ASTM D3268-91(2000)e1
(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)
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 [mu]g of gaseous fluoride at a 15 L/min (0.5 ft /min) sampling rate or about 0.1 to 50 [mu]g/m . 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 parentheses may be approximate.
1.3 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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e1
Designation: D 3268 – 91 (Reapproved 2000)
Standard Test Method for
Separation and Collection of Particulate and Gaseous
Fluorides in the Atmosphere (Sodium Bicarbonate-Coated
1,2
Glass Tube and Particulate Filter Method)
This standard is issued under the fixed designation D 3268; 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.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—Editorial corrections were made throughout in March 2000.
1. Scope 2. Referenced Documents
1.1 The sodium bicarbonate-coated glass tube and mem- 2.1 ASTM Standards:
brane filter method provides a means for the separation and D 1193 Specification for Reagent Water
collection of gaseous atmospheric forms of fluoride reactive D 1356 Terminology Relating to Sampling and Analysis of
with sodium bicarbonate and particulate forms of fluoride Atmospheres
which are collected by a filter. The test method is applicable to D 1357 Practice for Planning the Sampling of the Ambient
12-h sampling periods, collecting 1 to 500 µg of gaseous Atmosphere
fluoride at a 15 L/min (0.5 ft /min) sampling rate or about 0.1 D 3266 Test Method forAutomated Separation and Collec-
to 50 µg/m . The length of the sampling period can therefore tion of Particulate and Acidic Gaseous Fluoride in the
be adjusted so that the amount of fluoride collected will fall Atmosphere (Double Paper Tape Sampler Method)
within this range.The actual lower limit of the test method will D 3267 Test Method for Separation and Collection of Par-
depend upon the sensitivity of the analytical method employed ticulate and Water-Soluble Gaseous Fluorides in the At-
and the quality of reagents used in tube preparation and mosphere (Filter and Impinger Method)
analysis. It is recommended that the lower limit of detection D 3269 Test Methods for Analysis for Fluoride Content of
should be considered as two times the standard deviation of the the Atmosphere and Plant Tissues (Manual Procedures)
monthly arithmetic mean blank value.Any values greater than D 3270 Test Methods for Analysis for Fluoride Content of
the blank by less than this amount should be reported as “blank the Atmosphere and Plant Tissues (Semiautomated
value.” Method)
1.2 The values stated in SI units are to be regarded as
3. Terminology
standard.The inch-pound units in parentheses may be approxi-
mate. 3.1 Definitions—For definitions of terms used in this test
method refer to Terminology D 1356.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Gaseous fluorides are removed from the air stream by
priate safety and health practices and determine the applica-
reaction with sodium bicarbonate coated on the inside wall of
bility of regulatory limitations prior to use.
a borosilicate glass tube (Note 1). Particulate fluorides are
collected on a filter following the tube. The fluoride collected
This test method is under the jurisdiction of ASTM Committee D-22 on
by the tube is eluted with water or buffer and analyzed for
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom-
fluoride. The particulate matter collected by the filter is eluted
mittee D22.03 on Ambient Atmospheres and Source Emissions.
with acid and analyzed for fluoride (1-4) . The results are
Current edition approved July 15, 1991. Published October 1991. Originally
published as D 3268 – 73 T. Last previous edition D 3268 – 89.
This test method was originally editorially adapted from the Intersociety
CommitteeMethod 42222-01-72T;12202-03-72T,“HealthLaboratoryScience”Vol Annual Book of ASTM Standards, Vol. 11.01.
9, No. 4, 1972, pp. 308–313. This revision has been adapted from “Methods ofAir Annual Book of ASTM Standards, Vol. 11.03.
Sampling and Analysis,” Intersociety Committee, James P. Lodge, Jr., ed., 3rd ed., The boldface numbers in parentheses refer to references at the end of this test
Lewis Publishers, Inc., 1989, pp. 347–351. method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 3268
FIG. 1 Sodium Bicarbonate-Coated Glass Tube Illustrating Simple Heating Device
reported as µg/m of gaseous or particulate in air at 25°C 6. Interferences
(77°F) and 101.3 kPa (29.92 in. Hg).
6.1 Significant amounts of acid aerosols or gases might
neutralize or acidify the bicarbonate coating and prevent
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
quantitative uptake of gaseous fluoride from the atmosphere. If
D 3266 or Test Method D 3267 for comparison since the filter for
this potential interference needs to be evaluated, the alkalinity
collecting particulate precedes the absorbers for gases Mandl and Wein-
of the water extract may provide relevant information.
stein (2) provide some information relative to potential loss of particulate
6.2 The presence of large amounts of aluminum or certain
matter.
other metals or phosphates can interfere with subsequent
analyses of the tubes or filters by calorimetric or electrometric
5. Significance and Use
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
7.1 Glass Tubing—1200-mm (4-ft) lengths of 7-mm inside
filter, the fluoride may be eluted with a small volume of eluant
diameter borosilicate glass tubing, coated with sodium bicar-
(see Section 10 for specific instructions on fluoride elution).
bonate, according to the requirements outlined in 7.6.
Elutionintoasmallvolumeandthesensitivityoftheanalytical
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 (Fig. 2).
D 3268
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
NOTE 2—Use of material other than that recommended in footnote 6 or
7.4 Light Bulb or Cone Heater, 30-W, installed to heat the
Fig. 2 will result in gaseous fluoride absorption on the material.
gases to a temperature where condensation will not occur.
7.3 Air Sampling System:
7.5 Configuration of Sampling Equipment—Fig. 1 is a
7.3.1 The tube and filter are followed by an air sampling
sketch of the sampling system. Other systems that meet the
system which is capable of sampling at a rate of 15 L/min (0.5
requirements outlined, are also satisfactory.
ft /min) and measuring the total air sampled on a time rate
7.6 Criteria for Coating of the Borosilicate Tubes:
basis or with a totalizing meter. See Test Method D 3267 for
7.6.1 Thecoatingshallbevisibleuniformcoatingonthefull
sampling equipment, and the configuration and calibration.
length of the tube.
7.3.2 The system shall be equipped so that pressure and
7.6.2 The coating shall not contain any large crystals or
temperature of the gas at the point of metering also are known
heavy local deposits which could flake off and be collected
for correcting sample volumes to standard conditions of 101.3
with the aerosol fluorides.
kPa (29.92 in. Hg) at 25°C (77°F).
7.6.3 The total coating shall contain less than 1 µg of
7.3.3 Assemble the sampling system so that the inlet of the
tube is 4 to 6 m above ground level (see Practice D 1357) and fluoride when analyzed without exposure, including all the
reagentsusedintheprocedure.Thisisthereagentblankforthe
protectedfromraininsuchamannerasnottointerferewiththe
free passage of aerosol fluorides. procedure.
D 3268
7.6.4 Preparedtubesshallbesealeduntiltimeofuse.Serum 8.11 Wetting Agent, for use in the sodium bicarbonate
tube caps that have been thoroughly rinsed with reagent water solution to promote even wetting of the tube.
(8.2) are recommended for this purpose.
9. Procedure
7.6.5 Tubes shall be carried through the field procedure
9.1 Coating of Borosilicate Glass Tubes:
withoutexposureandalsothesubsequentanalyticalprocedures
9.1.1 Clean the tubes successively with detergent (8.3),
to provide a sampling and analytical blank value. Check any
alcoholic KOH solution (8.4), and distilled water.
materials that may come into contact with the tubes for
9.1.2 While still wet from the cleaning, wet the internal
freedom from contamination with fluoride. These field blanks
surface of the tube with the 5 % NaHCO solution (8.5).
will provide the data for the monthly arithmetic mean blank
9.1.3 Allow the tube to drain for about 10 s and dry the
value. See Note 3.
coating rapidly by passing hot, dry fluoride-free air downward
NOTE 3—Do not expose
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