ASTM D2357-1974(2003) Standard for Qualitative Classification of Surfactants by Infrared Absorption《用红外线吸收法进行表面活性剂的质量分类》.pdf

1、Designation: D 2357 74 (Reapproved 2003)Standard forQualitative Classification of Surfactants by InfraredAbsorption1This standard is issued under the fixed designation D 2357; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea

2、r 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 standard covers the qualitative classification ofsynthetic detergent products or mixtures of synthetic dete

3、r-gents. It is applicable to built detergent formulations as well asindividual surfactant compositions.NOTE 1The organic active ingredient must be isolated from builtsyndet compositions in accordance with Test Method D 2358.1.2 This standard does not purport to address all of thesafety concerns, if

4、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 ASTM Standards:D 2358 Test Method for Separation of Active Ingre

5、dientfrom Surfactant and Syndet Compositions23. Summary of Classification3.1 A portion of the active ingredient is scanned in theinfrared region of the spectrum from at least 2 to 15 m.Qualitative identification of surfactant type is based on thepresence of infrared absorption bands attributable to

6、specificfunctional groups.3.2 A listing of absorption bands corresponding to thecharacteristic functional groups of some of the more commontypes of commercial surfactants is included in this method. Useof available detergent reference spectra may provide additionalinformation.4. Apparatus4.1 Spectro

7、photometer, recording, infrared.4.2 Dies and Press, for preparation of KBr disks.4.3 Detergent Reference Spectra.5. Reagents5.1 Mineral Oil, USP.5.2 Potassium Bromide (KBr), infrared quality, powdered.5.3 Additional Reagents, as specified in Test MethodD 2358.6. Preparation of Sample6.1 Sample in Pu

8、re FormIf the sample is in pure form orcontains only volatile solvents, dry the sample in accordancewith 5.8 of Test Method D 2358, and obtain the infraredspectrum of the dried sample.6.2 For Built Surfactants and Synthetic DetergentCompositionsObtain the infrared spectrum of the activeingredient(s)

9、 separated in accordance with Test MethodD 2358.7. Procedure7.1 Whenever possible, the infrared spectrum should beobtained directly from the organic material, by formation of afilm between salt blocks, and by recording the spectrumbetween 2 and 15 m. The film is satisfactory if the spectrumshows 10

10、to 30 % transmittance in the strongest absorptionregion.7.2 If the physical properties of the sample prevent use ofthe film technique, the spectrum may be made from a mineraloil mull. Form the mull by adding 2 to 3 drops of mineral oilto a small quantity of sample contained in a polished grindingsur

11、face (agate) mortar, and grinding for a minimum of 5 min.This should produce a very fine syrupy dispersion. Use themull as a film between salt blocks and obtain the spectrum asin 7.1.7.3 If the sample can be obtained in dry, powdered form, theKBr pressed-disk method may be used. Grind the samplesuff

12、iciently fine to prevent radiation scatter, and add approxi-mately 1 part sample to 19 parts of dry powdered KBr. Usingsuitable equipment, form the disk at room temperature in1This classification is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents, and is the direct responsi

13、bility of Subcommittee D12.12 onAnalysis of Soaps and Synthetic Detergents.Current edition approved April 29, 1974. Published June 1974. Originallypublished as D 2357 65 T. Last previous edition D 2357 69.2Annual Book of ASTM Standards, Vol 15.04.1Copyright ASTM International, 100 Barr Harbor Drive,

14、 PO Box C700, West Conshohocken, PA 19428-2959, United States.vacuum, under pressure of 10 to 30 tons/in.2Obtain thespectrum of the disk, sample between 2 and 15 m as in 7.1.38. Identification of Components8.1 Note the wavelength position of each specific absorptionband.8.2 Identify the absorption b

15、ands in terms of functionalgroups by the use of data in Table 1 or other appropriatereference source.TABLE 1 Infrared Absorption Bands of Typical Commercial DetergentsDetergent Wavelength, m Frequency, cm1Band ShapeABand IntensityBIdentityAlkylbenzene sulfonate 6.7 1493 shoulder weak aromatic bands8

16、.1 to 8.5 1235 to 1176 broadCstrong sulfonate group8.8 1136 sharp moderate sulfonate group9.6 1042 sharp strong ABS bands9.9 1010 sharp strong ABS bands12.0 833 broad moderate para substitutionFatty alcohol sulfate 8.0 1250 sharpDstrong organic sulfate group8.3 1205 sharpDstrong organic sulfate grou

17、p9.2 1087 sharp moderate most characteristic alcohol sulfate band10.3 971 broad weak characteristic alcohol sulfate bands10.8 926 broad weak characteristic alcohol sulfate bandsSulfonated amide (taurate) 6.1 1639 sharp strong amide carbonyl6.4 1563 shoulder weak secondary amide8.1 to 8.5 1235 to 117

18、6 broad strong sulfonate group9.4 1064 sharp strong C|CzN or alkyl sulfonateSulfonated ester (isethionate) 5.8 1724 sharp strong ester carbonyl6.4 1563 broad weak soap8.1 to 8.5 1235 to 1176 broad strong sulfonate group8.5 1176 broad strong ester C|CzO9.4 1064 sharp strong alkyl sulfonateSulfated mo

19、noglyceride 3.0 3333 sharp strong hindered OH5.8 1724 sharp strong ester carbonyl7.9 1266 sharpEstrong organic sulfate8.1 1235 sharpEstrong organic sulfate8.5 1176 broad moderate ester C|CzO9.0 1111 broad weak H|CzC|CzOH secondary9.4 1064 sharp moderate H|CzC|CzOH secondarySulfated phenoxy ether 6.2

20、 1613 sharp weak aromatic bands6.6 1515 sharp moderate aromatic bands7.4 1351 broad weak polyethylene oxide8.0 to 8.2 1250 to 1220 broad strong organic sulfate8.7 to 9.2 1149 to 1087 broad strong polyethylene oxide10.5 to 10.9 952 to 917 broad moderate polyethylene oxide12.0 833 broad moderate para

21、substitutionEthoxylated fatty acid 2.9 3448 sharp moderate OH5.8 1724 sharp strong ester carbonyl7.4 1351 sharp moderate polyethylene oxide8.7 to 9.2 1149 to 1087 broad strong polyethylene oxide10.5 to 10.9 952 to 917 broad strong polyethylene oxide8.5 1176 shoulder moderate ester C|CzOEthoxylated f

22、atty alcohol 2.9 3448 sharp moderate OH7.4 1351 sharp strong polyethylene oxide8.7 to 9.2 1149 to 1087 broad strong polyethylene oxide9.4 1064 sharp moderate C|CzOH10.5 to 10.9 952 to 917 broad strong polyethylene oxideEthoxylated alkyl phenol 2.9 3448 sharp moderate OH6.2 1613 sharp moderate aromat

23、ic bands6.6 1515 sharp strong aromatic bands7.4 1351 sharp strong polyethylene oxide8.0 1250 sharp strong characteristic alkylphenol polyether band8.4 1190 sharp strong characteristic alkylphenol polyether band8.7 to 9.2 1149 to 1087 broad strong polyethylene oxide12.0 833 broad moderate para substi

24、tutionGlyceryl monostearate 3.0 3333 broad strong OH3For details of infrared experimental techniques, see Jones, R. N. and Sandorfy,C., “The Application of Infrared and Raman Spectrometry to the Elucidation ofMolecular Structure.” Technique of Organic Chemistry, Vol IX, 1956. IntersciencePublishers,

25、 Inc., New York, NY.D 2357 74 (2003)2Detergent Wavelength, m Frequency, cm1Band ShapeABand IntensityBIdentity5.8 1724 sharp strong ester carbonyl8.5 1176 broad weak ester C|CzO9.0 1111 broad moderate C|CzOH secondary9.4 1064 broad moderate C|CzOH secondary9.6 1042 broad moderate C|CzOH primaryMono-a

26、lkylol amide 3.0 3333 sharp strong OH3.2 3125 shoulder weak NH6.1 1639 sharp strong amide carbonyl6.4 1563 sharp strong secondary amide9.4 1064 sharp moderate C|CzOH9.6 1042 sharp moderate C|CzOH10.8 926 broad weak ethanolSoap 6.4 1563 sharp strong carboxylate (sodium)10.4 962 broad weak organic aci

27、d salt band10.8 926 broad weak organic acid salt band13.8 725 sharp medium characteristic for soap14.4 694 sharp medium characteristic for soapAliphatic quaternary ammonium chloride 2.9 3448 sharp strong typical quaternary ammonium compound bands6.1 1639 broad weak typical quaternary ammonium compou

28、nd bands10.2 to 10.6 980 to 943 sharp moderate typical quaternary ammonium compound bands10.9 917 sharp weak typical quaternary ammonium compound bandsAlcohol polyether sulfate 7.4 1351 broad weak polyethylene oxide7.9 to 8.2 1266 to 1220 broadFstrong organic sulfate8.7 to 9.2 1149 to 1087 broad str

29、ong polyethylene oxide10.5 to 10.9 952 to 917 broad strong polyethylene oxideAlpha olefin sulfonate 2.9 3448 broad weak |CzOH3.4 2940 sharp moderate |CzCH23.5 2950 sharp moderate |CzCH26.8 1470 sharp moderate |CzCH28.4 1190 broad strong sulfonate9.4 1070 sharp strong sulfonate10.3 970 broad weak tra

30、ns olefinABand shape descriptions are based on spectra scanned linearly with respect to wavelength.BSome bands marked “weak” in the attached table may not appear in all materials.CMay appear as two separate broad bands.DMay appear as a broad 8.0 to 8.3-m band.EMay appear as a broad 7.9 to 8.2-m band

31、.FMay appear as separate 8.0 to 8.3-m bands.8.3 From reference spectra of known standards obtained inthe same manner as the unknown samples, identify the types ofsurfactants present from their characteristic functional groups.NOTE 2Application of chemical tests to a portion of the activeingredient m

32、ay assist in the identification of components, particularly inthe case of surfactant mixtures.8.4 Table 1 lists some of the more common types ofcommercial surfactants and the wavelengths of their character-istic absorption bands. This table is intended only as a guide tospectral interpretation and q

33、ualitative classification of surfac-tants. Reference should also be made to ASTM STP 358, SerialNumber List of Compound Names and References to Pub-lished Infrared Spectra.49. Keywords9.1 infrared absorption; surfactant functional groups4Available as a separate publication.D 2357 74 (2003)3ASTM Inte

34、rnational takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely

35、 their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand sho

36、uld be addressed 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 Sta

37、ndards, at 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 2357 74 (2003)4