ASTM D1607-91(2011)
(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 μg/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 D1608.
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 parentheses are for information only.
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. See also 7.2.2 for other precautions.
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Designation: D1607 − 91 (Reapproved 2011)
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.Anumber 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 U.S. Department of Defense.
1. Scope D1356Terminology Relating to Sampling and Analysis of
2 Atmospheres
1.1 This test method covers the manual determination of
D1357Practice for Planning the Sampling of the Ambient
nitrogen dioxide (NO ) in the atmosphere in the range from 4
3 Atmosphere
to 10 000 µg/m (0.002 to 5 ppm(v)) when sampling is
D1608Test Method for Oxides of Nitrogen in Gaseous
conducted in fritted-tip bubblers.
Combustion Products (Phenol-Disulfonic Acid Proce-
1.2 For concentrations of NO in excess of 10 mg/m (5
dures)
ppm(v)), as occur in industrial atmospheres, gas burner stacks,
D3195Practice for Rotameter Calibration
or automotive exhaust, or for samples relatively high in sulfur
D3609Practice for Calibration Techniques Using Perme-
dioxide content, other methods should be applied. See for
ation Tubes
example Test Method D1608.
D3631Test Methods for Measuring Surface Atmospheric
Pressure
1.3 The maximum sampling period is 60 min at a flow rate
of 0.4 L/min. E1Specification for ASTM Liquid-in-Glass Thermometers
E128Test Method for Maximum Pore Diameter and Perme-
1.4 The values stated in SI units are to be regarded as
ability of Rigid Porous Filters for Laboratory Use
standard. The values given in parentheses are for information
only.
3. Terminology
1.5 This standard does not purport to address all of the
3.1 Fordefinitionsoftermsusedinthistestmethod,referto
safety concerns, if any, associated with its use. It is the
Terminology D1356.
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
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-violetcolorisproducedwithin15min,theintensity
of which is measured spectrophotometrically at 550 nm.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 Nitrogendioxideplaysanimportantroleinphotochemi-
D1071Test Methods for Volumetric Measurement of Gas-
cal smog-forming reactions and, in sufficient concentrations, is
eous Fuel Samples
deleterious to health, agriculture, materials, and visibility.
D1193Specification for Reagent Water
5.2 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
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient converted to NO by oxygen and other atmospheric oxidants.
Atmospheres and Source Emissions.
Nitrogendioxidemayalsobegeneratedfromprocessesinvolv-
Current edition approved Oct. 1, 2011. Published October 2011. Originally
ing nitric acid, nitrates, the use of explosives, and welding.
approved in 1958. Last previous edition approved in 2005 as D1607–91(2005).
DOI: 10.1520/D1607-91R11.
6. Interferences
Adaptedfrom“SelectedMethodsfortheMeasurementofAirPollutants,”PHS
Publication No 999-AP-11, May 1965.Asimilar version has been submitted to the
6.1 Aten-foldratioofsulfurdioxide(SO)toNO produces
2 2
Intersociety Committee.
no effect. A thirty-fold ratio slowly bleaches the color to a
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 (2011)
slight extent.The addition of acetone to the reagent retards the acid mixture, and rinse well with water and redetermine the
fadingbyformingatemporaryadditionproductwithSO .This maximum pore diameter.
permits reading the color intensity within 4 to 5 h (instead of
NOTE 1—Caution: Do not dispose of this reagent in the drain system.
the 45 min required without the acetone) without appreciable
7.2.3 Rinse the bubbler thoroughly with water and allow to
losses.
dry before using.
6.2 A five-fold ratio of ozone to NO will cause a small
7.3 Mist Eliminator or Gas Drying Tube, filled with acti-
interference, the maximal effect occurring in 3 h. The reagent
vated charcoal or soda lime is used to prevent damage to the
assumes a slightly orange tint.
flowmeter and pump.
6.3 Peroxyacetyl nitrate (PAN) can produce a color change
7.4 Air-Metering Device—Acalibrated, glass, variable-area
intheabsorbingreagent.However,inordinaryambientair,the
flowmeter, or dry gas meter coupled with a flow indicator
concentration of PAN is too low to cause any significant error
capable of accurately measuring a flow of 0.4 L/min.
in the measurement of NO .
7.5 Thermometer—ASTM Thermometer 33C, meeting the
6.4 Interferences may exist from other nitrogen oxides and
requirements of Specification E1, will be suitable for most
other gases that might be found in polluted air.
applications of this test method.
7. Apparatus
7.6 Manometer, accurate to 670 Pa (0.20 in. Hg). See Test
7.1 Sampling Probe—A glass or TFE-fluorocarbon (pre- Methods D3631.
ferred) tube, 6 to 10 mm in diameter provided with a
7.7 Air Pump—A suction pump capable of drawing the
downwindfacingintake(funnelortip).Thedeadvolumeofthe
required sample flow for intervals of up to 60 min is suitable.
system should be kept minimal to avoid losses of NO on the
7.8 Spectrophotometer or Colorimeter— An instrument
surfaces of the apparatus.
suitable for measuring the intensity of absorption at 550 nm,
7.2 Absorber—Anall-glassbubblerwitha60-µmmaximum
with stoppered tubes or cuvettes. The wavelength band-width
pore diameter frit, similar to that illustrated in Fig. 1.
is not critical for this determination.
7.2.1 The porosity of the fritted bubbler, as well as the
7.9 Stopwatch or Timer.
sampling flow rate, affect absorption efficiency. An efficiency
of over 95% may be expected with a flow rate of 0.4 L/min or
8. Reagents and Materials
less and a maximum pore diameter of 60 µm. Frits having a
maximum pore diameter less than 60 µm will have a higher
8.1 Reagent grade chemicals shall be used in all tests. All
efficiency but will require an inconvenient pressure drop for
reagents shall conform to the specifications of the Committee
sampling. Considerably lower efficiencies are obtained with
on Analytical Reagents of the American Chemical Society,
coarser frits.
where such specifications are available. Other grades may be
7.2.2 Measure the porosity of an absorber in accordance
used, provided it is first ascertained that the reagent is of
with Test Method E128. If the frit is clogged or visibly
sufficiently high purity to permit its use without lessening the
discolored, carefully clean with concentrated chromic-sulfuric
accuracy of the determination.
8.2 Purity of Water—Unlessotherwiseindicated,watershall
bedeionizedwaterinaccordancewithSpecificationD1193for
Type I or II reagent water. Water shall be free of nitrite.
8.3 Absorbing Reagent—Dissolve5gof anhydrous sulfa-
nilic acid (or 5.5 g of sulfanilic acid monohydrate) in almost a
L of water containing 140 mL of glacial acetic acid. Gentle
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 .
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 (2011)
8.4 N-(1-Naphthyl)-Ethylenediamine Dihydrochloride, weight of NaNO is 69.1, this is equivalent to (24.6/
Stock Solution (0.1 %)—Dissolve 0.1 g of the reagent in 100 69.1)×(46.0⁄0.82)=20 µg NO .
mLof water. Solution will be stable for several months if kept 10.2.2.2 For convenience, standard conditions are taken as
well-stoppered in a brown bottle in the refrigerator. 101 kPa (29.92 in. Hg) and 25°C, at which the molar gas
(Alternatively, preweighed amounts of the solid reagent may volumeis24.47L.Thisisveryclosetothestandardconditions
be stored.) used for air-handling equipment–101 kPa (29.92 in. Hg), 70°F
(21.1°C), and 50% relative humidity, at which the molar gas
8.5 Sodium Nitrite, Standard Solution (0.0246 g/L)—One
volume is 24.76 L, or 1.2% greater. Ordinarily, the correction
mL of this working solution of sodium nitrite (NaNO )
ofthesamplevolumetothesestandardconditionsisslightand
produces a color equivalent to that of 20 µg of NO in1Lof
may be omitted, however, for greatest bias, it may be made by
airat101kPa(29.92in.Hg)and25°C(see10.1).Preparefresh
m
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