ASTM D3329-03(2009)

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

SIGNIFICANCE AND USE
This test method provides a measurement of commonly found impurities in commercially available methyl isobutyl ketone. The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be used for specification acceptance.
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 The following applies to all specified limits in this standard; for purposes of determining conformance with this standard, an observed value or a calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the round-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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.
1.5 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: 30-Nov-2009
• 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

• Replaces: ASTM D3329-03 - Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography
• Effective Date: 01-Dec-2009
• 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: 01-Dec-2009
• Referred By: ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
• Effective Date: 01-Dec-2009
• Referred By: ASTM D1153-22 - Standard Specification for Methyl Isobutyl Ketone
• Effective Date: 01-Dec-2009

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: D3329 − 03 (Reapproved 2009)
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 Department of Defense.
1. Scope* and Related Products
D2593 Test Method for Butadiene Purity and Hydrocarbon
1.1 This test method covers the determination of the purity
Impurities by Gas Chromatography
of methyl isobutyl ketone (MIBK) by gas chromatography and
E29 Practice for Using Significant Digits in Test Data to
in addition provides a means for measuring certain impurities
Determine Conformance with Specifications
such as methyl isobutyl carbinol which are of interest. Impu-
E180 Practice for Determining the Precision of ASTM
rities such as water and acidity are measured by other appro-
Methods for Analysis and Testing of Industrial and Spe-
priate ASTM procedures and the results are used to normalize
cialty Chemicals (Withdrawn 2009)
the chromatographic value.
E260 Practice for Packed Column Gas Chromatography
1.2 The following applies to all specified limits in this
standard; for purposes of determining conformance with this
3. Summary of Test Method
standard, an observed value or a calculated value shall be
3.1 A representative specimen is introduced onto a gas-
rounded off “to the nearest unit” in the last right-hand digit
liquid partition column. Methyl isobutyl ketone is separated
used in expressing the specification limit, in accordance with
from impurities such as acetone, 2-propanol, pentanone, mesi-
the round-off method of Practice E29.
tyl oxide, methyl isobutyl carbinol, and several unidentified
1.3 The values stated in SI units are to be regarded as the
compounds as the components are transported through the
standard. The values given in parentheses are for information
column by an inert carrier gas. The separated components are
only.
measured in the effluent by a detector and recorded as a
chromatogram. The chromatogram is interpreted by applying
1.4 This standard does not purport to address all of the
component attenuation and detector response factors to the
safety concerns, if any, associated with its use. It is the
peak areas, and the relative concentrations are determined by
responsibility of the user of this standard to establish appro-
relating the individual peak responses to the total peak re-
priate safety and health practices and determine the applica-
sponse.WaterandacidityaremeasuredinaccordancewithTest
bility of regulatory limitations prior to use.
Methods D1364 and D1613 and the results are used to
1.5 For specific hazard information and guidance, see the
normalize the values obtained by gas chromatography.
supplier’s Material Safety Data Sheet for the materials listed in
this test method.
4. Significance and Use
2. Referenced Documents
4.1 This test method provides a measurement of commonly
found impurities in commercially available methyl isobutyl
2.1 ASTM Standards:
ketone. The measurement of these impurities and the results
D1364 Test Method for Water in Volatile Solvents (Karl
thereof can individually or when totaled and subtracted from
Fischer Reagent Titration Method)
100 (assay) be used for specification acceptance.
D1613 Test Method for Acidity in Volatile Solvents and
Chemical Intermediates Used in Paint, Varnish, Lacquer,
5. Apparatus
5.1 Chromatograph—Any gas liquid chromatographic in-
This test method is under the jurisdiction of ASTM Committee D01 on Paint
strument having either a thermal conductivity or flame ioniza-
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. tion detector provided the system has sufficient sensitivity and
Current edition approved Dec. 1, 2009. Published December 2009. Originally
stability to obtain for 0.01 % of impurity a recorder deflection
approved in 1974. Last previous edition approved in 2003 as D3329 – 03. DOI:
of at least 2 mm at a signal-to-noise ratio of at least 5 to 1. The
10.1520/D3329-03R09.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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
D3329 − 03 (2009)
specimen size used in judging the sensitivity must be such that 6.2.1 Liquid Phase—The materials successfully used in
the column is not overloaded, which would result in peak cooperative test work are listed in Table 1. (See Note 1.)
broadening, loss of resolution, shifting retention times and
NOTE 1—Suppliers of liquid phases and supports can be found in
formation of leading peaks.
Research Report RR:D01-1042, available from ASTM International
Headquarters.
5.2 Column—Any column capable of resolving methyl
isobutyl ketone from the impurities that may be present. 6.2.2 Solid Support—The materials and their mesh sizes
Possible impurities are hydrocarbons, acetone, 2-propanol, successfully used in cooperative work are shown in Table 1.
2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide iso- (See Note 1.)
mer, and methyl isobutyl carbinol. Columns that meet this 6.2.3 Tubing Material—Copper, stainless steel, and alumi-
requirementaredescribedinTable1.Othercolumns,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
thatacolumngivestherequiredseparationandthepeakshapes 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.
7. Preparation of Apparatus
5.4 Recorder—A recording potentiometer with a full-scale
7.1 Column Preparation—The method used to prepare the
deflection of 5 mV or less, full-scale response time of2sor
column is not critical provided that the finished column
less, and sufficient sensitivity and stability to meet the require-
produces the required separation (Note 2). Partitioning liquids,
ments of 5.1.
supports, and loading levels used successfully in cooperative
6. Reagents and Materials work are listed in Table 1.
6.1 Carrier Gas—Carrier gas appropriate to the type of
NOTE 2—Asuitable method for column preparation is described in Test
Method D2593. Additional useful information may be found in Practice
detector used. Helium or hydrogen may be employed with
E260.
thermal conductivity detectors and nitrogen, helium, or argon
with flame ionization detectors. The minimum purity of the 7.1.1 Prepacked columns conforming to requirements listed
carrier gas used should be 99.95 mol %. (Warning —If in Table 1 and in 5.2 and 6.2 may be obtained from any
hydrogen is used, take special safety precautions to ensure that reputable chromatography supply company.
the system is free from leaks and that the effluent is vented
7.2 Chromatograph—Install the column in the chromato-
properly.)
graph and establish the operating conditions required to give
6.2 Column Materials: the desired separation.Allow sufficient time for the instrument
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, eth
...

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3329–03 Designation:D3329–03(Reapproved2009)
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 Department of Defense.
1. 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3The following applies to all specified limits in this standard; for purposes of determining conformance with this standard, an
observed value or a calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the
specification limit, in accordance with the round-off method of Practice E29.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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.
1.5 For specific hazard information and guidance, see the supplier’s Material Safety Data Sheet for the materials listed in this
test method.
2. Referenced Documents
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
D1613 Test Method forAcidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related
Products
D2593 Test Method for Butadiene Purity and Hydrocarbon Impurities by Gas Chromatography
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E180 Practice for Determining the Precision ofASTM Methods forAnalysis and Testing of Industrial and Specialty Chemicals
E260 Practice for Packed Column Gas Chromatography
3. Summary of Test Method
3.1 A representative specimen is introduced onto a gas-liquid partition column. Methyl isobutyl ketone is separated from
impurities such as acetone, 2-propanol, pentanone, mesityl oxide, methyl isobutyl carbinol, and several unidentified compounds
as the components are transported through the column by an inert carrier gas. The separated components are measured in the
effluent by a detector and recorded as a chromatogram. The chromatogram is interpreted by applying component attenuation and
detectorresponsefactorstothepeakareas,andtherelativeconcentrationsaredeterminedbyrelatingtheindividualpeakresponses
to the total peak response. Water and acidity are measured in accordance with Test Methods D1364 and D1613 and the results are
used to normalize the values obtained by gas chromatography.
4. Significance and Use
4.1 This test method provides a measurement of commonly found impurities in commercially available methyl isobutyl ketone.
The measurement of these impurities and the results thereof can individually or when totaled and subtracted from 100 (assay) be
used for specification acceptance.
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved Dec. 1, 2003.2009. Published December 2003.2009. Originally approved in 1974. Last previous edition approved in 19992003 as
D3329–99.D3329 – 03. DOI: 10.1520/D3329-03R09.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
D3329–03 (2009)
5. Apparatus
5.1 Chromatograph—Any gas liquid chromatographic instrument having either a thermal conductivity or flame ionization
detector provided the system has sufficient sensitivity and stability to obtain for 0.01 % of impurity a recorder deflection of at least
2 mm at a signal-to-noise ratio of at least 5 to 1. The specimen size used in judging the sensitivity must be such that the column
is not overloaded, which would result in peak broadening, loss of resolution, shifting retention times and formation of leading
peaks.
5.2 Column—Any column capable of resolving methyl isobutyl ketone from the impurities that may be present. Possible
impurities are hydrocarbons, acetone, 2-propanol, 2-pentanone, 3-pentanone, mesityl oxide, mesityl oxide isomer, and methyl
isobutyl carbinol. Columns that meet this requirement are described in Table 1. Other columns, including capillary columns, may
be used, provided the user establishes that a column gives the required separation and the peak shapes are satisfactory for
measurement so that the precision requirements of Section 12 are met.
5.3 Specimen Introduction System—Any system capable of introducing a representative specimen onto the column. Microlitre
syringes have been used successfully.
5.4 Recorder—A recording potentiometer with a full-scale deflection of 5 mV or less, full-scale response time of2sor less,
and sufficient sensitivity and stability to meet the requirements of 5.1.
6. Reagents and Materials
6.1 Carrier Gas—Carrier gas appropriate to the type of detector used. Helium or hydrogen may be employed with thermal
conductivity detectors and nitrogen, helium, or argon with flame ionization detectors. The minimum purity of the carrier gas used
shouldbe99.95mol %.(Warning—Ifhydrogenisused,takespecialsafetyprecautionstoensurethatthesystemisfreefromleaks
and that the effluent is vented properly.)
6.2 Column Materials:
6.2.1 Liquid Phase—The materials successfully used in cooperative test work are listed in Table 1. (See Note 1.)
NOTE 1—Suppliers of liquid phases and supports can be found in Research Report D01-1042, available from ASTM International Headquarters.
6.2.2 Solid Support—The materials and their mesh sizes successfully used in cooperative work are shown inTable 1. (See Note
1.)
6.2.3 Tubing Material—Copper, stainless steel, and aluminum have been found satisfactory for column tubing.The tubing must
be nonreactive with the substrate, sample, and carrier gas and be of uniform internal diameter.
6.3 Standards for Calibration and Identification—Standard samples of all components present are needed for identification by
retention time and for calibration for quantitative measurements.
7. Preparation of Apparatus
7.1 Column Preparation—The method used to prepare the column is not critical provided that the finished column produces
the required separation (Note 2). Partitioning liquids, supports, and loading levels used successfully in cooperative work are listed
in Table 1.
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, 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
...