Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils

SIGNIFICANCE AND USE
3.1 This test method is intended for use in the determination of the unsaponifiable, nonvolatile matter contained in sulfated oils for the purpose of quality assurance.
SCOPE
1.1 This test method covers the determination of the unsaponifiable, nonvolatile (above 80°C) matter existing in a sample of sulfated oil by saponifying the desulfated fatty matter and extracting the unsaponifiable matter, and extracting the unsaponifiable matter from the soap solution with ethyl ether.  
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-2019
Technical Committee
D31 - Leather
Drafting Committee
D31.08 - Fats and Oils

Relations

Effective Date
01-Apr-2019
Effective Date
01-Apr-2019
Effective Date
01-Apr-2019
Effective Date
01-Apr-2012
Effective Date
01-Apr-2012
Effective Date
01-Apr-2009
Effective Date
01-Apr-2006
Effective Date
01-Apr-2006
Effective Date
10-May-2003
Effective Date
10-Oct-1997
Effective Date
01-Jan-1995
Effective Date
01-Jan-1995
Effective Date
01-Jan-1995
Effective Date
01-Jan-1995
Effective Date
01-Apr-2019

Overview

ASTM D5553-95(2019) is an international standard that defines a test method for the determination of unsaponifiable, nonvolatile matter in sulfated oils. Developed by ASTM International, this standard supports quality assurance by specifying a precise laboratory procedure for identifying the portion of sulfated oil samples that do not react during saponification and remain nonvolatile above 80°C. This test method is particularly relevant for industries relying on the consistent quality and composition of sulfated oils.

Key Topics

  • Scope: The method applies to any sulfated oil sample, determining components that do not saponify and are nonvolatile at temperatures above 80°C.
  • Procedure Outline:
    • Saponification of desulfated fatty matter in a glass flask with an air condenser.
    • Extraction of unsaponifiable matter from the soap solution using ethyl ether.
    • Sequential washing of ether extracts to purify the unsaponifiable fraction.
    • Gravimetric determination of residue after evaporating ether and drying at controlled temperatures.
  • Apparatus and Reagents:
    • Saponification flask, ethyl ether, alcoholic and aqueous potassium hydroxide (KOH) solutions.
  • Calculation: Unsaponifiable nonvolatile matter is calculated as a percentage based on the mass of the final residue relative to the original sample.
  • Safety and Compliance: The standard emphasizes the need for appropriate safety, health, and environmental practices, and encourages compliance with applicable regulatory requirements.

Applications

The ASTM D5553-95(2019) test method is vital across several sectors, particularly where sulfated oils are critical to product quality and process performance, such as:

  • Leather Industry: Used to assess the purity of sulfated oils applied in tanning and finishing processes, ensuring product performance and minimizing the presence of undesirable by-products.
  • Quality Control Laboratories: Essential for routine analysis during the production and certification of sulfated oils to uphold consistent specifications.
  • Research and Development: Provides a standardized approach for evaluating new formulations or modifications in raw materials.
  • Material Certification: Assures buyers and specifiers that supplied oils meet stringent international standards for unsaponifiable, nonvolatile matter.

Related Standards

  • ASTM D5350 - Test Method for Determination of Organically Combined Sulfuric Anhydride by Titration, Method A.
  • ASTM D5351 - Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Method B.
  • ASTM D5353 - Test Method for Determination of Total Desulfated Fatty Matter.

These related ASTM standards provide complementary methods for evaluating sulfated oil components, including sulfur content and total fatty matter, and can be used in conjunction with ASTM D5553-95(2019) for comprehensive quality assessments.


Utilizing ASTM D5553-95(2019) ensures reliable and repeatable measurement of unsaponifiable, nonvolatile matter in sulfated oils, supporting international trade, regulatory compliance, and product integrity in industries where these materials are essential. For more details or to purchase the standard, visit ASTM International.

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Frequently Asked Questions

ASTM D5553-95(2019) is a standard published by ASTM International. Its full title is "Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils". This standard covers: SIGNIFICANCE AND USE 3.1 This test method is intended for use in the determination of the unsaponifiable, nonvolatile matter contained in sulfated oils for the purpose of quality assurance. SCOPE 1.1 This test method covers the determination of the unsaponifiable, nonvolatile (above 80°C) matter existing in a sample of sulfated oil by saponifying the desulfated fatty matter and extracting the unsaponifiable matter, and extracting the unsaponifiable matter from the soap solution with ethyl ether. 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.

SIGNIFICANCE AND USE 3.1 This test method is intended for use in the determination of the unsaponifiable, nonvolatile matter contained in sulfated oils for the purpose of quality assurance. SCOPE 1.1 This test method covers the determination of the unsaponifiable, nonvolatile (above 80°C) matter existing in a sample of sulfated oil by saponifying the desulfated fatty matter and extracting the unsaponifiable matter, and extracting the unsaponifiable matter from the soap solution with ethyl ether. 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.

ASTM D5553-95(2019) is classified under the following ICS (International Classification for Standards) categories: 75.080 - Petroleum products in general. The ICS classification helps identify the subject area and facilitates finding related standards.

ASTM D5553-95(2019) has the following relationships with other standards: It is inter standard links to ASTM D5553-95(2012), ASTM D5353-95(2019), ASTM D5350-95(2019), ASTM D5350-95(2012), ASTM D5353-95(2012), ASTM D5351-93(2009), ASTM D5353-95(2006), ASTM D5350-95(2006), ASTM D5351-93(2003), ASTM D5351-93(1997), ASTM D5353-95, ASTM D5350-95, ASTM D5353-95(2001), ASTM D5350-95(2001), ASTM D5560-95(2018). Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

ASTM D5553-95(2019) is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

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:D5553 −95 (Reapproved 2019)
Standard Test Method for
Determination of the Unsaponifiable Nonvolatile Matter in
Sulfated Oils
This standard is issued under the fixed designation D5553; 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 (´) 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
3.1 This test method is intended for use in the determination
unsaponifiable, nonvolatile (above 80°C) matter existing in a
of the unsaponifiable, nonvolatile matter contained in sulfated
sample of sulfated oil by saponifying the desulfated fatty
oils for the purpose of quality assurance.
matter and extracting the unsaponifiable matter, and extracting
the unsaponifiable matter from the soap solution with ethyl
4. Apparatus and Reagents
ether.
4.1 Saponification Flask—The apparatus required for the
1.2 The values stated in SI units are to be regarded as
saponification consists of a glass flask provided with an air
standard. No other units of measurement are included in this
condenser.
standard.
4.2 Ethyl Ether.
1.3 This standard does not purport to address all of the
4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)—
safety concerns, if any, associated with its use. It is the
Dissolveapproximately,butnotlessthan,28gofKOHinethyl
responsibility of the user of this standard to establish appro-
alcohol and dilute to 1 L.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
1.4 This international standard was developed in accor-
Dissolve 28 g of potassium hydroxide (KOH) in water and
dance with internationally recognized principles on standard-
dilute to 1 L.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Procedure
mendations issued by the World Trade Organization Technical
5.1 The procedure consists of decomposing the sample with
Barriers to Trade (TBT) Committee.
mineralacid,extractingthedesulfatedfattymatter,saponifying
the latter, and extracting the unsaponifiable matter from the
2. Referenced Documents
soap solution with ethyl ether.
2.1 ASTM Standards:
5.1.1 Desulfated Fatty Matter—Determine the desulfated
D5350 Test Method for Determination of Organically Com-
fatty matter as described in the determination of total desul-
bined Sulfuric Anhydride by Titration, Test Method A
fated fatty matter. See Test Methods D5350, D5351, and
D5351 Test Method for Determination of Organically Com-
D5353.
bined Sulfuric Anhydride by Extraction Titration, Test
5.1.2 Saponification—Accurately weigh 2 to 2.5 g of the
Method B
desulfated fatty matter in the flask, add 25 mL of the alcoholic
D5353 Test Method for Determination of Total Desulfated
KOH solution, and simmer the contents (without loss of
Fatty Matter
alcohol) for 1 h with occasional swirling, over an electric hot
plate or other source of heat.
1 5.1.3 Extraction—Transfer the content of the flask to a
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
250-mL separatory funnel and wash the flask several times
method was developed in cooperation with the American Leather Chemists Assn.
with a total of 50 mL of water, pouring it into the separatory
(Method H 47–1957).
funnel. Extract the solution while still warm (about 30°C) with
Current edition approved April 1, 2019. Published April 2019. Originally
50 mL of ether (rinse the saponification flask with the ether
approved in 1994. Last previous edition approved in 2012 as D5553 – 95(2012).
DOI: 10.1520/D5553-95R19.
before adding it to the separatory funnel), shaking vigorously
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
for about 1 min, and allow the layers to settle and clear. Draw
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
off the lower layer in a second 250-mL separatory funnel and
Standards volume information, refer to the standard’
...

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