1、Designation: D5630 06D5630 13Standard Test Method forAsh Content in Plastics1This standard is issued under the fixed designation D5630; 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 parenthe
2、ses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method was developed to determine the inorganic content of plastics by destructive ashing procedures. Ash levelsof 0.01 % or above are covered
3、 by this test method.1.2 These ashing procedures are used only to quantify the residual solids in the polymer and can not be used to identify theindividual chemical components of the ash, qualitatively.1.3 This test method is limited to those materials (including glass) that are stable to 900C. Test
4、 Method D2584 is recommendedfor unknown samples, and in instances where fusion of the inorganic portions may be of concern.1.4 Fluorinated polymers and polymers containing halogenated components have not been included in these procedures.1.5 Two procedures for determining the inorganic residue in pl
5、astics are listed as follows:1.5.1 ProcedureA, Muffle-Furnace Technique For 5 50 gram samples. Samples are flamed over a burner prior to being ashedin a muffle furnace.1.5.2 Procedure B, Rapid-Ash Muffle-Furnace Technique For 5 50 210 gram samples. Samples are ignited and ashed ina muffle furnace.NO
6、TE 1For more efficient ashing, the plastic sample should be in the form of powder or pellet.NOTE 2This test method provides consistent results of filler content for a specific filler in a specific resin. However, this method may not providethe absolute filler content in all cases. This includes poly
7、mers filled with CaCO3, nano clays, and Carbon Black.NOTE 3Procedure B is similarequivalent to ISO 3451/1-1981(E). 3451/1-(E), Method A.1.6 The values stated in SI units are to be regarded as the standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated wi
8、th its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. See Section 9 for specific precautionary statements.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology
9、 Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating to PlasticsD2584 Test Method for Ignition Loss of Cured Reinforced ResinsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 ISO Standard:ISO 3451/1-1981(E)3451/1-(E) PlasticsDeterm
10、ination ofAsh Part 1,AshPart 1: General Methods, 5.3 MethodADirectCalcination33. Terminology3.1 DefinitionsFor definitions of plastics terms, see Terminologies D883 and D1600. There are no terms in this test methodthat require new or other than dictionary definitions.1 This test method is under the
11、jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved Sept. 1, 2006April 1, 2013. Published October 2006April 2013. Originally approved in 1994. Last previous edition approved in 20012006 asD5630 - 01.D56
12、30 - 06. DOI: 10.1520/D5630-06.10.1520/D5630-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available f
13、rom American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may n
14、ot be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the e
15、nd of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Summary of Test Method4.1 This test method is based on a loss in weight of a plastic sample when combusted to oxidize all organic matter.5. Significance and Use5.1
16、Inorganic residues from plastics ashing may be antiblock, fillers, reinforcements, catalyst residues, colorants, etc. Thequantitative amounts of each are important variables of the manufacturing process.6. Interferences6.1 A flame height of over 2.5 cm from the burner is likely to cause a loss of fi
17、ne particles.6.2 Large sample sizes (Note 5) could result in the evolution of pyrolysis products that could affect the ash recovery.6.3 Furnace doors must be in the closed position during the ignition period to prevent too-rapid oxidation and combustion ofthe sample (Note 7).6.4 Ensure that all cruc
18、ibles are cooled to ambient temperature before weighing.7. Apparatus7.1 BalanceAbalance having the capability to weigh the sample to the nearest 0.0001 g. The balance shouldshall be checkedperiodically to ensure accuracy.7.2 CruciblesPorcelain Porcelain, platinum, or quartz-fiber, of sufficient size
19、.size and inert to the material being tested. Thequartz-fiber crucible is only used in Procedure B.NOTE 3Coors porcelain crucibles, or CEM quartz-fiber crucibles No. 303040,4 or equivalents, may be used.7.3 Muffle FurnaceElectric-resistance-heated or microwave-heated furnace, capable of maintaining
20、a temperature of900 6 25C.NOTE 4If an electric muffle furnace is used, it should be positioned in a well-ventilated hood. If a microwave furnace is used, it should be positionedwithin or adjacent to the hood and the exhaust tube vented into the hood to or to the atmosphere through duct work to preve
21、nt breathing of the byproductsof the combustion. A microwave furnace should be capable of providing an air flow of 2.8 m3/min to be moved through the microwave cavity.cavity isrecommended.7.4 Cooling AssemblyA nichrome triangle is positioned over a polypropylene funnel connected to a dry compressed-
22、airsource, or equivalent. See Fig. 1, Procedure B. Calibrate the air flow with a wet test meter or bubblemeter to yield a flow rate ofapproximately 30 L/min.7.5 Burner.7.6 Desiccator.8. Reagents and Materials8.1 DesiccantMaterials suitable for use in the desiccator may be chosen from the following:8
23、.1.1 Anhydrous Calcium Sulfate.8.1.2 Silica Gel.9. Safety Precautions9.1 Always wear safety glasses when working in the laboratory.9.2 Exercise all normal safety precautions when working with open flames and high temperatures. Use insulated gloves and longcrucible tongs when transferring crucibles.9
24、.3 Always work with an appropriately vented muffle furnace or under a fume hood when ashing. Irritant fumes are given offby the polymer during ashing.10. Sampling, Test Specimens, and Test Units10.1 For hygroscopic materials such as nylons, etc., dry sample specimens to constant weight before testin
25、g.11. Preparation and Apparatus11.1 Crucible PreparationClean the porcelain or platinum crucibles with tap water and an abrasive detergent. Ensure that anybaked-in residue is removed from the crucibles completely. Quartz-fiber crucibles are disposable items and do not require cleaning.11.2 Fire (con
26、dition) the clean crucibles in a muffle furnace at the set operating temperature for 5 min to burn off any residuein the crucibles.D5630 13211.3 After firing (conditioning) the crucibles, place them in a desiccator to cool for 20 to 30 min (porcelain or platinumcrucibles) or 2 min (quartz-fiber cruc
27、ibles). Handle the crucibles with tongs only.12. Calibration and Standardization12.1 Calibrate the analytical balances in accordance with the manufacturers procedure.13. Procedure AMuffle Furnace Technique13.1 Sample TypeDetermine the type of polymer and anticipated amount of inorganics in the polym
28、er to be ashed. Determinethe ashing temperature, ashing time, and sample size required to perform the ash analysis in accordance with Table A1.1.13.2 Preashing ProcedureWeigh a clean, dry porcelain or platinum crucible to the nearest 0.0001 g. Record the resultingvalue as W1.13.2.1 Weigh approximate
29、ly the amount of material in accordance with Table A1.1 into the preweighed crucible. Record theresulting value as W2.13.2.2 Place the crucible on a burner. (The diameter of the flame equals approximately 2.5 cm, and the height of the flame equalsjust enough to touch the wire gauze holding the cruci
30、ble.) Ensure that the material does not overflow the crucible. When the flashpoint of the polymer is attained (which is approximately 600C for most plastics), the polymer begins to burn. To prevent the lossof fine particles, ensure that the flame intensity appearing from the crucible is low and that
31、 the flame height is not over 2.5 cm.Continue flaming until there are no visible flames appearing in the crucible.13.3 Muffle FurnaceUsing tongs, remove the crucible from the burner, and place it in the muffle furnace (electric ormicrowave) set at the desired temperature in accordance with Table A1.
32、1.13.4 After the prescribed duration in the muffle furnace (as specified in Table A1.1), using tongs, remove the crucible from themuffle furnace and place it in a desiccator until cool.13.5 Weigh the cooled crucible and record the resulting value as W3.13.6 After recording the data, place the crucib
33、le into the muffle furnace at the recommended temperature. Remove the sampleafter 30 min and cool in a desiccator. Weigh the cooled crucible and record the weight. If the current weight varies more than 2mg, continue ashing the sample at the recommended temperature until constant weight is reached.1
34、3.7 Calculate the ash content of the sample in accordance with Eq 1.FIG. 1 Cooling AssemblyD5630 13314. Procedure BRapid-Ash Muffle Furnace Technique14.1 Sample TypeDetermine the type of polymer and anticipated amounts of inorganics in the polymer to be ashed. Determinethe ashing temperature, ashing
35、 time, and sample size required to perform the ash analysis in accordance with Table A1.2.14.2 WeighingWeigh a clean, dry, porcelain crucibleporcelain, platinum, or a quartz-fiber crucible to the nearest 0.0001 g.Record the resulting value as W1.14.2.1 Weigh approximately the amount of material give
36、n in Table A1.2 into the weighed crucible. Record the resulting valueas W2.NOTE 5Experience has shown that 2.0-g samples can be ignited consistently at 800C without problems in a muffle furnace. Sample weights largerthan 810 g are not recommended.recommended unless the equipment manual states the in
37、strument can handle larger sample sizes.NOTE 6The procedure is applicable to pelletized resins and compact products such as sheets and molded articles. Powdered materials may requiremodifications in the crucible size and ignition conditions due to their voluminous nature.14.3 Muffle FurnacePlace the
38、 crucible containing the sample into a muffle furnace set at the desired temperature in accordancewith Table A1.2 and close the muffle furnace door tightly.NOTE 7The door of the muffle furnace should be closed during the ignition period. If a microwave furnace is used, the ceramic door of the furnac
39、eshould be maintained in a tightly closed position during the ignition period.14.4 After the prescribed duration in the muffle furnace (as specified in Table A1.2), carefully remove the crucible from themuffle furnace and place it in a dessicator until cool.NOTE 8The residual ash should be free of a
40、ny carbonaceous matter after the ignition period. Due to variations in furnace design and geometry,however, minor variations in ignition temperature or time, or both, may be required.NOTE 9If the cooling assembly shown in Fig. 1 is used to accelerate the cooling process for porcelain crucibles, posi
41、tion the crucible on the triangleof the cooling assembly and adjust the dry-air flow to approximately 30 L/min. Allow the crucible to cool to ambient temperature.14.5 Weigh the cooled crucible, and record the resulting value of W3.14.6 After recording the data, place the crucible into the muffle fur
42、nace at the recommended temperature. Remove the crucibleafter 5 min, and cool in a desiccator. Weigh the cooled crucible and record the resulting value. If the current weight varies morethan 2 mg, continue ashing the sample at the recommended temperature until constant weight is reached.14.7 An alte
43、rnative technique suggested in Research Report RR:D20-1215 involves using a single, extended ashing time toachieve constant weight. As the time period involved depends on both material and context, documentation is needed ofequivalence to the results obtained using the multiple ashing procedure of 1
44、4.4 through 14.6.14.8 Calculate the ash content of the sample in accordance with Eq 1.15. Calculation or Interpretation of Results15.1 Calculate the ash, mass %, in the analysis sample as follows:ash,mass %5 W3 2W1!W2 2W1!3100 (1)ppm ash,mass %5W3 2W 1!W2 2W1! 3106 (2)ppm ash 5W3 2W 1!W2 2W1! 3106 (
45、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 of sample, g.16. Report16.1 Report the ash content, mass %, to the second decimal (hundredth of a percent) if the value is equal to or greater than 1 %
46、.Report the results to the nearest 10 ppm if the ash content mass percent is less than 1 % (see Eq 2).17. Precision and Bias417.1 PrecisionThe results from a collaborative study are given in Table 1. The data were analyzed in accordance with PracticeE691. A total of eight laboratories participated i
47、n this study of eight materials.4 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D20-1215.D5630 13417.2 Concept of r and RIf Sr and SR have been calculated from a large enough body of data, and for test results that wereaverage
48、s from testing two specimens, then:17.2.1 Repeatability Limit, r (comparing two test results for the same material, obtained by the same operator using the sameequipment on the same day)The two test results should be judged not equivalent if they differ by more than the r value for thatmaterial.17.2
49、.2 Reproducibility Limit, R (comparing two test results for the same material, obtained by different operators using differentequipment in different laboratories)The two test results should be judged not equivalent if they differ by more than the R valuefor that material.17.2.3 Any judgment in accordance with 17.2.1 or 17.2.2 would have an approximate 95 % (0.95) probability of being correct.17.3 BiasSince there is no accepted reference material suitable for determining the bias for this test method, bias was notdetermined.18.
