1、Designation: D5667 95 (Reapproved 2015)Standard Test Method forRubber From Synthetic SourcesTotal and Water SolubleAsh1This standard is issued under the fixed designation D5667; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 The values
3、stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 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
4、 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D5668 Test Methods for Rubber From Synthetic SourcesVolatile MatterPART ATOTAL ASH3. Summary of Test Method3.1 A dried sample is accurately weighed into a taredcru
5、cible and ignited in a muffle furnace at about 550 C untilall the carbonaceous material is oxidized. The crucible is thenallowed 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 b
6、e used for quality control of rubber production.4.2 The total and water soluble ash content of a rubber canaffect the properties of compounded, vulcanized rubber such aswater absorption, swell, electrical properties, etc.5. Apparatus5.1 Crucible, tared, having a minimum volume of 25 cm3ofsample.NOTE
7、 1If water soluble ash is to be determined, use a fine-porosityfritted glass or sintered porcelain filtering crucible, placing 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 Muf
8、fle Furnace, capable of being maintained at 550 625 C.5.4 Glass Stirring Rod.5.5 Rubber Policeman.5.6 Drying Oven.6. Sample Preparation6.1 Prepare the sample by drying in accordance with TestMethods D5668Method A or Method B.7. Procedure7.1 Accurately weigh 3 to5gofthedried and sheetedsample in the
9、tared crucible, which has been ignited to constantweight at 550 6 25 C. In the case of alum-coagulated rubbers,which tend 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
10、6 25 C and allow it to remain there until thecarbonaceous material has been completely oxidized.NOTE 2Caution: Do not open 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
11、 6 25 C for 30 min. Then raise the temperature to 550 625 C and heat for at least1horuntil all the carbonaceous material hasbeen oxidized. Reduce temperature to 300 C before removing.7.2 After the carbon has been completely oxidized, removethe crucible from the furnace, cool it to room temperature i
12、nthe desiccator, and weigh it. If the ash line is within 3 mm ofthe rim of the crucible, discard the ash and rerun the analysis.7.3 Reheat the crucible and its contents for about 30 min at550 6 25 C, remove the crucible from the furnace, cool it to1This test method is under the jurisdiction of ASTM
13、Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved June 1, 2015. Published September 2015. Originallyapproved in 1995. Last previous edition approved in 2010 as D5667 95 (2010).DOI: 10.1520/D5667-95R15.2For referenced ASTM sta
14、ndards, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
15、PA 19428-2959. United States1room 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 the ashedsample and proceed to Method B.8. Calculation8.1 Calculate the percentage of total
16、 ash as follows:Total Ash, % 5 C 2 B!/A 2 B# 3100 (1)where:A = mass of crucible plus original dried sample, g, andB = mass of crucible, g, andC = mass of crucible plus ash, g.PART BWATER SOLUBLE ASH9. Summary of Test Methods9.1 The ash obtained in Part A is digested and washed withthree 30 cm3portio
17、ns 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 the 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. Al
18、low to stand for 5 min, stirringwith the glass rod tipped with the rubber policeman. Filter withsuction and repeat the digestion and filtration with two addi-tional 30 cm3portions of hot water. Dry the crucible for1hinan air oven at 105 6 5 C.10.2 If the sintered porcelain crucible was used, place i
19、n amuffle furnace at 550 6 25 C for 1 h. Cool the crucible in adesiccator and weigh it.10.3 If the fritted glass crucible was used, follow the heatingand cooling procedure described in Note 3. Finally, weigh thecrucible and contents at room temperature.11. Calculation11.1 Calculate the percentage wa
20、ter soluble ash as follows:Water Soluble Ash, % 5 C 2 D!/A 2 B# 3100 (2)where:A = mass of crucible plus original dried sample, g,B = mass of crucible, g,C = mass of crucible plus total ash, g, andD = mass of crucible plus insoluble ash, g.12. Keywords12.1 ash; synthetic rubber; total ash; water solu
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