ASTM D5399-95
(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
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 The values stated in SI units are standard. The values given in parentheses are for information purposes only.
1.3 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: D 5399 – 95
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.2 final boiling point (FBP)—the point at which a cumu-
lative area count equal to 99.5 % of the total area under the
1.1 This test method covers the determination of the boiling
chromatogram is obtained.
point distribution of hydrocarbon solvents by capillary gas
chromatography. This test method is limited to samples having
4. Summary of Test Method
a minimum initial boiling point of 37°C (99°F), a maximum
4.1 The sample is introduced into a capillary gas chromato-
final boiling point of 285°C (545°F), and a boiling range of 5
graphic column that separates hydrocarbons in the order of
to 150°C (9 to 270°F) as measured by this test method.
increasing boiling point. The column temperature is raised at a
1.2 The values stated in SI units are standard. The values
reproducible rate and the area under the chromatogram is
given in parentheses are for information purposes only.
recorded throughout the run. Boiling points are assigned from
1.3 This standard does not purport to address all of the
a calibration curve obtained under the same conditions by
safety concerns, if any, associated with its use. It is the
running a known mixture of hydrocarbons covering the boiling
responsibility of the user of this standard to establish appro-
range expected in the sample. From these data, the boiling
priate safety and health practices and determine the applica-
point distribution of the sample is obtained.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents
5.1 The gas chromatographic determination of the boiling
2.1 ASTM Standards:
point distribution of hydrocarbon solvents can be used as an
D 86 Test Method for Distillation of Petroleum Products
alternative to conventional distillation methods for control of
D 850 Test Method for Distillation of Industrial Aromatic
solvents quality during manufacture, and specification testing.
Hydrocarbons and Related Materials
5.2 Boiling point distribution data can be used to monitor
D 1078 Test Method for Distillation Range of Volatile
the presence of product contaminants and compositional varia-
Organic Liquids
tion during the manufacture of hydrocarbon solvents.
D 2887 Test Method for Boiling Range Distribution of
5.3 Boiling point distribution data obtained by this test
Petroleum Fractions by Gas Chromatography
method are not equivalent to those obtained by Test Methods
D 2892 Test Method for Distillation of Crude Petroleum
4 D 86, D 850, D 1078, D 2887, D 2892, and D 3710.
(15-Theoretical Plate Column)
D 3710 Test Method for Boiling Range Distribution of
6. Apparatus
Gasoline and Gasoline Fractions by Gas Chromatography
6.1 Chromatograph—Any gas chromatograph that can
E 691 Practice for Conducting an Interlaboratory Study to
5 handle capillary column and has the following characteristics:
Determine the Precision of a Test Method
6.1.1 Detector—A flame ionization detector (FID) capable
3. Terminology of continuous operation at a temperature equivalent to the
maximum column temperature employed.
3.1 Definitions:
6.1.2 Column Temperature Programmer—The chromato-
3.1.1 initial boiling point (IBP)—the point at which a
graph must be capable of reproducible linear temperature
cumulative area count equal to 0.5 % of the total area under the
programming over a range sufficient to establish a retention
chromatogram is obtained.
time of 1 min for n-pentane and to allow elution of entire
1 sample within a reasonable time period.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
6.1.3 Sample Inlet System—The sample inlet system must
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.35 on Solvents, Plasticizers, and Chemical Intermediates.
be capable of operating continuously at a temperature up to the
Current edition approved Nov. 10, 1995. Published January 1996. Originally
maximum column temperature employed, or provide on-
published as D 5399 – 93. Last previous edition D 5399 – 93.
column injection.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 06.04.
NOTE 1—The use of cool, on-column injection using an automatic
Annual Book of ASTM Standards, Vol 05.02.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5399
injector or sampler has been shown to provide better precision relative to NOTE 3—Warning: Air and hydrogen are compressed gases under high
manual injection. pressure. Hydrogen is an extremely flammable gas.
6.1.4 Column—A 10 to 30 m by 0.53 mm inside diameter
8. Preparation of Apparatus
by 3-μm bonded methyl silicone, fused silica, or equivalent
8.1 Column Preparation—The column must be conditioned
column that elutes components in order of boiling points, and
at the maximum operating temperature to reduce baseline shifts
meets the resolution criteria specified in 8.2 must be used (see
due to bleeding of column substrate.
8.4).
6.1.5 Integrator—Means must be provided for determining NOTE 4—The column can be conditioned using the following proce-
dure:
the accumulated area under the chromatogram. This can be
done by means of a computer or electronic integrator. A timing
(a) Disconnect the column from the detector,
device can be used to record the area at set time intervals. The
(b) Purge the column at ambient temperature with carrier
same basis for measuring time must be used to determine the
gas for at least 30 min,
retention times in the calibration, and the sample. The maxi-
(c) With carrier gas flowing through the column, raise the
mum signal measured must be within the linear range of the
column temperature to the maximum operating temperature
measuring system used.
and maintain the temperature at this level for 12 to 16 h,
6.1.6 Flow Controller—The chromatograph must be
(d) Cool the column to ambient temperature,
equipped with a constant-flow device capable of maintaining
(e) Reconnect the column to the detector,
the carrier gas at a constant flow rate throughout the tempera-
(f) Set the detector temperature to at least 5°C higher than
ture program.
the maximum column temperature, and
6.1.7 Sample Introduction—A microsyringe is required for
(g) Program the column temperature up to the maximum
the introduction of the sample to the gas chromatograph (see
several times with normal carrier flow until a stable, flat
Note 1).
baseline is obtained.
8.2 Column Resolution—To test column resolution, inject
7. Reagents and Materials
the same volume of the calibration mixture as used during
7.1 Purity of Reagents—Reagent grade chemicals shall be
normal sample analysis and obtain the chromatogram by the
used in the preparation of the calibration mixture.
procedure described in Section 9. Using the n-dodecane (C )
7.2 Calibration Mixture—A synthetic blend of pure liquid
and n-tridecane (C ) peaks, and Fig. 1, calculate the resolu-
hydrocarbons of known boiling points. The components of the
tion, R, as calculated from the equation:
calibration mixture are listed in Table 1 and prepared by
R 5 2D/~Y 1 Y ! (1)
1 2
mixing equivolume quantities of the components. At least one
component in the mixture must have a boiling point equal to or
where:
lower than the initial boiling point of the sample, and one
D 5 time, s, between n-C and n-C apexes,
12 13
component must have a retention time greater than any
Y 5 peak width of n-C ,s,and
1 12
component in the sample.
Y 5 peak width of n-C ,s.
2 13
7.3 Carrier Gas, helium (high purity)—Additional purifica- The resolution, R, thus calculated must be between eight and
tion is recommended by the use of molecular sieves or other
twelve to be acceptable.
suitable agents to remove water, oxygen, and hydrocarbons.
8.3 Skewing of Peaks—Calculate the ratio A/B on peaks in
the calibration mixture as shown in Fig. 2. Call the width in
NOTE 2—Warning: Helium is a compressed gas under high pressure.
seconds of the part of the peak ahead of the time of the apex at
7.4 Detector Gases, air, hydrogen (high purity)—Additional
5 % of peak height A, and call B to equal the width in seconds
purification for air and hydrogen is recommended by the use of
of the part of the peak after the time of the apex at 5 % of peak
molecular sieves, activated carbons, or other suitable agents to
height. This ratio must not be less than 0.5 nor more than 2.0
remove water and organics.
8.4 Typical instrument parameters are as follows:
8.4.1 Column length equals 10 to 30 m,
TABLE 1 Calibration Mixture
8.4.2 Column material and size equal fused silica
...
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