ASTM D5176-91(2003)
(Test Method)Standard Test Method for Total Chemically Bound Nitrogen in Water by Pyrolysis and Chemiluminescence Detection
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 the standard. The values given in parentheses are for information only.
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
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Standards Content (Sample)
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Designation:D5176–91(Reapproved2003)
Standard Test Method for
Total Chemically Bound Nitrogen in Water by Pyrolysis and
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope contacted with ozone (O ) producing metastable nitrogen
dioxide (NO *). As the NO * decays, light is emitted and
1.1 This test method covers the determination of the total 2 2
detected by a photomultiplier tube. The resulting signal is a
nitrogen content of water in concentrations from 0.5 to 1000
measure of the total chemically bound nitrogen in the sample.
mg/L. Higher nitrogen concentrations may be determined by
making the proper dilutions.
5. Significance and Use
1.2 This test method does not determine molecular nitrogen
5.1 This test method is useful for the determination of total
(N ).
chemically bound nitrogen in wastewaters and other waters.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
6. Apparatus
only.
6.1 Pyrolysis Furnace—An electric tube furnace capable of
1.4 This standard does not purport to address all of the
achieving a temperature of 1100°C. The furnace may be single
safety concerns, if any, associated with its use. It is the
or multizoned and may have common or separate and inde-
responsibility of the user of this standard to establish appro-
pendent temperature controls.
priate safety and health practices and determine the applica-
6.2 Pyrolysis Tube—The pyrolysis tube must be fabricated
bility of regulatory limitations prior to use.
from quartz and should be designed to ensure complete
2. Referenced Documents pyrolysis of a wide variety of samples.
6.3 Chemiluminescence Detector—The detector shall have
2.1 ASTM Standards:
a photomultiplier tube capable of sensing the light emission of
D 1129 Terminology Relating to Water
2 the decaying NO *. The detector shall have digital display,
D 1193 Specification for Reagent Water
onboard ozone generator and analog output for data system or
D 2777 Practice for Determination of Precision and Bias of
2 strip chart recorder.
Applicable Methods of Committee D19 on Water
6.4 Recorder (optional)—The recorder shall be able to
3. Terminology accept a 1 V full scale signal and to provide a chart speed of 1
cm/min.
3.1 Definitions—For definitions of terms used in this test
6.5 Microlitre Syringe—Any standard series of microlitre
method, refer to Terminology D 1129.
syringes with stainless steel needles is acceptable. See manu-
3.2 Definition of Term Specific to This Standard:
facturer’s instructions for appropriate syringe sizes.
3.2.1 total chemically bound nitrogen—all inorganic and
6.6 Syringe Drive Mechanism—The syringe drive shall be
organicnitrogeninthesample,exceptmolecularnitrogen(N ).
capable of driving the sample from a microlitre syringe at a
4. Summary of Test Method controlled, reproducible rate.
6.7 Sample Boat—Samples with high concentrations of
4.1 The sample of water is introduced into a stream of
suspended matter or dissolved nonvolatile compounds may
oxygen or inert/oxygen mix flowing through a quartz pyrolysis
tendtoplugthesyringeneedleuponinjectionintothepyrolysis
tube. Oxidative pyrolysis converts chemically bound nitrogen
tube. In this case a sample boat of quartz or platinum, with or
to nitric oxide (NO). The gas stream is dried and the NO is
without quartz wool, should be used, in conjunction with the
appropriate pyrolysis tube. The pyrolysis tube shall allow the
This test method is under the jurisdiction of ASTM Committee D19 on Water
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
Organic Substances in Water.
Current edition approved March 10, 2003. Published July 2003. Originally The apparatus described in 6.1-6.7 is manufactured byAntek Instruments, Inc.,
approved in 1991. Last previous edition approved in 1995 as D 5176 – 91 (1995). Houston, TX and Dohrmann Division of Rosemount Analytical Inc., Santa Clara,
Annual Book of ASTM Standards, Vol 11.01. 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.
D5176–91 (2003)
introduction of the sample into the boat by microlitre syringe 9.4 Boat Injection—Fill the microlitre syringe to the mark
without interrupting the gas flow system. and inject the sample directly into the boat while holding the
needle in contact with the side of the boat or with the quartz
7. Reagents and Materials
wool.
9.5 Determine each calibration standard and the zero blank
7.1 Purity of Reagents—Reagent grade chemicals shall be
three times and record the net response from the average of
used.Unlessotherwiseindicated,itisintendedthatallreagents
each set of standard responses.
shall conform to the specifications of the Committee on
9.6 By injecting the same volumetric amount of sample for
Analytical Reagents of the American Chemical Society.
each determination, the only variables will be total nitrogen
Other grades may be used, provided it is first determined that
concentrationanddetectorresponse(digitaldisplay).Construct
the reagent is of sufficiently high purity to permit its use
a curve plotting milligrams of N per litre versus detector
without lessening the accuracy of the determination.
response. Check the complete calibration curve at least once
7.2 Purity of Water—Unless otherwise indicated, references
per week; check one or two standards daily.
to water shall be understood to mean reagent water conforming
to Specification D 1193, Type I.
10. Procedure
7.3 Inert Gas, Argon (minimum purity 99.99 %).
7.4 Oxygen (minimum purity 99.6 %).
10.1 Flush the microlitre syringe several times with the
7.5 Stock Solution, Pyridine (10 000 mg N/L)—Prepare by
unknown sample. Inject the sample at a controlled rate of 1 to
accurately weighing 5.647 g of pyridine into a 100 mL
2 µg/s as described in 9.3 or inject the sample into the sample
volumetric flask and dilute to 100 mL with water.
boat (see 6.7) as described in 9.4.
7.6 Pyridine Solutions, Standard (1000, 500, 100, 50, 10, 5,
10.2 Set instrument parameters as reco
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