ASTM D7845-17
(Test Method)Standard Test Method for Determination of Chemical Species in Marine Fuel Oil by Multidimensional Gas Chromatography/Mass Spectrometry
Standard Test Method for Determination of Chemical Species in Marine Fuel Oil by Multidimensional Gas Chromatography/Mass Spectrometry
SIGNIFICANCE AND USE
5.1 The test method allows the quantitation of chemical species at low levels in marine fuel oils and cutter stocks. A great many types and concentrations of chemical species are found in marine fuel oils. A root cause relationship between the presence of such species or their concentration in fuels and any failure modes allegedly induced by the use of these fuels has not been established. This test method is necessary to establish test conditions required for future ISO 8217:2010 as defined in section 5.5 and Annex B item (d). Additional compounds may be determined by using the same conditions and by selecting required mass spectral selected ions, accordingly.
SCOPE
1.1 This test method covers the quantitative determination of a variety of chemical species in marine fuel oil (bunker fuel oil) by gas chromatography/mass spectrometry. By using the same conditions and by selecting required mass spectral selected ions, the test method may be used for the determination of other species than those for which precision statements and limits of detection have been established.
1.2 An example list of chemical species for which a limit of quantification has been determined by means of this test method is given in Table 1.
1.3 Other refinery hydrocarbon fractions and their mixtures may be tested using the same test method conditions. However, the precision of this test method reflects the compounds in Table 1.
1.4 Results are reported to the nearest 1.0 mg/kg.
1.5 The values stated in SI units are to be regarded as standard.
1.5.1 Exception—
1.6 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: D7845 − 17
Standard Test Method for
Determination of Chemical Species in Marine Fuel Oil by
1
Multidimensional Gas Chromatography/Mass Spectrometry
This standard is issued under the fixed designation D7845; 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* D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.1 This test method covers the quantitative determination
Measurement System Performance
of a variety of chemical species in marine fuel oil (bunker fuel
2.2 Other Standards:
oil) by gas chromatography/mass spectrometry. By using the
ISO 8217:2010 Petroleum Products—Fuels (Class F)—
same conditions and by selecting required mass spectral
3
Specifications of Marine Fuels
selected ions, the test method may be used for the determina-
tion of other species than those for which precision statements
3. Terminology
and limits of detection have been established.
3.1 Definitions:
1.2 An example list of chemical species for which a limit of
3.1.1 direct or open split interface, n—anyGC/MSinterface
quantification has been determined by means of this test
used to maintain atmospheric pressure at capillary column
method is given in Table 1.
outlet.
1.3 Other refinery hydrocarbon fractions and their mixtures
3.1.2 reconstructed ion chromatogram (RIC), n—a limited
maybetestedusingthesametestmethodconditions.However,
mass chromatogram representing the intensities of ion mass
the precision of this test method reflects the compounds in
spectrometric currents for only those ions having particular
Table 1.
mass to charge ratios used in this test method to selectively
1.4 Results are reported to the nearest 1.0 mg⁄kg.
extract and identify components in the presence of a complex
hydrocarbon matrix.
1.5 The values stated in SI units are to be regarded as
standard.
3.1.3 total ion chromatogram (TIC), n—mass spectrometer
1.5.1 Exception—Non-SI values are given for psig.
computer output representing either the summed intensities of
all scanned ion currents or a sample of the current in the ion
1.6 This standard does not purport to address all of the
beam for each spectrum scan plotted against the corresponding
safety concerns, if any, associated with its use. It is the
spectrum number.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.1.4 wall coated open tubular (WCOT), n—a type of
bility of regulatory limitations prior to use.
capillary column prepared by coating or bonding the inside
wall of the capillary with a thin film of stationary phase.
2. Referenced Documents
2
4. Summary of Test Method
2.1 ASTM Standards:
D4307 Practice for Preparation of Liquid Blends for Use as
4.1 Asuitable internal standard, ethylbenzene d-10 is added
Analytical Standards
to the sample, which is then introduced into a gas chromato-
graph equipped with two columns configured with a Deans
switching system between the two columns. The sample first
passes through the polydimethylsiloxane (WCOT) pre-column
which then performs a separation of the light hydrocarbon
1
This test method is under the jurisdiction of ASTM Committee D02 on
fractionandeliminatesthehighboilinghydrocarbonfractionto
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
vent. The compounds of interest and internal standard are
Subcommittee D02.04.0M on Mass Spectroscopy.
Current edition approved Jan. 15, 2017. Published February 2017. Originally
transferred to the high resolution polydimethylsiloxane
approved in 2013. Last previous edition approved in 2016 as D7845 – 16. DOI:
(WCOT) analytical column for chromatographic separation.
10.1520/D7845-17.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 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
1
---------------------- Page: 1 ----------------------
D7845 − 17
TABLE 1 Component Table
ture program rate must repeat to within 0.1 °C and provide
Limit of Quantitation retention time repeatability of 0.05 min throughout the tem-
mg/kg
perature program.
n-butyl alcohol 10
6.1.2 Pre-Column Colum
...
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: D7845 − 16 D7845 − 17
Standard Test Method for
Determination of Chemical Species in Marine Fuel Oil by
1
Multidimensional Gas Chromatography/Mass Spectrometry
This standard is issued under the fixed designation D7845; 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 quantitative determination of a variety of chemical species in marine fuel oil (bunker fuel oil)
by gas chromatography/mass spectrometry. By using the same conditions and by selecting required mass spectral selected ions,
the test method may be used for the determination of other species than those for which precision statements and limits of detection
have been established.
1.2 An example list of chemical species for which a limit of quantification has been determined by means of this test method
is given in Table 1.
1.3 Other refinery hydrocarbon fractions and their mixtures may be tested using the same test method conditions. However, the
precision of this test method reflects the compounds in Table 1.
1.4 Results are reported to the nearest 1.0 mg ⁄kg.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1
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
D02.04.0M on Mass Spectroscopy.
Current edition approved April 1, 2016Jan. 15, 2017. Published April 2016February 2017. Originally approved in 2013. Last previous edition approved in 20132016 as
D7845 – 13.D7845 – 16. DOI: 10.1520/D7845-16.10.1520/D7845-17.
TABLE 1 Component Table
Limit of Quantitation
mg/kg
n-butyl alcohol 10
Cyclohexanol 10
n-butyl ether 10
n-butyl acrylate 10
Styrene 10
alpha-pinene 10
Phenol 20
alpha-methyl styrene 10
beta-pinene 10
4-methyl styrene 10
trans-B-methyl styrene 10
3-methyl styrene 10
2-methyl styrene 10
Dicyclopentadiene 10
Limonene 10
Indene 20
1-phenyl ethanol 20
para, alpha-Dimethyl styrene 20
2,5 dimethyl styrene 20
2,4 dimethyl styrene 20
2-phenyl ethanol (phenylethanol) 20
2-Ethyl Phenol 50
2,4 Dimethyl Phenol 20
4-Ethyl Phenol (co elutes with 3-ethylphenol) 20
2-Phenoxy-1-propanol 50
2-Phenoxy ethanol 50
4-isopropylphenol 50
1-Phenoxy-2-Propanol 20
Styrene Glycol 50
*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
1
---------------------- Page: 1 ----------------------
D7845 − 17
1.5.1 Exception—Non-SI values are given for psig.
1.6 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
2.1 ASTM Standards:
D4307 Practice for Preparation of Liquid Blends for Use as Analytical Standards
2
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.
2
---------------------- Page: 2 ----------------------
D7845 − 17
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
2.2 Other Standards:
3
ISO 8217:2010 Petroleum Products—Fuels (Class F)—Specifications of Marine Fuels
3. Terminology
3.1 Definitions:
3.1.1 direct or open split interface, n—any GC/MS interface used to maintain atmospheric pressure at capillary column outlet.
3.1.2 reconstructed ion chromatogram (RIC), n—a limited mass chromatogram representing the intensities of ion mass
spectrometric currents for only those ions having particular mass to charge ratios used in this test method to selectively extract and
identify components in the presence of a complex hydrocarbon matrix.
3.1.3 total ion chromatogram (TIC), n—mass spectrometer computer output representing either the summed intensities of all
scanned ion currents or a sample of the current in the ion beam for each spectrum scan plotted against the corresponding spec
...
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