ASTM_D_5566_-_95_2011.pdf

Designation:D556695(Reapproved 2011)Standard Test Method forDetermination of Inorganic Salt Content of Sulfated andSulfonated Oils1This standard is issued under the fixed designation D5566;the number immediately following the designation indicates the year oforiginal adoption or,in the case of 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 a sample ofsulfonated or sulfated oil,or both,the inorganic sulfates,chlorides,and all other salts that are insoluble in a mixture ofoleic acid and carbon tetrachloride.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 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.Significance and Use2.1 This test method is intended to be used for the determi-nation of the inorganic salt content of sulfated and sulfonatedfats and oils for the purpose of quality control.3.Apparatus3.1 Gooch Crucible or Filter PaperEither may be usedfor filtering.Ignite the Gooch crucible in a larger crucible,supported by a ring and assembled as shown in Fig.1.If filterpaper is used,it may be a 9-cm general purpose ashless filterpaper.3.2 Thermometer.4.Reagents4.1 Carbon Tetrachloride(CCl4).4.2 Ethyl Ether.4.3 Oleic Acid.5.Procedure5.1 The procedure consists of dehydrating the sample,dissolving in a solvent,filtering,igniting,and weighing theresidue.In the presence of ammonium salts,the residue is notignited but only dried to constant weight.The presence ofsodium acetate does not interfere with this test method.5.1.1 In the Absence of Ammonium SaltsWeigh 3 to 5 g ofthe sample and place in a 250-mL beaker,add an approxi-mately equal amount of oleic acid,and heat the mixture on anoil bath,while stirring constantly with a thermometer,at atemperature of 105 to 110C until practically free from water.Continue the heating until the temperature of the contentsreaches 118 to 120C and maintain at that temperature forabout 5 min.If the dehydrated sample upon cooling does notremain liquid,add more oleic acid.Dissolve the dehydratedsample in 100 mL of CCl4warmed to 50 to 55C,and filterthrough a counterpoised filter paper or a Gooch crucible.Pass75 mL of CCl4through the crucible and again ignite,cool in adesiccator,and weigh.Repeat the process of washing withCCl4until there is no further loss in weight.Wash the residuewith three 15-mL portions of a solution of oleic acid in CCl4(2%),then with six 15-mL portions of hot CCl4,and finallywith two 15-mL portions of ether or until the residue is freefrom oil.Take care that the top of the filter is thoroughlywashed.Transfer the last traces of the residue to the filter byallowing the solvent to evaporate when the salts become freeflowing.Dry the residue at 125 to 130C for 45 min,cool in adesiccator,and weigh.Ignite the residue at a dull red heat for15 min,weigh,and repeat the ignition until constant weight isobtained.5.1.2 In the Presence of Ammonium SaltsProceed asdescribed in 6.1.1 for the determination of inorganic salts in theabsence of ammonium salts with the following exceptions:(1)in preparing the Gooch crucible,do not ignite but heat it at 1056 2C for 45 min and repeat the heating until constant weightis obtained,and(2)heat the residue,whether in a Goochcrucible or on a filter paper as in(1),but do not ignite it.6.Calculation6.1 The method of calculation depends upon whether or notammonium salts are present in the sample.1This 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 48-1957).Current edition approved Jan.1,2011.Published March 2011.Originallyapproved in 1994.Last previous edition approved in 2006 as D5566 95(2006).DOI:10.1520/D5566-95R11.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.1.1 Calculate the inorganic sulfates and chlorides includ-ing ammonium salts as follows:Inorganic sulfates and chlorides,including(1)ammonium salts,%5A/B!3100where:A=weight of dried residue,g,andB=weight of sample,g.6.1.2 Calculate the nonvolatile inorganic sulfates and chlo-rides(in the absence of ammonium salts)as follows:Nonvolatile,inorganic sulfates and chlorides;%5A/B!3100(2)where:A=weight of ignited residue,g,andB=weight of sample,g.NOTE1In the absence of ammonium salts,the difference between thepercentage of the dried residue and the percentage of the ignited residueshall not be greater than 0.25%.7.Precision and Bias7.1 This tes