1、Designation: D 4573 03 (Reapproved 2009)Standard Test Method forRubber ChemicalsDetermination of Oil Content in Oil-Treated Sulfur1This standard is issued under the fixed designation D 4573; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 su
3、lfurs. 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:2D 4483 Practice for Evaluating Precision for Test M
5、ethodStandards 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;”
6、it 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 levelo
7、f oil added to the sulfur to help maintain the oil content atrequired levels.5. Apparatus5.1 Filtering Crucible,30cm3, 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 Analy
8、tical 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 Amer
9、ican 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
10、Saturated 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. D
11、ecant off thesulfur saturated hexane, and filter just prior to use in the test.Store in a capped bottle.7. Procedure7.1 Tare a 30 cm3filter 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.
12、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 Jan. 1, 2009. Published March 2009. Originallyapproved in 1986. Last previous edition approved in 2003 as D 4573 03.2For re
13、ferenced 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 Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications , Ameri
14、canChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USP
15、C), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 disperse the sulfur specimen.7.
16、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 drops and not a steady stream
17、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 during filtration.7.6 When filtrat
18、ion 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 transfer the filtercrucible to a
19、 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 the percent oil extracted from th
20、e oil-treatedsulfur sample as follows:% Oil 5 1 2 W2/ W11 C!# 3 100 (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 “blank” after filtration in g,
21、 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. Precision and Bias410.1 Th
22、is precision and bias section has been prepared inaccordance with Practice D 4483. 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 thematerials (rubbers) used i
23、n 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 protocols thatinclude this test met
24、hod.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 measurements of the property
25、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 ascending orderof material average
26、 or level, for each of the materials evalu-ated.10.6 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 ap
27、propriate 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
28、tabulated in the4Supporting 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 LaboratoryASrr (r) SRR (R)Oil Treated, 90 % InsolubleSulfurB
29、17.84 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 material average).= repeatability = 2.83 3 the square root of
30、 the repeatability variance.(r) = repeatability (as a percent of material average).SR= reproducibility standard deviation.R = reproducibility = 2.83 3 the square root of the reproducibility variance.(R) = reproducibility (as a percent of material average).BNo values omitted.D 4573 03 (2009)2Precisio
31、n 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 testmethod has been establi
32、shed 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 samplepopulations.10.9 Re
33、peatability 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 two test results.10.
34、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 sulfur; rubber chemic
35、als; 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
36、rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additio
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38、STM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4573 03 (2009)3
