ASTM D7184-13
(Test Method)Standard Test Method for Ultra Low Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
Standard Test Method for Ultra Low Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure Chemiluminescence Detection
SIGNIFICANCE AND USE
5.1 This test method is useful to detect and quantify nitrogen-containing compounds at a concentration of 0.03 to 1 mg N/kg in light aromatic hydrocarbons used or produced in manufacturing process. These nitrogen-containing compounds are undesirable in finished aromatic products and may be used in setting specification for determining the total nitrogen content in aromatic hydrocarbons.
5.2 This test method requires the use of reduced pressure at the detector. Loss of vacuum or pressure fluctuations impact the sensitivity of the detector and the ability to determine nitrogen concentrations less than 1 mg N/kg.
SCOPE
1.1 This test method covers the determination of total nitrogen in aromatic hydrocarbons, such as benzene, toluene, and xylene.
1.2 This test method is applicable for samples containing nitrogen from 0.38 to 1.2 mg N/kg. For higher nitrogen concentrations refer to Test Method D6069 or D4629. With careful analytical technique, this method can be used to successfully analyze concentrations below the current scope (see Appendix X1).
1.3 In determining the conformance of the test results using this method to applicable specifications; results shall be rounded off in accordance with the rounding-off method of Practice E29.
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 specific hazard statements, see Section 9.
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Designation: D7184 − 13
StandardTest Method for
Ultra Low Nitrogen in Aromatic Hydrocarbons by Oxidative
Combustion and Reduced Pressure Chemiluminescence
1
Detection
This standard is issued under the fixed designation D7184; 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* Chemiluminescence Detection
D6069 Test Method for Trace Nitrogen in Aromatic Hydro-
1.1 This test method covers the determination of total
carbons by Oxidative Combustion and Reduced Pressure
nitrogen in aromatic hydrocarbons, such as benzene, toluene,
Chemiluminescence Detection
and xylene.
D6809 Guide for Quality Control and Quality Assurance
1.2 This test method is applicable for samples containing
Procedures for Aromatic Hydrocarbons and Related Ma-
nitrogen from 0.38 to 1.2 mg N/kg. For higher nitrogen
terials
concentrations refer to Test Method D6069 or D4629. With
E29 Practice for Using Significant Digits in Test Data to
careful analytical technique, this method can be used to
Determine Conformance with Specifications
successfully analyze concentrations below the current scope
E691 Practice for Conducting an Interlaboratory Study to
(see Appendix X1).
Determine the Precision of a Test Method
2.2 Other Documents:
1.3 In determining the conformance of the test results using
this method to applicable specifications; results shall be OSHA Regulations, 29 CFR paragraphs 1910. 1000 and
3
1910.1200
rounded off in accordance with the rounding-off method of
Practice E29.
3. Terminology
1.4 The values stated in SI units are to be regarded as
3.1 Definitions:
standard. No other units of measurement are included in this
3.1.1 oxidative pyrolysis, n—a process in which a sample
standard.
undergoes combustion in an oxygen rich environment at
1.5 This standard does not purport to address all of the
temperatures greater than 900°C.
safety concerns, if any associated with its use. It is the
3.1.2 pyrolytic decomposition, n—combusting a compound
responsibility of the user of this standard to establish appro-
to decompose it to carbon dioxide, water and elemental oxides.
priate safety and health practices and determine the applica-
3.1.3 reduced pressure chemiluminescence, n—a chemical
bility of regulatory limitations prior to use. For specific hazard
reaction at pressure less than 760 mm mercury (Hg) in which
statements, see Section 9.
light is emitted.
2. Referenced Documents
4. Summary of Test Method
2
2.1 ASTM Standards:
4.1 A specimen is introduced into a carrier gas stream, at a
D3437 Practice for Sampling and Handling Liquid Cyclic
controlled rate, and incorporated into a high temperature
Products
furnace (900 to 1150°C) where an excess of oxygen is added.
D4629 Test Method for Trace Nitrogen in Liquid Petroleum
Pyrolysis converts hydrocarbons in the specimen to carbon
HydrocarbonsbySyringe/InletOxidativeCombustionand
dioxide and water. Organic nitrogen and inorganic nitrogen
compounds, present in the specimen, are converted to nitric
1
This test method is under the jurisdiction of ASTM Committee D16 on
oxide (NO). Nitric oxide reacts with ozone in the detector
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
producing nitrogen dioxide molecules in an excited state. As
Subcommittee D16.04 on Instrumental Analysis.
the excited nitrogen dioxide molecules relax to ground state,
Current edition approved July 1, 2013. Published July 1, 2013. Originally
approved in 2007. Last previous edition approved in 2012 as D7184 – 12. DOI: light is emitted.This light is detected by a photomultiplier tube
10.1520/D7184-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
*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 ----------------------
D7184 − 13
or by a photodiode with the resulting signal proportional to the 7.8 Automatic Boat Drive System—If the instrument is
concentration of nitrogen in the sample. Operating the detector equippedwithaboatinletsystemtheboatshouldbeintroduced
at a reduced pressure lowers the probability of the excited into the furnace at a controlled rate.
nitrogen dioxide mol
...
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: D7184 − 12 D7184 − 13
Standard Test Method for
Ultra Low Nitrogen in Aromatic Hydrocarbons by Oxidative
Combustion and Reduced Pressure Chemiluminescence
1
Detection
This standard is issued under the fixed designation D7184; 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 nitrogen in aromatic hydrocarbons, such as benzene, toluene, and xylene.
1.2 This test method is applicable for samples containing nitrogen from 0.38 to 1.2 mg N/kg. For higher nitrogen concentrations
refer to Test Method D6069 or D4629. With careful analytical technique, this method can be used to successfully analyze
concentrations below the current scope (see Appendix X1).
1.3 In determining the conformance of the test results using this method to applicable specifications; results shall be rounded
off in accordance with the rounding-off method of Practice E29.
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 specific hazard statements, see Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D4629 Test Method for Trace Nitrogen in Liquid Petroleum Hydrocarbons by Syringe/Inlet Oxidative Combustion and
Chemiluminescence Detection
D6069 Test Method for Trace Nitrogen in Aromatic Hydrocarbons by Oxidative Combustion and Reduced Pressure
Chemiluminescence Detection
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Documents:
3
OSHA Regulations, 29 CFR paragraphs 1910. 1000 and 1910.1200
3. Terminology
3.1 Definitions:
3.1.1 oxidative pyrolysis, n—a process in which a sample undergoes combustion in an oxygen rich environment at temperatures
greater than 900°C.
3.1.2 pyrolytic decomposition, n—combusting a compound to decompose it to carbon dioxide, water and elemental oxides.
3.1.3 reduced pressure chemiluminescence, n—a chemical reaction at pressure less than 760 mm mercury (Hg) in which light
is emitted.
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of Subcommittee
D16.04 on Instrumental Analysis.
Current edition approved Dec. 1, 2012July 1, 2013. Published January 2013July 1, 2013. Originally approved in 2007. Last previous edition approved in 20072012 as
D7184 – 07.12. DOI: 10.1520/D7184-12.10.1520/D7184-13.
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.
3
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
*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 ----------------------
D7184 − 13
4. Summary of Test Method
4.1 A specimen is introduced into a carrier gas stream, at a controlled rate, and incorporated into a high temperature furnace
(900 to 1150°C) where an excess of oxygen is added. Pyrolysis converts hydrocarbons in the specimen to carbon dioxide and water.
Organic nitrogen and inorganic nitrogen compounds, present in the specimen, are converted to nitric oxide (NO). Nitric oxide
reacts with ozone in the detector producing nitrogen dioxide molecules in an excited state. As the excited nitrogen dioxide
molecules relax to ground state, light is emitted. This light is detected by a photomultiplier tube or by a ph
...
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