ASTM D3268-91(2005)
(Test Method)Standard Test Method for Separation and Collection of Particulate and Gaseous Fluorides in the Atmosphere (Sodium Bicarbonate-Coated Glass Tube and Particulate Filter Method)
Standard Test Method for Separation and Collection of Particulate and Gaseous Fluorides in the Atmosphere (Sodium Bicarbonate-Coated Glass Tube and Particulate Filter Method)
SIGNIFICANCE AND USE
The sodium bicarbonate coated tube filter method provides a means of separating and collecting atmospheric gaseous fluoride and particulate fluoride samples.
Since the samples are collected on the dry tube and filter, the fluoride may be eluted with a small volume of eluant (see Section 10 for specific instructions on fluoride elution). Elution into a small volume and the sensitivity of the analytical methods employed allow the analysis of the collected fluoride to fractional parts of a microgram per cubic metre on samples taken for a 12-h period.
SCOPE
1.1 The sodium bicarbonate-coated glass tube and membrane filter method provides a means for the separation and collection of gaseous atmospheric forms of fluoride reactive with sodium bicarbonate and particulate forms of fluoride which are collected by a filter. The test method is applicable to 12-h sampling periods, collecting 1 to 500 g of gaseous fluoride at a 15 L/min [0.5 ft3/min] sampling rate or about 0.1 to 50 g/m 3. The length of the sampling period can therefore be adjusted so that the amount of fluoride collected will fall within this range. The actual lower limit of the test method will depend upon the sensitivity of the analytical method employed and the quality of reagents used in tube preparation and analysis. It is recommended that the lower limit of detection should be considered as two times the standard deviation of the monthly arithmetic mean blank value. Any values greater than the blank by less than this amount should be reported as "blank value."
1.2 The values stated in SI units are to be regarded as standard. The inch-pound units in brackets may be approximate.
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.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3268 – 91 (Reapproved 2005)
Standard Test Method for
Separation and Collection of Particulate and Gaseous
Fluorides in the Atmosphere (Sodium Bicarbonate-Coated
Glass Tube and Particulate Filter Method)
This standard is issued under the fixed designation D3268; 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 D1356 Terminology Relating to Sampling and Analysis of
Atmospheres
1.1 The sodium bicarbonate-coated glass tube and mem-
D1357 Practice for Planning the Sampling of the Ambient
brane filter method provides a means for the separation and
Atmosphere
collection of gaseous atmospheric forms of fluoride reactive
D3266 Test Method for Automated Separation and Collec-
with sodium bicarbonate and particulate forms of fluoride
tion of Particulate and Acidic Gaseous Fluoride in the
which are collected by a filter. The test method is applicable to
Atmosphere (Double Paper Tape Sampler Method)
12-h sampling periods, collecting 1 to 500 µg of gaseous
D3267 Test Method for Separation and Collection of Par-
fluoride at a 15 L/min [0.5 ft /min] sampling rate or about 0.1
ticulate and Water-Soluble Gaseous Fluorides in the At-
to50µg/m .Thelengthofthesamplingperiodcanthereforebe
mosphere (Filter and Impinger Method)
adjustedsothattheamountoffluoridecollectedwillfallwithin
D3269 Test Methods for Analysis for Fluoride Content of
this range. The actual lower limit of the test method will
the Atmosphere and Plant Tissues (Manual Procedures)
depend upon the sensitivity of the analytical method employed
D3270 Test Methods for Analysis for Fluoride Content of
and the quality of reagents used in tube preparation and
the Atmosphere and Plant Tissues (Semiautomated
analysis. It is recommended that the lower limit of detection
Method)
shouldbeconsideredastwotimesthestandarddeviationofthe
monthly arithmetic mean blank value.Any values greater than
3. Terminology
the blank by less than this amount should be reported as “blank
3.1 Definitions—For definitions of terms used in this test
value.”
method refer to Terminology D1356.
1.2 The values stated in SI units are to be regarded as
standard. The inch-pound units in brackets may be approxi-
4. Summary of Test Method
mate.
4.1 Gaseous fluorides are removed from the air stream by
1.3 This standard does not purport to address all of the
reaction with sodium bicarbonate coated on the inside wall of
safety concerns, if any, associated with its use. It is the
a borosilicate glass tube (Note 1). Particulate fluorides are
responsibility of the user of this standard to establish appro-
collected on a filter following the tube. The fluoride collected
priate safety and health practices and determine the applica-
by the tube is eluted with water or buffer and analyzed for
bility of regulatory limitations prior to use.
fluoride. The particulate matter collected by the filter is eluted
2. Referenced Documents with acid and analyzed for fluoride (1-4) . The results are
2 reported as µg/m of gaseous or particulate in air at 25°C
2.1 ASTM Standards:
[77°F] and 101.3 kPa [29.92 in. Hg].
D1193 Specification for Reagent Water
NOTE 1—Some particulate matter will collect on the wall of the sample
tube. If this loss is to be evaluated, use test methods such as Test Method
This test method is under the jurisdiction of ASTM Committee D22 on Air
D3266orTestMethodD3267forcomparisonsincethefilterforcollecting
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient
particulate precedes the absorbers for gases Mandl and Weinstein (2)
Atmospheres and Source Emissions.
provide some information relative to potential loss of particulate matter.
Current edition approved Oct. 1, 2005. Published January 2006. Originally
´1
approved in 1973. Last previous edition approved in 2000 as D3268 - 91 (2000) .
DOI: 10.1520/D3268-91R05.
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 references at the end of this test
the ASTM website. method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3268 – 91 (2005)
FIG. 1 Sodium Bicarbonate-Coated Glass Tube Illustrating Simple Heating Device
5. Significance and Use analyses of the tubes or filters by calorimetric or electrometric
methods. This is a problem inherent with any collection
5.1 The sodium bicarbonate coated tube filter method pro-
method for fluoride.
vides a means of separating and collecting atmospheric gas-
eous fluoride and particulate fluoride samples.
7. Apparatus
5.2 Since the samples are collected on the dry tube and
filter, the fluoride may be eluted with a small volume of eluant
7.1 Glass Tubing—1200-mm [4-ft] lengths of 7-mm inside
(see Section 10 for specific instructions on fluoride elution).
diameter borosilicate glass tubing, coated with sodium bicar-
Elutionintoasmallvolumeandthesensitivityoftheanalytical
bonate, in accordance with the requirements outlined in 7.6.
methods employed allow the analysis of the collected fluoride
7.2 Filter and Holder—Connect the tubing directly to the
to fractional parts of a microgram per cubic metre on samples
filterholderandfilterforthecollectionofparticulatematterfor
taken for a 12-h period.
particulate fluoride analysis (see Fig. 2).
NOTE 2—Use of material other than that recommended in footnote 6 or
6. Interferences
Fig. 2 will result in gaseous fluoride absorption on the material.
6.1 Significant amounts of acid aerosols or gases might
7.3 Air Sampling System:
neutralize or acidify the bicarbonate coating and prevent
quantitative uptake of gaseous fluoride from the atmosphere. If 7.3.1 The tube and filter are followed by an air sampling
this potential interference needs to be evaluated, the alkalinity system which is capable of sampling at a rate of 15 L/min [0.5
of the water extract may provide relevant information. ft /min] and measuring the total air sampled on a time rate
6.2 The presence of large amounts of aluminum or certain basis or with a totalizing meter. See Test Method D3267 for
other metals or phosphates can interfere with subsequent sampling equipment, and the configuration and calibration.
D3268 – 91 (2005)
FIG. 2 Details of Attachment of the Filter Assembly and Limiting Orifice to a Bicarbonate-Coated Tube (7-mm Inside diameter).
(A) Polypropylene Filter Holder. (B) Plastic Female Connector, (C) Limiting Orifice
7.3.2 The system shall be equipped so that pressure and 7.6.1 Thecoatingshallbevisibleuniformcoatingonthefull
temperature of the gas at the point of metering also are known length of the tube.
for correcting sample volumes to standard conditions of 101.3 7.6.2 The coating shall not contain any large crystals or
kPa [29.92 in. Hg] at 25°C [77°F]. heavy local deposits which could flake off and be collected
7.3.3 Assemble the sampling system so that the inlet of the with the aerosol fluorides.
tube is 4 to 6 m above ground level (see Practice D1357) and 7.6.3 The total coating shall contain less than 1 µg of
protectedfromraininsuchamannerasnottointerferewiththe fluoride when analyzed without exposure, including all the
free passage of aerosol fluorides. reagentsusedintheprocedure.Thisisthereagentblankforthe
7.4 Light Bulb or Cone Heater, 30-W, installed to heat the procedure.
gases to a temperature where condensation will not occur. 7.6.4 Preparedtubesshallbesealeduntiltimeofuse.Serum
7.5 Configuration of Sampling Equipment—Fig. 1 is a tube caps that have been thoroughly rinsed with reagent water
sketch of the sampling system. Other systems that meet the (8.2) are recommended for this purpose.
requirements outlined, are also satisfactory. 7.6.5 Tubes shall be carried through the field procedure
7.6 Criteria for Coating of the Borosilicate Tubes: withoutexposureandalsothesubsequentanalyticalprocedures
D3268 – 91 (2005)
to provide a sampling and analytical blank value. Check any 9.1.1 Clean the tubes successively with detergent (8.3),
materials that may come into contact with the tubes for alcoholic KOH solution (8.4), and distilled water.
freedom from contamination with fluoride. These field blanks 9.1.2 While still wet from the cleaning, wet the internal
will provide the data for the monthly arithmetic mean blank surface of the tube with the 5 % NaHCO solution (8.5).
value. See Note 3.
9.1.3 Allow the tube to drain for about 10 s and dry the
coating rapidly by passing hot, dry fluoride-free air downward
NOTE 3—Do not expose the tubes except during sampling.
through the tube, while it is hanging in a vertical position.
9.1.4 Provide the hot fluoride-free air stream by blowing air
8. Reagents
througha4to 8-mesh soda-lime trap and then through 1200
8.1 Purity of Reagents—Reagent grade chemicals shall be
mm [4
...
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