1、Designation:D534795(Reapproved 2012)Standard Test Method forDetermination of the Ash Content of Fats and Oils1This standard is issued under the fixed designation D5347;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last
2、revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()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 ofleather and in
3、 the manufacture of fatliquors and other softeningand stuffing compounds.This test method was derived fromTest Method D1951.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of
4、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.See Section 5 forspecific hazard statements.2.Referenced Documents2.1 A
5、STM Standards:2D1951 Test Method for Ash in Drying Oils and Fatty Acids(Withdrawn 2003)33.Significance and Use3.1 This test method is intended to determine the ashcontent of fats and oils used in the softening and stuffing ofleather,as well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 purpos
6、e.The ash content of fats and oils is measured forthe purpose of quality assurance.4.Apparatus4.1 Crucible,porcelain or high-silica glass(Note 1),50-mLcapacity.NOTE1Platinum is not recommended.Boiled oils or oils contami-nated with driers containing lead may ruin platinum by alloy formation.4.2 Elec
7、tric Muffle Furnace.4.3 Desiccator,containing 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.)NOTE2Magnesium perchlorate and barium perchlorate are alsoeffici
8、ent desiccators and were previously 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 i
9、s a strong oxidizer and reactsviolently 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,
10、or fumes.It causessevere 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,p
11、lace in a 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 m
12、oving 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 theoil in the 4
13、-oz bottle has been added.Reweigh the sample1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 27-1957).Curr
14、ent edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5347 95(2006).DOI:10.1520/D5347-95R12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of
15、ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 bottle to
16、 obtain the total weight of sample used,which will besomewhat over 100 g.6.4 Continue 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.Calculation7.1 Calculate the ash content,A,of the sample as follows:A,%5R/S!3100(1)or,A,ppm5R/S!31 000000(2)where:R=residue(6.4),
