ASTM D2074-07(2019)

Standard Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method

ABSTRACT
These alternative test methods cover the indicator procedure for determining the total, primary, secondary, and tertiary amine values of fatty amines. These procedures are not applicable to fatty amidoamines and fatty diamines. The apparatus includes Erlenmeyer flasks and magnetic stirrer. Reagent grade chemicals shall be used in all tests and includes the following: water, bromphenol blue indicator solution, bromcresol green indicator solution, chloroform, hydrochloric acid standard solution, isopropyl alcohol, phenyl isothiocyanate, and salicylaldehyde. The procedure of determining the total amine values are detailed and the formula of calculating the total amine values is given.
SCOPE
1.1 These alternative test methods cover the indicator procedure for determining the total, primary, secondary, and tertiary amine values of fatty amines. These procedures are not applicable to fatty amidoamines and fatty diamines.  
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: 30-Sep-2019
• ICS: 71.080.30 - Organic nitrogen compounds
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.33 - Polymers and Resins

Relations

• Replaces: ASTM D2074-07(2013) - Standard Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty Amines by Alternative Indicator Method
• Effective Date: 01-Oct-2019
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999

Overview

ASTM D2074-07(2019) provides standardized alternative indicator methods for determining total, primary, secondary, and tertiary amine values of fatty amines. Developed by ASTM International and the American Oil Chemists’ Society, this standard is vital for professionals analyzing fatty amines in various industries, using precise chemical titration techniques. The test methods outlined are not applicable to fatty amidoamines or fatty diamines, ensuring specificity and reliability in results.

The standard employs indicator-based titration procedures and specifies the required apparatus, such as Erlenmeyer flasks and magnetic stirrers, as well as the purity and type of chemicals used, ensuring consistency and reproducibility across laboratories.

Key Topics

• Types of Amine Values: The standard defines and details methods for measuring total, primary, secondary, and tertiary amine values, essential metrics in chemical analysis and quality assurance for fatty amines.
• Sample Preparation: Guidance is provided on proper sample handling, including melting, weighing, and mixing for precise analytical results.
• Apparatus and Reagents: Specifies the use of standard laboratory equipment and high-purity reagents such as reagent water, bromphenol blue indicator solution, bromcresol green indicator solution, chloroform, hydrochloric acid standard solutions, isopropyl alcohol, phenyl isothiocyanate, and salicylaldehyde.
• Indicator Titration Procedures: Step-by-step protocols for titrations using appropriate indicators and standard solutions, ensuring accurate endpoint detection.
• Calculation Methods: Explicit formulas are provided for calculating amine values based on titrant volume, normality, and specimen weight. These calculations are integral for determining the composition and quality of fatty amine samples.
• Precision and Bias: While detailed precision and bias data are yet to be established, the long-standing use of these methods attests to their practical efficacy and reliability.

Applications

ASTM D2074-07(2019) is widely applied in:

• Quality Control: Used by manufacturers of surfactants, lubricants, and chemical intermediates for verifying the amine content in fatty amines before further processing or market release.
• Research and Development: Supports the development of new chemical products involving fatty amines by providing accurate amine value analysis.
• Compliance and Specification Testing: Ensures that fatty amines meet both internal and external quality specifications, a requirement for both suppliers and end-users in regulated industries.
• Analytical Laboratories: Forms a part of routine analyses where the chemical composition of fatty amines must be precisely controlled and documented.

Related Standards

Refer to these key documents for additional guidelines and procedures:

• ASTM D1193: Specification for Reagent Water - outlines the required purity for water used in laboratory testing.
• ASTM Standards on Analytical Reagents: Provide specifications for reagent grade chemicals, ensuring quality and consistency in analytical work.
• Guidelines from the American Oil Chemists’ Society: Offer additional context and methods for lipid and fatty amine analysis.

For organizations concerned with chemical analysis, quality control, and standard compliance related to fatty amines, ASTM D2074-07(2019) is an essential reference, assuring reliable and standardized test outcomes in laboratory and industrial settings.

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: D2074 − 07 (Reapproved 2019)
Standard Test Methods for
Total, Primary, Secondary, and Tertiary Amine Values of
Fatty Amines by Alternative Indicator Method
This standard is issued under the fixed designation D2074; 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.
These test methods were prepared jointly by ASTM and the American Oil Chemists’ Society.
1. Scope 3.1.3 tertiary amine value, n—the number of milligrams of
potassium hydroxide (KOH) equivalent to the tertiary amine
1.1 These alternative test methods cover the indicator pro-
basicity in1gof sample.
cedure for determining the total, primary, secondary, and
3.1.4 total amine value, n—the number of milligrams of
tertiary amine values of fatty amines. These procedures are not
potassium hydroxide (KOH) equivalent to the basicity in1gof
applicable to fatty amidoamines and fatty diamines.
sample.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Apparatus
standard.
4.1 Erlenmeyer Flasks, wide-mouth, alkali-resistant,
1.3 This standard does not purport to address all of the
borosilicate-glass, 250-mL capacity.
safety concerns, if any, associated with its use. It is the
4.2 Magnetic Stirrer, with an inert plastic-coated stirring
responsibility of the user of this standard to establish appro-
bar.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
5. Reagents
1.4 This international standard was developed in accor-
5.1 Purity of Reagents—Reagent grade chemicals shall be
dance with internationally recognized principles on standard-
used in all tests. Unless otherwise indicated, it is intended that
ization established in the Decision on Principles for the
all reagents shall conform to the specifications of the Commit-
Development of International Standards, Guides and Recom-
tee onAnalytical Reagents of theAmerican Chemical Society,
mendations issued by the World Trade Organization Technical
where such specifications are available. Other grades may be
Barriers to Trade (TBT) Committee.
used, provided it is first ascertained that the reagent is of
2. Referenced Documents
sufficiently high purity to permit its use without lessening the
2.1 ASTM Standards: accuracy of the determination.
D1193 Specification for Reagent Water
5.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
3. Terminology
to Type II of Specification D1193.
3.1 Definitions:
5.3 Bromphenol Blue Indicator Solution—Dissolve 0.2 g of
3.1.1 primary amine value, n—the number of milligrams of
bromphenol blue in 100 mL of methanol, ethanol, or isopro-
potassium hydroxide (KOH) equivalent to the primary amine
panol.
basicity in1gof sample.
5.4 Bromcresol Green Indicator Solution—Dissolve 0.1 g of
3.1.2 secondary amine value, n—the number of milligrams
bromcresol green sodium salt in 100 mL of water.
of potassium hydroxide (KOH) equivalent to the secondary
amine basicity in1gof sample.
5.5 Chloroform (CHCl ).
5.6 Hydrochloric Acid, Standard Solution (0.1 N)—Add 17
These test methods are under the jurisdiction of ASTM Committee D01 on
mLofconcentratedhydrochloricacid(HCl,spgr1.19)to1000
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.33 on Polymers and Resins.
Current edition approved Oct. 1, 2019. Published October 2019. Originally
approved in 1962. Last previous edition approved in 2013 as D2074 – 07(2013). ACS Reagent Chemicals, Specifications and Procedures for Reagents and
DOI: 10.1520/D2074-07R19. Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2074 − 07 (2019)
mL of isopropyl alcohol in a 2-L volumetric flask. Make up to point (Note 1 and Note 2). The yellow may fade back to green
volume after cooling to room temperature. Standardize with upon standing, but this may be disregarded if the yellow color
sodium carbonate using bromcresol green as the indicator. is bright and the addition of another millilitre of 0.2 N HCl
does not change th
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