1、Designation: D4075 06 (Reapproved 2017)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 U.S. Department of Defense.1. Scope1
3、.1 These 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 11201.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in
4、 thisstandard.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.
5、(For a specificwarning statement, see 6.1.)1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the Wo
6、rld Trade Organization TechnicalBarriers to Trade (TBT) Committee.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 B
7、lack ManufacturingIndustriesE300 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 atom
8、ic absorption byflame technique 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, calcul
9、ations, and pre-cision statements 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
10、familiar with all aspects of 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.
11、4. Significance and Use4.1 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, esp
12、ecially 10, 100,200 and 500-cm3volumetric flasks.5.4 Pipets, of 1, 2, 5, and 10-cm3capacity. One cubiccentimetre pipets graduated in tenths and hundredths areespecially useful.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and Rubber-like Materials and are the direct r
13、esponsibility of SubcommitteeD11.11 on Chemical Analysis.Current edition approved May 1, 2017. Published May 2017. Originallyapproved in 1981. Last previous edition approved in 2012 as D4075 06 (2012).DOI: 10.1520/D4075-06R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orco
14、ntact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international sta
15、ndard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.5
16、Microlitre Syringes, 1 and 10 mm3(L) are recom-mended.5.6 Plastic Bottles, suitable for storage of standard solu-tions.5.7 Atomic Absorption Spectrophotometer, operating in theflame mode. The instrument must be operated according to themanufacturers directions for optimum performance for flameoperat
17、ion.6. Reagents6.1 Standard solution for metals to be determined in eachcompounding 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 ofsolutio
18、n. Suitable dilutions with water will bring these concen-trated solutions into 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
19、 out this procedure. All reagents shall be of analyticalgrade, and distilled, 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 lo
20、t (see PracticeE300).7.2 The analyst shall select a test portion from the sample 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 appropr
21、iate to the atomic absorptionspectrophotometer being used.8.2 Instrument calibration 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 l
22、ess than0.1 %.NOTE 1Micrograms per gram, parts per million, and milligrams 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 wi
23、thPractice D4483. Refer to this practice for terminology andother testing statistical 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 OXIDE
24、11. Scope11.1 This test method covers the analysis of zinc oxide forcopper, 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 dissoluti
25、on problems.11.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization Technic
26、alBarriers to Trade (TBT) Committee.12. Summary of Test Method12.1 A “slurry” of zinc oxide and water 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 forc
27、opper, cadmium, manganese and lead is for quality assurance,but this test method may be used for other 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), c
28、oncentrated.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 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
29、portion. For small test portions, 10 cm3will suffice, forlarger test portions, up to 30 cm3may be needed.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 p
30、oint,then add 1 to 2 cm3of concentrated HNO3. Continue heatingfor no more than 5 min. Remove the beaker 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 a
31、nd finalvolume of solution is left to the discretion of the analyst and must bedetermined by prior knowledge of the approximate amount of copper,cadmium, and lead in the type of zinc oxide being analyzed.D4075 06 (2017)217.3 Carry a blank throughout the entire procedure, usingthe same quantities of
32、reagents but without a test portion.Subtract any positive blank value, in an appropriate manner,before calculating 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 direct
33、ions for optimum instru-ment performance.NOTE 4Zinc oxide solution for measurement must fall within thelinear range of the instrument. Any solution that does not meet thiscriterion must be diluted suitably to fall within this range.18. Calculation18.1 See Section 8.19. Report19.1 See Section 9.20. P
34、recision and Bias320.1 This precision and bias section has been prepared inaccordance with Practice 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
35、 periodof a few days separates replicate test results. A test result is theaverage value, as specified 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 oxi
36、de), number of laboratories, numberof testing days.20.4 The results of the precision calculations for 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 “
37、appropriate value” of r, R, (r), or (R), thatis, that value to be used in decisions about test results (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 givenma
38、terial in routine testing operations.20.6 RepeatabilityThe repeatability, r, of this test methodhas 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
39、 be considered as derived from different ornonidentical sample populations.20.7 ReproducibilityThe 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 t
40、est methodprocedures, that differ by more than the tabulated R (for anygiven level) must be considered 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
41、 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 the arithmetic mean of the two testresults.20.9 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (or true) testprope
42、rty value. Reference values do not exist for this testmethod since the value (of the test property) 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 H
43、eadquarters and maybe obtained by requesting Research Report RR:D11-1019.TABLE 1 Details on Interlaboratory 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 (2017)3ASTM Internati
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49、r, Cadmium, Manganese, and Lead in Zinc OxideNOTE 1Sr= 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)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
