1、Designation: D 5668 99 (Reapproved 2003)Standard Test Methods forRubber From Synthetic SourcesVolatile Matter1This standard is issued under the fixed designation D 5668; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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 four test methods: a hot millmethod, two oven methods and a press method for thedetermination
3、of moisture and other volatile matter content insynthetic rubber.1.2 Either oven method shall be used especially when therubber is too tacky to be handled satisfactorily on a hot mill.1.3 The press method shall be used for rubbers that are toocrumbly to be retained satisfactorily on a laboratory mil
4、l.1.4 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-
5、priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 3182 Practice for RubberMaterials, Equipment andProcedures for Mixing Standard Compounds and Prepar-ing Standard Vulcanized SheetsD 4483 Practice fo
6、r Determining Precision for Test MethodStandards in the Rubber and Carbon Black IndustriesE 145 Specification for Gravity-Convention and Forced-Ventilation Ovens3. Significance and Use3.1 These test methods are mainly intended for refereepurposes but can also be used for quality control of rubberpro
7、duction.3.2 The amount of volatiles can affect processing and curecharacteristics of compounded rubber.4. Apparatus4.1 Mill, as described in Practice D 3182.4.2 Oven, as described in Practice E 145.4.3 Press, as described in Practice D 3182.METHOD AHOT-MILL TEST METHOD5. Summary of Test Method5.1 A
8、weighed sample of rubber is sheeted out on a heatedmill until all the volatile matter is driven off. The sample isweighed again and the percentage of volatile matter is calcu-lated.6. Procedure6.1 Weigh a test sample of at least 250 g to the nearest 0.1g.6.2 Pass the weighed sample repeatedly for 4
9、min through alaboratory mill maintained at 100 6 5C (212 6 9F) with thedistance between the rolls at 0.25 6 0.05 mm (0.010 6 0.002in.) as determined by a lead slug for 4 min. Do not allow thesample to band, and take care to avoid any loss of sample.Weigh the sample to the nearest 0.1 g. Pass the sam
10、ple throughthe mill for an additional 2 min and reweigh. If the weights atthe end of the 4- and 6-min periods are within 0.1 g, calculatethe volatile matter; if not, continue passing the sample throughthe mill for 2-min periods until the weight remains constantwithin 0.1 g.7. Calculation7.1 Calculat
11、e the percentage of volatile matter as follows:Volatile Matter, % 5 A 2 B!/A# 3 100 (1)where:A = mass of original sample, g, andB = mass of sample after milling, g.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 o
12、n ChemicalAnalysis.Current edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 1995. Last previous edition approved in 1999 as D 566899.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book
13、of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.METHOD BOVEN TEST METHODLARGE TEST SPECIMEN8. Summary of Test Method8.1 A weighed sa
14、mple of rubber is sheeted out on alaboratory mill, then placed in an oven and dried to constantweight. The difference in weight before and after drying iscalculated as volatile matter.9. Procedure9.1 Sheet out a sample (at least 250 g) of rubber on alaboratory mill with the distance between the roll
15、s set at 0.256 0.05 mm (0.010 6 0.002 in.) with the temperature of the rollbeing no greater than 32C (90F). Pass the rubber twicebetween the rolls.9.2 Weigh the entire sheet to the nearest 0.1 g and place ina forced air circulation oven set at 100 6 5C (212 6 9F) sothat both sides are exposed to the
16、 draft. Allow the sheet toremain in the oven until the mass is constant to within 0.1 g.One hour is usually sufficient for rubbers containing no morethan 1.0 % moisture.10. Calculation10.1 Calculate the percentage volatile matter as follows:Volatile Matter, % 5 A 2 B!/A# 3 100 (2)where:A = mass of s
17、ample before placing in the oven, g, andB = mass of sample after drying in the oven, g.METHOD COVEN TEST METHODSMALL TEST SPECIMEN11. Summary of Test Method11.1 A weighed sample of rubber is sheeted out on alaboratory mill, then placed in an oven and dried to constantweight. The difference in weight
18、 before and after drying iscalculated as volatile matter.12. Procedure12.1 Sheet out about 250 g of a sample of rubber on alaboratory mill with the distance between the rolls set at 0.256 0.05 mm (0.010 6 0.002 in.) and the temperature of the rollbeing no greater than 32C (90F). Pass the rubber twic
19、ebetween the rolls.12.2 Select a 10-g sample (cut in small pieces approxi-mately 25 mm3) weighed to the nearest 0.001 g and place in aforced air circulation oven set at 100 6 5C (212 6 9F) for 1h so that the sample has the largest surface area exposed to thehot air. Allow to cool in a desiccator and
20、 weigh. Repeat theheating for further 30-min periods until the mass does notdecrease by more than 0.01 % of the initial mass in successiveweighings. One hour is usually sufficient for rubbers contain-ing no more than 1.0 % moisture.13. Calculation13.1 Calculate the percentage volatile matter as foll
21、ows:Volatile Matter, % 5 A 2 B!/A# 3 100 (3)where:A = mass of sample before placing in the oven, g, andB = mass of sample after drying in the oven, g.METHOD DPRESS TEST METHOD14. Summary of Test Method14.1 A sample of rubber is blended on a laboratory mill,weighed, then placed in a heated press unde
22、r pressure until allthe volatiles are driven off. The sample is weighed again andthe loss of volatile matter is calculated from the loss in mass.15. Procedure15.1 Sheet out about 250 g of a sample of rubber on alaboratory mill with the distance between the rolls set at 1.460.05 mm (0.055 6 0.002 in.
23、) and the temperature of the rollsbeing no greater than 32C (90F). Pass the sample twicebetween the rolls.15.2 Weigh 5 to7gofthemilled sample to the nearest0.001 g.15.3 Place between two polytetrafluoroethylene coatedmetal sheets in a press with the platens maintained at 150 610C (302 6 18F) and pre
24、ss at 5500 6 275 kPa (800 6 40psi) for 3 min.15.4 If the sample is cloudy or contains bubbles, press againfor 3 min. Allow to cool in a desiccator and weigh.16. Calculation16.1 Calculate the percentage of volatiles as follows:Volatile matter, % 5 A 2 B!/A# 3 100 (4)where:A = mass of the sample befor
25、e heating in the press, g, andB = mass of the sample after drying in the press, g.17. Precision17.1 Precision statements are being prepared in accordancewith Practice D 4483. They will be added as a revision to thesetest methods when they are completed.18. Keywords18.1 synthetic rubber; volatileD 56
26、68 99 (2003)2ASTM 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 such patent rights, and the riskof infringement of suc
27、h 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 invited either for revision of this standard or for addit
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29、 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).D 5668 99 (2003)3
