ASTM D7500-14
(Test Method)Standard Test Method for Determination of Boiling Range Distribution of Distillates and Lubricating Base Oils—in Boiling Range from 100 °C to 735 °C by Gas Chromatography
Standard Test Method for Determination of Boiling Range Distribution of Distillates and Lubricating Base Oils—in Boiling Range from 100 °C to 735 °C by Gas Chromatography
SIGNIFICANCE AND USE
5.1 The boiling range distribution of medium and heavy petroleum distillate fractions provides an insight into the composition of feed stocks and products related to petroleum refining processes (for example, hydrocracking, hydrotreating, visbreaking, or deasphalting). The gas chromatographic simulation of this determination 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 distillates (IBP > 100 °C) and heavy petroleum distillate fractions beyond the scope of Test Method D2887 (538 °C).
5.3 Boiling range distributions obtained by this test method have not been analyzed for correlation to those obtained by low efficiency distillation, such as with Test Method D86 or D1160. This test method does not claim agreement between these physical distillations and simulated distillation. Efforts to resolve this question will continue. When successful resolutions of the questions are determined, this test method will be revised accordingly.
SCOPE
1.1 This test method covers the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionization detection. This standard test method has been developed through the harmonization of two test methods, Test Method D6352 and IP 480. As both of these methods cover the same scope and include very similar operating conditions, it was agreed that a single standard method would benefit the global simulated distillation community.
1.2 This test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphthas, reformates, gasolines, diesel). Components containing hetero atoms (for example alcohols, ethers, acids, or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, or D7213 for possible applicability to analysis of these types of materials. This method is also not suitable for samples that will not elute completely from the gas chromatographic column, leaving residues. For such samples as crude oils and residues, see Test Methods D5307 and D7169.
1.3 This test method is applicable to distillates with initial boiling points above 100 ºC and final boiling points below 735 ºC (carbon 110); for example, distillates (IBP > 100 °C), base oils and lubricating base stocks.
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: D7500 − 14
StandardTest Method for
Determination of Boiling Range Distribution of Distillates
and Lubricating Base Oils—in Boiling Range from 100 °C to
735 °C by Gas Chromatography
This standard is issued under the fixed designation D7500; 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 by capillary gas D86 Test Method for Distillation of Petroleum Products at
chromatography using flame ionization detection. This stan- Atmospheric Pressure
dard test method has been developed through the harmoniza- D1160 Test Method for Distillation of Petroleum Products at
tion of two test methods, Test Method D6352 and IP 480. As Reduced Pressure
both of these methods cover the same scope and include very D2887 Test Method for Boiling Range Distribution of Pe-
similar operating conditions, it was agreed that a single troleum Fractions by Gas Chromatography
standard method would benefit the global simulated distillation D5307 Test Method for Determination of Boiling Range
community. Distribution of Crude Petroleum by Gas Chromatography
(Withdrawn 2011)
1.2 This test method is not applicable for the analysis of
D6352 Test Method for Boiling Range Distribution of Pe-
petroleum or petroleum products containing low molecular
troleum Distillates in Boiling Range from 174 °C to 700
weight components (for example naphthas, reformates,
°C by Gas Chromatography
gasolines, diesel). Components containing hetero atoms (for
D7096 Test 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,or D7213 for possible applicability to analysis of these
D7169 Test Method for Boiling Point Distribution of
types of materials.This method is also not suitable for samples
Samples with Residues Such as Crude Oils and Atmo-
that will not elute completely from the gas chromatographic
spheric and Vacuum Residues by High Temperature Gas
column, leaving residues. For such samples as crude oils and
Chromatography
residues, see Test Methods D5307 and D7169.
D7213 Test Method for Boiling Range Distribution of Pe-
1.3 This test method is applicable to distillates with initial
troleum Distillates in the Boiling Range from 100 °C to
boiling points above 100 ºC and final boiling points below
615 °C by Gas Chromatography
735 ºC (carbon 110); for example, distillates (IBP > 100 °C),
E355 Practice for Gas ChromatographyTerms and Relation-
base oils and lubricating base stocks.
ships
E594 Practice for Testing Flame Ionization Detectors Used
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this in Gas or Supercritical Fluid Chromatography
E1510 Practice for Installing Fused Silica Open Tubular
standard.
Capillary Columns in Gas Chromatographs
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 2.2 ISO Standard:
responsibility of the user of this standard to establish appro-
ISO 3170 Petroleum Liquids Manual Sampling
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
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
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of the ASTM website.
Subcommittee D02.04.0H on Chromatographic Distribution Methods. The last approved version of this historical standard is referenced on
Current edition approved Oct. 1, 2014. Published December 2014. Originally www.astm.org.
approved in 2008. Last previous edition approved in 2012 as D7500 – 12. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D7500-14. 4th Floor, New York, NY 10036, http://www.ansi.org.
*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
D7500 − 14
3. Terminology Sample vaporization is provided by separate heating of the
point of injection or in conjunction with column oven heating.
3.1 Definitions—This test method makes reference to many
4.3 The column oven temperature is raised at a specified
common gas chromatographic procedures, terms, and relation-
linear rate to affect separation of the hydrocarbon components
ships. For definitions of these terms used in this test method,
in order of increasing boiling point. The elution of sample
refer to Practices E355, E594, and E1510.
components is quantitatively determined using a flame ioniza-
3.2 Definitions of Terms Specific to This Standard:
tion detector. The detector signal is recorded as area slices for
3.2.1 areaslice,n—thearearesultingfromtheintegrationof
consecutive retention time intervals during the analysis.
the chromatographic detector signal within a specified reten-
4.4 Retentiontimesofknownnormalparaffinhydrocarbons,
tiontimeinterval.Inareaslicemode(see6.4.1),peakdetection
spanning the scope of the test method, are determined and
parameters are bypassed and the detector signal integral is
correlated to their boiling point temperatures. The normalized
recorded as area slices of consecutive, fixed duration time
cumulative corrected sample areas for each consecutive re-
intervals.
corded time interval are used to calculate the boiling range
3.2.2 corrected area slice, n—an area slice corrected for
distribution. The boiling point temperature at each reported
baseline offset by subtraction of the exactly corresponding area
percent off increment is calculated from the retention time
slice in a previously recorded blank (non-sample) analysis.
calibration.
3.2.3 cumulativecorrectedarea,n—theaccumulatedsumof
5. Significance and Use
correctedareaslicesfromthebeginningoftheanalysisthrough
a given retention time, ignoring any non-sample area (for
5.1 The boiling range distribution of medium and heavy
example, solvent).
petroleum distillate fractions provides an insight into the
composition of feed stocks and products related to petroleum
3.2.4 final boiling point (FBP), n—the temperature (corre-
refining processes (for example, hydrocracking, hydrotreating,
spondingtotheretentiontime)atwhichacumulativecorrected
visbreaking, or deasphalting). The gas chromatographic simu-
area count equal to 99.5 % of the total sample area under the
lationofthisdeterminationcanbeusedtoreplaceconventional
chromatogram is obtained.
distillation methods for control of refining operations.This test
3.2.5 initial boiling point (IBP), n—the temperature (corre-
method can be used for product specification testing with the
spondingtotheretentiontime)atwhichacumulativecorrected
mutual agreement of interested parties.
area count equal to 0.5 % of the total sample area under the
5.2 This test method extends the scope of boiling range
chromatogram is obtained.
determination by gas chromatography to include distillates
3.2.6 slice rate, n—the frequency used in sampling (analog)
(IBP > 100 °C)andheavypetroleumdistillatefractionsbeyond
the chromatographic detector signal during an analysis. The
the scope of Test Method D2887 (538 °C).
slice rate is expressed in Hz (for example integrations or slices
5.3 Boiling range distributions obtained by this test method
per second).
havenotbeenanalyzedforcorrelationtothoseobtainedbylow
3.2.7 slice time, n—the inverse function of the acquisition
efficiencydistillation,suchaswithTestMethodD86orD1160.
rate. It is the time duration of each sampling pulse usually
This test method does not claim agreement between these
expressed in seconds. The slice time is the time at the end of
physical distillations and simulated distillation. Efforts to
each contiguous area slice.
resolve this question will continue. When successful resolu-
3.2.8 total sample area, n—the cumulative corrected area,
tions of the questions are determined, this test method will be
from the initial area point to the final area point, where the
revised accordingly.
chromatographic signal has returned to baseline after complete
sample elution. 6. Apparatus
6.1 Chromatograph—Thegaschromatographicsystemused
3.3 Abbreviations—Acommon abbreviation of hydrocarbon
shall have the following performance characteristics:
compounds is to designate the number of carbon atoms in the
6.1.1 Carrier Gas Flow Control—The chromatograph shall
compound. A prefix is used to indicate the carbon chain form,
beequippedwithcarriergaspressureorflowcontrolcapableof
while a subscripted suffix denotes the number of carbon atoms
(for example n-C for normal-decane, i-C for iso- maintaining constant carrier gas flow to 61 % throughout the
10 14
column temperature program cycle.
tetradecane).
6.1.2 Column Oven—Capable of sustained and linear pro-
grammed temperature operation from near ambient (for
4. Summary of Test Method
example, 30 °C to 35 °C) up to 430 °C.
4.1 The boiling range distribution determination by distilla-
6.1.3 Column Temperature Programmer—The chromato-
tion is simulated by the use of gas chromatography. A
graph shall be capable of linear programmed temperature
non-polar open tubular (capillary) gas chromatographic col-
operation up to 430 °C at selectable linear rates up to
umnisusedtoelutethehydrocarboncomponentsofthesample
10 °C⁄min. The programming rate shall be sufficiently repro-
in order of increasing boiling point.
ducible to obtain the retention time repeatability of 0.1 min
4.2 A sample aliquot is diluted with a viscosity reducing (6 s) for each component in the calibration mixture described
solvent and introduced into the chromatographic system. in 7.5.
D7500 − 14
TABLE 2 Typical Operating Conditions for Gas Chromatograph
6.1.4 Detector—This test method requires the use of a flame
ionizationdetector(FID).Thedetectorshallmeetorexceedthe Column length, m 5
Column internal diameter, mm 0.53
following specifications in accordance with Practice E594.
Column material Metal
Check the detector according the instrument manufacturers
Stationary phase type methyl silicone
instructions. Film thickness, µm 0.09 to 0.17
Initial column temperature, °C 35
6.1.4.1 Operating Temperature—100 °C to 430 °C.
Initial hold time, min 0
6.1.4.2 Connection of the column to the detector shall be
Final column temperature, °C 430
Final hold time, min 10
such that no temperature below the column temperature exists
Program rate, °C/min 10
between the column and the detector. Refer to Practice E1510
Injector initial temperature, °C 100
for proper installation and conditioning of the capillary col-
Injector final temperature, °C 430
umn. Injector program rate, °C/min 15
Detector temperature, °C 450
6.1.5 Sample Inlet System—Any sample inlet system ca-
A
Make-up gas flow, He or N2, mL/min 20
A
pable of meeting the performance specification in Annex A3
Hydrogen Flow, mL/min 45
A
Air Flow, mL/min 450
and execute the conditions of Table 2. Programmable tempera-
Carrier gas He
ture vaporization (PTV) and cool on-column (COC) injection
Carrier gas flow rate, constant flow, mL/ 19
systems have been used successfully.
min
A,B
Sample size, µL 1.0
6.2 Microsyringe—A microsyringe with a 23-gauge or
Sample concentration, % (m/m) 2
smaller stainless steel needle is used for on-column sample
Injector PTV or COC
A
introduction. Syringes of 0.1 to 10-µL capacity are available.
Consult with the manufacturer’s operations manual.
B
Monitor skewness when varying the injection volume.
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. Fused silica (aluminum coated) and stainless
eluting peaks (peak processing mode). In addition, the system
steelcolumnswith0.53 mmto0.75 mminternaldiameterhave
shall be capable of converting the continuously integrated
been successfully used. Cross-linked or bonded 100 %
detector signal into area slices of fixed duration (slice mode).
dimethyl-polysiloxane stationary phases with film thickness of
These contiguous area slices, collected for the entire analysis,
0.09 µm to 0.17 µm have been used. The column length and
are stored for later processing.Asimilar collection of contigu-
liquid phase film thickness shall allow the elution of C n-
ousslicesisalsocollectedfortheblankrun.Itisnecessarythat
paraffin (BP = 735 °C). The column and conditions shall
the number of slices collected for sample and blank analysis
provide separation of typical petroleum hydrocarbons in order
are the same. The electronic range of the integrator/computer
of increasing boiling point and meet the column performance
(for example 1 V, 10 V) shall be operated within the linear
requirements of A3.2.1. The column shall provide a resolution
range of the detector/electrometer system used.
not less than 2 and not higher than 4 using the test method
operating conditions in Table 2.
NOTE 1—Some gas chromatographs have an algorithm built into their
operating software that allows a mathematical model of the baseline
6.4 Data Acquisition System:
profile to be stored in memory. This profile is automatically subtracted
6.4.1 Integrator/Computer System—Means shall be pro-
from the detector signal on subsequent sample runs to compensate for the
vided for determining the accumulated area under the chro- column bleed. Some integration systems also store and automatically
subtract a blank analysis from subsequent analytical determinations.
matogram. This can be done by means of an electronic
integratororcomputer-basedchromatographydatasystem.The
7. Reagents and Materials
integrator/computer system shall have normal chromato-
graphic software for measuring the retention time and areas of
7.1 Liquid Stationary Phase—A methyl silicone stationary
phase for the column.
A
TABLE 1 Reference Material 5010
7.2 Carrier Gases—Helium, of at least 99.999 % (v/v)
% Dist.
°C °F r, °C R, °C r, °F R, °F purity. Any oxygen present is removed by a chemical resin
m/m
filter. (Warning—Follow the safety instructions fro
...
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: D7500 − 12 D7500 − 14
Standard Test Method for
Determination of Boiling Range Distribution of Distillates
and Lubricating Base Oils—in Boiling Range from 100100 °C
to 735°C735 °C by Gas Chromatography
This standard is issued under the fixed designation D7500; 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 range distribution of petroleum products by capillary gas
chromatography using flame ionization detection. This standard test method has been developed through the harmonization of two
test methods, Test Method D6352 and IP 480. As both of these methods cover the same scope and include very similar operating
conditions, it was agreed that a single standard method would benefit the global simulated distillation community.
1.2 This test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight
components (for example naphthas, reformates, gasolines, diesel). Components containing hetero atoms (for example alcohols,
ethers, acids, or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, or D7213 for
possible applicability to analysis of these types of materials. This method is also not suitable for samples that will not elute
completely from the gas chromatographic column, leaving residues. For such samples as crude oils and residues, see Test Methods
D5307 and D7169.
1.3 This test method is applicable to distillates with initial boiling points above 100ºC100 ºC and final boiling points below
735ºC735 ºC (carbon 110); for example, distillates (IBP > 100°C),(IBP > 100 °C), base oils and lubricating base stocks.
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
D5307 Test Method for Determination of Boiling Range Distribution of Crude Petroleum by Gas Chromatography (Withdrawn
2011)
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
D7213 Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100 °C to 615 °C by Gas
Chromatography
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 Nov. 1, 2012Oct. 1, 2014. Published April 2013December 2014. Originally approved in 2008. Last previous edition approved in 20102012 as
D7500D7500 – 12.-10. DOI: 10.1520/D7500-12.10.1520/D7500-14.
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.
The last approved version of this historical standard is referenced on www.astm.org.
*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
D7500 − 14
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
2.2 ISO Standard:
ISO 3170 Petroleum Liquids Manual Sampling
3. Terminology
3.1 Definitions—This test method makes reference to many common gas chromatographic procedures, terms, and relationships.
For definitions of these terms used in this test method, refer to 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 6.4.1), 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 frequency used in sampling (analog) the chromatographic detector signal during an analysis. The slice
rate is expressed in Hz (for example integrations or slices per second).
3.2.7 slice time, n—the inverse function of the acquisition rate. It is the time duration of each sampling pulse usually expressed
in seconds. 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 area point to the final area point, where the
chromatographic signal has returned to baseline after complete sample elution.
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 n-C for normal-decane, i-C for iso-tetradecane).
10 14
4. Summary of Test Method
4.1 The boiling range distribution determination by distillation is simulated by the use of gas chromatography. 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 specified linear rate to affect 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 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 the test method, are determined and
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 medium and heavy petroleum distillate fractions provides an insight into the composition
of feed stocks and products related to petroleum refining processes (for example, hydrocracking, hydrotreating, visbreaking, or
deasphalting). The gas chromatographic simulation of this determination 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.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
D7500 − 14
5.2 This test method extends the scope of boiling range determination by gas chromatography to include distillates
(IBP > 100°C)(IBP > 100 °C) and heavy petroleum distillate fractions beyond the scope of Test Method D2887 (538°C).(538 °C).
5.3 Boiling range distributions obtained by this test method have not been analyzed for correlation to those obtained by low
efficiency distillation, such as with Test Method D86 or D1160. This test method does not claim agreement between these physical
distillations and simulated distillation. Efforts to resolve this question will continue. When successful resolutions of the questions
are determined, this test method will be revised accordingly.
6. Apparatus
6.1 Chromatograph—The gas chromatographic system used shall have the following performance characteristics:
6.1.1 Carrier Gas Flow Control—The chromatograph shall be equipped with carrier gas pressure or flow control capable of
maintaining constant carrier gas flow to 61 % throughout the column temperature program cycle.
6.1.2 Column Oven—Capable of sustained and linear programmed temperature operation from near ambient (for example,
3030 °C to 35°C)35 °C) up to 430°C.430 °C.
6.1.3 Column Temperature Programmer—The chromatograph shall be capable of linear programmed temperature operation up
to 430°C430 °C at selectable linear rates up to 10°C/min.10 °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.
6.1.4 Detector—This test method requires the use of a flame ionization detector (FID). The detector shall meet or exceed the
following specifications in accordance with Practice E594. Check the detector according the instrument manufacturers instructions.
6.1.4.1 Operating Temperature—100100 °C to 430°C.430 °C.
6.1.4.2 Connection of the column to the detector shall be such that no temperature below the column temperature exists between
the column and the detector. Refer to Practice E1510 for proper installation and conditioning of the capillary column.
6.1.5 Sample Inlet System—Any sample inlet system capable of meeting the performance specification in Annex A3 and execute
the conditions of Table 2. Programmable temperature vaporization (PTV) and cool on-column (COC) injection systems have been
used successfully.
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 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. Fused silica (aluminum coated) and stainless steel columns with 0.530.53 mm to 0.75-mm0.75 mm internal diameter have
been successfully used. Cross-linked or bonded 100 % dimethyl-polysiloxane stationary phases with film thickness of 0.09 μm to
0.17 μm have been used. The column length and liquid phase film thickness shall allow the elution of C n-paraffin (BP =
735°C).735 °C). The column and conditions shall provide separation of typical petroleum hydrocarbons in order of increasing
boiling point and meet the column performance requirements of A3.2.1. The column shall provide a resolution not less than 2 and
not higher than 4 using the test method operating conditions in Table 2.
6.4 Data Acquisition System:
6.4.1 Integrator/Computer System—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 processing
mode). In addition, the system shall be capable of converting the continuously integrated detector signal into area slices of fixed
duration (slice mode). These contiguous area slices, collected for the entire analysis, are stored for later processing. A similar
collection of contiguous slices is also collected for the blank run. It is necessary that the number of slices collected for sample and
A
TABLE 1 Reference Material 5010
% Dist.
°C °F r, °C R, °C r, °F R, °F
m/m
IBP 421 789 3 9 5 16
5 476 888 2 4 4 8
10 491 916 2 4 3 7
20 510 950 2 5 3 9
30 524 975 2 5 3 9
40 536 998 2 5 3 9
50 548 1018 2 5 3 9
60 559 1039 2 5 3 9
70 572 1061 2 5 3 9
80 585 1085 2 5 3 9
90 602 1116 2 5 3 9
95 617 1142 2 5 3 9
FBP 661 1223 9 17 16 31
A
Values obtained from including Reference Oil 5010 in the ILS sample set.
D7500 − 14
TABLE 2 Typical Operating Conditions for Gas Chromatograph
Column length, m 5
Column internal diameter, mm 0.53
Column material Metal
Stationary phase type methyl silicone
Film thickness, μm 0.09 to 0.17
Initial column temperature, °C 35
Initial hold time, min 0
Final column temperature, °C 430
Final hold time, min 10
Program rate, °C/min 10
Injector initial temperature, °C 100
Injector final temperature, °C 430
Injector program rate, °C/min 15
Detector temperature, °C 450
A
Make-up gas flow, He or N2, mL/min 20
A
Hydrogen Flow, mL/min 45
A
Air Flow, mL/min 450
Carrier gas He
Carrier gas flow rate, constant flow, mL/ 19
min
A,B
Sample size, μL 1.0
Sample concentration, % (m/m) 2
Injector PTV or COC
A
Co
...
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