1、Designation: D 5347 95 (Reapproved 2006)Standard Test Method forDetermination of the Ash Content of Fats and Oils1This standard is issued under the fixed designation D 5347; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the ashcontent of fats and oils used in the softening and stuffing of
3、leather and in the manufacture of fatliquors and other softeningand stuffing compounds. This test method was derived fromTest Method D 1951.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated
4、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. See Section 5 forspecific hazard statements.2. Referenced Documents2.1 ASTM Standards:2D 1951 Test Method
5、for Ash in Drying Oils and FattyAcids33. Significance and Use3.1 This test method is intended to determine the ashcontent of fats and oils used in the softening and stuffing ofleather, as well as those used in the manufacture of products forsuch purpose. The ash content of fats and oils is measured
6、forthe purpose of quality assurance.4. Apparatus4.1 Crucible, porcelain or high-silica glass (Note 1), 50-mLcapacity.NOTE 1Platinum is not recommended. Boiled oils or oils contami-nated with driers containing lead may ruin platinum by alloy formation.4.2 Electric Muffle Furnace.4.3 Desiccator, conta
7、ining an efficient desiccant.Anhydrouscalcium sulfate (CaSO4), phosphorus pentoxide (P2O5)orconcentrated sulfuric acid (H2SO4, sp gr 1.84) are satisfactory.(WarningSee 5.1 and 5.2 for specific hazards.)NOTE 2Magnesium perchlorate and barium perchlorate are alsoefficient desiccators and were previous
8、ly listed in this section. Howeverbecause of their explosive danger, and the availability of other safermaterials, the recommendation for their use has been discontinued.4.4 Oil Sample Bottle, 4-oz (120-mL).4.5 Triangle, Nichrome or clay.5. Hazards5.1 Phosphorus Pentoxide is a strong oxidizer and re
9、actsviolently with water, reducing agents, and organic matter.Causes burns. Avoid contact with skin or eyes, or clothing, orinhalation as dust. Refer to suppliers Material Safety DataSheet.5.2 Sulfuric Acid is corrosive to skin, eyes and mucousmembranes in the form of liquid, mist, or fumes. It caus
10、essevere burns. Take care to prevent the contact of the acid witheyes or skin or on clothing. In making dilute solutions, alwaysadd the acid to water with care. See suppliers Material SafetyData Sheet.6. Procedure6.1 Ignite the crucible in the muffle furnace at 550 to 650C.Cool slightly, place in a
11、desiccator for 1 h, and weigh to 0.1mg.6.2 Fill a 4-oz (120-mL) sample bottle with the sample andweigh to 0.05 g. Pour about 20 g of the sample from the bottleinto the crucible supported on a triangle, using care so that nooil runs down the outside of the crucible or bottle.6.3 Heat gently by moving
12、 a flame on the bottom and sidesof the crucible until the oil ignites. Reduce the size of the flameuntil the heat is just sufficient to keep the sample burning.When the first batch of oil has burned out, add about 20 g moreof the sample and continue in the same manner until all of the1This test meth
13、od is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils.This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 27-1957).Current edition approved April 1, 2006. Published April 2006.
14、Originallyapproved in 1993. Last previous edition approved in 2001 as D 5347 95(2001).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
15、 page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.oil in the 4-oz bottle has been added. Reweigh the samplebottle to obtain the total weight of sample used, which will besomewhat over 100 g.6.4 Conti
16、nue heating the crucible until the oil is oxidized toa black char and transfer to a muffle furnace. Heat at 550 to650C for 1 h. Remove from the furnace, cool slightly, place ina desiccator, and cool to room temperature. Weigh and repeatheating in the furnace to constant weight (within 0.1 mg).7. Cal
17、culation7.1 Calculate the ash content, A, of the sample as follows:A,%5 R/S! 3 100 (1)or,A, ppm 5 R/S! 3 1 000 000 (2)where:R = residue (6.4), g, andS = sample used, g.8. Precision and Bias8.1 Precision and bias were not established at the time thistest method was written. An effort is being made to
18、 obtain theprecision and, if obtainable, it will be published in futurerevisions. This test method has been in use for many years, andits usefulness has been well established.9. Keywords9.1 ash content; fatliquors; fats and oils; leather; softeningand stuffing compoundsASTM International takes no po
19、sition 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 patent rights, and the riskof infringement of such rights, are entirely their own responsibi
20、lity.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 either for revision of this standard or for additional standardsand should be addressed to A
21、STM 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 hearing you shouldmake your views known to the ASTM Committee on Standards, at the addres
22、s 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 standard 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).D 5347 95 (2006)2
