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ASTM D2959-95(2009)

(Test Method)

Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants

Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants

ABSTRACT
This test method covers the determination of ethylene oxide content in polyethoxylated nonionic surfactants. It can also be used for compounds containing propylene oxide or any compounds (glycols and glycol and polyglycol ethers and esters) which form unstable 1,2-diiodides on reaction with hydroiodic acid. The apparatus is comprised of the following: heat source which shall be an electric heater provided with a sliding rheostat or other means of heat control; flasks which shall be equipped with a standard ground-glass joint; condensers with standard joints; gas bubbler filled with dibutyl phthalate; buret; and pipet. The dual apparatus is designed to permit a sample and a blank to be run simultaneously. Reagent grade chemicals or reagents of sufficiently high purity including water, carbon dioxide or nitrogen, lubricant, dibutyl phthalate, glass beads, hydroiodic acid, hydrochloric acid, methanol, potassium dichromate, potassium iodide solution, sodium thiosulfate, and starch indicator solution shall be used in all tests. The ethylene oxide content shall be calculated from the amount of sodium thiosulfate solution required to titrate the sample and the blank, normality of sodium thiosulfate, and weight of the sample. Standard deviations for repeatability and reproducibility shall be estimated to determine the acceptability of the results.
SCOPE
1.1 This test method covers the determination of ethylene oxide in polyethoxylated nonionic surfactants. It can also be used for compounds containing propylene oxide or any compounds (glycols and glycol and polyglycol ethers and esters) which form unstable 1,2-diiodides on reaction with hydriodic acid.  
Note 1—Compounds in which the oxyalkylene group is connected to a nitrogen cannot be entirely decomposed. This can be used to determine the percent of an ethoxylated surfactant in a mixture, if the ethylene oxide content of the ethoxylated surfactant is known.
Note 2—This method reports results as percent ethylene oxide. If this method is applied to unknown compounds or compositions, the analyst should be aware of the possible presence of material other than ethylene oxide.
Note 3—For use on built syndet compositions the organic active ingredient must be isolated in accordance with Test Method D2358.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.

General Information

Status
Historical
Publication Date
30-Sep-2009
ICS
71.100.40 - Surface active agents
Technical Committee
D12 - Soaps and Other Detergents
Drafting Committee
D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components
Current Stage
Ref Project

Relations

Replaces
ASTM D2959-95(2003) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants
Effective Date
01-Oct-2009
Replaced By
ASTM D2959-95(2017) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants
Effective Date
01-Jan-2017
Referred By
ASTM D4252-89(2017) - Standard Test Methods for Chemical Analysis of Alcohol Ethoxylates and Alkylphenol Ethoxylates
Effective Date
01-Oct-2009

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ASTM D2959-95(2009) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic SurfactantsASTM D2959-95(2009) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants
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ASTM D2959-95(2009) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants
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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: D2959 − 95 (Reapproved 2009)
Standard Test Method for
Ethylene Oxide Content of Polyethoxylated Nonionic
1
Surfactants
This standard is issued under the fixed designation D2959; 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 D2358 TestMethodforSeparationofActiveIngredientfrom
Surfactant and Syndet Compositions
1.1 This test method covers the determination of ethylene
oxide in polyethoxylated nonionic surfactants. It can also be
3. Summary of Test Method
used for compounds containing propylene oxide or any com-
3.1 By cleaving nonionic surfactants containing polyethyl-
pounds (glycols and glycol and polyglycol ethers and esters)
ene oxide chains with hydriodic acid, the unstable 1,2-
which form unstable 1,2-diiodides on reaction with hydriodic
diiodoethane is formed. This vicinal diiodide decomposes to
acid.
form ethylene and iodine.
NOTE 1—Compounds in which the oxyalkylene group is connected to a
nitrogencannotbeentirelydecomposed.Thiscanbeusedtodeterminethe
percent of an ethoxylated surfactant in a mixture, if the ethylene oxide
content of the ethoxylated surfactant is known.
NOTE 2—This method reports results as percent ethylene oxide. If this
method is applied to unknown compounds or compositions, the analyst
should be aware of the possible presence of material other than ethylene
oxide.
3.2 The percent ethylene oxide is determined by measuring
NOTE 3—For use on built syndet compositions the organic active
the amount of free iodine formed, since one mole of iodine is
ingredient must be isolated in accordance with Test Method D2358.
formed for each mole of ethylene oxide in the polyoxyalkylene
1.2 The values stated in SI units are to be regarded as
chain. The free iodine is titrated with a standard sodium
standard. No other units of measurement are included in this
thiosulfate solution.
standard.
4. Apparatus (Fig. 1)
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 Heat Sources, two. The source of heat should be an
responsibility of the user of this standard to establish appro-
electric heater provided with a sliding rheostat or other means
priate safety and health practices and determine the applica-
of heat control.
bility of regulatory limitations prior to use. Material Safety
4.2 Flasks, two, 100-mL, round bottom. Each flask should
Data Sheets are available for reagents and materials. Review
be equipped with a standard ground-glass joint to accommo-
them for hazards prior to usage.
date a vertical condenser, and with a side arm through which
2. Referenced Documents carbon dioxide can be passed to blanket the reaction mixture.
2
4.3 Condensers, two, with standard joints to fit the flasks.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
4.4 Gas Bubbler, filled with dibutyl phthalate.
4.5 Buret, 50-mL, with 0.1-mL graduations.
1
This method is under the jurisdiction of ASTM Committee D12 on Soaps and
Other Detergents and is the direct responsibility of Subcommittee D12.12 on
4.6 Pipet, 5-mL.
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components.
Current edition approved Oct. 1, 2009. Published December 2009. Originally
5. Reagents
approved in 1971 as D2959 – 71 T. Last previous edition approved in 2003 as
D2959 – 95(2003). DOI: 10.1520/D2959-95R09.
5.1 Purity of Reagents—Reagent grade chemicals shall be
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
all reagents shall conform to the specifications of the Commit-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tee onAnalytical Reagents of theAmerican Chemical Society,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D2959 − 95 (2009)
5.12 Sodium Thiosulfate, Standard Solution (0.1 N)—
Dissolve 24.8 g of sodium thiosulfate (Na S O ) in water and
2 2 3
dilute to 1000 mL. Standardize by accurately weighing 0.16 to
0.22 g of finely ground and dried K Cr O into a 500-mL
2 2 7
iodine flask. Dissolve in 25 mLof water, add 5 mLof HCl and
15 mL of KI solution and swirl to mix. Allow to stand for 5
min, then add 100 mL of distilled water. Titrate with standard
Na S O solution, shaking continuously until the yellow color
2 2 3
has almost disappeared. Add a small amount of Paragon
4
indicator or1
...

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Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils

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These test methods cover the chemical analysis of sulfonated and sulfated oils. Water by distillation with volatile solvent and moisture and volatile matter by hot-plate shall be tested to meet the requirements prescribed. Titration test, extraction-titration test, and ash-gravimetric test shall be performed to meet the requirements specified. Total desulfated fatty matter, total active ingredients, unsaponifiable non-volatile matter, inorganic salts, total alkalinity, and total ammonia shall be tested to meet the requirements prescribed. In the absence of ammonium or triethanolamine soaps test method, brine test method, and in the presence of ammonium or triethanolamine soaps test method shall be performed to meet the requirements prescribed. Water-immiscible organic solvents volatile with steam shall be tested to meet the requirements prescribed.
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1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the following order:    
Section  
Moisture:  
Test Method A. Water by Distillation with Volatile Solvent  
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Sulfonates)  
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29 – 32  
Total Active Ingredients  
33 – 36  
Unsaponifiable Nonvolatile Matter  
37 – 41  
Inorganic Salts  
42 – 46  
Total Alkalinity  
47 – 49  
Total Ammonia  
50 – 52  
Acidity as Free Fatty Acids or Acid Number:  
Test Method A. In the Absence of Ammonium or Triethanolamine Soaps  
53 – 56  
Test Method B. In the Presence of Dark Colored Oils but in the
Absence of Ammonium or Triethanolamine Soaps (Brine Test)  
57 – 60  
Test Method C. In the Presence of Ammonium or Triethanolamine Soaps  
61 – 63  
Water-Immiscible Organic Solvents Volatile with Steam  
64 – 70  
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Standard Test Method for Particle Size of Soaps and Other Detergents

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3.1 This test method assures that the particle size of soaps and detergents conforms to specifications having to do with density and packaging, among others. It also offers a means of controlling the amount of potentially hazardous very low particle size material.
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ASTM D501-03(2023)(Test Method)
Standard Test Methods of Sampling and Chemical Analysis of Alkaline Detergents

ABSTRACT
These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents. These detergents include caustic soda, soda ash, modified soda (sequicarbonate type), sodium bicarbonate, sodium metasilicate, trisodium phosphate, tetrasodium pyrophosphate, borax, and sodium triphosphate. Different tests shall be conducted in order to determine the following properties of the detergents: total alkalinity, matter insoluble in water content, apparent density, ignition loss, pH level, turbidity, temperature rise, and particle size. Chemical analysis of the samples shall be performed by using either reverse-flow ion-exchange chromatography or paper chromatography.
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1.1 These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents.  
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Sections  
Caustic Soda:  
Sampling  
5  
Total Alkalinity as Sodium Oxide (Na2O)  
6 – 8  
Sodium Hydroxide (NaOH)  
9 – 11  
Carbonate as Sodium Carbonate (Na2CO3)  
12  
Carbon Dioxide (CO2) by the Evolution Method  
13 – 16  
Soda Ash:  
Sampling  
17  
Matter Volatile at 150 °C to 155 °C  
18 and 19  
Total Alkalinity as Sodium Carbonate (Na2CO3 )  
20 – 22  
Sodium Bicarbonate (NaHCO3)  
23 – 25  
Sodium Bicarbonate (NaHCO3) by Potentiometric Titration  
26 – 28  
Matter Insoluble in Water  
29 and 30  
Apparent Density  
31 and 32  
Modified Soda (Sequicarbonate Type):  
Sampling  
33  
Total Alkalinity as Sodium Oxide (Na2O)  
34 – 36  
Sodium Bicarbonate (NaHCO3) and Sodium Carbonate (Na2CO3)  
37 – 39  
Matter Insoluble in Water  
40  
Sodium Bicarbonate:  
Sampling  
41  
Sodium Bicarbonate, Sodium Carbonate, and Free Moisture  
42 – 45  
Matter Insoluble in Water  
46  
Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosil- icate:  
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47  
Total Alkalinity as Sodium Oxide (Na2O)  
48 – 50  
Total Silica as SiO2  
51 – 53  
Sodium Metasilicate (Na2SiO3·5H2O)  
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Sodium Sesquisilicate (3Na2O·2SiO2·11H2O)  
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Matter Insoluble in Water  
56 and 57  
Loss on Ignition of Sodium Sesquisilicate (3Na2O·2SiO2 ·11H2O)  
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Orthophosphate  
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Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates

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These test methods cover the sampling and chemical analysis of paste, powder, or liquid detergent fatty alkyl sulfates. The different procedure for sampling and chemical analysis of past, powder, or liquid detergent are presented and discussed in details. Distillation test, titration test, and gravimetric test shall be performed to meet the requirements prescribed. The calculations methods for chlorides as sodium chloride are presented in details.
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Sections  
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Ester SO3:  
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Chlorides Calculated as Sodium Chloride (NaCl)  
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Standard Test Method for Cloud Point of Nonionic Surfactants

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3.1 The cloud point temperature is a reproducible characteristic of certain  pure  nonionic surfactants. It is also characteristic of certain nonionic surfactant formulated systems. This test method is appropriate for both systems.
Note 1: If the transition from a distinctly cloudy to a clear solution is not sharp, that is, if it does not take place within a range of 1 °C, this test method is not appropriate.
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1.1 This test method covers a procedure to determine the “cloud point” of nonionic surfactants or detergent systems. Cloud Point is the temperature at which dissolved components (solids or liquids) are no longer completely soluble, precipating as a second phase giving the fluid a cloudy appearance. It is limited to those surfactants and detergent systems for which the visible solubility change occurs over a range of 1 °C or less at concentrations of 0.5 % to 1.0 % in DI water between 30 °C and 95 °C.  
1.2 Chemical Limitations—Nonionic surfactants that exhibit a characteristic cloud point in general terms consist of a water-in-soluble moiety condensed with 50 % to 75 % by weight of ethylene oxide. If the level of ethoxylation is too low the surfactant may not be water soluble at temperatures less than 30 °C, and if it is too high no cloud point may exist.  
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ASTM D820-93(2023)(Test Method)
Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents

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These test methods detail the standard procedures for the chemical analysis of soaps containing synthetic detergents. The analytical procedures include the determination of the following chemical properties and substances: moisture and other matter volatile at a specified temperature; free alkali or free acid; anhydrous, salt-free soda soap; alcohol-soluble matter; matter insoluble in water; total alkalinity of matter insoluble in alcohol (alkaline salts); sodium silicate; phosphates; phosphates by colorimetric method using molybdenum blue); unsaponified and unsaponifiable matter; free fatty matter; chlorides in alcohol-soluble matter; rosin by McNicoll method; synthetic detergent by difference; and neutral inorganic salts.
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7 and 8  
Anhydrous, Salt-Free, Soda Soap  
9 – 12  
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Matter Insoluble in Water  
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Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts)  
16 and 17  
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Phosphates  
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Phosphate (Colorimetric Method Using Molybdenum Blue)  
29 – 34  
Unsaponified and Unsaponifiable Matter  
35 – 39  
Free Fatty Matter  
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Chlorides in Alcohol-Soluble Matter  
41 – 43  
Rosin (McNicoll Method)  
44 – 47  
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Neutral, Inorganic Salts  
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Standard Test Method for Foaming Properties of Surface-Active Agents

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This test method covers the determination of foaming properties of surface-active agents. Glass tubing apparatus for this test method shall include pipet and a receiver. Apparatus requirements like dimensions, shape, calibration marks, rubber stoppers, etc., shall conform to the specifications as indicated in this standard method. Test solution preparation shall include water preheating, adding the surface-active agent while stirring, and solution aging. Test procedure for foaming properties determination shall be done while surface-active solution is aging as indicated in this standard test method. Report shall include test solution concentration, temperature, water hardness, and foam height.
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Standard Guide for Evaluating Stain Removal Performance in Home Laundering

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5.1 This guide suggests a number of staining agents that are representative of stains commonly encountered in household laundry. The assessment need not be limited to this suggested list of stains, especially if special product types or end uses are being evaluated. This guide can be used to compare stain removal performance of products; however, there is no confirmed basis for correlation of this controlled laboratory technique with consumers’ ranking of stain removal performance.  
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5.3 The procedure is applicable to all types of home laundry products including detergents, presoak and prespotter products, bleaches, and detergent boosters and is expected to be applicable to horizontal and vertical axis machines.  
5.4 It is not intended for the evaluation of products or conditions normally associated with commercial laundering or dry cleaning establishments.
SCOPE
1.1 This is a guide for evaluating stain removal performance of home laundry products or home laundering conditions. It provides guidance for the selection, preparation, application, and examination of various types of stains on test fabrics that are subjected to controlled but practical stain removal treatment conditions.  
1.2 There is no single combination of stain and fabric that will predict the overall performance of a product or treatment method. A single test, even with a variety of stains/fabrics, can only predict how products or treatment methods compare under the particular conditions chosen for evaluations. A series of assessments is necessary to evaluate the many aspects of stain removal performance and to simulate consumer experience more closely.  
1.3 In this guide, the use of both traditional top-loader washing machines as well as front and top-loading high-efficiency washers is addressed.  
1.4 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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ASTM
ASTM D4008-19(Guide)
Standard Guide for Measuring Anti-Soil Deposition Properties of Laundry Detergents

SIGNIFICANCE AND USE
5.1 The guide can be used to compare anti-redeposition performance of products; however, there is no confirmed basis for correlation of this controlled laboratory technique with consumers’ ranking of anti-redeposition performance.
SCOPE
1.1 This guide provides direction for measuring the ability of detergents to prevent the deposition of soils from detergent solutions onto fabrics. It is intended as a laboratory screening test to aid in the formulation of detergent products, for quality control, and as a basis between the purchaser and seller in standardizing specific products' performance.  
1.2 The anti-soil deposition performance of detergent products will vary greatly depending on the type of soils and fabrics used in the test. Therefore, selection of the soils, fabrics, reference detergents, and test conditions shall be made by agreement between the interested parties on the basis of experience.  
1.3 There is no single or combination of oily soils or particulate soils, or both, that will precisely predict overall the performance of a product or treatment with respect to anti-redeposition as perceived by a consumer. This guide is intended to assess or compare detergent performance with respect to the anti-redeposition performance for the specific soil chosen.  
1.4 The values stated in either inch-pound or SI units are to be regarded separately as the standard. The values given in parentheses are for information only.  
1.5 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, health, and environmental 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.  
1.6 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.

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  • Guide
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