ASTM D1607-91(2005)
(Test Method)Standard Test Method for Nitrogen Dioxide Content of the Atmosphere (Griess-Saltzman Reaction)
Standard Test Method for Nitrogen Dioxide Content of the Atmosphere (Griess-Saltzman Reaction)
SIGNIFICANCE AND USE
Nitrogen dioxide plays an important role in photochemical smog-forming reactions and, in sufficient concentrations, is deleterious to health, agriculture, materials, and visibility.
In combustion processes, significant amounts of nitric oxide (NO) may be produced by combination of atmospheric nitrogen and oxygen; at ambient temperatures NO can be converted to NO2 by oxygen and other atmospheric oxidants. Nitrogen dioxide may also be generated from processes involving nitric acid, nitrates, the use of explosives, and welding.
SCOPE
1.1 This test method covers the manual determination of nitrogen dioxide (NO2) in the atmosphere in the range from 4 to 10 000 g/m3 (0.002 to 5 ppm(v)) when sampling is conducted in fritted-tip bubblers.
1.2 For concentrations of NO2 in excess of 10 mg/m3 (5 ppm(v)), as occur in industrial atmospheres, gas burner stacks, or automotive exhaust, or for samples relatively high in sulfur dioxide content, other methods should be applied. See for example Test Method D 1608.
1.3 The maximum sampling period is 60 min at a flow rate of 0.4 L/min.
1.4 The values stated in SI units are to be regarded as standard. The values given in brackets are for information only.
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. See also for other precautions.
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Designation:D1607–91(Reapproved 2005)
Standard Test Method for
Nitrogen Dioxide Content of the Atmosphere (Griess-
Saltzman Reaction)
This standard is issued under the fixed designation D1607; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D1357 Practice for Planning the Sampling of the Ambient
2 Atmosphere
1.1 This test method covers the manual determination of
D1608 Test Method for Oxides of Nitrogen in Gaseous
nitrogen dioxide (NO ) in the atmosphere in the range from 4
Combustion Products (Phenol-Disulfonic Acid Proce-
to 10 000 µg/m (0.002 to 5 ppm(v)) when sampling is
dures)
conducted in fritted-tip bubblers.
D3195 Practice for Rotameter Calibration
1.2 For concentrations of NO in excess of 10 mg/m (5
D3609 Practice for Calibration Techniques Using Perme-
ppm(v)), as occur in industrial atmospheres, gas burner stacks,
ation Tubes
or automotive exhaust, or for samples relatively high in sulfur
D3631 Test Methods for Measuring Surface Atmospheric
dioxide content, other methods should be applied. See for
Pressure
example Test Method D1608.
E1 Specification for ASTM Liquid-in-Glass Thermometers
1.3 The maximum sampling period is 60 min at a flow rate
E128 Test Method for Maximum Pore Diameter and Per-
of 0.4 L/min.
meability of Rigid Porous Filters for Laboratory Use
1.4 The values stated in SI units are to be regarded as
standard.Thevaluesgiveninbracketsareforinformationonly.
3. Terminology
1.5 This standard does not purport to address all of the
3.1 For definitions of terms used in this test method, refer to
safety concerns, if any, associated with its use. It is the
Terminology D1356.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use. See also 7.2.2 for
4.1 The NO is absorbed in an azo-dye-forming reagent
other precautions.
(1). Ared-violet color is produced within 15 min, the intensity
2. Referenced Documents of which is measured spectrophotometrically at 550 nm.
2.1 ASTM Standards:
5. Significance and Use
D1071 Test Methods for Volumetric Measurement of Gas-
5.1 Nitrogendioxideplaysanimportantroleinphotochemi-
eous Fuel Samples
cal smog-forming reactions and, in sufficient concentrations, is
D1193 Specification for Reagent Water
deleterious to health, agriculture, materials, and visibility.
D1356 Terminology Relating to Sampling and Analysis of
5.2 In combustion processes, significant amounts of nitric
Atmospheres
oxide (NO) may be produced by combination of atmospheric
nitrogen and oxygen; at ambient temperatures NO can be
converted to NO by oxygen and other atmospheric oxidants.
This test method is under the jurisdiction of ASTM Committee D22 on Air
Nitrogendioxidemayalsobegeneratedfromprocessesinvolv-
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient
ing nitric acid, nitrates, the use of explosives, and welding.
Atmospheres and Source Emissions.
Current edition approved Oct. 1, 2005. Published January 2006. Originally
6. Interferences
´1
approved in 1958. Last previous edition approved in 2000 as D1607 - 91(2000) .
DOI: 10.1520/D1607-91R05.
6.1 Aten-foldratioofsulfurdioxide(SO )toNO produces
2 2
Adapted from “Selected Methods for the Measurement ofAir Pollutants,” PHS
no effect. A thirty-fold ratio slowly bleaches the color to a
Publication No 999-AP-11, May 1965. A similar version has been submitted to the
slight extent. The addition of acetone to the reagent retards the
Intersociety Committee.
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 boldface numbers in parentheses refer to the list of references appended to
the ASTM website. this method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1607–91 (2005)
fadingbyformingatemporaryadditionproductwithSO .This 7.2.3 Rinse the bubbler thoroughly with water and allow to
permits reading the color intensity within 4 to 5 h (instead of dry before using.
the 45 min required without the acetone) without appreciable 7.3 Mist Eliminator or Gas Drying Tube, filled with acti-
losses. vated charcoal or soda lime is used to prevent damage to the
6.2 A five-fold ratio of ozone to NO will cause a small flowmeter and pump.
interference, the maximal effect occurring in 3 h. The reagent 7.4 Air-Metering Device—Acalibrated, glass, variable-area
assumes a slightly orange tint. flowmeter, or dry gas meter coupled with a flow indicator
6.3 Peroxyacetyl nitrate (PAN) can produce a color change capable of accurately measuring a flow of 0.4 L/min.
in the absorbing reagent. However, in ordinary ambient air, the 7.5 Thermometer—ASTM Thermometer 33C, meeting the
concentration of PAN is too low to cause any significant error requirements of Specification E1, will be suitable for most
in the measurement of NO . applications of this test method.
6.4 Interferences may exist from other nitrogen oxides and 7.6 Manometer, accurate to 670 Pa (0.20 in. Hg). See Test
other gases that might be found in polluted air. Methods D3631.
7.7 Air Pump—A suction pump capable of drawing the
7. Apparatus
required sample flow for intervals of up to 60 min is suitable.
7.8 Spectrophotometer or Colorimeter— An instrument
7.1 Sampling Probe—A glass or TFE-fluorocarbon (pre-
suitable for measuring the intensity of absorption at 550 nm,
ferred) tube, 6 to 10 mm in diameter provided with a
with stoppered tubes or cuvettes. The wavelength band-width
downwindfacingintake(funnelortip).Thedeadvolumeofthe
is not critical for this determination.
system should be kept minimal to avoid losses of NO on the
7.9 Stopwatch or Timer.
surfaces of the apparatus.
7.2 Absorber—An all-glass bubbler with a 60-µm maxi-
8. Reagents and Materials
mum pore diameter frit, similar to that illustrated in Fig. 1.
7.2.1 The porosity of the fritted bubbler, as well as the 8.1 Reagent grade chemicals shall be used in all tests. All
reagents shall conform to the specifications of the Committee
sampling flow rate, affect absorption efficiency. An efficiency
of over 95 % may be expected with a flow rate of 0.4 L/min or on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
less and a maximum pore diameter of 60 µm. Frits having a
used, provided it is first ascertained that the reagent is of
maximum pore diameter less than 60 µm will have a higher
sufficiently high purity to permit its use without lessening the
efficiency but will require an inconvenient pressure drop for
accuracy of the determination.
sampling. Considerably lower efficiencies are obtained with
8.2 Purity of Water—Unless otherwise indicated, water
coarser frits.
shall be deionized water in accordance with Specification
7.2.2 Measure the porosity of an absorber in accordance
D1193 for Type I or II reagent water. Water shall be free of
with Test Method E128. If the frit is clogged or visibly
nitrite.
discolored, carefully clean with concentrated chromic-sulfuric
acid mixture, and rinse well with water and redetermine the 8.3 Absorbing Reagent—Dissolve5gof anhydrous sulfa-
nilic acid (or 5.5 g of sulfanilic acid monohydrate) in almost a
maximum pore diameter.
L of water containing 140 mL of glacial acetic acid. Gentle
NOTE 1—Caution: Do not dispose of this reagent in the drain system.
heating is permissible to speed up the process. To the cooled
mixture, add 20 mL of the 0.1 % stock solution of N-(1-
naphthyl)-ethylenediamine dihydrochloride, and 10 mL of
acetone. Dilute to 1 L. The solution will be stable for several
months if kept well-stoppered in a brown bottle in the
refrigerator. The absorbing reagent shall be at room tempera-
ture before use. Avoid lengthy contact with air during prepa-
rationandusesincediscolorationofreagentwillresultbecause
of absorption of NO .
8.4 N-(1-Naphthyl)-Ethylenediamine Dihydrochloride,
Stock Solution (0.1 %)—Dissolve 0.1 g of the reagent in 100
mL of water. Solution will be stable for several months if kept
well-stoppered in a brown bottle in the refrigerator. (Alterna-
tively,preweighedamountsofthesolidreagentmaybestored.)
8.5 Sodium Nitrite, Standard Solution (0.0246 g/L)—One
mL of this working solution of sodium nitrite (NaNO )
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
FIG. 1 Fritted Bubbler for Sampling Nitrogen Dioxide MD.
D1607–91 (2005)
produces a color equivalent to that of 20 µg of NO in1Lof slope of the line, and denote it as K, the volume of NO ,inµL,
2 2
airat101kPa(29.92in.Hg)and25°C(see10.1).Preparefresh intercepted at an absorbance of 1.0.
just before use by dilution from a stock solution containing 10.2.2 Alternate Procedure:
2.46 g of the reagent grade granular solid per litre. Assay the 10.2.2.1 Standardization is based upon the empirical obser-
solid reagent. The stock solution is stable for 90 days at room vation (1, 2, 5) that 0.82 mol of NaNO produces the same
temperature, and for 1 year in a brown bottle under refrigera- color as 1 m
...
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