ASTM D7213-14
(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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D7213 − 14
StandardTest 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* D1160TestMethodforDistillationofPetroleumProductsat
Reduced Pressure
1.1 Thistestmethodcoversthedeterminationoftheboiling
D2887Test Method for Boiling Range Distribution of Pe-
range distribution of petroleum products. This test method is
troleum Fractions by Gas Chromatography
applicable to petroleum distillates having an initial boiling
D2892Test Method for Distillation of Crude Petroleum
point greater than 100°C and a final boiling point less than
(15-Theoretical Plate Column)
615°C at atmospheric pressure as measured by this test
D4626Practice for Calculation of Gas Chromatographic
method.
Response Factors
1.2 The test method is not applicable for analysis of
D6352Test Method for Boiling Range Distribution of Pe-
petroleum distillates containing low molecular weight compo-
troleum Distillates in Boiling Range from 174 °C to 700
nents (for example, naphthas, reformates, gasolines, crude
°C by Gas Chromatography
oils). Materials containing heterogeneous components (for
D7096Test Method for Determination of the Boiling Range
example, alcohols, ethers, acids or esters) or residue are not to
Distribution of Gasoline by Wide-Bore Capillary Gas
be analyzed by this test method. See Test Methods D7096,
Chromatography
D2887, D6352,or D7169.
D7169 Test Method for Boiling Point Distribution of
Samples with Residues Such as Crude Oils and Atmo-
1.3 This test method uses the principles of simulated distil-
lation methodology. spheric and Vacuum Residues by High Temperature Gas
Chromatography
1.4 The values stated in SI units are to be regarded as
E355PracticeforGasChromatographyTermsandRelation-
standard. No other units of measurement are included in this
ships
standard.
E594Practice for Testing Flame Ionization Detectors Used
1.5 This standard does not purport to address all of the
in Gas or Supercritical Fluid Chromatography
safety concerns, if any, associated with its use. It is the
E1510Practice for Installing Fused Silica Open Tubular
responsibility of the user of this standard to establish appro-
Capillary Columns in Gas Chromatographs
priate safety and health practices and determine the applica-
3. Terminology
bility of regulatory limitations prior to use.
3.1 Definitions—This test method makes reference to many
2. Referenced Documents
common gas chromatographic procedures, terms, and relation-
ships. Detailed definitions of these can be found in Practices
2.1 ASTM Standards:
E355, E594, and E1510.
D86Test Method for Distillation of Petroleum Products at
Atmospheric Pressure
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
1 retention time interval. In area slice mode (see 6.4.2), peak
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of detection parameters are bypassed and the detector signal
Subcommittee D02.04.0H on Chromatographic Distribution Methods.
integralisrecordedasareaslicesofconsecutive,fixedduration
Current edition approved Oct. 1, 2014. Published December 2014. Originally
time intervals.
ε1
approved in 2005. Last previous edition approved in 2012 as D7213–12 . DOI:
10.1520/D7213-14.
3.2.2 corrected area slice, n—an area slice corrected for
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
baseline offset, by subtraction of the exactly corresponding
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
area slice in a previously recorded blank (non-sample) analy-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sis.
*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 − 14
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
agreement of interested parties.
3.2.5 initial boiling point (IBP), n—the temperature (corre-
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,
from the initial point to the final area point.
6.1 Chromatograph—Thegaschromatographicsystemused
3.3 Abbreviations—Acommonabbreviationofhydrocarbon shall have the following performance characteristics:
compounds is to designate the number of carbon atoms in the
6.1.1 Column Oven—Capable of sustained and linear pro-
compound.Aprefix is used to indicate the carbon chain form,
grammed temperature operation from near ambient (for
while a subscripted suffix denotes the number of carbon atoms
example, 35°C to 50°C) up to 400°C.
(for example, normal decane n-C ; iso-tetradecane = i-C ).
l0 l4
6.1.2 Column Temperature Programmer—The chromato-
graph shall be capable of linear programmed temperature
4. Summary of Test Method
operation up to 400°C at selectable linear rates up to
20°C⁄min. The programming rate shall be sufficiently repro-
4.1 The boiling range distribution by distillation is simu-
ducible to obtain the retention time repeatability of 0.1 min
latedbytheuseofgaschromatography.Thesolventshouldnot
(6s) for each component in the calibration mixture described
interfere with measurement of the sample in the 100°C to
in 7.5.
615°Crange,anditshouldbeapolar.Anon-polaropentubular
(capillary) gas chromatographic column is used to elute the
6.1.3 Detector—This test method requires a flame ioniza-
hydrocarbon components of the sample in order of increasing
tion detector (FID). The detector shall meet or exceed the
boiling point.
following specifications as detailed in Practice E594. The
flame jet should have an orifice of approximately 0.45mm to
4.2 A sample aliquot is diluted with a viscosity reducing
0.50 mm.
solvent and introduced into the chromatographic system.
6.1.3.1 Operating Temperature, 400°C.
Sample vaporization is provided by separate heating of the
point of injection or in conjunction with column oven heating. 6.1.3.2 Sensitivity, >0.005 coulombs/g carbon.
-11
6.1.3.3 Minimum Detectability,1×10 g carbon/s.
4.3 Thecolumnoventemperatureisraisedatareproducible
6.1.3.4 Linear Range, >10 .
linear rate to effect separation of the hydrocarbon components
in order of increasing boiling point. The elution of sample 6.1.3.5 Connection of the column to the detector shall be
components is quantitatively determined using a flame ioniza-
such that no temperature below the column temperature exists.
tion detector. The detector signal integral is recorded as area
Refer to Practice E1510 for proper installation and condition-
slices for consecutive retention time intervals during the
ing of the capillary column.
analysis.
6.1.4 Sample Inlet System—Any sample inlet system ca-
pable of meeting the performance specification in 7.6 may be
4.4 Retention times of known normal paraffin hydrocarbons
used. Programmed temperature vaporization (PTV) and pro-
spanningthescopeofthistestmethod(C -C )aredetermined
5 60
grammable cool on-column injection systems have been used
and correlated to their boiling point temperatures.The normal-
successfully.
ized cumulative corrected sample areas for each consecutive
recorded time interval are used to calculate the boiling range 6.1.5 Carrier Gas Flow Control—The chromatograph shall
distribution. The boiling point temperature at each reported beequippedwithcarriergaspressureorflowcontrolcapableof
percent off increment is calculated from the retention time maintaining constant carrier gas flow control through the
calibration. column throughout the column temperature program cycle.
D7213 − 14
6.2 Microsyringe—A microsyringe with a 23 gauge or other suitable agents to remove water, oxygen, and hydrocar-
smaller stainless steel needle is used for on-column sample bons.Availablepressureshallbesufficienttoensureaconstant
introduction. Syringes of 0.1µL to 10 µL capacity are avail- carrier gas flow rate.
able.
7.2 Hydrogen—Hydrogen of high purity (for example,
6.2.1 Automatic syringe injection is recommended to
hydrocarbon-free) is used as fuel for the flame ionization
achieve best precision.
detector (FID). (Warning—Hydrogen is an extremely flam-
6.3 Column—This test method is limited to the use of mable gas under high pressure.)
non-polar wall coated open tubular (WCOT) columns of high
7.3 Air—High purity (for example, hydrocarbon-free) com-
thermal stability. Glass, fused silica, and stainless steel
pressed air is used as the oxidant for the flame ionization
columns, with a 0.53 mm diameter have been successfully
detector(FID).(Warning—Compressedairisagasunderhigh
used. Cross-linked or bonded 100% dimethyl-polysiloxane
pressure and supports combustion.)
stationary phases with film thickness of 0.5µm to 1.0 µm have
7.4 Solvents—Unless otherwise indicated, it is intended that
been used. The column length and liquid phase film thickness
all solvents conform to the specifications of the committee on
shall allow the elution of at least C n-paraffin (BP= 615°C).
analytical Reagents of the American Chemical Society where
The column and conditions shall provide separation of typical
such specifications are available. Other grades may be used
petroleum hydrocarbons in order of increasing boiling point
provided it is first ascertained that the solvent is of sufficiently
and meet the column resolution requirements of 8.2.1. The
high purity to permit its use without lessening the accuracy of
column shall provide a resolution between one and ten using
the determination.
this test method’s operating conditions.
7.4.1 CarbonDisulfide(CS )—(99+%pure)maybeusedas
6.4 Data Acquisition System:
a viscosity reducing solvent and as a means of reducing mass
6.4.1 Recorder—A 0mV to 1 mV range recording potenti-
of sample introduced onto the column to ensure linear detector
ometer or equivalent, with a full-scale response time of2sor
response and reduced peak skewness. It is miscible with
less may be used to provide a graphical display.
asphaltic hydrocarbons and provides a relatively small re-
6.4.2 Integrator—Means shall be provided for determining
sponsewiththeFID.Thequality(hydrocarboncontent)should
the accumulated area under the chromatogram. This can be
be determined by this test method prior to use as a sample
done by means of an electronic integrator or computer-based
diluent. (Warning— Carbon disulfide is extremely flammable
chromatography data system. The integrator/computer system
and toxic.)
shallhavenormalchromatographicsoftwareformeasuringthe
7.5 Cyclohexane (C H )—(99+% pure) may be used as a
6 12
retention time and areas of eluting peaks (peak detection
viscosity reducing solvent. It is miscible with asphaltic
mode). In addition, the system shall be capable of converting
hydrocarbons, however, it responds well to the FID. The
the continuously integrated detector signal into area slices of
quality(hydrocarboncontent)shouldbedeterminedbythistest
fixed duration (area slice mode). These contiguous area slices,
method prior to use as a sample diluent. (Warning—
collectedfortheentireanalysis,arestoredforlaterprocessing.
Cyclohexane is flammable.)
Theelectronicrangeoftheintegrator/computer(forexample,1
V, 10 V) shall be operated within the linear range of the
7.6 Calibration Mixture—A qualitative mixture of
detector/electrometer system used. n-paraffins (nominally C to C ) dissolved in a suitable
5 60
solvent. The final concentration should be approximately one
NOTE 1—Some gas chromatographs have an algorithm built into their
part of n-paraffin mixture to one hundred parts of solvent. At
operating software that allows a mathematical model of the baseline
profile to be stored in memory. This profile is automatically subtracted least one compound in the mixture shall have a boiling point
from the detector signal on subsequent sample runs to compensate for the
lower than the initial boiling point of the sample being
column bleed. Some integration systems also store and automatically
analyzed, as defined in the scope of this test method (1.1).The
subtract a blank analysis from subsequent analytical determinations.
calibration mixture shall contain at least 13 known n-paraffins
(for example, C,C,C,C,C ,C ,C ,C ,C ,C ,C ,
6 7 8 9 10 12 16 20 30 40 50
7. Reagents and Materials
C ,C ). Boiling points of n-paraffins are listed in Table 1.
52 60
7.1 Carrier Gas—Helium or hydrogen of high purity.
NOTE
...
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.
´1
Designation: D7213 − 12 D7213 − 14
Standard Test Method for
Boiling Range Distribution of Petroleum Distillates in the
Boiling Range from 100100 °C to 615°C615 °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.
ε NOTE—Editorial changes made in April 2013.
1. 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°C100 °C and a final boiling point less than
615°C615 °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 D3710D7096, D2887, D6352, or
D5307D7169.
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 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
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)
D3710 Test Method for Boiling Range Distribution of Gasoline and Gasoline Fractions by Gas Chromatography (Withdrawn
2014)
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
D5307D7096 Test Method for Determination of the Boiling Range Distribution of Crude Petroleum by Gasoline by Wide-Bore
Capillary Gas Chromatography (Withdrawn 2011)
D6352D7169 Test Method for Boiling Range Distribution of Petroleum Distillates in Boiling Range from 174 °C to 700 °C by
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 Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0H on Chromatographic Distribution Methods.
Current edition approved Dec. 1, 2012Oct. 1, 2014. Published December 2012December 2014. Originally approved in 2005. Last previous edition approved in 20112012
ε1
as D7213 – 12 D7213–11. DOI: 10.1520/D7213-12.10.1520/D7213-14.
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 − 14
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 100100 °C to 615°C615 °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
5 60
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)(538 °C) and below Test Method D6352
(700°C).(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:
D7213 − 14
6.1.1 Column Oven—Capable of sustained and linear programmed temperature operation from near ambient (for example,
3535 °C to 50°C)50 °C) up to 400°C.400 °C.
6.1.2 Column Temperature Programmer—The chromatograph shall be capable of linear programmed temperature operation up
to 400°C400 °C at selectable linear rates up to 20°C/min.20 °C ⁄min. The programming rate shall be sufficiently reproducible to
obtain the retention time repeatability of 0.1 min (6 s) (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 0.450.45 mm to 0.50 mm.
6.1.3.1 Operating Temperature, 400°C.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 0.10.1 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 0.50.5 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).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 00 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
3 3
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.)
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D7213 − 14
7.4 Solvents—Unless other
...
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