ASTM D3125-97(2001)
(Test Method)Standard Test Method for Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid
Standard Test Method for Monomethyl Ether of Hydroquinone in Colorless Monomeric Acrylate Esters and Acrylic Acid
SCOPE
1.1 This test method covers the determination of monomethyl ether of hydroquinone (MEHQ) in colorless monomeric acrylate esters and acrylic acid. The test method is applicable to the determination of MEHQ in the concentration range from 0 to 1200 parts per million.
1.2 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
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. Specific precautionary statements are given in Section 8.
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Designation:D3125–97 (Reapproved 2001)
Standard Test Method for
Monomethyl Ether of Hydroquinone in Colorless Monomeric
Acrylate Esters and Acrylic Acid
This standard is issued under the fixed designation D 3125; 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 4. Significance and Use
1.1 This test method covers the determination of monom- 4.1 Acrylic acid and its esters are normally inhibited with
ethyl ether of hydroquinone (MEHQ) in colorless monomeric MEHQ only. This procedure presents a rapid and accurate
acrylate esters and acrylic acid. The test method is applicable method of determining the MEHQ content of fresh acrylic acid
to the determination of MEHQ in the concentration range from and acrylate esters in the absence of other inhibitors.
0 to 1200 parts per million. 4.2 MEHQ effectiveness may decline with age and this
1.2 For hazard information and guidance, see the supplier’s decline in effectiveness may not be indicated by this test
Material Safety Data Sheet. method.
1.3 This standard does not purport to address all of the
5. Interferences
safety concerns, if any, associated with its use. It is the
5.1 Hydroquinone (HQ), thiodiphenylamine, diphenylphe-
responsibility of whoever uses this standard to consult and
establish appropriate safety and health practices and deter- nylene-diamine and p-hydroxydiphenylamine interfere if
present.
mine the applicability of regulatory limitations prior to use.
Specific precautionary statements are given in Section 8.
6. Apparatus
2. Referenced Documents
6.1 Spectrophotometer, with borosilicate-glass cells for de-
2.1 ASTM Standards: termining absorbance at 420 nm.
6.2 Volumetric Flasks, 50 and 100-mL capacity.
D 1193 Specification for Reagent Water
E 180 Practice for Determining the Precision of ASTM 6.3 Measuring Pipets, 5 and 10-mL capacity.
Methods forAnalysis and Testing of Industrial Chemicals
7. Reagents
3. Summary of Test Method
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 As shown in the equation, MEHQ reacts with nitrous used.Unlessotherwiseindicated,itisintendedthatallreagents
shall conform to the specifications of the Committee on
acid (sodium nitrite in acidic media) to form the nitroso
derivative which equilibrates between two structures. Analytical Reagents of the American Chemical Society where
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent grade water
conforming to Type IV of Specification D 1193.
3.2 The yellow color of the nitroso compound is measured
7.3 Acetic Acid, glacial.
spectrophotometrically at a wavelength of 420 nm.
7.4 Monomethyl Ether of Hydroquinone (MEHQ) (4-
methoxyphenol).
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved June 10, 1997. Published September 1997. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 3125 – 72. Last previous edition D 3125 – 93. listed by the American Chemical Society, see Analar Standards for Laboratory
IUPAC-approved name is 4-methoxyphenol. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
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D3125
7.5 Sodium Nitrite Solution (2 %)—Dissolve2gof sodium curve, determine the micrograms of MEHQ corresponding to
nitrite (NaNO ) in water and dilute to 100 mL. the absorbance obtained.
11. Calculation
8. Hazards
11.1 Calculate the concentration of MEHQ in ppm as
8.1 Store samples of acrylic monomers in amber bottles or
follows:
protect from light by other means to aid in preventing
polymerization. Keep samples away from heat sources and
MEHQ, ppm 5 M/S (1)
chemicals that can cause free radical polymerization. Acrylic
where:
monomers can polymerize violently, evolving considerable
M = micrograms of MEHQ from calibration curve and
heat. Keep sample container size to a minimum. The inhibitor,
S = grams of specimen used in the test.
monomethyl/ester of hydroquinone, requir
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