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ASTM D1681-05

(Test Method)

Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure

Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure

SIGNIFICANCE AND USE
This test method determines anionic detergents commonly found in laundry, dishwashing, and other cleaning materials. Accurate determination of the anionic active substance is highly important in assessing the cost and effectiveness of such cleaning substances.
SCOPE
1.1 Direct titration of an anionic surfactant with a standardized cationic reagent is a simple and convenient method for the quantitative determination of the content of active ingredient. The end point is detffected by the transfer of a colored complex from an organic solvent phase to an aqueous phase. The relationship between anionic and cationic agents is not always stoichiometric, and for maximum accuracy the anionic type of interest should first be characterized and then used to standardize the cationic reagent. In most cases, however, the different anionic surfactants likely to be encountered react in the same proportions. That is, a cationic titrating solution standardized against a characterized anionic agent can be used to analyze other anionics of known molecular weights.
1.2 This test method is applicable to alkylaryl sulfonates and fatty alkyl sulfates. Low results are obtained with alkylbenzene sulfonates having the alkyl chain length less than eight carbon atoms. Low results are also obtained for alkyl sulfates with the alkyl chain length of less than twelve carbon atoms. The anionic surfactants characterized in accordance with Sections should be the sodium salt and not amine, ammonium, or potassium salts. In case only amine or ammonium salts are available, they should be first converted to the sodium salt before proceeding with this analysis.
1.3 The analytical procedures appear in the following order:SectionsSeparation of Alcohol-Soluble Matter8 and 9Separation of Oil-Free Sulfonate10 and 11 Determination of Sodium Chloride (NaCl) Content12-17 Characterization of Anionic Surfactant Standard:Part I. Determination of Surfactant, SO3  Content, and Solution Molarity18-20Part II. Determination of Surfactant, SO3  and Active IngredientContents Combining Weight, and Solution Molarity21-24 Standardization of Cationic Reagent25-29Quantitative Determination of Anionic Surfactant by Cationic Titration30-33
1.4This 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. For a specific hazards statement, see Section .

General Information

Status
Historical
Publication Date
30-Apr-2005
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 D1681-92(1997) - Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure
Effective Date
01-May-2005
Referred By
ASTM D5806-95(2017) - Standard Test Method for Disinfectant Quaternary Ammonium Salts by Potentiometric Titration
Effective Date
01-May-2005
Referred By
ASTM D2358-16 - Standard Test Method for Separation of Active Ingredient from Surfactant and Syndet Compositions
Effective Date
01-May-2005
Referred By
ASTM D4251-89(2016) - Standard Test Method for Active Matter in Anionic Surfactants by Potentiometric Titration
Effective Date
01-May-2005

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ASTM D1681-05 - Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration ProcedureASTM D1681-05 - Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure
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ASTM D1681-05 - Standard Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure
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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: D1681 − 05
StandardTest Method for
Synthetic Anionic Active Ingredient in Detergents by
1
Cationic Titration Procedure
This standard is issued under the fixed designation D1681; 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 1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 Direct titration of an anionic surfactant with a standard-
responsibility of the user of this standard to establish appro-
ized cationic reagent is a simple and convenient method for the
priate safety and health practices and determine the applica-
quantitative determination of the content of active ingredient.
bility of regulatory limitations prior to use. For a specific
Theendpointisdetffectedbythetransferofacoloredcomplex
hazards statement, see Section 7.
from an organic solvent phase to an aqueous phase. The
relationship between anionic and cationic agents is not always
2. Referenced Documents
stoichiometric, and for maximum accuracy the anionic type of
2
2.1 ASTM Standards:
interest should first be characterized and then used to standard-
D1193 Specification for Reagent Water
ize the cationic reagent. In most cases, however, the different
anionic surfactants likely to be encountered react in the same
3. Summary of Test Method
proportions. That is, a cationic titrating solution standardized
against a characterized anionic agent can be used to analyze 3.1 This test method involves isolating alkylaryl sulfonate
other anionics of known molecular weights.
orfattyalkylsulfatebyextractionwithethylalcoholtoremove
inorganic salts, extracting the alcohol-soluble material with
1.2 This test method is applicable to alkylaryl sulfonates
petroleum ether to remove unsulfonatable matter, correcting
and fatty alkyl sulfates. Low results are obtained with alkyl-
for sodium chloride present, and determining the active ingre-
benzenesulfonateshavingthealkylchainlengthlessthaneight
dientcombiningweight.Thecharacterizedsurfactantisusedto
carbon atoms. Low results are also obtained for alkyl sulfates
standardize a cationic reagent which in turn is used to titrate
with the alkyl chain length of less than twelve carbon atoms.
similar anionic surfactants.
The anionic surfactants characterized in accordance with
Sections 17-23 should be the sodium salt and not amine,
4. Significance and Use
ammonium, or potassium salts. In case only amine or ammo-
4.1 This test method determines anionic detergents com-
nium salts are available, they should be first converted to the
monly found in laundry, dishwashing, and other cleaning
sodium salt before proceeding with this analysis.
materials. Accurate determination of the anionic active sub-
1.3 The analytical procedures appear in the following order:
stance is highly important in assessing the cost and effective-
Sections
ness of such cleaning substances.
Separation of Alcohol-Soluble Matter 8 and 9
Separation of Oil-Free Sulfonate 10 and 11
5. Interferences
Determination of Sodium Chloride (NaCl) Content 12-17
Characterization of Anionic Surfactant Standard:
5.1 With the exception of picrate, perchlorate, thiocyanate,
Part I. Determination of Surfactant, SO Content, and Solution 18-20
3
Molarity
nitrate, dichromate, and chromate, common inorganic anions
Part II. Determination of Surfactant, SO and Active Ingredient 21-24
3
and low molecular weight organic anions do not interfere with
Contents Combining Weight, and Solution Molarity
this analysis. However, sulfonates of xylene, cunene, or tolu-
Standardization of Cationic Reagent 25-29
Quantitative Determination of Anionic Surfactant by Cationic 30-33
ene interfere positively. Since the cationic titration is con-
Titration
ducted under acidic conditions, soap does not interfere. Soap
must not be present in the anionic surfactant characterized in
accordance with Sections 17-23.
1
This test method is under the jurisdiction of ASTM Committee D12 on Soaps
and Other Detergentsand is the direct responsibility of Subcommittee D12.12 on
2
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2005. Published June 2005. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1959. Last previous edition approved in 1997 as D1681 – 92(1997). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D1681-05. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO
...

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ASTM D500-95(2023)(Test Method)
Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils

ABSTRACT
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.
SCOPE
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  
4 – 9  
Test Method B. Moisture and Volatile Matter by Hot-Plate Method  
10 – 14  
Organically Combined Sulfuric Anhydride:  
Test Method A. Titration Test  
15 – 19  
Test Method B. Extraction-Titration Test  
20 – 24  
Test Method C. Ash-Gravimetric Test (in the Presence of True
Sulfonates)  
25 – 28  
Total Desulfated Fatty Matter  
29 – 32  
Total Active Ingredients  
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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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ASTM D502-89(2023)(Test Method)
Standard Test Method for Particle Size of Soaps and Other Detergents

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This test method covers the determination of the particle size of soaps and other detergents by hand sieving and machine sieving methods.  
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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.
SCOPE
1.1 These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents.  
1.2 The procedures appear in the following order:    
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:  
Sampling  
47  
Total Alkalinity as Sodium Oxide (Na2O)  
48 – 50  
Total Silica as SiO2  
51 – 53  
Sodium Metasilicate (Na2SiO3·5H2O)  
54  
Sodium Sesquisilicate (3Na2O·2SiO2·11H2O)  
55  
Matter Insoluble in Water  
56 and 57  
Loss on Ignition of Sodium Sesquisilicate (3Na2O·2SiO2 ·11H2O)  
58 and 59  
Sodium Orthosilicate (Na4SiO4)  
60  
Trisodium Phosphate:  
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Trisodium Phosphate (Na3PO4) Content and Phosphorus Pentoxide (P2O5)  
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Matter Insoluble in Water  
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74  
Tetrasodium Pyrophosphate
(Na4P2O7)  
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Matter Insoluble in Water  
80 and 81  
Loss on Ignition  
82 and 83  
Borax:  
Sampling  
84  
Total Borate and Excess Alkalinity or Acidity  
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Matter Insoluble in Water  
88 and 89  
Sodium Triphosphate:  
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90  
Tritratable Na2O  
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Total P2O5:  
Preferred Method  
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Alternative Method  
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pH Titration  
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Paper Chromatographic Method  
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pH of 1 percent Solution  
128  
Turbidity  
129  
Temperature Rise  
130 – 134  
Sulfate  
135 – 137  
Ignition Loss  
140 and 141  
Matter Insoluble in Water  
142 – 144  
Particle Size  
145  
Orthophosphate  
146 – 151  
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ASTM D1570-95(2023)(Test Method)
Standard Test Methods for Sampling and Chemical Analysis of Fatty Alkyl Sulfates

ABSTRACT
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.
SCOPE
1.1 These test methods cover the sampling and chemical analysis of paste, powder, or liquid detergent fatty alkyl sulfates.  
1.2 The procedures for sampling and analysis appear in the following order:    
Sections  
Sampling:  
Powders and Flakes Packed in Cans or Cartons  
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Ester SO3:  
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Sections  
Ester SO3:  
Method B. Gravimetric Test Method  
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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

ABSTRACT
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.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of soaps containing synthetic detergents.  
1.2 The analytical procedures appear in the following order:    
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Matter Insoluble in Water  
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Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts)  
16 and 17  
Sodium Silicate  
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Phosphates  
21 – 28  
Phosphate (Colorimetric Method Using Molybdenum Blue)  
29 – 34  
Unsaponified and Unsaponifiable Matter  
35 – 39  
Free Fatty Matter  
40  
Chlorides in Alcohol-Soluble Matter  
41 – 43  
Rosin (McNicoll Method)  
44 – 47  
Synthetic Detergent (by Difference)  
48  
Neutral, Inorganic Salts  
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Standard Test Method for Foaming Properties of Surface-Active Agents

ABSTRACT
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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1.1 This test method covers the determination of the foaming properties of surface-active agents as defined in Terminology D459. This test method is applicable under limited and controlled conditions, but does not necessarily yield information correlating with specific end uses. This method is subjected to the operator of the method as the foam heights are not always level and an average height is determined by the user so it is more of a qualitative measurement in these instances. However, for foam measurements results taken on more flat uniform samples this method has more of a quantitative quality.  
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SIGNIFICANCE AND USE
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.  
5.2 The evaluations generated by this guide should be regarded as diagnostic screening tests that are useful in formulation studies, quality control, and ingredient raw material qualification. This guide provides considerable flexibility in choosing specific stains, washing conditions, and laboratory equipment appropriate to the objective of the evaluation. This procedural latitude may result in a reduced level of interlaboratory precision and such comparison of results must be evaluated with caution.  
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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