ASTM D7213-15(2019)
(Test Method)Standard Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100 °C to 615 °C by Gas Chromatography
Standard Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100 °C to 615 °C by Gas Chromatography
SIGNIFICANCE AND USE
5.1 The boiling range distribution of light and medium petroleum distillate fractions provides an insight into the composition of feed stocks and products related to petroleum refining process, This gas chromatographic determination of boiling range can be used to replace conventional distillation methods for control of refining operations. This test method can be used for product specification testing with the mutual agreement of interested parties.
5.2 This test method extends the scope of boiling range determination by gas chromatography to include light and medium petroleum distillate fractions beyond the scope of Test Method D2887 (538 °C) and below Test Method D6352 (700 °C).
5.3 Boiling range distributions obtained by this test method are theoretically equivalent to those obtained by true boiling point (TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillation such as those obtained with Test Method D86 or D1160.
SCOPE
1.1 This test method covers the determination of the boiling range distribution of petroleum products. This test method is applicable to petroleum distillates having an initial boiling point greater than 100 °C and a final boiling point less than 615 °C at atmospheric pressure as measured by this test method.
1.2 The test method is not applicable for analysis of petroleum distillates containing low molecular weight components (for example, naphthas, reformates, gasolines, crude oils). Materials containing heterogeneous components (for example, alcohols, ethers, acids or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, D6352, or D7169.
1.3 This test method uses the principles of simulated distillation methodology.
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 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D7213 − 15 (Reapproved 2019)
Standard Test Method for
Boiling Range Distribution of Petroleum Distillates in the
Boiling Range from 100 °C to 615 °C by Gas
Chromatography
This standard is issued under the fixed designation D7213; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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
2.1 ASTM Standards:
1.1 Thistestmethodcoversthedeterminationoftheboiling
range distribution of petroleum products. This test method is D86Test Method for Distillation of Petroleum Products and
Liquid Fuels at Atmospheric Pressure
applicable to petroleum distillates having an initial boiling
point greater than 100°C and a final boiling point less than D1160TestMethodforDistillationofPetroleumProductsat
Reduced Pressure
615°C at atmospheric pressure as measured by this test
method. D2887Test Method for Boiling Range Distribution of Pe-
troleum Fractions by Gas Chromatography
1.2 The test method is not applicable for analysis of
D2892Test Method for Distillation of Crude Petroleum
petroleum distillates containing low molecular weight compo-
(15-Theoretical Plate Column)
nents (for example, naphthas, reformates, gasolines, crude
D4626Practice for Calculation of Gas Chromatographic
oils). Materials containing heterogeneous components (for
Response Factors
example, alcohols, ethers, acids or esters) or residue are not to
D6352Test Method for Boiling Range Distribution of Pe-
be analyzed by this test method. See Test Methods D7096,
troleum Distillates in Boiling Range from 174°C to
D2887, D6352,or D7169.
700°C by Gas Chromatography
1.3 This test method uses the principles of simulated distil-
D7096Test Method for Determination of the Boiling Range
lation methodology.
Distribution of Gasoline by Wide-Bore Capillary Gas
Chromatography
1.4 The values stated in SI units are to be regarded as
D7169 Test Method for Boiling Point Distribution of
standard. No other units of measurement are included in this
Samples with Residues Such as Crude Oils and Atmo-
standard.
spheric and Vacuum Residues by High Temperature Gas
1.5 This standard does not purport to address all of the
Chromatography
safety concerns, if any, associated with its use. It is the
E355PracticeforGasChromatographyTermsandRelation-
responsibility of the user of this standard to establish appro-
ships
priate safety, health, and environmental practices and deter-
E594Practice for Testing Flame Ionization Detectors Used
mine the applicability of regulatory limitations prior to use.
in Gas or Supercritical Fluid Chromatography
1.6 This international standard was developed in accor-
E1510Practice for Installing Fused Silica Open Tubular
dance with internationally recognized principles on standard-
Capillary Columns in Gas Chromatographs
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
3. Terminology
mendations issued by the World Trade Organization Technical
3.1 Definitions—This test method makes reference to many
Barriers to Trade (TBT) Committee.
common gas chromatographic procedures, terms, and relation-
ships. Detailed definitions of these can be found in Practices
E355, E594, and E1510.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0H on Chromatographic Distribution Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2005. Last previous edition approved in 2015 as D7213–15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7213-15R19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7213 − 15 (2019)
3.2 Definitions of Terms Specific to This Standard: tion detector. The detector signal integral is recorded as area
3.2.1 area slice, n—the area, resulting from the integration slices for consecutive retention time intervals during the
analysis.
of the chromatographic detector signal, within a specified
retention time interval. In area slice mode (see 6.4.2), peak
4.4 Retention times of known normal paraffin hydrocarbons
detection parameters are bypassed and the detector signal
spanningthescopeofthistestmethod(C -C )aredetermined
5 60
integralisrecordedasareaslicesofconsecutive,fixedduration
and correlated to their boiling point temperatures.The normal-
time intervals.
ized cumulative corrected sample areas for each consecutive
3.2.2 corrected area slice, n—an area slice corrected for recorded time interval are used to calculate the boiling range
baseline offset, by subtraction of the exactly corresponding distribution. The boiling point temperature at each reported
area slice in a previously recorded blank (non-sample) analy- percent off increment is calculated from the retention time
sis. calibration.
3.2.3 cumulativecorrectedarea,n—theaccumulatedsumof
5. Significance and Use
correctedareaslicesfromthebeginningoftheanalysisthrough
5.1 The boiling range distribution of light and medium
a given retention time, ignoring any non-sample area (for
petroleum distillate fractions provides an insight into the
example, solvent).
composition of feed stocks and products related to petroleum
3.2.4 final boiling point (FBP), n—the temperature (corre-
refining process, This gas chromatographic determination of
spondingtotheretentiontime)atwhichacumulativecorrected
boiling range can be used to replace conventional distillation
area count equal to 99.5% of the total sample area under the
methods for control of refining operations. This test method
chromatogram is obtained.
can be used for product specification testing with the mutual
3.2.5 initial boiling point (IBP), n—the temperature (corre- agreement of interested parties.
spondingtotheretentiontime)atwhichacumulativecorrected
5.2 This test method extends the scope of boiling range
area count equal to 0.5% of the total sample area under the
determination by gas chromatography to include light and
chromatogram is obtained.
mediumpetroleumdistillatefractionsbeyondthescopeofTest
3.2.6 slice rate, n—the time interval used to integrate the
Method D2887 (538°C) and below Test Method D6352
continuous (analog) chromatographic detector response during (700°C).
an analysis. The slice rate is expressed in Hz (for example,
5.3 Boiling range distributions obtained by this test method
integrations or slices per second).
are theoretically equivalent to those obtained by true boiling
3.2.7 slice time, n—the cumulative slice rate (analysis time)
point(TBP)distillation(seeTestMethodD2892).Theyarenot
associatedwitheachareaslicethroughoutthechromatographic
equivalent to results from low efficiency distillation such as
analysis. The slice time is the time at the end of each those obtained with Test Method D86 or D1160.
contiguous area slice.
6. Apparatus
3.2.8 total sample area, n—the cumulative corrected area,
6.1 Chromatograph—Thegaschromatographicsystemused
from the initial point to the final area point.
shall have the following performance characteristics:
3.3 Abbreviations—Acommonabbreviationofhydrocarbon
6.1.1 Column Oven—Capable of sustained and linear pro-
compounds is to designate the number of carbon atoms in the
grammed temperature operation from near ambient (for
compound.Aprefix is used to indicate the carbon chain form,
example, 35°C to 50°C) up to 400°C.
while a subscripted suffix denotes the number of carbon atoms
6.1.2 Column Temperature Programmer—The chromato-
(for example, normal decane n-C ; iso-tetradecane = i-C ).
l0 l4
graph shall be capable of linear programmed temperature
operation up to 400°C at selectable linear rates up to
4. Summary of Test Method
20°C⁄min. The programming rate shall be sufficiently repro-
ducible to obtain the retention time repeatability of 0.1 min
4.1 The boiling range distribution by distillation is simu-
(6s) for each component in the calibration mixture described
latedbytheuseofgaschromatography.Thesolventshouldnot
in 7.5.
interfere with measurement of the sample in the 100°C to
6.1.3 Detector—This test method requires a flame ioniza-
615°Crange,anditshouldbeapolar.Anon-polaropentubular
tion detector (FID). The detector shall meet or exceed the
(capillary) gas chromatographic column is used to elute the
following specifications as detailed in Practice E594. The
hydrocarbon components of the sample in order of increasing
flame jet should have an orifice of approximately 0.45mm to
boiling point.
0.50 mm.
4.2 A sample aliquot is diluted with a viscosity reducing
6.1.3.1 Operating Temperature, 400°C.
solvent and introduced into the chromatographic system.
6.1.3.2 Sensitivity, >0.005 coulombs/g carbon.
Sample vaporization is provided by separate heating of the
-11
6.1.3.3 Minimum Detectability,1×10 g carbon/s.
point of injection or in conjunction with column oven heating. 6
6.1.3.4 Linear Range, >10 .
4.3 Thecolumnoventemperatureisraisedatareproducible 6.1.3.5 Connection of the column to the detector shall be
linear rate to effect separation of the hydrocarbon components such that no temperature below the column temperature exists.
in order of increasing boiling point. The elution of sample Refer to Practice E1510 for proper installation and condition-
components is quantitatively determined using a flame ioniza- ing of the capillary column.
D7213 − 15 (2019)
6.1.4 Sample Inlet System—Any sample inlet system ca- 7. Reagents and Materials
pable of meeting the performance specification in 7.6 may be
7.1 Carrier Gas—Helium or hydrogen of high purity.
used. Programmed temperature vaporization (PTV) and pro-
(Warning—Heliumandhydrogenarecompressedgasesunder
grammable cool on-column injection systems have been used
high pressure; hydrogen is an extremely flammable gas under
successfully.
high pressure.)These gases may be used as the carrier gas and
6.1.5 Carrier Gas Flow Control—The chromatograph shall
should not contain more than 5 mL/m of oxygen. The total
beequippedwithcarriergaspressureorflowcontrolcapableof
amount of impurities should not exceed 10 mL/m .Additional
maintaining constant carrier gas flow control through the
purification is recommended by the use of molecular sieves or
column throughout the column temperature program cycle.
other suitable agents to remove water, oxygen, and hydrocar-
bons.Availablepressureshallbesufficienttoensureaconstant
6.2 Microsyringe—A microsyringe with a 23 gauge or
carrier gas flow rate.
smaller stainless steel needle is used for on-column sample
7.2 Hydrogen—Hydrogen of high purity (for example,
introduction. Syringes of 0.1µL to 10 µL capacity are avail-
hydrocarbon-free) is used as fuel for the flame ionization
able.
detector (FID). (Warning—Hydrogen is an extremely flam-
6.2.1 Automatic syringe injection is recommended to
mable gas under high pressure.)
achieve best precision.
7.3 Air—High purity (for example, hydrocarbon-free) com-
6.3 Column—This test method is limited to the use of
pressed air is used as the oxidant for the flame ionization
non-polar wall coated open tubular (WCOT) columns of high
detector(FID).(Warning—Compressedairisagasunderhigh
thermal stability. Glass, fused silica, and stainless steel
pressure and supports combustion.)
columns, with a 0.53 mm diameter have been successfully
7.4 Solvents—Unless otherwise indicated, it is intended that
used. Cross-linked or bonded 100% dimethyl-polysiloxane
all solvents conform to the specifications of the committee on
stationary phases with film thickness of 0.5µm to 1.0 µm have
analytical Reagents of the American Chemical Society where
been used. The column length and liquid phase film thickness
such specifications are available. Other grades may be used
shall allow the elution of at least C n-paraffin (BP= 615°C).
provided it is first ascertained that the solvent is of sufficiently
The column and conditions shall provide separation of typical
high purity to permit its use without lessening the accuracy of
petroleum hydrocarbons in order of increasing boiling point
the determination.
and meet the column resolution requirements of 8.2.1. The
7.4.1 CarbonDisulfide(CS )—(99+%pure)maybeusedas
column shall provide a resolution between one and ten using 2
a viscosity reducing solvent and as a means of reducing mass
this test method’s operating conditions.
of sample introduced onto the column to ensure linear detector
6.4 Data Acquisition System:
response and reduced peak skewness. It is miscible with
6.4.1 Recorder—A 0mV to 1 mV range recording potenti-
asphaltic hydrocarbons and provides a relatively small re-
ometer or equivalent, with a full-scale response time of2sor
sponsewiththeFID.Thequality(hydrocarboncontent)should
less may be used to provide a graphical display. be determined by this test method prior to use as a sample
diluent. (Warning— Carbon disulfide is extremely flammable
6.4.2 Integrator—Means shall be provided for determining
and toxic.)
the accumulated area under the chromatogram. This can be
done by means of an electronic integrator or computer-based
7.5 Cyclohexane (C H )—(99+% pure) may be used as a
6 12
chromatography data system. The integrator/computer system
viscosity reducing solvent. It is miscible with asphaltic
shallhavenormalchromatographicsoftwareformeasuringthe
hydrocarbons, however, it responds well to the FID. The
retention time and areas of eluting peaks (peak detection
quality(hydrocarboncontent)shouldbedeterminedbythistest
mode). In addition, the system shall be capable of converting
method prior to use as a sample diluent. (Warning—
the continuously integrated detector signal into area slices of
Cyclohexane is flammable.)
fixed duration (area slice mode). These contiguous area slices,
7.6 Calibration Mixture—A qualitative mixture of
collectedfortheentireanalysis,arestoredforlaterprocessing.
n-paraffins (nominally C to C ) dissolved in a suitable
5 60
Theelectronicrangeoftheintegrator/computer(forexample,1
solvent. The final concentration should be approximately one
V, 10 V) shall be operated within the linear range of the
part of n-paraffin mixture to one hundred parts of solvent. At
detect
...
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: D7213 − 15 (Reapproved 2019)
Standard Test Method for
Boiling Range Distribution of Petroleum Distillates in the
Boiling Range from 100 °C to 615 °C by Gas
Chromatography
This standard is issued under the fixed designation D7213; 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 boiling 2.1 ASTM Standards:
range distribution of petroleum products. This test method is D86 Test Method for Distillation of Petroleum Products and
applicable to petroleum distillates having an initial boiling Liquid Fuels at Atmospheric Pressure
point greater than 100 °C and a final boiling point less than D1160 Test Method for Distillation of Petroleum Products at
Reduced Pressure
615 °C at atmospheric pressure as measured by this test
method. D2887 Test Method for Boiling Range Distribution of Pe-
troleum Fractions by Gas Chromatography
1.2 The test method is not applicable for analysis of
D2892 Test Method for Distillation of Crude Petroleum
petroleum distillates containing low molecular weight compo-
(15-Theoretical Plate Column)
nents (for example, naphthas, reformates, gasolines, crude
D4626 Practice for Calculation of Gas Chromatographic
oils). Materials containing heterogeneous components (for
Response Factors
example, alcohols, ethers, acids or esters) or residue are not to
D6352 Test Method for Boiling Range Distribution of Pe-
be analyzed by this test method. See Test Methods D7096,
troleum Distillates in Boiling Range from 174 °C to
D2887, D6352, or D7169.
700 °C by Gas Chromatography
1.3 This test method uses the principles of simulated distil-
D7096 Test Method for Determination of the Boiling Range
lation methodology.
Distribution of Gasoline by Wide-Bore Capillary Gas
Chromatography
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this D7169 Test Method for Boiling Point Distribution of
Samples with Residues Such as Crude Oils and Atmo-
standard.
spheric and Vacuum Residues by High Temperature Gas
1.5 This standard does not purport to address all of the
Chromatography
safety concerns, if any, associated with its use. It is the
E355 Practice for Gas Chromatography Terms and Relation-
responsibility of the user of this standard to establish appro-
ships
priate safety, health, and environmental practices and deter-
E594 Practice for Testing Flame Ionization Detectors Used
mine the applicability of regulatory limitations prior to use.
in Gas or Supercritical Fluid Chromatography
1.6 This international standard was developed in accor-
E1510 Practice for Installing Fused Silica Open Tubular
dance with internationally recognized principles on standard-
Capillary Columns in Gas Chromatographs
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
3. Terminology
mendations issued by the World Trade Organization Technical
3.1 Definitions—This test method makes reference to many
Barriers to Trade (TBT) Committee.
common gas chromatographic procedures, terms, and relation-
ships. Detailed definitions of these can be found in Practices
E355, E594, and E1510.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0H on Chromatographic Distribution Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2005. Last previous edition approved in 2015 as D7213 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7213-15R19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7213 − 15 (2019)
3.2 Definitions of Terms Specific to This Standard: tion detector. The detector signal integral is recorded as area
slices for consecutive retention time intervals during the
3.2.1 area slice, n—the area, resulting from the integration
of the chromatographic detector signal, within a specified analysis.
retention time interval. In area slice mode (see 6.4.2), peak
4.4 Retention times of known normal paraffin hydrocarbons
detection parameters are bypassed and the detector signal
spanning the scope of this test method (C -C ) are determined
5 60
integral is recorded as area slices of consecutive, fixed duration
and correlated to their boiling point temperatures. The normal-
time intervals.
ized cumulative corrected sample areas for each consecutive
3.2.2 corrected area slice, n—an area slice corrected for recorded time interval are used to calculate the boiling range
baseline offset, by subtraction of the exactly corresponding distribution. The boiling point temperature at each reported
area slice in a previously recorded blank (non-sample) analy- percent off increment is calculated from the retention time
sis. calibration.
3.2.3 cumulative corrected area, n—the accumulated sum of
5. Significance and Use
corrected area slices from the beginning of the analysis through
5.1 The boiling range distribution of light and medium
a given retention time, ignoring any non-sample area (for
petroleum distillate fractions provides an insight into the
example, solvent).
composition of feed stocks and products related to petroleum
3.2.4 final boiling point (FBP), n—the temperature (corre-
refining process, This gas chromatographic determination of
sponding to the retention time) at which a cumulative corrected
boiling range can be used to replace conventional distillation
area count equal to 99.5 % of the total sample area under the
methods for control of refining operations. This test method
chromatogram is obtained.
can be used for product specification testing with the mutual
3.2.5 initial boiling point (IBP), n—the temperature (corre- agreement of interested parties.
sponding to the retention time) at which a cumulative corrected
5.2 This test method extends the scope of boiling range
area count equal to 0.5 % of the total sample area under the
determination by gas chromatography to include light and
chromatogram is obtained.
medium petroleum distillate fractions beyond the scope of Test
3.2.6 slice rate, n—the time interval used to integrate the Method D2887 (538 °C) and below Test Method D6352
continuous (analog) chromatographic detector response during
(700 °C).
an analysis. The slice rate is expressed in Hz (for example,
5.3 Boiling range distributions obtained by this test method
integrations or slices per second).
are theoretically equivalent to those obtained by true boiling
3.2.7 slice time, n—the cumulative slice rate (analysis time)
point (TBP) distillation (see Test Method D2892). They are not
associated with each area slice throughout the chromatographic equivalent to results from low efficiency distillation such as
analysis. The slice time is the time at the end of each
those obtained with Test Method D86 or D1160.
contiguous area slice.
6. Apparatus
3.2.8 total sample area, n—the cumulative corrected area,
6.1 Chromatograph—The gas chromatographic system used
from the initial point to the final area point.
shall have the following performance characteristics:
3.3 Abbreviations—A common abbreviation of hydrocarbon
6.1.1 Column Oven—Capable of sustained and linear pro-
compounds is to designate the number of carbon atoms in the
grammed temperature operation from near ambient (for
compound. A prefix is used to indicate the carbon chain form,
example, 35 °C to 50 °C) up to 400 °C.
while a subscripted suffix denotes the number of carbon atoms
6.1.2 Column Temperature Programmer—The chromato-
(for example, normal decane n-C ; iso-tetradecane = i-C ).
l0 l4 graph shall be capable of linear programmed temperature
operation up to 400 °C at selectable linear rates up to
4. Summary of Test Method
20 °C ⁄min. The programming rate shall be sufficiently repro-
ducible to obtain the retention time repeatability of 0.1 min
4.1 The boiling range distribution by distillation is simu-
(6 s) for each component in the calibration mixture described
lated by the use of gas chromatography. The solvent should not
in 7.5.
interfere with measurement of the sample in the 100 °C to
6.1.3 Detector—This test method requires a flame ioniza-
615 °C range, and it should be apolar. A non-polar open tubular
tion detector (FID). The detector shall meet or exceed the
(capillary) gas chromatographic column is used to elute the
following specifications as detailed in Practice E594. The
hydrocarbon components of the sample in order of increasing
flame jet should have an orifice of approximately 0.45 mm to
boiling point.
0.50 mm.
4.2 A sample aliquot is diluted with a viscosity reducing
6.1.3.1 Operating Temperature, 400 °C.
solvent and introduced into the chromatographic system.
6.1.3.2 Sensitivity, >0.005 coulombs/g carbon.
Sample vaporization is provided by separate heating of the -11
6.1.3.3 Minimum Detectability, 1 × 10 g carbon/s.
point of injection or in conjunction with column oven heating.
6.1.3.4 Linear Range, >10 .
4.3 The column oven temperature is raised at a reproducible 6.1.3.5 Connection of the column to the detector shall be
linear rate to effect separation of the hydrocarbon components such that no temperature below the column temperature exists.
in order of increasing boiling point. The elution of sample Refer to Practice E1510 for proper installation and condition-
components is quantitatively determined using a flame ioniza- ing of the capillary column.
D7213 − 15 (2019)
6.1.4 Sample Inlet System—Any sample inlet system ca- 7. Reagents and Materials
pable of meeting the performance specification in 7.6 may be
7.1 Carrier Gas—Helium or hydrogen of high purity.
used. Programmed temperature vaporization (PTV) and pro-
(Warning—Helium and hydrogen are compressed gases under
grammable cool on-column injection systems have been used
high pressure; hydrogen is an extremely flammable gas under
successfully.
high pressure.) These gases may be used as the carrier gas and
6.1.5 Carrier Gas Flow Control—The chromatograph shall
should not contain more than 5 mL/m of oxygen. The total
be equipped with carrier gas pressure or flow control capable of
amount of impurities should not exceed 10 mL/m . Additional
maintaining constant carrier gas flow control through the
purification is recommended by the use of molecular sieves or
column throughout the column temperature program cycle.
other suitable agents to remove water, oxygen, and hydrocar-
bons. Available pressure shall be sufficient to ensure a constant
6.2 Microsyringe—A microsyringe with a 23 gauge or
carrier gas flow rate.
smaller stainless steel needle is used for on-column sample
7.2 Hydrogen—Hydrogen of high purity (for example,
introduction. Syringes of 0.1 µL to 10 µL capacity are avail-
hydrocarbon-free) is used as fuel for the flame ionization
able.
detector (FID). (Warning—Hydrogen is an extremely flam-
6.2.1 Automatic syringe injection is recommended to
mable gas under high pressure.)
achieve best precision.
7.3 Air—High purity (for example, hydrocarbon-free) com-
6.3 Column—This test method is limited to the use of
pressed air is used as the oxidant for the flame ionization
non-polar wall coated open tubular (WCOT) columns of high
detector (FID). (Warning—Compressed air is a gas under high
thermal stability. Glass, fused silica, and stainless steel
pressure and supports combustion.)
columns, with a 0.53 mm diameter have been successfully
7.4 Solvents—Unless otherwise indicated, it is intended that
used. Cross-linked or bonded 100 % dimethyl-polysiloxane
all solvents conform to the specifications of the committee on
stationary phases with film thickness of 0.5 µm to 1.0 µm have
analytical Reagents of the American Chemical Society where
been used. The column length and liquid phase film thickness
such specifications are available. Other grades may be used
shall allow the elution of at least C n-paraffin (BP = 615 °C).
provided it is first ascertained that the solvent is of sufficiently
The column and conditions shall provide separation of typical
high purity to permit its use without lessening the accuracy of
petroleum hydrocarbons in order of increasing boiling point
the determination.
and meet the column resolution requirements of 8.2.1. The
7.4.1 Carbon Disulfide (CS )—(99+ % pure) may be used as
column shall provide a resolution between one and ten using
a viscosity reducing solvent and as a means of reducing mass
this test method’s operating conditions.
of sample introduced onto the column to ensure linear detector
6.4 Data Acquisition System:
response and reduced peak skewness. It is miscible with
6.4.1 Recorder—A 0 mV to 1 mV range recording potenti-
asphaltic hydrocarbons and provides a relatively small re-
ometer or equivalent, with a full-scale response time of 2 s or
sponse with the FID. The quality (hydrocarbon content) should
less may be used to provide a graphical display.
be determined by this test method prior to use as a sample
diluent. (Warning— Carbon disulfide is extremely flammable
6.4.2 Integrator—Means shall be provided for determining
and toxic.)
the accumulated area under the chromatogram. This can be
done by means of an electronic integrator or computer-based
7.5 Cyclohexane (C H )—(99+ % pure) may be used as a
6 12
chromatography data system. The integrator/computer system
viscosity reducing solvent. It is miscible with asphaltic
shall have normal chromatographic software for measuring the
hydrocarbons, however, it responds well to the FID. The
retention time and areas of eluting peaks (peak detection
quality (hydrocarbon content) should be determined by this test
mode). In addition, the system shall be capable of converting
method prior to use as a sample diluent. (Warning—
the continuously integrated detector signal into area slices of
Cyclohexane is flammable.)
fixed duration (area slice mode). These contiguous area slices,
7.6 Calibration Mixture—A qualitative mixture of
collected for the entire analysis, are stored for later processing.
n-paraffins (nominally C to C ) dissolved in a suitable
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The electronic range of the integrator/computer (for example, 1
solvent. The final concentration should
...
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: D7213 − 15 D7213 − 15 (Reapproved 2019)
Standard Test Method for
Boiling Range Distribution of Petroleum Distillates in the
Boiling Range from 100 °C to 615 °C by Gas
Chromatography
This standard is issued under the fixed designation D7213; 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*Scope
1.1 This test method covers the determination of the boiling range distribution of petroleum products. This test method is
applicable to petroleum distillates having an initial boiling point greater than 100 °C and a final boiling point less than 615 °C at
atmospheric pressure as measured by this test method.
1.2 The test method is not applicable for analysis of petroleum distillates containing low molecular weight components (for
example, naphthas, reformates, gasolines, crude oils). Materials containing heterogeneous components (for example, alcohols,
ethers, acids or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, D6352, or D7169.
1.3 This test method uses the principles of simulated distillation methodology.
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 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D1160 Test Method for Distillation of Petroleum Products at Reduced Pressure
D2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
D2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)
D4626 Practice for Calculation of Gas Chromatographic Response Factors
D6352 Test Method for Boiling Range Distribution of Petroleum Distillates in Boiling Range from 174 °C to 700 °C by Gas
Chromatography
D7096 Test Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary Gas
Chromatography
D7169 Test Method for Boiling Point Distribution of Samples with Residues Such as Crude Oils and Atmospheric and Vacuum
Residues by High Temperature Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
E1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.04.0H on Chromatographic Distribution Methods.
Current edition approved July 1, 2015Dec. 1, 2019. Published Ju;y 2015December 2019. Originally approved in 2005. Last previous edition approved in 20142015 as
D7213 – 14.D7213 – 15. DOI: 10.1520/D7213-15.10.1520/D7213-15R19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. 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
D7213 − 15 (2019)
3. Terminology
3.1 Definitions—This test method makes reference to many common gas chromatographic procedures, terms, and relationships.
Detailed definitions of these can be found in Practices E355, E594, and E1510.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 area slice, n—the area, resulting from the integration of the chromatographic detector signal, within a specified retention
time interval. In area slice mode (see 6.4.2), peak detection parameters are bypassed and the detector signal integral is recorded
as area slices of consecutive, fixed duration time intervals.
3.2.2 corrected area slice, n—an area slice corrected for baseline offset, by subtraction of the exactly corresponding area slice
in a previously recorded blank (non-sample) analysis.
3.2.3 cumulative corrected area, n—the accumulated sum of corrected area slices from the beginning of the analysis through
a given retention time, ignoring any non-sample area (for example, solvent).
3.2.4 final boiling point (FBP), n—the temperature (corresponding to the retention time) at which a cumulative corrected area
count equal to 99.5 % of the total sample area under the chromatogram is obtained.
3.2.5 initial boiling point (IBP), n—the temperature (corresponding to the retention time) at which a cumulative corrected area
count equal to 0.5 % of the total sample area under the chromatogram is obtained.
3.2.6 slice rate, n—the time interval used to integrate the continuous (analog) chromatographic detector response during an
analysis. The slice rate is expressed in Hz (for example, integrations or slices per second).
3.2.7 slice time, n—the cumulative slice rate (analysis time) associated with each area slice throughout the chromatographic
analysis. The slice time is the time at the end of each contiguous area slice.
3.2.8 total sample area, n—the cumulative corrected area, from the initial point to the final area point.
3.3 Abbreviations—A common abbreviation of hydrocarbon compounds is to designate the number of carbon atoms in the
compound. A prefix is used to indicate the carbon chain form, while a subscripted suffix denotes the number of carbon atoms (for
example, normal decane n-C ; iso-tetradecane = i-C ).
l0 l4
4. Summary of Test Method
4.1 The boiling range distribution by distillation is simulated by the use of gas chromatography. The solvent should not interfere
with measurement of the sample in the 100 °C to 615 °C range, and it should be apolar. A non-polar open tubular (capillary) gas
chromatographic column is used to elute the hydrocarbon components of the sample in order of increasing boiling point.
4.2 A sample aliquot is diluted with a viscosity reducing solvent and introduced into the chromatographic system. Sample
vaporization is provided by separate heating of the point of injection or in conjunction with column oven heating.
4.3 The column oven temperature is raised at a reproducible linear rate to effect separation of the hydrocarbon components in
order of increasing boiling point. The elution of sample components is quantitatively determined using a flame ionization detector.
The detector signal integral is recorded as area slices for consecutive retention time intervals during the analysis.
4.4 Retention times of known normal paraffin hydrocarbons spanning the scope of this test method (C -C ) are determined and
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correlated to their boiling point temperatures. The normalized cumulative corrected sample areas for each consecutive recorded
time interval are used to calculate the boiling range distribution. The boiling point temperature at each reported percent off
increment is calculated from the retention time calibration.
5. Significance and Use
5.1 The boiling range distribution of light and medium petroleum distillate fractions provides an insight into the composition
of feed stocks and products related to petroleum refining process, This gas chromatographic determination of boiling range can
be used to replace conventional distillation methods for control of refining operations. This test method can be used for product
specification testing with the mutual agreement of interested parties.
5.2 This test method extends the scope of boiling range determination by gas chromatography to include light and medium
petroleum distillate fractions beyond the scope of Test Method D2887 (538 °C) and below Test Method D6352 (700 °C).
5.3 Boiling range distributions obtained by this test method are theoretically equivalent to those obtained by true boiling point
(TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillation such as those
obtained with Test Method D86 or D1160.
6. Apparatus
6.1 Chromatograph—The gas chromatographic system used shall have the following performance characteristics:
6.1.1 Column Oven—Capable of sustained and linear programmed temperature operation from near ambient (for example,
35 °C to 50 °C) up to 400 °C.
D7213 − 15 (2019)
6.1.2 Column Temperature Programmer—The chromatograph shall be capable of linear programmed temperature operation up
to 400 °C at selectable linear rates up to 20 °C ⁄min. The programming rate shall be sufficiently reproducible to obtain the retention
time repeatability of 0.1 min (6 s) for each component in the calibration mixture described in 7.5.
6.1.3 Detector—This test method requires a flame ionization detector (FID). The detector shall meet or exceed the following
specifications as detailed in Practice E594. The flame jet should have an orifice of approximately 0.45 mm to 0.50 mm.
6.1.3.1 Operating Temperature, 400 °C.
6.1.3.2 Sensitivity, >0.005 coulombs/g carbon.
-11
6.1.3.3 Minimum Detectability, 1 × 10 g carbon/s.
6.1.3.4 Linear Range, >10 .
6.1.3.5 Connection of the column to the detector shall be such that no temperature below the column temperature exists. Refer
to Practice E1510 for proper installation and conditioning of the capillary column.
6.1.4 Sample Inlet System—Any sample inlet system capable of meeting the performance specification in 7.6 may be used.
Programmed temperature vaporization (PTV) and programmable cool on-column injection systems have been used successfully.
6.1.5 Carrier Gas Flow Control—The chromatograph shall be equipped with carrier gas pressure or flow control capable of
maintaining constant carrier gas flow control through the column throughout the column temperature program cycle.
6.2 Microsyringe—A microsyringe with a 23 gauge or smaller stainless steel needle is used for on-column sample introduction.
Syringes of 0.1 μL to 10 μL capacity are available.
6.2.1 Automatic syringe injection is recommended to achieve best precision.
6.3 Column—This test method is limited to the use of non-polar wall coated open tubular (WCOT) columns of high thermal
stability. Glass, fused silica, and stainless steel columns, with a 0.53 mm diameter have been successfully used. Cross-linked or
bonded 100 % dimethyl-polysiloxane stationary phases with film thickness of 0.5 μm to 1.0 μm have been used. The column length
and liquid phase film thickness shall allow the elution of at least C n-paraffin (BP = 615 °C). The column and conditions shall
provide separation of typical petroleum hydrocarbons in order of increasing boiling point and meet the column resolution
requirements of 8.2.1. The column shall provide a resolution between one and ten using this test method’s operating conditions.
6.4 Data Acquisition System:
6.4.1 Recorder—A 0 mV to 1 mV range recording potentiometer or equivalent, with a full-scale response time of 2 s or less may
be used to provide a graphical display.
6.4.2 Integrator—Means shall be provided for determining the accumulated area under the chromatogram. This can be done by
means of an electronic integrator or computer-based chromatography data system. The integrator/computer system shall have
normal chromatographic software for measuring the retention time and areas of eluting peaks (peak detection mode). In addition,
the system shall be capable of converting the continuously integrated detector signal into area slices of fixed duration (area slice
mode). These contiguous area slices, collected for the entire analysis, are stored for later processing. The electronic range of the
integrator/computer (for example, 1 V, 10 V) shall be operated within the linear range of the detector/electrometer system used.
NOTE 1—Some gas chromatographs have an algorithm built into their operating software that allows a mathematical model of the baseline profile to
be stored in memory. This profile is automatically subtracted from the detector signal on subsequent sample runs to compensate for the column bleed.
Some integration systems also store and automatically subtract a blank analysis from subsequent analytical determinations.
7. Reagents and Materials
7.1 Carrier Gas—Helium or hydrogen of high purity. (Warning—Helium and hydrogen are compressed gases under high
pressure; hydrogen is an extremely flammable gas under high pressure.) These gases may be used as the carrier gas and should
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not contain more than 5 mL/m of oxygen. The total amount of impurities should not exceed 10 mL/m . Additional purification
is recommended by the use of molecular sieves or other suitable agents to remove water, oxygen, and hydrocarbons. Available
pressure shall be sufficient to ensure a constant carrier gas flow rate.
7.2 Hydrogen—Hydrogen of high purity (for example, hydrocarbon-free) is used as fuel for the flame ionization detector (FID).
(Warning—Hydrogen is an extremely flammable gas under high pressure.)
7.3 Air—High purity (for example, hydrocarbon-free) compressed air is used as the oxidant for the flame ionization detector
(FID). (Warning—Compressed air is a gas under high pressure and supports combustion.)
7.4 Solvents—Unless otherwise indicated, it is intended that all solvents conform to the specifications of the committee on
analytical Reagents of the American Chemical Society where such specifications are available. Other grades may be used provided
it is first ascertained that the solvent is of sufficiently high purity to permit its use without lessening the accuracy of the
determination.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures
...
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