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ASTM D820-93(2023)

(Test Method)

Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents

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:    
Sections  
Moisture and Other Matter Volatile at 105°C (Oven Method)  
5 and 6  
Free Alkali or Free Acid  
7 and 8  
Anhydrous, Salt-Free, Soda Soap  
9 – 12  
Alcohol-Soluble Matter  
13 and 14  
Matter Insoluble in Water  
15 and 15  
Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts)  
16 and 17  
Sodium Silicate  
18 – 20  
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  
49  
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 problems, 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.  
1.5 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.

General Information

Status
Published
Publication Date
30-Jun-2023
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

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ASTM D820-93(2023) - Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents
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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: D820 − 93 (Reapproved 2023)
Standard Test Methods for
Chemical Analysis of Soaps Containing Synthetic
1
Detergents
This standard is issued under the fixed designation D820; 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
2
1.1 These test methods cover procedures for the chemical 2.1 ASTM Standards:
analysis of soaps containing synthetic detergents. D216 Method of Test for Distillation of Natural Gasoline
3
(Withdrawn 1988)
1.2 The analytical procedures appear in the following order:
D459 Terminology Relating to Soaps and Other Detergents
Sections
D875 Method for Calculating of Olefins and Aromatics in
Moisture and Other Matter Volatile at 105°C (Oven Method) 5 and 6 Petroleum Distillates from Bromine Number and Acid
3
Free Alkali or Free Acid 7 and 8
Absorption (Withdrawn 1984)
Anhydrous, Salt-Free, Soda Soap 9 – 12
D1193 Specification for Reagent Water
Alcohol-Soluble Matter 13 and 14
Matter Insoluble in Water 15 and 15 D1768 Test Method for Sodium Alkylbenzene Sulfonate in
Total Alkalinity of Matter Insoluble in Alcohol (Alkaline Salts) 16 and 17
Synthetic Detergents by Ultraviolet Absorption
Sodium Silicate 18 – 20
D2357 for Qualitative Classification of Surfactants by Infra-
Phosphates 21 – 28
Phosphate (Colorimetric Method Using Molybdenum Blue) 29 – 34
red Absorption
Unsaponified and Unsaponifiable Matter 35 – 39
D2358 Test Method for Separation of Active Ingredient from
Free Fatty Matter 40
Surfactant and Syndet Compositions
Chlorides in Alcohol-Soluble Matter 41 – 43
Rosin (McNicoll Method) 44 – 47 D3049 Test Method for Synthetic Anionic Ingredient by
Synthetic Detergent (by Difference) 48
Cationic Titration
Neutral, Inorganic Salts 49
1.3 The values stated in SI units are to be regarded as
3. Terminology
standard. No other units of measurement are included in this
3.1 Definitions:
standard.
3.2 The term synthetic detergent in these test methods is
1.4 This standard does not purport to address all of the
defined in accordance with Terminology D459, as follows:
safety problems, if any, associated with its use. It is the
3.3 synthetic detergent—a detergent produced by chemical
responsibility of the user of this standard to establish appro-
synthesis and comprising an organic composition other than
priate safety, health, and environmental practices and deter-
soap.
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
3.4 For definitions of other terms used in these test methods,
dance with internationally recognized principles on standard-
refer to Terminology D459.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- 4. Purity of Reagents and Materials
mendations issued by the World Trade Organization Technical
4.1 Purity of Reagents—Reagent grade chemicals shall be
Barriers to Trade (TBT) Committee.
used in all tests. Unless otherwise indicated, it is intended that
1
These test methods are under the jurisdiction of ASTM Committee D12 on
2
Soaps and Other Detergentsand 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 July 1, 2023. Published July 2023. Originally approved the ASTM website.
3
in 1945. Last previous edition approved in 2016 as D820 – 93 (2016). DOI: The last approved version of this historical standard is referenced on
10.1520/D0820-93R23. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D820 − 93 (2023)
surfactant mixtures containing borax are unreliable, due to solubility of
all reagents shall conform to the specifications of the Commit-
borax in hot alcohol.
tee on Analytical Reagents of the American Chemical Society,
4
where such specifications are available. Other grades may be
ANHYDROUS, SALT-FREE, SODA SOAP
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
9. Apparatus
accuracy of the determination.
9.1 Extrac
...

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Sampling:  
Powders and Flakes Packed in Cans or Cartons  
4  
Powders and Flakes in Bulk  
5  
Liquids  
6  
Pastes  
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Preparation of Sample  
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Sections  
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3.1 The guide, as now constituted, is not suitable for ranking of hand dishwashing products, since no basis is available at this time for correlation of the foam stability of these products using any particular food soil or combination of soils with consumers' ranking of performance.  
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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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Sections  
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Sodium Hydroxide (NaOH)  
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Apparent Density  
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Total Alkalinity as Sodium Oxide (Na2O)  
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Matter Insoluble in Water  
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58 and 59  
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61  
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Tetrasodium Pyrophosphate
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Matter Insoluble in Water  
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Loss on Ignition  
82 and 83  
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Total Borate and Excess Alkalinity or Acidity  
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Matter Insoluble in Water  
88 and 89  
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Tritratable Na2O  
91 – 94  
Total P2O5:  
Preferred Method  
95 – 97  
Alternative Method  
98 – 101  
pH Titration  
102 – 107  
Quantitative Separation and Measurement of Various Phosphates:  
Reverse-Flow Ion-Exchange Chromatography (Preferred Method)  
108 – 119  
Paper Chromatographic Method  
120 – 127  
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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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
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SIGNIFICANCE AND USE
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SIGNIFICANCE AND USE
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.
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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.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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