1、Designation: D 5667 95 (Reapproved 2005)Standard Test Method forRubber From Synthetic SourcesTotal and Water SolubleAsh1This standard is issued under the fixed designation D 5667; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 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. Scope1.1 This test method covers a test method for the determi-nation of ash content in synthetic rubber.1.2 This sta
3、ndard 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 and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1
4、ASTM Standards:2D 5668 Test Methods for Rubber from Synthetic SourcesVolatile MatterPART ATOTAL ASH3. Summary of Test Method3.1 A dried sample is accurately weighed into a taredcrucible and ignited in a muffle furnace at about 550C until allthe carbonaceous material is oxidized. The crucible is then
5、allowed to cool in a desiccator and weighed, and the percent-age of ash is calculated.4. Significance and Use4.1 These tests are mainly intended for referee purposes butcan also be used for quality control of rubber production.4.2 The total and water soluble ash content of a rubber canaffect the pro
6、perties of compounded, vulcanized rubber such aswater absorption, swell, electrical properties, etc.5. Apparatus5.1 Crucible, tared, having a minimum volume of 25 cm3ofsample.NOTE 1If water soluble ash is to be determined, use a fine-porosityfritted glass or sintered porcelain filtering crucible, pl
7、acing a small amountof ashless filter paper in the bottom of the crucible in order to prevent lossof liquid pyrolysis products.5.2 Ashless Filter Paper, 150 mm in diameter.5.3 Muffle Furnace, capable of being maintained at 550 625C.5.4 Glass Stirring Rod.5.5 Rubber Policeman.5.6 Drying Oven.6. Sampl
8、e Preparation6.1 Prepare the sample by drying in accordance with TestMethods D 5668Method A or Method B.7. Procedure7.1 Accurately weigh 3 to5gofthedried and sheetedsample in the tared crucible, which has been ignited to constantweight at 550 6 25C. In the case of alum-coagulated rubbers,which tend
9、to boil over during ashing, wrap the sample tightlyin a 150-mm ashless filter paper before ashing. Place thecrucible containing the sample directly into the muffle furnaceat 550 6 25C and allow it to remain there until thecarbonaceous material has been completely oxidized.NOTE 2Caution: Do not open
10、the door of the furnace for at least 1 hafter the crucible has been placed in the furnace.NOTE 3If fritted glass crucible is used, place the crucible in the mufflefurnace at 300 6 25C for 30 min. Then raise the temperature to 550 625C and heat for at least1horuntil all the carbonaceous material hasb
11、een oxidized. Reduce temperature to 300C before removing.7.2 After the carbon has been completely oxidized, removethe crucible from the furnace, cool it to room temperature inthe desiccator, and weigh it. If the ash line is within 3 mm ofthe rim of the crucible, discard the ash and rerun the analysi
12、s.7.3 Reheat the crucible and its contents for about 30 min at550 6 25C, remove the crucible from the furnace, cool it toroom temperature in the desiccator, and weigh it. If the massdiffers by more than 1 % from the previous reading, repeat thisstep.7.4 If water soluble ash is to be determined, save
13、 the ashedsample and proceed to Method B.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved May 1, 2005. Published May 2005. Originallyapproved in 1995. Last previous edition
14、 approved in 2000 as D 5667 - 95(2000).2For referenced 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.1Copyright ASTM Intern
15、ational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8. Calculation8.1 Calculate the percentage of total ash as follows:Total Ash, % 5 C 2 B!/A 2 B 3 100 (1)where:A = mass of crucible plus original dried sample, g, andB = mass of crucible, g, andC = mass of cr
16、ucible plus ash, g.PART BWATER SOLUBLE ASH9. Summary of Test Methods9.1 The ash obtained in Part A is digested and washed withthree 30 cm3portions of water, the crucible and contents aredried in an oven, and the crucible is then placed in a mufflefurnace. The crucible is then cooled, weighed, and th
17、e percent-age of soluble ash is calculated.10. Procedure10.1 Add 30 cm3of hot deionized water, at a temperature of80 to 90C, to the crucible. Allow to stand for 5 min, stirringwith the glass rod tipped with the rubber policeman. Filter withsuction and repeat the digestion and filtration with two add
18、i-tional 30 cm3portions of hot water. Dry the crucible for1hinan air oven at 105 6 5C.10.2 If the sintered porcelain crucible was used, place in amuffle furnace at 550 6 25C for 1 h. Cool the crucible in adesiccator and weigh it.10.3 If the fritted glass crucible was used, follow the heatingand cool
19、ing procedure described in Note 3. Finally, weigh thecrucible and contents at room temperature.11. Calculation11.1 Calculate the percentage water soluble ash as follows:Water Soluble Ash, % 5 C 2 D!/A 2 B 3 100 (2)where:A = mass of crucible plus original dried sample, g,B = mass of crucible, g,C = m
20、ass of crucible plus total ash, g, andD = mass of crucible plus insoluble ash, g.12. Keywords12.1 ash; synthetic rubber; total ash; water soluble ashASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
21、 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 time by the responsible technical committee and must be reviewed every f
22、ive 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 receive careful consideration at a meeting of theresponsible technical
23、 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 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 5667 95 (2005)2
