ASTM D5347-1995(2012) Standard Test Method for Determination of the Ash Content of Fats and Oils 《脂肪和油中灰分含量测定的标准试验方法》.pdf

1、Designation: D5347 95 (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

2、 last 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 oflea

3、ther and in 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 ad

4、dress 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. See Section 5 forspecific hazard statements.2. Referen

5、ced Documents2.1 ASTM Standards:2D1951 Test Method forAsh 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 purp

6、ose. 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.NOTE 1Platinum is not recommended. Boiled oils or oils contami-nated with driers containing lead may ruin platinum by alloy formation

7、.4.2 Electric 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.)NOTE 2Magnesium perchlorate and barium perchlora

8、te are alsoefficient 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.

9、1 Phosphorus Pentoxide is 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 mucousmembra

10、nes in the form of liquid, mist, 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

11、 furnace at 550 to 650C.Cool slightly, place 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 o

12、f the crucible or bottle.1This 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).Current edition approve

13、d 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 ASTMStanda

14、rds volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.

15、3 Heat gently by moving 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 al

16、l of theoil 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 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

17、 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,%5 R/S! 3 100 (1)or,A, ppm 5 R/S! 3 1 000 000 (2)where:R = residue (6.4),

18、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 obtain theprecision and, if obtainable, it will be published in futurerevisions. This test method has been in use for many years, andits usefu

19、lness has been well established.9. Keywords9.1 ash content; fatliquors; fats and oils; leather; softeningand stuffing compoundsASTM 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

20、expressly advised that determination of the validity of any such patent 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 re

21、vised, either reapproved or withdrawn. Your comments are invited either 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

22、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 address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United S

23、tates. 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5347 95 (2012)2