ASTM D7398-11(2016)
(Test Method)Standard Test Method for Boiling Range Distribution of Fatty Acid Methyl Esters (FAME) in the Boiling Range from 100 °C to 615 °C by Gas Chromatography
Standard Test Method for Boiling Range Distribution of Fatty Acid Methyl Esters (FAME) in the Boiling Range from 100 °C to 615 °C by Gas Chromatography
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Designation: D7398 − 11 (Reapproved 2016)
Standard Test Method for
Boiling Range Distribution of Fatty Acid Methyl Esters
(FAME) in the Boiling Range from 100 °C to 615 °C by Gas
Chromatography
This standard is issued under the fixed designation D7398; 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
1.1 Thistestmethodcoversthedeterminationoftheboiling 2.1 ASTM Standards:
rangedistributionoffattyacidmethylesters(FAME).Thistest D86Test Method for Distillation of Petroleum Products and
method is applicable to FAMES (biodiesel, B100) having an Liquid Fuels at Atmospheric Pressure
initial boiling point greater than 100°C and a final boiling D1160TestMethodforDistillationofPetroleumProductsat
point less than 615°C at atmospheric pressure as measured by Reduced Pressure
this test method. D2887Test Method for Boiling Range Distribution of Pe-
troleum Fractions by Gas Chromatography
1.2 The test method can also be applicable to blends of
D2892Test Method for Distillation of Crude Petroleum
diesel and biodiesel (B1 through B100), however precision for
(15-Theoretical Plate Column)
these samples types has not been evaluated.
D4626Practice for Calculation of Gas Chromatographic
1.3 The test method is not applicable for analysis of
Response Factors
petroleum containing low molecular weight components (for
D6352Test Method for Boiling Range Distribution of Pe-
example naphthas, reformates, gasolines, crude oils).
troleum Distillates in Boiling Range from 174°C to
1.4 Boiling range distributions obtained by this test method 700°C by Gas Chromatography
D6751Specification for Biodiesel Fuel Blend Stock (B100)
are not equivalent to results from low efficiency distillation
such as those obtained with Test Method D86 or D1160, for Middle Distillate Fuels
especially the initial and final boiling points. D7213Test Method for Boiling Range Distribution of Pe-
troleum Distillates in the Boiling Range from 100°C to
1.5 This test method uses the principles of simulated distil-
615°C by Gas Chromatography
lation methodology. See Test Methods D2887, D6352, and
E355PracticeforGasChromatographyTermsandRelation-
D7213.
ships
1.6 The values stated in SI units are to be regarded as
E594Practice for Testing Flame Ionization Detectors Used
standard. The values given in parentheses are for information
in Gas or Supercritical Fluid Chromatography
only.
E1510Practice for Installing Fused Silica Open Tubular
1.7 This standard does not purport to address all of the Capillary Columns in Gas Chromatographs
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions:
priate safety and health practices and determine the applica-
3.1.1 This test method makes reference to many common
bility of regulatory limitations prior to use.
gas chromatographic procedures, terms, and relationships.
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 April 1, 2016. Published May 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2007. Last previous edition approved in 2011 as D7398–11. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7398-11R16. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7398 − 11 (2016)
3.1.2 biodiesel, n—fuel composed of mono-alkyl esters of 4. Summary of Test Method
long chain fatty acids derived from vegetable oils or animal
4.1 The boiling range distribution by distillation is simu-
fats, designated B100.
lated by the use of gas chromatography. A non-polar open
3.2 Definitions of Terms Specific to This Standard: tubular(capillary)gaschromatographiccolumnisusedtoelute
thehydrocarbonandFAMEcomponentsofthesampleinorder
3.2.1 areaslice,n—arearesultingfromtheintegrationofthe
of increasing boiling point.
chromatographic detector signal within a specified retention
time interval. In area slice mode (6.4.2), peak detection
4.2 A sample aliquot is diluted with a viscosity reducing
parameters are bypassed and the detector signal integral is
solvent and introduced into the chromatographic system. The
recorded as area slices of consecutive, fixed duration time
solvent shall be apolar and not interfere with measurement of
intervals.
thesampleinthe100°Cto615°Crange.Samplevaporization
is provided by separate heating of the point of injection or in
3.2.2 atmospheric equivalent temperature (AET),
conjunction with column oven heating.
n—temperature converted from the measured vapor tempera-
ture obtained at sub-ambient pressure to atmospheric equiva-
4.3 Thecolumnoventemperatureisraisedatareproducible
lenttemperature(AET)correspondingtotheequivalentboiling
linear rate to effect separation of the FAME components in
point at atmospheric pressure, 101.3kPa (760mm Hg), The
order of increasing boiling point relative to a n-paraffin
AET is the expected distillate temperature if the distillation
calibration mixture. The elution of sample components is
was performed at atmospheric pressure and there was no
quantitatively determined using a flame ionization detector.
thermal decomposition.
The detector signal integral is recorded as area slices for
consecutive retention time intervals during the analysis.
3.2.3 corrected area slice, n—area slice corrected for base-
line offset, by subtraction of the exactly corresponding area
4.4 Retentiontimesofknownnormalparaffinhydrocarbons,
slice in a previously recorded blank (non-sample) analysis.
spanning the scope of the test method (C –C ), are deter-
5 60
mined and correlated to their boiling point temperatures. The
3.2.4 cumulative corrected area, n—accumulated sum of
normalized cumulative corrected sample areas for each con-
correctedareaslicesfromthebeginningoftheanalysisthrough
secutiverecordedtimeintervalareusedtocalculatetheboiling
a given retention time, ignoring any non-sample area (for
range distribution. The boiling point temperature at each
example, solvent).
reported percent off increment is calculated from the retention
3.2.5 initial boiling point (IBP), n—temperature (corre-
time calibration.
spondingtotheretentiontime)atwhichacumulativecorrected
4.5 The retention time versus boiling point curve is cali-
area count equal to 0.5% of the total sample area under the
brated with normal paraffin hydrocarbons since these boiling
chromatogram is obtained.
points are well defined. A mixture of FAMEs is analyzed to
3.2.6 final boiling point (FBP), n—temperature (corre-
check column resolution. A triglyceride is analyzed to verify
spondingtotheretentiontime)atwhichacumulativecorrected
the system’s ability to detect unreacted oil.
area count equal to 99.5% of the total sample area under the
chromatogram is obtained.
5. Significance and Use
3.2.7 slice rate, n—frequency of data sampling or the
5.1 The boiling range distribution of FAMES provides an
frequencyofdatabunchingprovidedthatthefrequencyofdata
insight into the composition of product related to the transes-
acquisition is larger than the frequency of bunching. The unit
terificationprocess.Thisgaschromatographicdeterminationof
of frequency is points/seconds or Hz.
boiling range can be used to replace conventional distillation
3.2.8 slice time, n—cumulative slice rate (analysis time)
methods for product specification testing with the mutual
associatedwitheachareaslicethroughoutthechromatographic
agreement of interested parties.
analysis. The slice time is the time at the end of each
5.2 Biodiesel (FAMES) exhibits a boiling point rather than
contiguous area slice.
a distillation curve. The fatty acid chains in the raw oils and
3.2.9 total sample area, n—cumulative corrected area, from
fats from which biodiesel is produced are mainly comprised of
the initial point to the final area point.
straight chain hydrocarbons with 16 to 18 carbons that have
similar boiling temperatures. The atmospheric boiling point of
3.3 Abbreviations:
biodiesel generally ranges from 330°C to 357°C. The Speci-
3.3.1 Acommonabbreviationofhydrocarboncompoundsis
fication D6751 value of 360°C max at 90% off by Test
to designate the number of carbon atoms in the compound. A
MethodD1160wasincorporatedasanprecautiontoensurethe
prefix is used to indicate the carbon chain form, while a
fuel has not been adulterated with high boiling contaminants.
subscripted suffix denotes the number of carbon atoms (for
example, normal decane n-C ; iso-tetradecane = i-C ).
10 14
6. Apparatus
3.3.2 A common abbreviation for FAME compounds is to
designate the number of carbon atoms and number of double 6.1 Chromatograph—The following gas chromatographic
bonds in the compound. The number of carbon atoms is system performance characteristics are required:
denoted by a number after the “C” and the number following 6.1.1 Column Oven—Capable of sustained and linear pro-
a colon indicates the number of double bonds (for example, grammed temperature operation from near ambient (for ex-
C16:2 ; FAME with 16 carbon atoms and 2 double bonds). ample 35°C to 50°C) up to 400°C.
D7398 − 11 (2016)
6.1.2 Column Temperature Programmer—The chromato- done by means of an electronic integrator or computer based
graph must be capable of linear programmed temperature chromatography data system. The integrator/computer system
operation up to 400°C at selectable linear rates up to shall have normal chromatographic software for measuring the
20°C⁄min. The programming rate must be sufficiently repro- retention time and areas of eluting peaks (peak detection
ducible to obtain the retention time repeatability of 0.03min mode). In addition, the system shall be capable of converting
(3s) for each component in the calibration mixture described the continuously integrated detector signal into area slices of
in 7.3. fixed duration (area slice mode). These contiguous area slices,
6.1.3 Detector—This test method requires a flame ioniza- collectedfortheentireanalysis,arestoredforlaterprocessing.
The electronic range of the integrator/computer (for example,
tion detector (FID). The detector must meet or exceed the
following specifications as detailed in Practice E594. The 1V, 10V) shall be operated within the linear range of the
detector/electrometer system used.
specification of flame jet orifice is approximately 0.45mm
(0.018in.).
NOTE 1—Some gas chromatographs have an algorithm built into their
6.1.3.1 Operating Temperature, 400°C.
operating software that allows a mathematical model of the baseline
6.1.3.2 Sensitivity, >0.005 coulombs/g carbon. profile to be stored in memory. This profile is automatically subtracted
-11
from the detector signal on subsequent sample runs to compensate for the
6.1.3.3 Minimum Detectability,1×10 g carbon / s.
column bleed. Some integration systems also store and automatically
6.1.3.4 Linear Range, >10
subtract a blank analysis from subsequent analytical determinations.
6.1.3.5 Connection of the column to the detector must be
such that no temperature below the column temperature exists. 7. Reagents and Materials
Refer to Practice E1510 for proper installation and condition-
7.1 Gases—Thefollowingcompressedgasesareutilizedfor
ing of the capillary column.
the operation of the gas chromatograph.
6.1.4 Sample Inlet System—Any sample inlet system ca-
7.1.1 Helium, 99.999%. (Warning—Compressed gas un-
pableofmeetingtheperformancespecificationin6.1.5and7.3
der high pressure.) This gas can be used as carrier gas. Ensure
may be used. Programmed temperature vaporization (PTV)
sufficient pressure for a constant carrier gas flow rate. It is not
and programmable cool on-column injection systems have
to contain more than 5mL⁄m of oxygen and the total amount
been used successfully.
of impurities are not to exceed 10mL⁄m .
6.1.5 Carrier Gas Flow Control—The chromatograph shall
7.1.2 Nitrogen, 99.999%. (Warning—Compressed gas un-
be equipped with carrier flow control capable of maintaining
der high pressure.) This gas can be used as carrier gas. Ensure
constant carrier gas flow control through the column through-
sufficient pressure for a constant carrier gas flow rate. It is not
out the column temperature program cycle as measured with
to contain more than 5mL⁄m of oxygen and the total amount
the use of flow a sensor. Flow rate must be maintained within
of impurities are not to exceed 10mL⁄m .
1% through out the temperature program.
7.1.3 Hydrogen, 99.999%. (Warning—Extremely flam-
mable gas under high pressure.) The total impurities are not to
6.2 Microsyringe—A microsyringe with a 23 gauge or
exceed 10 mL/m . This gas can be used as carrier gas. Ensure
smaller stainless steel needle is used for on-column sample
sufficient pressure for a constant carrier gas flow rate. It is also
introduction. Syringes of 0.1µL to 10µL capacity are avail-
used as fuel for the flame ionization detector (FID).
able.
7.1.4 Air, 99.999%. (Warning—Compressed gas under
6.2.1 Automatic syringe injection is recommended to
high pressure and supports combustion.) Total impurities are
achieve best precision.
not to exceed 10mL⁄m . This gas is used to sustain combus-
6.3 Column—This test method is limited to the use of
tion in the flame ionization detector (FID).
non-polar wall coated open tubular (WCOT) columns of high
7.2 Solvents—Unless otherwise indicated, it is intended that
thermal stability. Glass, fused silica, and stainless steel
all solvents conform to the specifications of the committee on
columns, with a 0.53mm diameter have been successfully
analytical Reagents of the American Chemical Society where
used. Cross-linked or bonded 100% dimethyl-polysiloxane
such specifications are available. Other grades may be used
stationary phases with film thickness of 0.5µm to 1.0µm have
provided it is first ascertained that the solvent is of sufficiently
been used. The column length and liquid phase film thickness
high purity to permit its use without lessening the accuracy of
shall allow the elution of at least C n-paraffin (BP = 615°C)
the determination.
and triolein. The column and conditions shall provide separa-
7.2
...
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: D7398 − 11 D7398 − 11 (Reapproved 2016)
Standard Test Method for
Boiling Range Distribution of Fatty Acid Methyl Esters
(FAME) in the Boiling Range from 100100 °C to 615°C615 °C
by Gas Chromatography
This standard is issued under the fixed designation D7398; 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 fatty acid methyl esters (FAME). This test
method is applicable to FAMES (biodiesel, B100) 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 can also be applicable to blends of diesel and biodiesel (B1 through B100), however precision for these
samples types has not been evaluated.
1.3 The test method is not applicable for analysis of petroleum containing low molecular weight components (for example
naphthas, reformates, gasolines, crude oils).
1.4 Boiling range distributions obtained by this test method are not equivalent to results from low efficiency distillation such
as those obtained with Test Method D86 or D1160, especially the initial and final boiling points.
1.5 This test method uses the principles of simulated distillation methodology. See Test Methods D2887, D6352, and D7213.
1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.7 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 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
D6751 Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels
D7213 Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100 °C to 615 °C by 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
3. Terminology
3.1 Definitions:
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 Oct. 1, 2011April 1, 2016. Published November 2011May 2016. Originally approved in 2007. Last previous edition approved in 20072011 as
D7398D7398 – 11.-07. DOI: 10.1520/D7398-11.10.1520/D7398-11R16.
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
D7398 − 11 (2016)
3.1.1 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.
3.1.2 biodiesel, n—fuel composed of mono-alkyl esters of long chain fatty acids derived from vegetable oils or animal fats,
designated B100.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 area slice, n—area resulting from the integration of the chromatographic detector signal within a specified retention time
interval. In area slice mode (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 atmospheric equivalent temperature (AET), n—temperature converted from the measured vapor temperature obtained at
sub-ambient pressure to atmospheric equivalent temperature (AET) corresponding to the equivalent boiling point at atmospheric
pressure, 101.3 kPa (760 mm 101.3 kPa (760 mm Hg), The AET is the expected distillate temperature if the distillation was
performed at atmospheric pressure and there was no thermal decomposition.
3.2.3 corrected area slice, n—area slice corrected for baseline offset, by subtraction of the exactly corresponding area slice in
a previously recorded blank (non-sample) analysis.
3.2.4 cumulative corrected area, n—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).
3.2.5 initial boiling point (IBP), n—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 final boiling point (FBP), n—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.
3.2.7 slice rate, n—frequency of data sampling or the frequency of data bunching provided that the frequency of data acquisition
is larger than the frequency of bunching. The unit of frequency is points/seconds or Hz.
3.2.8 slice time, n—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.
3.2.9 total sample area, n—cumulative corrected area, from the initial point to the final area point.
3.3 Abbreviations:
3.3.1 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 ).
10 14
3.3.2 A common abbreviation for FAME compounds is to designate the number of carbon atoms and number of double bonds
in the compound. The number of carbon atoms is denoted by a number after the “C” and the number following a colon indicates
the number of double bonds (for example, C16:2 ; FAME with 16 carbon atoms and 2 double bonds).
4. Summary of Test Method
4.1 The boiling range distribution 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 and FAME 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. The solvent
shall be apolar and not interfere with measurement of the sample in the 100100 °C to 615°C615 °C range. 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 FAME components in order
of increasing boiling point relative to a n-paraffin calibration mixture. 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 the test method (C – C ), are determined
5 60
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.
4.5 The retention time versus boiling point curve is calibrated with normal paraffin hydrocarbons since these boiling points are
well defined. A mixture of FAMEs is analyzed to check column resolution. A triglyceride is analyzed to verify the system’s ability
to detect unreacted oil.
5. Significance and Use
5.1 The boiling range distribution of FAMES provides an insight into the composition of product related to the transesterifi-
cation process. This gas chromatographic determination of boiling range can be used to replace conventional distillation methods
for product specification testing with the mutual agreement of interested parties.
D7398 − 11 (2016)
5.2 Biodiesel (FAMES) exhibits a boiling point rather than a distillation curve. The fatty acid chains in the raw oils and fats
from which biodiesel is produced are mainly comprised of straight chain hydrocarbons with 16 to 18 carbons that have similar
boiling temperatures. The atmospheric boiling point of biodiesel generally ranges from 330330 °C to 357°C.357 °C. The
Specification D6751 value of 360°C360 °C max at 90 % off by Test Method D1160 was incorporated as an precaution to ensure
the fuel has not been adulterated with high boiling contaminants.
6. Apparatus
6.1 Chromatograph—The following gas chromatographic system performance characteristics are required:
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 must 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 must be sufficiently reproducible to
obtain the retention time repeatability of 0.03 min (3 s) 0.03 min (3 s) for each component in the calibration mixture described in
7.3.
6.1.3 Detector—This test method requires a flame ionization detector (FID). The detector must meet or exceed the following
specifications as detailed in Practice E594. The specification of flame jet orifice is approximately 0.45 mm (0.018 in.).0.45 mm
(0.018 in.).
6.1.3.1 Operating Temperature, 400°C.400 °C.
6.1.3.2 Sensitivity, >0.005 coulombs/ g 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 must 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 6.1.5 and 7.3 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 flow control capable of maintaining
constant carrier gas flow control through the column throughout the column temperature program cycle as measured with the use
of flow a sensor. Flow rate must be maintained within 1 % through out the temperature program.
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 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 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 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) and
triolein. The column and conditions shall provide separation of typical petroleum hydrocarbons and saturated FAMES in order of
increasing boiling point and meet the column resolution requirements of 8.2.1. The column shall provide a resolution between five
(5) and fifteen (15) using the test method operating conditions.
6.4 Data Acquisition System:
6.4.1 Recorder—A 00 mV to 1 mV 1 mV range recording potentiometer or equivalent, with a full-scale response time of 2 s
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) 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 Gases—The following compressed gases are utilized for the operation of the gas chromatograph.
7.1.1 Helium, 99.999 %. (Warning—Compressed gas under high pressure.) This gas can be used as carrier gas. Ensure
suffic
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