ASTM D3893-03(2009)
(Test Method)Standard Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by Gas Chromatography
Standard Test Method for Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by Gas Chromatography
SIGNIFICANCE AND USE
This procedure is designed to determine the purity of the two ketones, methyl isoamyl ketone and methyl amyl ketone, and to obtain the concentration of their various impurities, several of which are critical in the application of these solvents.
SCOPE
1.1 This test method covers the determination of the purity of methyl amyl ketone and methyl isoamyl ketone. In addition, the method determines total ketones and various impurities which may include acetone, isopropyl alcohol, methyl propyl ketone, methyl isobutyl ketone, methyl butyl ketone, methyl isobutyl carbinol, mesityl oxide, methyl isoamyl ketone, methyl butyl carbinol, methyl amyl ketone, and diisobutyl ketone.
1.2 Water and acid cannot be determined by this test method. They must be determined by other appropriate ASTM procedures, and the results used to normalize the chromatographic data.
1.3 For purposes of determining conformance of an observed 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 E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
1.6 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.
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Designation: D3893 − 03 (Reapproved 2009)
Standard Test Method for
Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by
Gas Chromatography
This standard is issued under the fixed designation D3893; 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.
1. Scope* 2. Referenced Documents
1.1 This test method covers the determination of the purity 2.1 ASTM Standards:
of methyl amyl ketone and methyl isoamyl ketone. In addition, D1364 Test Method for Water in Volatile Solvents (Karl
the method determines total ketones and various impurities Fischer Reagent Titration Method)
which may include acetone, isopropyl alcohol, methyl propyl D1613 Test Method for Acidity in Volatile Solvents and
ketone, methyl isobutyl ketone, methyl butyl ketone, methyl Chemical Intermediates Used in Paint, Varnish, Lacquer,
isobutyl carbinol, mesityl oxide, methyl isoamyl ketone, and Related Products
methyl butyl carbinol, methyl amyl ketone, and diisobutyl E29 Practice for Using Significant Digits in Test Data to
ketone. Determine Conformance with Specifications
E180 Practice for Determining the Precision of ASTM
1.2 Water and acid cannot be determined by this test
Methods for Analysis and Testing of Industrial and Spe-
method. They must be determined by other appropriateASTM
cialty Chemicals (Withdrawn 2009)
procedures, and the results used to normalize the chromato-
graphic data.
3. Summary of Method
1.3 For purposes of determining conformance of an ob-
3.1 A representative specimen is introduced onto a gas-
served or a calculated value using this test method to relevant
liquid partition column. The separated components are mea-
specifications, test result(s) shall be rounded “off to the nearest
sured in the effluent by a detector and recorded as a chromato-
unit” in the last right-hand digit used in expressing the
gram.Thechromatogramisinterpretedbyapplyingcomponent
specification limit, in accordance with the rounding-off method
attenuation and detector response factors to the peak areas and
of Practice E29.
relative concentrations are determined by relating the indi-
1.4 The values stated in SI units are to be regarded as
vidual peak responses to the total peak response. Water and
standard. No other units of measurement are included in this
acidity are measured by Test Methods D1364 and D1613,
standard. respectively, and the results are used to normalize the values
obtained by gas chromatography.
1.5 For hazard information and guidance, see the supplier’s
Material Safety Data Sheet.
4. Significance and Use
1.6 This standard does not purport to address all of the
4.1 Thisprocedureisdesignedtodeterminethepurityofthe
safety concerns, if any, associated with its use. It is the
two ketones, methyl isoamyl ketone and methyl amyl ketone,
responsibility of the user of this standard to establish appro-
and to obtain the concentration of their various impurities,
priate safety and health practices and determine the applica-
severalofwhicharecriticalintheapplicationofthesesolvents.
bility of regulatory limitations prior to use.
1 2
This test method is under the jurisdiction of ASTM Committee D01 on Paint For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Related Coatings, Materials, andApplications and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2009. Published January 2010. Originally the ASTM website.
approved in 1980. Last previous edition approved in 2003 as D3893 – 03. DOI: The last approved version of this historical standard is referenced on
10.1520/D3893-03R09. 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
D3893 − 03 (2009)
5. Apparatus about 40 mL of methylene chloride and add to the solid
support. Add additional methylene chloride to wet and cover
5.1 Chromatograph—Any gas-liquid chromatographic in-
the solid support. Evaporate the methylene chloride in a fume
strument having either a thermal conductivity or flame ioniza-
hood with gentle stirring and under a gentle stream of nitrogen.
tiondetectorandsufficientsensitivityandstabilitytoobtainfor
0.01 % impurity in the specimen a recorder deflection of at 7.2 Place 50 g of the solid support in a large evaporating
least 20 mm at a signal-to-noise ratio of at least 5 to 1. A dish. Dissolve 10 g of the phenyl methyl silicone in about 40
recording integrator or computer data processing system may mL of methylene chloride and add to the solid support. Add
also be used. additional methylene chloride to wet and cover the solid
5.1.1 The injection port of the chromatograph must have a support. Evaporate the methylene chloride in a fume hood with
volume of at least 1.2 mLto provide for proper vaporization of gentle stirring and under a gentle stream of nitrogen.
the specimen. The use of a smaller injection port or on-column
7.3 Add 12 g of the packing prepared in 7.1 and 12 g of the
injection causes peak broadening and tailing.
packing prepared in 7.2 to a small glass bottle or beaker and
5.2 Column—Four and one half m of 3.2-mm stainless steel mix well. The mixture is used as the column packing material.
tubing packed with 80 to 90-mesh acid-washed, base-washed,
7.4 Column Preparation—The method used to pack the
and silanized diatomaceous earth support coated with 10.0 %
column is not critical provided that the finished column
20 000 molecular weight polyethylene glycol and a 8.33 %
produces the required separation of all of the components to be
phenyl methyl (50:50) silicone.Acapillary column, capable of
determined.
the required separation may also be used.
8. Calibration and Standardization
5.3 Specimen Introduction System—Any system capable of
introducing a representative specimen onto the column. Micro-
8.1 Chromatograph—Install the column in the chromato-
liter syringes have been used successfully.
graph and adjust the operating parameters as directed in Table
1.Allow sufficient time for the instrument to reach equilibrium
5.4 Recorder—A recording potentiometer with a full-scale
as indicated by a stable recorder baseline.
deflection of 1 mV, full-scale response time of1sor less, and
sufficient sensitivity and stability to meet the requirements of
8.2 Determine the retention time of each component by
5.1.
injecting small amounts either separately or in known mix-
tures. The components should elute close to the typical
6. Reagents and Materials
retention times given in Table 1 and the chromatograms should
closely approximate those shown in Fig. 1 and Fig. 2.
6.1 Carrier Gas, appropriate to the type of detector used.
Helium or hydrogen may be employed with thermal conduc-
8.3 The area under each peak of the chromatogram is
tivity detectors and nitrogen, helium, or argon with flame
considered a quantitative measure of the corresponding com-
ionization detectors. The minimum purity of the carrier gas
pound. The relative area is proportional to concentration if the
used should be 99.95 mol %. An oxygen removal system is
detector responds equally to all the sample components. The
recommended for the carrier gas.
response to different components is generally significantly
6.1.1 Warning—If hydrogen is used, take special safety
different for both flame ionization and thermal conductivity
precautions to ensure that the system is free of leaks and that
detectors. This difference in detector response may be cor-
the effluent is vented properly.
rected by use of relative response factors obtained by injecting
6.2 Column Materials:
6.2.1 Liquid Phase—20 00
...
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:D3893–03 Designation:D3893–03(Reapproved2009)
Standard Test Method for
Purity of Methyl Amyl Ketone and Methyl Isoamyl Ketone by
Gas Chromatography
This standard is issued under the fixed designation D3893; 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.
1. Scope*
1.1 This test method covers the determination of the purity of methyl amyl ketone and methyl isoamyl ketone. In addition, the
method determines total ketones and various impurities which may include acetone, isopropyl alcohol, methyl propyl ketone,
methyl isobutyl ketone, methyl butyl ketone, methyl isobutyl carbinol, mesityl oxide, methyl isoamyl ketone, methyl butyl
carbinol, methyl amyl ketone, and diisobutyl ketone.
1.2Water1.2 Water and acid cannot be determined by this test method. They must be determined by other appropriate ASTM
procedures, and the results used to normalize the chromatographic data.
1.3 For purposes of determining conformance of an observed 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 E29.
1.4This 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.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 For hazard information and guidance, see the supplier’s Material Safety Data Sheet.
1.6 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.
2. Referenced Documents
2.1 ASTM Standards:
D1364 Test Method for Water in Volatile Solvents (Karl Fischer Reagent Titration Method)
D1613 Test Method for Acidity in Volatile Solvents and Chemical Intermediates Used in Paint, Varnish, Lacquer, and Related
Products
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
3. Summary of Method
3.1 Arepresentative specimen is introduced onto a gas-liquid partition column. 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
detector response factors to the peak areas and relative concentrations are determined by relating the individual peak responses to
the total peak response. Water and acidity are measured by Test Methods D1364 and D1613, respectively, and the results are used
to normalize the values obtained by gas chromatography.
4. Significance and Use
4.1 This procedure is designed to determine the purity of the two ketones, methyl isoamyl ketone and methyl amyl ketone, and
to obtain the concentration of their various impurities, several of which are critical in the application of these solvents.
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 July 10, 2003. Published August 2003. Originally approved in 1980. Last previous edition approved in 1999 as D3893-99. DOI:
10.1520/D3893-03.
Current edition approved Dec. 1, 2009. Published December 2009. Originally approved in 1980. Last previous edition approved in 2003 as D3893 - 03. DOI:
10.1520/D3893-03R09.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 06.04.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.
D3893–03 (2009)
5. Apparatus
5.1 Chromatograph—Any gas-liquid chromatographic instrument having either a thermal conductivity or flame ionization
detector and sufficient sensitivity and stability to obtain for 0.01 % impurity in the specimen a recorder deflection of at least 20
mm at a signal-to-noise ratio of at least 5 to 1. A recording integrator or computer data processing system may also be used.
5.1.1 The injection port of the chromatograph must have a volume of at least 1.2 mL to provide for proper vaporization of the
specimen. The use of a smaller injection port or on-column injection causes peak broadening and tailing.
5.2 Column—Four and one half m of 3.2-mm stainless steel tubing packed with 80 to 90-mesh acid-washed, base-washed, and
silanized diatomaceous earth support coated with 10.0 % 20 000 molecular weight polyethylene glycol and a 8.33 % phenyl
methyl (50:50) silicone. A capillary column, capable of the required separation may also be used.
5.3 Specimen Introduction System—Any system capable of introducing a representative specimen onto the column. Microliter
syringes have been used successfully.
5.4 Recorder—A recording potentiometer with a full-scale deflection of 1 mV, full-scale response time of1sor less, and
sufficient sensitivity and stability to meet the requirements of 5.1.
6. Reagents and Materials
6.1 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 should be
99.95 mol %. An oxygen removal system is recommended for the carrier gas.
6.1.1 Warning—If hydrogen is used, take special safety precautions to ensure that the system is free of leaks and that the
effluent is vented properly.
6.2 Column Materials:
6.2.1 Liquid Phase—20 000 molecular weight polyethylene glycol and phenyl methyl (50:50) silicone.
6.2.2 Solid Support—Acid-washed, base-washed, and silanized diatomaceous earth, 80 to 90 mesh.
6.2.3 Solvents—Methylene chloride, reagent grade.
6.2.4 Tubing Material—The stainless steel tubing must be of uniform internal diameter and must be clean. Wash the inside of
the tubing with methylene chloride, then water, and finally methyl alcohol and blow dry with nitrogen.
6.3 Standards for Calibration and Identification—Standardsamplesofallcomponentsareneededforestablishingidentification
by retention time and for calibration for quantitative measurements. In most cases, the pure compounds required for calibration
cannot be purchased and must be purified by distillation before use.
7. Preparation of Column
7.1 Place 50 g of the solid support, 80 to 90 mesh, in a large evaporating dish. Dissolve 12.5 g of the polyethylene glycol in
about 40 mL of methylene chloride and add to the solid support. Add additional methylene chloride to wet and cover the solid
support. Evaporate the methylene chloride in a fume hood with gentle stirring and under a gentle stream of nitrogen.
7.2 Place 50 g of the solid support in a large evaporating dish. Dissolve 10 g of the phenyl methyl silicone in about 40 mL of
methylene chloride and add to the solid support.Add additional methylene chloride to wet and cover the solid support. Evaporate
the methylene chloride in a fume hood with gentle stirring and under a gentle stream of nitrogen.
7.3 Add 12 g of the packing prepared in 7.1 and 12 g of the packing prepared i
...
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