ASTM D7212-13
(Test Method)Standard Test Method for Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray Fluorescence Spectrometry Using a Low-Background Proportional Counter
Standard Test Method for Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray Fluorescence Spectrometry Using a Low-Background Proportional Counter
SIGNIFICANCE AND USE
5.1 This test method determines total sulfur in automotive fuels with a typical analysis time around 10 min per sample.
5.2 The quality of automotive fuel is related to the amount of sulfur present. Knowledge of sulfur level is necessary for processing purposes.
5.3 Sulfur level in automotive fuels affects performance characteristics and air quality. Federal, state, and local agencies regulate the level of sulfur in fuel delivered at the pump.
5.4 This test method can be referenced in specification documents to determine if the material meets the desired sulfur content.
5.5 If this test method is applied to petroleum matrices with significantly different composition to those used in the interlaboratory precision study, then the caution 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 the total sulfur content of automotive fuels with a concentration range from 7 mg/kg to 50 mg/kg.
1.1.1 The pooled limit of quantitation of this test method as obtained by statistical analysis of interlaboratory test results is 7 mg/kg sulfur.
1.2 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mg/kg sulfur.
1.3 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: D7212 − 13
Standard Test Method for
Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray
Fluorescence Spectrometry Using a Low-Background
1
Proportional Counter
This standard is issued under the fixed designation D7212; 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* D6792 Practice for Quality System in Petroleum Products
and Lubricants Testing Laboratories
1.1 This test method specifies an energy-dispersive X-ray
D7343 Practice for Optimization, Sample Handling,
fluorescence (EDXRF) method for the determination of the
Calibration, and Validation of X-ray Fluorescence Spec-
total sulfur content of automotive fuels with a concentration
trometry Methods for Elemental Analysis of Petroleum
range from 7 mg/kg to 50 mg/kg.
Products and Lubricants
1.1.1 The pooled limit of quantitation of this test method as
E29 Practice for Using Significant Digits in Test Data to
obtained by statistical analysis of interlaboratory test results is
Determine Conformance with Specifications
7 mg/kg sulfur.
1.2 The values stated in SI units are to be regarded as the
3. Terminology
standard. The preferred concentration units are mg/kg sulfur.
3.1 Definitions of Terms Specific to This Standard:
1.3 This standard does not purport to address all of the
3.1.1 low background proportional counter, n—an X-ray
safety concerns, if any, associated with its use. It is the
proportional counter that can suppress the noise generated
responsibility of the user of this standard to establish appro-
when incident X rays are absorbed near the wall with resulting
priate safety and health practices and determine the applica-
incomplete charge collection.
bility of regulatory limitations prior to use.
3.1.1.1 Discussion—An electrode shield close to the wall
detects incomplete charge collection and associated electronic
2. Referenced Documents
detection circuitry rejects those events. In comparison to
2
2.1 ASTM Standards:
conventional proportional counters, this gives lower spectral
D4045 Test Method for Sulfur in Petroleum Products by
background and a lower limit of detection.
Hydrogenolysis and Rateometric Colorimetry
D4057 Practice for Manual Sampling of Petroleum and
4. Summary of Test Method
Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and
4.1 The sample is placed in the beam emitted from an X-ray
Petroleum Products
source with titanium target and primary filtration so that
D6299 Practice for Applying Statistical Quality Assurance
excitation is by essentially monochromatic radiation of
and Control Charting Techniques to Evaluate Analytical
4.51 keV and virtually no background at 2.3 keV. A low
Measurement System Performance
background proportional counter measures the intensity of the
D6300 Practice for Determination of Precision and Bias fluorescent sulfur K series intensity and argon K series inten-
Data for Use in Test Methods for Petroleum Products and
sity (from residual air) and the accumulated counts are com-
Lubricants
pared with counts from previously prepared calibration stan-
dards to obtain the sulfur concentration in mg/kg. If chlorine is
expected to be present in some samples then other regions of
1
the spectrum must be measured to provide compensation for
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
spectral overlap. One group of calibration standards is required
D02.03 on Elemental Analysis.
to span the concentration range from 0 to 150 mg/kg sulfur.
Current edition approved June 15, 2013. Published August 2013. Originally
NOTE 1—Operation of analyzers using X-ray tubes is to be conducted
approved in 2006. Last previous edition approved in 2007 as D7212 – 07. DOI:
in accordance with the manufacturer’s safety instructions and federal,
10.1520/D7212-13.
2
state, and local regulations governing the use of ionizing radiation.
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
4.2 Practice D7343 should be consulted regarding standard
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. operating protocols in XRF analysis.
*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 ----------------------
D7212 − 13
5. Significance and Use rays and spectral overlap), spectral overlap correct
...
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: D7212 − 07 D7212 − 13
Standard Test Method for
Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray
Fluorescence Spectrometry Using a Low-Background
1
Proportional Counter
This standard is issued under the fixed designation D7212; 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 specifies an energy-dispersive X-ray fluorescence (EDXRF) method for the determination of the total
sulfur content of automotive fuels with a concentration range from 7 mg/kg to 50 mg/kg.
1.1.1 The pooled limit of quantitation of this test method as obtained by statistical analysis of interlaboratory test results is 7
mg/kg sulfur.
1.2 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mg/kg sulfur.
1.3 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:
D4045 Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
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 Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants
D6792 Practice for Quality System in Petroleum Products and Lubricants Testing Laboratories
D7343 Practice for Optimization, Sample Handling, Calibration, and Validation of X-ray Fluorescence Spectrometry Methods
for Elemental Analysis of Petroleum Products and Lubricants
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 low background proportional counter, n—an X-ray proportional counter that can suppress the noise generated when
incident X rays are absorbed near the wall with resulting incomplete charge collection.
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 May 1, 2007June 15, 2013. Published June 2007August 2013. Originally approved in 2006. Last previous edition approved in 20062007 as
D7212D7212 – 07.–06. DOI: 10.1520/D7212-07.10.1520/D7212-13.
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.
3.1.1.1 Discussion—
An electrode shield close to the wall detects incomplete charge collection and associated electronic detection circuitry rejects those
events. In comparison to conventional proportional counters, this gives lower spectral background and a lower limit of detection.
*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 ----------------------
D7212 − 13
4. Summary of Test Method
4.1 The sample is placed in the beam emitted from an X-ray source with titanium target and primary filtration so that excitation
is by essentially monochromatic radiation of 4.51 keV and virtually no background at 2.3 keV. A low background proportional
counter measures the intensity of the fluorescent sulfur K series intensity and argon K series intensity (from residual air) and the
accumulated counts are compared with counts from previously prepared calibration standards to obtain the sulfur concentration
in mg/kg. If chlorine is expected to be present in some samples then other regions of the spectrum must be measured to provide
compensation for spectral overlap. One group of calibration standards is required to span the concentration range from 0 to 150
mg/kg sulfur.
NOTE 1—Operation of analyzers using X-ray tubes
...
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