ASTM D3266-91(2011)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3266 − 91 (Reapproved 2011)
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 U.S. Department of Defense.
1. Scope ticulate and Gaseous Fluorides in the Atmosphere (So-
dium Bicarbonate-Coated Glass Tube and Particulate
1.1 This test method describes the automatic separation and
Filter Method)
collection on chemically treated paper tapes of particulate and
D3269 Test Methods for Analysis for Fluoride Content of
gaseous forms of acidic fluorides in the atmosphere by means
the Atmosphere and Plant Tissues (Manual Procedures)
of a double paper tape sampler. The sampler may be pro-
(Withdrawn 2010)
grammed to collect and store individual air samples obtained
D3270 Test Methods for Analysis for Fluoride Content of
over time periods from several minutes to 3 h. A 30.5-m
the Atmosphere and Plant Tissues (Semiautomated
(100-ft) tape will allow unattended operation for the automatic
Method)
collection of up to 600 samples.
D3609 Practice for Calibration Techniques Using Perme-
1.2 The values stated in SI units are to be regarded as
ation Tubes
standard. The values given in parentheses are for information
D3614 Guide for Laboratories Engaged in Sampling and
only.
Analysis of Atmospheres and Emissions
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—For definitions of terms used in this test
priate safety and health practices and determine the applica-
method, refer to Terminology D1356.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
2 4.1 Air is drawn through an air inlet tube (see Practice
2.1 ASTM Standards:
D1357) and is first passed through an acid-treated prefilter
D1071 Test Methods for Volumetric Measurement of Gas-
paper tape to remove particulate matter which may contain
eous Fuel Samples
fluoride and then through an alkali-treated paper tape to
D1193 Specification for Reagent Water
remove acidic fluoride gases.
D1356 Terminology Relating to Sampling and Analysis of
Atmospheres
4.2 The exhaust air is filtered through soda lime-glass wool,
D1357 Practice for Planning the Sampling of the Ambient and the cleaned air is used to pressurize the front compartment
Atmosphere
to prevent fluoride contamination of the paper tapes from the
D3195 Practice for Rotameter Calibration ambient air.
D3268 Test Method for Separation and Collection of Par-
4.3 Automatically, at the end of the preset sampling period,
the vacuum pump is turned off, the tapes are indexed, and after
indexing the vacuum pump is turned on. Indexing results in a
This test method is under the jurisdiction of ASTM Committee D22 on Air
“dead time” of several seconds.
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient
Atmospheres and Source Emissions.
4.4 The paper tapes are removed from the sampler after a
Current edition approved Oct. 1, 2011. Published October 2011. Originally
selected period of operation and taken to an analytical work
approved in 1973. Last previous edition approved in 2005 as D3266 – 91(2005).
DOI: 10.1520/D3266-91R11.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3266 − 91 (2011)
area where the individual sample spots are cut out, treated to
dissolve the fluoride, and analyzed by potentiometric or pho-
4,5,6
tometric methods.
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
FIG. 1 Dual Tape Sampler Flow Schematic
(13.2.2.1) may provide relevant information.
6.3 Aluminum or certain other metals or phosphates can
sampler used for dust collection. The commercially available
interfere with subsequent analyses of the tapes by photometric
apparatus requires modification, as described in this test
or electrometric methods. These potential interferences are
method, prior to use. It consists of the following:
discussed in Test Methods D3269 and D3270.
7.1.1 Heated Inlet—I , TFE-fluorocarbon, 1 m (3.3 ft) in
6.4 There are several limitations of the test method that
length,9.5mm( ⁄8in.)(outsidediameter),encasedina9.5mm
could possibly occur:
( ⁄8 in.) (inside diameter) aluminum tube. See Fig. 1. The
6.4.1 Although the acid-treated medium retentive prefilter
aluminum jacket is wrapped in a constant wattage heating wire
has been shown to allow passage of hydrofluoric acid, it will
of 25 W/m (8 W/ft). The tube is connected to the instrument
restrict passage of particulate matter only as small as about 1
with a TFE-fluorocarbon fitting.
µm.Thus,smallerparticulatemattermaypassthroughthefilter
7.1.1.1 Rainshield, R —Constructed of TFE-fluorocarbon.
s
and impinge on or pass through the alkali-treated second tape.
7.1.1.2 Proportional Temperature Controller—H , with
6.4.2 The maximum sampling time recommended in the
thermocouple reference point located at the bottom of the
method is 3 h. This time is limited to minimize the possible
sample chamber.
effect of particulate matter sorbing the acidic fluoride gases or
7.1.1.3 Inlet Thermostat—T .
reducing the sampling rate.
7.1.1.4 Inlet Pressure Gauge—M with shutoff valve, V .
5 1
One side of the gauge is connected to a TFE-fluorocarbon run
7. Apparatus
tee placed between the intake tube and the sample block, and
7.1 The double paper tape sampler is a modification of and
the other side is connected to a TFE-fluorocarbon run tee
utilizes the basic principles of the sequential paper tape
placed at the entrance to the intake tubing.
7.1.2 Sampler—See Figs. 1 and 2.
7.1.2.1 The upper part of the sampling block and sample
Mandl, R. H., Weinstein, L. H., Weiskopf, G. J., and Major, J. L., “The
inlettube(Note1)areconstructedofpolytetrafluoroethyleneto
Separation and Collection of Gaseous and Particulate Fluorides,” Paper CP-25A,
2D International Clean Air Congress, Washington, DC, 1970.
minimize reactivity with acidic fluoride gases. The upper part
Weinstein,L.H.,andMandl,R.H.,“TheSeparationandCollectionofGaseous
of the sampling block (T ) has a cylindrical cavity 25.4 mm (1
p
and Particulate Fluorides,” VDI Berichte Nr., Vol 164, 1971, pp. 53–63.
in.) in diameter with the inlet tube to the cavity perpendicular
Lodge, James P. Jr., ed., “Methods ofAir Sampling andAnalysis,” Intersociety
Committee, 3rd ed., Lewis Publishers, Inc., 1988, pp. 352–356. to the paper tapes. The lower part of the sampling block (T )
g
The sole source of supply of the apparatus known to the committee at this time
isAnderson Samplers,Atlanta, GA. If you are aware of alternative suppliers, please
provide this information toASTM International Headquarters. Your comments will Zankel, K. L., McGirr, R., Romm, M. Campbell, Miller, R. “Measurement of
receive careful consideration at a meeting of the responsible technical committee, Ambient Ground-Level Concentrations of Hydrogen Fluoride,” Journal of The Air
which you may attend. Pollution Control Association, Vol 37, 1987, pp. 1191–1196.
D3266 − 91 (2011)
FIG. 2 Schematic Drawing of Double Paper Tape Sampler
shall be constructed of stainless steel with a 25.4 mm (1-in.) perforated at regular intervals, or by some other means, to
cylindrical cavity. The outlet tube from the cylindrical cavity locate the collected sample spots for subsequent analysis. A
passes at a right angle into the pump compartment. The lower relay is wired in series with the indexing mechanism to turn off
block shall be spring-loaded with a total force of 1.36 kg (3 lb) the vacuum pump during tape transport.
against the lower surface of the upper block. The surfaces of 7.1.2.4 Interval Timer, used to provide desired sampling
thetwoblocksshallbemachinedflattoensureatightseal.The times.
lower block shall be lowered by means of an electric solenoid 7.1.2.5 Carbon-Vane Vacuum Pump, to sample air, of nomi-
which counteracts the spring pressure. nal 30 L/min (1 ft /min) free-air capacity. This provides a
7.1.2.2 Capstans, positioned to guide the paper tapes sampling rate through two tapes of about 15 L/min (0.5
through the sampling block and to the take-up reel. ft /min). Exhaust air from the pump is passed through a soda
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 .
D3266 − 91 (2011)
8.3 Chemically treated medium retentive filter paper tape
38-mm (1.5-in.) wide shall be used as the prefilter.
8.4 Chemically treated soft open filter paper 38-mm (1.5-
in.) wide shall be used to remove acidic gaseous fluorides.
8.5 Citric Acid, Alcoholic, Solution (0.1 M)—Dissolve
4.203 g of citric acid monohydrate in 200 mL of 95 % ethyl
alcohol.
8.6 Sodium Hydroxide, Alcoholic Glycerin Solution (0.5
N)—Dissolve4.000gofNaOHpelletsin200mLof95 %ethyl
alcohol containing 5 % glycerol.
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.
FIG. 3 Inlet Flow Calibration Schematic
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
7.1.2.7 Flow Indicator—0–30 L/min (0–1 ft /min) M .
volumetric flask. Swirl to mix, cool, and dilute to 1 L with
7.1.2.8 Paper Tape—38-mm (1.5-in.) wide, appropriately
reagent water. Mix thoroughly.
treated chemically (10.1).
7.1.2.9 Provision shall be made for manual override of the 8.10 Sodium Hydroxide Solution (1.0 N)—Dissolve 40.0 g
tape transport mechanism.
of NaOH in 250 mLof reagent water in a 1000-mLvolumetric
7.1.2.10 All fittings shall be constructed of TFE- flask. Swirl to mix, cool, and dilute to 1000 mL with reagent
fluorocarbon.
water. Mix thoroughly.
7.2 Calibration Equipment—See Fig. 3.
8.11 Sodium Hydroxide Solution(5.0 N)Dissolve 200.0 g of
7.2.1 Inlet CalibrationAdapter—To connect hose from flow
NaOH in a 1-Lvolumetric flask. Swirl to mix, cool, and dilute
calibration equipment to sampler inlet.
to 1 L with water. Mix thoroughly.
7.2.2 Flow Meter—M , 0–30 L/min (0–1 ft /min), cali-
8.12 Hydrogen Fluoride Permeation Tube—200 ng/min at
brated in accordance with Practice D3195.
35°C is satisfactory.
7.2.3 Wet Testmeter—M ,calibratedinaccordancewithTest
Methods D1071.
9. Sampling
7.3 HF Permeation Tube Calibrator—A permeation tube
9.1 See Practice D1357 for general sampling guidelines.
device, modified as described in Footnote 10. See also Practice
D3609.All components of the calibrator that come into contact
9.2 Carefully align the sample block assembly to minimize
with HF shall be constructed of TFE-fluorocarbon.
leakage.
8. Reagents and Materials
9.3 Adjust temperature controller for a temperature of 54°C
(130°F).
8.1 Purity of Reagents—All reagents shall conform to the
specifications of the Committee on Analytical Reagents of the
9.4 Adjust flow rate to 15 L/min (0.5 ft /min).
American Chemical Society, where such specifications are
9.5 Adjust timer to required sample time.
available.
9.6 When temperature of inlet is stable at 54°C, at a flow
8.2 Purity of Water—Water shall be Grade II Reagent
rate of 15 L/min, advance tape, and commence sampling.
conforming to Specification D1193. Additionally, the water
used in the sampling and analytical procedures shall be
9.7 Record the reading of the inlet pressure gauge, M , for
demonstrated by testing with a specific ion electrode or by
measurementoftheairflowthroughtheinlettube.Theairflow
concentration and photometric analysis to contain less than
should remain reasonably constant over the sampling period
0.005 µg/mm of fluoride.
selected.
9.8 Prior to removing the tapes, the reading of the static
Reagent Chemicals, American Chemical Society Specifications, American
pressure meter should again be recorded to provide an average
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
air flow measurement over the total operational period.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
9.9 Remove the paper tapes at convenient intervals and
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC
...