1、Designation: D4075 06 (Reapproved 2012)Standard Test Methods forRubber Compounding MaterialsFlame Atomic AbsorptionAnalysisDetermination of Metals1This standard is issued under the fixed designation D4075; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 the 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 Th
3、ese test methods 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 thi
4、sstandard.1.4 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 determine the applica-bility of regulatory limitations prior to use. (For
5、 a specificwarning statement, see 6.1.)2. Referenced Documents2.1 ASTM Standards:2D4004 Test Methods for RubberDetermination of MetalContent by Flame Atomic Absorption (AAS) AnalysisD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustrie
6、sE300 Practice 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 techn
7、ique are also 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 stat
8、ements will 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 o
9、f this analytical 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 MethodsD4004 for these methods.4. Significance and Use4.1
10、These test 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
11、-cm3volumetric 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 unde
12、r the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved May 1, 2012. Published June 2012. Originallyapproved in 1981. Last previous edition approved in 2006 as D4075 06. DOI:10.1520/D4075-06R12.2For refer
13、enced 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
14、 Conshohocken, PA 19428-2959, United 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 eachcom
15、pounding material may be prepared 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 i
16、nto the linear working range of 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 distille
17、d, deionized, or distilled deionized 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 PracticeE300).7.2 The analyst shall select a test portion from the s
18、ample insuch a way that it is 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 ca
19、libration methods (possible with 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
20、perkilogram are equivalent. Micrograms 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 D4483. Refer to this practice for terminology andother testing s
21、tatistical concept explanations.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,
22、 cadmium, lead, and manganese.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 wat
23、er is heated with HCl,to which 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 ot
24、her purposes, such asresearch, 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 sampl
25、e. Weigh to0.1 mg for small samples 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 n
26、eeded.NOTE 2Failure to observe 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 be
27、aker from the hot plate,allow 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
28、knowledge of the approximate 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
29、the metal content of the zinc 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
30、 of the instrument. Any solution that does not meet thiscriterion must be diluted suitably to fall within this range.D4075 06 (2012)218. 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
31、 D4483. Refer to Practice D4483 forterminology 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 specif
32、ied by this test method, obtained on 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 f
33、or repeatabil-ity and reproducibility 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 resu
34、lts (obtainedwith this test method). 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
35、 been established as the appropriate 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
36、reproducibility, R, of this testmethod 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 consi
37、dered to have come from different ornonidentical 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 resul
38、ts isexpressed as a percentage of the 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 prope
39、rty) is exclusivelydefined by the test 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 Int
40、erlaboratory Precision Test ProgramsAnalysisNumber ofLaboratoriesTypes ofZnO(Tested)Numberof DaysCopper in ZnO 8 1 3Cadmium in ZnO 8 2 3Manganese in ZnO 8 1 3Lead in ZnO 8 2 3D4075 06 (2012)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with
41、 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 standard is subject to revision at any time by the responsible techni
42、cal 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 International Headquarters. Your comments will receive careful consideratio
43、n 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 below.This standard is copyrighted by ASTM International, 100 Barr Harb
44、or 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.
45、astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 2 Type 1Precision for Copper, Cadmium, Manganese, and Lead in Zinc OxideNOTESr= within laboratory standard deviation.r = repeatability (in measurement units).(r) = repeata
46、bility (in percent).SR= between laboratory standard deviation.R = reproducibility (in measurement units).(R) = reproducibility (in percent).(ZnO)MaterialAnalysis 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 19.1D4075 06 (2012)4
