1、Designation: D4252 89 (Reapproved 2009)Standard Test Methods forChemical Analysis of Alcohol Ethoxylates and AlkylphenolEthoxylates1This standard is issued under the fixed designation D4252; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 These test methods cover the various test methods usedto evaluate those properties pertinent to th
3、e characterization ofalcohol ethoxylates and alkylphenol ethoxylates with respect tosuitability for desired uses.1.2 The procedures for sampling and analysis appear in thefollowing order:SectionsSamplingLiquids 6Solids 7Methods of Chemical AnalysisWater or moisture 8Refractive index 9 and 10pH 11Aci
4、dity or basicity 12 and 13Hydroxyl number 14-20Cloud point 21Iodine number 22Ash 23Iron 24Ethylene oxide content 25Polyethylene glycols 26-321.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport
5、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. Material SafetyData Sheets are available for reag
6、ents and materials. Reviewthem for hazards prior to usage. Specific hazard statementsappear in Section 5 and Note 1 and Note 3.2. Referenced Documents2.1 ASTM Standards:2D459 Terminology Relating to Soaps and Other DetergentsD482 Test Method for Ash from Petroleum ProductsD1068 Test Methods for Iron
7、 in WaterD1172 Guide for pH of Aqueous Solutions of Soaps andDetergentsD1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1218 Test Method for Refractive Index and RefractiveDispersion of Hydrocarbon LiquidsD1613 Test Method for Acidity in Volat
8、ile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD1959 Test Method for Iodine Value of Drying Oils andFatty Acids3D2024 Test Method for Cloud Point of Nonionic Surfac-tantsD2959 Test Method for Ethylene Oxide Content of Poly-ethoxylated Nonionic SurfactantsE
9、180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical AnalysisE203 Test Method for Water Using Volumetric Karl FischerTitration
10、E394 Test Method for Iron in Trace Quantities Using the1,10-Phenanthroline Method3. Significance and Use3.1 Alcohol ethoxylates and alkylphenol ethoxylates areimportant surfactants in household and industrial cleaners.They may be used as either nonionic surfactants or sulfated and1These test methods
11、 are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Current edition approved Oct. 1, 2009. Published December 2009. Originallyapprove
12、d in 1983. Last previous edition approved in 2003 as D4252 89(2003).DOI: 10.1520/D4252-89R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document
13、Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.used as anionic surfactants. Careful control of the ethoxy
14、latecharacteristics is desired as variations may result in eitherdesirable or undesirable end-use properties.4. Purity of Reagents4.1 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
15、 AnalyticalReagents of the American Chemical Society, where suchspecifications are available.4Other 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.4.2 Unless otherwise indicated
16、, references to water shall beunderstood to mean Type III reagent water conforming toSpecification D1193.5. Safety Precautions5.1 All reagents and chemicals should be handled with care.Before using any chemical, read and follow all safety precau-tions and instructions on the manufacturer label. Clea
17、n up anyspill immediately. For information on cleaning up spills refer tothe Laboratory Disposal Manual, Manufacturing ChemistsAssociation, Washington, DC.SAMPLING6. Liquids6.1 Thoroughly mix the sample before sampling. If a solidlayer or crystals have formed on the bottom of the bottle, meltin an o
18、ven or water bath at 55C and mix well before sampling.7. Solids7.1 Melt in an oven or water bath at 55C and mix wellbefore sampling. If it is necessary to heat at temperatures above60C, replace the gas cap with an inert gas, such as oxygen-freenitrogen, helium, or argon before heating.WATER OR MOIST
19、URE8. Procedure8.1 Determine water or moisture in accordance with TestMethod E203.REFRACTIVE INDEX9. Procedure9.1 Measure the refractive index at 50C in accordance withTest Method D1218.10. Precision10.1 The following criteria should be used for judging theacceptability of results:5,610.1.1 Repeatab
20、ility (Single Analyst)The standard devia-tion of results (each the average of duplicates), obtained by thesame analyst on different days, has been estimated to be0.00021 units absolute at 36 df. Two such averages should beconsidered suspect (95 % confidence level) if they differ bymore than 0.00059
21、units absolute.10.1.2 Reproducibility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be0.00059 units absolute at 7 df. Two such averages should beconsidered suspect (95 % confidence level) if
22、they differ bymore than 0.0020 units absolute.10.1.3 Checking Limits for DuplicatesReport the refrac-tive index of the sample to the nearest 0.0001. Duplicate runsthat agree within 0.00025 units are acceptable for averaging(95 % confidence level).pH11. Procedure11.1 Determine the pH in accordance wi
23、th Test MethodD1172, except prepare the solution by transferring 1 6 0.001g of the sample to a 100 mL volumetric flask and diluting inaccordance with Test Method D1172. Measure the pH 10 minafter diluting the sample solution to volume.ACIDITY OR BASICITY12. Procedure12.1 Determine acidity or basicit
24、y in accordance with TestMethod D1613 using a 3+1 solution of isopropyl alcohol andwater as the solvent and a 10-g sample.13. Precision13.1 The following criteria should be used for judging theacceptability of results:6,713.1.1 Repeatability (Single Analyst)The standard devia-tion of results (each t
25、he average of duplicates), obtained by thesame analyst on different days, has been estimated to be 0.017meq/100 g at 27 df. Two such averages should be consideredsuspect (95 % confidence level) if they differ by more than0.049 meq/100 g.13.1.2 Reproducibility (Multilaboratory)The standard de-viation
26、 of results (each the average of duplicates), obtained byanalysts in different laboratories, has been established to be0.12 meq/100 g at 5 df. Two such averages should be4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the te
27、sting 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.5The precision estimates are based on an inter
28、laboratory study on ALFONICt1412-60, MAKONt-10, NEODOLt 25-9, PLURONICt 25R1, and TERGITOL15-S-3 by nine laboratories.6Statistical analysis was performed in accordance with Practice E180 fordeveloping precision estimates. Data supporting the precision statements are on fileat ASTM International Head
29、quarters. Request RR: D12-1004.7The precision estimates are based on an interlaboratory study on ALFONICt1412-60, MAKONt-10, NEODOLt 25-9, PLURONICt 25R1 and TERGITOLt15-S-3 by six laboratories.D4252 89 (2009)2considered suspect (95 % confidence level) if they differ bymore than 0.44 meq/100 g.13.1.
30、3 Checking Limits for DuplicatesReport the acidityor basicity of the sample to the nearest 0.05 meq/100 g.Duplicate runs that agree within 0.051 meq/100 g are accept-able for averaging (95 % confidence level).HYDROXYL NUMBER14. Terminology14.1 Definition:14.1.1 hydroxyl numberthe number of milligram
31、s of po-tassium hydroxide equivalent to the hydroxyl content of1gofsample.15. Summary of Test Method15.1 The hydroxyl groups are esterified by reaction withphthalic anhydride in a pyridine medium at the temperature ofreflux of the mixture. After cooling, the excess of phthalicanhydride is hydrolyzed
32、 with water and the phthalic acidformed is titrated to the phenolphthalein end point withstandard sodium hydroxide solution. The hydroxyl content iscalculated from the difference in titration of the blank and ofthe sample solution.16. Apparatus16.1 Reflux Assembly, consisting of a reflux condenser a
33、nda 250-mL Erlenmeyer flask, 24/40 standard taper joint withTFE-fluorocarbon sleeves.16.2 Buret, 50 mL, graduated in 0.1-mL intervals. Class Aor equivalent.16.3 Pipet, 25-mL capacity, Class A or equivalent.16.4 Insulating Pad,312 by 312 by 1 in., preferably notasbestos.17. Reagents17.1 Pyridine, A.
34、R.To be acceptable, each lot should passthe following quality test: Place7gofphthalic anhydride and50 mL of pyridine (Warningsee Note 1) in a glass-stopperedflask, shake vigorously until dissolved. Heat at 50 or 60C for30 min, allow to stand at room temperature in the dark for 24h and then measure t
35、he Pt-Co color (Test Method D1209). Thepyridine is acceptable if the color does not exceed 200.NOTE 1Warning: Avoid breathing pyridine vapors, as they are toxic.Dispose of pyridine wastes in a well ventilated hood.17.2 Sodium Hydroxide,(1N), carbonate free. Purchase orprepare, standardize, and store
36、 according to Practice E200.17.3 Phthalic Anhydride ReagentDissolve 98 6 1gofphthalic anhydride in 700 mL of pyridine (Note 1), shake toeffect solution. Store in a brown bottle. Preferably, the solutionshould stand overnight before using. Prepare a fresh reagenteach week or more frequently if the Pt
37、-Co color (Test MethodD1209) exceeds a value of 200.17.4 Sodium Hydroxide (0.1 N)Purchase or prepare, stan-dardize, and store according to Practice E200.17.5 Hydrochloric Acid (0.1 N)Purchase or prepare bydiluting 8.3 mL of concentrated hydrochloric acid to 1 L withdistilled water. Standardize and s
38、tore according to PracticeE200.17.6 Phenolphthalein Indicator SolutionDissolve1gofphenolphthalein in 100 mL of pyridine.17.7 Isopropyl Alcohol,A.R.18. Procedure18.1 Weigh into a clean and dry 250-mL Erlenmeyer flaskwith ground glass joint to the nearest 0.1 mg an amount ofsample calculated by means
39、of the following equation but donot use more than 10 g of sample:Amount of Sample, g 5MF 3 100(1)where:M = molecular weight of sample andF = number of hydroxyl groups per molecule.18.2 Pipet accurately 25 mL of phthalic anhydride reagentinto the flask and swirl to effect solution. Add two boilingchi
40、ps, attach a dry reflux condenser with a ground glass jointfitted with a TFE-fluorocarbon sleeve to the flask, and refluxfor1honanelectric hotplate.18.3 Turn off the hotplate and insert an insulated padbetween the flask and the hot plate. Allow to cool for 20 min.Wash down the condenser, first with
41、25 mL of pyridine andthen with 25 mL of water.18.4 Remove the flask from the condenser.Add 4 or 5 dropsof phenolphthalein indicator to the flask and titrate withstandard 1 N sodium hydroxide solution to a faint pink endpoint (Note 2).18.5 Make a blank determination following 18.2-18.4.NOTE 2It is es
42、sential that the sample titration requires at least threefourths of the blank titration. The difference between the two titrationsshould be of the order of 10 mL. If this is not the case the sample sizeshould be adjusted accordingly and the analysis rerun.18.6 Determine the free acidity or free alka
43、linity as de-scribed in Section 12 or as follows: To 25 mL of a 3 + 1isopropyl alcohol/water mixture in a 250-mL Erlenmeyer flaskadd 2 to 3 drops of phenolphthalein indicator solution andtitrate with standard 0.1 N sodium hydroxide solution to a faintpink. Accurately weigh 10 to 20 g of sample and a
44、dd to thecontents of the flask.18.7 If the solution is colorless titrate with standard 0.1 Nsodium hydroxide solution to a faint pink. If the solution ispink titrate with standard 0.1 N hydrochloric acid to justcolorless.19. Calculations19.1 Calculate the hydroxyl number from the followingequations:
45、19.1.1 For samples containing free acidity:Hydroxyl Number, mg KOH/g 5FB 2 S!NW1C 3 N1W1G3 56.1(2)19.1.2 For samples containing free alkalinity:Hydroxyl Number, mg KOH/g 5FB 2 S!NW2C 3 N1W1G3 56.1(3)D4252 89 (2009)3where:B = volume of 1 N sodium hydroxide solution requiredfor blank titration (18.5),
46、 mL,S = volume of 1 N sodium hydroxide solution requiredfor sample titration (18.4), mL,N = normality of 1 N sodium hydroxide solution,W = weight of sample taken (18.1), g,C = volume of 0.1 N sodium hydroxide/hydrochloric acidrequired for acidity/alkalinity titration (18.7), mL,N1= normality of 0.1
47、N sodium hydroxide/hydrochloricacid used for acidity/alkalinity titration (18.7), andW1= weight of sample used for acidity/alkalinity titration(18.6), g.19.2 Calculate the apparent molecular weight from thefollowing equation:Apparent Molecular Weight 556,100H3 F (4)where:H = hydroxyl number (mg KOH/
48、g sample).F = number of hydroxyl groups per molecule.20. Precision20.1 The following criteria should be used for judging theacceptability of the results:6,820.1.1 Repeatability (Single Analyst)The standard devia-tion of results (each the average of duplicates), obtained by thesame analyst on differe
49、nt days, has been estimated to be 1.10 %relative at 30 df. Two such averages should be consideredsuspect (95 % confidence level) if they differ by more than3.18 % relative.20.1.2 Reproducibility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be1.80 % relative at 6 df. Two such averages should be consid-ered suspect (95 % confidence level) if they differ by more than6.21 % relative.20.1.3 Checking Limits for DuplicatesReport the hy-droxyl number of
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