ASTM D3268-91(2011)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3268 − 91 (Reapproved 2011)
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 U.S. 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
3 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
(Withdrawn 2010)
and the quality of reagents used in tube preparation and
D3270 Test Methods for Analysis for Fluoride Content of
analysis. It is recommended that the lower limit of detection
the Atmosphere and Plant Tissues (Semiautomated
shouldbeconsideredastwotimesthestandarddeviationofthe
Method)
monthly arithmetic mean blank value.Any values greater than
the blank by less than this amount should be reported as “blank
3. Terminology
value.”
3.1 Definitions—For definitions of terms used in this test
1.2 The values stated in SI units are to be regarded as
method refer to Terminology D1356.
standard.The inch-pound units in parentheses may be approxi-
mate.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
4.1 Gaseous fluorides are removed from the air stream by
safety concerns, if any, associated with its use. It is the
reaction with sodium bicarbonate coated on the inside wall of
responsibility of the user of this standard to establish appro-
a borosilicate glass tube (Note 1). Particulate fluorides are
priate safety and health practices and determine the applica-
collected on a filter following the tube. The fluoride collected
bility of regulatory limitations prior to use.
by the tube is eluted with water or buffer and analyzed for
fluoride. The particulate matter collected by the filter is eluted
2. Referenced Documents
with acid and analyzed for fluoride (1-4). The results are
2.1 ASTM Standards: 3
reported as µg/m of gaseous or particulate in air at 25°C
D1193 Specification for Reagent Water
(77°F) and 101.3 kPa (29.92 in. Hg).
NOTE 1—Some particulate matter will collect on the wall of the sample
This test method is under the jurisdiction of ASTM Committee D22 on Air
tube. If this loss is to be evaluated, use 7test methods such asTest Method
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient
D3266orTestMethodD3267forcomparisonsincethefilterforcollecting
Atmospheres and Source Emissions.
particulate precedes the absorbers for gases Mandl and Weinstein (2)
Current edition approved Oct. 1, 2011. Published October 2011. Originally
approved in 1973. Last previous edition approved in 2005 as D3268 – 91 (2005).
DOI: 10.1520/D3268-91R11.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM www.astm.org.
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 (2011)
FIG. 1 Sodium Bicarbonate-Coated Glass Tube Illustrating Simple Heating Device
provide some information relative to potential loss of particulate matter.
6.2 The presence of large amounts of aluminum or certain
other metals or phosphates can interfere with subsequent
5. Significance and Use
analyses of the tubes or filters by calorimetric or electrometric
5.1 The sodium bicarbonate coated tube filter method pro- methods. This is a problem inherent with any collection
vides a means of separating and collecting atmospheric gas-
method for fluoride.
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
Elutionintoasmallvolumeandthesensitivityoftheanalytical
bicarbonate, in accordance with the requirements outlined in
methods employed allow the analysis of the collected fluoride
7.6.
to fractional parts of a microgram per cubic metre on samples
7.2 Filter and Holder—Connect the tubing directly to the
taken for a 12-h period.
filterholderandfilterforthecollectionofparticulatematterfor
particulate fluoride analysis (see Fig. 2).
6. Interferences
NOTE 2—Use of material other than that recommended in footnote 6 or
6.1 Significant amounts of acid aerosols or gases might
Fig. 2 will result in gaseous fluoride absorption on the material.
neutralize or acidify the bicarbonate coating and prevent
quantitative uptake of gaseous fluoride from the atmosphere. If 7.3 Air Sampling System:
this potential interference needs to be evaluated, the alkalinity 7.3.1 The tube and filter are followed by an air sampling
of the water extract may provide relevant information. system which is capable of sampling at a rate of 15 L/min (0.5
D3268 − 91 (2011)
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
ft /min) and measuring the total air sampled on a time rate 7.5 Configuration of Sampling Equipment—Fig. 1 is a
basis or with a totalizing meter. See Test Method D3267 for sketch of the sampling system. Other systems that meet the
sampling equipment, and the configuration and calibration. requirements outlined, are also satisfactory.
7.3.2 The system shall be equipped so that pressure and
7.6 Criteria for Coating of the Borosilicate Tubes:
temperature of the gas at the point of metering also are known
7.6.1 Thecoatingshallbevisibleuniformcoatingonthefull
for correcting sample volumes to standard conditions of 101.3
length of the tube.
kPa (29.92 in. Hg) at 25°C (77°F).
7.6.2 The coating shall not contain any large crystals or
7.3.3 Assemble the sampling system so that the inlet of the
heavy local deposits which could flake off and be collected
tube is 4 to 6 m above ground level (see Practice D1357) and
with the aerosol fluorides.
protectedfromraininsuchamannerasnottointerferewiththe
7.6.3 The total coating shall contain less than 1 µg of
free passage of aerosol fluorides.
fluoride when analyzed without exposure, including all the
7.4 Light Bulb or Cone Heater, 30-W, installed to heat the reagentsusedintheprocedure.Thisisthereagentblankforthe
gases to a temperature where condensation will not occur. procedure.
D3268 − 91 (2011)
7.6.4 Preparedtubesshallbesealeduntiltimeofuse.Serum acid] to 500 mL of distilled water. Stir and add 5 N NaOH
tube caps that have been thoroughly rinsed with reagent water solution (8.7) slowly until pH is between 5.0 and 5.5. Cool and
(8.2) are recommended for this purpose. dilute to 1 L.
7.6.5 Tubes shall be carried through the field procedure
8.10 TISAB (1+1)—Dilute the full strength TISAB (8.9)
withoutexposureandalsothesubsequentanalyticalprocedures
with an equal amount of water.
to provide a sampling and analytical blank value. Check any
8.11 Wetting Agent, for use in the sodium bicarbonate
materials that may come into contact with the tubes for
solution to promote even wetting of the tube.
freedom from contamination with fluoride. These field blanks
will provide the data for the monthly arithmetic mean blank
9. Procedure
value. See Note 3.
9.1 Coating of Borosilicate Glass Tubes:
NOTE 3—Do not expose the tubes except during sampling.
9.1.1 Clean the tubes successively with detergent (8.3),
alcoholic KOH solution (8.4), and distilled water.
8. Reagents
9.1.2 While still wet from the cleaning, wet the internal
8.1 Purity of Reagents—Reagent grade chemicals shall be
surface of the tube wit
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