1、Designation: D 5668 09Standard 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 last revision. A nu
2、mber in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover a hot mill method, two ovenmethods, and a press method for the determination of moistureand other volatile matte
3、r content in synthetic 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 mill.1.4 The values stated in SI units
4、 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-priate safety and health practices
5、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 for Evaluating Precision for Test Me
6、thodStandards in the Rubber and Carbon Black ManufacturingIndustriesE 145 Specification for Gravity-Convection 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 rubberproduction.3.2 The amount
7、 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 Specification E 145.4.3 Press, as described in Practice D 3182.METHOD AHOT-MILL TEST METHOD5. Summary of Test Method5.1 A weighed sample of
8、 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 min through alabo
9、ratory mill maintained at 100 6 5C (212 6 9F) with thedistance between the rolls set at 0.50 6 0.05 mm (0.020 60.002 in.) as determined by a lead slug. 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 sample throughthe mill for
10、 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 Calculate the percentage of vol
11、atile 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 on ChemicalAnalysis.Curre
12、nt edition approved May 1, 2009. Published May 2009. Originallyapproved in 1995. Last previous edition approved in 2008 as D 5668 08.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume infor
13、mation, 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 sample of rubber is sheeted out
14、 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 rolls set at 0.506 0.05 mm (0.020
15、 6 0.002 in.) with the temperature of the rollbeing no greater than 50C (122F). 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 draft. Allow the sheet tore
16、main 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 sample before placing in the o
17、ven, 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 before and after drying isca
18、lculated 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 0.506 0.05 mm (0.020 6 0.002 in.) and the temperature of the rollbeing no greater than 50C (122F). Pass the rubber twicebetween the rolls.12.2 Sele
19、ct 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 weigh. Repeat theheating fo
20、r 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 follows:Volatile Matter, % 5 A 2
21、 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 under pressure until allthe volat
22、iles 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 1.4 60.05 mm (0.055 6 0.002 in.) and the temperature of the
23、 rollsbeing no greater than 50C (122F). 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 press at 5500 6 275 kPa (800 6
24、 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 before heating in the press, g, a
25、ndB = 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; volatileD5668092ASTM International takes
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