ASTM D1617-90(1996)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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 1617 – 90 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
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 lyzed by the reagent, particularly at 98°C, and are a possible
source of error. Ketones interfere only slightly with this
1.1 This test method covers the determination of the ester
procedure. Aldehydes consume some alkali, but the error
value of solvents and thinners used in lacquers and other
introduced by small amounts is negligible.
coatings.
1.2 This standard does not purport to address all of the
6. Apparatus
safety concerns, if any, associated with its use. It is the
6.1 Pressure Bottle, 200 to 350-mL capacity, made from
responsibility of the user of this standard to establish appro-
heat-resistant glass.
priate safety and health practices and determine the applica-
6.2 Container for Pressure Bottle—A suitable safety device
bility of regulatory limitations prior to use. For a specific
to contain the pressure bottle. A metal container with hinged
hazard statement, see Note 2.
top and perforated bottom, a strong synthetic fabric or canvas
1.3 For hazard information and guidance, see the supplier’s
bag, or a safety shield may be used.
Material Safety Data Sheet.
6.3 Ampoule, 1 or 2-mL capacity.
2. Referenced Documents 6.4 Weighing Pipet, Lunge or similar type.
6.5 Erlenmeyer Flasks, 250-mL glass-stoppered.
2.1 ASTM Standards:
6.6 Buret, 50-mL capacity.
D 1193 Specification for Reagent Water
6.7 Boiling Water Bath.
3. Summary of Test Method
7. Reagents
3.1 The specimen is reacted with a measured excess of
7.1 Purity of Reagents—Reagent grade chemicals shall be
aqueous potassium hydroxide, using isopropanol as a mutual
used in all tests. Unless otherwise indicated, it is intended that
solvent if necessary. The amount of potassium hydroxide
all reagents shall conform to the specifications of the Commit-
consumed, which is determined by titrating the excess with
tee on Analytical Reagents of the American Chemical Society,
standard mineral acid, is a measure of the ester originally
where such specifications are available. Other grades may be
present.
used provided it is first ascertained that the reagent is of
3.2 Since this determination is based on an acidimetric
sufficiently high purity to permit its use without lessening the
titration, a suitable correction should be applied if the acidity of
accuracy of the determination.
the sample exceeds the limit of the specification.
7.2 Purity of Water—Unless otherwise indicated, references
4. Significance and Use to water shall be understood to mean reagent water conforming
to Type IV of Specification D 1193.
4.1 This test method is useful in determining the assay of
7.3 Hydrochloric Acid, Standard (0.5 N)—Prepare 0.5 N
solvents and thinners which are esters or solutions of esters of
hydrochloric acid (HCl) and standardize to four significant
carboxylic acid. The ester value is calculated as percent ester.
figures.
This test method has its greatest application where the solvent
7.4 Isopropyl Alcohol (99 %).
or thinner is not a pure ester. This test method may be used in
7.5 Phenolphthalein Indicator Solution—Dissolve1gof
assessing compliance to specification.
phenolphthalein in 100 mL of methanol, ethanol, or isopropyl
5. Interferences
alcohol.
5.1 Organic chlorides, nitriles, and amides may be hydro-
Bottles of this type, equipped with lever-type closures, can be obtained from
Preiser Scientific, PO Box 1330, 94 Oliver St., St. Albans, WV 25177.
1 4
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, and Applications 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. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
D 1617
7.6 Potassium Hydroxide, Standard Solution (1.0 N)— 8.8 If a white precipitate develops in the specimen flasks or
Dissolve 66 g of potassium hydroxide (KOH) pellets in water bottles, add sufficient water to dissolve the salt. Add the same
and dilute to 1 L with water (see Note 1). amount of water to each of the blanks. Add 6 to 8 drops of the
7.7 Sulfuric Acid, Standard (0.5 N)—Prepare 0.5 N sulfuric phenolphthalein indicator solution to each flask or bottle and
acid (H SO ) and standardize to four significant figures. titrate with 0.5 N H SO just to the disappearance of the pink
2 4 2 4
color. If more than 25 mL of isopropyl alcohol were added in
8. Procedure
accordance with 8.3, titrate with 0.5 N HCl.
8.1 Prepare a sufficient number of 250-mL, glass-stoppered
8.9 Measure the temperature of the acid titrant. If the
Erlenmeyer flasks to make all blank and test determinations in
temperature of the reagent at the time the ester determination is
duplicate. Use heat-resistant pres
...