ASTM D5349-19

Standard Test Method for Determination of the Moisture and Volatile Content of Sulfonated, Sulfated Oils and Fatliquors by Oven Method

SIGNIFICANCE AND USE
3.1 This test method is intended to determine the moisture and volatile content of sulfonated, sulfated oil, fats, oils, fatliquors, and softening compounds.
SCOPE
1.1 This test method covers the determination of moisture and other volatile material under conditions of the test. It is applicable to sulfonated, sulfated oils, fats, oils, fatliquors, and softening compounds.  
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-Oct-2019
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5349-95(2012) - Standard Test Method for Determination of the Moisture and Volatile Content of Sulfonated and Sulfated Oils by Hot-Plate Method
• Effective Date: 01-Nov-2019
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM D500-95(2009) - Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
• Effective Date: 01-Oct-2009
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-06 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004

Overview

ASTM D5349-19 is the internationally recognized standard test method for determining the moisture and volatile content in sulfonated, sulfated oils, fats, oils, fatliquors, and softening compounds. Developed under the jurisdiction of ASTM Committee D31 on Leather, this standard provides a precise oven method for measuring water and volatile substances contained in products commonly used in the leather industry, as well as other industrial applications requiring accurate composition analysis of fatliquor and oil-based formulations.

This method is essential for quality control, process monitoring, and specification compliance, ensuring consistency and performance in materials such as sulfonated oils and fatliquors. The standard follows globally accepted principles established by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Key Topics

• Moisture and Volatile Content: ASTM D5349-19 details the determination of water and volatile substances in target oils and compounds by using an oven-based rapid evaporation process at approximately 105 °C.
• Applicability: The method is suitable for sulfonated and sulfated oils, fats, oils, and fatliquors, provided these do not contain reactive additives like mineral acids or certain volatile components.
• Test Apparatus: The procedure requires a glass beaker, accurate weighing instruments, a mechanical-convection oven with temperature control, desiccators, appropriate thermometers, and analytical scales with a minimum readability of three decimal places.
• Procedure: Samples are weighed and subjected to controlled oven heating, allowing moisture and volatiles to evaporate. Weight loss calculations determine the percentage of volatile content.
• Precision: The standard includes detailed guidance on repeatability and reproducibility limits, ensuring reliable results across laboratories.

Applications

ASTM D5349-19 offers significant practical value for:

• Leather Processing and Manufacturing: Accurate moisture and volatile content determination is crucial for the effectiveness and quality of fatliquors and softening agents during leather softening, stuffing, and finishing.
• Quality Assurance: Routine testing of input materials using this standard helps manufacturers comply with product specifications and maintain consistent performance in oils and softening compounds.
• Research and Product Development: Formulators benefit from this method when comparing or improving oil-based formulations for industrial, cosmetic, or leather-related uses.
• Regulatory Compliance: Following ASTM D5349-19 assists manufacturers and laboratories in meeting international quality and safety requirements for chemical analysis of sulfonated and sulfated products.

Related Standards

ASTM D5349-19 references and complements several other ASTM standards, including:

• ASTM D500 - Test Methods for Chemical Analysis of Sulfonated and Sulfated Oils
• ASTM E691 - Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• ASTM E177 - Practice for Use of the Terms Precision and Bias in ASTM Test Methods

For further technical details, laboratory best practices, or additional chemical analysis methods, users should consult these related documents and standards.

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Keywords: ASTM D5349-19, moisture content, volatile content, sulfonated oils, sulfated oils, fatliquors, oven method, leather industry, quality control, standard test method, analytical testing.

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: D5349 − 19
Standard Test Method for
Determination of the Moisture and Volatile Content of
Sulfonated, Sulfated Oils and Fatliquors by Oven Method
This standard is issued under the fixed designation D5349; 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 moisture 3.1 This test method is intended to determine the moisture
and other volatile material under conditions of the test. It is and volatile content of sulfonated, sulfated oil, fats, oils,
applicable to sulfonated, sulfated oils, fats, oils, fatliquors, and fatliquors, and softening compounds.
softening compounds.
4. Apparatus
1.2 The values stated in SI units are to be regarded as
4.1 Oven, mechanical-convection draft capable of setting at
standard. No other units of measurement are included in this
100 – 105 °C with a thermoregulatory system,
standard.
4.2 Glass Beakers, 100 to 150 mL,
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.3 Desiccator, containing an efficient desiccant,
responsibility of the user of this standard to establish appro-
4.4 Analytical Scale, capable of reading at minimum 3
priate safety, health, and environmental practices and deter-
decimal places.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor-
5. Procedure
dance with internationally recognized principles on standard-
5.1 Weigh a beaker that has been previously dried and
ization established in the Decision on Principles for the
cooled in a desiccator.
Development of International Standards, Guides and Recom-
5.2 Accurately weigh 0.5 g of a well-mixed sample into the
mendations issued by the World Trade Organization Technical
beaker. Place the beaker in the oven, with the temperature set
Barriers to Trade (TBT) Committee.
to 105 – 100 °C.
2. Referenced Documents
5.3 After exactly 1 h, remove the beaker from the oven.
Cool to room temperature in a desiccator and weigh.
2.1 ASTM Standards:
D500 Test Methods of ChemicalAnalysis of Sulfonated and
6. Calculation and Report
Sulfated Oils
6.1 Report the moisture and volatile matter in percent, by
E691 Practice for Conducting an Interlaboratory Study to
weight, employing the calculation:
Determine the Precision of a Test Method
E177 Practice for Use of the Terms Precision and Bias in
% Volatile matter ~moisture!5 @~S 1 B! 2 D ⁄ S# 3100 (1)
ASTM Test Methods
where:
S = linitial sample weight,
B = weight of empty beaker, and
This test method is under the jurisdiction ofASTM Committee D31 on Leather
D = weight of dried sample plus beaker.
and is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis test
method was developed in cooperation with the American Leather Chemists Assn.
6.2 Reference this test method in the test report.
(Method H 41–1957).
Current edition approved Nov. 1, 2019. Published December 2019. Originally
7. Precision and Bias
approved in 1993. Last previous edition approved in 2012 as D5349 – 95(2012).
DOI: 10.1520/D5349-19.
7.1 The precision of this test method is based on an
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
inter-laboratory study ofASTM D5349 conducted in 2019. Six
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
laboratories tested five leather oils. Every “test result” repre-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sents an individual determination, and all participants reported
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5349 − 19
TABLE 1 Volatile Matter
Material Average Repeatability Standard Reproducibility Standard Repeatability Limi
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5349 − 95 (Reapproved 2012) D5349 − 19
Standard Test Method for
Determination of the Moisture and Volatile Content of
Sulfonated and Sulfonated, Sulfated Oils and Fatliquors by
Hot-PlateOven Method
This standard is issued under the fixed designation D5349; 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
1.1 This test method covers the determination of the percentage of water moisture and other compounds volatile at about 100°C
existing in a sample of sulfonated or sulfated oil, or both, by rapid evaporation. This test method is applicable only to sulfonated
and sulfated oils that do not contain the following: mineral acids, free sulfonic acids or free sulfuric acid esters, ammonia, acetic
acid or similar volatile acids, alkali hydroxides, carbonates, acetates or similar salts that may react with oleic acid at elevated
temperatures liberating volatile acids, or glycerin, diethylene glycol, xylene, or other compounds of similar volatility. This test
method was derived from Test Methods volatile material under conditions of the test. It is applicable to sulfonated, sulfated oils,
fats, oils, fatliquors, and softening compounds.D500, Sections 10 through 14.
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 safety, health, and healthenvironmental 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.
2. Referenced Documents
2.1 ASTM Standards:
D500 Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
3. Significance and Use
3.1 This test method is intended to determine the moisture and volatile content of sulfonated, sulfated oil, fats, oils, and
fatliquors used in the softening and stuffing of leather.fatliquors, and softening compounds.
4. Apparatus
4.1 Oven, The apparatus required consists of a glass-stoppered weighing flask, a glass beaker, and a suitable
thermometer.mechanical-convection draft capable of setting at 100 – 105 °C with a thermoregulatory system,
4.1.1 Weighing Flasks, any suitable glass-stoppered weighing flask of 10 to 15-mL capacity.
4.1.2 Beaker, Griffin low-form glass beaker with an approximate capacity of 150 mL and a diameter of about 5 cm.
4.1.3 Heat Source—The source of heat may be either an electric hot plate with or without asbestos paper or board cover, or an
open flame under a suitable asbestos board and a wire gauze (to spread the heat).
4.1.4 Thermometer, graduated from 90 to 150°C, about 3 in. in length, and substantially constructed.
This test method is under the jurisdiction of ASTM Committee D31 on Leather and is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis test method
was developed in cooperation with the American Leather Chemists Assn. (Method H 41–1957).
Current edition approved April 1, 2012Nov. 1, 2019. Published April 2012December 2019. Originally approved in 1993. Last previous edition approved in 20062012 as
D5349 – 95(2006).(2012). DOI: 10.1520/D5349-95R12.10.1520/D5349-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5349 − 19
4.2 Glass Beakers, 100 to 150 mL,
4.3 Desiccator, containing an efficient desiccant,
4.4 Analytical Scale, capable of reading at minimum 3 decimal places.
5. Reagents
5.1 Desiccating Agent—Any suitable desiccating agent may be used.
NOTE 1—Recent investigations seem to indicate that calcium chloride is unreliable as a laboratory desiccating agent.
5.2 Oleic Acid.
5. Procedure
5.1 Weigh a beaker that has been previously dried and cooled in a desiccator.
5.2 Weigh approximately 5Accurately weigh 0.5 g of oleic acid into the beaker and insert the thermometer. Heat the oleic acid
gradually, while stirring with the thermometer, until the temperature reaches 130°C. a well-mixed sample into the beaker. Place
the beaker in an oven at 105 to 100°C for 15 min, cool in a desiccator, and weigh. Repeat the heating over the hot plate and in
the oven until two successive weighings differ by less than 1.5 mg.the oven, with the temperature set to 105 – 100 °C.
5.3 Place about 6 g of the sample in the weighing flask and determine the weight a
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