1、Designation: D297 13D297 15Standard Test Methods forRubber ProductsChemical Analysis1This standard is issued under the fixed designation D297; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 These test methods cover the qualitative and quantitative an
3、alysis of the composition of rubber products of the “R” family(see 3.1). Many of these test methods may be applied to the analysis of natural and synthetic crude rubbers.1.1.1 Part A consists of general test methods for use in the determination of some or all of the major constituents of a rubberpro
4、duct.1.1.2 Part B covers the determination of specific polymers present in a rubber product.1.1.3 The test methods appear in the following order:Part A. General Test Methods: SectionsRubber Polymer Content by the Indirect Method 11 13Determinations and Report for the General Method 14 and 15Density
5、16Extract Analysis 17 26Sulfur Analysis 27 33Fillers Analysis 34 40Ash Analysis 41 51Part B. Determination of Rubber Polymers 52 581.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.1.3 This standard does not purport to address
6、all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific precautionary or warning statements are given in 31.4
7、.5, 31.6, 37.4.2, 38.4.2, 45.1.3, 53.2.3.5,54.4.2, 54.6, 56.5.3, and 57.7.3; and X1.3.3 and X2.4.1.6.2. Referenced Documents2.1 ASTM Standards:2D982 Test Method for Organic Nitrogen in Paper and PaperboardD1416 Test Methods for Rubber from Synthetic SourcesChemical Analysis (Withdrawn 1996)3D1418 Pr
8、actice for Rubber and Rubber LaticesNomenclatureD1646 Test Methods for RubberViscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)D3040 Practice for Preparing Precision Statements for Standards Related to Rubber and Rubber Testing (Withdrawn 1987)3D3156 Practice for
9、 RubberChromatographic Analysis of Antidegradants (Antioxidants, Antiozonants and Stabilizers)D3452 Practice for RubberIdentification by Pyrolysis-Gas ChromatographyD3677 Test Methods for RubberIdentification by Infrared SpectrophotometryD4483 Practice for Evaluating Precision for Test Method Standa
10、rds in the Rubber and Carbon Black Manufacturing IndustriesE11 Specification for Woven Wire Test Sieve Cloth and Test SievesE131 Terminology Relating to Molecular SpectroscopyE200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical AnalysisE442 Test
11、Method for Chlorine, Bromine, or Iodine in Organic Compounds by Oxygen Flask Combustion (Withdrawn 1996)3E443 Test Method for Sulfur in Organic Compounds by Oxygen Flask Combustion (Withdrawn 1996)31 These test methods are under the jurisdiction of ASTM Committee D11 on Rubber and are the direct res
12、ponsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved May 1, 2013July 1, 2015. Published May 2013August 2015. Originally approved in 1928. Last previous edition approved in 20062013 asD297 93 (2006).D297 13. DOI: 10.1520/D0297-13.10.1520/D0297-15.2 For referencedASTM stand
13、ards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.T
14、his document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior edit
15、ions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsThe nomenclature and
16、 abbreviations used for natural and synthetic rubbers are in accordance with PracticeD1418.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytic
17、al Reagents of the American Chemical Society, wheresuch specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.4.2 Purity of WaterUnless otherwise i
18、ndicated, references to water shall be understood to mean distilled water or water ofequal purity.5. Concentration of Reagents5.1 Concentrated Acids and Ammonium HydroxideWhen acids and ammonium hydroxide are specified by name or chemicalformula only, it is understood that concentrated reagents of t
19、he following densities or concentrations are intended:Density,Mg/m3Acetic acid, HC2H3O2 (99.7 %) 1.05Formic acid, HCOOH 1.22Hydrochloric acid, HCl 1.19Hydrofluoric acid, HF (49 %) 1.16Nitric acid, HNO3 1.42Phosphoric acid, H3PO4 (85 %) 1.70Sulfuric acid, H2SO4 1.84Ammonium hydroxide, NH4OH 0.90The d
20、esired densities or concentrations of all other concentrated acids are stated whenever they are specified.5.2 Diluted Acids and Ammonium HydroxideConcentrations of diluted acids and ammonium hydroxide, except whenstandardized, are specified as a ratio stating the number of volumes of the concentrate
21、d reagent to be added to a given number ofvolumes of water, as in the following example: HCl (1 + 9) means 1 volume of concentrated HCl (density 1.19) mixed with 9volumes of water. Acids shall be added to water slowly, with stirring.5.3 Standard SolutionsConcentrations of standard solutions are expr
22、essed as normalities or as volume of solution that reactswith or contains a given mass of material being used or determined, for example: 0.1 N Na2S2O3 solution, or CuSO4 solution (1cm3 = 0.001 g Cu).5.4 Nonstandardized SolutionsConcentrations of nonstandardized solutions prepared by dissolving a gi
23、ven mass in a solventare specified in grams of the reagent (as weighted out)/dm3 of solution, and it is understood that water is the solvent unlessotherwise specified, for example: NaOH (10 g/dm3) means 10 g of NaOH dissolved in water and diluted with water to 1 dm3 (Note1). In the case of certain r
24、eagents the concentration may be specified as a percentage by mass, for example: ethanol (50 %) meansa solution containing 50 g of ethanol per 100 g of solution. Other nonstandardized solutions may be specified by name only, andthe concentration of such solutions will be governed by the instructions
25、 for their preparation.NOTE 1Whenever a hydrated salt is used in the preparation of a reagent (for example, BaCl22H2O) the preparation of the reagent is described indetail. When an anhydrous salt is used in preparing a simple aqueous solution the reagent is listed by title only and details of the pr
26、eparation are not given.PART A. GENERAL TEST METHODS6. Scope and Application6.1 The general test methods described cover the analysis of many types of rubber products to determine the amount and typeof nonrubber constituents and to calculate indirectly from these data the amount of rubber constituen
27、t.6.2 The applications and limitations of the test methods to analysis of specific types of rubber products are given in the scopesof the various test methods. Application to types of rubber products not specified in the scope of a particular test method shall beverified by application to a control
28、of known and similar composition.4 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U
29、.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.D297 1526.3 Special test methods for analysis are given for rubber products containing glue, free carbon, antimony, lead, mineral oil,waxy hydrocarbons, and barium carbonate.6.4
30、For the determination of the amount of a rubber polymer present in a rubber product, an indirect test method is given bywhich the nonrubber constituents are determined individually or in groups, and the rubber polymer content is determined bydifference (Sections 11 13). If, in using this test method
31、, fillers are determined by the ashing test method (Section 35 or 36),satisfactory results will be obtained, except where there are found to be present decomposable compounding ingredients such ascarbonates that decompose at 550C, clay, asbestine, talc, hydrated silica, antimony sulfide, halogen-con
32、taining components, andsilicone polymers. No test method of filler determination herein described will give accurate results in the presence of clay, silica,talc, or any other hydrated filler unless a correction can be made for losses of water of hydration on ashing. This correction canbe made only
33、if the nature and quantity of these fillers are known. The indirect test method will not give accurate results in thepresence of halogen-containing components or silicone rubber. In the presence of antimony sulfide or carbonates decomposing at550C, but in the absence of the above interfering constit
34、uents, approximate correction can be made by means of determinationof total antimony (Section 50) or of the metal associated with the decomposable carbonate (usually calcium, Section 45) or (Section49) and calculation of the original composition of the compounding ingredient from these data.6.5 If f
35、actice or high percentages of mineral rubber are present, no accurate test method is known for determination of rubbercontent or for complete analysis of the rubber product.6.6 For the determination of the rubber content of hard rubber products, no accurate test method is described herein if fillers
36、decomposable at 550C are present.7. Blank Determinations7.1 Blanks shall be run on all determinations to check the purity of the materials used and deductions shall be made accordingly.8. Check Analyses8.1 Duplicate determinations shall be made and shall check within the limits specified in the test
37、 method, when these are stated.9. Preparation of Samples9.1 Before preparing a sample for analysis, the analyst shall, by inspection, assure himself that it has not been contaminated.The sample to be analyzed shall be selected by taking pieces from various parts of the original sample and separating
38、 them fromforeign matter. Because of the variety of rubber products to which this test method can be applied, no single procedure for reducingthe sample to the required fineness is applicable to all samples. Therefore, several alternative procedures for this purpose aredescribed in 9.2 to 9.7. The a
39、nalyst is expected to select the one most suitable to the sample that he is analyzing and the equipmentavailable.9.2 For vulcanized soft rubber, unvulcanized rubber, crude rubber, and many samples of reclaimed rubber, it is preferable to mixthe sample and grind it by passing it two or three times th
40、rough a clean, cold, laboratory rubber mill. The rubber will come fromthe mill in the form of a coarse powder or a rough sheet. If the product is in the form of a sheet, the adjustment of the mill shallbe such that the thickness of the final sheet is no greater than 0.5 mm. If the sample is sticky,
41、it shall be rolled in a liner materialthat will not adhere to or contaminate the sample. If the milled sample is a powder, it shall be transferred to a No. 14 (1.40-mm)sieve5 and rubbed through the sieve. Grinding shall be continued until the entire sample passes through the sieve.9.3 In the absence
42、 of milling machinery, the sample may be prepared by cutting it with scissors so that it will pass a No. 14(1.40-mm) sieve.6,7 The sample may be cut into long strips that are fine enough to pass freely through the sieve and the strips fedthrough by hand, or the sample may be cut into small fragments
43、 and shaken through the sieve. The cutting shall be continued untilthe entire sample passes through the sieve. If necessary, to prevent sticking, different fragments of the sieved sample may besegregated by wrapping in a liner material that will not adhere to or contaminate the sample.9.4 Certain ve
44、ry glutinous samples may be prepared for extraction analysis as follows: Place a weighed 2-g sample of thematerial between two pieces of ashless filter paper that has been extracted in accordance with Section 21. The papers should beapproximately 500 by 100 mm (20 by 4 in.) and the sample should be
45、placed near one end. Flatten the sample and spread itthroughout the length of the filter paper by passing the “sandwich” lengthwise, through a cold, closely set, even-speed rubbercalender.The gross thickness of the resulting sheet should not be greater than 1.0 mm. If a rubber calender is not availa
46、ble, a similarsheet may be obtained by placing the sample in a hydraulic press or a vise. In the latter case, the sample may be roughly spreadby hand throughout the length of the filter paper and pressure applied to small areas at a time until the whole sample has beenflattened.5 Detailed requiremen
47、ts for these sieves are given in Specification E11.6 The sole source of supply of compressed volume densimeters known to the committee at this time is C. W. Brabender Instruments, Inc., 50 E. Wesley St., SouthHackensack, NJ 07606.7 If you are aware of alternative suppliers, please provide this infor
48、mation to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.D297 1539.5 Samples of rubberized cloth, whose overall thickness is no greater than 1.0 mm, may be prepared for analysis by cuttingthe
49、m into pieces 1.5 mm square and then mixing well. If the fabric is easily removed, it should be separated, unless an analysisof the whole cloth is desired.9.6 Samples of rubber cements shall be evaporated to dryness in a vacuum oven at a temperature not higher than 30C. Theresidue may then be analyzed as an unvulcanized sample.Aseparate sample of the cement shall be distilled under reduced pressureif examination of the solvent is desired.9.7 Samples of hard rubber shall be reduced to powder form by filing, cleaned with a magnet, and sieved thr
