Standard Test Method for Nitrogen in Petroleum and Petroleum Products by Boat-Inlet Chemiluminescence

SIGNIFICANCE AND USE
Many nitrogen compounds can contaminate refinery catalysts. They tend to be the most difficult class of compounds to hydrogenate, so the nitrogen content remaining in the product of a hydrotreator is a measure of the effectiveness of the hydrotreating process. In lubricating oils the concentration of nitrogen is a measure of the presence of nitrogen containing additives. This test method is intended for use in plant control and in research.
SCOPE
1.1 This test method covers the determination of nitrogen in liquid hydrocarbons, including petroleum process streams and lubricating oils in the concentration range from 40 to 10 000 μg/g nitrogen. For light hydrocarbons containing less than 100 μg/g nitrogen, Test Method D4629 can be more appropriate.
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. Specific warning statements are given in Section 6, 7.1, 8.2, and 8.2.2.

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Publication Date
14-Apr-2012
Current Stage
Ref Project

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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5762 − 12
Standard Test Method for
Nitrogen in Petroleum and Petroleum Products by Boat-Inlet
1
Chemiluminescence
This standard is issued under the fixed designation D5762; 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* high-temperature combustion tube where the nitrogen is oxi-
dized to nitric oxide (NO) in an oxygen atmosphere. The NO
1.1 Thistestmethodcoversthedeterminationofnitrogenin
contacts ozone and is converted to excited nitrogen dioxide
liquid hydrocarbons, including petroleum process streams and
(NO ).ThelightemittedastheexcitedNO decaysisdetected
2 2
lubricating oils in the concentration range from 40 to 10000
byaphotomultipliertube,andtheresultingsignalisameasure
µg⁄gnitrogen.Forlighthydrocarbonscontaininglessthan100
of the nitrogen contained in the sample.
µg/g nitrogen, Test Method D4629 can be more appropriate.
1.2 The values stated in SI units are to be regarded as
4. Significance and Use
standard. No other units of measurement are included in this
4.1 Many nitrogen compounds can contaminate refinery
standard.
catalysts.Theytendtobethemostdifficultclassofcompounds
1.3 This standard does not purport to address all of the
to hydrogenate, so the nitrogen content remaining in the
safety concerns, if any, associated with its use. It is the
product of a hydrotreator is a measure of the effectiveness of
responsibility of the user of this standard to establish appro-
the hydrotreating process. In lubricating oils the concentration
priate safety and health practices and determine the applica-
of nitrogen is a measure of the presence of nitrogen containing
bility of regulatory limitations prior to use. Specific warning
additives. This test method is intended for use in plant control
statements are given in Section 6, 7.1, 8.2, and 8.2.2.
and in research.
2. Referenced Documents
5. Apparatus
2
2.1 ASTM Standards:
5.1 Boat Inlet System,capableofbeingsealedtotheinletof
D4057Practice for Manual Sampling of Petroleum and
the combustion tube and swept with inert gas. The boats are
Petroleum Products
fabricated from platinum or quartz. To aid quantitative liquid
D4177Practice for Automatic Sampling of Petroleum and
injection, it is recommended to add a small piece of quartz
Petroleum Products
woolorsuitableequivalent(see6.8)totheboat.Theboatdrive
D4629Test Method for Trace Nitrogen in Liquid Petroleum
mechanism should be able to fully insert the boat into the
HydrocarbonsbySyringe/InletOxidativeCombustionand
furnace tube inlet section. A drive mechanism that advances
Chemiluminescence Detection
and withdraws the sample boat into and out of the furnace at a
D6299Practice for Applying Statistical Quality Assurance
controlled and repeatable rate is required.
and Control Charting Techniques to Evaluate Analytical
5.2 Chemiluminescence Detector, capable of measuring
Measurement System Performance
lightemittedfromthereactionbetweennitricoxideandozone,
and containing a variable attenuation amplifier, integrator, and
3. Summary of Test Method
readout.
3.1 A hydrocarbon sample is placed on a sample boat at
NOTE 1—Detectors designed to maintain the chemiluminescence reac-
room temperature. The sample and boat are advanced into a
tion cell at reduced pressure are acceptable for use and were included in
the instruments used to determine the precision of this test method.
1
This test method is under the jurisdiction of ASTM Committee D02 on
5.3 Combustion Tube, fabricated from quartz. The inlet end
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
ofthetubeshallbelargeenoughtoacceptthesampleboatand
Subcommittee D02.03 on Elemental Analysis.
tohavesidearmsforintroductionofoxygenandinertgas.The
Current edition approved April 15, 2012. Published June 2012. Originally
construction is such that the carrier gases sweep the inlet zone
approved in 1995. Last previous edition approved in 2011 as D5762–11. DOI:
10.1520/D5762-12.
transporting all of the volatilized sample into a high-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
temperature oxidation zone. The oxidation section should be
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
large enough to ensure complete oxidation of the sample.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Combustion tubes recommended for the two furnaces in 5.5.1
*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. Unite
...

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.
Designation:D5762–11 Designation: D5762 – 12
Standard Test Method for
Nitrogen in Petroleum and Petroleum Products by Boat-Inlet
1
Chemiluminescence
This standard is issued under the fixed designation D5762; 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 nitrogen in liquid hydrocarbons, including petroleum process streams and
lubricating oils in the concentration range from 40 to 10 000 µg/g nitrogen. For light hydrocarbons containing less than 100 µg/g
nitrogen, Test Method D4629 can be more appropriate.
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. Specific warning statements are given in Section 6, 7.1, 8.2, and 8.2.2.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4629 Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and
Chemiluminescence Detection
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
3. Summary of Test Method
3.1 A hydrocarbon sample is placed on a sample boat at room temperature. The sample and boat are advanced into a
high-temperature combustion tube where the nitrogen is oxidized to nitric oxide (NO) in an oxygen atmosphere. The NO contacts
ozone and is converted to excited nitrogen dioxide (NO ). The light emitted as the excited NO decays is detected by a
2 2
photomultiplier tube, and the resulting signal is a measure of the nitrogen contained in the sample.
4. Significance and Use
4.1 Many nitrogen compounds can contaminate refinery catalysts. They tend to be the most difficult class of compounds to
hydrogenate, so the nitrogen content remaining in the product of a hydrotreator is a measure of the effectiveness of the
hydrotreating process. In lubricating oils the concentration of nitrogen is a measure of the presence of nitrogen containing
additives. This test method is intended for use in plant control and in research.
5. Apparatus
5.1 Boat Inlet System, capable of being sealed to the inlet of the combustion tube and swept with inert gas. The boats are
fabricated from platinum or quartz. To aid quantitative liquid injection, it is recommended to add a small piece of quartz wool or
suitable equivalent (see 6.8) to the boat. The boat drive mechanism should be able to fully insert the boat into the furnace tube
inlet section. A drive mechanism that advances and withdraws the sample boat into and out of the furnace at a controlled and
repeatable rate is required.
5.2 Chemiluminescence Detector , capable of measuring light emitted from the reaction between nitric oxide and ozone, and
containing a variable attenuation amplifier, integrator, and readout.
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 1, 2011. Published July 2011. Originally approved in 1995. Last previous edition approved in 2010 as D5762–10. DOI: 10.1520/D5762-11.
Current edition approved April 15, 2012. Published June 2012. Originally approved in 1995. Last previous edition approved in 2011 as D5762–11. DOI:
10.1520/D5762-12.
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

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D5762 – 12
NOTE 1—Detectors designed to maintain the chemiluminescence rea
...

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