ASTM D5453-12
(Test Method)Standard Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
Standard Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
SIGNIFICANCE AND USE
4.1 Some process catalysts used in petroleum and chemical refining can be poisoned when trace amounts of sulfur bearing materials are contained in the feedstocks. This test method can be used to determine sulfur in process feeds sulfur in finished products, and can also be used for purposes of regulatory control.
SCOPE
1.1 This test method covers the determination of total sulfur in liquid hydrocarbons, boiling in the range from approximately 25 to 400°C, with viscosities between approximately 0.2 and 20 cSt (mm 2/S) at room temperature.
1.2 Three separate interlaboratory studies (ILS) on precision, and three other investigations that resulted in an ASTM research report, have determined that this test method is applicable to naphthas, distillates, engine oil, ethanol, Fatty Acid Methyl Ester (FAME), and engine fuel such as gasoline, oxygen enriched gasoline (ethanol blends, E-85, M-85, RFG), diesel, biodiesel, diesel/biodiesel blends, and jet fuel. Samples containing 1.0 to 8000 mg/kg total sulfur can be analyzed (Note 1).Note 1—Estimates of the pooled limit of quantification (PLOQ) for the precision studies were calculated. Values ranged between less than 1.0 and less than 5.0 mg/kg (see Section 8 and 15.1).
1.3 This test method is applicable for total sulfur determination in liquid hydrocarbons containing less than 0.35 % (m/m) halogen(s).
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 and health practices and determine the applicability of regulatory limitations prior to use. For warning statements, see 3.1, 6.3, 6.4, Section 7, and 8.1.
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Designation: D5453 − 12
StandardTest Method for
Determination of Total Sulfur in Light Hydrocarbons, Spark
Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by
1
Ultraviolet Fluorescence
This standard is issued under the fixed designation D5453; 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
2
1.1 Thistestmethodcoversthedeterminationoftotalsulfur 2.1 ASTM Standards:
in liquid hydrocarbons, boiling in the range from approxi- D1298Test Method for Density, Relative Density, or API
mately 25 to 400°C, with viscosities between approximately Gravity of Crude Petroleum and Liquid Petroleum Prod-
2
0.2 and 20 cSt (mm /S) at room temperature. ucts by Hydrometer Method
D4052Test Method for Density, Relative Density, and API
1.2 Three separate interlaboratory studies (ILS) on
Gravity of Liquids by Digital Density Meter
precision, and three other investigations that resulted in an
D4057Practice for Manual Sampling of Petroleum and
ASTMresearchreport,havedeterminedthatthistestmethodis
Petroleum Products
applicable to naphthas, distillates, engine oil, ethanol, Fatty
D4177Practice for Automatic Sampling of Petroleum and
Acid Methyl Ester (FAME), and engine fuel such as gasoline,
Petroleum Products
oxygen enriched gasoline (ethanol blends, E-85, M-85, RFG),
D6299Practice for Applying Statistical Quality Assurance
diesel, biodiesel, diesel/biodiesel blends, and jet fuel. Samples
and Control Charting Techniques to Evaluate Analytical
containing 1.0 to 8000 mg/kg total sulfur can be analyzed
Measurement System Performance
(Note 1).
3. Summary of Test Method
NOTE1—Estimatesofthepooledlimitofquantification(PLOQ)forthe
precisionstudieswerecalculated.Valuesrangedbetweenlessthan1.0and
3.1 A hydrocarbon sample is either directly injected or
less than 5.0 mg/kg (see Section 8 and 15.1).
placedinasampleboat.Thesampleorboat,orboth,isinserted
1.3 This test method is applicable for total sulfur determi-
into a high temperature combustion tube where the sulfur is
nation in liquid hydrocarbons containing less than 0.35%
oxidizedtosulfurdioxide(SO )inanoxygenrichatmosphere.
2
(m⁄m) halogen(s).
Water produced during the sample combustion is removed and
1.4 The values stated in SI units are to be regarded as the sample combustion gases are next exposed to ultraviolet
standard. No other units of measurement are included in this (UV) light.The SO absorbs the energy from the UVlight and
2
standard. isconvertedtoexcitedsulfurdioxide(SO *).Thefluorescence
2
emitted from the excited SO * as it returns to a stable state,
2
1.5 This standard does not purport to address all of the
SO , is detected by a photomultiplier tube and the resulting
2
safety concerns, if any, associated with its use. It is the
signal is a measure of the sulfur contained in the sample.
responsibility of the user of this standard to establish appro-
(Warning—Exposure to excessive quantities of ultraviolet
priate safety and health practices and determine the applica-
(UV) light is injurious to health. The operator must avoid
bility of regulatory limitations prior to use. For warning
exposing any part of their person, especially their eyes, not
statements, see 3.1, 6.3, 6.4, Section 7, and 8.1.
only to direct UV light but also to secondary or scattered
radiation that is present.)
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
2
Subcommittee D02.03 on Elemental Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2012. Published February 2013. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2009 as D5453–09. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5453-12. 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
1
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D5453 − 12
FIG. 1 Conventional Combustion Tubes
4. Significance and Use 5.4 Drier Tube—The apparatus must be equipped with a
mechanism for the removal of water vapor. The oxidation
4.1 Some process catalysts used in petroleum and chemical
reaction produces water vapor which must be eliminated prior
refining can be poisoned when trace amounts of sulfur bearing
tomeasurementbythedetector.Thiscanbeaccomplishedwith
materials a
...
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: D5453 − 09 D5453 − 12
Standard Test Method for
Determination of Total Sulfur in Light Hydrocarbons, Spark
Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by
1
Ultraviolet Fluorescence
This standard is issued under the fixed designation D5453; 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 determination of total sulfur in liquid hydrocarbons, boiling in the range from approximately
2
25 to 400°C, with viscosities between approximately 0.2 and 20 cSt (mm /S) at room temperature.
1.2 Three separate interlaboratory studies (ILS) on precision, and three other investigations that resulted in an ASTM research
report, have determined that this test method is applicable to naphthas, distillates, engine oil, ethanol, Fatty Acid Methyl Ester
(FAME), and engine fuel such as gasoline, oxygen enriched gasoline (ethanol blends, E-85, M-85, RFG), diesel, biodiesel,
diesel/biodiesel blends, and jet fuel. Samples containing 1.0 to 8000 mg/kg total sulfur can be analyzed (Note 1).
NOTE 1—Estimates of the pooled limit of quantification (PLOQ) for the precision studies were calculated. Values ranged between less than 1.0 and
less than 5.0 mg/kg (see Section 8 and 15.1).
1.3 This test method is applicable for total sulfur determination in liquid hydrocarbons containing less than 0.35 % (m/m)
halogen(s).
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 and health practices and determine the applicability of regulatory
limitations prior to use. For warning statements, see 3.1, 6.3, 6.4, Section 7, and 8.1.
2. Referenced Documents
2
2.1 ASTM Standards:
D1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products by
Hydrometer Method
D4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter
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
3. Summary of Test Method
3.1 A hydrocarbon sample is either directly injected or placed in a sample boat. The sample or boat, or both, is inserted into
a high temperature combustion tube where the sulfur is oxidized to sulfur dioxide (SO ) in an oxygen rich atmosphere. Water
2
produced during the sample combustion is removed and the sample combustion gases are next exposed to ultraviolet (UV) light.
The SO absorbs the energy from the UV light and is converted to excited sulfur dioxide (SO *). The fluorescence emitted from
2 2
the excited SO * as it returns to a stable state, SO , is detected by a photomultiplier tube and the resulting signal is a measure of
2 2
the sulfur contained in the sample. (Warning—Exposure to excessive quantities of ultraviolet (UV) light is injurious to health. The
operator must avoid exposing any part of their person, especially their eyes, not only to direct UV light but also to secondary or
scattered radiation that is present.)
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 June 15, 2009Nov. 1, 2012. Published July 2009February 2013. Originally approved in 1993. Last previous edition approved in 20082009 as
D5453–08b.–09. DOI: 10.1520/D5453-09.10.1520/D5453-12.
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.
*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 ----------------------
D5453 − 12
FIG. 1 Conventional
...
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