ASTM D7500-15(2019)
(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, 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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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: D7500 − 15 (Reapproved 2019)
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
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 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the determination of the boiling
ization established in the Decision on Principles for the
range distribution of petroleum products by capillary gas
Development of International Standards, Guides and Recom-
chromatography using flame ionization detection. This stan-
mendations issued by the World Trade Organization Technical
dard test method has been developed through the harmoniza-
Barriers to Trade (TBT) Committee.
tion of two test methods, Test Method D6352 and IP 480. As
both of these methods cover the same scope and include very
2. Referenced Documents
similar operating conditions, it was agreed that a single
2.1 ASTM Standards:
standard method would benefit the global simulated distillation
D86 Test Method for Distillation of Petroleum Products and
community.
Liquid Fuels at Atmospheric Pressure
1.2 This test method is not applicable for the analysis of
D1160 Test Method for Distillation of Petroleum Products at
petroleum or petroleum products containing low molecular
Reduced Pressure
weight components (for example naphthas, reformates,
D2887 Test Method for Boiling Range Distribution of Pe-
gasolines, diesel). Components containing hetero atoms (for
troleum Fractions by Gas Chromatography
example alcohols, ethers, acids, or esters) or residue are not to
D5307 Test Method for Determination of Boiling Range
be analyzed by this test method. See Test Methods D7096,
Distribution of Crude Petroleum by Gas Chromatography
D2887,or D7213 for possible applicability to analysis of these 3
(Withdrawn 2011)
types of materials.This method is also not suitable for samples
D6352 Test Method for Boiling Range Distribution of Pe-
that will not elute completely from the gas chromatographic
troleum Distillates in Boiling Range from 174 °C to
column, leaving residues. For such samples as crude oils and
700 °C by Gas Chromatography
residues, see Test Methods D5307 and D7169.
D7096 Test Method for Determination of the Boiling Range
1.3 This test method is applicable to distillates with initial
Distribution of Gasoline by Wide-Bore Capillary Gas
boiling points above 100 ºC and final boiling points below
Chromatography
735 ºC (carbon 110); for example, distillates (IBP > 100 °C), D7169 Test Method for Boiling Point Distribution of
base oils and lubricating base stocks.
Samples with Residues Such as Crude Oils and Atmo-
spheric and Vacuum Residues by High Temperature Gas
1.4 The values stated in SI units are to be regarded as
Chromatography
standard. No other units of measurement are included in this
D7213 Test Method for Boiling Range Distribution of Pe-
standard.
troleum Distillates in the Boiling Range from 100 °C to
1.5 This standard does not purport to address all of the
615 °C by Gas Chromatography
safety concerns, if any, associated with its use. It is the
E355 Practice for Gas ChromatographyTerms 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 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D02.04.0H on Chromatographic Distribution Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2019. Published December 2019. Originally the ASTM website.
approved in 2008. Last previous edition approved in 2015 as D7500 – 15. DOI: The last approved version of this historical standard is referenced on
10.1520/D7500-15R19. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7500 − 15 (2019)
E1510 Practice for Installing Fused Silica Open Tubular 4. Summary of Test Method
Capillary Columns in Gas Chromatographs
4.1 The boiling range distribution determination by distilla-
2.2 ISO Standard:
tion is simulated by the use of gas chromatography. A
ISO 3170 Petroleum Liquids Manual Sampling
non-polar open tubular (capillary) gas chromatographic col-
umnisusedtoelutethehydrocarboncomponentsofthesample
3. Terminology
in order of increasing boiling point.
3.1 Definitions—This test method makes reference to many
4.2 A sample aliquot is diluted with a viscosity reducing
common gas chromatographic procedures, terms, and relation- solvent and introduced into the chromatographic system.
ships. For definitions of these terms used in this test method, Sample vaporization is provided by separate heating of the
refer to Practices E355, E594, and E1510. point of injection or in conjunction with column oven heating.
3.2 Definitions of Terms Specific to This Standard:
4.3 The column oven temperature is raised at a specified
3.2.1 areaslice,n—thearearesultingfromtheintegrationof linear rate to affect separation of the hydrocarbon components
the chromatographic detector signal within a specified reten- in order of increasing boiling point. The elution of sample
tiontimeinterval.Inareaslicemode(see6.4.1),peakdetection components is quantitatively determined using a flame ioniza-
parameters are bypassed and the detector signal integral is tion detector. The detector signal is recorded as area slices for
recorded as area slices of consecutive, fixed duration time consecutive retention time intervals during the analysis.
intervals.
4.4 Retentiontimesofknownnormalparaffinhydrocarbons,
3.2.2 corrected area slice, n—an area slice corrected for spanning the scope of the test method, are determined and
baseline offset by subtraction of the exactly corresponding area
correlated to their boiling point temperatures. The normalized
slice in a previously recorded blank (non-sample) analysis. cumulative corrected sample areas for each consecutive re-
corded time interval are used to calculate the boiling range
3.2.3 cumulativecorrectedarea,n—theaccumulatedsumof
distribution. The boiling point temperature at each reported
correctedareaslicesfromthebeginningoftheanalysisthrough
percent off increment is calculated from the retention time
a given retention time, ignoring any non-sample area (for
calibration.
example, solvent).
3.2.4 final boiling point (FBP), n—the temperature (corre-
5. Significance and Use
spondingtotheretentiontime)atwhichacumulativecorrected
5.1 The boiling range distribution of medium and heavy
area count equal to 99.5 % of the total sample area under the
petroleum distillate fractions provides an insight into the
chromatogram is obtained.
composition of feed stocks and products related to petroleum
3.2.5 initial boiling point (IBP), n—the temperature (corre-
refining processes (for example, hydrocracking, hydrotreating,
spondingtotheretentiontime)atwhichacumulativecorrected
visbreaking, or deasphalting). The gas chromatographic simu-
area count equal to 0.5 % of the total sample area under the
lationofthisdeterminationcanbeusedtoreplaceconventional
chromatogram is obtained.
distillation methods for control of refining operations.This test
method can be used for product specification testing with the
3.2.6 slice rate, n—the frequency used in sampling (analog)
mutual agreement of interested parties.
the chromatographic detector signal during an analysis. The
slice rate is expressed in Hz (for example integrations or slices
5.2 This test method extends the scope of boiling range
per second).
determination by gas chromatography to include distillates
3.2.7 slice time, n—the inverse function of the acquisition (IBP > 100 °C)andheavypetroleumdistillatefractionsbeyond
rate. It is the time duration of each sampling pulse usually the scope of Test Method D2887 (538 °C).
expressed in seconds. The slice time is the time at the end of
5.3 Boiling range distributions obtained by this test method
each contiguous area slice.
havenotbeenanalyzedforcorrelationtothoseobtainedbylow
3.2.8 total sample area, n—the cumulative corrected area,
efficiencydistillation,suchaswithTestMethodD86orD1160.
from the initial area point to the final area point, where the This test method does not claim agreement between these
chromatographic signal has returned to baseline after complete
physical distillations and simulated distillation. Efforts to
sample elution. resolve this question will continue. When successful resolu-
tions of the questions are determined, this test method will be
3.3 Abbreviations—Acommon abbreviation of hydrocarbon
revised accordingly.
compounds is to designate the number of carbon atoms in the
compound. A prefix is used to indicate the carbon chain form,
6. Apparatus
while a subscripted suffix denotes the number of carbon atoms
(for example n-C for normal-decane, i-C for iso- 6.1 Chromatograph—Thegaschromatographicsystemused
10 14
tetradecane).
shall have the following performance characteristics:
6.1.1 Carrier Gas Flow Control—The chromatograph shall
beequippedwithcarriergaspressureorflowcontrolcapableof
maintaining constant carrier gas flow to 61 % throughout the
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. column temperature program cycle.
D7500 − 15 (2019)
TABLE 2 Typical Operating Conditions for Gas Chromatograph
6.1.2 Column Oven—Capable of sustained and linear pro-
grammed temperature operation from near ambient (for Column length, m 5
Column internal diameter, mm 0.53
example, 30 °C to 35 °C) up to 430 °C.
Column material Metal
6.1.3 Column Temperature Programmer—The chromato-
Stationary phase type methyl silicone
graph shall be capable of linear programmed temperature Film thickness, µm 0.09 to 0.17
Initial column temperature, °C 35
operation up to 430 °C at selectable linear rates up to
Initial hold time, min 0
10 °C⁄min. The programming rate shall be sufficiently repro-
Final column temperature, °C 430
Final hold time, min 10
ducible to obtain the retention time repeatability of 0.1 min
Program rate, °C/min 10
(6 s) for each component in the calibration mixture described
Injector initial temperature, °C 100
in 7.5.
Injector final temperature, °C 430
6.1.4 Detector—This test method requires the use of a flame Injector program rate, °C/min 15
Detector temperature, °C 450
ionizationdetector(FID).Thedetectorshallmeetorexceedthe
A
Make-up gas flow, He or N2, mL/min 20
A
following specifications in accordance with Practice E594.
Hydrogen Flow, mL/min 45
A
Air Flow, mL/min 450
Check the detector according the instrument manufacturers
Carrier gas He
instructions.
Carrier gas flow rate, constant flow, mL/ 19
6.1.4.1 Operating Temperature—100 °C to 430 °C.
min
A,B
Sample size, µL 1.0
6.1.4.2 Connection of the column to the detector shall be
Sample concentration, % (m/m) 2
such that no temperature below the column temperature exists
Injector PTV or COC
between the column and the detector. Refer to Practice E1510
A
Consult with the manufacturer’s operations manual.
for proper installation and conditioning of the capillary col-
B
Monitor skewness when varying the injection volume.
umn.
6.1.5 Sample Inlet System—Any sample inlet system ca-
pable of meeting the performance specification in Annex A3
of increasing boiling point and meet the column performance
and execute the conditions of Table 2. Programmable tempera-
requirements of A3.2.1. The column shall provide a resolution
ture vaporization (PTV) and cool on-column (COC) injection
not less than 2 and not higher than 4 using the test method
systems have been used successfully.
operating conditions in Table 2.
6.2 Microsyringe—A microsyringe with a 23-gauge or
6.4 Data Acquisition System:
smaller stainless steel needle is used for on-column sample
6.4.1 Integrator/Computer System—Means shall be pro-
introduction. Syringes of 0.1 µL to 10 µL capacity are avail-
vided for determining the accumulated area under the chro-
able.
matogram. This can be done by means of an electronic
6.2.1 Automatic syringe injection is recommended to
integratororcomputer-basedchromatographydatasystem.The
achieve best precision.
integrator/computer system shall have normal chromato-
6.3 Column—This test method is limited to the use of
graphic software for measuring the retention time and areas of
non-polar wall coated open tubular (WCOT) columns of high
eluting peaks (peak processing mode). In addition, the system
thermal stability. Fused silica (aluminum coated) and stainless
shall be capable of converting the continuously integrated
steelcolumnswith0.53 mmto0.75 mminternaldiameterhave
detector signal into area slices of fixed duration (slice mode).
been successfully used. Cross-linked or bonded 100 %
These contiguous area slices, collected for the entire analysis,
dimethyl-polysiloxane stationary phases with film thickness of
are stored for later processing.Asimilar collection of contigu-
0.09 µm to 0.17 µm have been used. The column length and
ousslicesisalsocollectedfortheblankrun.Itisnecessarythat
liquid phase film thickness shall allow the elution of C n-
110 the number of slices collected for sample and blank analysis
paraffin (BP = 735 °C). The column and conditions shall
are the same. The electronic range of the integrator/computer
provide separation of typical petroleum hydrocarbons in order
(for example 1 V, 10 V) shall be operated within the linear
range of the detector/electrometer system used.
A
TABLE 1 Reference Material 5010 NOTE 1—Some gas chromatographs have an algorithm built into their
operating software that allows a mathematical model of the baseline
% Dist.
°C °F r, °C R, °C r, °F R, °F
profile to be stored in memory. This profile is automaticall
...
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