1、Designation: D2357 11 (Reapproved 2016)Standard forQualitative Classification of Surfactants by InfraredAbsorption1This standard is issued under the fixed designation D2357; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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 This standard covers the qualitative classification ofsynthetic detergent products or mixtures of synthetic deter-g
3、ents. 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 D2358.1.2 This standard does not purport to address all of thesafety concerns, if any,
4、 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:2D2358 Test Method for Separation ofActive Ingredient
5、 fromSurfactant and Syndet Compositions3. Summary of Classification3.1 A portion of the active ingredient is scanned in theinfrared region of the spectrum from at least 2.5 to 15 m(4000 to 667 cm1). Qualitative identification of surfactant typeis based on the presence of infrared absorption bands at
6、tribut-able to specific functional groups.3.2 A listing of absorbance 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. Appa
7、ratus4.1 Spectrophotometer, recording, infrared, or Fourier trans-form Infrared (FTIR if available).4.2 Dies and Press, for preparation of KBr disks.4.3 Detergent Reference Spectra.4.4 Appropriate Sampling AccessoriesATR, Diffuse re-flectance and others as appropriate.5. Reagents5.1 Potassium Bromid
8、e (KBr), infrared quality, powdered.5.2 Additional Reagents, as specified in Test MethodD2358.6. Preparation of Sample6.1 Sample in Pure FormIf the sample is in pure form orcontains only volatile solvents, dry the sample in accordancewith 5.8 of Test Method D2358, and obtain the infraredspectrum of
9、the dried sample.6.2 For Built Surfactants and Synthetic DetergentCompositionsObtain the infrared spectrum of the activeingredient(s) separated in accordance with Test Method D2358.7. Procedure7.1 Whenever possible, the infrared spectrum should beobtained directly from the organic material, by forma
10、tion of afilm between salt blocks, and by recording the spectrumbetween 2.5 and 15 m (4000 and 667 cm1). The film issatisfactory if the spectrum shows 10 to 30 % transmittance inthe strongest absorbance region.7.2 Alternatively, the sample may be applied to an ATRcrystal and the spectrum collected a
11、ccording to the manufac-turers instructions. Care should be taken to use an appropriateATR crystal material as different crystals will produce inter-ference in different regions of the spectrum. Diamond crystalsare generally preferred for durability but they will produceinterference in the 3.85 to 5
12、.5 m (2600 to 1800 cm1) regionof the spectrum. A correction factor may need to be applied tothe spectrum to change the absorbance values to what would beexpected in a transmission spectrum. most software packageshave algorithms to perform this correction.7.3 If the sample can be obtained in dry, pow
13、dered form, thediffuse reflectance or KBr pressed-disk method may be used.Grind the sample sufficiently fine to prevent radiation scatter,1This classification is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents and is the direct responsibility of Subcommittee D12.12 onAnalys
14、is and Specifications of Soaps, Synthetics, Detergents and their Components.Current edition approved July 1, 2016. Published August 2016. Originallyapproved in 1965 as D2357 65 T. Last previous edition approved in 2011 asD2357 11. DOI: 10.1520/D2357-11R16.2For referenced ASTM standards, visit the AS
15、TM website, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. Unite
16、d States1and add approximately 1 part sample to 19 parts of drypowdered KBr. For diffuse reflectance load this mixture intothe accessory according to the manufacturers instructions. Toprepare a KBr disk, using suitable equipment, form the disk atroom temperature in vacuum, under pressure of 10 to 30
17、tons/in.2(150 to 450 MPa). Obtain the spectrum of the samplebetween 2.5 and 15 m (4000 and 667 cm1)asin7.1.37.4 Other sample accessories may be used to collect spectraprovided they work in the appropriate wavelength/frequencyrange and any interferences are known and accounted for in theinterpretatio
18、n.8. Identification of Components8.1 Note the wavelength/frequency position of each specificabsorption band.8.2 Identify the absorption bands in terms of functionalgroups by the use of data in Table 1 or other appropriatereference source.TABLE 1 Infrared Absorption Bands of Typical Commercial Deterg
19、entsDetergent Wavelength, m Frequency, cm1Band ShapeABand IntensityBIdentityAlkylbenzene sulfonate 6.7 1493 shoulder weak aromatic bands8.1 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 br
20、oad moderate para substitutionFatty alcohol sulfate 8.0 1250 sharpDstrong organic sulfate group8.3 1205 sharpDstrong organic sulfate group9.2 1087 sharp moderate most characteristic alcohol sulfate band10.3 971 broad weak characteristic alcohol sulfate bands10.8 926 broad weak characteristic alcohol
21、 sulfate bandsSulfonated amide (taurate) 6.1 1639 sharp strong amide carbonyl6.4 1563 shoulder weak secondary amide8.1 to 8.5 1235 to 1176 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
22、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 monoglyceride 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
23、 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 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
24、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 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
25、broad strong polyethylene oxide10.5 to 10.9 952 to 917 broad strong polyethylene oxide8.5 1176 shoulder moderate ester C|CzOEthoxylated fatty 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|CzO
26、H10.5 to 10.9 952 to 917 broad strong polyethylene oxideEthoxylated alkyl phenol 2.9 3448 sharp moderate OH6.2 1613 sharp moderate aromatic bands6.6 1515 sharp strong aromatic bands7.4 1351 sharp strong polyethylene oxide8.0 1250 sharp strong characteristic alkylphenol polyether band8.4 1190 sharp s
27、trong characteristic alkylphenol polyether band3For 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, Inc.
28、, New York, NY.D2357 11 (2016)2TABLE 1 ContinuedDetergent Wavelength, m Frequency, cm1Band ShapeABand IntensityBIdentity8.7 to 9.2 1149 to 1087 broad strong polyethylene oxide12.0 833 broad moderate para substitutionGlyceryl monostearate 3.0 3333 broad strong OH5.8 1724 sharp strong ester carbonyl8.
29、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-alkylol 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 sha
30、rp 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 acid salt band10.8 926 broad weak organic acid salt band13.8 725 sharp medium characteristic for soap14.4 694 sharp medium characteristic for soapAlip
31、hatic quaternary ammonium chloride 2.9 3448 sharp strong typical quaternary ammonium compound bands6.1 1639 broad weak typical quaternary ammonium compound bands10.2 to 10.6 980 to 943 sharp moderate typical quaternary ammonium compound bands10.9 917 sharp weak typical quaternary ammonium compound b
32、andsAlcohol 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 strong polyethylene oxide10.5 to 10.9 952 to 917 broad strong polyethylene oxideAlpha olefin sulfonate 2.9 3448 broad weak |CzOH3.4 2940 sharp moderat
33、e |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 trans olefinABand shape descriptions are based on spectra scanned linearly with respect to wavelength.BSome bands marked “weak” in the attached table
34、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.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, identi
35、fy the types ofsurfactants present from their characteristic functional groups.NOTE 2Application of chemical tests to a portion of the activeingredient may assist in the identification of components, particularly inthe case of surfactant mixtures.8.4 Table 1 lists some of the more common types ofcom
36、mercial surfactants and the wavelengths/frequencies oftheir characteristic absorbance bands. This table is intendedonly as a guide to spectral interpretation and qualitativeclassification of surfactants. Reference should also be made toASTM STP 358, Serial Number List of Compound Names andReferences
37、 to Published Infrared Spectra.49. Precision and Bias9.1 Since this standard is for qualitative analysis only,precision and bias do not apply. The accuracy of theidentification, however, may be affected by impurities in thesample. New surfactant molecules not listed in Table 1 andother molecules wit
38、h similar functional groups may also lead toerroneous identifications. Care should be taken to referenceappropriate standard spectra whenever possible to avoid errors.10. Keywords10.1 infrared absorbance; surfactant functional groups4Available as a separate publication.D2357 11 (2016)3ASTM Internati
39、onal 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 thei
40、r 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 should b
41、e 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 Standard
42、s, 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 11 (2016)4
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