1、Designation: D 5630 06Standard Test Method forAsh Content in Plastics1This standard is issued under the fixed designation D 5630; 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 parentheses in
2、dicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method was developed to determine the inor-ganic content of plastics by destructive ashing procedures. Ashlevels of 0.01 % or above are covered by
3、this test method.1.2 These ashing procedures are used only to quantify theresidual solids in the polymer and can not be used to identifythe individual chemical components of the ash, qualitatively.1.3 This test method is limited to those materials (includingglass) that are stable to 900C. Test Metho
4、d D 2584 isrecommended for unknown samples, and in instances wherefusion of the inorganic portions may be of concern.1.4 Fluorinated polymers and polymers containing haloge-nated components have not been included in these procedures.1.5 Two procedures for determining the inorganic residue inplastics
5、 are listed as follows:1.5.1 Procedure A, Muffle-Furnace TechniqueFor550gram samples. Samples are flamed over a burner prior to beingashed in a muffle furnace.1.5.2 Procedure B, Rapid-Ash Muffle-Furnace TechniqueFor550gram samples. Samples are ignited and ashed in amuffle furnace.NOTE 1For more effi
6、cient ashing, the plastic sample should be in theform of powder or pellet.NOTE 2Procedure B is similar to ISO 3451/1-1981(E).1.6 The values stated in SI units are to be regarded as thestandard.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. I
7、t 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. See Section 9 forspecific precautionary statements.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating
8、to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 2584 Test Method for Ignition Loss of Cured ReinforcedResinsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:ISO 3451/1-1981(E) PlasticsDetermination ofAsh Part1,
9、 General Methods, 5.3 Method ADirect Calcination33. Terminology3.1 DefinitionsFor definitions of plastics terms, see Ter-minologies D 883 and D 1600. There are no terms in this testmethod that require new or other than dictionary definitions.4. Summary of Test Method4.1 This test method is based on
10、a loss in weight of a plasticsample when combusted to oxidize all organic matter.5. Significance and Use5.1 Inorganic residues from plastics ashing may be anti-block, fillers, reinforcements, catalyst residues, colorants, etc.The quantitative amounts of each are important variables of themanufacturi
11、ng process.6. Interferences6.1 A flame height of over 2.5 cm is likely to cause a loss offine particles.6.2 Large sample sizes (Note 5) could result in the evolutionof pyrolysis products that could affect the ash recovery.6.3 Furnace doors must be in the closed position during theignition period to
12、prevent too-rapid oxidation and combustionof the sample (Note 7).6.4 Ensure that all crucibles are cooled to ambient tempera-ture before weighing.7. Apparatus7.1 BalanceA balance having the capability to weigh thesample to the nearest 0.0001 g. The balance should be checkedperiodically to ensure acc
13、uracy.7.2 CruciblesPorcelain or quartz-fiber, of sufficient size.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Sept. 1, 2006. Published October 2006. Originallyapprov
14、ed in 1994. Last previous edition approved in 2001 as D 5630 - 01.2For 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 Summary page onthe ASTM web
15、site.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, U
16、nited States.NOTE 3Coors porcelain crucibles, or CEM quartz-fiber crucibles No.303040,4or equivalents, may be used.7.3 Muffle FurnaceElectric-resistance-heated ormicrowave-heated furnace, capable of maintaining a tempera-ture of 900 6 25C.NOTE 4If an electric muffle furnace is used, it should be pos
17、itioned ina well-ventilated hood. If a microwave furnace is used, it should bepositioned within or adjacent to the hood and the exhaust tube vented intothe hood to prevent breathing of the byproducts of the combustion. Amicrowave furnace should be capable of providing an air flow of 2.8m3/min to be
18、moved through the microwave cavity.7.4 Cooling AssemblyA nichrome triangle is positionedover a polypropylene funnel connected to a dry compressed-airsource, or equivalent. See Fig. 1, Procedure B. Calibrate the airflow with a wet test meter or bubblemeter to yield a flow rateof approximately 30 L/mi
19、n.7.5 Burner.7.6 Desiccator.8. Reagents and Materials8.1 DesiccantMaterials suitable for use in the desiccatormay be chosen from the following:8.1.1 Anhydrous Calcium Sulfate.8.1.2 Silica Gel.9. Safety Precautions9.1 Always wear safety glasses when working in the labo-ratory.9.2 Exercise all normal
20、safety precautions when workingwith open flames and high temperatures. Use insulated glovesand long crucible tongs when transferring crucibles.9.3 Always work with an appropriately vented muffle fur-nace or under a fume hood when ashing. Irritant fumes aregiven off by the polymer during ashing.10. S
21、ampling, Test Specimens, and Test Units10.1 For hygroscopic materials such as nylons, etc., drysample specimens to constant weight before testing.11. Preparation and Apparatus11.1 Crucible PreparationClean the porcelain crucibleswith tap water and an abrasive detergent. Ensure that anybaked-in resid
22、ue is removed from the crucibles completely.Quartz-fiber crucibles are disposable items and do not requirecleaning.11.2 Fire (condition) the clean crucibles in a muffle furnaceat the set operating temperature for 5 min to burn off anyresidue in the crucibles.11.3 After firing (conditioning) the cruc
23、ibles, place them ina desiccator to cool for 20 to 30 min (porcelain crucibles) or 2min (quartz-fiber crucibles). Handle the crucibles with tongsonly.12. Calibration and Standardization12.1 Calibrate the analytical balances in accordance withthe manufacturers procedure.13. Procedure AMuffle Furnace
24、Technique13.1 Sample TypeDetermine the type of polymer andanticipated amount of inorganics in the polymer to be ashed.Determine the ashing temperature, ashing time, and samplesize required to perform the ash analysis in accordance withTable A1.1.13.2 Preashing ProcedureWeigh a clean, dry porcelaincr
25、ucible to the nearest 0.0001 g. Record the resulting value asW1.13.2.1 Weigh approximately the amount of material inaccordance with Table A1.1 into the preweighed crucible.Record the resulting value as W2.13.2.2 Place the crucible on a burner. (The diameter of theflame equals 2.5 cm, and the height
26、of the flame equals justenough to touch the wire gauze holding the crucible.) Ensurethat the material does not overflow the crucible. When the flashpoint of the polymer is attained (which is approximately 600Cfor most plastics), the polymer begins to burn. To prevent theloss of fine particles, ensur
27、e that the flame intensity appearingfrom the crucible is low and that the flame height is not over2.5 cm. Continue flaming until there are no visible flamesappearing in the crucible.13.3 Muffle FurnaceUsing tongs, remove the cruciblefrom the burner, and place it in the muffle furnace (electric ormic
28、rowave) set at the desired temperature in accordance withTable A1.1.4Porcelain crucibles are available from catalogs such as Fisher. CEM quartz-fiber crucibles are available from CEM Corp., Matthews, NC.FIG. 1 Cooling AssemblyD563006213.4 After the prescribed duration in the muffle furnace (asspecif
29、ied in TableA1.1), using tongs, remove the crucible fromthe muffle furnace and place it in a desiccator until cool.13.5 Weigh the cooled crucible and record the resultingvalue as W3.13.6 After recording the data, place the crucible into themuffle furnace at the recommended temperature. Remove thesam
30、ple after 30 min and cool in a desiccator. Weigh the cooledcrucible and record the weight. If the current weight variesmore than 2 mg, continue ashing the sample at the recom-mended temperature until constant weight is reached.13.7 Calculate the ash content of the sample in accordancewith Equation 1
31、.14. Procedure BRapid-Ash Muffle Furnace Technique14.1 Sample TypeDetermine the type of polymer andanticipated amounts of inorganics in the polymer to be ashed.Determine the ashing temperature, ashing time, and samplesize required to perform the ash analysis in accordance withTable A1.2.14.2 Weighin
32、gWeigh a clean, dry, porcelain crucible or aquartz-fiber crucible to the nearest 0.0001 g. Record theresulting value as W1.14.2.1 Weigh approximately the amount of material given inTable A1.2 into the weighed crucible. Record the resultingvalue as W2.NOTE 5Experience has shown that 2.0-g samples can
33、 be ignitedconsistently at 800C without problems in a muffle furnace. Sampleweights larger than 8 g are not recommended.NOTE 6The procedure is applicable to pelletized resins and compactproducts such as sheets and molded articles. Powdered materials mayrequire modifications in the crucible size and
34、ignition conditions due totheir voluminous nature.14.3 Muffle FurnacePlace the crucible containing thesample into a muffle furnace set at the desired temperature inaccordance with Table A1.2 and close the muffle furnace doortightly.NOTE 7The door of the muffle furnace should be closed during theigni
35、tion period. If a microwave furnace is used, the ceramic door of thefurnace should be maintained in a tightly closed position during theignition period.14.4 After the prescribed duration in the muffle furnace (asspecified in TableA1.2), carefully remove the crucible from themuffle furnace and place
36、it in a dessicator until cool.NOTE 8The residual ash should be free of any carbonaceous matterafter the ignition period. Due to variations in furnace design and geometry,however, minor variations in ignition temperature or time, or both, may berequired.NOTE 9If the cooling assembly shown in Fig. 1 i
37、s used to acceleratethe cooling process for porcelain crucibles, position the crucible on thetriangle of the cooling assembly and adjust the dry-air flow to approxi-mately 30 L/min. Allow the crucible to cool to ambient temperature.14.5 Weigh the cooled crucible, and record the resultingvalue of W3.
38、14.6 After recording the data, place the crucible into themuffle furnace at the recommended temperature. Remove thecrucible after 5 min, and cool in a desiccator. Weigh the cooledcrucible and record the resulting value. If the current weightvaries more than 2 mg, continue ashing the sample at therec
39、ommended temperature until constant weight is reached.14.7 An alternative technique suggested in Research ReportRR: D20-1215 involves using a single, extended ashing time toachieve constant weight. As the time period involved dependson both material and context, documentation is needed ofequivalence
40、 to the results obtained using the multiple ashingprocedure of 14.4 through 14.6.14.8 Calculate the ash content of the sample in accordancewith Eq. 1.15. Calculation or Interpretation of Results15.1 Calculate the ash, mass %, in the analysis sample asfollows:ash, mass % 5W32 W1!W22 W1!3 100 (1)ppm a
41、sh, mass % 5W32 W1!W22 W1!3 106(2)where:W1= mass of sample crucible, g,W2= mass of sample crucible, g, plus mass of sample, g,andW3= mass of sample crucible, g, plus ashed mass ofsample, g.16. Report16.1 Report the ash content, mass %, to the second decimal(hundredth of a percent) if the value is eq
42、ual to or greater than1 %. Report the results to the nearest 10 ppm if the ash contentmass percent is less than 1 % (see Equation 2).17. Precision and Bias517.1 PrecisionThe results from a collaborative study aregiven in Table 1. The data were analyzed in accordance withPractice E 691. A total of ei
43、ght laboratories participated in thisstudy of eight materials.17.2 Concept of r and RIf Srand SRhave been calculatedfrom a large enough body of data, and for test results that wereaverages from testing two specimens, then:5Supporting data have been filed at ASTM International Headquarters and maybe
44、obtained by requesting Research Report RR: D20-1215.TABLE 1 Precision Summary (Procedures A and B)AMaterial/Filler Mean,% SrSRVrVRrRHDPE/antiblock 0.015 0.0038 0.0052 25.5 34.7 0.0107 0.0146LDPE/antiblock 0.149 0.0047 0.0054 3.2 3.6 0.0132 0.0151LDPE/antiblock 0.437 0.0047 0.0059 1.1 1.3 0.0131 0.01
45、65LDPE/antiblock 1.00 0.0090 0.0090 0.9 0.9 0.0253 0.0253PET/SiO23.18 0.0448 0.0448 1.4 1.4 0.1253 0.1253PET/TiO212.46 0.0461 0.0515 0.4 0.4 0.1292 0.1441Nylon/glass 33.16 0.2715 0.2822 0.8 0.9 0.7602 0.7902PET/TiO244.81 0.3707 0.4000 0.8 0.9 1.0379 1.1201Average 4.3 5.5ASris the within-laboratory r
46、epeatability and SRis the between-laboratoryreproducibility. r and R are the 95 % limits for a single sample for repeatability andreproducibility, respectively. VD563006317.2.1 Repeatability Limit, r (comparing two test results forthe same material, obtained by the same operator using thesame equipm
47、ent on the same day)The two test results shouldbe judged not equivalent if they differ by more than the r valuefor that material.17.2.2 Reproducibility Limit, R (comparing two test resultsfor the same material, obtained by different operators usingdifferent equipment in different laboratories)The tw
48、o testresults should be judged not equivalent if they differ by morethan the R value for that material.17.2.3 Any judgment in accordance with 17.2.1 or 17.2.2would have an approximate 95 % (0.95) probability of beingcorrect.17.3 BiasSince there is no accepted reference materialsuitable for determini
49、ng the bias for this test method, bias wasnot determined.18. Keywords18.1 antiblock; ash; mineral fillers; muffle furnace; plastics;polymer; residues; thermoplastics; thermosetsANNEX(Mandatory Information)A1. ASH ANALYSIS TABLESTABLE A1.1 Procedure APolymerTypeAsh Content,%Sample Size,gFurnaceTemperature,CDuration,min* 0.011 50 800 30* 15 10 800 30* 580 5 800 30* LDPE, LLDPE, MDPE, HDPE, PP, ionomer, EVA, EEA, thermoplastic elastomers, other olefinic polymers andcopolymers, and thermosets* 0.011 50 900 30* 15 10 900 30* 560 5 900
