1、Designation: D4573 03 (Reapproved 2014)Standard Test Method forRubber ChemicalsDetermination of Oil Content in Oil-Treated Sulfur1This standard is issued under the fixed designation D4573; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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 This test method covers the determination of the amountof hydrocarbon oils added to oil-treated sulf
3、urs. The testmethod is employed when the amount of oil added is 1 % ormore of the total sample.1.2 The values 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,
4、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:2D4483 Practice for Evaluating Precision for Test Meth
5、odStandards in the Rubber and Carbon Black ManufacturingIndustries3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 lot samplea production sample representative of astandard production unit, normally referred to as “the sample.”3.1.2 specimenalso known as the “test portion;” it
6、is theactual material used in the analysis; it must be representative ofthe lot sample.4. Significance and Use4.1 This test method measures the hydrocarbon oils addedto sulfur to help control dusting of the sulfur. It can be used forresearch, development, and quality control to measure the levelof o
7、il added to the sulfur to help maintain the oil content atrequired levels.5. Apparatus5.1 Filtering Crucible, 30 cm3, medium porosity sinteredglass.5.2 Vacuum Filter Flask, 500 cm3and filter crucible holder.5.3 Circulating Air Oven, capable of 70 6 2C explosionproof, vented.5.4 Desiccator.5.5 Analyt
8、ical Balance, sensitive to 0.001 g.5.6 Conical (Erlenmeyer) Flask, 250 cm3.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the Ameri
9、can Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Fine Particle Size Pure Sulfur (45 m or smaller).6.3 Hexane S
10、aturated With Sulfur:6.3.1 Method of PreparationIn a well-ventilated hood, ina suitable size container equipped with an air stirrer andexternal heater, mix hexane and sulfur for 2 h while heating to40C maximum. Continue to stir while the mixture cools toroom temperature. Allow to settle for 12 h. De
11、cant off thesulfur saturated hexane, and filter just prior to use in the test.Store in a capped bottle.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved July 1, 2014. Publis
12、hed November 2014. Originallyapproved in 1986. Last previous edition approved in 2009 as D4573 03 (2009).DOI: 10.1520/D4573-03R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informat
13、ion, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemi
14、cals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Procedure7.1 Tare a 30 cm3filt
15、er crucible (see 5.1) to the nearest0.001 g.7.2 Into a 250 cm3conical flask (see 5.6) weigh, to thenearest 0.001 g, 5 6 0.5g(W1) of the oil-treated sulfurspecimen.7.3 In a well-ventilated hood, add 20 cm3of the freshlyfiltered sulfur-saturated hexane (see 6.3) to the flask. Gentlyswirl the flask to
16、disperse the sulfur specimen.7.4 Vacuum filter this mixture quantitatively through thepreviously tared filter crucible (see 5.1), contained in the filtercrucible holder, into a 500 cm3vacuum filter flask (see 5.2)adjusting the suction to pull the filtrate through the filtercrucible at a rate forming
17、 drops and not a steady stream offiltrate.7.5 Wash the residue in the flask with three successive 50cm3of sulfur-saturated hexane, quantitatively transferring eachwashing through the filter crucible.NOTE 1Filtration should take 8 to 15 min to complete. Do not allowthe filter cake to dry or crack dur
18、ing filtration.7.6 When filtration is complete, increase the suction to pullthe last traces of filtrate through the filter cake, leaving thevacuum on for 30 s after the last drop of filtrate falls.7.7 Remove the filter crucible from the holder and place it inan oven (see 5.3)at706 2C for 1 h. Then t
19、ransfer the filtercrucible to a desiccator for 0.5 to 1 h.7.8 Remove the filter crucible from the desiccator andweigh it to the nearest 0.001 g (W2).7.9 Repeat steps 7.1 7.8 on a 5.0 6 0.5 g sample of puresulfur as a blank (B1). The weight of the “blank” residue is(B2).8. Calculation8.1 Calculate th
20、e percent oil extracted from the oil-treatedsulfur sample as follows:% Oil 5 1 2 W2/W11C!# 3100 (1)Cf5 1 2B2B1(2)where:W1= mass of oil treated sulfur sample (see 7.2)ing,W2= mass of oil treated sulfur sample after filtration (see7.8)ing,B1= mass of pure sulfur “blank” in g,B2= mass of pure sulfur “b
21、lank” after filtration in g, andCf= correction factor for “blank.”NOTE 2Cfmay be positive or negative.9. Report9.1 Report the following information:9.1.1 Proper identification of samples, and9.1.2 Percent of extracted oil from two individual determi-nations and their average to the nearest 0.01 %.10
22、. Precision and Bias410.1 This precision and bias section has been prepared inaccordance with Practice D4483. Refer to this practice forterminology and other statistical details.10.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with th
23、ematerials (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 materials and the specific testing protocol
24、s thatinclude this test method.10.3 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, as specified by this method, obtained on twodeterminations or me
25、asurements of the property or parameterin question.10.4 Two different materials were used in the interlabora-tory program. These were tested in six laboratories on twodifferent days.10.5 The results of the precision calculations for repeatabil-ity and reproducibility are given in Table 1, in ascendi
26、ng orderof material average or level, for each of the materials evalu-ated.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1049.TABLE 1 Type 1 Precision ResultsOil Content (Sulfur)Material AverageWithin LaboratoryABetween La
27、boratoryASrr (r) SRR (R)Oil Treated, 90 % InsolubleSulfurB17.84 0.175 0.496 2.78 1.081 3.060 17.1Oil Treated, 90 % InsolubleSulfurA20.32 0.247 0.699 3.44 0.360 1.020 5.0Pooled ValuesB18.97 0.211 0.597 3.14 0.806 2.281 12.0ASr= repeatability standard deviation.r = reproducibility (as a percent of mat
28、erial average).= repeatability = 2.83 the square root of the repeatability variance.(r) = repeatability (as a percent of material average).SR= reproducibility standard deviation.R = reproducibility = 2.83 the square root of the reproducibility variance.(R) = reproducibility (as a percent of material
29、 average).BNo values omitted.D4573 03 (2014)210.6 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 value to be used indecisions about test results (obtained with the test method).The appro
30、priate 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.10.7 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value tab
31、ulated in thePrecision Table. Two single test results, obtained under normaltest method procedures, that differ by more than this tabulatedr (for any given level) must be considered as derived fromdifferent or nonidentical sample populations.10.8 ReproducibilityThe reproducibility, R, of this testme
32、thod 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 level) must beconsidered to have come from different or nonidentical samp
33、lepopulations.10.9 Repeatability and reproducibility expressed as a per-cent of the mean level, (r) and (R), have equivalent applicationstatements as above for r and R. For the (r) and (R) statements,the difference in the two single test results is expressed as apercent of the arithmetic mean of the
34、 two test results.10.10 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, therefore, cannot be determined.11. Keywords11.1 oil content; oil-treated
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