1、Designation: D 5354 95 (Reapproved 2006)Standard Test Method forDetermination of Total Active Ingredients in Sulfonated andSulfated Oils1This standard is issued under the fixed designation D 5354; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 of 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 totalactive ingredients in a sample of sul
3、fonated or sulfated oil, orboth, as it exists in the original sample by extracting theundecomposed sulfonated or sulfated fat and other fatty matterover an acidified concentrated salt solution. Free alkali or alkalibound as soap is not included. This test method was derivedfrom Test Methods D 500.NO
4、TE 1In the case of sulfated oils only, this determination may alsobe estimated by calculation (see 6.3), as it is equivalent to the sum of thedesulfated fatty matter and neutralized organically combined sulfuricanhydride.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This st
5、andard 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. Referenced Documents2.1
6、 ASTM Standards:2D 500 Test Methods of Chemical Analysis of Sulfonatedand Sulfated Oils3. Significance and Use3.1 This test method is intended for the determination of thetotal active ingredients contained in sulfonated and sulfatedoils. Free alkali and alkaline soaps are excluded.4. Reagents4.1 Eth
7、yl Ether.4.2 Methyl Orange Indicator Solution (1 g/L)Dissolve 0.1g of methyl orange in 100 mL of water.4.3 Sodium Chloride (NaCl), solid.4.4 Sodium Sulfate (Na2SO4), anhydrous.4.5 Potassium Hydroxide, Alcoholic Standard Solution (0.5N)Accurately prepare and standardize a 0.5 N alcoholicpotassium hyd
8、roxide (KOH) solution, the strength of whichshall be expressed as milligrams of KOH per millilitre; 1 mLof 0.5 N alcoholic KOH solution is equivalent to 28.05 mg ofKOH.5. Procedure5.1 The procedure consists of isolating and purifying thefatty matter as it exists in the original oil by dissolving the
9、sample in a solvent, acidifying and washing with saturatedbrine, and weighing the purified extract. Proceed as describedin the determination of organically combined sulfuric anhy-dride, Test Method B, in the absence of ammonia (6.1.1),retaining the separated active ingredients in the 150-mL beakerin
10、stead of transferring it to a crucible. Evaporate the filtrate toa total volume of about 20 mL, add exactly 2 mL of alcoholicKOH solution, mix the contents by swirling, and finallyevaporate until practically free from ether.NOTE 2With highly sulfonated or sulfated oil, it may be necessary toadd 5 to
11、 10 mL of the alcoholic KOH solution in order to stabilize theresidue.5.2 Dry the residue at 108 to 112C for 112 h, cool in adesiccator, and weigh. Repeat the heating for 30-min periodsuntil constant weight is obtained.6. Calculation6.1 Correction for the Alkali AddedCalculate the correc-tion for th
12、e alkali added as follows:Correction for alkali added, g 5 0.0006791 AS (1)where:A = millilitres of KOH solution added,1This test method is under the jurisdiction ofASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This testmethod was developed in
13、 cooperation with the American Leather Chemists Assn.(Method H 46-1957).Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1993. Last previous edition approved in 2001 as D 5354 95(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
14、ASTM Customer 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.S = strength of KOH soluti
15、on, mg of KOH/mL,and0.0006791 = molecular ratio of (K H): KOH divided by1000.6.2 Total Active IngredientsCalculate the total activeingredients as follows:Total active ingredients, % 5 B 2 C!/D 3 100 (2)where:B = weight of residue, g,C = alkali correction, andD = weight of sample, g.6.3 Total Active
16、Ingredients Calculation Method (for Sul-fated Oils Only)Calculate the total active ingredients by thecalculation method that is applicable to sulfated oils only, asfollows:T 5 P 1 NaSO42/SO2! 3 Y (3)orT 5 P 1 1.4875 3 Y (4)where:T = total active ingredients, %P = total desulfated fatty matter, %, an
17、dY = percentage of combined SO3.NOTE 3The factor 1.4875 is based on the assumption that thedesulfated fatty matter becomes polymerized at the point where the SO3splits off and no hydroxyl groups are formed. If the latter are formed thefactor becomesNaSO32 1!/SO35 1.275. (5)Calculated results were in
18、 better agreement with actual determinationswhen the higher factor was used.7. Precision and Bias7.1 Although this test method is widely used, precision andbias information is not available at this time.8. Keywords8.1 leather; sulfonated and sulfated oils; total activeingredientsASTM International t
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21、essed 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 the ASTM Committee on Standards, at
22、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).D 5354 95 (2006)2
