ASTM D5176-08

Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection

SIGNIFICANCE AND USE
This test method is useful for the determination of total chemically bound nitrogen in wastewaters and other waters.
SCOPE
1.1 This test method covers the determination of the total nitrogen content of water in concentrations from 0.5 to 1000 mg/L. Higher nitrogen concentrations may be determined by making the proper dilutions.
1.2 This test method does not determine molecular nitrogen (N2).
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.

General Information

• Status: Historical
• Publication Date: 30-Apr-2008
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D5176-91(2003) - Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection
• Effective Date: 01-May-2008
• Replaced By: ASTM D5176-08(2015) - Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection
• Effective Date: 15-Jun-2015
• Referred By: ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-May-2008

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5176 − 08
StandardTest Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
1
Chemiluminescence Detection
This standard is issued under the fixed designation D5176; 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 4. Summary of Test Method
4.1 The sample of water is introduced into a stream of
1.1 This test method covers the determination of the total
oxygen or inert/oxygen mix flowing through a quartz pyrolysis
nitrogen content of water in concentrations from 0.5 to 1000
tube. Oxidative pyrolysis converts chemically bound nitrogen
mg/L. Higher nitrogen concentrations may be determined by
to nitric oxide (NO). The gas stream is dried and the NO is
making the proper dilutions.
contacted with ozone (O ) producing metastable nitrogen
3
1.2 This test method does not determine molecular nitrogen
dioxide (NO *). As the NO * decays, light is emitted and
2 2
(N ).
2
detected by a photomultiplier tube. The resulting signal is a
measure of the total chemically bound nitrogen in the sample.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
5. Significance and Use
standard.
5.1 This test method is useful for the determination of total
1.4 This standard does not purport to address all of the
chemically bound nitrogen in wastewaters and other waters.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3
6. Apparatus
priate safety and health practices and determine the applica-
6.1 Pyrolysis Furnace—An electric tube furnace capable of
bility of regulatory limitations prior to use.
achieving a temperature of 1100°C. The furnace may be single
or multizoned and may have common or separate and inde-
2. Referenced Documents
pendent temperature controls.
2
2.1 ASTM Standards:
6.2 Pyrolysis Tube— The pyrolysis tube must be fabricated
D1129 Terminology Relating to Water
from quartz and should be designed to ensure complete
D1193 Specification for Reagent Water
pyrolysis of a wide variety of samples.
D2777 Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water 6.3 Chemiluminescence Detector —The detector shall have
a photomultiplier tube capable of sensing the light emission of
the decaying NO *. The detector shall have digital display,
3. Terminology
2
onboard ozone generator and analog output for data system or
3.1 Definitions—For definitions of terms used in this test
strip chart recorder.
method, refer to Terminology D1129.
6.4 Recorder (optional)—The recorder shall be able to
3.2 Definitions of Terms Specific to This Standard:
accept a 1 V full scale signal and to provide a chart speed of 1
3.2.1 total chemically bound nitrogen—all inorganic and
cm/min.
organicnitrogeninthesample,exceptmolecularnitrogen(N ).
2
6.5 Microlitre Syringe—Any standard series of microlitre
syringes with stainless steel needles is acceptable. See manu-
facturer’s instructions for appropriate syringe sizes.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
6.6 Syringe Drive Mechanism—The syringe drive shall be
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
capable of driving the sample from a microlitre syringe at a
Current edition approved May 1, 2008. Published June 2008. Originally
controlled, reproducible rate.
approved in 1991. Last previous edition approved in 2003 as D5176 – 91 (2003).
DOI: 10.1520/D5176-08.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM The apparatus described in 6.1-6.7 is manufactured byAntek Instruments, Inc.,
Standards volume information, refer to the standard’s Document Summary page on Houston, TX and Dohrmann Division of Rosemount Analytical Inc., Santa Clara,
the ASTM website. CA, and was used in the validation study of this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D5176 − 08
6.7 Sample Boat— Samples with high concentrations of injected, withdraw the syringe needle. Retract the plunger so
suspended matter or dissolved nonvolatile compounds may that the sample meniscus is again at the 1 µLpoint and note the
tendtoplugthesyringeneedleuponinjectionintothepyrolysis plunger position. The true amount injected is the difference
tube. In this case a sample boat of quartz or platin
...

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:D5176–91(Reapproved2003) Designation:D5176–08
Standard Test Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
1
Chemiluminescence Detection
This standard is issued under the fixed designation D 5176; 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 the total nitrogen content of water in concentrations from 0.5 to 1000 mg/L.
Higher nitrogen concentrations may be determined by making the proper dilutions.
1.2 This test method does not determine molecular nitrogen (N ).
2
1.3The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
D 2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D 1129.
3.2 Definition of Term Specific to This Standard:
3.2.1 total chemically bound nitrogen—all inorganic and organic nitrogen in the sample, except molecular nitrogen (N ).
2
4. Summary of Test Method
4.1 The sample of water is introduced into a stream of oxygen or inert/oxygen mix flowing through a quartz pyrolysis tube.
Oxidative pyrolysis converts chemically bound nitrogen to nitric oxide (NO).The gas stream is dried and the NO is contacted with
ozone (O ) producing metastable nitrogen dioxide (NO *).As the NO * decays, light is emitted and detected by a photomultiplier
3 2 2
tube. The resulting signal is a measure of the total chemically bound nitrogen in the sample.
5. Significance and Use
5.1 This test method is useful for the determination of total chemically bound nitrogen in wastewaters and other waters.
3
6. Apparatus
6.1 Pyrolysis Furnace—An electric tube furnace capable of achieving a temperature of 1100°C. The furnace may be single or
multizoned and may have common or separate and independent temperature controls.
6.2 Pyrolysis Tube— The pyrolysis tube must be fabricated from quartz and should be designed to ensure complete pyrolysis
of a wide variety of samples.
6.3 Chemiluminescence Detector —The detector shall have a photomultiplier tube capable of sensing the light emission of the
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved March 10, 2003. Published July 2003. Originally approved in 1991. Last previous edition approved in 1995 as D5176–91(1995).
Current edition approved May 1, 2008. Published June 2008. Originally approved in 1991. Last previous edition approved in 2003 as D 5176 – 91 (2003).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The apparatus described in 6.1-6.7 is manufactured by Antek Instruments, Inc., Houston, TX and Dohrmann Division of Rosemount Analytical Inc., Santa Clara, CA,
and was used in the validation study of this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D5176–08
decaying NO *. The detector shall have digital display, onboard ozone generator and analog output for data system or strip chart
2
recorder.
6.4 Recorder (optional)—The recorder shall be able to accept a 1 V full scale signal and to provide a chart speed of 1 cm/min.
6.5 Microlitre Syringe—Anystandardseriesofmicrolitresyringeswithstainlesssteelneedlesisacceptable.Seemanufacturer’s
instructions for app
...