ASTM D7220-12
(Test Method)Standard Test Method for Sulfur in Automotive, Heating, and Jet Fuels by Monochromatic Energy Dispersive X-ray Fluorescence Spectrometry
Standard Test Method for Sulfur in Automotive, Heating, and Jet Fuels by Monochromatic Energy Dispersive X-ray Fluorescence Spectrometry
SIGNIFICANCE AND USE
This test method provides measurement of total sulfur in automotive, No. 2 heating, and jet fuels with a minimum of sample preparation. A typical analysis time is 180 to 360 s per sample.
The quality of automotive, No. 2 heating, and jet fuel can be related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuel.
If this test method is applied to petroleum materials with matrices significantly different from the calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting the results.
SCOPE
1.1 This test method specifies an energy-dispersive X-ray fluorescence (EDXRF) method for the determination of total sulfur in automotive, No. 2 heating, and jet fuels with a concentration range of 3 to 942 mg/kg.
1.1.1 The pooled limit of quantitation of this test method as obtained by statistical analysis of inter laboratory test results is 3 mg/kg sulfur.
1.1.2 This test method is applicable to gasoline, oxygen enriched gasoline (RFG), diesel, diesel/biodiesel blends containing up to twenty volume percent biodiesel, kerosene, jet fuel, jet fuel/biodiesel blends containing up to five volume percent biodiesel and No. 2 home heating oil.
1.2 A fundamental assumption in this test method is that the standard and sample matrix is well matched. Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other heteroatoms.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 The preferred concentration units are mg/kg sulfur.
1.4 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: D7220 − 12
Standard Test Method for
Sulfur in Automotive, Heating, and Jet Fuels by
Monochromatic Energy Dispersive X-ray Fluorescence
1
Spectrometry
This standard is issued under the fixed designation D7220; 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 D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.1 This test method specifies an energy-dispersive X-ray
D6299 Practice for Applying Statistical Quality Assurance
fluorescence (EDXRF) method for the determination of total
and Control Charting Techniques to Evaluate Analytical
sulfur in automotive, No. 2 heating, and jet fuels with a
Measurement System Performance
concentration range of 3 to 942 mg/kg.
D6300 Practice for Determination of Precision and Bias
1.1.1 The pooled limit of quantitation of this test method as
Data for Use in Test Methods for Petroleum Products and
obtained by statistical analysis of inter laboratory test results is
Lubricants
3 mg/kg sulfur.
E29 Practice for Using Significant Digits in Test Data to
1.1.2 This test method is applicable to gasoline, oxygen
Determine Conformance with Specifications
enriched gasoline (RFG), diesel, diesel/biodiesel blends con-
taining up to twenty volume percent biodiesel, kerosene, jet
3. Terminology
fuel, jet fuel/biodiesel blends containing up to five volume
percent biodiesel and No. 2 home heating oil. 3.1 Definitions:
3.1.1 monochromatic X-radiation, n—an incident X-ray
1.2 Afundamental assumption in this test method is that the
beam on a sample having a selected photon energy with a
standard and sample matrix is well matched. Matrix mismatch
narrow energy bandwidth of 65% relative to the selected
can be caused by C/H ratio differences between samples and
energy.
standards or by the presence of other heteroatoms.
3.1.1.1 Discussion—Monochromatic X-ray radiation in
1.3 The values stated in SI units are to be regarded as
EDXRFinstrumentationcanbeobtainedbyusingBraggoptics
standard. No other units of measurement are included in this
(at an angle ofè=45 6 5°, in the low energy range). Bragg
standard.
optics (monochromators) create very intense mono-energetic
1.3.1 The preferred concentration units are mg/kg sulfur.
radiation. A combination of a selected X-ray tube (typically a
1.4 This standard does not purport to address all of the
Pd or Ag anode) with a highly ordered pyrolytic graphite
safety concerns, if any, associated with its use. It is the
(HOPG) Bragg optic can be used to create monochromatic
responsibility of the user of this standard to establish appro-
radiationofthecharacteristicradiationoftheanodematerialof
priate safety and health practices and determine the applica-
the X-ray tube. The use of such radiation for sample excitation
bility of regulatory limitations prior to use.
resultsinincreasedsensitivityforthedeterminationofsulfurin
petroleum products.
2. Referenced Documents
2 3.2 Abbreviations:
2.1 ASTM Standards:
3.2.1 DBS—actual mass of Di-n-butyl sulfide, g
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
3.2.2 Kcps—kilo-counts per second.
3.2.3 EDXRF—Energy dispersive X-ray spectrometry
1
This test method is under the jurisdiction of ASTM Committee D02 on
3.2.4 PTFE—Polytetrafluorethylene
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.03 on Elemental Analysis.
3.2.5 SDBS—mass % of sulfur in Di-n-butyl sulfide, typi-
Current edition approved Jan. 15, 2012. Published March 2012. Originally
cally 21.91%
approved in 2006. Last previous edition approved in 2006 as D7220–06. DOI:
10.1520/D7220-12.
3.2.6 SStd—mg/kg sulfur in the calibration standard
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
3.2.7 SStock—mg/kg of sulfur in the stock standard
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 3.2.8 STK—actual mass of stock standard, g
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7220 − 12
4. Summary of Test Method 7. Apparatus
4.1 ThesampleisplacedinthemonochromaticX-raybeam, 7.1 Monochromatic X-ray Fluorescence Analyzer—A
and the peak area of the sulfur Kα line at 2.307 keV is Monochromatic Excitation Energy Dispersive XRF spectrom-
measured. The background spectrum, measured with a sulfur eter may be used if its design incorporates as a minimum, the
free white oil or other matrix matching blank sam
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D7220–06 Designation:D7220–12
Standard Test Method for
Sulfur in Automotive Fuels by Polarization X-ray
Fluorescence SpectrometrySulfur in Automotive, Heating,
and Jet Fuels by Monochromatic Energy Dispersive X-ray
1
Fluorescence Spectrometry
This standard is issued under the fixed designation D7220; 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
1.1This test method specifies an energy-dispersive X-ray fluorescence (EDXRF) method for the determination of total sulfur in
automotive fuels with a concentration range of 6 mg/kg to 50 mg/kg.
1.1.1The pooled limit of quantitation of this test method as obtained by statistical analysis of inter laboratory test results is
6mg/kg sulfur.
1.1 This test method specifies an energy-dispersive X-ray fluorescence (EDXRF) method for the determination of total sulfur
in automotive, No. 2 heating, and jet fuels with a concentration range of 3 to 942 mg/kg.
1.1.1 The pooled limit of quantitation of this test method as obtained by statistical analysis of inter laboratory test results is
3 mg/kg sulfur.
1.1.2 This test method is applicable to gasoline, oxygen enriched gasoline (RFG), diesel, diesel/biodiesel blends containing up
to twenty volume percent biodiesel, kerosene, jet fuel, jet fuel/biodiesel blends containing up to five volume percent biodiesel and
No. 2 home heating oil.
1.2 Afundamental assumption in this test method is that the standard and sample matrix is well matched. Matrix mismatch can
be caused by C/H ratio differences between samples and standards or by the presence of other heteroatoms.
1.3The values stated in SI units are to be regarded as the standard. The preferred concentration units are mg/kg sulfur.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3.1 The preferred concentration units are mg/kg sulfur.
1.4 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
Elemental Analysis.
Current edition approved Feb. 15, 2006. Published March 2006. DOI: 10.1520/D7220-06.
Current edition approved Jan. 15, 2012. Published March 2012. Originally approved in 2006. Last previous edition approved in 2006 as D7220–06. DOI:
10.1520/D7220-12.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D7220–12
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
2.2 ISO Standard:
ISO 4259Determination and application of precision data in relation to methods of test
3. Terminology
3.1 Definitions:
3.1.1 polarization X-ray fluorescencemonochromatic X-radiation, n—typically a polarization EDXRF instrument is used. In
difference to direct excitation EDXRF spectrometry, polarization X-ray fluorescence uses polarized radiation for excitation.
Combined with Cartesian geometry (of excitation, sample and detection system) this results in a significant improvement of the
detection limit compared to direct excitation EDXRF. —an incident X-ray beam on a sample having a selected photon energy with
a narrow energy bandwidth of 65% relative to the selected energy.
3.1.1.1 Discussion—Monochromatic X-ray radiation in EDXRF instrumentation can be obtained by using Bragg optics (at an
angle ofè=45 6 5°, in the low energy range). Bragg optics (monochromators) create very intense mono-energetic radiation. A
combination of a se
...
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