1、Designation: D 5553 95 (Reapproved 2006)Standard Test Method forDetermination of the Unsaponifiable Nonvolatile Matter inSulfated Oils1This standard is issued under the fixed designation D 5553; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year 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 unsa-ponifiable, nonvolatile (above 80C) mat
3、ter existing in asample of sulfated oil by saponifying the desulfated fattymatter and extracting the unsaponifiable matter, and extractingthe unsaponifiable matter from the soap solution with ethylether.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not pu
4、rport 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 prior to use.2. Referenced Documents2.1 ASTM Standards:2D
5、 5350 Test Method for Determination of OrganicallyCombined Sulfuric Anhydride by Titration, Test Method AD 5351 Test Method for Determination of OrganicallyCombined SulfuricAnhydride by Extraction Titration, TestMethod BD 5353 Test Method for Determination of Total DesulfatedFatty Matter3. Significa
6、nce and Use3.1 This test method is intended for use in the determinationof the unsaponifiable, nonvolatile matter contained in sulfatedoils for the purpose of quality assurance.4. Apparatus and Reagents4.1 Saponification FlaskThe apparatus required for thesaponification consists of a glass flask pro
7、vided with an aircondenser.4.2 Ethyl Ether.4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)Dissolve approximately, but not less than, 28 g of KOH in ethylalcohol and dilute to 1 L.4.4 Potassium Hydroxide Aqueous Solution (28 g/L)Dissolve 28 g of potassium hydroxide (KOH) in water anddilute to 1
8、L.5. Procedure5.1 The procedure consists of decomposing the sample withmineral acid, extracting the desulfated fatty matter, saponifyingthe latter, and extracting the unsaponifiable matter from thesoap solution with ethyl ether.5.1.1 Desulfated Fatty MatterDetermine the desulfatedfatty matter as des
9、cribed in the determination of total des-ulfated fatty matter. See Test Methods D 5350, D 5351, andD 5353.5.1.2 SaponificationAccurately weigh 2 to 2.5 g of thedesulfated fatty matter in the flask, add 25 mL of the alcoholicKOH solution, and simmer the contents (without loss ofalcohol) for 1 h with
10、occasional swirling, over an electric hotplate or other source of heat.5.1.3 ExtractionTransfer the content of the flask to a250-mL separatory funnel and wash the flask several timeswith a total of 50 mL of water, pouring it into the separatoryfunnel. Extract the solution while still warm (about 30C
11、) with50 mL of ether (rinse the saponification flask with the etherbefore adding it to the separatory funnel), shaking vigorouslyfor about 1 min, and allow the layers to settle and clear. Drawoff the lower layer in a second 250-mL separatory funnel andextract in a similar manner with two 50-mL porti
12、ons of ether.5.1.4 Preliminary Water WashingAdd 20 mL of water tothe combined ether layer, turn the separatory funnel andcontents over gently about six times, and allow the layers tosettle and clear. Draw off the lower layer and discard. Wash theether layer twice more with 20-mL portions of water, s
13、hakingvigorously after each addition.5.1.5 Alkali and Water WashingAdd 20 mL of aqueousKOH solution to the washed ether layer, turn the separatoryfunnel and contents over gently about six times, and allow thelayers to settle and clear. Draw off the lower layer and discard.Wash the ether layer with 2
14、0 mL of water, shaking vigorously.Continue washing with 20 mL of KOH solution followed by 201This 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 Ameri
15、can Leather Chemists Assn.(Method H 471957).Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1994. Last previous edition approved in 2001 as D 5553 95(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at ser
16、viceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.mL of water, shaking vigorously after each addition, u
17、ntil thealkali layer upon strong acidification with HCl and settling fora few minutes is only faintly opalescent. Finally wash the etherlayer with 20-mL portions of water until the wash water is nolonger pink to phenolphthalein.5.1.6 Solvent RemovalTransfer the ether layer to a150-mL beaker (counter
18、balance the beaker if the amount ofunsaponifiable matter is small and important) and evaporateover a hot-water bath until practically free of ether. Heat thebeaker at 75 to 80C until constant weight is obtained.NOTE 1A 30 % alcoholic solution by volume is the most satisfactorysolution from which to
19、extract the unsaponifiable matter.NOTE 2If emulsions form, add 5 mL of alcohol, pouring it down theside of the funnel.NOTE 3It is important to maintain the volume of ether at not less than150 mL, otherwise small quantities of unsaponifiable matter may be lost.NOTE 4To check whether or not the unsapo
20、nifiable matter is freefrom fatty acids, dissolve the residue in 10 mL of freshly boiled neutralalcohol and titrate with 0.1 N alcoholic KOH solution, using phenolphtha-lein as the indicator. Not more than 0.1 mL should be required forneutralization. If more is required, the determination has not be
21、en carriedout effectively and must be repeated.6. Calculation6.1 Calculate the unsaponifiable matter as follows:U 5 R/G! 3 P (1)where:U = unsaponifiable nonvolatile matter, %,R = weight of residue, g,G = weight of desulfated fatty matter, g, andP = desulfated fatty matter, %.7. Precision and Bias7.1
22、 This test method is adopted from the procedures of theAmerican Leather ChemistsAssociation where it has long beenin use and was approved for publication before the inclusion ofprecision and bias statements was mandated. The originalinterlaboratory test data are no longer available. The user iscauti
23、oned to verify by the use of reference materials, ifavailable, that the precision and bias (or reproducibility) of thistest method is adequate for the contemplated use.8. Keywords8.1 leather; nonvolatile matter; sulfated oils; unsaponifiableASTM International takes no position respecting the validit
24、y 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 responsibility.This standard is subject
25、 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 ASTM International Headquarter
26、s. 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 address shown below.This standard i
27、s 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 5553 95 (2006)2
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