ASTM D2617-2017a Standard Test Method for Total Ash in Leather《皮革中总灰分的标准试验方法》.pdf

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1、Designation: D2617 17aStandard Test Method forTotal Ash in Leather1This standard is issued under the fixed designation D2617; 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 indica

2、tes 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. Scope1.1 This test method covers the determination of total ash inleather.1.2 This sta

3、ndard 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, health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.3 This int

4、ernational 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 TechnicalBarriers to Trade (TBT)

5、 Committee.2. Referenced Documents2.1 ASTM Standards:2D2807 Test Method for Chromic Oxide in Leather (Perchlo-ric Acid Oxidation)D2813 Practice for Sampling Leather for Physical andChemical Tests3. Summary of Test Method3.1 The sample is ignited in air at 600 6 25 C untilconstant mass is attained. T

6、he weighed residual matter istermed “ash” and is calculated as a percentage of the originalsample.4. Significance and Use4.1 This test method is useful in determining the approxi-mate amount of nonvolatile inorganic material in leather. Thismay be in the form of salts or oxides of the elements. In a

7、mixed chrome tannage, the approximate percentage of otherelements in the leather may be determined by subtracting thechromic oxide that may be conveniently determined on the ash.(See Test Method D2807.)4.2 The temperature of 600 C specified is high enough toproduce a reproducible result but it does

8、not completelydehydrate such oxides as aluminum oxide, (Al2O3) and chro-mic oxide (Cr2O3). Likewise, such salts as sulfates andphosphates may be incompletely dehydrated, and if alkalis andchromium are present simultaneously, oxidation to chromatemay occur. Therefore, caution is advised in drawing co

9、nclu-sions based on quantitative relations of the elements.5. Apparatus5.1 Crucible, 30 to 50-mL, high-form, platinum or porce-lain.5.1.1 Suitable Glassware or Crucible, able to withstandtemperatures up to 625 C and the acids required for TestMethod D2807 may be used.5.2 Electric Furnace, with contr

10、oller or rheostat andpyrometer, capable of maintaining a temperature of 600 625C.6. Test Specimen6.1 The specimen shall consist of 1 to5gofleather from thecomposite sample prepared in accordance with PracticeD2813.NOTE 1In some leathers, silicones or other organometallic complexesthat are solvent, s

11、oluble, and ash producing are used. It may be desirableto obtain ash on an extracted sample, and if so, it should be indicated onthe report.7. Procedure7.1 Weigh accurately (to 1 mg) into a tared crucible 1 to 5g of leather, prepared as described in 6.1, and preferably atsufficiently close equilibri

12、um with the laboratory humidity thatit does not gain or lose mass at a significant rate. Place thecrucible and sample in the furnace and maintain at 600 6 25C for a period of 4 h 6 5 min. (Note 2). Remove the cruciblefrom the furnace, cool in a desiccator, and weigh (Note 3).Record the mass.NOTE 2Th

13、e above procedure is satisfactory with most leathers. With1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.06 on Chemical Analysis. Thistest method was developed in cooperation with the American Leather ChemistsAssn. (St

14、andard Method B15 1969).Current edition approved Sept. 1, 2017. Published September 2017. Originallyapproved in 1969. Last previous edition approved in 2017 as D2617 17. DOI:10.1520/D2617-17A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at ser

15、viceastm.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 standard was developed in accordance

16、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.1heavily oiled or stuffed leather, star

17、t with a cold furnace and raisetemperature gradually to 600 C, or burn off the oil carefully over a gasburner before placing the crucible in the hot furnace.NOTE 3If it is difficult to burn off the carbon, as evidenced byinspection, moisten the ash with a few drops of 1+1 nitric acid, drycarefully o

18、ver a low flame, and then transfer to the furnace and heat asbefore. If this procedure is unsuccessful, digest the ash in the crucible with15 to 20 mL of hot water for a few minutes, and filter the suspensionthrough an ashless high-retention filter paper. Transfer the paper andinsoluble residue to t

19、he crucible and ignite at 600 6 25 C as describedabove. Cool, add the filtrate to the crucible, evaporate carefully to dryness,then ignite at 600 6 25C to constant mass as described above.8. Calculations8.1 Calculate the percentage of ash in the leather weighed asfollows:Ash, % 5 A 2 B!/C 2 B!# 3100

20、 (1)where:A = mass of the ash and crucible,B = mass of the crucible, andC = mass of the sample and crucible.8.2 If it is desired to convert the percentage obtained aboveto the dry basis, perform a moisture determination on a portionof the same sample weighed under the same conditions as inSection 7.

21、 If the percentage moisture found is D, then calculatethe percentage of ash on a dry basis as follows:Ash, dry basis, % 5 A 2 B!/C 2 B!# 3 100/1 2 D/100!# (2)where A, B, and C have the same meaning as in 8.1.8.3 The ash may be determined on a sample conditioned asto temperature and relative humidity

22、. In this case, weigh thesample under identically controlled temperature and humidity,and report the results in such a manner as to indicate this fact,for example:Ash X C, Y % relative humidity! 5 Z % (3)9. Precision and Bias39.1 PrecisionThe precision of this test method is largelylimited by the ho

23、mogeneity of the sample in a complex naturalmaterial such as leather.9.1.1 RepeatabilityAt the 95 % confidence level, dupli-cate determinations by the same operator should not differ bymore than 0.14 % ash.9.1.2 ReproducibilityAt the 95 % confidence level, theaverage of duplicate determinations in e

24、ach of two laboratoriesby different operators should not differ by more than 0.20 %ash.9.2 BiasInasmuch as all leathers contain an unknownamount of natural or inherent ash, no meaningful statement canbe made with respect to bias.10. Keywords10.1 aluminum oxide; ash; chromic oxideASTM International t

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29、phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D31 -0089.D2617 17a2