ASTM D5354-95(2012)

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

SIGNIFICANCE AND USE
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 31-Mar-2012
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5354-95(2006) - Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils
• Effective Date: 01-Apr-2012
• Replaced By: ASTM D5354-95(2020) - Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils
• Effective Date: 01-Apr-2020

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5354 − 95 (Reapproved 2012)
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 4. Reagents
1.1 This test method covers the determination of the total 4.1 Ethyl Ether.
active ingredients in a sample of sulfonated or sulfated oil, or
4.2 MethylOrangeIndicatorSolution(1g/L)—Dissolve0.1
both, as it exists in the original sample by extracting the
g of methyl orange in 100 mL of water.
undecomposed sulfonated or sulfated fat and other fatty matter
4.3 Sodium Chloride (NaCl), solid.
overanacidifiedconcentratedsaltsolution.Freealkalioralkali
bound as soap is not included. This test method was derived
4.4 Sodium Sulfate (Na SO ), anhydrous.
2 4
from Test Methods D500.
4.5 Potassium Hydroxide, Alcoholic Standard Solution (0.5
NOTE 1—In the case of sulfated oils only, this determination may also
N)—Accurately prepare and standardize a 0.5 N alcoholic
be estimated by calculation (see 6.3), as it is equivalent to the sum of the
potassium hydroxide (KOH) solution, the strength of which
desulfated fatty matter and neutralized organically combined sulfuric
shall be expressed as milligrams of KOH per millilitre; 1 mL
anhydride.
of 0.5 N alcoholic KOH solution is equivalent to 28.05 mg of
1.2 The values stated in SI units are to be regarded as
KOH.
standard. No other units of measurement are included in this
standard.
5. Procedure
1.3 This standard does not purport to address all of the
5.1 The procedure consists of isolating and purifying the
safety concerns, if any, associated with its use. It is the
fatty matter as it exists in the original oil by dissolving the
responsibility of the user of this standard to establish appro-
sample in a solvent, acidifying and washing with saturated
priate safety and health practices and determine the applica-
brine, and weighing the purified extract. Proceed as described
bility of regulatory limitations prior to use.
in the determination of organically combined sulfuric
anhydride, Test Method B, in the absence of ammonia (6.1.1),
2. Referenced Documents
retainingtheseparatedactiveingredientsinthe150-mLbeaker
2.1 ASTM Standards:
instead of transferring it to a crucible. Evaporate the filtrate to
D500Test Methods of ChemicalAnalysis of Sulfonated and
a total volume of about 20 mL, add exactly 2 mL of alcoholic
Sulfated Oils
KOH solution, mix the contents by swirling, and finally
evaporate until practically free from ether.
3. Significance and Use
NOTE 2—With highly sulfonated or sulfated oil, it may be necessary to
3.1 Thistestmethodisintendedforthedeterminationofthe
add 5 to 10 mL of the alcoholic KOH solution in order to stabilize the
total active ingredients contained in sulfonated and sulfated residue.
oils. Free alkali and alkaline soaps are excluded.
5.2 Dry the residue at 108 to 112°C for 1 ⁄2 h, cool in a
desiccator, and weigh. Repeat the heating for 30-min periods
until constant weight is obtained.
This test method is under the jurisdiction ofASTM Committee D31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
6. Calculation
...