ASTM D2804-02(2007)
(Test Method)Standard Test Method for Purity of Methyl Ethyl Ketone By Gas Chromatography
Standard Test Method for Purity of Methyl Ethyl Ketone By Gas Chromatography
SIGNIFICANCE AND USE
This test method provides a measurement of commonly found impurities in commercially available methyl ethyl ketone. The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be used for specification purposes.
SCOPE
1.1 This test method covers the determination of the purity of methyl ethyl ketone by gas chromatography. Impurities including water, acidity, and nonvolatile matter are measured by appropriate ASTM procedures and the results are used to normalize the chromatographic value.
1.2 For purposes of determining conformance of an observed value or a calculated value using this test method to relevant specifications, test result(s) shall be rounded off "to the nearest unit" in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2804 − 02 (Reapproved 2007)
StandardTest 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 Department of Defense.
1. Scope* E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1.1 This test method covers the determination of the purity
E180 Practice for Determining the Precision of ASTM
of methyl ethyl ketone by gas chromatography. Impurities
Methods for Analysis and Testing of Industrial and Spe-
including water, acidity, and nonvolatile matter are measured
cialty Chemicals (Withdrawn 2009)
by appropriate ASTM procedures and the results are used to
normalize the chromatographic value.
3. Summary of Test Method
1.2 For purposes of determining conformance of an ob-
3.1 A representative specimen is introduced into a gas-
served value or a calculated value using this test method to
chromatographic column.The methyl ethyl ketone is separated
relevant specifications, test result(s) shall be rounded off “to
from other impurities such as hydrocarbons, alcohols, acetone,
the nearest unit” in the last right-hand digit used in expressing
di- sec-butyl ether, and ethyl acetate as the components are
the specification limit, in accordance with the rounding-off
transported through the column by an inert carrier gas. The
method of Practice E29.
separated components are measured in the effluent by a
1.3 The values stated in SI units are to be regarded as
detector and recorded as a chromatogram. The chromatogram
standard. No other units of measurement are included in this
is interpreted by applying component-attenuation and detector-
standard.
response factors to the peak areas, and the relative concentra-
tion is determined by relating individual peak response to the
1.4 For hazard information and guidance, see the supplier’s
total peak response. Water, acidity, and nonvolatiles are mea-
Material Safety Data Sheet.
sured by the procedures listed in 3.2, and the results are used
2. Referenced Documents
to normalize the results obtained by gas chromatography.
2.1 ASTM Standards:
3.2 The appropriate ASTM test methods are:
D1353 Test Method for Nonvolatile Matter in Volatile Sol-
3.2.1 Water—Test Method D1364.
vents for Use in Paint, Varnish, Lacquer, and Related
3.2.2 Acidity—Test Method D1613.
Products
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
D1613 Test Method for Acidity in Volatile Solvents and
4.1 This test method provides a measurement of commonly
Chemical Intermediates Used in Paint, Varnish, Lacquer,
found impurities in commercially available methyl ethyl ke-
and Related Products
tone. The measurement of these impurities and the results
D2593 Test Method for Butadiene Purity and Hydrocarbon
thereof can individually or when totaled and subtracted from
Impurities by Gas Chromatography
100 (assay) be used for specification purposes.
D4626 Practice for Calculation of Gas Chromatographic
Response Factors
5. Apparatus
5.1 Chromatograph—Any gas chromatograph having either
This test method is under the jurisdiction of ASTM Committee D01 on Paint
a thermal-conductivity or flame ionization detector provided
and Related Coatings, Materials, andApplications and is the direct responsibility of
the system has sufficient sensitivity and stability to obtain for
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
0.01 weight % of impurity a recorder deflection of at least 2
Current edition approved June 1, 2007. Published June 2007. Originally
approved in 1969. Last previous edition approved in 2002 as D2804 – 02. DOI:
mm at a signal-to-noise ratio of at least 5 to 1. The specimen
10.1520/D2804-02R07.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2804 − 02 (Reapproved 2007)
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
impurities are paraffins, acetone, methanol, ethanol, propanol, 6.2.2 Solid Support—The support for use in the packed
isopropanol, tert-butanol, sec-butanol, di-sec-butyl ether, and column is usually (PTFE)-fluorocarbon, crushed firebrick, or
ethyl acetate. The peaks should be resolved, quantitatively in diatomaceous earth. Table 1 lists conditions used successfully
proportion to concentration, within a practical elapsed time. in cooperative work (see Note 1).
Columns that meet the requirements of this test method are
NOTE 1—See research report for additional information, available from
listedinTable1.Othercolumnsmaybeused,providedtheuser
ASTM International Headquarters. Request RR:D01-1107.
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
5.3 Specimen Introduction System—Any specimen system
found to be satisfactory for column tubing. The material must
capable of introducing a representative specimen into the
be nonreactive with the substrate, sample, and carrier gas.
columnmaybeused.Systemsthathavebeenusedsuccessfully
to introduce 1 to 10-µL of methyl ethyl ketone specimens
6.3 Standards for Calibration and Identification —Standard
include microlitre syringes, micropipets, and liquid sampling samples for all components present are needed for identifica-
valves.
tion by retention time, and for calibration for quantitative
measurements (Note 2).
5.4 Recorder—An electronic integrator or a recording po-
tentiometer with a full-scale deflection of 5 mV or less,
NOTE 2—Mixtures of components may be used, provided there is no
full-scale response time of 2 s or less, and sufficient sensitivity
uncertainty as to the identity or concentration of compounds involved.
to meet the requirements of 5.1.
7. Preparation of Apparatus
6. Reagents and Materials
7.1 Column Preparation—The method used to prepare the
6.1 Carrier Gas, appropriate to the type of detector used.
column is not critical provided that the finished column
Helium or hydrogen may be employed with thermal conduc-
produces the required separation (Note 3). Partitioning liquids,
tivity detectors, and nitrogen, helium, or argon with ionization
supports, and loading levels used successfully in cooperative
detectors. The minimum purity of any carrier should be 99.95
work are listed in Table 1. These may be obtained from most
mol %.
chromatography supply houses.
6.1.1 Warning—If hydrogen is used, take special safety
precautiontoensurethatthesystemisfreeofleaksandthatthe
NOTE 3—Asuitable method for column preparation is described in Test
Method D2593.
effluent is vented properly.
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 propylsiloxane
Liquid phase, weight % 10 28 20 20 20 1.2 µm film
Support type TFE resin Pink, diato- Pink, diato- White, diato- Pink, diato- none
maceous earth maceous earth maceous earth ma
...
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