ASTM D2617-2017 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 12D2617 17Standard 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

2、 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. Scope1.1 This test method covers the determination of total ash in leather.1.2

3、This standard does not purport to address all of the safety concerns, if any, associated with 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.1.3 This internationa

4、l standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2

5、. Referenced Documents2.1 ASTM Standards:2D2807 Test Method for Chromic Oxide in Leather (Perchloric Acid Oxidation)D2813 Practice for Sampling Leather for Physical and Chemical Tests3. Summary of Test Method3.1 The sample is ignited in air at 600 6 25C 25 C until constant mass is attained. The weig

6、hed residual matter is termed“ash” and is calculated as a percentage of the original sample.4. Significance and Use4.1 This test method is useful in determining the approximate amount of nonvolatile inorganic material in leather. This may bein the form of salts or oxides of the elements. In a mixed

7、chrome tannage, the approximate percentage of other elements in theleather may be determined by subtracting the chromic oxide that may be conveniently determined on the ash. (See Test MethodD2807.)4.2 The temperature of 600C 600 C specified is high enough to produce a reproducible result but it does

8、 not completelydehydrate such oxides as aluminum oxide, (Al2O3) and chromic oxide (Cr2O3). Likewise, such salts as sulfates and phosphates maybe incompletely dehydrated, and if alkaliesalkalis and chromium are present simultaneously, oxidation to chromate may occur.Therefore, caution is advised in d

9、rawing conclusions based on quantitative relations of the elements.5. Apparatus5.1 Crucible, 30 to 50-mL, high-form, platinum or porcelain.5.1.1 Suitable Glassware or Crucible, able to withstand temperatures up to 625 C and the acids required for Test MethodD2807 may be used.5.2 Electric Muffle Furn

10、ace, with controller or rheostat and pyrometer, capable of maintaining a temperature of 600 6 25C.6. Test Specimen6.1 The specimen shall consist of 1 to 5 g of leather from the composite sample prepared in accordance with anPracticeD2813accepted procedure1 This test method is under the jurisdiction

11、of ASTM Committee D31 on Leather and is the direct responsibility of Subcommittee D31.06 on Chemical Analysis. This testmethod was developed in cooperation with the American Leather Chemists Assn. (Standard Method B15 1969).Current edition approved April 1, 2012April 1, 2017. Published April 2012May

12、 2017. Originally approved in 1969. Last previous edition approved in 20062012 asD2617 06.D2617 12. DOI: 10.1520/D2617-12.10.1520/D2617-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume

13、information, refer to the standards Document Summary page on the ASTM website.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 not be technically possible to adequate

14、ly 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,

15、 PA 19428-2959. United States1NOTE 1In some leathers, silicones or other organometallic complexes that are solvent, soluble, and ash producing are used. It may be desirable toobtain ash on an extracted sample, and if so, it should be indicated on the report.7. Procedure7.1 Weigh accurately (to 1 mg)

16、 into a tared crucible 1 to 5 g of leather, prepared as described in 6.1, and preferably at sufficientlyclose equilibrium with the laboratory humidity that it does not gain or lose mass at a significant rate. Place the crucible and samplein the muffle furnace and maintain at 600 6 25C 600 6 25 C for

17、 a period of 4 h 6 5 min. (Note 2). Remove the crucible fromthe furnace, cool in a desiccator, and weigh (Note 3). Record the mass.NOTE 2The above procedure is satisfactory with most leathers. With heavily oiled or stuffed leather, start with a cold muffle and raise temperaturegradually to 600C, 600

18、 C, or burn off the oil carefully over a gas burner before placing the crucible in the hot furnace.NOTE 3If it is difficult to burn off the carbon, as evidenced by inspection, moisten the ash with a few drops of 1+1 nitric acid, dry carefully overa low flame, and then transfer to the muffle and heat

19、 as before. If this procedure is unsuccessful, digest the ash in the crucible with 15 to 20 mL of hotwater for a few minutes, and filter the suspension through an ashless high-retention filter paper. Transfer the paper and insoluble residue to the crucibleand ignite at 600 6 25C 25 C as described ab

20、ove. Cool, add the filtrate to the crucible, evaporate carefully to dryness, then ignite at 600 6 25C toconstant mass as described above.8. Calculations8.1 Calculate the percentage of ash in the leather weighed as follows:Ash,%5A 2B!/C 2B!# 3100 (1)where:A = mass of the ash and crucible,B = mass of

21、the crucible, andC = mass of the sample and crucible.8.2 If it is desired to convert the percentage obtained above to the dry basis, perform a moisture determination on a portion ofthe same sample weighed under the same conditions as in Section 7. If the percentage moisture found is D, then calculat

22、e thepercentage of ash on a dry basis as follows:Ash,dry basis,%5A 2B!/C 2B!# 3100/12D/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 as to temperature and relative humidity. In this case, weigh the sampleunder identically controlled

23、temperature and humidity, and report the results in such a manner as to indicate this fact, for example:Ash X C,Y %relative humidity!5Z % (3)9. Precision and Bias39.1 PrecisionThe precision of this test method is largely limited by the homogeneity of the sample in a complex naturalmaterial such as l

24、eather.9.1.1 RepeatabilityAt the 95 % confidence level, duplicate determinations by the same operator should not differ by more than0.14 % ash.9.1.2 ReproducibilityAt the 95 % confidence level, the average of duplicate determinations in each of two laboratories bydifferent operators should not diffe

25、r by more than 0.20 % ash.9.2 BiasInasmuch as all leathers contain an unknown amount of natural or inherent ash, no meaningful statement can be madewith respect to bias.3 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D31 -0089

26、.D2617 17210. Keywords10.1 aluminum oxide; ash; chromic oxideASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such p

27、atent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited ei

28、ther for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair

29、 hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this stan

30、dard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (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:/ Acceptable procedures are published in the Journal of the American Leather Chemists Association, Vol 51, 1956, p. 497; see Practice D2813.D2617 173