ASTM D2804-22

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2804 − 22
Standard Test Method for
Purity of Methyl Ethyl Ketone By Gas Chromatography
This standard is issued under the fixed designation D2804; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope D1613 Test Method for Acidity in Volatile Solvents and
Chemical Intermediates Used in Paint, Varnish, Lacquer,
1.1 This test method covers the determination of the purity
and Related Products
of methyl ethyl ketone by gas chromatography. Impurities
D2593 Test Method for Butadiene Purity and Hydrocarbon
including water, acidity, and nonvolatile matter are measured
Impurities by Gas Chromatography
by appropriate ASTM procedures and the results are used to
D4626 Practice for Calculation of Gas Chromatographic
normalize the chromatographic value.
Response Factors
1.2 For purposes of determining conformance of an ob-
E29 Practice for Using Significant Digits in Test Data to
served value or a calculated value using this test method to
Determine Conformance with Specifications
relevant specifications, test result(s) shall be rounded off “to
E180 Practice for Determining the Precision of ASTM
the nearest unit” in the last right-hand digit used in expressing
Methods for Analysis and Testing of Industrial and Spe-
the specification limit, in accordance with the rounding-off
cialty Chemicals (Withdrawn 2009)
method of Practice E29.
3. Summary of Test Method
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
3.1 A representative specimen is introduced into a gas-
standard.
chromatographic column.The methyl ethyl ketone is separated
from other impurities such as hydrocarbons, alcohols, acetone,
1.4 For hazard information and guidance, see the supplier’s
di-sec-butyl ether, and ethyl acetate as the components are
Material Safety Data Sheet.
transported through the column by an inert carrier gas. The
1.5 This international standard was developed in accor-
separated components are measured in the effluent by a
dance with internationally recognized principles on standard-
detector and recorded as a chromatogram. The chromatogram
ization established in the Decision on Principles for the
is interpreted by applying component-attenuation and detector-
Development of International Standards, Guides and Recom-
response factors to the peak areas, and the relative concentra-
mendations issued by the World Trade Organization Technical
tion is determined by relating individual peak response to the
Barriers to Trade (TBT) Committee.
total peak response. Water, acidity, and nonvolatiles are mea-
2. Referenced Documents sured by the procedures listed in 3.2, and the results are used
2 to normalize the results obtained by gas chromatography.
2.1 ASTM Standards:
D1353 Test Method for Nonvolatile Matter in Volatile Sol- 3.2 The appropriate ASTM test methods are:
3.2.1 Water—Test Method D1364.
vents for Use in Paint, Varnish, Lacquer, and Related
Products 3.2.2 Acidity—Test Method D1613.
3.2.3 Nonvolatile Matter—Test Method D1353.
D1364 Test Method for Water in Volatile Solvents (Karl
Fischer Reagent Titration Method)
4. Significance and Use
1 4.1 This test method provides a measurement of commonly
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
found impurities in commercially available methyl ethyl ke-
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
tone. The measurement of these impurities and the results
Current edition approved Jan. 1, 2022. Published January 2022. Originally
thereof can individually or when totaled and subtracted from
approved in 1969. Last previous edition approved in 2012 as D2804 – 02 (2012)
100 (assay) be used for specification purposes.
which was withdrawn January 2021 and reinstated in January 2022. DOI: 10.1520/
D2804-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2804 − 22
5. Apparatus tivity detectors, and nitrogen, helium, or argon with ionization
detectors. The minimum purity of any carrier should be 99.95
5.1 Chromatograph—Any gas chromatograph having either
mol %.
a thermal-conductivity or flame ionization detector provided
6.1.1 Warning—If hydrogen is used, take special safety
the system has sufficient sensitivity and stability to obtain for
precautiontoensurethatthesystemisfreeofleaksandthatthe
0.01 weight % of impurity a recorder deflection of at least 2
effluent is vented properly.
mm at a signal-to-noise ratio of at least 5 to 1. The specimen
size to be used in judging the sensitivity must be such that the 6.2 Column Materials:
column is not overloaded. 6.2.1 Liquid Phase—The materials successfully used in
cooperative work as liquid phases are listed in Table 1 (see
5.2 Column—Anycolumncapableofresolvingmethylethyl
Note 1).
ketone from the impurities that may be present. Possible
6.2.2 Solid Support—The support for use in the packed
impurities are paraffins, acetone, methanol, ethanol, propanol,
column is usually (PTFE)-fluorocarbon, crushed firebrick, or
isopropanol, tert-butanol, sec-butanol, di-sec-butyl ether, and
diatomaceous earth. Table 1 lists conditions used successfully
ethyl acetate. The peaks should be resolved, quantitatively in
in cooperative work (see Note 1).
proportion to concentration, within a practical elapsed time.
Columns that meet the requirements of this test method are
NOTE 1—See research report for additional information, available from
ASTM International Headquarters. Request RR:D01-1107.
listedinTable1.Othercolumnsmaybeused,providedtheuser
establishes that a column gives the required separation and the
6.2.3 Tubing Material—Copper, stainless steel, nickel cop-
precision requirements of Section 13 are met.
per alloy, aluminum, and various plastic materials have been
found to be satisfactory for column tubing. The material must
5.3 Specimen Introduction System—Any specimen system
be nonreactive with the substrate, sample, and carrier gas.
capable of introducing a representative specimen into the
columnmaybeused.Systemsthathavebeenusedsuccessfully
6.3 Standards for Calibration and Identification—Standard
to introduce 1 to 10-µL of methyl ethyl ketone specimens
samples for all components present are needed for identifica-
include microlitre syringes, micropipets, and liquid sampling
tion by retention time, and for calibration for quantitative
valves.
measurements (Note 2).
5.4 Recorder—An electronic integrator or a recording po-
NOTE 2—Mixtures of components may be used, provided there is no
tentiometer with a full-scale deflection of 5 mV or less,
uncertainty as to the identity or concentration of compounds involved.
full-scale response time of 2 s or less, and sufficient sensitivity
7. Preparation of Apparatus
to meet the requirements of 5.1.
7.1 Column Preparation—The method used to prepare the
6. Reagents and Materials
column is not critical provided that the finished column
6.1 Carrier Gas, appropriate to the type of detector used. produces the required separation (Note 3). Partitioning liquids,
Helium or hydrogen may be employed with thermal conduc- supports, and loading levels used successfully in cooperative
TABLE 1 Columns and Conditions Used Successfully in Cooperative Work
Case I Case II Case III Case IV Case V Case VI
Column: packed packed packed packed packed capillary
Liquid phase polyethylene polyethylene polyethylene polyethylene polyethylene polytrifluoro-
glycol 1500 glycol 400 glycol 300 glycol 200 glycol 1500 propylsiloxa
...