1、Designation: D 4075 06Standard Test Methods forRubber Compounding MaterialsFlame Atomic AbsorptionAnalysisDetermination of Metals1This standard is issued under the fixed designation D 4075; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, the year of 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test method
3、s cover the determination of metals inrubber compounding materials by flame atomic absorption.1.2 The test methods include the following materials:SectionsZinc oxide 11-201.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 T
4、his 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 determine the applica-bility of regulatory limitations prior to use. (For a specificwarn
5、ing statement, see 6.1.)2. Referenced Documents2.1 ASTM Standards:2D 4004 Test Methods for RubberDetermination of MetalContent by Flame Atomic Absorption (AAS) AnalysisD 4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE 300 Practi
6、ce for Sampling Industrial Chemicals2.2 Other Documents:2.2.1 Literature pertinent to the particular atomic absorptionspectrophotometric equipment used for the analysis espe-cially the manufacturers recommendations for optimumperformance. Standard texts on atomic absorption byflame technique are als
7、o helpful.3. Summary of Test Methods3.1 The compounding material is suitably sampled, pre-pared according to the appropriate sections of these testmethods, and examined by flame absorption spectrophotom-etry for metals.3.2 Sample preparation, procedures, calculations, and pre-cision statements will
8、be found in each section dealing with aparticular compounding material.3.3 The analysis of metals in compounding materials de-pends on the skill of the operator in the use of the flame atomicabsorption equipment. It is, therefore, assumed that the opera-tor is familiar with all aspects of this analy
9、tical technique. Nodetails are given here for the proper operation of the equipmentor interpretation of results obtained.3.4 These test methods do not cover the determination ofmetals in raw rubbers or finished products. See Test MethodsD 4004 for these methods.4. Significance and Use4.1 These test
10、methods are suitable for process control, forproduct acceptance, and for research and development.5. Apparatus5.1 Balances, capable of weighing accurately to 60.1 mg or60.1 g, depending on sample mass required.5.2 Hot Plate.5.3 Common Borosilicate Glassware, especially 10, 100,200 and 500-cm3volumet
11、ric flasks.5.4 Pipets, of 1, 2, 5, and 10-cm3capacity. One cubiccentimetre pipets graduated in tenths and hundredths areespecially useful.5.5 Microlitre Syringes, 1 and 10 mm3(L) are recom-mended.5.6 Plastic Bottles, suitable for storage of standard solu-tions.1These test methods are under the juris
12、diction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Oct. 1, 2006. Published October 2006. Originallyapproved in 1981. Last previous edition approved in 2002 as D 4075 02.2For referenced ASTM standards, visit the
13、 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, U
14、nited States.5.7 Atomic Absorption Spectrophotometer, operating in theflame mode. The instrument must be operated according to themanufacturers directions for optimum performance for flameoperation.6. Reagents6.1 Standard solution for metals to be determined in eachcompounding material may be prepar
15、ed from pure metals,metallic compounds, or purchased from a chemical supplyhouse as standard solutions. The usual concentrations ofsolutions is 1000 g of the metal per cubic centimetre ofsolution. Suitable dilutions with water will bring these concen-trated solutions into the linear working range of
16、 the instrument.It is recommended that standards below 1 g/cm3be preparedfresh, while those above 1 g/cm3may be stored. (WarningObserve all recognized health and safety precautions whilecarrying out this procedure. All reagents shall be of analyticalgrade, and distilled, deionized, or distilled deio
17、nized watershall be used for sample preparation and required dilutions.)7. Sampling7.1 Sampling shall be carried out in the best possible way toensure that the sample is representative of the lot (see PracticeE 300).7.2 The analyst shall select a test portion from the sample insuch a way that it is
18、as representative of the sample as possible.This sampling shall be at the discretion of the analyst.8. Calculation8.1 Calculation may be by graph, by equation, or bycalibration techniques appropriate to the atomic absorptionspectrophotometer being used.8.2 Instrument calibration methods (possible wi
19、th moremodern equipment) shall be carried out as suggested by themanufacturer.9. Report9.1 Report the metal content as a percent, if more than orequal to 0.1 % or as milligrams per kilogram, if less than0.1 %.NOTE 1Micrograms per gram, parts per million, and milligrams perkilogram are equivalent. Mi
20、crograms per gram and milligrams perkilogram are preferred in SI.10. Precision and Bias10.1 The precision statements found under each individualcompounding material were prepared in accordance withPractice D 4483. Refer to this practice for terminology andother testing statistical concept explanatio
21、ns.10.2 A test result is the average of two individual determi-nations that fall within the LSD (Least Significant Difference)limit for repeatability as stated in each precision section.ZINC OXIDE11. Scope11.1 This test method covers the analysis of zinc oxide forcopper, cadmium, lead, and manganese
22、.11.2 Any zinc oxide, suitable for rubber compounding, maybe analyzed by this procedure.11.3 This test method is not suitable for zinc oxide with leadcontent above about 1.0 % because of dissolution problems.12. Summary of Test Method12.1 A “slurry” of zinc oxide and water is heated with HCl,to whic
23、h a small amount of HNO3is added. The metal soughtis determined by flame atomic absorption.13. Significance and Use13.1 The principal reason for analysis of zinc oxide forcopper, cadmium, manganese and lead is for quality assurance,but this test method may be used for other purposes, such asresearch
24、, process control, etc.14. Apparatus14.1 See Section 5.15. Reagents15.1 See Section 6, and in addition:15.2 Hydrochloric Acid (HCl), concentrated,15.3 Nitric Acid (HNO3), concentrated.16. Sampling16.1 See Section 7.17. Procedure17.1 Accurately weigh a 0.2 to 10.0-g sample. Weigh to0.1 mg for small s
25、amples and 2 6 0.1 g for large samples intoa 150-cm3beaker. Add enough water to make a thick “slurry.”Add enough concentrated HCl to effect complete dissolution ofthe test portion. For small test portions, 10 cm3will suffice, forlarger test portions, up to 30 cm3may be needed.NOTE 2Failure to observ
26、e this sequence will result in a hard cake ofzinc oxide, which will be difficult to dissolve in the wateracid mixture.17.2 Heat the solution on a hot plate to the boiling point,then add 1 to 2 cm3of concentrated HNO3. Continue heatingfor no more than 5 min. Remove the beaker from the hot plate,allow
27、 it to cool and quantitatively transfer the solution to a200-cm3volumetric flask making it up to volume with water.NOTE 3Variations in the amount of test portion to weigh and finalvolume of solution is left to the discretion of the analyst and must bedetermined by prior knowledge of the approximate
28、amount of copper,cadmium, and lead in the type of zinc oxide being analyzed.17.3 Carry a blank throughout the entire procedure, usingthe same quantities of reagents but without a test portion.Subtract any positive blank value, in an appropriate manner,before calculating the metal content of the zinc
29、 oxide.17.4 Complete the analysis, using standard flame atomicabsorption techniques appropriate to the instrument used andfollowing the manufacturers directions for optimum instru-ment performance.NOTE 4Zinc oxide solution for measurement must fall within thelinear range of the instrument. Any solut
30、ion that does not meet thiscriterion must be diluted suitably to fall within this range.D407506218. Calculation18.1 See Section 8.19. Report19.1 See Section 9.20. Precision and Bias320.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Refer to Practice D 4483 for
31、terminology and other statistical calculation details.20.2 A Type 1 (interlaboratory) precision was evaluated.Both repeatability and reproducibility are short term, a periodof a few days separates replicate test results. A test result is theaverage value, as specified by this test method, obtained o
32、n twodeterminations or measurements of the property or parameterin question.20.3 Table 1 gives the details on the interlaboratory testing;materials (types of zinc oxide), number of laboratories, numberof testing days.20.4 The results of the precision calculations for repeatabil-ity and reproducibili
33、ty are given in Table 2.20.5 The precision of this test method for any analysis maybe expressed in the format of the following statements whichuse what is called an “appropriate value” of r, R, (r), or (R), thatis, that value to be used in decisions about test results (obtainedwith this test method)
34、. The appropriate value is that value of ror R associated with a mean level in Table 2 closest to the meanlevel under consideration at any given time, for any givenmaterial in routine testing operations.20.6 RepeatabilityThe repeatability, r, of this test methodhas been established as the appropriat
35、e value tabulated in Table2. Two single test results, obtained under normal test methodprocedures, that differ by more than this tabulated r (for anygiven level) must be considered as derived from different ornonidentical sample populations.20.7 ReproducibilityThe reproducibility, R, of this testmet
36、hod has been established as the appropriate value for anyparameter tabulated in Table 2. Two single test results obtainedin two different laboratories, under normal test method proce-dures, that differ by more than the tabulated R (for any givenlevel) must be considered to have come from different o
37、rnonidentical sample populations.20.8 Repeatability and reproducibility expressed as a per-centage of the mean level, (r) and (R), have equivalentapplication statements as above for r and R. For the (r) and (R)statements, the difference in the two single test results isexpressed as a percentage of t
38、he arithmetic mean of the two testresults.20.9 BiasIn test method terminology, bias is the differ-ence between an average test value and the reference (or true)test property value. Reference values do not exist for this testmethod since the value (of the test property) is exclusivelydefined by the t
39、est method. Bias, therefore, cannot be deter-mined.21. Keywords21.1 atomic absorption analysis; metals; zinc oxide3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D11-1019.TABLE 1 Details on Interlaboratory Precision Test Progra
40、msAnalysisNumber ofLaboratoriesTypes ofZnO(Tested)Numberof DaysCopper in ZnO 8 1 3Cadmium in ZnO 8 2 3Manganese in ZnO 8 1 3Lead in ZnO 8 2 3D4075063ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
41、 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 reviewed every f
42、ive 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 technical
43、 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,
44、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).TABLE 2 Type 1Precision for Copp
45、er, Cadmium, Manganese, and Lead in Zinc OxideNOTESr= within laboratory standard deviation.r = repeatability (in measurement units).(r) = repeatability (in percent).SR= between laboratory standard deviation.R = reproducibility (in measurement units).(R) = reproducibility (in percent).(ZnO)MaterialAn
46、alysis For(mg/kg)Mean ValueWithin Laboratories Between LaboratoriesSrr (r) SRR (R)1 copper 6.5 0.456 1.29 19.9 0.930 2.63 40.51 cadmium 1.9 1.07 3.03 159.0 1.41 3.99 210.02 cadmium 236.0 5.32 15.1 6.40 27.4 77.5 32.91 manganese 41.0 1.19 3.37 8.22 5.38 15.2 37.11 lead 12.0 0.70 1.98 16.5 1.81 5.12 42.72 lead 932.0 9.42 26.7 2.86 63.0 178.0 19.1D4075064
