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ASTM D1617-90(2001)

(Test Method)

Standard Test Method for Ester Value of Solvents and Thinners

Standard Test Method for Ester Value of Solvents and Thinners

SCOPE
1.1 This test method covers the determination of the ester value of solvents and thinners used in lacquers and other coatings.  
1.2 This standard does not purport to address all of the safety problems, 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. For a specific hazard statement, see Note 2.
1.3 For hazard information and guidance, see the supplier's Material Safety Data Sheet.

General Information

Status
Historical
Publication Date
31-Dec-2000
ICS
87.060.30 - Solvents
Technical Committee
D01 - Paint and Related Coatings, Materials, and Applications
Drafting Committee
D01.35 - Solvents, Plasticizers, and Chemical Intermediates
Current Stage
Ref Project

Relations

Replaces
ASTM D1617-90(1996) - Standard Test Method for Ester Value of Solvents and Thinners
Effective Date
01-Jan-2001
Replaced By
ASTM D1617-07 - Standard Test Method for Ester Value of Solvents and Thinners
Effective Date
01-Jun-2007
Referred By
ASTM D268-22 - Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
Effective Date
01-Jan-2001
Referred By
ASTM D2634-07(2021) - Standard Specification for Methyl Amyl Acetate (95 % Grade)
Effective Date
01-Jan-2001
Referred By
ASTM D608-05(2019) - Standard Specification for Dibutyl Phthalate
Effective Date
01-Jan-2001
Referred By
ASTM D5137-07(2021) - Standard Specification for Hexyl Acetate
Effective Date
01-Jan-2001

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ASTM D1617-90(2001) - Standard Test Method for Ester Value of Solvents and ThinnersASTM D1617-90(2001) - Standard Test Method for Ester Value of Solvents and Thinners
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ASTM D1617-90(2001) - Standard Test Method for Ester Value of Solvents and Thinners
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D1617–90(Reapproved2001)
Standard Test Method for
1
Ester Value of Solvents and Thinners
This standard is issued under the fixed designation D 1617; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 5. Interferences
1.1 This test method covers the determination of the ester 5.1 Organic chlorides, nitriles, and amides may be hydro-
value of solvents and thinners used in lacquers and other lyzed by the reagent, particularly at 98°C, and are a possible
coatings. source of error. Ketones interfere only slightly with this
1.2 This standard does not purport to address all of the procedure. Aldehydes consume some alkali, but the error
safety concerns, if any, associated with its use. It is the introduced by small amounts is negligible.
responsibility of the user of this standard to establish appro-
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Pressure Bottle, 200 to 350-mL capacity, made from
bility of regulatory limitations prior to use. For a specific
hazard statement, see Note 2. heat-resistant glass.
6.2 Container for Pressure Bottle—Asuitable safety device
1.3 For hazard information and guidance, see the supplier’s
Material Safety Data Sheet. to contain the pressure bottle. A metal container with hinged
top and perforated bottom, a strong synthetic fabric or canvas
2. Referenced Documents
bag, or a safety shield may be used.
2.1 ASTM Standards: 6.3 Ampoule, 1 or 2-mL capacity.
2
D 1193 Specification for Reagent Water 6.4 Weighing Pipet, Lunge or similar type.
6.5 Erlenmeyer Flasks, 250-mL glass-stoppered.
3. Summary of Test Method
6.6 Buret, 50-mL capacity.
3.1 The specimen is reacted with a measured excess of 6.7 Boiling Water Bath.
aqueous potassium hydroxide, using isopropanol as a mutual
7. Reagents
solvent if necessary. The amount of potassium hydroxide
consumed, which is determined by titrating the excess with 7.1 Purity of Reagents—Reagent grade chemicals shall be
standard mineral acid, is a measure of the ester originally used in all tests. Unless otherwise indicated, it is intended that
present. all reagents shall conform to the specifications of the Commit-
3.2 Since this determination is based on an acidimetric tee onAnalytical Reagents of theAmerican Chemical Society,
3
titration,asuitablecorrectionshouldbeappliediftheacidityof where such specifications are available. Other grades may be
the sample exceeds the limit of the specification. used provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
4. Significance and Use
accuracy of the determination.
4.1 This test method is useful in determining the assay of
7.2 Purity of Water—Unless otherwise indicated, references
solvents and thinners which are esters or solutions of esters of to water shall be understood to mean reagent water conforming
carboxylic acid. The ester value is calculated as percent ester.
to Type IV of Specification D 1193.
This test method has its greatest application where the solvent 7.3 Hydrochloric Acid, Standard (0.5 N)—Prepare 0.5 N
or thinner is not a pure ester. This test method may be used in
hydrochloric acid (HCl) and standardize to four significant
assessing compliance to specification. figures.
1 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, andApplications and is the direct responsibility of Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved May 25, 1990. Published July 1990. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 1617 – 58 T. Last previous edition D 1617 – 85. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
2
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D1617
NOTE 2—Precaution: Enclose each bottle securely in a suitable safety
7.4 Isopropyl Alcohol (99 %).
device to restrain fragments of glass should the pressure bottle rupture.
7.5 Phenolphthalein Indicator Solution—Dissolve1gof
phenolphthalein in 100 mL of methanol, et
...

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1.1 Although the pine chemical industry has been a continuing producer of chemical products for many centuries, the nature of the industry, its products, and its terminology have changed. In particular, the original practice of recovering pine chemical through the processing of the exudate from pine trees has been supplemented by their extraction by solvent products of the wood pulping industry. For many years the industry was known as the Naval Stores industry but that term has gradually been replaced by the more descriptive and meaningful term, Pine Chemicals Industry. Thus, this terminology contains some old terms now mostly of historic value, together with the terms of the modern pine chemical industry.2  
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5.1 In order to calculate the volatile organic content (VOC) of paints containing EPA exempt solvents, it is necessary to know the acetone, methyl acetate, or parachlorobenzotrifluoride content. This gas chromatographic test method provides a simple and direct way for measuring these solvents. Each analyte is measured with respect to a unique internal standard. For acetone, the internal standard used is acetone-d6, for methyl acetate it is methyl acetate-d3, and for PCBTF it is metachlorobenzotrifluoride (MCBTF). These unique analyte/internal standard pairs behave very nearly as single solvents with respect to evaporation rate and adsorption rate onto a coated silica fiber (SPME) but are separable on a gas chromatograph (GC) capillary column. The only critical analytical technique required for successfully performing this test method is the ability of an analyst to weigh a paint sample and internal standard, corresponding to the analyte of interest, into a septum capped vial. After weighing, solvent evaporation has no effect on the final value of the determination. Since whole paint is not injected into the gas chromatograph, the analytical system is never compromised.
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1.1 This test method is for the determination of acetone, methyl acetate, or parachlorobenzotrifluoride (PCBTF), or combination of any of the three, in paints and coatings, by solid phase microextraction (SPME) headspace sampling, and subsequent injection into a gas chromatograph. It has been evaluated for cellulose nitrate, acrylic, and urethane solvent-borne systems. The established working range of this test method is: acetone, 28 to 90 %; methyl acetate, 12 to 22 %; parachlorobenzotrifluoride, 10 to 17 %. There is no reason to believe that it will not work outside these ranges. A minor modification of this test method would make it suitable for the analysis of the same analytes in water-borne coatings (see Note 1).
Note 1: Water-borne paints are internally standardized and diluted with water followed by addition of solid sodium chloride.  
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.  
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