1、Designation: D 4574 06Standard Test Methods forRubber Compounding MaterialsDetermination of AshContent1This standard is issued under the fixed designation D 4574; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 These test methods cover the determination of ashcontent of rubber chemicals.1.2 The test methods include the following mater
3、ials:Material SectionSulfur 7-13p-Phenylenediamine Antioxidants 14-22Benzothiazole Sulfenamide Accel-erators14-221.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety
4、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 ASTM Standards:2D 4483 Practice for Evaluating Prec
5、ision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD 4676 Classification for Rubber CompoundingMaterialsAntidegradants3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 “lot” samplea production sample representative ofa standard production unit,
6、normally referred to as “thesample.”3.1.2 test unitthe actual material used in the analysis. Itmust be representative of the “lot” sample.4. Summary of Test Methods4.1 The ash content is determined by heating a knownquantity of the rubber chemical on a hot plate or over a gasburner to volatilize the
7、 sample and then heating in a mufflefurnace to complete the ashing process.4.2 Sample preparation, procedures, calculations, and pre-cision statements will be found in each section dealing with aparticular rubber chemical.5. Significance and Use5.1 These test methods are suitable for the determinati
8、on ofthe ash content of rubber compounding materials. The testmethods may be used for quality control, product acceptance,or research and development. Classification D 4676 prescribespercent ash as an important characteristic of rubber anti-degradants.6. Apparatus6.1 Muffle Furnace, capable of tempe
9、rature regulation of625C between 500 and 800C.6.2 Hot Plate (or laboratory gas burner).6.3 Laboratory Fume Hood.6.4 Porcelain Combustion Crucible, capsule form, 25-cm3capacity.6.5 Porcelain Crucible, high form, size 0, 15-cm3capacity.6.6 Clay Triangle.6.7 Steel Crucible Tongs.6.8 Heat Resistant Glov
10、es.6.9 Desiccator.6.10 Analytical Balance, sensitive to 0.0001 g.6.11 Air Circulating Oven, capable of 70 6 2C.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Oct. 1, 2
11、006. Published October 2006. Originallyapproved in 1986. Last previous edition approved in 2002 as D 4574 02.2For 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 sta
12、ndards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.SULFUR7. Scope7.1 This test method is used for the determination of the ashcontent of sulfur.8. Summary of Test Method8.1 The ash content
13、 of sulfur is determined by the controlledburning of the sulfur, followed by ashing in a furnace at 600C.9. Apparatus9.1 See Section 6.10. Procedure10.1 Dry6gormore of sulfur in an oven at 70C for 2 h.Cool in a desiccator.10.2 Weigh a 5-g specimen to the nearest 0.0001 g into apreviously ignited, we
14、ighed, 25-cm3porcelain crucible. In awell-ventilated hood, place the crucible on a hot plate and heatto 400 to 500C, burning off all of the sulfur; or burn off thesulfur by moderate heating over a gas burner. When all of thesulfur is gone, transfer the crucible to a muffle furnace and heatto 600 6 2
15、5C for at least 20 min. Cool in a desiccator andweigh.11. Calculation11.1 Calculate the percent ash as follows:A 5 B/C! 3 100 (1)where:A = ash, %,B = mass of ash, g, andC = mass of sample, g.12. Report12.1 Report the following information:12.1.1 Proper identification of the sample, and12.1.2 Results
16、 of two individual determinations and theiraverage reported as percent ash to the nearest 0.01 %.13. Precision and Bias313.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical details.13.2 The precision r
17、esults in this precision and bias sectiongive an estimate of the precision of this test method with thematerials (rubbers) used in the particular interlaboratory pro-grams as described below. The precision parameters should notbe used for acceptance/rejection testing of any group ofmaterials without
18、 documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.13.3 A Type 1 (interlaboratory) precision was evaluated in1986. Both repeatability and reproducibility are short term. Aperiod of a few days separates replicate test r
19、esults.Atest resultis the mean value, as specified by this test method, obtained ontwo determinations or measurements of the property or param-eter in question.13.4 Three different materials were used in the interlabora-tory program. They were tested in seven laboratories on twodifferent days.13.5 T
20、he results of the precision calculations for repeatabil-ity and reproducibility are given in Table 1, in ascending orderof material average or level, for each of the materials evalu-ated.NOTE 1The percent ash values have been multiplied by 100 to avoidleading zeros in Table 1. The values of Sr,r,SR,
21、 and R are influenced bythis multiplication factor, for example: Sr(percent ash times 100)/100 = Sr(actual or true percent ash basis).13.6 The precision of this test method may be expressed inthe format of the following statements which use an “appro-priate value” of r, R,(r), or (R), that is, that
22、value to be used indecisions about test results (obtained with the test method).The appropriate value is that value of r and R associated witha mean level in Table 1 closest to the mean level underconsideration at any given time, for any given material inroutine testing operations.13.7 Repeatability
23、The repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 1. Two single test results, obtained under normal testmethod procedures, that differ by more than this tabulated r(for any given level) must be considered as derived fromdifferent or nonidentical
24、 sample populations.13.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value tabulatedin Table 1. Two single test results obtained in two differentlaboratories, under normal test method procedures, that differby more than the tabulated R (for any g
25、iven level) must beconsidered to have come from different or nonidentical samplepopulations.NOTE 2The values of r and R are relatively large, whereas the averageor mean test level is small (close to zero). This is typical for this type ofprecision measurement process. This should be kept in mind whe
26、never useis made of r and R.13.9 The relative repeatability (r) and reproducibility (R)have been omitted from Table 1 since the level of values tested3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D11-1050.TABLE 1 Precision Re
27、sultsAsh, %, 3 100Material AverageWithin LaboratoryABetween LaboratoryASrrSRRInsolubleSulfurA (OilTreated, 90 %)0.39 0.318 0.901 0.507 1.43General PurposeGround Sulfur3.43 0.847 2.399 1.560 4.41InsolubleSulfurB (OilTreated, 90 %)7.75 1.772 5.015 2.150 6.08Pooled ValuesB3.85 1.149 3.251 1.561 4.41ASr
28、= repeatability standard deviation.r = repeatability (2.83 3 the square root of the repeatability variance).SR= reproducibility standard deviation.R = reproducibility (2.83 3 the square root of the reproducibility variance).BNo values omitted.D4574062was extremely low and approached the limits of se
29、nsitivity ofthe test method. Under these circumstances the relative valuesbecome trivial.13.10 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (or true)test property value. Reference values have not been evaluatedfor this test method. Bias, the
30、refore, cannot be determined.ACCELERATORS AND ANTIDEGRADANTS14. Scope14.1 This test method describes the determination of the ashcontent of accelerators and antidegradants.15. Summary of Test Method15.1 The ash content is determined by heating a knownquantity of material over a gas burner to remove
31、organicmaterial leaving a carbonaceous mass. Ashing is completed ina muffle furnace. The remaining ash, measured by massdifference, is expressed as a percent of the original material.16. Significance and Use16.1 The ash content of a sample is the amount of allnoncarbon components that remain after c
32、ombustion, indepen-dent of chemical form. In effect, the analysis measures residualinorganic impurities that can remain with the product at lowlevels following the manufacturing process.16.2 The quantity of ash in accelerators or antidegradantscan affect the performance of these additives in rubber
33、ifcritical levels are exceeded.17. Apparatus17.1 See Section 6.18. Sampling18.1 To ensure homogeneity, at least 250 g of the lot sampleshould be well blended prior to removing the test unit.19. Procedure19.1 Ignite the 15-cm3crucible in the muffle furnace at 7506 25C for 30 min.19.2 Transfer the cru
34、cible to the desiccator, cool to roomtemperature and weigh to the nearest 0.0001 g (B).19.3 Weigh a 5-g test unit to the nearest 0.0001 g into theignited crucible (C). Place the crucible in the clay triangle, andcarefully heat the crucible and contents with the gas burneruntil all volatile material
35、and pyrolysis products have beenremoved (gases may flame) and the residue has been carbon-ized.19.4 Transfer the crucible to the muffle furnace at 750625C and ignite for 2 h.19.5 Carefully transfer the crucible containing the ash to thedesiccator, cool to room temperature, and reweigh to thenearest
36、0.0001 g (D).19.6 Repeat the procedure on a second test unit.20. Calculation20.1 Calculate the percent ash to the nearest 0.01 % asfollows:A 5 D 2 B!/C 2 B!# 3 100 (2)where:A = ash, %,B = mass of crucible, g,C = mass of crucible plus test unit, g, andD = mass of crucible plus the ash, g.21. Report21
37、.1 Report the following information:21.1.1 Proper identification of the sample, and21.1.2 Results obtained from two individual determinationsand their average, reported to the nearest 0.01 %.22. Precision and Bias322.1 This precision and bias section has been prepared inaccordance with Practice D 44
38、83. Refer to Practice D 4483 forterminology and other statistical details.22.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials (rubbers) used in the particular interlaboratory pro-grams as described below. The precision
39、parameters should notbe used for acceptance/rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing protocols thatinclude this test method.22.3 A Type 1 (interlaboratory) precision was evaluated in1987. Both repe
40、atability and reproducibility are short term. Aperiod of a few days separates replicate test results.Atest resultis the mean value, as specified by this test method, obtained ontwo determinations or measurements of the property or param-eter in question.22.4 Six different materials were used in the
41、interlaboratoryprogram. These were tested in seven laboratories on twodifferent days.22.5 The results of the precision calculations for repeatabil-ity and reproducibility are given in Table 2, in ascending orderof material average or level, for each of the materials evalu-ated.22.6 The precision of
42、this test method may be expressed inthe format of the following statements which use an “appro-priate value” of r, R,(r), or (R), that is, that value to be used indecisions about test results (obtained with the test method).The appropriate value is that value of r or R associated with aTABLE 2 Ash C
43、ontent, PPD Antidegradants and Accelerators, %MaterialAver-ageWithin LaboratoryABetween LaboratoryASrrSRRM1-6PPD 0.02 0.012 0.033 0.013 0.036M2-IPPD 0.01 0.004 0.013 0.009 0.026M3-BMPPD 0.01 0.007 0.020 0.012 0.034M4-DTPD 0.02 0.005 0.015 0.008 0.025M5-DCBS 0.03 0.002 0.006 0.007 0.020M6-TBBS 0.05 0
44、.005 0.016 0.009 0.027Pooled valuesB0.02 0.007 0.020 0.010 0.028ASr= repeatability standard deviation.r = repeatability (2.83 3 the square root of the repeatability variance).SR= reproducibility standard deviation.R = reproducibility (2.83 3 the square root of the reproducibility variance).BNo value
45、s omitted.D4574063mean level in Table 2 closest to the mean level underconsideration at any given time, for any given material inroutine testing operations.22.7 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 2. Two single test re
46、sults, obtained under normal testmethod procedures, that differ by more than this tabulated r(for any given level) must be considered as derived fromdifferent or nonidentical sample populations.22.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate val
47、ue tabulatedin Table 2. Two single test results obtained in two differentlaboratories, under normal test method procedures, that differby more than the tabulated R (for any given level) must beconsidered to have come from different or nonidentical samplepopulations.22.9 The relative repeatability, (
48、r), and reproducibility, (R),have been omitted from Table 2 since the level of values testedwas extremely low and approached the limits of sensitivity ofthe test method. Under these circumstances the relative valuesbecome trivial.22.10 BiasIn test method terminology, bias is the differ-ence between
49、an average test value and the reference (or true)test property value. Reference values have not been evaluatedfor this test method. Bias, therefore, cannot be determined.23. Keywords23.1 accelerators; antidegradants; ash; rubber compoundingmaterials; sulfurASTM 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 such rights, are enti
