ASTM D4252-89(2017)
(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
3.1 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:
Sections
Sampling
Liquids
6
Solids
7
Methods of Chemical Analysis
Water or moisture
8
Refractive index
9 and 10
pH
11
Acidity or basicity
12 and 13
Hydroxyl number
14 – 20
Cloud point
21
Iodine number
22
Ash
23
Iron
24
Ethylene oxide content
25
Polyethylene glycols
26 – 32
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4252 − 89 (Reapproved 2017)
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 2. Referenced Documents
1.1 These test methods cover the various test methods used 2.1 ASTM Standards:
to evaluate those properties pertinent to the characterization of D459 Terminology Relating to Soaps and Other Detergents
alcoholethoxylatesandalkylphenolethoxylateswithrespectto D482 Test Method for Ash from Petroleum Products
suitability for desired uses. D1068 Test Methods for Iron in Water
D1172 Guide for pH of Aqueous Solutions of Soaps and
1.2 The procedures for sampling and analysis appear in the
Detergents
following order:
D1193 Specification for Reagent Water
Sections
D1209 Test Method for Color of Clear Liquids (Platinum-
Sampling
Liquids 6 Cobalt Scale)
Solids 7
D1218 Test Method for Refractive Index and Refractive
Methods of Chemical Analysis
Dispersion of Hydrocarbon Liquids
Water or moisture 8
Refractive index 9 and 10 D1613 Test Method for Acidity in Volatile Solvents and
pH 11
Chemical Intermediates Used in Paint, Varnish, Lacquer,
Acidity or basicity 12 and 13
and Related Products
Hydroxyl number 14–20
Cloud point 21 D1959 Test Method for Iodine Value of Drying Oils and
Iodine number 22
Fatty Acids (Withdrawn 2006)
Ash 23
D2024 Test Method for Cloud Point of Nonionic Surfactants
Iron 24
Ethylene oxide content 25
D2959 Test Method for Ethylene Oxide Content of Poly-
Polyethylene glycols 26–32
ethoxylated Nonionic Surfactants
1.3 The values stated in SI units are to be regarded as
E180 Practice for Determining the Precision of ASTM
standard. No other units of measurement are included in this
Methods for Analysis and Testing of Industrial and Spe-
standard.
cialty Chemicals (Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage
1.4 This standard does not purport to address all of the
of Standard and Reagent Solutions for ChemicalAnalysis
safety concerns, if any, associated with its use. It is the
E203 Test Method for Water Using Volumetric Karl Fischer
responsibility of the user of this standard to establish appro-
Titration
priate safety and health practices and determine the applica-
E394 Test Method for Iron in Trace Quantities Using the
bility of regulatory limitations prior to use. Material Safety
1,10-Phenanthroline Method
Data Sheets are available for reagents and materials. Review
them for hazards prior to usage. Specific hazard statements
3. Significance and Use
appear in Section 5 and Note 1 and Note 3.
3.1 Alcohol ethoxylates and alkylphenol ethoxylates are
important surfactants in household and industrial cleaners.
These test methods are under the jurisdiction of ASTM Committee D12 on
Soaps and Other Detergents and are the direct responsibility of Subcommittee For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and their contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Components. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Jan. 1, 2017. Published February 2017. Originally the ASTM website.
approved in 1983. Last previous edition approved in 2009 as D4252 – 89(2009). The last approved version of this historical standard is referenced on
DOI: 10.1520/D4252-89R17. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4252 − 89 (2017)
Theymaybeusedaseithernonionicsurfactantsorsulfatedand 10. Precision
used as anionic surfactants. Careful control of the ethoxylate
10.1 The following criteria should be used for judging the
characteristics is desired as variations may result in either 5,6
acceptability of results:
desirable or undesirable end-use properties.
10.1.1 Repeatability (Single Analyst)—The standard devia-
tion of results (each the average of duplicates), obtained by the
4. Purity of Reagents
same analyst on different days, has been estimated to be
4.1 Reagent-grade chemicals shall be used in all tests. 0.00021 units absolute at 36 df. Two such averages should be
Unless otherwise indicated, it is intended that all reagents shall considered suspect (95 % confidence level) if they differ by
conform to the specifications of the Committee on Analytical more than 0.00059 units absolute.
Reagents of the American Chemical Society, where such 10.1.2 Reproducibility (Multilaboratory)—The standard de-
specifications are available. Other grades may be used, pro- viation of results (each the average of duplicates), obtained by
vided it is first ascertained that the reagent is of sufficiently analysts in different laboratories, has been estimated to be
high purity to permit its use without lessening the accuracy of 0.00059 units absolute at 7 df. Two such averages should be
the determination. considered suspect (95 % confidence level) if they differ by
more than 0.0020 units absolute.
4.2 Unless otherwise indicated, references to water shall be
10.1.3 Checking Limits for Duplicates—Report the refrac-
understood to mean Type III reagent water conforming to
tive index of the sample to the nearest 0.0001. Duplicate runs
Specification D1193.
that agree within 0.00025 units are acceptable for averaging
(95 % confidence level).
5. Safety Precautions
pH
5.1 All reagents and chemicals should be handled with care.
Before using any chemical, read and follow all safety precau-
11. Procedure
tions and instructions on the manufacturer label. Clean up any
spillimmediately.Forinformationoncleaningupspillsreferto
11.1 Determine the pH in accordance with Test Method
the Laboratory Disposal Manual, Manufacturing Chemists
D1172, except prepare the solution by transferring 1 6 0.001
Association, Washington, DC.
g of the sample to a 100 mL volumetric flask and diluting in
accordance with Test Method D1172. Measure the pH 10 min
SAMPLING
after diluting the sample solution to volume.
6. Liquids
ACIDITY OR BASICITY
6.1 Thoroughly mix the sample before sampling. If a solid
12. Procedure
layer or crystals have formed on the bottom of the bottle, melt
inanovenorwaterbathat55°Candmixwellbeforesampling.
12.1 Determine acidity or basicity in accordance with Test
Method D1613 using a 3+1 solution of isopropyl alcohol and
7. Solids
water as the solvent and a 10-g sample.
7.1 Melt in an oven or water bath at 55°C and mix well
13. Precision
beforesampling.Ifitisnecessarytoheatattemperaturesabove
60°C,replacethegascapwithaninertgas,suchasoxygen-free 13.1 The following criteria should be used for judging the
6,7
nitrogen, helium, or argon before heating.
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
0.049 meq/100 g.
Method E203.
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 ALFONIC®
1412-60, MAKON®-10, NEODOL® 25-9, PLURONIC® 25R1, and TERGITOL
15-S-3 by nine laboratories.
4 6
Reagent Chemicals, American Chemical Society Specifications, American Statistical analysis was performed in accordance with Practice E180 for
Chemical Society, Washington, DC. For suggestions on the testing of reagents not developing precision estimates. Data supporting the precision statements are on file
listed by the American Chemical Society, see Analar Standards for Laboratory at ASTM International Headquarters. Request RR: RR:D12-1004.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia The precision estimates are based on an interlaboratory study on ALFONIC®
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, 1412-60, MAKON®-10, NEODOL® 25-9, PLURONIC® 25R1 and TERGITOL®
MD. 15-S-3 by six laboratories.
D4252 − 89 (2017)
considered suspect (95 % confidence level) if they differ by 17.5 Hydrochloric Acid (0.1 N)—Purchase or prepare by
more than 0.44 meq/100 g. diluting 8.3 mL of concentrated hydrochloric acid to 1 L with
distilled water. Standardize and store according to Practice
13.1.3 Checking Limits for Duplicates—Report the acidity
or basicity of the sample to the nearest 0.05 meq/100 g. E200.
Duplicate runs that agree within 0.051 meq/100 g are accept-
17.6 Phenolphthalein Indicator Solution—Dissolve1gof
able for averaging (95 % confidence level).
phenolphthalein in 100 mL of pyridine.
HYDROXYL NUMBER 17.7 Isopropyl Alcohol, A. R.
18. Procedure
14. Terminology
18.1 Weigh into a clean and dry 250-mL Erlenmeyer flask
14.1 Definitions:
with ground glass joint to the nearest 0.1 mg an amount of
14.1.1 hydroxyl number—the number of milligrams of po-
sample calculated by means of the following equation but do
tassium hydroxide equivalent to the hydroxyl content of1gof
not use more than 10 g of sample:
sample.
M
Amount of Sample, g 5 (1)
F 3100
15. Summary of Test Method
where:
15.1 The hydroxyl groups are esterified by reaction with
phthalic anhydride in a pyridine medium at the temperature of M = molecular weight of sample and
reflux of the mixture. After cooling, the excess of phthalic F = number of hydroxyl groups per molecule.
anhydride is hydrolyzed with water and the phthalic acid
18.2 Pipet accurately 25 mL of phthalic anhydride reagent
formed is titrated to the phenolphthalein end point with
into the flask and swirl to effect solution. Add two boiling
standard sodium hydroxide solution. The hydroxyl content is
chips, attach a dry reflux condenser with a ground glass joint
calculated from the difference in titration of the blank and of
fitted with a TFE-fluorocarbon sleeve to the flask, and reflux
the sample solution.
for1honan electric hotplate.
18.3 Turn off the hotplate and insert an insulated pad
16. Apparatus
between the flask and the hot plate. Al
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