ASTM D5353-1995(2006) Standard Test Method for Determination of Total Desulfated Fatty Matter《全部脱硫脂肪物的标准试验方法》.pdf

1、Designation: D 5353 95 (Reapproved 2006)Standard Test Method forDetermination of Total Desulfated Fatty Matter1This standard is issued under the fixed designation D 5353; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the totaldesulfated fatty matter in a sample of sulfated oils by decom-p

3、osition with diluted mineral acids and extraction of thedecomposed fat. This test method is not applicable to samplesthat are not completely decomposed upon boiling with mineralacids. This test method was derived from Test Methods D 500,Sections 29 through 32.1.2 The values stated in SI units are to

4、 be regarded as thestandard.1.3 This standard 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

5、prior to use.2. Referenced Documents2.1 ASTM Standards:2D 500 Test Methods of Chemical Analysis of Sulfonatedand Sulfated OilsD 5350 Test Method for Determination of OrganicallyCombined Sulfuric Anhydride by Titration, Test Method AD 5351 Test Method for Determination of OrganicallyCombined Sulfuric

6、Anhydride by Extraction Titration, TestMethod B3. Significance and Use3.1 This test method is intended for the determination of thetotal desulfated matter contained in sulfated oils following theirtotal decomposition with dilute mineral acid.4. Reagents4.1 Ethyl Ether.4.2 Sulfuric Acid (1 + 19)Caref

7、ully mix one volume ofconcentrated sulfuric acid (H2SO4, sp gr 1.84) into 19 volumesof water while stirring.5. Procedure5.1 The procedure consists of decomposing the sample withH2SO4, extracting the fatty matter with ether, evaporating thesolvent, and weighing the residue. After cooling, transfer th

8、etitrated solution obtained after determining organically com-bined sulfuric anhydride in accordance with Test MethodD 5350 or Test Method D 5351 (6.1.2) into a 250-mL separa-tory funnel and shake with 50 mL of ether. Draw off the waterlayer into another separatory funnel and extract twice with25-mL

9、 portions of ether. Wash the combined ether layers with15-mL portions of water until the wash water is neutral tomethyl orange. Transfer the ether layer to a tared 150-mLbeaker, evaporate on the water bath until practically free fromsolvent, dry in a hot-air oven at 105 to 110C for 30 min, coolin a

10、desiccator, and weigh. Repeat the heating for 30-minperiods until constant weight is obtained.NOTE 1Reserve the extracted fatty matter for the subsequent deter-mination of unsaponifiable matter (Sections 37 through 41 of TestMethods D 500).6. Calculation6.1 Calculate the total desulfated fatty matte

11、r as follows:Total desulfated fatty matter, % 5 A/B! 3 100where:A = weight of residue, g, andB = weight of sample, g.7. Precision and Bias7.1 Although this test method is widely used, precision andbias information is not available at this time.8. Keywords8.1 desulfated matter; leather; sulfated fats

12、 and oils1This test method 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 45-1957).Current edition approved April 1, 2006

13、. Published April 2006. Originallyapproved in 1993. Last previous edition approved in 2001 as D 5353 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 st

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18、 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 5353 95 (2006)2