1、Designation: D3673 89 (Reapproved 2016)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 48Sodium Sulfate 914Neutral Oil 1519Chlorides Calculated as Sodium Chloride (NaCl) 2024Alkalinity 2529pH 30 and 31Determination of Color 3237Determination of Active Content by Methylene Blue Titration 38471.2 The values stated in SI units are to be
4、 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 de
5、termine 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 Solutions
6、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 indicated
7、, 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 permit
8、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 flaskhea
9、ted 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 to thef
10、lask. 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 or other
11、 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 insert
12、ed 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 Analysis a
13、nd Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved July 1, 2016. Published August 2016. Originallyapproved in 1978. Last previous edition approved in 2009 as D3673 89(2009).DOI: 10.1520/D3673-89R16.2For referenced ASTM standards, visit the ASTM website, w
14、ww.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 suggestion
15、s 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.Copyright ASTM International, 100 B
16、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1condenser 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 condenser fulf
17、illing 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 25Over 50
18、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 mL at t
19、op). 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 division
20、s.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 specifie
21、d in 4.1.4) an amount of sample according tothe percentage of moisture expected, as follows:Moisture Expected, %Weight of Sampleto Be Used, gA0to5,incl 505Over 5 to 17, incl 50 5Over 17 to 30, incl 40 4Over 30 to 50, incl 30 3Over 50 to 70, incl 30 3Over 70 to 85, incl 25 2AWeighed to the nearest 0.
22、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 condenser and poursuffi
23、cient 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 directly to the flask with
24、 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 with 5-mL portions of x
25、ylene 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 bottom of the receiver. Ref
26、lux 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 and readthe volume of wa
27、ter.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 (2016)27. Calculation7.1 Calculate the percentage of moisture as follows:Moisture, % 5 V 30.998!/W# 3100 (1)where:V = volume of wa
28、ter, 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. Two such averages shoul
29、d 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 % absolute at 8 degrees of fre
30、edom. 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 averaging (95 % confi-dence
31、 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 Viewing LampSmall tungste
32、n 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 %)7Dissolve7gin100mLofwater. Prepare the solutionfresh daily.10.4 Hy
33、drochloric 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)Dissolve1 g of phenolphthalein in 100 mL of 95 % ethanol.10.7 Sodium Sulfate So
34、lution (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 volume with water. Calculate
35、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 lavenderwhen edge-lighted by a tungs
36、ten 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 indicator solution to each beake
37、r.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 mL of Ba(ClO4)2solution is req
38、uired 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 required for 5-mLaliquot of Na2S
39、O4solution.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 solution.Add 0.1 N HCl until the sol
40、ution 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 Stir the solution for 15 min mor
41、e in the cold bath.Remove the solution from the bath and let it settle for a fewminutes at room temperature.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 No. 2124 has been found s
42、atisfactory 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 (2016)312.6 Filter the solution through filter paper into a 50-mLvolumetric flask. Wash the filter cake with water. Use thewashes to
43、 dilute the solution to volume.12.7 Pipet 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.12.8 Titrate the solution slowly with 0.02 N Ba(ClO4)2solution. Use magnetic stirring. Illuminate the solution hori-zontally with
44、 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 tobring the aqueous volume to
45、 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%5355 N23 VA 3 W(4)where:N2= norm
46、ality 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 deviationof results (each the average of duplicates) obtained by the sameanalyst on different days, has been est
47、imated 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 duplicates) obtained byanalysts in diffe
48、rent 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 to the nearest 0.01 %. Duplica
49、te 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 range between 30
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