ASTM D1617-90(2001)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D1617–90(Reapproved2001)
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 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.
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,
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,
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.
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, ethanol, or isopropyl
8.7 Reaction at Room Temperature—Allow the specimen to
alcohol.
stand together with the blanks at room temperature for the
7.6 Potassium Hydroxide, Standard Solution (1.0 N)—Dis-
length of time specified in Table 1.
solve 66 g of potassium hydroxide (KOH) pellets in water and
8.8 If a white precipitate develops in the specimen flasks or
dilute to 1 L with water (see Note 1).
bottles, add sufficient water to dissolve the salt. Add the same
7.7 Sulfuric Acid, Standard (0.5 N)—Prepare 0.5 N sulfuric
amount of water to each of the blanks.Add 6 to 8 drops of the
acid (H SO ) and standardize to four significant figures.
phenolphthalein indicator solution to each flask or bottle and
2 4
titrate with 0.5 N H SO just to the disappearance of the pink
2 4
8. Procedure
color. If more than 25 mL of isopropyl alcohol were added in
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 deter
...