1、Designation: D4574 06 (Reapproved 2017)Standard Test Methods forRubber Compounding MaterialsDetermination of AshContent1This standard is issued under the fixed designation D4574; 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 () 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
3、following materials:Material SectionSulfur 713p-Phenylenediamine Antioxidants 1422Benzothiazole Sulfenamide Accel-erators14221.3 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 o
4、f 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.1.5 This international standard was developed in accor-dance with
5、internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2
6、D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4676 Classification for Rubber Compounding MaterialsAntidegradants3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 “lot” samplea production sample representat
7、ive of astandard production unit, normally referred to as “the sample.”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
8、 over a gasburner to volatilize the 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 metho
9、ds are suitable for the determination ofthe ash content of rubber compounding materials. The testmethods may be used for quality control, product acceptance,or research and development. Classification D4676 prescribespercent ash as an important characteristic of rubber antidegra-dants.6. Apparatus6.
10、1 Muffle Furnace, capable of temperature 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 Cruc
11、ible Tongs.6.8 Heat Resistant Gloves.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 Rubber-like Materials and are the direct responsibility of SubcommitteeD1
12、1.11 on Chemical Analysis.Current edition approved May 1, 2017. Published May 2017. Originallyapproved in 1986. Last previous edition approved in 2012 as D4574 06 (2012).DOI: 10.1520/D4574-06R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
13、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, PA 19428-2959. United StatesThis international standard was developed in accordan
14、ce with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1SULFUR7. Scope7.1 This test method
15、is used for the determination of the ashcontent of sulfur.7.2 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations i
16、ssued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.8. Summary of Test Method8.1 The ash content 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
17、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, weighed, 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 mo
18、derate heating over a gas burner. When all of thesulfur is gone, transfer the crucible to a muffle furnace and heatto 600 6 25C for at least 20 min. Cool in a desiccator andweigh.11. Calculation11.1 Calculate the percent ash as follows:A 5 B/C! 3100 (1)where:A = ash, %,B = mass of ash, g, andC = mas
19、s of sample, g.12. Report12.1 Report the following information:12.1.1 Proper identification of the sample, and12.1.2 Results 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 i
20、naccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.13.2 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 des
21、cribed below. The precision 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.13.3 A Type 1 (interlaboratory) precision was
22、 evaluated in1986. Both repeatability 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.13.4 Three differe
23、nt materials were used in the interlabora-tory program. They were tested in seven laboratories on twodifferent days.13.5 The 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 ev
24、alu-ated.NOTE 1The percent ash values have been multiplied by 100 to avoidleading zeros in Table 1. The values of Sr,r,SR, 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 b
25、e 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 and R associated witha mean level in Table 1 closest to t
26、he mean level underconsideration at any given time, for any given material inroutine testing operations.13.7 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 1. Two single test results, obtained under normal testmethod procedures,
27、that differ by more than this tabulated r(for any given level) must be considered as derived fromdifferent or nonidentical sample populations.13.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value tabulatedin Table 1. Two single test results obta
28、ined in two differentlaboratories, under normal test method procedures, that differ3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1050.TABLE 1 Precision ResultsAsh, %, 100Material AverageWithin LaboratoryABetween Laboratory
29、ASrrSRRInsolubleSulfurA (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= repeatability standard deviation.r = repeatability (2.83 the square
30、root of the repeatability variance).SR= reproducibility standard deviation.R = reproducibility (2.83 the square root of the reproducibility variance).BNo values omitted.D4574 06 (2017)2by more than the tabulated R (for any given level) must beconsidered to have come from different or nonidentical sa
31、mplepopulations.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 whenever useis made of r and R.13.9 The relative repeatability (r) and reproduc
32、ibility (R)have been omitted from Table 1 since the level of values testedwas extremely low and approached the limits of sensitivity 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 va
33、lue and the reference (or true)test property value. Reference values have not been evaluatedfor this test method. Bias, therefore, cannot be determined.ACCELERATORS AND ANTIDEGRADANTS14. Scope14.1 This test method describes the determination of the ashcontent of accelerators and antidegradants.14.2
34、This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Tra
35、de (TBT) Committee.15. Summary of Test Method15.1 The ash content is determined by heating a knownquantity of material over a gas burner to remove organicmaterial leaving a carbonaceous mass. Ashing is completed ina muffle furnace. The remaining ash, measured by massdifference, is expressed as a per
36、cent of the original material.16. Significance and Use16.1 The ash content of a sample is the amount of allnoncarbon components that remain after combustion, indepen-dent of chemical form. In effect, the analysis measures residualinorganic impurities that can remain with the product at lowlevels fol
37、lowing the manufacturing process.16.2 The quantity of ash in accelerators or antidegradantscan affect the performance of these additives in rubber 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 ble
38、nded 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 crucible 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
39、 crucible (C). Place the crucible in the clay triangle, andcarefully heat the crucible and contents with the gas burneruntil all volatile material 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 750625
40、C and ignite for 2 h.19.5 Carefully transfer the crucible containing the ash to thedesiccator, cool to room temperature, and reweigh to thenearest 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
41、 B!# 3100 (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. Report21.1 Report the following information:21.1.1 Proper identification of the sample, and21.1.2 Results obtained from two individual determinationsand their ave
42、rage, reported to the nearest 0.01 %.22. Precision and Bias322.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.22.2 The precision results in this precision and bias sectiongive an estimate of t
43、he 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 documentation that they are applicable tothose particular mat
44、erials and the specific testing protocols thatinclude this test method.22.3 A Type 1 (interlaboratory) precision was evaluated in1987. Both repeatability and reproducibility are short term. Aperiod of a few days separates replicate test results.Atest resultis the mean value, as specified by this tes
45、t method, obtained ontwo determinations or measurements of the property or param-eter in question.22.4 Six different materials were used in the interlaboratoryprogram. These were tested in seven laboratories on twodifferent days.22.5 The results of the precision calculations for repeatabil-ity and r
46、eproducibility are given in Table 2, in ascending orderof material average or level, for each of the materials evalu-ated.D4574 06 (2017)322.6 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, t
47、hat 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 amean level in Table 2 closest to the mean level underconsideration at any given time, for any given material inroutine testing operations.22.7 Repeatabil
48、ityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 2. 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 nonidenti
49、cal sample populations.22.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value 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, (r), and reproducibility, (R),have been omitted from Table 2 since the level of values testedwas extremely low and approach
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