ASTM D4415-91(1996)e1
(Test Method)Standard Test Methods for Determination of Dimer in Acrylic Acid
Standard Test Methods for Determination of Dimer in Acrylic Acid
SCOPE
1.1 Test Method A --Describes a chemical (titrametric) procedure for the determination of acrylic acid dimer in acrylic acid. This procedure may be applicable to other unsaturated organic acids.
1.2 Test Method B--Describes a gas chromatographic procedure for the determination of acrylic acid dimer in acrylic acid. Other impurities may also be determined simultaneously.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
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e1
Designation: D 4415 – 91 (Reapproved 1996)
Standard Test Methods for
Determination of Dimer in Acrylic Acid
This standard is issued under the fixed designation D 4415; 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.
e NOTE—Keywords were added editorially in May 1996.
1. Scope graph containing an appropriate capillary column for separa-
tion. The separated components are measured in the column
1.1 Test Method A—Describes a chemical (titrametric) pro-
effluent by a detector and recorded as a chromatogram. The
cedure for the determination of acrylic acid dimer in acrylic
peak areas are measured and the concentration of the compo-
acid. This procedure may be applicable to other unsaturated
nents of interest are calculated by reference to the internal
organic acids.
standard.
1.2 Test Method B—Describes a gas chromatographic pro-
cedure for the determination of acrylic acid dimer in acrylic
4. Significance and Use
acid. Other impurities may also be determined simultaneously.
4.1 These test methods provide a measurement of the dimer
1.3 This standard does not purport to address all of the
content of acrylic acid. The results of this measurement can be
safety concerns, if any, associated with its use. It is the
used for specification purposes but must be on an as-shipped
responsibility of the user of this standard to establish appro-
basis since the dimer content will vary with the age and the
priate safety and health practices and determine the applica-
storage temperature of the acrylic acid.
bility of regulatory limitations prior to use. For specific hazard
statements, see Section 8.
5. Interferences
5.1 Test Method A—If present, ester impurities present in
2. Referenced Documents
the acrylic acid will be determined as dimer.
2.1 ASTM Standards:
5.2 Test Method B—Impurities having the same or similar
D 268 Guide for Sampling and Testing Volatile Solvents
retention times as the acrylic acid on the column used may
and Chemical Intermediates for Use in Paint and Related
2 cause abnormally high results.
Coatings and Materials
D 1193 Specification for Reagent Water
6. Apparatus
D 4052 Test Method for Density and Relative Density of
4 6.1 Test Method A:
Liquids by Digital Density Meter
6.1.1 Pressure Bottle, 200 to 350-mL capacity, with lever-
E 200 Practice for Preparation, Standardization, and Stor-
5 type closure and made of heat-resistant glass.
age of Standard Solutions for Chemical Analysis
6.1.2 Container for Pressure Bottle— A suitable safety
device to contain the pressure bottle. A metal container with a
3. Summary of Test Methods
hinged top and perforated bottom, a strong synthetic fabric or
3.1 Test Method A—The acid specimen is neutralized and
canvas bag, or a safety shield may be used.
the dimer (Acrylic acid dimer, CH =CH-COO-CH -CH -
2 2 2
6.1.3 Open-Top Vial, 3 to 5-mL capacity, of such diameter to
COOH) determined by saponification and titration. Purity of
fit the pressure bottle.
the acid can also be determined by carrying out the first
6.1.4 Buret, 100-mL capacity.
neutralization, quantitatively, but this is not covered in this
6.1.5 Buret, 50-mL capacity, calibrated.
method.
6.1.6 Boiling Water Bath.
3.2 Test Method B—An internal standard, n-dodecane, is
6.2 Test Method B:
added to the sample and then introduced into a gas chromato-
6.2.1 Gas Chromatograph—Any gas chromatograph having
a flame ionization detector (FID) or any other detector,
This test method is under the jurisdiction of ASTM Committee D01 on Paint provided the system has sufficient sensitivity and stability to
and Related Coatings, Materials, and Applications and is the direct responsibility of
obtain, for a 0.01 % impurity in the specimen, a recorder
Subcommittee D01.35 on Solvents, Plasticizers and Chemical Intermediates.
Current edition approved Sept. 15, 1991. Published November 1991. Originally
published as D 4415 – 84. Last previous edition D 4415 – 89.
Annual Book of ASTM Standards, Vol 06.04.
3 6
Annual Book of ASTM Standards, Vol 11.01. Bottles of this type, equipped with lever-type closures and protective bags, can
Annual Book of ASTM Standards, Vol 05.02. be obtained from Preiser Scientific, 900 McCorkle Ave. SW, P.O. Box 551,
Annual Book of ASTM Standards, Vol 15.05. Charleston, WV 25322.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 4415
FIG. 1 Typical Chromatogram of Acrylic Acid
deflection of at least 20 mm at a signal to noise ratio of at least and sufficient sensitivity and stability to meet the requirements
5to1. of 6.2.1. A recording integrator or computerized data station
6.2.1.1 The chromatograph should be capable of tempera- may also be used.
ture programming. 6.2.5 Gas Purifiers—The use of a gas purifier, to remove
6.2.1.2 The injection port or system should be one suitable moisture and other contaminants from the carrier gas, and an
for the capillary column used. Split injection techniques should oxygen trap or oxygen removal system is strongly recom-
be used. mended to prolong column life.
6.2.2 Column—A 30 to 50-m long by 0.32-mm inside 6.2.6 Volumetric Flasks, 100-mL capacity.
diameter fused silica capillary column with a 0.2 to 0.3-μm film
7. Reagents and Materials
of a bonded, esterified polyethylene glycol phase. Any other
column, capable of providing the necessary separation and
7.1 Test Method A:
precision, may be used.
7.1.1 Purity of Reagents—Reagent grade chemicals shall be
6.2.3 Sample Introduction System—Any system capable of
used in all tests. Unless otherwise indicated, it is intended that
introducing a representative specimen into the column. Mi-
all reagents shall conform to the specifications of the commit-
crolitre syringes and autosampler systems have been used
tee on analytical reagents of the American Chemical Society,
successfully.
where such specifications are available. Other grades may be
6.2.4 Recorder—A recording potentiometer with a full-
scale deflection of 1 mV, full scale response time of1sor less,
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Phase is known under various names and trademarks, including, but not limited listed by the American Chemical Society, see Analar Standards for Laboratory
to, FFAP, AT-1000, SP-1000, SUPEROX-FA, NUKOL, DB-FFAP, 007-FFAP, and Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
BP-21. Columns with these phases or equivalents are available from many vendors and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
of gas chromatography supplies. MD.
D 4415
TABLE 1 Instrument Conditions Found Satisfactory for
used, provided it is first ascertained that the reagent is of
Measuring Dimer and Other Impurities in Acrylic Acid (see Fig. 1)
sufficiently high purity to permit its use without lessening the
Column 30 m by 0.32 mm ID fused silica capillary
accuracy of the determination.
Stationary phase Bonded, esterified polyethylene glycol
7.1.2 Purity of Water—Unless otherwise indicated, refer-
Column oven 100°C, held for 5 min, then programmed to 220°C at
ences to water shall be understood to mean reagent water
5°C/min and held until analysis is complete
Injection port Split injector; split ratio range 15:1 to 60:1; 250°C
conforming to Type IV of Specification D 1193.
Detector FID; 25 mL/min helium makeup gas; 300°C
7.1.3 Methanol (99 %).
Carrier gas Helium; flow rate 3.5 to 4.3 mL/min (72 to 90 cm/s)
7.1.4 Phenolphthalein Indicator (10-g/L solution)— Specimen size 1 μL
Dissolve1gof phenolphthalein in methanol and dilute to 100
mL. Titrate this solution with 0.1 N sodium hydroxide (NaOH)
solution to a faint pink coloration.
solution to the bottles and titrate to a pink end point with 0.5 N
7.1.5 Sodium Hydroxide, Standard Solution (0.5 N)—
NaOH solution.
Prepare and standardize in accordance with Practice E 200.
10.1.5 To the bottles in the procedure in 10.1.4, carefully
7.1.6 Sodium Hydroxide, Standard Solution (0.1 N)—
introduce 40 mL of 0.1 N NaOH solu
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