ASTM D3329-99

Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography

SCOPE
1.1 This test method covers the determination of the purity of methyl isobutyl ketone (MIBK) by gas chromatography and in addition provides a means for measuring certain impurities such as methyl isobutyl carbinol which are of interest. Impurities such as water and acidity are measured by other appropriate ASTM procedures and the results are used to normalize the chromatographic value.  
1.2 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.  
1.3 For specific hazard information and guidance, see the supplier's Material Safety Data Sheet for the materials listed in this test method.

General Information

• Status: Historical
• Publication Date: 09-Jun-1999
• ICS: 71.080.80 - Aldehydes and ketones
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.35 - Solvents, Plasticizers, and Chemical Intermediates

Relations

• Replaced By: ASTM D3329-03 - Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography
• Effective Date: 01-Dec-2003
• Referred By: ASTM D268-22 - Standard Guide for Sampling and Testing Volatile Solvents and Chemical Intermediates for Use in Paint and Related Coatings and Material
• Effective Date: 10-Jun-1999
• Referred By: ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
• Effective Date: 10-Jun-1999
• Referred By: ASTM D1153-22 - Standard Specification for Methyl Isobutyl Ketone
• Effective Date: 10-Jun-1999

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 3329 – 99
Standard Test Method for
1,2
Purity of Methyl Isobutyl Ketone by Gas Chromatography
This standard is issued under the fixed designation D 3329; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope * from impurities such as acetone, 2-propanol, pentanone, mesi-
tyl oxide, methyl isobutyl carbinol, and several unidentified
1.1 This test method covers the determination of the purity
compounds as the components are transported through the
of methyl isobutyl ketone (MIBK) by gas chromatography and
column by an inert carrier gas. The separated components are
in addition provides a means for measuring certain impurities
measured in the effluent by a detector and recorded as a
such as methyl isobutyl carbinol which are of interest. Impu-
chromatogram. The chromatogram is interpreted by applying
rities such as water and acidity are measured by other appro-
component attenuation and detector response factors to the
priate ASTM procedures and the results are used to normalize
peak areas, and the relative concentrations are determined by
the chromatographic value.
relating the individual peak responses to the total peak re-
1.2 This standard does not purport to address all of the
sponse. Water and acidity are measured in accordance with Test
safety concerns, if any, associated with its use. It is the
Methods D 1364 and D 1613 and the results are used to
responsibility of the user of this standard to establish appro-
normalize the values obtained by gas chromatography.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Significance and Use
1.3 For specific hazard information and guidance, see the
4.1 This test method provides a measurement of commonly
supplier’s Material Safety Data Sheet for the materials listed in
found impurities in commercially available methyl isobutyl
this test method.
ketone. The measurement of these impurities and the results
2. Referenced Documents thereof can individually or when totaled and subtracted from
100 (assay) be used for specification acceptance.
2.1 ASTM Standards:
D 1364 Test Method for Water in Volatile Solvents (Karl
5. Apparatus
Fischer Reagent Titration Method)
5.1 Chromatograph—Any gas liquid chromatographic in-
D 1613 Test Method for Acidity in Volatile Solvents and
strument having either a thermal conductivity or flame ioniza-
Chemical Intermediates Used in Paint, Varnish, Lacquer,
3 tion detector provided the system has sufficient sensitivity and
and Related Products
stability to obtain for 0.01 % of impurity a recorder deflection
D 2593 Test Method for Butadiene Purity and Hydrocarbon
4 of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The
Impurities by Gas Chromatography
specimen size used in judging the sensitivity must be such that
E 180 Practice for Determining the Precision of ASTM
5 the column is not overloaded, which would result in peak
Methods for Analysis and Testing of Industrial Chemicals
6 broadening, loss of resolution, shifting retention times and
E 260 Practice for Packed Column Gas Chromatography
formation of leading peaks.
3. Summary of Test Method 5.2 Column—Any column capable of resolving methyl
isobutyl ketone from the impurities that may be present.
3.1 A representative specimen is introduced onto a gas-
Possible impurities are hydrocarbons, acetone, 2-propanol,
liquid partition column. Methyl isobutyl ketone is separated
2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide iso-
mer, and methyl isobutyl carbinol. Columns that meet this
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
requirement are described in Table 1. Other columns, including
and Related Coatings, Materials, and Applications and is the direct responsibility of
capillary columns, may be used, provided the user establishes
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
that a column gives the required separation and the peak shapes
Current edition approved June 10, 1999. Published August 1999. Originally
are satisfactory for measurement so that the precision require-
published as D 3329 – 74. Last previous edition D 3329 – 94a.
IUPAC approved name is 4-methyl-2-pentanone.
ments of Section 12 are met.
Annual Book of ASTM Standards, Vol 06.04.
5.3 Specimen Introduction System—Any system capable of
Annual Book of ASTM Standards, Vol 05.01.
5 introducing a representative specimen onto the column. Mi-
Annual Book of ASTM Standards, Vol 15.05.
Annual Book of ASTM Standards, Vol 14.02. crolitre syringes have been used successfully.
*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.
D 3329
TABLE 1 Columns and Conditions Used Successfully in Cooperative Work (See Note 2)
Case I Case II Case III Case IV Case V Case VI
Column:
Liquid phase polyethylene glycol, polyethylene glycol, ethylene oxide/ polyethylene glycol, polyethylene glycol, polyethylene glycol
MW 1450 MW 540 propylene oxide MW 20M MW 3350
copolymer
Liquid phase, weight % 15 20 20 25 25 1.2 μm film
Support diatomaceous earth, diatomaceous earth diatomaceous earth, diatomaceous earth diatomaceous earth capillary
acid washed acid washed
Support mesh size 60 to 80 60 to 80 45 to 60 60 to 80 60 to 80 N/A
Length, ft (m) 20 (6.1) 18 (5.5) 20 (6.1) 10 (3.0) 12 (3.7) 33 (10)
1 1 1 1 1
Diameter, in. (mm) ⁄8 (3.2) ⁄4 (6.4) ⁄4(6.4) ⁄8 (3.2) ⁄4 (6.4) 0.021 (0.53)
Temperature, °C 90 100 160 75 to 200 145 40 to 180 at
programmed at 5°/min
4°/min
Carrier gas: helium helium helium helium helium helium
Flow rate, mL/min 30 50 60 20 80 5
Typical retention time, min:
Methyl isobutyl ketone 9.3 27.2 8.1 11.2 7.7 1.84
Relative retention time,
MIBK 5 1.00:
Acetone 0.42 0.39 0.52 0.42 0.39 0.36
2-propanol 0.66 0.57 0.65 0.56 0.59
2- and 3-pentanone 0.85 0.82 0.78 . . 0.79
Methyl isobutyl ketone 1.00 1.00 1.00 1.00 1.00 1.00
a-Mesityl oxide 1.45 1.41 1.27 . . .
b-Mesityl oxide 1.89 1.85 1.63 1.24 1.52 .
Methyl isobutyl carbinol 2.11 2.07 1.48 1.42 1.95 2.24
5.4 Recorder—A recording potentiometer with a full-scale produces the required separation (Note 3). Partitioning liquids,
deflection of 5 mV or less, full-scale response time of2sor supports, and loading levels used successfully in cooperative
less, and sufficient sensitivity and stability to meet the require- work are listed in Table 1.
ments of 5.1.
NOTE 3—A suitable method for column preparation is described in Test
Method D 2593. Additional useful information may be found in Practice
6. Reagents and Materials
E 260.
6.1 Carrier Gas—Carrier gas appropriate to the type of
7.1.1 Prepacked columns conforming to requirements listed
detector used. Helium or hydrogen may be employed with
in Table 1 and in 5.2 and 6.2 may be obtained from any
thermal conductivity detectors and nitrogen, helium, or argon
reputable chromatography supply company.
with flame ionization detectors. The minimum purity of the
7.2 Chromatograph—Install the column in the chromato-
carrier gas used should be 99.95 mol %.
graph and establish the operating conditions required to give
NOTE 1—Precaution: If hydrogen is used, take special safety precau-
the desired separation. Allow sufficient time for the instrument
tions to ensure that the system is free from leaks and that the effluent is
to reach equilibrium as indicated by a stable recorder baseline.
vented properly.
Control the detector temperature so that it is consta
...