ASTM D5354-95(2001)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5354–95 (Reapproved 2001)
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.4 Sodium Sulfate (Na SO ), anhydrous.
2 4
4.5 Potassium Hydroxide, Alcoholic Standard Solution (0.5
1.1 This test method covers the determination of the total
N)—Accurately prepare and standardize a 0.5 N alcoholic
active ingredients in a sample of sulfonated or sulfated oil, or
potassium hydroxide (KOH) solution, the strength of which
both, as it exists in the original sample by extracting the
shall be expressed as milligrams of KOH per millilitre; 1 mL
undecomposed sulfonated or sulfated fat and other fatty matter
of 0.5 N alcoholic KOH solution is equivalent to 28.05 mg of
overanacidifiedconcentratedsaltsolution.Freealkalioralkali
KOH.
bound as soap is not included. This test method was derived
from Test Methods D500.
5. Procedure
NOTE 1—In the case of sulfated oils only, this determination may also
5.1 The procedure consists of isolating and purifying the
be estimated by calculation (see 6.3), as it is equivalent to the sum of the
fatty matter as it exists in the original oil by dissolving the
desulfated fatty matter and neutralized organically combined sulfuric
sample in a solvent, acidifying and washing with saturated
anhydride.
brine, and weighing the purified extract. Proceed as described
1.2 The values stated in SI units are to be regarded as the
in the determination of organically combined sulfuric anhy-
standard.
dride, Test Method B, in the absence of ammonia (6.1.1),
1.3 This standard does not purport to address all of the
retainingtheseparatedactiveingredientsinthe150-mLbeaker
safety concerns, if any, associated with its use. It is the
instead of transferring it to a crucible. Evaporate the filtrate to
responsibility of the user of this standard to establish appro-
a total volume of about 20 mL, add exactly 2 mL of alcoholic
priate safety and health practices and determine the applica-
KOH solution, mix the contents by swirling, and finally
bility of regulatory limitations prior to use.
evaporate until practically free from ether.
2. Referenced Documents
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
2.1 ASTM Standards:
residue.
D500 Test Methods of Chemical Analysis of Sulfonated
5.2 Dry the residue at 108 to 112°C for 1 ⁄2 h, cool in a
and Sulfated Oils
desiccator, and weigh. Repeat the heating for 30-min periods
3. Significance and Use
until constant weight is obtained.
3.1 Thistestmethodisintendedforthedeterminationofthe
6. Calculation
total active ingredients contained in sulfonated and sulfated
6.1 Correction for the Alkali Added—Calculate the correc-
oils. Free alkali and alkaline soaps are excluded.
tion for the alkali added as follows:
4. Reagents
Correctionforalkaliadded,g 50.00
...