1、Designation: D 4571 06Standard Test Methods forRubber Compounding MaterialsDetermination of VolatileMaterial1This standard is issued under the fixed designation D 4571; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 These test methods cover the determination of the lossof volatile materials in various rubber chemicals based on themas
3、s loss upon heating at 70C.1.2 These test methods for the determination of volatilematter include the following materials:SectionSulfur 7-14p-Phenylenediamine antidegradants 15-231.3 The values stated in SI units are to regarded as thestandard. The values given in parentheses are for informationonly
4、.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.2. Referenced
5、Documents2.1 ASTM Standards:2D 4483 Practice for Evaluating Precision 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
6、 production sample representative ofa standard production unit, 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 rubber chemicals are weighed before and afterheating at 70C.4.2
7、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 compounding materials. The testmethods may be
8、used for quality control, product acceptance,or research and development. Classification D 4676 prescribespercent volatile material as an important characteristic ofrubber antidegradants.6. Apparatus6.1 Weighing Bottle, low form, 82 cm3capacity.6.2 Explosion-proof, Vented Air Circulating Oven, capab
9、leof 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 components, and sulfur.8. Summary of
10、 Test Method8.1 The sulfur specimen is weighed before and after heatingfor2hat70C. The measured loss of mass is the volatilematerial 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 maxi
11、mum limit, it may safely be concluded thatmoisture (water) is below that limit and is not present inexcessive amounts.9.2 Testing at temperatures higher than 70C results ingreater volatilization of sulfur.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and is the direct
12、 responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Oct. 1, 2006. Published October 2006. Originallyapproved in 1986. Last previous edition approved in 2002 as D 4571 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Serv
13、ice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.10. Apparatus10.1 See Section 6.11. Procedur
14、e11.1 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 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
15、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!# 3 100 (1)where:V = volatiles, %,A = original specimen mass in grams, andB = heated specimen mass in grams.13. Report13.1 Report results obtained from two individua
16、l 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 D 4483. Refer to Practice D 4483 forterminology and other statistical details.14.2 The precision results in this precision and bias secti
17、ongive 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 documentation that they are applicable
18、 tothose particular materials and the specific testing protocols thatinclude this test method.14.3 A Type 1 (interlaboratory) precision was evaluated in1986. Both repeatability and reproducibility are short term. Aperiod of a few days separates replicate test results.Atest resultis the mean value, a
19、s 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 interlabora-tory program. These were tested in seven laboratories on twodifferent days.14.5 The results of the precision calculatio
20、ns 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 test method may be expressed inthe format of the following statements which use an “appro-priate value” of r, R,(r)or(R), th
21、at 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 closest to the mean level underconsideration at any given time, for any given material inroutine testing operations.14.7 Re
22、peatabilityThe 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 samp
23、le populations.14.8 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 given
24、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 small (close to zero). This is typical for this type ofprecision measurement process. This should be kept in mind whenever
25、 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 the limits of sensitivity ofthe test method. Under these circumstances the relative valuesbecome trivial.14.10 BiasIn test
26、 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, therefore, cannot be determined.p-PHENYLENEDIAMINE ANTIDEGRADANT15. Scope15.1 This test method describes the
27、determination of vola-tile materials in p-phenylenediamine antidegradants and isbased on the mass loss upon heating at 70C.15.2 The measured loss on heating represents volatile or-ganics plus moisture.16. Summary of Test Method16.1 The p-phenylenediamine test unit is weighed beforeand after heating
28、for3hat70C. The measured difference inmass is the volatile material.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, PercentMaterialAver-ageWithin LaboratoryABetween L
29、aboratoryASrrSRRGeneral 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 deviation.r = repeatability = 2.83
30、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.D457106217. Significance and Use17.1 The quantity of volatile material inp-phenylenediamines can affect performance o
31、f these anti-degradants in rubber if they exceed critical levels.17.2 Since the loss on heating is an empirical and nonspe-cific method, it is essential that the prescribed analysis condi-tions (sample container, oven temperature, oven air flow,cooling conditions, and so forth) be controlled so that
32、 resultsare meaningful.17.3 Prolonged heating or overheating of the sample or thetest unit can result in high heat loss values due to oxidativegeneration 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
33、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 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 theneare
34、st 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 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 th
35、e stopper andtransfer the bottle to the desiccator for a period of timesufficient for the assembly to equilibrate at room temperature.Reweigh the bottle 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
36、 %as follows:H 5 B 2 C!/B 2 A!# 3 100 (2)where:H = heating loss, %,A = mass of weighing bottle and stopper, g,B = mass of weighing bottle, stopper, and test unit beforeheating, g, andC = mass of weighing bottle, stopper, and test unit afterheating, g.22. Report22.1 Report the following information:2
37、2.1.1 Proper identification of the sample, and22.1.2 Results obtained from two individual determinationsand their average, to the nearest 0.01 %.23. Precision and Bias323.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology an
38、d other statistical details.23.2 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 test method, obtained ontwo determinations or
39、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 laboratories on twodifferent days.23.4 The results of the precision calculations for repeatabil-ity and reproducibility are given in Table 2, in as
40、cending orderof material average or level, for each of the materials evalu-ated.23.5 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 value to be used indecisions about test results (obtai
41、ned 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.23.6 RepeatabilityThe repeatability, r, of this test methodhas been estab
42、lished 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 nonidentical sample populations.23.7 ReproducibilityThe reproducibi
43、lity, 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 differe
44、nt or nonidentical samplepopulations.23.8 The relative repeatability (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.23.
45、9 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, therefore, cannot be determined.24. Keywords24.1 antidegradants; rubber compounding materials; s
46、ulfur;volatile contentTABLE 2 Volatile Materials of p-Phenylenediamine, PercentMaterialAver-ageWithin 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 ValuesB0.0
47、9 0.021 0.061 0.045 0.129ASr= 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.D4571063ASTM International ta
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