1、Designation: D 5054 90 (Reapproved 2009)Standard Test Method forRubber ChemicalsDiphenyl Guanidine (DPG) and Di-o-tolyl-guanidine (DOTG) Assay1This standard is issued under the fixed designation D 5054; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e case of revision, 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 assay ofdiphenyl guanidine (DPG) and di-o
3、-tolyl-guanidine (DOTG).It is based on a visual titration of DPG or DOTG withhydrochloric acid (HCl).1.2 The assay is determined as mass percent.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purp
4、ort 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 Documents2.1 ASTM Standards:2D 1
5、193 Specification for Reagent WaterD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 DPG or DOTG is dissolved in methanol and titratedwith HCl solution using bromophenol blue indicator.4. Significance
6、and Use4.1 DPG and DOTG are used for rubber and latex vulcani-zation acceleration. The amount of DPG or DOTG may be ofimportance in predicting performance in rubber compoundsand for raw material purchase and control.4.2 This test method may be used as a quality control tooland for research and devel
7、opment work.5. Interferences5.1 Alkaline contaminants that are titratable with HCl inter-fere with the results.6. Apparatus6.1 Erlenmeyer Flask, 200-cm3.6.2 Graduated Cylinder, 25-cm3.6.3 Magnetic Stirrer.6.4 Analytical Balance, having a sensitivity of 60.1 mg.6.5 Buret, 50-cm3capacity.7. Reagents a
8、nd Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Othe
9、r grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Types I,
10、II, or III of Specification D 1193.7.3 Methanol, analytical reagent.7.4 Hydrochloric Acid (HCl) (0.1 N).7.5 Bromophenol Blue Indicator Solution (0.4 g/cm3)Dissolve 0.4 g bromophenol blue in 1000 cm3methanol.8. Sampling8.1 Depending upon the purpose of the testing, samplingshall be at the discretion
11、of the analyst to obtain as represen-tative a sample as possible of the lot to be tested.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, 2009. Published September
12、2009. Originallyapproved in 1990. Last previous edition approved in 2004 as D 5054 90 (2004)1.2For referenced 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
13、 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 Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K.,
14、 and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.9. Procedure9.1 Accurately weigh about 1.0 g of the test specimen to
15、thenearest 0.1 mg and carefully transfer it to a 200-cm3Erlenm-eyer flask.9.2 Using a graduated cylinder, dissolve the specimen byadding 25 cm3of methanol.9.3 With stirring, add 5 drops of bromophenol blue indicatorsolution.9.4 Titrate with 0.1 N HCl solution. The color change at theend point is fro
16、m blue-violet to green.10. Calculation10.1 Calculate the percent DPG, A, as follows:A 5V 3 N 3 0.2112W3 100 (1)where:V = volume of 0.1 N HCl used, for titration of thesample, cm3,N = normality of the HCl solution,W = sample used, g, and0.2112 = millimole mass of DPG.10.2 Calculate the percent DOTG,
17、B, as follows:B 5V 3 N 3 0.2393W3 100 (2)where:0.2393 = millimole mass of DOTG.11. Report11.1 Report the following information:11.1.1 Proper identification of the sample, and11.1.2 Results obtained from the two individual determina-tions and their average, reported to the nearest 0.1 %.12. Precision
18、 and Bias12.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 forterminology and other statistical calculation details.12.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with
19、 thematerials used in the particular interlaboratory programs asdescribed in this section. The precision parameters should notbe used for acceptance or rejection testing of any group ofmaterials without documentation that they are applicable tothose particular materials and the specific testing prot
20、ocols thatinclude this test method.12.3 A Type 1 (interlaboratory) precision was evaluated in1988. 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, of the assayresults.12.4 A
21、 DPG sample and a DOTG sample were analyzed inten laboratories on two different days.12.5 The results of the precision calculations for repeatabil-ity and reproducibility are given in Table 1.12.6 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriate value in
22、Table 1.Twosingle test results, obtained under normal test method proce-dures, that differ by more than the tabulated r (for any givenlevel) must be considered as derived from different or noniden-tical sample populations.12.7 ReproducibilityThe reproducibility, R, of this testmethod has been establ
23、ished as the appropriate value in Table1. Two single test results obtained in two different laboratories,under normal test method procedures, that differ by more thanthe tabulated R (for any given level) must be considered tohave come from different or nonidentical sample populations.12.8 Repeatabil
24、ity 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.12.9 BiasI
25、n 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.12.10 The full details and test results of the interlaboratorytest prog
26、ram used for this precision section are complete and inthe process of being prepared in the proper format forsubmission as a research report to ASTM Headquarters.13. Keywords13.1 di-o-tolyl-guanidine (DOTG); diphenyl guanidine(DPG)TABLE 1 DPG/DOTG Assay, %Mate-rialAverageWithin LaboratoryABetween La
27、boratoriesASrr (r) SRR (R)DPGDOTG98.2097.160.2070.1410.5860.3990.5970.4110.5670.6391.6051.8091.641.86ASr= repeatability standard deviation.r = repeatability = 2.83 times the square root of the repeatability variance.(r) = repeatability (as percent material average).SR= reproducibility standard devia
28、tion.R = reproducibility = 2.83 times the square root of the reproducibility variance.(R) = reproducibility (as percent of material average).D 5054 90 (2009)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standa
29、rd. 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 standard is subject to revision at any time by the responsible technical committee and must be reviewe
30、d 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 International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible
31、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 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 5054 90 (2009)3
