that freshmaterial is used for each test, unless it can be shown that reusedoes not affect the resul
18、ts. The activated carbon shall bescreened through a 14-mesh screen immediately prior to use toeliminate fines.7. Test Specimens7.1 The test specimens shall be 50 mm diameter disks madeof the plastic material to be tested. Three specimens of eachformulation shall be tested.7.2 Thickness of the test s
19、pecimens shall be 0.25 6 0.025mm.NOTE 3If other thicknesses are desired due to purchase specificationsor other considerations, they may be used, but shall be specified in thereport.7.3 Direct comparison of values between materials shouldnot be made unless all specimens so compared do not vary bymore
20、 than 610 % from a given nominal thickness. Thisprecaution is necessary because of discrepancies that may arisedue to edge effects, depletion of volatiles, and the fact that thepercent weight loss is an inverse function of thickness.8. Conditioning8.1 ConditioningCondition the test specimens at 23 6
21、2C and 50 6 5 % relative humidity for not less than 20 h priorto test in accordance with Procedure A of Practice D 618.Preferably, specimens shall be suspended to assure free aircirculation among the specimens. In cases of disagreement, thetolerances shall be 61C and 62 % relative humidity.9. Proced
22、ureTest Method A, Direct Contact withActivated Carbon9.1 Weigh the conditioned specimens individually on theanalytical balance and designate this weight as W1. Weight ofindividual specimens shall be within a tolerance of 610 %.9.2 Spread 120 cm3of activated carbon evenly on thebottom of a container.
23、 Place one specimen on top of theactivated carbon and cover it with 120 cm3of activated carbon.Place a second specimen (Note 3) on top of the first and coverit with 120 cm3of the carbon, followed by a third specimen andthen 120 cm3more of activated carbon. Place a cover on thecontainer in such a man
24、ner that the container will be vented.This is necessary to assure that any possible pressure build-upin the container during heating is relieved. Take care that in nocase shall the carbon be packed by pressure other than theweight of the composite sandwich in the container.NOTE 4Only specimens of th
25、e same composition or formulation shallbe tested in a single container, because of the possibility of cross-migration between varying compositions.9.3 Place the container upright in the oven or bath. Unlessotherwise specified, the temperature of the oven or bath shallbe 70 6 1C and the duration of t
26、he test 24 h.9.4 At the end of the 24-h period, remove the container fromthe oven or bath. Then, within 1 h, remove the specimens fromthe container, brush free of carbon, and recondition in accor-dance with Section 8.9.5 After reconditioning, reweigh the specimens and desig-nate this weight as W2. W
27、eight of individual specimens shall bewithin a tolerance of 610 %.10. ProcedureTest Method B, Wire Cage10.1 Proceed as in Section 9 (Test Method A), except placeevery individual specimen in a small metal wire-mesh cageconstructed as indicated in 5.5, and maintain the temperature at100 6 1C.NOTE 5If
28、other conditions of test are desired, they may be employed,but shall be specified in the report.11. Calculation11.1 Calculate the volatile loss, expressed as percent weightloss based on the original specimen weight, as follows:weight loss, % 5 W12 W2!/W1# 3 100 (1)where:W1= initial weight of test sp
29、ecimen, andW2= final weight of test specimen.12. Report12.1 Report the following information:12.1.1 Complete identification of the material tested, includ-ing type, source, manufacturers code number, and previoushistory,12.1.2 Actual thickness to the nearest 0.025 mm for each ofthe three specimens t
30、ested, and the average of the three,12.1.3 Percent weight loss recorded to two significant fig-ures of each of the three specimens, and the average of thethree,12.1.4 Any observations as to distortion or change inappearance of the specimens,12.1.5 Type of activated carbon used, and12.1.6 Test temper
31、ature and duration of test.TABLE 1 Plasticizer VolatilityRound Robin TestMaterial VolatilityAverageLoss,%SrASRBrCRDSample 1 High 19.46 0.70 2.43 1.98 6.88Sample 2 Medium 3.83 0.35 0.87 0.98 2.48Sample 3 Low 0.81 0.12 0.42 0.35 1.20ASr= within-laboratory standard deviation of the average.BSR= between
32、-laboratories standard deviation of the average.Cr = 2.8 Sr.DR = 2.8 SR.D 1203 94 (2003)213. Precision and Bias13.1 Precision:613.1.1 Table 1 is based on a round robin conducted in 1988per Practice E 691, involving three materials tested by fivelaboratories. All tests were run by Test Method A for 2
33、4 h at90C. For each material, all the samples were prepared at onesource, but the individual specimens were prepared by thelaboratory which tested them. Each test result was the averageof 23 individual determinations. Three laboratories obtainedtwo test results for each material, whereas two test la
34、boratoriesobtained one test result for each material.13.1.1.1 The properties used in the analysis are volatility ofplasticizer from the plastic. The three materials were selectedto represent low, medium, and high volatility plasticizers.NOTE 6Caution: The following explanations of r and R (13.1.2-13
35、.1.2.3) are only intended to present a means of considering theapproximate precision of this test method. The data in Table 1 should notbe rigorously applied to acceptance or rejection of material, as those dataare specific to this round robin and may not be representative of other lots,conditions,
36、materials, or laboratories.Users of these test methods should apply the principles outlined inPractice E 691 to generate data specific to their laboratory and materials,or between specific laboratories. The principles of 13.1.2-13.1.2.3 wouldthen be valid for such data.13.1.2 Concept of r and RIf Sr
37、and SRhave beencalculated from a large enough body of data, and for test resultsthat were averages from testing 23 specimens:13.1.2.1 Repeatability, r (comparing two test results for thesame material, obtained by the same operator using the sameequipment on the same day)The two test results should b
38、ejudged not equivalent if they differ by more than the r value ofthe material.13.1.2.2 Reproducibility, R (comparing two test results forthe same material, obtained by different operators using differ-ent equipment on different days)The two test results shouldbe judged not equivalent if they differ
39、by more than the R valuefor that material.13.1.2.3 Any judgment in accordance with 13.1.2.1 or13.1.2.2 would have approximate 95 % (0.95) probability ofbeing correct.13.2 BiasThere are no recognized standards by which toestimate bias of these test methods.14. Keywords14.1 methanol extract; PVC resin
40、SUMMARY OF CHANGESThis section identifies the location of selected changes to these test methods. For the convenience of the user,Committee D20 has highlighted those changes that may impact the use of these test methods. This section mayalso include descriptions of the changes or reasons for the cha
41、nges, or both.D 120394 (1999)e1: (1) Removed all inch-pound units.ASTM International takes no position respecting 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 s
42、uch 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 reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invi
43、ted 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 theresponsible technical committee, which you may attend. If you feel that your comments have not received
44、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 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).6Supporting data are available from ASTM Headquarters. Request RR: D20-1129.D 1203 94 (2003)3
