ASTM D4629-17
(Test Method)Standard Test Method for Trace Nitrogen in Liquid Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection
Standard Test Method for Trace Nitrogen in Liquid Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection
SIGNIFICANCE AND USE
4.1 Some process catalysts used in petroleum and chemical refining may be poisoned when even trace amounts of nitrogenous materials are contained in the feedstocks. This test method can be used to determine bound nitrogen in process feeds and may also be used to control nitrogen compounds in finished products.
SCOPE
1.1 This test method covers the determination of the trace total nitrogen naturally found in liquid hydrocarbons boiling in the range from approximately 50 °C to 400 °C, with viscosities between approximately 0.2 cSt and 10 cSt (mm2/s) at room temperature. This test method is applicable to naphthas, distillates, and oils containing 0.3 mg/kg to 100 mg/kg total nitrogen. For liquid hydrocarbons containing more than 100 mg/kg total nitrogen, Test Method D5762 can be more appropriate. This test method has been successfully applied, during interlaboratory studies, to sample types outside the range of the scope by dilution of the sample in an appropriate solvent to bring the total nitrogen concentration and viscosity to within the range covered by the test method. However, it is the responsibility of the analyst to verify the solubility of the sample in the solvent and that direct introduction of the diluted sample by syringe into the furnace does not cause low results due to pyrolysis of the sample or solvent in the syringe needle.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. See 6.2, 6.4, 6.5, 6.9, and Section 7.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4629 − 17
Designation: 379/88
Standard Test Method for
Trace Nitrogen in Liquid Hydrocarbons by Syringe/Inlet
1
Oxidative Combustion and Chemiluminescence Detection
This standard is issued under the fixed designation D4629; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* 2. Referenced Documents
2
1.1 This test method covers the determination of the trace
2.1 ASTM Standards:
total nitrogen naturally found in liquid hydrocarbons boiling in
D1298 Test Method for Density, Relative Density, or API
the range from approximately 50 °C to 400 °C, with viscosities
Gravity of Crude Petroleum and Liquid Petroleum Prod-
2
between approximately 0.2 cSt and 10 cSt (mm /s) at room
ucts by Hydrometer Method
temperature. This test method is applicable to naphthas,
D4052 Test Method for Density, Relative Density, and API
distillates, and oils containing 0.3 mg⁄kg to 100 mg⁄kg total
Gravity of Liquids by Digital Density Meter
nitrogen. For liquid hydrocarbons containing more than
D5762 Test Method for Nitrogen in Liquid Hydrocarbons,
100 mg⁄kg total nitrogen, Test Method D5762 can be more
Petroleum and Petroleum Products by Boat-Inlet Chemi-
appropriate. This test method has been successfully applied,
luminescence
during interlaboratory studies, to sample types outside the
D6299 Practice for Applying Statistical Quality Assurance
range of the scope by dilution of the sample in an appropriate
and Control Charting Techniques to Evaluate Analytical
solvent to bring the total nitrogen concentration and viscosity
Measurement System Performance
to within the range covered by the test method. However, it is
the responsibility of the analyst to verify the solubility of the
3. Summary of Test Method
sample in the solvent and that direct introduction of the diluted
3.1 The sample of liquid petroleum hydrocarbon is intro-
sample by syringe into the furnace does not cause low results
due to pyrolysis of the sample or solvent in the syringe needle. duced either by syringe or boat inlet system, into a stream of
inert gas (helium or argon). The sample is vaporized and
1.2 The values stated in SI units are to be regarded as
carried to a high temperature zone where oxygen is introduced
standard. No other units of measurement are included in this
and organically bound nitrogen is converted to nitric oxide
standard.
(NO). The NO contacts ozone, and is converted to excited
1.3 This standard does not purport to address all of the
nitrogen dioxide (NO ). The light emitted as the excited NO
2 2
safety concerns, if any, associated with its use. It is the
decays is detected by a photomultiplier tube and the resulting
responsibility of the user of this standard to establish appro-
signal is a measure of the nitrogen contained in the sample.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See 6.2, 6.4, 6.5,
4. Significance and Use
6.9, and Section 7.
1.4 This international standard was developed in accor-
4.1 Some process catalysts used in petroleum and chemical
dance with internationally recognized principles on standard-
refining may be poisoned when even trace amounts of nitrog-
ization established in the Decision on Principles for the
enous materials are contained in the feedstocks. This test
Development of International Standards, Guides and Recom-
method can be used to determine bound nitrogen in process
mendations issued by the World Trade Organization Technical
feeds and may also be used to control nitrogen compounds in
Barriers to Trade (TBT) Committee.
finished products.
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 Dec. 15, 2017. Published February 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1986. Last previous edition approved in 2017 as D4629 – 12 (2017). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D4629-17. 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, We
...
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: D4629 − 12 (Reapproved 2017) D4629 − 17
Designation: 379/88
Standard Test Method for
Trace Nitrogen in Liquid Petroleum Hydrocarbons by
Syringe/Inlet Oxidative Combustion and Chemiluminescence
1
Detection
This standard is issued under the fixed designation D4629; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope Scope*
1.1 This test method covers the determination of the trace total nitrogen naturally found in liquid hydrocarbons boiling in the
2
range from approximately 50 °C to 400 °C, with viscosities between approximately 0.2 cSt and 10 cSt (mm /s) at room
temperature. This test method is applicable to naphthas, distillates, and oils containing 0.3 mg ⁄kg to 100 mg ⁄kg total nitrogen. For
liquid hydrocarbons containing more than 100 mg ⁄kg total nitrogen, Test Method D5762 can be more appropriate. This test method
has been successfully applied, during interlaboratory studies, to sample types outside the range of the scope by dilution of the
sample in an appropriate solvent to bring the total nitrogen concentration and viscosity to within the range covered by the test
method. However, it is the responsibility of the analyst to verify the solubility of the sample in the solvent and that direct
introduction of the diluted sample by syringe into the furnace does not cause low results due to pyrolysis of the sample or solvent
in the syringe needle.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. See 6.2, 6.4, 6.5, 6.9, and Section 7.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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
D5762 Test Method for Nitrogen in Liquid Hydrocarbons, Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
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 The sample of liquid petroleum hydrocarbon is introduced either by syringe or boat inlet system, into a stream of inert gas
(helium or argon). The sample is vaporized and carried to a high temperature zone where oxygen is introduced and organically
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
D02.03 on Elemental Analysis.
Current edition approved July 1, 2017Dec. 15, 2017. Published July 2017February 2018. Originally approved in 1986. Last previous edition approved in 20122017 as
D4629 – 12.D4629 – 12 (2017). DOI: 10.1520/D4629-12R17.10.1520/D4629-17.
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 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 ----------------------
D4629 − 17
bound nitrogen is converted to nitric oxide (NO). The NO contacts ozone, and is converted to excited nitrogen dioxide (NO ). The
2
light emitted as the excited NO decays is detected by a photomultiplier tube and the resulting signal is a measure of the nitrogen
2
contained in the sample.
4. Sig
...
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