ASTM D4017-96a

Standard Test Method for Water in Paints and Paint Materials by Karl Fischer Method

SCOPE
1.1 This test method is applicable to all paints and paint materials, including resins, monomers, and solvents, with the exception of aldehydes and certain active metals, metal oxides, and metal hydroxides. While the evaluation was limited to pigmented products containing amounts of water in the 30 to 70% range, there is reason to believe that higher and lower concentrations can be determined by this test method.
1.2  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. Specific hazard statements are given in Section 7.

General Information

• Status: Historical
• Publication Date: 09-Jan-2002
• ICS: 87.040 - Paints and varnishes
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaced By: ASTM D4017-02 - Standard Test Method for Water in Paints and Paint Materials by Karl Fischer Method
• Effective Date: 10-Jan-2002
• Referred By: ASTM D5530-22 - Standard Test Method for Total Moisture of Hazardous Waste Fuel by Karl Fischer Titrimetry
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7358-07(2018) - Standard Test Method for Water Content of Paints by Quantitative Calcium Hydride Reaction Test Kit
• Effective Date: 10-Jan-2002
• Referred By: ASTM D4143-16(2022) - Standard Guide for Testing Latex Vehicles
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6336-11(2021) - Standard Practice for Evaluation of Flushing Vehicles for Pigment Wetting Using a Vacuum Modified Sigma Blade Mixer
• Effective Date: 10-Jan-2002
• Referred By: ASTM D5325-03(2021) - Standard Test Method for Determination of Weight Percent Volatile Content of Water-Borne Aerosol Paints
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6886-18 - Standard Test Method for Determination of the Weight Percent Individual Volatile Organic Compounds in Waterborne Air-Dry Coatings by Gas Chromatography
• Effective Date: 10-Jan-2002
• Referred By: ASTM D3960-05(2018) - Standard Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings
• Effective Date: 10-Jan-2002
• Referred By: ASTM E1868-10(2021) - Standard Test Methods for Loss-On-Drying by Thermogravimetry
• Effective Date: 10-Jan-2002
• Referred By: ASTM D2827-19 - Standard Specification for Styrene Monomer
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7768-12(2018) - Standard Test Method for Speciated Organic Volatile Content of Waterborne Multi-Component Coatings by Gas Chromatography
• Effective Date: 10-Jan-2002
• Referred By: ASTM D6511/D6511M-18 - Standard Test Methods for Solvent Bearing Bituminous Compounds
• Effective Date: 10-Jan-2002
• Referred By: ASTM D5324-16(2022) - Standard Guide for Testing Water-Borne Architectural Coatings
• Effective Date: 10-Jan-2002
• Referred By: ASTM D7270-07(2021) - Standard Guide for Environmental and Performance Verification of Factory-Applied Liquid Coatings
• Effective Date: 10-Jan-2002
• Referred By: ASTM E203-23 - Standard Test Method for Water Using Volumetric Karl Fischer Titration
• Effective Date: 10-Jan-2002

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4017 – 96a
Standard Test Method for
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Water in Paints and Paint Materials by Karl Fischer Method
This standard is issued under the fixed designation D 4017; 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 sulfur dioxide, and an alcohol. In the reaction with water,
iodine is reduced to hydrogen iodide. Once all the water is
1.1 This test method is applicable to all paints and paint
consumed, the appearance of free iodine is detected electro-
materials, including resins, monomers, and solvents, with the
chemically and the titration is stopped. The following depicts
exception of aldehydes and certain active metals, metal oxides,
the chemistry that takes place:
and metal hydroxides. While the evaluation was limited to
ROH+SO +RN � (RNH)SO R
2 3
pigmented products containing amounts of water in the 30 to
H O+I + (RNH)SO R + 2RN → (RNH)SO R + 2(RNH)I
2 2 3 4
70 % range, there is reason to believe that higher and lower
3.2 In classical Karl Fischer titrations the base used is
concentrations can be determined by this test method.
pyridine, and the solvent either methanol or methoxy ethanol.
1.2 This standard does not purport to address all of the
In order to accelerate the reaction when pyridine is used,
safety concerns, if any, associated with its use. It is the
1-ethylpiperidine is used as a catalyst/buffer. The additional
responsibility of the user of this standard to establish appro-
buffer capacity is usually already built in to most nonpyridine
priate safety and health practices and determine the applica-
6
based reagents such as hydranal (see Hydranal Manual).
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 7.
4. Significance and Use
2. Referenced Documents 4.1 Control of water content is often important in control-
ling the performance of paint and paint ingredients, and it is
2.1 ASTM Standards:
2
critical in controlling volatile organic compound (VOC) con-
D 1193 Specification for Reagent Water
tent.
D 3960 Practice for Determining Volatile Organic Com-
3
4.2 Paint materials are often insoluble in common Karl
pound (VOC) Content of Paint and Related Coatings
Fischer solvents such as methanol. Pyridine has been found to
E 180 Practice for Determining the Precision of ASTM
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be a nearly universal solvent for these materials; however, the
Methods for Analysis and Testing of Industrial Chemicals
4
Karl Fischer reaction is too slow in that solvent at room
E 203 Test Method for Water Using Karl Fischer Reagent
temperature. To speed it up, 1-ethylpiperidine is added at 5 %
2.2 Other Standard:
as a buffer, or “catalyst”.
EPA Federal Reference Method 24—Determination of
4.3 For nonpyridine based reagents, a number of different
Volatile Matter Content, Density, Volume Solids, and
5
solvent systems are available to increase solubility and to
Weight Solids of Surface Coatings
minimize interferences from ketones and aldehydes.
3. Summary of Test Method
5. Apparatus
3.1 The material is dissolved in a suitable solvent, and
5.1 Karl Fischer Apparatus, manual or automatic, encom-
titrated directly with standardized Karl Fischer reagent, to an
passed by the description in Test Method E 203. Apparatus
electrometric end point. The sluggish reaction with water in
should be equipped with a 25-mL buret, Class A, or equivalent.
pyridine is accelerated with a chemical catalyst,
5.2 Syringe, 100-μL capacity, with needle.
1-ethylpiperidine.
5.3 Syringes, 1-mL and 10-mL capacity, without needle, but
3.1.1 Karl Fischer reagent is a mixture of iodine, amine,
equipped with caps.
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This test method is under the jurisdiction of ASTM Committee D01 on Paint 6. Reagents
and Related Coatings, Materials, and Applications and is the direct responsibility of
6.1 Purity of Reagents—Reagent grade chemicals shall be
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Current
used in all tests. Unless otherwise indicated, it is intended that
edition approved July 10,1996. Published September 1996. Originally published as
D 4017 – 81. Last previous edition D 4017 – 96.
2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 06.01.
4
Annual Book of ASTM Standards, Vol 15.05.
5 6
Available from the Superintendent of Documents, U.S. Government Printing Available from Hoechst Celanese Corporation, Hydranal Technical Center, U.S.
Office, Washington, DC 20402. Highway 43, Bucks, AL 36512.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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