ASTM D5008-97e1
(Test Method)Standard Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol By Gas Chromatography
Standard Test Method for Ethyl Methyl Pentanol Content and Purity Value of 2-Ethylhexanol By Gas Chromatography
SCOPE
1.1 This test method covers the determination of ethyl methyl pentanol content and purity value of 2-ethylhexanol.
1.2 Water and acid cannot be determined by this test method and must be determined in accordance with Test Methods D1613 and E203 and those results used to normalize the chromatographic data.
1.3 This standard does not purport to address all of the safety problems, 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. For a specific hazard statement, see 6.1.1.
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 5008 – 97
Standard Test Method for
Ethyl Methyl Pentanol Content and Purity Value of
2-Ethylhexanol By Gas Chromatography
This standard is issued under the fixed designation D 5008; 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.
e NOTE—Research report footnote was added editorially in September 2000.
1. Scope E 203, respectively, and the results are used to normalize the
values obtained by gas chromatography. An internal standard
1.1 This test method covers the determination of ethyl
procedure is also included as an alternative calculation tech-
methyl pentanol content and purity value of 2-ethylhexanol.
nique. With this procedure, all impurities are determined
1.2 Water and acid cannot be determined by this test method
relative to the internal standard and the purity value is
and must be determined in accordance with Test Methods
determined by subtracting the sum of the impurities, water, and
D 1613 and E 203 and those results used to normalize the
acid from 100.
chromatographic data.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 This test method is used to determine the purity value
responsibility of the user of this standard to establish appro-
and ethyl methyl pentanol content of 2-ethylhexanol.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For a specific
5. Apparatus
hazard statement, see Note 1.
5.1 Chromatograph—Any gas chromatograph designed or
1.4 For hazard information and guidance, see the supplier’s
modified for use with capillary or wide-bore capillary columns.
Material Safety Data Sheet.
The gas chromatograph should be equipped with a flame
2. Referenced Documents ionization detector or other detector capable of operating with
these columns and capable of detecting impurities at a level of
2.1 ASTM Standards:
0.01 weight % with a signal to noise ratio of at least 5:1.
D 1613 Test Method for Acidity in Volatile Solvents and
5.2 Column—Any column capable of resolving
Chemical Intermediates Used in Paint, Varnish, Lacquer,
2-ethylhexanol from ethyl methyl pentanol and other impuri-
and Related Products
3 ties that may be present. The peaks should be resolved
E 203 Test Method for Water Using Karl Fischer Titration
quantitatively within a practical elapsed time. Columns that
3. Summary of Test Method meet the requirement of this test method are listed in Table 1.
Other columns may be used, provided the user establishes that
3.1 A representative specimen is introduced onto a capillary
a column gives the required separations.
column. The 2-ethylhexanol is separated from the ethyl methyl
5.3 Specimen Introduction System—Any system capable of
pentanol and other impurities while the components are trans-
introducing a representative specimen into the gas chromato-
ported through the column by an inert carrier gas. The
graph may be used. A 1-μL syringe has been used successfully.
separated components are measured in the effluent by a flame
5.4 Computing Integrator—Any computing integrator ca-
ionization detector and the areas for the peaks are determined
pable of accurately determining the peak areas generated
by a suitable integration technique. The data are interpreted by
during this analysis.
applying component detector response factors to the peak
5.5 Analytical Balance—The internal standard technique
areas, and the relative concentrations are determined by relat-
requires an analytical balance capable of measuring 0.1 mg.
ing the individual peak responses to the total peak response.
Acidity and water are measured by Test Methods D 1613 and
6. Reagents and Materials
6.1 Carrier Gas—Helium, purified nitrogen, or hydrogen
This test method is under the jurisdiction of ASTM Committee D01 on Paint
are suitable. The carrier gas should have a minimum purity of
and Related Coatings, Materials, and Applications and is the direct responsibility of
99.95 mol %.
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
Current edition approved Dec. 10, 1997. Published August 1998. Originally
NOTE 1—Precaution: If hydrogen is used, take special safety precau-
{1
published as D 5008–89. Last previous edition D 5008–89 (l993) .
tions to ensure that the chromatographic system is free from leaks.
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5008
TABLE 1 Conditions and Retention Times
Case I Case II Case III
Column:
Material fused silica fused silica fused silica
Length, m 10 10 30
Inside diameter, mm 0.53 0.53 0.32
Liquid phase immobilized polydimethylsiloxane immobilized polydimethylsiloxane immobilized polyethylene glycol
Film thickness,μ m 5 5 0.25
Injection system: direct flash vaporization direct flash vaporization split
Injection specimen size,μ L 0.1 0.1 1
Temperatures:
Column temperature, °C (isothermal) 85 85 120
Injection port temperature, °C 200 200 220
Detector temperature,° C 200 200 220
Gases:
Carrier gas helium helium helium
Carrier gas flow rate, mL/min 4 4 0.6
Carrier gas velocity, cm/s 30 30 20
Hydrogen flow rate (detector), mL/ 30 30 30
min
Air flow rate (detector), mL/min 300 300 300
Make-up gas none none helium
Make-up flow rate (detector), mL/min none none 30
AA
Injection split ratio 50:1
Calculation technique: normalization internal standard normalization
Typical retention time, min:
A A
2-ethyl-2-butanol (internal standard) 2.24
Ethyl methyl pentanol 5.75 5.75 5.74
2-ethylhexanol 7.76 7.76 7.24
A
Not applicable.
6.2 Detector Gases—Hydrogen and air are used for the men of the calibration mixture.
flame ionization detector. If a make-up gas is used, helium or 7.2.2 If a computing integrator is used, follow the manufac-
nitrogen are suitable. turer’s instruction manual to calculate relative response factors.
6.3 Standards for Calibration and Identification—Standard If manual calculations are used, calculate relative response
samples for all identifiable components present are needed for factors for each component as follows.
identification by retention time, and for calibration for quanti-
R 5 A 3 B / C 3 D (1)
~ ! ~ !
tative measurements. In the case of the internal standard
where:
method, pure (99.0 + %) 2-ethyl-1-butanol is specified as the
R = response factor for component of interest,
internal standard. Any other internal standard may be used
A = peak area of reference component,
provided it is not present in the sample and doesn’t interfere
B = weight of component of interest in calibration mix-
with any other
...
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