ASTM D3329-03(2023)

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: D3329 − 03 (Reapproved 2023)
Standard Test Method for
1,2
Purity of Methyl Isobutyl Ketone by Gas Chromatography
This standard is issued under the fixed designation D3329; 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 2. Referenced Documents
1.1 This test method covers the determination of the purity 2.1 ASTM Standards:
of methyl isobutyl ketone (MIBK) by gas chromatography and D1364 Test Method for Water in Volatile Solvents (Karl
in addition provides a means for measuring certain impurities Fischer Reagent Titration Method)
such as methyl isobutyl carbinol which are of interest. Impu- D1613 Test Method for Acidity in Volatile Solvents and
rities such as water and acidity are measured by other appro- Chemical Intermediates Used in Paint, Varnish, Lacquer,
priate ASTM procedures and the results are used to normalize and Related Products
the chromatographic value. D2593 Test Method for Butadiene Purity and Hydrocarbon
Impurities by Gas Chromatography
1.2 The following applies to all specified limits in this
E29 Practice for Using Significant Digits in Test Data to
standard; for purposes of determining conformance with this
Determine Conformance with Specifications
standard, an observed value or a calculated value shall be
E180 Practice for Determining the Precision of ASTM
rounded off “to the nearest unit” in the last right-hand digit
Methods for Analysis and Testing of Industrial and Spe-
used in expressing the specification limit, in accordance with
cialty Chemicals (Withdrawn 2009)
the round-off method of Practice E29.
E260 Practice for Packed Column Gas Chromatography
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
3. Summary of Test Method
only.
3.1 A representative specimen is introduced onto a gas-
1.4 This standard does not purport to address all of the
liquid partition column. Methyl isobutyl ketone is separated
safety concerns, if any, associated with its use. It is the
from impurities such as acetone, 2-propanol, pentanone, mesi-
responsibility of the user of this standard to establish appro-
tyl oxide, methyl isobutyl carbinol, and several unidentified
priate safety, health, and environmental practices and deter-
compounds as the components are transported through the
mine the applicability of regulatory limitations prior to use.
column by an inert carrier gas. The separated components are
1.5 For specific hazard information and guidance, see the
measured in the effluent by a detector and recorded as a
supplier’s Safety Data Sheet for the materials listed in this test
chromatogram. The chromatogram is interpreted by applying
method.
component attenuation and detector response factors to the
1.6 This international standard was developed in accor-
peak areas, and the relative concentrations are determined by
dance with internationally recognized principles on standard-
relating the individual peak responses to the total peak re-
ization established in the Decision on Principles for the
sponse. Water and acidity are measured in accordance with Test
Development of International Standards, Guides and Recom-
Methods D1364 and D1613 and the results are used to
mendations issued by the World Trade Organization Technical
normalize the values obtained by gas chromatography.
Barriers to Trade (TBT) Committee.
4. Significance and Use
4.1 This test method provides a measurement of commonly
This test method is under the jurisdiction of ASTM Committee D01 on Paint
found impurities in commercially available methyl isobutyl
and Related Coatings, Materials, and Applications and is the direct responsibility of
ketone. The measurement of these impurities and the results
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
thereof can individually or when totaled and subtracted from
Current edition approved July 1, 2023. Published August 2023. Originally
100 (assay) be used for specification acceptance.
approved in 1974. Last previous edition approved in 2017 as D3329 – 03 (2017).
DOI: 10.1520/D3329-03R23.
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
D3329 − 03 (2023)
5. Apparatus carrier gas used should be 99.95 mol %. (Warning—If hydro-
gen is used, take special safety precautions to ensure that the
5.1 Chromatograph—Any gas liquid chromatographic in-
system is free from leaks and that the effluent is vented
strument having either a thermal conductivity or flame ioniza-
properly.)
tion detector provided the system has sufficient sensitivity and
stability to obtain for 0.01 % of impurity a recorder deflection
6.2 Column Materials:
of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The
6.2.1 Liquid Phase—The materials successfully used in
specimen size used in judging the sensitivity must be such that
cooperative test work are listed in Table 1. (See Note 1.)
the column is not overloaded, which would result in peak
broadening, loss of resolution, shifting retention times and
NOTE 1—Suppliers of liquid phases and supports can be found in
Research Report RR:D01-1042, available from ASTM International
formation of leading peaks.
Headquarters.
5.2 Column—Any column capable of resolving methyl
6.2.2 Solid Support—The materials and their mesh sizes
isobutyl ketone from the impurities that may be present.
successfully used in cooperative work are shown in Table 1.
Possible impurities are hydrocarbons, acetone, 2-propanol,
2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide (See Note 1.)
isomer, and methyl isobutyl carbinol. Columns that meet this
6.2.3 Tubing Material—Copper, stainless steel, and alumi-
requirement are described in Table 1. Other columns, including
num have been found satisfactory for column tubing. The
capillary columns, may be used, provided the user establishes
tubing must be nonreactive with the substrate, sample, and
that a column gives the required separation and the peak shapes
carrier gas and be of uniform internal diameter.
are satisfactory for measurement so that the precision require-
6.3 Standards for Calibration and Identification—Standard
ments of Section 12 are met.
samples of all components present are needed for identification
5.3 Specimen Introduction System—Any system capable of
by retention time and for calibration for quantitative measure-
introducing a representative specimen onto the column. Mi-
ments.
crolitre syringes have been used successfully.
5.4 Recorder—A recording potentiometer with a full-scale
7. Preparation of Apparatus
deflection of 5 mV or less, full-scale response time of 2 s or
7.1 Column Preparation—The method used to prepare the
less, and sufficient sensitivity and stability to meet the require-
column is not critical provided that the finished column
ments of 5.1.
produces the required separation (Note 2). Partitioning liquids,
6. Reagents and Materials supports, and loading levels used successfully in cooperative
work are listed in Table 1.
6.1 Carrier Gas—Carrier gas appropriate to the type of
detector used. Helium or hydrogen may be employed with
NOTE 2—A suitable method for column preparation is described in Test
thermal conductivity detectors and nitrogen, helium, or argon
Method D2593. Additional useful information may be found in Practice
with flame ionization detectors. The minimum purity of the E260.
TABLE 1 Columns and Conditions Used Successfully in Cooperative Work (See Note 1)
Case I Case II Case III Case IV Case V Case VI
Column:
Liquid phase polyethylene glycol, polyethylene glycol, ethylene oxide/ polyethylene glycol, polyethy
...