ASTM D5354-95
(Test Method)Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils
Standard Test Method for Determination of Total Active Ingredients in Sulfonated and Sulfated Oils
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 the 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.
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Designation: D 5354 – 95
Standard Test Method for
Determination of Total Active Ingredients in Sulfonated and
Sulfated Oils
This standard is issued under the fixed designation D 5354; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope N)—Accurately prepare and standardize a 0.5 N alcoholic
potassium hydroxide (KOH) solution, the strength of which
1.1 This test method covers the determination of the total
shall be expressed as milligrams of KOH per millilitre; 1 mL of
active ingredients in a sample of sulfonated or sulfated oil, or
0.5 N alcoholic KOH solution is equivalent to 28.05 mg of
both, as it exists in the original sample by extracting the
KOH.
undecomposed sulfonated or sulfated fat and other fatty matter
over an acidified concentrated salt solution. Free alkali or alkali
5. Procedure
bound as soap is not included. This test method was derived
5.1 The procedure consists of isolating and purifying the
from Test Methods D 500.
fatty matter as it exists in the original oil by dissolving the
NOTE 1—In the case of sulfated oils only, this determination may also
sample in a solvent, acidifying and washing with saturated
be estimated by calculation (see 6.3), as it is equivalent to the sum of the
brine, and weighing the purified extract. Proceed as described
desulfated fatty matter and neutralized organically combined sulfuric
in the determination of organically combined sulfuric anhy-
anhydride.
dride, Test Method B, in the absence of ammonia (6.1.1),
1.2 The values stated in SI units are to be regarded as the
retaining the separated active ingredients in the 150-mL beaker
standard.
instead of transferring it to a crucible. Evaporate the filtrate to
1.3 This standard does not purport to address all of the
a total volume of about 20 mL, add exactly 2 mL of alcoholic
safety concerns, if any, associated with its use. It is the
KOH solution, mix the contents by swirling, and finally
responsibility of the user of this standard to establish appro-
evaporate until practically free from ether.
priate safety and health practices and determine the applica-
NOTE 2—With highly sulfonated or sulfated oil, it may be necessary to
bility of regulatory limitations prior to use.
add 5 to 10 mL of the alcoholic KOH solution in order to stabilize the
residue.
2. Referenced Documents
5.2 Dry the residue at 108 to 112°C for 1 ⁄2 h, cool in a
2.1 ASTM Standards:
desiccator, and weigh. Repeat the heating for 30-min periods
D 500 Test Methods of Chemical Analysis of Sulfonated
until constant weight is obtained.
and Sulfated Oils
6. Calculation
3. Significance and Use
6.1 Correction for the Alkali Added—Calculate the correc-
3.1 This test method is intended for the determination of the
tion for the alkali added as follows:
total active ingredients contained in sulfonated and sulfated
oils. Free alkali and alkaline soaps are excluded.
Correction for alkali added, g 5 0.0006791 AS (1)
4. Reagents
where:
A 5 millilitres of KOH solution added,
4.1 Ethyl Ether.
S 5 strength of KOH solution, mg o
...
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