ASTM D5176-08(2015)

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

SIGNIFICANCE AND USE
5.1 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: 14-Jun-2015
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D5176-08 - 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: 15-Jun-2015

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2015)
Standard Test Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
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
nitrogen content of water in concentrations from 0.5 to 1000 oxygen or inert/oxygen mix flowing through a quartz pyrolysis
tube. Oxidative pyrolysis converts chemically bound nitrogen
mg/L. Higher nitrogen concentrations may be determined by
making the proper dilutions. to nitric oxide (NO). The gas stream is dried and the NO is
contacted with ozone (O ) producing metastable nitrogen
1.2 This test method does not determine molecular nitrogen
dioxide (NO *). As the NO * decays, light is emitted and
2 2
(N ).
detected by a photomultiplier tube. The resulting signal is a
1.3 The values stated in SI units are to be regarded as
measure of the total chemically bound nitrogen in the sample.
standard. No other units of measurement are included in this
standard.
5. Significance and Use
1.4 This standard does not purport to address all of the
5.1 This test method is useful for the determination of total
safety concerns, if any, associated with its use. It is the
chemically bound nitrogen in wastewaters and other waters.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 6. Apparatus
bility of regulatory limitations prior to use.
6.1 Pyrolysis Furnace—An electric tube furnace capable of
achieving a temperature of 1100°C. The furnace may be single
2. Referenced Documents
or multizoned and may have common or separate and inde-
2.1 ASTM Standards: pendent temperature controls.
D1129 Terminology Relating to Water
6.2 Pyrolysis Tube—The pyrolysis tube must be fabricated
D1193 Specification for Reagent Water
from quartz and should be designed to ensure complete
D2777 Practice for Determination of Precision and Bias of
pyrolysis of a wide variety of samples.
Applicable Test Methods of Committee D19 on Water
6.3 Chemiluminescence Detector—Thedetectorshallhavea
photomultiplier tube capable of sensing the light emission of
3. Terminology
the decaying NO *. The detector shall have digital display,
3.1 Definitions:
onboard ozone generator and analog output for data system or
3.1.1 For definitions of terms used in this standard, refer to
strip chart recorder.
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, n—all inorganic and
cm/min.
organicnitrogeninthesample,exceptmolecularnitrogen(N ).
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.
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 June 15, 2015. Published June 2015. Originally
controlled, reproducible rate.
approved in 1991. Last previous edition approved in 2008 as D5176 – 08. DOI:
10.1520/D5176-08R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM The apparatus described in 6.1 – 6.7 is manufactured by Antek Instruments,
Standards volume information, refer to the standard’s Document Summary page on Inc., Houston, TX and Dohrmann Division of Rosemount Analytical Inc., Santa
the ASTM website. 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
D5176 − 08 (2015)
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 platinum, with or between the two plunger positions.
without quartz wool, should be used, in conjunction with the
NOTE 1—If water samples contain high concentrations of suspended
appropriate pyrolysis tube. The pyrolysis tube shall allow the
matter or dissolved nonvolatile compounds, the syringe needle may tend
introduction of the sample into the boat by microlitre syringe
to plug or the precision and bias of the test method may be degraded. In
such a case, the sample boat system should be used (see 6.7).
without interrupting the gas flow system.
9.4 Boat Injection—Fill the microlitre syringe to the mark
7. Reagents and Materials
and inject the sample directly into the boat while holding the
7.1 Purity of Reagents—Reagent grade chemicals shall be
needle in contact with the side of the boat or with the quartz
used.Unlessotherwiseindicated,itisintendedthatallreagents
wool.
shall conform to the specifications of the Committee on
9.5 Determine each calibration standard and the zero blank
Analytical Reagents of the American Chemical Society.
three times and record the net response from the average of
Other grades may be used, provided it is first determined that
each set of standard responses.
the reagent is of sufficiently high purity to permit its use
9.6 By injecting the same volumetric amount of sample for
without lessening the accuracy of the determination.
each determination, the only variables will be total nitrogen
7.2 Purity of Water—Unless otherwise indicated, references
concentrationanddetectorresponse(digitaldisplay).Construct
to water shall be understood to mean reagent water that meets
a curve plotting milligrams of N per litre versus detector
the purity specifications of Type I or Type II water, presented
response. Check the complete calibration curve at least once
in Specification D1193.
per week; check one or two standards daily.
7.3 Inert Gas, Argon (minimum purit
...

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: D5176 − 08 D5176 − 08 (Reapproved 2015)
Standard Test Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
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
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 ).
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
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this test method, refer to Terminology D1129.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total chemically bound nitrogen—nitrogen, n—all inorganic and organic nitrogen in the sample, except molecular nitrogen
(N ).
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.
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.
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 May 1, 2008June 15, 2015. Published June 2008June 2015. Originally approved in 1991. Last previous edition approved in 20032008 as
D5176 – 91 (2003).D5176 – 08. DOI: 10.1520/D5176-08.10.1520/D5176-08R15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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
D5176 − 08 (2015)
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 —Detector—The detector shall have a photomultiplier tube capable of sensing the light
emission of the decaying NO *. The detector shall have digital display, onboard ozone generator and analog output for data system
or strip chart 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—Any standard series of microlitre syringes with stainless steel needles is acceptable. See manufacturer’s
instructions for appropriate syringe sizes.
6.6 Syringe Drive Mechanism—The syringe drive shall be capable of driving the sample from a microlitre syringe at a
controlled, reproducible rate.
6.7 Sample Boat—Samples with high concentrations of suspended matter or dissolved nonvolatile compounds may tend to plug
the syringe needle upon injection into the pyrolysis tube. In this case a sample boat of quartz or platinum, with or without quartz
wool, should be used, in conjunction with the appropriate pyrolysis tube. The pyrolysis tube shall allow the introduction of the
sample into the boat by microlitre syringe without interrupting the gas flow system.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used. Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society. Other grades may be
used, provided it is first determined that the reagent is of sufficiently high purity to permit its use without lessening the accuracy
of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water that meets the
purity specifications of Type I or Type II water, presented in Specification D1193.
7.3 Inert Gas, Argon (minimum purity 99.99 %).
7.4 Oxygen (minimum purity 99.6 %).
7.5 Stock Solution, Pyridine (10 000 mg N/L)—Prepare by accurately weighing 5.647 g of pyridine into a 100 mL volumetric
flask and dilute to 100 mL with water.
7.6 Pyridine Solutions, Standard (1000, 500, 100, 50, 10, 5, 1, and 0.5 mg N/L)—Dilute ten volumes of the stock solution (see
6.5) with 90 volumes of water to prepare a 1000 mg N/L standard. Similarly, by serial dilution with water, prepare 500, 100, 50,
10, 5, 1, and 0.5 mg N/L standards.
8. Preparation of Apparatus
8.1 Assemble apparatus according to manufacturer’s instructions.
9. Calibration and Standardization
9.1 Use the water that was used to prepare the standards as a zero blank standard.
9.2 A sample size of 5 to 10 μL is sufficient to cover the concentration range of this test method. The volume of the sample shall
be accurately determined.
9.3 Syringe Injection—Fill the syringe to the 5 μL mark and retract the plunger so that the liquid meniscus is at the 1 μL mark.
Note
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