ASTM D4629-08
(Test Method)Standard Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection
Standard Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and Chemiluminescence Detection
SIGNIFICANCE AND USE
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 to 400°C, with viscosities between approximately 0.2 and 10 cSt (mm2/s) at room temperature. This test method is applicable to naphthas, distillates, and oils containing 0.3 to 100 mg/kg total nitrogen. For liquid hydrocarbons containing more than 100 mg/kg total nitrogen, Test Method D 5762 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.
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An American National Standard
Designation:D4629–08
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 D 4629; 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 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 D 1298 Test Method for Density, Relative Density (Specific
the range from approximately 50 to 400°C, with viscosities Gravity), or API Gravity of Crude Petroleum and Liquid
2
between approximately 0.2 and 10 cSt (mm /s) at room Petroleum Products by Hydrometer Method
temperature. This test method is applicable to naphthas, distil- D 4052 Test Method for Density and Relative Density of
lates, and oils containing 0.3 to 100 mg/kg total nitrogen. For Liquids by Digital Density Meter
liquid hydrocarbons containing more than 100 mg/kg total D 5762 Test Method for Nitrogen in Petroleum and Petro-
nitrogen, Test Method D 5762 can be more appropriate. This leum Products by Boat-Inlet Chemiluminescence
test method has been successfully applied, during interlabora- D 6299 Practice for Applying Statistical Quality Assurance
tory studies, to sample types outside the range of the scope by and Control Charting Techniques to Evaluate Analytical
dilution of the sample in an appropriate solvent to bring the Measurement System Performance
total nitrogen concentration and viscosity to within the range
3. Summary of Test Method
covered by the test method. However, it is the responsibility of
the analyst to verify the solubility of the sample in the solvent 3.1 The sample of liquid petroleum hydrocarbon is intro-
duced either by syringe or boat inlet system, into a stream of
and that direct introduction of the diluted sample by syringe
into the furnace does not cause low results due to pyrolysis of inert gas (helium or argon). The sample is vaporized and
carried to a high temperature zone where oxygen is introduced
the sample or solvent in the syringe needle.
1.2 The values stated in SI units are to be regarded as and organically bound nitrogen is converted to nitric oxide
(NO). The NO contacts ozone, and is converted to excited
standard. No other units of measurement are included in this
standard. nitrogen oxide (NO ). The light emitted as the excited NO
2 2
decays is detected by a photomultiplier tube and the resulting
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the signal is a measure of the nitrogen contained in the sample.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
4.1 Some process catalysts used in petroleum and chemical
bility of regulatory limitations prior to use. See 6.2, 6.4, 6.5,
refining may be poisoned when even trace amounts of nitrog-
6.9, and Section 7.
enous materials are contained in the feedstocks. This test
1
This test method is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D02.03 on Elemental Analysis. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved July 1, 2008. Published August 2008. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1986. Last previous edition approved in 2007 as D 4629–02(2007). 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 ----------------------
D4629–08
method can be used to determine bound nitrogen in process 6. Reagents
feeds and may also be used to control nitrogen compounds in
6.1 Purity of Reagents—Reagent grade chemicals shall be
finished products.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
3
5. Apparatus
teeonAnalyticalReagentsoftheAmericanChemicalSociety,
where such specifications are available. Other grades may be
5.1 Furnace, electric, held at a temperature sufficient to
used, provided it is
...
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.
An American National Standard
Designation:D4629–02 (Reapproved 2007) Designation:D4629–08
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 D 4629; 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 Department of Defense.
1. 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 to 400°C, with viscosities between approximately 0.2 and 10 cSt (mm /s) at room temperature. This
test method is applicable to naphthas, distillates, and oils containing 0.3 to 100 mg/kg total nitrogen. For liquid hydrocarbons
containing more than 100 mg/kg total nitrogen, Test Method D 5762 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
appropriatesolventtobringthetotalnitrogenconcentrationandviscositytowithintherangecoveredbythetestmethod.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.
1.2The values stated in SI units are to be regarded as standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1298 TestMethodforDensity,RelativeDensity(SpecificGravity),orAPIGravityofCrudePetroleumandLiquidPetroleum
Products by Hydrometer Method
D 4052 Test Method for Density and Relative Density of Liquids by Digital Density Meter
D 5762 Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence
D 6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement 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
bound nitrogen is converted to nitric oxide (NO). The NO contacts ozone, and is converted to excited nitrogen oxide (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.
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 MayJuly 1, 2007.2008. Published July 2007.August 2008. Originally approved in 1986. Last previous edition approved in 20022007 as
D 4629–02(2007).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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 ----------------------
D4629–08
4. 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.
5. Apparatus
5.1 Furnace, electric, held at a temperatu
...
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