1、Designation: D 3673 89 (Reapproved 2003)Standard Test Methods forChemical Analysis of Alpha Olefin Sulfonates1This standard is issued under the fixed designation D 3673; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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 These test methods cover the chemical analysis of alphaolefin sulfonates. The analytical procedures appear in thefollo
3、wing 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 This standard does not purpor
4、t 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. For specificprecaution statement see 36.1. Mate
5、rial safety data sheets areavailable for reagents and materials. Review them for hazardsprior to usage.2. Referenced Documents2.1 ASTM Standards:D 1172 Test Method for pH of Aqueous Solutions of Soapsand Detergents2D 1193 Specification for Reagent Water3D 1209 Test Method for Color of Clear Liquids
6、(Platinum-Cobalt Scale)4D 3049 Test Method for Synthetic Anionic Ingredient byCationic Titration23. Purity of Reagents3.1 Reagent-grade chemicals shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalR
7、eagents of the American Chemical Society, where suchspecifications are available.5Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.3.2 Unless otherwise indicated, references
8、 to water shall beunderstood to mean Type III reagent water conforming toSpecification D 1193.MOISTURE BY THE DISTILLATIONMETHOD4. Apparatus4.1 The apparatus required shall consist of a glass flaskheated by suitable means and provided with a reflux condenserdischarging into a trap and connected to t
9、he 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 theflask. A suitable assembly of the apparatus is illustrated in Fig.1.4.1.1 Flask, 1-L capacity, either
10、 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 means of heat control.4.1.3 CondenserA water-cooled glass reflux condenser(Fig. 1), having a jacket
11、 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 inserted in the trapmay be ground off at an angle of 30 from the vertical axis ofthe condenser. When inser
12、ted into the trap, the tip of thecondenser 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 of1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Othe
13、r Detergents, and are the direct responsibility of SubcommitteeD12.12 on Analysis of Soaps and Synthetic Detergents.Current edition approved May 26, 1989. Published July 1989. Originallypublished as D 3673 78. Last previous edition D 3673 87.2Annual Book of ASTM Standards, Vol 15.04.3Annual Book of
14、ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 06.04.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemic
15、als, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.condenser, but any other condenser
16、 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, mL0 to 5, incl 5Over 5 to 17, incl 10Over 17 to 30, incl 25Over 30 to 50, incl 25
17、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
18、 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
19、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
20、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
21、eighed to the nearest 0.25 g.Immediately add about 250 mL of xylene. Place a small, thinsheet of long-fiber, chemical-resistant glass6wool 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
22、 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
23、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
24、 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 Nichrome7wire. Move the wire up and downin the condenser occasionally, thus causing the water to settleat the bot
25、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
26、and readthe volume of water.7. Calculation7.1 Calculate the percentage of moisture as follows:Moisture, % 5 V 3 0.998!/W# 3 100 (1)6Borosilicate glass has been found satisfactory for this purpose.7“Nichrome” is a trademark of the Driver-Harris Co.FIG. 1 Assembly of Distillation ApparatusD 3673 89 (2
27、003)2where:V = volume of water, mL at 20C, andW = weight of sample, g.8. Precision and Bias88.1 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 freed
28、om. 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 % a
29、bsolute 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
30、averaging (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.
31、6 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 %)9Dissolve7gin100mLofwater. Prepare thes
32、olution 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 % ethano
33、l.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 volum
34、e 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 Solution10Dissolve 0.1 g ofSulfonazo III in 100 mL of water. Pass the solution through acation exchange column if it looks blue rather than lavenderwhe
35、n 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 indicat
36、or 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 mL of
37、 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 require
38、d 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 solution.Ad
39、d 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 Stir th
40、e 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 Pipet
41、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 a small tungsten lamp at the side of the
42、beaker.Titrate to a color change from lavender-pink to a blue color thatpersists for 1 min.8Supporting data are available from ASTM Headquarters, 100 Barr HarborDrive, West Conshohoken, PA 19428. Request RR:D12-1002 and RR: D12-1007.9Eastman Organic Chemical No. 2124 has been found satisfactory for
43、thispurpose.10Sulfonazo III 3,6-bis-(o-sulfophenylazo)-4,5-dihydroxy-2,7-naphthalenedi-sulfonic acid is available from the Aldrich Chemical Co.D 3673 89 (2003)3NOTE 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 to
44、bring 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%5355
45、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 Bias814.1 Repeatability (Single Analyst)The standard devia-tion of results (each the average of duplicates) obtained by thesame analyst on
46、 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 duplicates)
47、 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 t
48、o 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
49、.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 30and 60C or n-pentane having a distillation range between33C and 41C.16.3 Ethanol-Water (1 + 1)Mix 1 volume of ethanol with1 volume of water.16.4 Phenolphthalein Indicator Solution.16.5 Sodium Hydroxide Solution (0.1N)Dissolve ap-proximately4gofsodium hydroxide (NaOH) in water anddilut
