ASTM D2617-2012 Standard Test Method for Total Ash in Leather 《皮革总灰分的标准试验方法》.pdf

1、Designation: D2617 12Standard 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 indicat

2、es 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 This test method covers the determination of total ash inleather.1.2 This standard

3、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.2. Referenced Documents2.1 ASTM S

4、tandards: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 25C until constantmass is attained. The weighed residual matter is termed “ash”and

5、 is calculated as a percentage of the original sample.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 amixed chrome tannage, the approximate percen

6、tage 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 600C specified is high enough toproduce a reproducible result but it does not completelydehydrate such oxides as alumin

7、um oxide, (Al2O3) and chro-mic oxide (Cr2O3). Likewise, such salts as sulfates andphosphates may be incompletely dehydrated, and if alkaliesand chromium are present simultaneously, oxidation to chro-mate may occur. Therefore, caution is advised in drawingconclusions based on quantitative relations o

8、f the elements.5. Apparatus5.1 Crucible, 30 to 50-mL, high-form, platinum or porce-lain.5.2 Electric Muffle Furnace, with controller 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 p

9、repared in accordance with an acceptedprocedure.3NOTE 1In some leathers, silicones or other organometallic complexesthat are solvent, soluble, 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 acc

10、urately (to 1 mg) into a tared crucible 1 to 5g of leather, prepared as described in 6.1, and preferably atsufficiently close equilibrium with the laboratory humidity thatit does not gain or lose mass at a significant rate. Place thecrucible and sample in the muffle furnace and maintain at 6006 25C

11、for a period of 4 h 6 5 min. (Note 2). Remove thecrucible from the furnace, cool in a desiccator, and weigh(Note 3). Record the mass.NOTE 2The above procedure is satisfactory with most leathers. Withheavily oiled or stuffed leather, start with a cold muffle and raisetemperature gradually to 600C, or

12、 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 over a low flame, and then transfer to the muffle and heat asbefor

13、e. 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 the crucible and ignite at 600 6 25C as described1This test method

14、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. (Standard Method B15 1969).Current edition approved April 1, 2012. Published Ap

15、ril 2012. Originallyapproved in 1969. Last previous edition approved in 2006 as D2617 06. DOI:10.1520/D2617-12.2For 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 s

16、tandards Document Summary page onthe ASTM website.3Acceptable procedures are published in the Journal of the American LeatherChemists Association, Vol 51, 1956, p. 497; see Practice D2813.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Stat

17、es.above. 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!# 3 100 (1)where:A = mass of the ash and crucible,B

18、= 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. If the percentage moisture found is D, then

19、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. In this case, weigh thesample under identic

20、ally 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 Bias49.1 PrecisionThe precision of this test method is largelylimited by the homogeneity of the sample in a complex naturalm

21、aterial 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 each of two laboratoriesby different operators

22、 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 takes no position respecting the validity of a

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27、g (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D31 -0089.D2617 122