1、Designation: D4571 06 (Reapproved 2017)Standard Test Methods forRubber Compounding MaterialsDetermination of VolatileMaterial1This standard is issued under the fixed designation D4571; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, the 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 the lossof volatile materials in various rubber chemicals
3、based on themass loss upon heating at 70C.1.2 These test methods for the determination of volatilematter include the following materials:SectionSulfur 714p-Phenylenediamine antidegradants 15231.3 The values stated in SI units are to regarded as thestandard. The values given in parentheses are for in
4、formationonly.1.4 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 and determine the applica-bility of regulatory limitations prior to use.1
5、.5 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
6、Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D4483 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 t
7、o This Standard:3.1.1 “lot” samplea production sample representative 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 rubber chemicals are weighed
8、 before and afterheating at 70C.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 determination ofvolatile material in rubber compoundin
9、g materials. The testmethods may be used for quality control, product acceptance,or research and development. Classification D4676 prescribespercent volatile material as an important characteristic ofrubber antidegradants.6. Apparatus6.1 Weighing Bottle, low form, 82 cm3capacity.6.2 Explosion-proof,
10、 Vented Air Circulating Oven, capableof temperature regulation of 70 6 2C.6.3 Analytical Balance, sensitive to 0.1 mg.6.4 Desiccator.SULFUR7. Scope7.1 This test method covers the measurement of the loss ofvolatiles from sulfur at 70C. The volatile components consistof moisture, low boiling organic c
11、omponents, and 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 issued by the World Trade Organizatio
12、n TechnicalBarriers to Trade (TBT) Committee.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.11 on Chemical Analysis.Current edition approved May 1, 2017. Published May 2017. Originallyapprov
13、ed in 1986. Last previous edition approved in 2012 as D4571 06 (2012).DOI: 10.1520/D4571-06R17.2For 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 Documen
14、t 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 accordance with internationally recognized principles on standardization established in the Decision on Prin
15、ciples for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.18. Summary of Test Method8.1 The sulfur specimen is weighed before and after heatingfor2hat70C. The measured loss of mass is the volati
16、lematerial content.9. Significance and Use9.1 This test method determines the volatile material insulfur at 70C. By ascertaining that the volatiles are lower thana predicted maximum limit, it may safely be concluded thatmoisture (water) is below that limit and is not present inexcessive amounts.9.2
17、Testing at temperatures higher than 70C results ingreater volatilization of sulfur.10. Apparatus10.1 See Section 6.11. Procedure11.1 Weigh the weighing bottle to the nearest 0.1 g (A).Then add approximately 5 g sulfur and weigh again (B). Makesure the sulfur covers the base of the bottle evenly.11.2
18、 Place the uncovered bottle in the 70C oven for 2 h.Remove the specimen, cover, and cool in a desiccator for 1 h(C). Weigh the cooled specimen to the nearest 0.1 mg.12. Calculation12.1 The volatile material is given by the following equa-tion:V 5 B 2 C!/B 2 A!# 3100 (1)where:V = volatiles, %,A = ori
19、ginal specimen mass in grams, andB = heated specimen mass in grams.13. Report13.1 Report results obtained from two individual determi-nations and their average to the nearest 0.01 %.14. Precision and Bias314.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer
20、to Practice D4483 forterminology and other statistical details.14.2 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 parameters
21、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.14.3 A Type 1 (interlaboratory) precision was evaluated in1986. Both repeatability a
22、nd 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.14.4 Three different materials were used in the interlabo
23、ra-tory program. These were tested in seven laboratories on twodifferent days.14.5 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 evalu-ated.14.6 The precision of this te
24、st 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 amean level in Table 1 c
25、losest to the mean level underconsideration at any given time, for any given material inroutine testing operations.14.7 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tabulated inTable 1. Two single test results, obtained under normal testmethod p
26、rocedures, that differ by more than this tabulated r(for any given level) must be considered as derived fromdifferent sample populations.14.8 ReproducibilityThe reproducibility, R, of this testmethod has been established as the appropriate value tabulatedin Table 1. Two single test results obtained
27、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.NOTE 1The values of r and R are relatively large, whereas the averageor mean test level is
28、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.14.9 The relative repeatability (r) and reproducibility (R)have been omitted from Table 1 since the level of values testedwas extremely low and approached
29、the limits of sensitivity ofthe test method. Under these circumstances the relative valuesbecome trivial.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1047.TABLE 1 Type 1 Precision ResultsVolatile Materials, PercentMateria
30、lAver-ageWithin LaboratoryABetween LaboratoryASrrSRRGeneral PurposeGround Sulfur0.07 0.018 0.053 0.045 0.127Oil Treated, 90 %Insolule SulfurA0.26 0.025 0.073 0.130 0.368Oil Treated, 90 %Insoluble SulfurB0.32 0.042 0.119 0.151 0.427Pooled ValuesB0.22 0.030 0.087 0.119 0.338ASr= repeatability standard
31、 deviation.r = repeatability = 2.83 the square root of the repeatability variance.SR= reproducibility standard deviation.R = reproducibility = 2.83 the square root of the reproducibility variance.BNo values omitted.D4571 06 (2017)214.10 BiasIn test method terminology, bias is the differ-ence between
32、 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.p-PHENYLENEDIAMINE ANTIDEGRADANT15. Scope15.1 This test method describes the determination of vola-tile materials in p-phenylened
33、iamine antidegradants and isbased on the mass loss upon heating at 70C.15.2 The measured loss on heating represents volatile or-ganics plus moisture.15.3 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decisio
34、n on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.16. Summary of Test Method16.1 The p-phenylenediamine test unit is weighed beforeand after heating for3hat70C. The measured dif
35、ference inmass is the volatile material.17. Significance and Use17.1 The quantity of volatile material inp-phenylenediamines can affect performance of these an-tidegradants in rubber if they exceed critical levels.17.2 Since the loss on heating is an empirical and nonspe-cific method, it is essentia
36、l that the prescribed analysis condi-tions (sample container, oven temperature, oven air flow,cooling conditions, and so forth) be controlled so that resultsare meaningful.17.3 Prolonged heating or overheating of the sample or thetest unit can result in high heat loss values due to oxidativegenerati
37、on of volatile degradation products.18. Apparatus18.1 See Section 6.19. Sampling19.1 To ensure homogeneity, at least 250 g of the “lot”sample should be well blended prior to removing the test unit.20. Procedure20.1 Dry a clean weighing bottle and stopper (stopperremoved) for 30 min in the specified
38、oven set at 70C. Placethe bottle and stopper in the desiccator and allow them to coolto room temperature. Weigh the bottle with a stopper to thenearest 0.1 mg (A).20.2 Weigh a nominal 20-g test unit into the weighing bottleto the nearest 0.1 mg (B).20.3 Place the weighing bottle containing the test
39、unit andthe stopper (with the stopper removed) in the specified oven,which has equilibrated at 70C, for 3 h.20.4 After the heating period, replace the stopper andtransfer the bottle to the desiccator for a period of timesufficient for the assembly to equilibrate at room temperature.Reweigh the bottl
40、e to the nearest 0.1 mg (C).20.5 Repeat the procedure on a second test unit.21. Calculation21.1 Calculate the percent heating loss to the nearest 0.1 %as follows:H 5 B 2 C!/B 2 A!# 3100 (2)where:H = heating loss, %,A = mass of weighing bottle and stopper, g,B = mass of weighing bottle, stopper, and
41、test unit beforeheating, g, andC = mass of weighing bottle, stopper, and test unit afterheating, g.22. Report22.1 Report the following information:22.1.1 Proper identification of the sample, and22.1.2 Results obtained from two individual determinationsand their average, to the nearest 0.01 %.23. Pre
42、cision and Bias323.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to Practice D4483 forterminology and other statistical details.23.2 A Type 1 (interlaboratory) precision was evaluated in1987. Both repeatability and reproducibility are short term. Aperiod
43、 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.23.3 Four different materials were used in the interlabora-tory program. These were tested in six l
44、aboratories on twodifferent days.23.4 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.TABLE 2 Volatile Materials of p -Phenylenediamine, PercentMaterialAver-age
45、Within LaboratoryABetween LaboratoryASrrSRRM1-6PPD 0.06 0.022 0.062 0.029 0.083M2-IPPD 0.08 0.004 0.011 0.026 0.075M3-BMPPD 0.19 0.034 0.098 0.073 0.026M4-DTPD 0.04 0.002 0.005 0.019 0.055Pooled ValuesB0.09 0.021 0.061 0.045 0.129ASr= repeatability standard deviation.r = repeatability = 2.83 the squ
46、are root of the repeatability variance.SR= reproducibility standard deviation.R = reproducibility = 2.83 the square root of the reproducibility variance.BNo values omitted.D4571 06 (2017)323.5 The precision of this test method may be expressed inthe format of the following statements which use an “a
47、ppro-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 amean level in Table 2 closest to the mean level underconsideration at any given time, for any given mat
48、erial inroutine testing operations.23.6 RepeatabilityThe 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 b
49、e considered as derived fromdifferent or nonidentical sample populations.23.7 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.23.8 The relative repeatability (r) and reproducibility (R)have been omitted from Tabl
