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

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
1
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
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
1
This test method is under the jurisdiction ofASTM Committee D31 on Leather
residue.
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
1
method was developed in cooperation with the American Leather Chemists Assn. 5.2 Dry the residue at 108 to 112°C for 1 ⁄2 h, cool in a
(Method H46-1957).
desiccator, and weigh. Repeat the heating for 30-min periods
Current edition approved April 1, 2020. Published April 2020. Originally
until constant weight is obtained.
approved in 1993. Last previous edition approved in 2012 as D5354–95(2012).
DOI: 10.1520/D5354-95R20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6. Calculation
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
6.1 Correction for the Alkali Added—Calculate the correc-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tion for the alkali added as follows:
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D5354 − 95 (2020)
Correctionforalkaliadded, g 5 0.0006791 AS (1
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