ASTM D4629-02
(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
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 400C, 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.
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:D4629–02
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 (e) 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 Gravity), or API Gravity of Crude Petroleum and Liquid
2
Petroleum Products by Hydrometer Method
1.1 This test method covers the determination of the trace
D 4052 Test Method for Density and Relative Density of
total nitrogen naturally found in liquid hydrocarbons boiling in
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Liquids by Digital Density Meter
the range from approximately 50 to 400°C, with viscosities
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D 4057 Practice for Manual Sampling of Petroleum and
between approximately 0.2 and 10 cSt (mm /s) at room
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Petroleum Products
temperature. This test method is applicable to naphthas, distil-
D 4177 Practice for Automatic Sampling of Petroleum and
lates, and oils containing 0.3 to 100 mg/kg total nitrogen. For
2
Petroleum Products
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
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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
Techniques to Evaluate Analytical Measurement System
dilution of the sample in an appropriate solvent to bring the
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Performance
total nitrogen concentration and viscosity to within the range
covered by the test method. However, it is the responsibility of
3. Summary of Test Method
the analyst to verify the solubility of the sample in the solvent
3.1 The sample of liquid petroleum hydrocarbon is intro-
and that direct introduction of the diluted sample by syringe
duced either by syringe or boat inlet system, into a stream of
into the furnace does not cause low results due to pyrolysis of
inert gas (helium or argon). The sample is vaporized and
the sample or solvent in the syringe needle.
carried to a high temperature zone where oxygen is introduced
1.2 The values stated in SI units are to be regarded as
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 oxide (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.
4.1 Some process catalysts used in petroleum and chemical
2. Referenced Documents refining may be poisoned when even trace amounts of nitrog-
enous materials are contained in the feedstocks. This test
2.1 ASTM Standards:
method can be used to determine bound nitrogen in process
D 1298 Practice for Density, Relative Density (Specific
feeds and may also be used to control nitrogen compounds in
finished products.
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 Annual Book of ASTM Standards, Vol 05.01.
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D02.03 on Elemental Analysis. Annual Book of ASTM Standards, Vol 05.02.
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Current edition approved April 10, 2002. Published July 2002. Originally Annual Book of ASTM Standards, Vol 05.03.
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published as D 4629–86. Last previous edition D 4629–96. Annual Book of ASTM Standards, Vol 05.04.
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D4629–02
5. Apparatus all reagents shall conform to the specifications of the Commit-
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tee onAnalytical Reagents of theAmerican Chemical Society,
5.1 Furnace, electric, held at a temperature sufficient to
where such specifications are available. Other grades may be
volatilize and pyrolyze all of the sample and oxidize the
used, provided it is first ascertained that the reagent is of
organically bound nitrogen to NO. Furnace temperature(s)
sufficiently high purity to permit its use without lessenin
...
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