1、Designation: D5553 95 (Reapproved 2012)Standard Test Method forDetermination of the Unsaponifiable Nonvolatile Matter inSulfated Oils1This standard is issued under the fixed designation D5553; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of 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 unsa-ponifiable, nonvolatile (above 80C) matter
3、 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 asstandard. No other units of measurement are i
4、ncluded in thisstandard.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 prio
5、r to use.2. Referenced Documents2.1 ASTM Standards:2D5350 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Titration, Test Method AD5351 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Extraction Titration, TestMethod BD5353 Test Method for De
6、termination of Total DesulfatedFatty Matter3. Significance 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 requi
7、red for thesaponification consists of a glass flask provided 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
8、g of potassium hydroxide (KOH) in water anddilute to 1 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
9、Fatty MatterDetermine the desulfatedfatty matter as described in the determination of total desul-fated fatty matter. See Test Methods D5350, D5351, andD5353.5.1.2 SaponificationAccurately weigh 2 to 2.5 g of thedesulfated fatty matter in the flask, add 25 mL of the alcoholicKOH solution, and simmer
10、 the contents (without loss ofalcohol) for 1 h with 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 separatoryfunn
11、el. Extract the solution while still warm (about 30C) 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
12、 andextract in a similar manner with two 50-mL portions 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 theet
13、her layer twice more with 20-mL portions of water, shakingvigorously after each addition.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
14、Leather Chemists Assn.(Method H 471957).Current edition approved April 1, 2012. Published April 2012. Originallyapproved in 1994. Last previous edition approved in 2006 as D5553 95(2006).DOI: 10.1520/D5553-95R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cus
15、tomer Service at serviceastm.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.5.1.5 Alkali and Water WashingAdd
16、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 20 mL of water, shaking vigorously.Continue washing with 20 mL of KOH so
17、lution followed by 20mL of water, shaking vigorously after each addition, until 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 phenolphthale
18、in.5.1.6 Solvent RemovalTransfer the ether layer to a150-mL beaker (counterbalance 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 % a
19、lcoholic solution by volume is the most satisfactorysolution from which to 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
20、 unsaponifiable matter may be lost.NOTE 4To check whether or not the unsaponifiable 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 re
21、quired forneutralization. If more is required, the determination has not been 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
22、fatty matter, g, andP = desulfated fatty matter, %.7. Precision and Bias7.1 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
23、originalinterlaboratory test data are no longer available. The user iscautioned 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
24、; unsaponifiableASTM 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 expressly advised that determination of the validity of any such patent rights, and the riskof infringement of
25、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 revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for ad
26、ditional standardsand should be addressed to ASTM 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
27、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 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5553 95 (2012)2
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