1、Designation: D3673 89 (Reapproved 2009)Standard Test Methods forChemical Analysis of Alpha Olefin Sulfonates1This standard is issued under the fixed designation D3673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t 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 These test methods cover the chemical analysis of alphaolefin sulfonates. The analytical procedures appear in thefollowin
3、g order:SectionsMoisture by the Distillation Method 4-8Sodium Sulfate 9-14Neutral Oil 15-19Chlorides Calculated as Sodium Chloride (NaCl) 20-24Alkalinity 25-29pH 30 and 31Determination of Color 32-37Determination of Active Content by Methylene Blue Titration 38-471.2 The values stated in SI units ar
4、e 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
5、 and determine the applica-bility of regulatory limitations prior to use. For specificprecaution statement see 36.1. Material safety data sheets areavailable for reagents and materials. Review them for hazardsprior to usage.2. Referenced Documents2.1 ASTM Standards:2D1172 Guide for pH of Aqueous Sol
6、utions of Soaps andDetergentsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D3049 Test Method for Synthetic Anionic Ingredient byCationic Titration3. Purity of Reagents3.1 Reagent-grade chemicals shall be used in all tests.Unless otherwise in
7、dicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.3Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to
8、permit its use without lessening the accuracy ofthe determination.3.2 Unless otherwise indicated, references to water shall beunderstood to mean Type III reagent water conforming toSpecification D1193.MOISTURE BY THE DISTILLATIONMETHOD4. Apparatus4.1 The apparatus required shall consist of a glass f
9、laskheated by suitable means and provided with a reflux condenserdischarging into a trap and connected to the flask. Theconnections between the trap and the condenser and flask shallbe interchangeable ground joints. The trap serves to collect andmeasure the condensed water and to return the solvent
10、to theflask. A suitable assembly of the apparatus is illustrated in Fig.1.4.1.1 Flask, 1-L capacity, either the short-neck, round-bottom type, or the Erlenmeyer type.4.1.2 Heat SourceEither an oil bath (for example, stearicacid or paraffin wax) or an electric heater provided with asliding rheostat o
11、r other means of heat control.4.1.3 CondenserA water-cooled glass reflux condenser(Fig. 1), having a jacket approximately 1534 in. (400 mm) inlength, with an inner tube38 to12 in. (9.5 to 12.7 mm) inoutside diameter, and not less than14 in. (6.35 mm) in insidediameter. The end of the condenser to be
12、 inserted in the trapmay be ground off at an angle of 30 from the vertical axis ofthe condenser. When inserted into the trap, the tip of the1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.12 on Ana
13、lysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved Oct. 1, 2009. Published March 2010. Originallyapproved in 1978. Last previous edition approved in 2003 as D3673 89(2003).DOI: 10.1520/D3673-89R09.2For referenced ASTM standards, visit the ASTM webs
14、ite, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For sug
15、gestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM Internationa
16、l, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.condenser shall be about14 in. (7 mm) above the surface of theliquid in the trap after the distillation conditions have beenestablished. Fig. 1 shows a conventional sealed-in type ofcondenser, but any other conden
17、ser fulfilling the detailedrequirements of this paragraph may be used.4.1.4 TrapFor greatest accuracy several trap sizes areallowable, depending upon the percentage of moisture ex-pected:Moisture Expected, % Size of Trap, mL0to5,incl 5Over 5 to 17, incl 10Over 17 to 30, incl 25Over 30 to 50, incl 25
18、Over 50 to 70, incl 25Over 70 to 85, incl 25Traps made of well-annealed glass, constructed essentiallyas shown in Fig. 1, and graduated to contain one of thefollowing specified volumes at 20C shall be used:4.1.4.1 Trap, 5-mL capacity, subdivided into 0.1-mL divi-sions with each 1-mL line numbered (5
19、 mL at top). The errorin any indicated capacity may not be greater than 0.05 mL.4.1.4.2 Trap, 10-mL capacity, subdivided from 0 to 1 mL in0.1-mL divisions and from 1 to 10 mL in 0.2-mL divisions.4.1.4.3 Trap, 25-mL capacity, subdivided from 0 to 1 mL in0.1-mL divisions and from 1 to 25 mL in 0.2-mL
20、divisions.NOTE 1The condenser and trap should be thoroughly cleaned beforeuse.5. Solvent5.1 XyleneSaturate xylene with water by shaking with asmall quantity of water and distill. Use the distillate for thedetermination.6. Procedure6.1 Transfer to the 1000-mL flask (equipped with the size ofthe trap
21、specified in 4.1.4) an amount of sample according tothe percentage of moisture expected, as follows:Moisture Expected, %Weight of Sampleto Be Used, gA0 to 5, incl 50 6 5Over 5 to 17, incl 50 6 5Over 17 to 30, incl 40 6 4Over 30 to 50, incl 30 6 3Over 50 to 70, incl 30 6 3Over 70 to 85, incl 25 6 2AW
22、eighed to the nearest 0.25 g.Immediately add about 250 mL of xylene. Place a small, thinsheet of long-fiber, chemical-resistant glass4wool on thesurface of the xylene. The glass wool should be thoroughlydried in the oven and held in the desiccator before use.6.2 Connect the flask and receiver to the
23、 condenser and poursufficient xylene down the condenser tube to cause a slightoverflow through the side tube. Wrap the flask and tube leadingto the receiver with glass wool, so that refluxing will be underbetter control.6.3 Heat the oil bath with a gas burner or other source ofheat, or apply heat di
24、rectly to the flask with an electric heaterand distill slowly. The rate at the start should be approximately100 drops per minute. When the greater part of the water hasdistilled over, increase the distillation rate to 200 drops perminute until no more water is collected. Rinse during thedistillation
25、 with 5-mL portions of xylene to wash down anymoisture adhering to the walls of the condenser. The water inthe receiver may be made to separate from the xylene by usinga spiral copper or Nichrome5wire. Move the wire up and downin the condenser occasionally, thus causing the water to settleat the bot
26、tom of the receiver. Reflux for at least 2 h, and shutoff the heat at the end of this period.NOTE 2In especially difficult cases of boil-over, add 10 to 15 mL ofoleic acid before beginning the distillation. Wash down the condenser with10 mL of xylene. Adjust the temperature of the distillate to 20C
27、and readthe volume of water.4Borosilicate glass has been found satisfactory for this purpose.5“Nichrome” is a trademark of the Driver-Harris Co.FIG. 1 Assembly of Distillation ApparatusD3673 89 (2009)27. Calculation7.1 Calculate the percentage of moisture as follows:Moisture, % 5 V 3 0.998!/W 3 100
28、(1)where:V = volume of water, mL at 20C, andW = weight of sample, g.8. Precision and Bias68.1 Repeatability (Single Analyst)The standard deviationof results (each the average of duplicates) obtained by the sameanalyst on different days, has been estimated to be 0.16 %absolute at 9 degrees of freedom
29、. Two such averages should beconsidered suspect (95 % confidence level) if they differ bymore than 0.5 % absolute.8.2 Reproducibility (Multilaboratory)The standard devia-tion of results (each the average of duplicates) obtained byanalysts in different laboratories, has been estimated to be0.47 % abs
30、olute at 8 degrees of freedom. Two such averagesshould be considered suspect (95 % confidence level) if theydiffer by more than 1.5 % absolute.8.3 Checking Limits for DuplicatesReport the moisturecontent of the sample to the nearest 0.01 %. Duplicate runs thatagree within 1.3 % are acceptable for av
31、eraging (95 % confi-dence level).SODIUM SULFATE9. Apparatus9.1 Beakers, 50 and 100-mL capacity.9.2 Buret, 10-mL capacity, with 0.05-mL divisions.9.3 Volumetric Flasks, 50, 250, and 1000-mL capacity.9.4 Magnetic Stirrer, with TFE-fluorocarbon-coated stirringbars.9.5 Transfer Pipet, 5-mL capacity.9.6
32、Viewing LampSmall tungsten lamp or flashlight.10. Reagents and Materials10.1 Acetone.10.2 Barium Perchlorate Solution (0.02N)Dissolve 3.4 gof anhydrous Ba(ClO4)2in water and dilute the solution to 1 L.10.3 2-Benzyl-2-thiopseudourea Hydrochloride Solution(7 %)7Dissolve 7 g in 100 mL of water. Prepare
33、 thesolution fresh daily.10.4 Hydrochloric Acid (1 N)Dilute 83 mL of hydrochlo-ric acid (HCl, sp gr 1.19) to 1 L with water.10.5 Hydrochloric Acid (0.1 N)Dilute 8.3 mL of HCl (spgr 1.19) to 1 L with water.10.6 Phenolphthalein Indicator Solution (10 g/L)Dissolve1gofphenolphthalein in 100 mL of 95 % e
34、thanol.10.7 Sodium Sulfate Solution (0.02 N)Dry the anhydrous,reagent-grade salt (Na2SO4)for4hat105C. Weigh about0.355 g of the dried salt into a 100-mL beaker. Record theweight within 60.1 mg. Dissolve the salt water. Quantitativelytransfer the solution to a 250-mL volumetric flask and dilute itto
35、volume with water. Calculate the normality of the solution asfollows:Normality, N15 0.05632 3 W (2)where W = grams of Na2SO4.10.8 Sulfonazo III Indicator Solution8Dissolve 0.1 g ofSulfonazo III in 100 mL of water. Pass the solution through acation exchange column if it looks blue rather than lavende
36、rwhen edge-lighted by a tungsten lamp.10.9 Filter Paper, smooth, hardened, ashless.11. Standardization11.1 Pipet 5.0-mL aliquots of standard Na2SO4solution intoeach of two 50-mL beakers. Place stirring bars in each beaker.Add 20 mL of acetone, 2 drops of 1 N HCl, and 4 to 5 dropsof Sulfonazo III ind
37、icator solution to each beaker.11.2 Titrate each Na2SO4solution with Ba(ClO4)2solutionusing a 10-mL buret. Stir the solution magnetically. Illuminatethe solution horizontally with a small tungsten lamp at the sideof the beaker. Titrate slowly to a color change from lavender-pink to blue (about 0.3 m
38、L of Ba(ClO4)2solution is required toproduce a good initial lavender color).11.3 From each titration, calculate the normality of theBa(ClO4)2solution as follows. Average the values obtained.Normality, N255 3 N1V(3)where:N1= normality of the Na2SO4solution, andV = millilitres of Ba(ClO4)2solution req
39、uired for 5-mLaliquot of Na2SO4solution.12. Procedure12.1 Weigh a 2-g sample into a 100-mL beaker or a 50-mLflask. Record the weight to 61 mg.12.2 Place a stirring bar in the container. Add 25 mL ofwater and stir until the sample is dissolved.12.3 Add a few drops of phenolphthalein indicator solutio
40、n.Add 0.1 N HCl until the solution is just acid. Do notover-acidify.12.4 Place the container in a cold-water bath (below 20C)on the magnetic stirrer. Add 10 mL of 2-benzyl-2-thiopseudourea hydrochloride at a fast drip through a buretwith vigorous stirring. Do not whip the liquid into a foam.12.5 Sti
41、r the solution for 15 min more in the cold bath.Remove the solution from the bath and let it settle for a fewminutes at room temperature.12.6 Filter the solution through filter paper into a 50-mLvolumetric flask. Wash the filter cake with water. Use thewashes to dilute the solution to volume.12.7 Pi
42、pet a 5-mL aliquot into a 50-mL beaker. Add 20 mLof acetone, 2 drops of 1 N HCl, and 4 to 5 drops of SulfonazoIII indicator solution.6Supporting data are available from ASTM Headquarters, 100 Barr HarborDrive, West Conshohoken, PA 19428. Request RR:D12-1002 and RR:D12-1007.7Eastman Organic Chemical
43、No. 2124 has been found satisfactory for thispurpose.8Sulfonazo III 3,6-bis-( o-sulfophenylazo)-4,5-dihydroxy-2,7-naphthalenedi-sulfonic acid is available from the Aldrich Chemical Co.D3673 89 (2009)312.8 Titrate the solution slowly with 0.02 N Ba(ClO4)2solution. Use magnetic stirring. Illuminate th
44、e solution hori-zontally with a small tungsten lamp at the side of the beaker.Titrate to a color change from lavender-pink to a blue color thatpersists for 1 min.NOTE 3The titration should be between 1 and 5 mL. If the titration isgreater than 5 mL, use a smaller aliquot of the sample and add water
45、tobring the aqueous volume to 5 mL total. If the titration is less than 1 mL,pipet a 10-mL aliquot into a 100-mL beaker and add 40 mL of acetone, 4drops of 1 N HCl, and 8 to 10 drops of Sulfonazo III indicator solution.13. Calculation13.1 Calculate the concentration of Na2SO4as follows:Na2SO4,wt%535
46、5 N23 VA 3 W(4)where:N2= normality of Ba(ClO4)2solution,V = volume of Ba(ClO4)2solution, mL,A = volume of aliquot, mL, andW = weight of sample, g.14. Precision and Bias614.1 Repeatability (Single Analyst)The standard devia-tion of results (each the average of duplicates) obtained by thesame analyst
47、on different days, has been estimated to be 0.01 %absolute at 8 degrees of freedom. Two such averages should beconsidered suspect (95 % confidence level) if they differ bymore than 0.03 % absolute.14.2 Reproducibility (Multilaboratory)The standard de-viation of results (each the average of duplicate
48、s) obtained byanalysts in different laboratories, has been estimated to be0.06 % absolute at 7 degrees of freedom. Two such averagesshould be considered suspect (95 % confidence level) if theydiffer by more than 0.2 % absolute.14.3 Checking Limits for DuplicatesReport the sodiumsulfate of the sample
49、 to the nearest 0.01 %. Duplicate runs thatagree within 0.1 % are acceptable for averaging (95 % confi-dence level).NEUTRAL OIL15. Apparatus15.1 Separatory Funnels, 250-mL capacity, with TFE-fluorocarbon stopcocks.15.2 Erlenmeyer Flasks, 250-mL capacity.15.3 Beakers, 250-mL capacity.15.4 Steam Bath.15.5 Vacuum Desiccator.16. Reagents16.1 Ethanol, freshly boiled, 95 % or higher and neutral tophenolphthalein indicator, conforming to either Formula No.3A or No. 30 of the U.S. Bureau of Internal Revenue.16.2 Petroleum Ether, with a distillation ra
