ASTM D5354-95(2020)

Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils

SIGNIFICANCE AND USE
3.1 This test method is intended for the determination of the total active ingredients contained in sulfonated and sulfated oils. Free alkali and alkaline soaps are excluded.
SCOPE
1.1 This test method covers the determination of the total active ingredients in a sample of sulfonated or sulfated oil, or both, as it exists in the original sample by extracting the undecomposed sulfonated or sulfated fat and other fatty matter over an acidified concentrated salt solution. Free alkali or alkali bound as soap is not included. This test method was derived from Test Methods D500.  
Note 1: In the case of sulfated oils only, this determination may also be estimated by calculation (see 6.3), as it is equivalent to the sum of the desulfated fatty matter and neutralized organically combined sulfuric anhydride.  
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, 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.

General Information

• Status: Published
• Publication Date: 31-Mar-2020
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5354-95(2012) - Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils
• Effective Date: 01-Apr-2020
• Refers: ASTM D500-95(2009) - Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
• Effective Date: 01-Oct-2009
• Refers: ASTM D500-95(2003) - Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
• Effective Date: 15-Apr-1995
• Refers: ASTM D500-95 - Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
• Effective Date: 01-Jan-1995

Overview

ASTM D5354-95(2020) is the internationally recognized standard test method for the determination of total active ingredients in sulfonated and sulfated oils. Developed and maintained by ASTM International, this method provides a reliable approach for quantifying the active compounds present in both sulfonated and sulfated oils. Critically, it excludes results from free alkali and alkaline soaps, ensuring that only the active ingredients intrinsic to the oil itself are measured. This standard supports quality control, process optimization, and regulatory compliance in industries that work with these specialized oils.

Key Topics

• Scope of Application: Applies specifically to original samples containing sulfonated or sulfated oils, evaluating total active ingredients via extraction over an acidified, concentrated salt solution.
• Free Alkali Exclusion: The method distinguishes between active oil components and free alkali or alkali bound as soap, which are not included in the determination.
• Calculation Methods: For sulfated oils, total active ingredients may also be calculated as the sum of desulfated fatty matter and neutralized, organically combined sulfuric anhydride.
• SI Units: All results and procedures under this standard utilize SI units exclusively.
• Safety and Responsibility: Users must independently ensure that appropriate safety, health, and environmental procedures are followed when applying this standard.
• Traceability and Compliance: Developed according to internationally recognized principles and World Trade Organization guidelines to facilitate global trade and regulatory acceptance.

Applications

ASTM D5354-95(2020) is widely used in several industries working with specialized sulfonated and sulfated oils, including:

• Leather Industry: Essential for the quality control of fatliquors and other oil-based leather treating agents where precise content of active ingredients affects product performance.
• Industrial Oil Production: Supports manufacturers of specialty lubricants and processing aids, where consistent active ingredient levels are crucial for formulation and customer specifications.
• Quality Control Laboratories: Provides a standardized, reproducible method that helps ensure product consistency and regulatory compliance.
• Research and Development: Useful in evaluating new formulations or processing aids that leverage sulfonated or sulfated oils.

By ensuring accurate determination of active oil materials, this standard underpins product quality, helps prevent batch variability, and meets customer as well as regulatory requirements.

Related Standards

Several ASTM standards and referenced documents are relevant to professionals working with ASTM D5354-95(2020):

• ASTM D500: Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils - foundational to the procedures outlined in D5354.
• Other ASTM Standards: Applicable supporting standards can be found on the ASTM International website, where document summaries and updated references are maintained.

Keywords: total active ingredients, sulfonated oils, sulfated oils, ASTM D5354, standardized test method, leather industry, quality control, SI units, regulatory compliance

For further details and procedure specifics, users are encouraged to consult the official ASTM publication and ensure all regulatory and safety protocols are in place. Regular use of this standard helps maintain consistent product quality and supports international best practices in oil analysis.

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: D5354 − 95 (Reapproved 2020)
Standard Test Method for
Determination of Total Active Ingredients in Sulfonated and
Sulfated Oils
This standard is issued under the fixed designation D5354; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Significance and Use
1.1 This test method covers the determination of the total 3.1 Thistestmethodisintendedforthedeterminationofthe
active ingredients in a sample of sulfonated or sulfated oil, or total active ingredients contained in sulfonated and sulfated
both, as it exists in the original sample by extracting the oils. Free alkali and alkaline soaps are excluded.
undecomposed sulfonated or sulfated fat and other fatty matter
overanacidifiedconcentratedsaltsolution.Freealkalioralkali 4. Reagents
bound as soap is not included. This test method was derived
4.1 Ethyl Ether.
from Test Methods D500.
4.2 MethylOrangeIndicatorSolution(1g/L)—Dissolve0.1
NOTE 1—In the case of sulfated oils only, this determination may also
g of methyl orange in 100 mL of water.
be estimated by calculation (see 6.3), as it is equivalent to the sum of the
4.3 Sodium Chloride (NaCl), solid.
desulfated fatty matter and neutralized organically combined sulfuric
anhydride.
4.4 Sodium Sulfate (Na SO ), anhydrous.
2 4
1.2 The values stated in SI units are to be regarded as
4.5 Potassium Hydroxide, Alcoholic Standard Solution (0.5
standard. No other units of measurement are included in this
N)—Accurately prepare and standardize a 0.5 N alcoholic
standard.
potassium hydroxide (KOH) solution, the strength of which
1.3 This standard does not purport to address all of the
shall be expressed as milligrams of KOH per millilitre; 1 mL
safety concerns, if any, associated with its use. It is the
of 0.5 N alcoholic KOH solution is equivalent to 28.05 mg of
responsibility of the user of this standard to establish appro-
KOH.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
5. Procedure
1.4 This international standard was developed in accor-
5.1 The procedure consists of isolating and purifying the
dance with internationally recognized principles on standard-
fatty matter as it exists in the original oil by dissolving the
ization established in the Decision on Principles for the
sample in a solvent, acidifying and washing with saturated
Development of International Standards, Guides and Recom-
brine, and weighing the purified extract. Proceed as described
mendations issued by the World Trade Organization Technical
in the determination of organically combined sulfuric
Barriers to Trade (TBT) Committee.
anhydride, Test Method B, in the absence of ammonia (6.1.1),
retainingtheseparatedactiveingredientsinthe150-mLbeaker
2. Referenced Documents
instead of transferring it to a crucible. Evaporate the filtrate to
2.1 ASTM Standards:
a total volume of about 20 mL, add exactly 2 mL of alcoholic
D500Test Methods of ChemicalAnalysis of Sulfonated and
KOH solution, mix the contents by swirling, and finally
Sulfated Oils
evaporate until practically free from ether.
NOTE 2—With highly sulfonated or sulfated oil, it may be necessary to
add 5 to 10 mL of the alcoholic KOH solution in order to stabilize the
This test method is under the jurisdiction ofASTM Committee D31 on Leather
residue.
and is the direct responsibility of Sub
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