ASTM D2357-74(1995)e1

Standard for Qualitative Classification of Surfactants by Infrared Absorption

SCOPE
1.1 This standard covers the qualitative classification of synthetic detergent products or mixtures of synthetic detergents. It is applicable to built detergent formulations as well as individual surfactant compositions.  Note 1-The organic active ingredient must be isolated from built syndet compositions in accordance with Test Method D2358.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Dec-1994
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

Relations

• Replaced By: ASTM D2357-74(2003) - Standard for Qualitative Classification of Surfactants by Infrared Absorption
• Effective Date: 29-Apr-1974
• Referred By: ASTM D820-93(2023) - Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents
• Effective Date: 01-Jan-1995

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 2357 – 74 (Reapproved 1995)
Standard for
Qualitative Classification of Surfactants by Infrared
Absorption
This standard is issued under the fixed designation D 2357; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Keywords were added editorially in February 1995.
1. Scope 4.2 Dies and Press, for preparation of KBr disks.
4.3 Detergent Reference Spectra.
1.1 This standard covers the qualitative classification of
synthetic detergent products or mixtures of synthetic deter-
5. Reagents
gents. It is applicable to built detergent formulations as well as
5.1 Mineral Oil, USP.
individual surfactant compositions.
5.2 Potassium Bromide (KBr), infrared quality, powdered.
NOTE 1—The organic active ingredient must be isolated from built
5.3 Additional Reagents, as specified in Test Method
syndet compositions in accordance with Test Method D 2358.
D 2358.
1.2 This standard does not purport to address all of the
6. Preparation of Sample
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 6.1 Sample in Pure Form—If the sample is in pure form or
priate safety and health practices and determine the applica-
contains only volatile solvents, dry the sample in accordance
bility of regulatory limitations prior to use. with 5.8 of Test Method D 2358, and obtain the infrared
spectrum of the dried sample.
2. Referenced Documents
6.2 For Built Surfactants and Synthetic Detergent
2.1 ASTM Standards:
Compositions—Obtain the infrared spectrum of the active
D 2358 Test Method for Separation of Active Ingredient
ingredient(s) separated in accordance with Test Method
from Surfactant and Syndet Compositions
D 2358.
3. Summary of Classification
7. Procedure
3.1 A portion of the active ingredient is scanned in the
7.1 Whenever possible, the infrared spectrum should be
infrared region of the spectrum from at least 2 to 15 μm.
obtained directly from the organic material, by formation of a
Qualitative identification of surfactant type is based on the
film between salt blocks, and by recording the spectrum
presence of infrared absorption bands attributable to specific
between 2 and 15 μm. The film is satisfactory if the spectrum
functional groups.
shows 10 to 30 % transmittance in the strongest absorption
3.2 A listing of absorption bands corresponding to the
region.
characteristic functional groups of some of the more common
7.2 If the physical properties of the sample prevent use of
types of commercial surfactants is included in this method. Use
the film technique, the spectrum may be made from a mineral
of available detergent reference spectra may provide additional
oil mull. Form the mull by adding 2 to 3 drops of mineral oil
information.
to a small quantity of sample contained in a polished grinding
surface (agate) mortar, and grinding for a minimum of 5 min.
4. Apparatus
This should produce a very fine syrupy dispersion. Use the
4.1 Spectrophotometer, recording, infrared.
mull as a film between salt blocks and obtain the spectrum as
in 7.1.
7.3 If the sample can be obtained in dry, powdered form, the
This classification is under the jurisdiction of ASTM Committee D-12 on Soaps
KBr pressed-disk method may be used. Grind the sample
and Other Detergents, and is the direct responsibility of Subcommittee D12.12 on
sufficiently fine to prevent radiation scatter, and add approxi-
Analysis of Soaps and Synthetic Detergents.
Current edition approved April 29, 1974. Published June 1974. Originally
mately 1 part sample to 19 parts of dry powdered KBr. Using
published as D 2357 – 65 T. Last previous edition D 2357 – 69.
suitable equipment, form the disk at room temperature in
Annual Book of ASTM Standards, Vol 15.04.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 2357
spectrum of the disk, sample between 2 and 15 μm as in 7.1.
vacuum, under pressure of 10 to 30 tons/in. Obtain the
8. Identification of Components
8.1 Note the wavelength position of each specific absorption
band.
8.2 Identify the absorption bands in terms of functional
groups by the use of data in Table 1 or other appropriate
reference source.
For details of infrared experimental techniques, see Jones, R. N. and Sandorfy,
C., “The Application of Infrared and Raman Spectrometry to the Elucidation of
Molecular Structure.” Technique of Organic Chemistry, Vol IX, 1956. Interscience
Publishers, Inc., New York, NY.
TABLE 1 Infrared Absorption Bands of Typical Commercial Detergents
−1 A B
Detergent Wavelength, μm Frequency, cm Band Shape Band Intensity Identity
Alkylbenzene sulfonate 6.7 1493 shoulder weak aromatic bands
C
8.1 to 8.5 1235 to 1176 broad strong sulfonate group
8.8 1136 sharp moderate sulfonate group
9.6 1042 sharp strong ABS bands
9.9 1010 sharp strong ABS bands
12.0 833 broad moderate para substitution
D
Fatty alcohol sulfate 8.0 1250 sharp strong organic sulfate group
D
8.3 1205 sharp strong organic sulfate group
9.2 1087 sharp moderate most characteristic alcohol sulfate band
10.3 971 broad weak characteristic alcohol sulfate bands
10.8 926 broad weak characteristic alcohol sulfate bands
Sulfonated amide (taurate) 6.1 1639 sharp strong amide carbonyl
6.4 1563 shoulder weak secondary amide
8.1 to 8.5 1235 to 1176 broad strong sulfonate group
9.4 1064 sharp strong C|CzN or alkyl sulfonate
Sulfonated ester (isethionate) 5.8 1724 sharp strong ester carbonyl
6.4 1563 broad weak soap
8.1 to 8.5 1235 to 1176 broad strong sulfonate group
8.5 1176 broad strong ester C|C
...