ASTM D3266-91(2005)
(Test Method)Standard Test Method for Automated Separation and Collection of Particulate and Acidic Gaseous Fluoride in the Atmosphere (Double Paper Tape Sampler Method)
Standard Test Method for Automated Separation and Collection of Particulate and Acidic Gaseous Fluoride in the Atmosphere (Double Paper Tape Sampler Method)
SIGNIFICANCE AND USE
This test method provides a means of automatically separating and collecting atmospheric particulate and acidic gaseous fluoride samples.
Since the samples are collected on dry tapes, the samples are in a form which allows elution of the fluoride content with a small volume of eluent. Consequently, the method allows analyses of air samples taken for a time period as short as several minutes.
SCOPE
1.1 This test method describes the automatic separation and collection on chemically treated paper tapes of particulate and gaseous forms of acidic fluorides in the atmosphere by means of a double paper tape sampler. The sampler may be programmed to collect and store individual air samples obtained over time periods from several minutes to 3 h. A 30.5-m [100-ft] tape will allow unattended operation for the automatic collection of up to 600 samples.
1.2 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3266–91(Reapproved2005)
Standard Test Method for
Automated Separation and Collection of Particulate and
Acidic Gaseous Fluoride in the Atmosphere (Double Paper
Tape Sampler Method)
This standard is issued under the fixed designation D3266; 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 D3269 Test Methods for Analysis for Fluoride Content of
the Atmosphere and Plant Tissues (Manual Procedures)
1.1 This test method describes the automatic separation and
D3270 Test Methods for Analysis for Fluoride Content of
collection on chemically treated paper tapes of particulate and
the Atmosphere and Plant Tissues (Semiautomated
gaseous forms of acidic fluorides in the atmosphere by means
Method)
of a double paper tape sampler. The sampler may be pro-
D3609 Practice for Calibration Techniques Using Perme-
grammed to collect and store individual air samples obtained
ation Tubes
over time periods from several minutes to 3 h. A 30.5-m
D3614 Guide for Laboratories Engaged in Sampling and
[100-ft] tape will allow unattended operation for the automatic
Analysis of Atmospheres and Emissions
collection of up to 600 samples.
1.2 The values stated in SI units are to be regarded as
3. Terminology
standard.Thevaluesgiveninbracketsareforinformationonly.
3.1 Definitions—For definitions of terms used in this test
1.3 This standard does not purport to address all of the
method, refer to Terminology D1356.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 Air is drawn through an air inlet tube (see Practice
bility of regulatory limitations prior to use.
D1357) and is first passed through an acid-treated prefilter
paper tape to remove particulate matter which may contain
2. Referenced Documents
fluoride and then through an alkali-treated paper tape to
2.1 ASTM Standards:
remove acidic fluoride gases.
D1071 Test Methods for Volumetric Measurement of Gas-
4.2 The exhaust air is filtered through soda lime-glass wool,
eous Fuel Samples
and the cleaned air is used to pressurize the front compartment
D1193 Specification for Reagent Water
to prevent fluoride contamination of the paper tapes from the
D1356 Terminology Relating to Sampling and Analysis of
ambient air.
Atmospheres
4.3 Automatically, at the end of the preset sampling period,
D1357 Practice for Planning the Sampling of the Ambient
the vacuum pump is turned off, the tapes are indexed, and after
Atmosphere
indexing the vacuum pump is turned on. Indexing results in a
D3195 Practice for Rotameter Calibration
“dead time” of several seconds.
D3268 Test Method for Separation and Collection of Par-
4.4 The paper tapes are removed from the sampler after a
ticulateandGaseousFluoridesintheAtmosphere(Sodium
selected period of operation and taken to an analytical work
Bicarbonate-Coated Glass Tube and Particulate Filter
area where the individual sample spots are cut out, treated to
Method)
dissolve the fluoride, and analyzed by potentiometric or pho-
3,4,5
tometric methods.
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
Atmospheres and Source Emissions.
Current edition approved Oct. 1, 2005. Published January 2006. Originally Mandl, R. H., Weinstein, L. H., Weiskopf, G. J., and Major, J. L. “The
´1
approved in 1973. Last previous edition approved in 2000 as D3266 - 91(2000) . SeparationandCollectionofGaseousandParticulateFluorides.”PaperCP-25A,2D
DOI: 10.1520/D3266-91R05. International Clean Air Congress, Washington, DC, 1970.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Weinstein, L. H., and Mandl, R. H. “The Separation and Collection of Gaseous
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM and Particulate Fluorides.” VDI Berichte Nr. Vol 164, 1971, pp. 53 to 63.
Standards volume information, refer to the standard’s Document Summary page on Lodge, James P. Jr., ed., “Methods ofAir Sampling andAnalysis,” Intersociety
the ASTM website. Committee, 3rd ed., Lewis Publishers, Inc., 1988, pp. 352–356.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3266–91 (2005)
5. Significance and Use
5.1 This test method provides a means of automatically
separating and collecting atmospheric particulate and acidic
gaseous fluoride samples.
5.2 Since the samples are collected on dry tapes, the
samples are in a form which allows elution of the fluoride
content with a small volume of eluent. Consequently, the
method allows analyses of air samples taken for a time period
as short as several minutes.
6. Interferences
6.1 Particulate metallic salts, such as those of aluminum,
iron, calcium, magnesium or rare-earth elements, may react
with and remove some or all of the acidic gaseous fluoride on
the prefilter. If interfering quantities of such particulate metal-
lic salts are present, the use of Test Methods D3268 is
recommended because the acidic fluoride gases are collected
prior to the filter.
6.2 Acid aerosols or gases might neutralize or acidify the
alkali-treated tape and prevent quantitative uptake of the acidic
fluoride gases from the atmosphere. If this potential interfer-
ence is present the decreased alkalinity of the water extract
(13.2.2.1) may provide relevant information.
6.3 Aluminum or certain other metals or phosphates can
interfere with subsequent analyses of the tapes by photometric
or electrometric methods. These potential interferences are
discussed in Test Methods D3269 and D3270.
FIG. 1 Dual Tape Sampler Flow Schematic
6.4 There are several limitations of the test method that
could possibly occur:
6.4.1 Although the acid-treated medium retentive prefilter
of 25 W/m (8 W/ft). The tube is connected to the instrument
has been shown to allow passage of hydrofluoric acid, it will
with a TFE-fluorocarbon fitting.
restrict passage of particulate matter only as small as about 1
7.1.1.1 Rainshield, R —Constructed of TFE-fluorocarbon.
s
µm.Thus,smallerparticulatemattermaypassthroughthefilter
7.1.1.2 Proportional Temperature Controller—H , with
and impinge on or pass through the alkali-treated second tape.
thermocouple reference point located at the bottom of the
6.4.2 The maximum sampling time recommended in the
sample chamber.
method is 3 h. This time is limited to minimize the possible
7.1.1.3 Inlet Thermostat—T .
effect of particulate matter sorbing the acidic fluoride gases or
7.1.1.4 Inlet Pressure Gauge—M with shutoff valve, V .
5 1
reducing the sampling rate.
One side of the gauge is connected to a TFE-fluorocarbon run
tee placed between the intake tube and the sample block, and
7. Apparatus
the other side is connected to a TFE-fluorocarbon run tee
7.1 The double paper tape sampler is a modification of and
placed at the entrance to the intake tubing.
utilizes the basic principles of the sequential paper tape
7.1.2 Sampler—See Figs. 1 and 2.
sampler used for dust collection. The commercially available
7.1.2.1 The upper part of the sampling block and sample
apparatus requires modification, as described in this test
inlettube(Note1)areconstructedofpolytetrafluoroethyleneto
method, prior to use. It consists of the following:
minimize reactivity with acidic fluoride gases. The upper part
7.1.1 Heated Inlet—I , TFE-fluorocarbon, 1 m [3.3 ft] in
of the sampling block (T ) has a cylindrical cavity 25.4 mm [1
p
length,9.5mm[ ⁄8in.](outsidediameter),encasedina9.5mm
in.] in diameter with the inlet tube to the cavity perpendicular
[ ⁄8 in.] (inside diameter) aluminum tube. See Fig. 1. The
to the paper tapes. The lower part of the sampling block (T )
g
aluminum jacket is wrapped in a constant wattage heating wire
shall be constructed of stainless steel with a 25.4 mm [1-in.]
cylindrical cavity. The outlet tube from the cylindrical cavity
passes at a right angle into the pump compartment. The lower
The sole source of supply of this apparatus known to the Committee is
block shall be spring-loaded with a total force of 1.36 kg [3 lb]
Anderson Samplers, Atlanta, GA. If you are aware of alternate suppliers, please
against the lower surface of the upper block. The surfaces of
provide this information to ASTM Headquarters, 100 Barr Harbor Drive, PO Box
thetwoblocksshallbemachinedflattoensureatightseal.The
C700, West Conshohocken, PA 19428–2959. Your comments will recieve careful
consideration at a meeting of the responsible technical committee, which you may
lower block shall be lowered by means of an electric solenoid
attend.
which counteracts the spring pressure.
Zankel, K. L., McGirr, R., Romm, M. Campbell, Miller, R. “Measurement of
7.1.2.2 Capstans, positioned to guide the paper tapes
Ambient Ground-Level Concentrations of Hydrogen Fluoride,” Journal of The Air
Pollution Control Association, Vol 37: 1191–1196 (1987). through the sampling block and to the take-up reel.
D3266–91 (2005)
FIG. 2 Schematic Drawing of Double Paper Tape Sampler
7.1.2.3 The paper tapes shall be drawn through the sample lime-glass wool filter (S ) and the filtered air is used to
p
block and wound on the take-up reels by ⁄30 Hz (2 rpm) pressurizethefrontcompartmentandpreventcontaminationby
synchronous motors. Indexing is accomplished either by me- fluorides from the ambient air.
chanical or photoelectric means to provide even spacing 7.1.2.6 Sample Flow Adjustment Valve—An inline needle
between samples. Provision is made by the use of tape valve, V .
perforated at regular intervals, or by some other means, to 7.1.2.7 Flow Indicator—0–30 L/min (0–1 ft /min) M .
locate the collected sample spots for subsequent analysis. A 7.1.2.8 Paper Tape—38-mm [1.5-in.] wide, appropriately
relay is wired in series with the indexing mechanism to turn off treated chemically (10.1).
the vacuum pump during tape transport. 7.1.2.9 Provision shall be made for manual override of the
7.1.2.4 Interval Timer, used to provide desired sampling tape transport mechanism.
times. 7.1.2.10 All fittings shall be constructed of TFE-
7.1.2.5 Carbon-Vane Vacuum Pump, to sample air, of nomi- fluorocarbon.
nal 30 L/min (1 ft /min) free-air capacity. This provides a 7.2 Calibration Equipment—See Fig. 3.
sampling rate through two tapes of about 15 L/min (0.5 7.2.1 InletCalibrationAdapter—Toconnecthosefromflow
ft /min). Exhaust air from the pump is passed through a soda calibration equipment to sampler inlet.
D3266–91 (2005)
8.7 Total Ionic Strength Adjustment Buffer (TISAB)—Add
57 mL of glacial acetic acid, 58 g of NaCl and 4.0 g of CDTA
((1,2-cyclohexylenedinitrilo)tetraacetic acid) to 500 mL of
distilled water. Stir and add 5 N NaOH solution (8.11) slowly
until pH is between 5.0 and 5.5. Cool and dilute to 1 L.
8.8 TISAB (1 + 1)—Dilute the full strength TISAB (8.7)
1 + 1 with an equal amount of reagent water.
8.9 Sulfuric Acid (1.0 N)—Add 28.0 mL of concentrated
H SO (sp gr 1.84) to 250 mL of reagent water in a 1-L
2 4
volumetric flask. Swirl to mix, cool, and dilute to 1 L with
reagent water. Mix thoroughly.
8.10 Sodium Hydroxide Solution (1.0 N)—Dissolve 40.0 g
of NaOH in 250 mLof reagent water in a 1000-mLvolumetric
flask. Swirl to mix, cool, and dilute to 1000 mL with reagent
water. Mix thoroughly.
8.11 Sodium Hydroxide Solution (5.0 N) Dissolve 200.0 g
of NaOH in a 1-L volumetric flask. Swirl to mix, cool, and
dilute to 1 L with water. Mix thoroughly.
8.12 Hydrogen Fluoride Permeation Tube—200 ng/min at
FIG. 3 Inlet Flow Calibration Schematic
35°C is satisfactory.
9. Sampling
7.2.2 Flow Meter—M , 0–30 L/min (0–1 ft /min), cali-
brated in accordance with Practice D3195. 9.1 See Practice D1357 for general sampling guidelines.
7.2.3 Wet Testmeter—M , calibrated in accordance with
3 9.2 Carefully align the sample block assembly to minimize
Test Methods D1071.
leakage.
7.3 HF Permeation Tube Calibrator—A permeation tube
9.3 Adjust temperature controller for a temperature of 54°C
device, modified as described in Footnote 10. See also Practice
[130°F].
D3609.All components of the calibrator that come into contact
9.4 Adjust flow rate to 15 L/min (0.5 ft /min).
with HF shall be constructed of TFE-fluorocarbon.
9.5 Adjust timer to required sample time.
9.6 When temperature of inlet is stable at 54°C, at a flow
8. Reagents and Materials
rate of 15 L/min, advance tape, and commence sampling.
8.1 Purity of Reagents—All reagents shall conform to the
9.7 Record the reading of the inlet pressure gauge, M , for
specifications of the Committee on Analytical Reagents of the
measurementoftheairflowthroughtheinlettube.Theairflow
American Chemical Society, where such specifications are
should remain reasonably constant over the sampling period
available.
selected.
8.2 Purity of Water—Water shall be Grade II Reagent
9.8 Prior to removing the tapes, the reading of the static
conforming to Specification D1193. Additionally, the water
pressure meter should again be recorded to provide an average
used in the sampling and analytical procedures shall be
air flow measurement over the total operational period.
demonstrated by testing with a specific ion electrode or by
9.9 Remove the paper tapes at convenient intervals and
concentration and photometric analysis to contain less than
place each in separate clean containers.
0.005 µg/mm of fluoride.
9.10 Analyze the individual samples by photometric or
8.3 Chemically treated medium retentive filter paper tape
electrometric methods as referenced below and described in
38-mm [1.5-in.] wide shall be used as the prefilter.
Test Methods D3269 and D3270.
8.4 Chemically treated soft open filter paper 38-mm [1.5-
in.] wide shall be used to remove acidic gaseous fluorides.
10. Preparation of Apparatus
8.5 Citric Acid, Alcoholic, Solution (0.1 M)—Dissolve
10.1 Treatment of Paper Tapes—Treat the paper tapes by
4.203 g of citric acid monohydrate in 200 mL of 95 % ethyl
passing the tapes through the appropriate impregnating solu-
alcohol.
tion and under a dryer and then rewinding. This is preferably
8.6 Sodium Hydroxide, Alcoholic Glycerin Solution (0.5
done with a continuous motor-driven system.
N)—Dissolve 4.000 g of NaOH pellets in 200 mL of 95 %
10.1.1 Treatment of the Medium Retentive Prefilter—Treat
...
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