1、Designation: D 4573 03Standard 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 revision, the year o
2、f last 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 This test method covers the determination of the amountof hydrocarbon oils added to oil-treated sulfurs. The testme
3、thod is employed when the amount of oil added is 1 % ormore of the total sample.1.2 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 det
4、ermine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black Industries23. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 lot samplea p
5、roduction sample representative of astandard production unit, normally referred to as “the sample.”3.1.2 specimenalso known as the “test portion;” 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 hydroc
6、arbon oils addedto sulfur to help control dusting of the sulfur. It can be used forresearch, development, and quality control to measure the levelof oil added to the sulfur to help maintain the oil content atrequired levels.5. Apparatus5.1 Filtering Crucible,30cm3, medium porosity sinteredglass.5.2
7、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 Analytical 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
8、tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficient
9、lyhigh 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 Saturated With Sulfur:6.3.1 Method of PreparationIn a well-ventilated hood, ina suitable size container equipped with an air stirrer andexternal heater,
10、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. Decant 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
11、 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 disperse the sul
12、fur 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)1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibi
13、lity of Subcommittee D11.11 on Chemical Analysis.Current edition approved June 10, 2003. Published June 2003. Originallyapproved in 1986. Last previous edition approved in 1998 as D 4573 98.2Annual Book of ASTM Standards, Vol 09.01.3Reagent Chemicals, American Chemical Society Specifications, Americ
14、anChemical 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. (USPC
15、), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.adjusting the suction to pull the filtrate through the filtercrucible at a rate forming drops and not a steady stream offiltrate.7.5 Wash the residue in the flask with t
16、hree 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 filtration is complete, increase the suction to pullthe la
17、st 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) at 70 6 2C for 1 h. Then transfer the filtercrucible to a dessictor for 0.5 to 1 h.7.8 Remove the filter
18、crucible from the dessicator and weighit 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 the oil-treatedsulfur sample as follows:% Oil 5 1 2
19、 W2/ W11 C!# 3 100 (1)Cf5 1 2B2B1(2)where:W1= mass of oil treated sulfur sample (see 7.2) in g,W2= mass of oil treated sulfur sample after filtration (see7.8) in g,B1= mass of pure sulfur “blank” in g,B2= mass of pure sulfur “blank” after filtration in g, andCf= correction factor for “blank.”NOTE 2C
20、fmay 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 This precision and bias section has been prepar
21、ed 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 in the particular interlaboratory pro-grams as
22、 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 method.10.3 A Type 1 (interlaboratory) precision
23、 was evaluated in1986. Both repeatability and reproducibility are short term; aperiod of a few days separates replicate test results. A test resultis the mean value, as specified by this method, obtained on twodeterminations or measurements of the property or parameterin question.10.4 Two different
24、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 or level, for each of the materials evalu-
25、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 appropriate value is that value of r or R ass
26、ociated 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 tabulated in thePrecision Table. Two single
27、 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 established as the appropr
28、iate value tabulated4Supporting 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 % InsolubleSul
29、furB17.84 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 roo
30、t of 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.D4573032in Table 1. T
31、wo 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 Repeatability and reproducibility expressed as a per-c
32、ent 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.10.10 BiasIn test method terminology, bias is the diffe
33、r-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 chemicals; sulfurASTM International takes no position resp
34、ecting 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 rights, are entirely their own responsibility.This s
35、tandard 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 additional standardsand should be addressed to ASTM Interna
36、tional Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown bel
37、ow.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).D4573033
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