ASTM D5399-04(2009)
(Test Method)Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography
SIGNIFICANCE AND USE
The gas chromatographic determination of the boiling point distribution of hydrocarbon solvents can be used as an alternative to conventional distillation methods for control of solvents quality during manufacture, and specification testing.
Boiling point distribution data can be used to monitor the presence of product contaminants and compositional variation during the manufacture of hydrocarbon solvents.
Boiling point distribution data obtained by this test method are not equivalent to those obtained by Test Methods D 86, D 850, D 1078, D 2887, D 2892, and D 3710.
SCOPE
1.1 This test method covers the determination of the boiling point distribution of hydrocarbon solvents by capillary gas chromatography. This test method is limited to samples having a minimum initial boiling point of 37°C (99°F), a maximum final boiling point of 285°C (545°F), and a boiling range of 5 to 150°C (9 to 270°F) as measured by this test method.
1.2 For purposes of determining conformance of an observed or 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 E 29.
1.3 The values stated in SI units are standard. The values given in parentheses are for information purposes 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.
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Designation:D5399–04(Reapproved2009)
Standard Test Method for
Boiling Point Distribution of Hydrocarbon Solvents by Gas
Chromatography
This standard is issued under the fixed designation D5399; 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* D2887 Test Method for Boiling Range Distribution of
Petroleum Fractions by Gas Chromatography
1.1 This test method covers the determination of the boiling
D2892 Test Method for Distillation of Crude Petroleum
point distribution of hydrocarbon solvents by capillary gas
(15-Theoretical Plate Column)
chromatography. This test method is limited to samples having
D3710 Test Method for Boiling Range Distribution of
a minimum initial boiling point of 37°C (99°F), a maximum
Gasoline and Gasoline Fractions by Gas Chromatography
final boiling point of 285°C (545°F), and a boiling range of 5
E29 Practice for Using Significant Digits in Test Data to
to 150°C (9 to 270°F) as measured by this test method.
Determine Conformance with Specifications
1.2 For purposes of determining conformance of an ob-
E691 Practice for Conducting an Interlaboratory Study to
served or calculated value using this test method to relevant
Determine the Precision of a Test Method
specifications, test result(s) shall be rounded off “to the nearest
unit” in the last right-hand digit used in expressing the
3. Terminology
specification limit, in accordance with the rounding-off method
3.1 Definitions:
of Practice E29.
3.1.1 initial boiling point (IBP), n—the point at which a
1.3 The values stated in SI units are standard. The values
cumulativeareacountequalto0.5 %ofthetotalareaunderthe
given in parentheses are for information purposes only.
chromatogram is obtained.
1.4 This standard does not purport to address all of the
3.1.2 final boiling point (FBP), n—the point at which a
safety concerns, if any, associated with its use. It is the
cumulative area count equal to 99.5 % of the total area under
responsibility of the user of this standard to establish appro-
the chromatogram is obtained.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents 4.1 The sample is introduced into a capillary gas chromato-
2 graphic column that separates hydrocarbons in the order of
2.1 ASTM Standards:
increasing boiling point. The column temperature is raised at a
D86 Test Method for Distillation of Petroleum Products at
reproducible rate and the area under the chromatogram is
Atmospheric Pressure
recorded throughout the run. Boiling points are assigned from
D850 Test Method for Distillation of Industrial Aromatic
a calibration curve obtained under the same conditions by
Hydrocarbons and Related Materials
running a known mixture of hydrocarbons covering the boiling
D1078 Test Method for Distillation Range of Volatile Or-
range expected in the sample. From these data, the boiling
ganic Liquids
point distribution of the sample is obtained.
1 5. Significance and Use
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.1 The gas chromatographic determination of the boiling
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
point distribution of hydrocarbon solvents can be used as an
Current edition approved June 1, 2009. Published June 2009. Originally
alternative to conventional distillation methods for control of
approved in 1993. Last previous edition approved in 2004 as D5399 – 04. DOI:
10.1520/D5399-04R09.
solvents quality during manufacture, and specification testing.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 Boiling point distribution data can be used to monitor
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the presence of product contaminants and compositional varia-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tion during the manufacture of hydrocarbon solvents.
*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.
D5399–04 (2009)
TABLE 1 Calibration Mixture
5.3 Boiling point distribution data obtained by this test
method are not equivalent to those obtained by Test Methods Peak Number Compound Identification Normal Boiling Point, °C
D86, D850, D1078, D2887, D2892, and D3710.
1 n-Pentane 36.1
2 2-Methyl Pentane 60.0
3 n-Hexane 68.9
6. Apparatus
4 2,4-Dimethyl Pentane 80.6
5 n-Heptane 98.3
6.1 Chromatograph—Any gas chromatograph that can
6 Toluene 110.6
handle capillary column and has the following characteristics:
7 n-Octane 125.6
6.1.1 Detector—A flame ionization detector (FID) capable 8 p-Xylene 138.3
9 n-Propyl Benzene 159.4
of continuous operation at a temperature equivalent to the
10 n-Decane 173.9
maximum column temperature employed.
11 n-Butyl Benzene 183.3
12 n-Dodecane 216.1
6.1.2 Column Temperature Programmer—The chromato-
13 n-Tridecane 235.6
graph must be capable of reproducible linear temperature
14 n-Tetradecane 253.9
programming over a range sufficient to establish a retention
15 n-Pentadecane 270.6
16 n-Hexadecane 287.2
time of 1 min for n-pentane and to allow elution of entire
sample within a reasonable time period.
6.1.3 Sample Inlet System—The sample inlet system must
7.3.1 Warning: Helium is a compressed gas under high
be capable of operating continuously at a temperature up to the
maximum column temperature employed, or provide on- pressure.
7.4 Detector Gases, air, hydrogen (high purity)—Additional
column injection.
purification for air and hydrogen is recommended by the use of
NOTE 1—The use of cool, on-column injection using an automatic
molecular sieves, activated carbons, or other suitable agents to
injector or sampler has been shown to provide better precision relative to
remove water and organics.
manual injection.
7.4.1 Warning: Air and hydrogen are compressed gases
6.1.4 Column—A10to30mby0.53mminsidediameterby
under high pressure. Hydrogen is an extremely flammable gas.
3-µm bonded methyl silicone, fused silica, or equivalent
column that elutes components in order of boiling points, and 8. Preparation of Apparatus
meets the resolution criteria specified in 8.2 must be used (see
8.1 Column Preparation—The column must be conditioned
8.4).
atthemaximumoperatingtemperaturetoreducebaselineshifts
6.1.5 Integrator—Means must be provided for determining
due to bleeding of column substrate.
the accumulated area under the chromatogram. This can be
NOTE 2—The column can be conditioned using the following proce-
done by means of a computer or electronic integrator.Atiming
dure:
device can be used to record the area at set time intervals. The
(a) Disconnect the column from the detector,
same basis for measuring time must be used to determine the
(b) Purge the column at ambient temperature with carrier
retention times in the calibration, and the sample. The maxi-
gas for at least 30 min,
mum signal measured must be within the linear range of the
(c) With carrier gas flowing through the column, raise the
measuring system used.
column temperature to the maximum operating temperature
6.1.6 Flow Controller—The chromatograph must be
and maintain the temperature at this level for 12 to 16 h,
equipped with a constant-flow device capable of maintaining
(d) Cool the column to ambient temperature,
the carrier gas at a constant flow rate throughout the tempera-
(e) Reconnect the column to the detector,
ture program.
(f) Set the detector temperature to at least 5°C higher than
6.1.7 Sample Introduction—A microsyringe is required for
the maximum column temperature, and
the introduction of the sample to the gas chromatograph (see
(g) Program the column temperature up to the maximum
Note 1).
several times with normal carrier flow until a stable, flat
baseline is obtained.
7. Reagents and Materials
8.2 Column Resolution—To test column resolution, inject
7.1 Purity of Reagents—Reagent grade chemicals shall be
the same volume of the calibration mixture as used during
used in the preparation of the calibration mixture.
normal sample analysis and obtain the chromatogram by the
7.2 Calibration Mixture—A synthetic blend of pure liquid
procedure described in Section 9. Using the n-dodecane (C )
hydrocarbons of known boiling points. The components of the
and n-tridecane (C ) peaks, and Fig. 1, calculate the resolu-
calibration mixture are listed in Table 1 and prepared by
tion, R, as calculated from the equation:
mixing equivolume quantities of the components. At least one
R 5 2D/~Y 1 Y ! (1)
1 2
component in the mixture must have a boiling point equal to or
lower than the initial boiling point of the sample, and one
where:
component must have a retention time greater than any
D = time, s, between n-C and n-C apexes,
12 13
component in the sample.
Y = peak width of n-C ,s,and
1 12
7.3 Carrier Gas, helium (high purity)—Additional purifica- Y = peak width of n-C ,s.
2 13
tion is recommended by the use of molecular sieves or other The resolution, R, thus calculated must be between eight and
suitable agents to remove water, oxygen, and hydrocarbons. twelve to be acceptable.
---------------
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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:D5399–95(Reapproved2000) Designation:D5399–04(Reapproved2009)
Standard Test Method for
Boiling Point Distribution of Hydrocarbon Solvents by Gas
Chromatography
This standard is issued under the fixed designation D 5399; 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 boiling point distribution of hydrocarbon solvents by capillary gas
chromatography. This test method is limited to samples having a minimum initial boiling point of 37°C (99°F), a maximum final
boiling point of 285°C (545°F), and a boiling range of 5 to 150°C (9 to 270°F) as measured by this test method.
1.2The values stated in SI units are standard. The values given in parentheses are for information purposes only.
1.3
1.2 For purposes of determining conformance of an observed or 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 E 29.
1.3 The values stated in SI units are standard. The values given in parentheses are for information purposes 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.
2. Referenced Documents
2.1 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products at Atmospheric Pressure
D 850 Test Method for Distillation of Industrial Aromatic Hydrocarbons and Related Materials
D 1078 Test Method for Distillation Range of Volatile Organic Liquids
D 2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
D 2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)
D 3710 Test Method for Boiling Range Distribution of Gasoline and Gasoline Fractions by Gas Chromatography
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions:
3.1.1 initial boiling point (IBP)initial boiling point (IBP), n—the point at which a cumulative area count equal to 0.5 % of the
total area under the chromatogram is obtained.
3.1.2 final boiling point (FBP)final boiling point (FBP), n—the point at which a cumulative area count equal to 99.5 % of the
total area under the chromatogram is obtained.
4. Summary of Test Method
4.1 Thesampleisintroducedintoacapillarygaschromatographiccolumnthatseparateshydrocarbonsintheorderofincreasing
boiling point.The column temperature is raised at a reproducible rate and the area under the chromatogram is recorded throughout
the run. Boiling points are assigned from a calibration curve obtained under the same conditions by running a known mixture of
hydrocarbons covering the boiling range expected in the sample. From these data, the boiling point distribution of the sample is
obtained.
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 Nov. 10, 1995. Published January 1996. Originally published as D5399–93. Last previous edition D5399–93.
Current edition approved June 1, 2009. Published June 2009. Originally approved in 1993. Last previous edition approved in 2004 as D 5399 – 04.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 05.01.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.
D5399–04 (2009)
5. Significance and Use
5.1 The gas chromatographic determination of the boiling point distribution of hydrocarbon solvents can be used as an
alternative to conventional distillation methods for control of solvents quality during manufacture, and specification testing.
5.2 Boiling point distribution data can be used to monitor the presence of product contaminants and compositional variation
during the manufacture of hydrocarbon solvents.
5.3Boiling point distribution data obtained by this test method are not equivalent to those obtained byTest Methods D86, D850,
D1078, D2887, D2892, and D3710
5.3 Boiling point distribution data obtained by this test method are not equivalent to those obtained by Test Methods D 86,
D 850, D 1078, D 2887, D 2892, and D 3710.
6. Apparatus
6.1 Chromatograph—Any gas chromatograph that can handle capillary column and has the following characteristics:
6.1.1 Detector—Aflame ionization detector (FID) capable of continuous operation at a temperature equivalent to the maximum
column temperature employed.
6.1.2 Column Temperature Programmer— The chromatograph must be capable of reproducible linear temperature program-
ming over a range sufficient to establish a retention time of 1 min for n-pentane and to allow elution of entire sample within a
reasonable time period.
6.1.3 Sample Inlet System—The sample inlet system must be capable of operating continuously at a temperature up to the
maximum column temperature employed, or provide on-column injection.
NOTE 1—The use of cool, on-column injection using an automatic injector or sampler has been shown to provide better precision relative to manual
injection.
6.1.4 Column—A10 to 30 m by 0.53 mm inside diameter by 3-µm bonded methyl silicone, fused silica, or equivalent column
that elutes components in order of boiling points, and meets the resolution criteria specified in 8.2 must be used (see 8.4).
6.1.5 Integrator—Means must be provided for determining the accumulated area under the chromatogram. This can be done
by means of a computer or electronic integrator. A timing device can be used to record the area at set time intervals. The same
basis for measuring time must be used to determine the retention times in the calibration, and the sample. The maximum signal
measured must be within the linear range of the measuring system used.
6.1.6 Flow Controller—The chromatograph must be equipped with a constant-flow device capable of maintaining the carrier
gas at a constant flow rate throughout the temperature program.
6.1.7 Sample Introduction—A microsyringe is required for the introduction of the sample to the gas chromatograph (see Note
1).
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in the preparation of the calibration mixture.
7.2 Calibration Mixture—A synthetic blend of pure liquid hydrocarbons of known boiling points. The components of the
calibration mixture are listed inTable 1 and prepared by mixing equivolume quantities of the components.At least one component
in the mixture must have a boiling point equal to or lower than the initial boiling point of the sample, and one component must
have a retention time greater than any component in the sample.
7.3 Carrier Gas, helium (high purity)—Additionalpurificationisrecommendedbytheuseofmolecularsievesorothersuitable
agents to remove water, oxygen, and hydrocarbons.
7.3.1 Warning: Helium is a compressed gas under high pressure.
TABLE 1 Calibration Mixture
Peak Number Compound Identification Normal Boiling Point, °C
1 n-Pentane 36.1
2 2-Methyl Pentane 60.0
3 n-Hexane 68.9
4 2,4-Dimethyl Pentane 80.6
5 n-Heptane 98.3
6 Toluene 110.6
7 n-Octane 125.6
8 p-Xylene 138.3
9 n-Propyl Benzene 159.4
10 n-Decane 173.9
11 n-Butyl Benzene 183.3
12 n-Dodecane 216.1
13 n-Tridecane 235.6
14 n-Tetradecane 253.9
15 n-Pentadecane 270.6
16 n-Hexadecane 287.2
D5399–04 (2009)
7.4 Detector Gases, air, hydrogen (high purity)—Additional purification for air and hydrogen is recommended by the use of
molecular sieves, activated carbons, or other suitable agents to remove water and organics.
7.4.1 Warning: Air and hydrogen are compressed gases under high pressure. Hydrogen is an extremely flammable gas.
8. Preparation of Apparatus
8.1 Column Preparation—Thecolumnmustbeconditionedatthemaximumoperatingtemperaturetoreducebaselineshiftsdue
to bleeding of column substrate.
NOTE 2—The column can be conditioned using the following procedure:
(a) Disconnect the column from the detector,
(b) Purge the column at ambient temperature with carrier gas for at least 30 min,
(c) With carrier gas flowing through the column, raise the column temperature to the maximum operating temperature and
maintain the temperature at this level for 12 to 16 h,
(d) Cool the column to ambient temperature,
(e) Reconnect the column to the detector,
(f) Set the detector temperature to at least 5°C higher than the maximum column temperature, and
(g) Program the column temperature up to the maximum several times with normal carrier flow until a stable, flat baseline is
obtained.
8.2 Column Resolution—To test column resolution, inject the same volume of the calibration mixture as used during normal
sample analysis and obtain the chromatogram by the procedure described in Section 9. Using the n-dodecane (C ) and n-t
...
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