ASTM D4252-89(2003)
(Test Method)Standard Test Methods for Chemical Analysis of Alcohol Ethoxylates and Alkylphenol Ethoxylates
Standard Test Methods for Chemical Analysis of Alcohol Ethoxylates and Alkylphenol Ethoxylates
SIGNIFICANCE AND USE
Alcohol ethoxylates and alkylphenol ethoxylates are important surfactants in household and industrial cleaners. They may be used as either nonionic surfactants or sulfated and used as anionic surfactants. Careful control of the ethoxylate characteristics is desired as variations may result in either desirable or undesirable end-use properties.
SCOPE
1.1 These test methods cover the various test methods used to evaluate those properties pertinent to the characterization of alcohol ethoxylates and alkylphenol ethoxylates with respect to suitability for desired uses.
1.2 The procedures for sampling and analysis appear in the following order: SectionsSamplingLiquids6Solids7Methods of Chemical AnalysisWater or moisture8Refractive index9 and 10pH11Acidity or basicity12 and 13Hydroxyl number14-20Cloud point21Iodine number22Ash23Iron24Ethylene oxide content25Polyethylene glycols26-32
1.3 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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage. Specific hazard statements appear in Section 5 and Note 1 and Note 3.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:D4252–89(Reapproved 2003)
Standard Test Methods for
Chemical Analysis of Alcohol Ethoxylates and Alkylphenol
Ethoxylates
This standard is issued under the fixed designation D4252; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D482 Test Method for Ash from Petroleum Products
D1068 Test Methods for Iron in Water
1.1 These test methods cover the various test methods used
D1172 Guide for pH of Aqueous Solutions of Soaps and
to evaluate those properties pertinent to the characterization of
Detergents
alcoholethoxylatesandalkylphenolethoxylateswithrespectto
D1193 Specification for Reagent Water
suitability for desired uses.
D1209 Test Method for Color of Clear Liquids (Platinum-
1.2 The procedures for sampling and analysis appear in the
Cobalt Scale)
following order:
D1218 Test Method for Refractive Index and Refractive
Sections
Dispersion of Hydrocarbon Liquids
Sampling
Liquids 6
D1613 Test Method for Acidity in Volatile Solvents and
Solids 7
Chemical Intermediates Used in Paint, Varnish, Lacquer,
Methods of Chemical Analysis
and Related Products
Water or moisture 8
Refractive index 9 and 10
D1959 Test Method for Iodine Value of Drying Oils and
pH 11
Fatty Acids
Acidity or basicity 12 and 13
Hydroxyl number 14-20 D2024 Test Method for Cloud Point of Nonionic Surfac-
Cloud point 21
tants
Iodine number 22
D2959 Test Method for Ethylene Oxide Content of Poly-
Ash 23
ethoxylated Nonionic Surfactants
Iron 24
Ethylene oxide content 25
E180 Practice for Determining the Precision of ASTM
Polyethylene glycols 26-32
Methods for Analysis and Testing of Industrial and Spe-
1.3 This standard does not purport to address all of the
cialty Chemicals
safety concerns, if any, associated with its use. It is the
E200 Practice for Preparation, Standardization, and Storage
responsibility of the user of this standard to establish appro-
of Standard and Reagent Solutions for Chemical Analysis
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Material Safety
E203 Test Method for Water Using Volumetric Karl Fischer
Data Sheets are available for reagents and materials. Review
Titration
them for hazards prior to usage. Specific hazard statements
E394 Test Method for Iron in Trace Quantities Using the
appear in Section 5 and Note 1 and Note 3.
1,10-Phenanthroline Method
2. Referenced Documents
3. Significance and Use
2.1 ASTM Standards:
3.1 Alcohol ethoxylates and alkylphenol ethoxylates are
D459 Terminology Relating to Soaps and Other Detergents
important surfactants in household and industrial cleaners.
Theymaybeusedaseithernonionicsurfactantsorsulfatedand
used as anionic surfactants. Careful control of the ethoxylate
These test methods are under the jurisdiction of ASTM Committee D12 on
Soaps and Other Detergents and are the direct responsibility of Subcommittee 12.12
on Analysis of Soaps and Synthetic Detergents. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved May 26, 1989. Published July 1989. Originally Annual Book of ASTM Standards, Vol 06.04.
published as D4252 – 83. Last previous edition D4252 – 88. DOI: 10.1520/D4252- Annual Book of ASTM Standards, Vol 06.03.
89R03. Withdrawn. The last approved version of this historical standard is referenced
Annual Book of ASTM Standards, Vol 15.04. on www.astm.org.
3 8
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4252–89 (2003)
characteristics is desired as variations may result in either 10. Precision
desirable or undesirable end-use properties.
10.1 The following criteria should be used for judging the
,
10 11
acceptability of results:
4. Purity of Reagents
10.1.1 Repeatability (Single Analyst)—The standard devia-
tion of results (each the average of duplicates), obtained by the
4.1 Reagent-grade chemicals shall be used in all tests.
same analyst on different days, has been estimated to be
Unless otherwise indicated, it is intended that all reagents shall
0.00021 units absolute at 36 df. Two such averages should be
conform to the specifications of the Committee on Analytical
considered suspect (95 % confidence level) if they differ by
Reagents of the American Chemical Society, where such
more than 0.00059 units absolute.
specifications are available. Other grades may be used, pro-
10.1.2 Reproducibility (Multilaboratory)—The standard de-
vided it is first ascertained that the reagent is of sufficiently
viation of results (each the average of duplicates), obtained by
high purity to permit its use without lessening the accuracy of
analysts in different laboratories, has been estimated to be
the determination.
0.00059 units absolute at 7 df. Two such averages should be
4.2 Unless otherwise indicated, references to water shall be
considered suspect (95 % confidence level) if they differ by
understood to mean Type III reagent water conforming to
more than 0.0020 units absolute.
Specification D1193.
10.1.3 Checking Limits for Duplicates—Report the refrac-
tive index of the sample to the nearest 0.0001. Duplicate runs
5. Safety Precautions
that agree within 0.00025 units are acceptable for averaging
5.1 All reagents and chemicals should be handled with care. (95 % confidence level).
Before using any chemical, read and follow all safety precau-
pH
tions and instructions on the manufacturer label. Clean up any
spillimmediately.Forinformationoncleaningupspillsreferto
11. Procedure
the Laboratory Disposal Manual, Manufacturing Chemists
11.1 Determine the pH in accordance with Test Method
Association, Washington, DC.
D1172, except prepare the solution by transferring 1 6 0.001
g of the sample to a 100 mL volumetric flask and diluting in
SAMPLING
accordance with Test Method D1172. Measure the pH 10 min
after diluting the sample solution to volume.
6. Liquids
6.1 Thoroughly mix the sample before sampling. If a solid
ACIDITY OR BASICITY
layer or crystals have formed on the bottom of the bottle, melt
12. Procedure
inanovenorwaterbathat55°Candmixwellbeforesampling.
12.1 Determine acidity or basicity in accordance with Test
7. Solids Method D1613 using a 3+1 solution of isopropyl alcohol and
water as the solvent and a 10-g sample.
7.1 Melt in an oven or water bath at 55°C and mix well
beforesampling.Ifitisnecessarytoheatattemperaturesabove
13. Precision
60°C,replacethegascapwithaninertgas,suchasoxygen-free
13.1 The following criteria should be used for judging the
nitrogen, helium, or argon before heating.
,
11 12
acceptability of results:
13.1.1 Repeatability (Single Analyst)—The standard devia-
WATER OR MOISTURE
tion of results (each the average of duplicates), obtained by the
same analyst on different days, has been estimated to be 0.017
8. Procedure
meq/100 g at 27 df. Two such averages should be considered
8.1 Determine water or moisture in accordance with Test
suspect (95 % confidence level) if they differ by more than
Method E203.
0.049 meq/100 g.
13.1.2 Reproducibility (Multilaboratory)—The standard de-
REFRACTIVE INDEX
viation of results (each the average of duplicates), obtained by
analysts in different laboratories, has been established to be
9. Procedure
0.12 meq/100 g at 5 df. Two such averages should be
9.1 Measure the refractive index at 50°C in accordance with
Test Method D1218.
The precision estimates are based on an interlaboratory study on ALFONICt
1412-60, MAKONt-10, NEODOLt 25-9, PLURONICt 25R1, and TERGITOL
15-S-3 by nine laboratories.
Statistical analysis was performed in accordance with Practice E180 for
Reagent Chemicals, American Chemical Society Specifications, American developing precision estimates. Data supporting the precision statements are on file
Chemical Society, Washington, DC. For suggestions on the testing of reagents not at ASTM Headquarters, 100 Barr Harbor Drive, West Conshohocken, PA 19428 as
listed by the American Chemical Society, see Analar Standards for Laboratory D12-1004.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia The precision estimates are based on an interlaboratory study on ALFONICt
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 1412-60, MAKONt-10, NEODOLt 25-9, PLURONICt 25R1 and TERGITOLt
MD. 15-S-3 by six laboratories.
D4252–89 (2003)
considered suspect (95 % confidence level) if they differ by 17.6 Phenolphthalein Indicator Solution—Dissolve1gof
more than 0.44 meq/100 g. phenolphthalein in 100 mL of pyridine.
13.1.3 Checking Limits for Duplicates—Report the acidity 17.7 Isopropyl Alcohol,A.R.
or basicity of the sample to the nearest 0.05 meq/100 g.
18. Procedure
Duplicate runs that agree within 0.051 meq/100 g are accept-
able for averaging (95 % confidence level).
18.1 Weigh into a clean and dry 250-mL Erlenmeyer flask
with ground glass joint to the nearest 0.1 mg an amount of
HYDROXYL NUMBER
sample calculated by means of the following equation but do
not use more than 10 g of sample:
14. Terminology
M
14.1 Definition:
Amount of Sample, g 5 (1)
F 3 100
14.1.1 hydroxyl number—the number of milligrams of po-
tassium hydroxide equivalent to the hydroxyl content of1gof
where:
sample.
M = molecular weight of sample and
F = number of hydroxyl groups per molecule.
15. Summary of Test Method
18.2 Pipet accurately 25 mL of phthalic anhydride reagent
15.1 The hydroxyl groups are esterified by reaction with
into the flask and swirl to effect solution. Add two boiling
phthalic anhydride in a pyridine medium at the temperature of
chips, attach a dry reflux condenser with a ground glass joint
reflux of the mixture. After cooling, the excess of phthalic
fitted with a TFE-fluorocarbon sleeve to the flask, and reflux
anhydride is hydrolyzed with water and the phthalic acid
for1honan electric hotplate.
formed is titrated to the phenolphthalein end point with
18.3 Turn off the hotplate and insert an insulated pad
standard sodium hydroxide solution. The hydroxyl content is
between the flask and the hot plate. Allow to cool for 20 min.
calculated from the difference in titration of the blank and of
Wash down the condenser, first with 25 mL of pyridine and
the sample solution.
then with 25 mL of water.
18.4 Remove the flask from the condenser.Add 4 or 5 drops
16. Apparatus
of phenolphthalein indicator to the flask and titrate with
16.1 Reflux Assembl
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