1、Designation: D3266 91 (Reapproved 2018)Standard Test Method forAutomated Separation and Collection of Particulate andAcidic Gaseous Fluoride in the Atmosphere (Double PaperTape Sampler Method)1This standard is issued under the fixed designation D3266; the number immediately following the designation
2、 indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agenci
3、es of the U.S. Department of Defense.1. Scope1.1 This test method describes the automatic separation andcollection on chemically treated paper tapes of particulate andgaseous forms of acidic fluorides in the atmosphere by meansof a double paper tape sampler. The sampler may be pro-grammed to collect
4、 and store individual air samples obtainedover time periods from several minutes to 3 h. A 30.5-m(100-ft) tape will allow unattended operation for the automaticcollection of up to 600 samples.1.2 The values stated in SI units are to be regarded asstandard. The values given in parentheses after SI un
5、its areincluded for information only and are not considered standard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices an
6、d deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-
7、mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1071 Test Methods for Volumetric Measurement of Gas-eous Fuel SamplesD1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtm
8、ospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphereD3195/D3195M Practice for Rotameter CalibrationD3268 Test Method for Separation and Collection of Par-ticulate and Gaseous Fluorides in the Atmosphere (So-dium Bicarbonate-Coated Glass Tube and ParticulateFilter Method)D3269 Te
9、st Methods for Analysis for Fluoride Content ofthe Atmosphere and Plant Tissues (Manual Procedures)(Withdrawn 2010)3D3270 Test Methods for Analysis for Fluoride Content ofthe Atmosphere and Plant Tissues (SemiautomatedMethod)D3609 Practice for Calibration Techniques Using Perme-ation TubesD3614 Guid
10、e for Laboratories Engaged in Sampling andAnalysis of Atmospheres and Emissions3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1356.4. Summary of Test Method4.1 Air is drawn through an air inlet tube (see PracticeD1357) and is first passed through
11、 an acid-treated prefilterpaper tape to remove particulate matter which may containfluoride and then through an alkali-treated paper tape toremove acidic fluoride gases.4.2 The exhaust air is filtered through soda lime-glass wool,and the cleaned air is used to pressurize the front compartmentto prev
12、ent fluoride contamination of the paper tapes from theambient air.4.3 Automatically, at the end of the preset sampling period,the vacuum pump is turned off, the tapes are indexed, and after1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibilit
13、y of Subcommittee D22.03 on AmbientAtmospheres and Source Emissions.Current edition approved June 1, 2018. Published June 2018. Originallyapproved in 1973. Last previous edition approved in 2011 as D3266 91 (2011).DOI: 10.1520/D3266-91R18.2For referenced ASTM standards, visit the ASTM website, www.a
14、stm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr
15、 Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recomme
16、ndations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1indexing the vacuum pump is turned on. Indexing results in a“dead time” of several seconds.4.4 The paper tapes are removed from the sampler after aselected period of operation and taken to an analytical work
17、area where the individual sample spots are cut out, treated todissolve the fluoride, and analyzed by potentiometric or pho-tometric methods.4,5,65. Significance and Use5.1 This test method provides a means of automaticallyseparating and collecting atmospheric particulate and acidicgaseous fluoride s
18、amples.5.2 Since the samples are collected on dry tapes, thesamples are in a form which allows elution of the fluoridecontent with a small volume of eluent. Consequently, themethod allows analyses of air samples taken for a time periodas short as several minutes.6. Interferences6.1 Particulate metal
19、lic salts, such as those of aluminum,iron, calcium, magnesium or rare-earth elements, may reactwith and remove some or all of the acidic gaseous fluoride onthe prefilter. If interfering quantities of such particulate metal-lic salts are present, the use of Test Method D3268 isrecommended because the
20、 acidic fluoride gases are collectedprior to the filter.6.2 Acid aerosols or gases might neutralize or acidify thealkali-treated tape and prevent quantitative uptake of the acidicfluoride gases from the atmosphere. If this potential interfer-ence is present the decreased alkalinity of the water extr
21、act(13.2.2.1) may provide relevant information.6.3 Aluminum or certain other metals or phosphates caninterfere with subsequent analyses of the tapes by photometricor electrometric methods. These potential interferences arediscussed in Test Methods D3269 and D3270.6.4 There are several limitations of
22、 the test method thatcould possibly occur:6.4.1 Although the acid-treated medium retentive prefilterhas been shown to allow passage of hydrofluoric acid, it willrestrict passage of particulate matter only as small as about 1m. Thus, smaller particulate matter may pass through the filterand impinge o
23、n or pass through the alkali-treated second tape.6.4.2 The maximum sampling time recommended in themethod is 3 h. This time is limited to minimize the possibleeffect of particulate matter sorbing the acidic fluoride gases orreducing the sampling rate.7. Apparatus77.1 The double paper tape sampler is
24、 a modification of andutilizes the basic principles of the sequential paper tapesampler used for dust collection. The commercially availableapparatus requires modification, as described in this testmethod, prior to use.8It consists of the following:7.1.1 Heated InletI1, TFE-fluorocarbon, 1 m (3.3 ft
25、) inlength, 9.5 mm (38 in.) (outside diameter), encased in a 9.5 mm(38 in.) (inside diameter) aluminum tube. See Fig. 1. Thealuminum jacket is wrapped in a constant wattage heating wireof 25 W/m (8 W/ft). The tube is connected to the instrumentwith a TFE-fluorocarbon fitting.7.1.1.1 Rainshield, RsCo
26、nstructed of TFE-fluorocarbon.7.1.1.2 Proportional Temperature ControllerH1, withthermocouple reference point located at the bottom of thesample chamber.7.1.1.3 Inlet ThermostatT1.7.1.1.4 Inlet Pressure GaugeM5with shutoff valve, V1.One side of the gauge is connected to a TFE-fluorocarbon runtee pla
27、ced between the intake tube and the sample block, and4Mandl, R. H., Weinstein, L. H., Weiskopf, G. J., and Major, J. L., “TheSeparation and Collection of Gaseous and Particulate Fluorides,” Paper CP-25A,2D International Clean Air Congress, Washington, DC, 1970.5Weinstein, L. H., and Mandl, R. H., “T
28、he Separation and Collection of Gaseousand Particulate Fluorides,” VDI Berichte Nr., Vol 164, 1971, pp. 5363.6Lodge, James P. Jr., ed., “Methods of Air Sampling and Analysis,” IntersocietyCommittee, 3rd ed., Lewis Publishers, Inc., 1988, pp. 352356.7The sole source of supply of the apparatus known t
29、o the committee at this timeis Anderson Samplers, Atlanta, GA. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technical committee,1which you may attend.8Zank
30、el, K. L., McGirr, R., Romm, M., Campbell, S. A., Miller, R. “Measure-ment of Ambient Ground-Level Concentrations of Hydrogen Fluoride,” Journal ofThe Air Pollution Control Association, Vol 37, 1987, pp. 11911196.FIG. 1 Dual Tape Sampler Flow SchematicD3266 91 (2018)2the other side is connected to a
31、 TFE-fluorocarbon run teeplaced at the entrance to the intake tubing.7.1.2 SamplerSee Figs. 1 and 2.7.1.2.1 The upper part of the sampling block and sampleinlet tube (Note 1) are constructed of polytetrafluoroethylene tominimize reactivity with acidic fluoride gases. The upper partof the sampling bl
32、ock (Tp) has a cylindrical cavity 25.4 mm (1in.) in diameter with the inlet tube to the cavity perpendicularto the paper tapes. The lower part of the sampling block (Tg)shall be constructed of stainless steel with a 25.4 mm (1-in.)cylindrical cavity. The outlet tube from the cylindrical cavitypasses
33、 at a right angle into the pump compartment. The lowerblock shall be spring-loaded with a total force of 1.36 kg (3 lb)against the lower surface of the upper block. The surfaces ofthe two blocks shall be machined flat to ensure a tight seal. Thelower block shall be lowered by means of an electric so
34、lenoidwhich counteracts the spring pressure.7.1.2.2 Capstans, positioned to guide the paper tapesthrough the sampling block and to the take-up reel.7.1.2.3 The paper tapes shall be drawn through the sampleblock and wound on the take-up reels by130 Hz (2 rpm)synchronous motors. Indexing is accomplish
35、ed either by me-chanical or photoelectric means to provide even spacingbetween samples. Provision is made by the use of tapeperforated at regular intervals, or by some other means, tolocate the collected sample spots for subsequent analysis. Arelay is wired in series with the indexing mechanism to t
36、urn offthe vacuum pump during tape transport.7.1.2.4 Interval Timer, used to provide desired samplingtimes.FIG. 2 Schematic Drawing of Double Paper Tape SamplerD3266 91 (2018)37.1.2.5 Carbon-Vane Vacuum Pump, to sample air, of nomi-nal 30 L/min (1 ft3/min) free-air capacity. This provides asampling
37、rate through two tapes of about 15 L/min (0.5ft3/min). Exhaust air from the pump is passed through a sodalime-glass wool filter (Sp) and the filtered air is used topressurize the front compartment and prevent contamination byfluorides from the ambient air.7.1.2.6 Sample Flow Adjustment ValveAn inlin
38、e needlevalve, V3.7.1.2.7 Flow Indicator030 L/min (01 ft3/min) M1.7.1.2.8 Paper Tape38-mm (1.5-in.) wide, appropriatelytreated chemically (10.1).7.1.2.9 Provision shall be made for manual override of thetape transport mechanism.7.1.2.10 All fittings shall be constructed of TFE-fluorocarbon.7.2 Calib
39、ration EquipmentSee Fig. 3.7.2.1 Inlet Calibration AdapterTo connect hose from flowcalibration equipment to sampler inlet.7.2.2 Flow MeterM4, 030 L/min (01 ft3/min), cali-brated in accordance with Practice D3195/D3195M.7.2.3 Wet TestmeterM3, calibrated in accordance with TestMethods D1071.7.3 HF Per
40、meation Tube CalibratorA permeation tubedevice, modified as described in Footnote 8. See also PracticeD3609.All components of the calibrator that come into contactwith HF shall be constructed of TFE-fluorocarbon.8. Reagents and Materials8.1 Purity of ReagentsAll reagents shall conform to thespecific
41、ations of the Committee on Analytical Reagents of theAmerican Chemical Society, where such specifications areavailable.98.2 Purity of WaterWater shall be Grade II Reagentconforming to Specification D1193. Additionally, the waterused in the sampling and analytical procedures shall bedemonstrated by t
42、esting with a specific ion electrode or byconcentration and photometric analysis to contain less than0.005 g/mm of fluoride.8.3 Chemically treated medium retentive filter paper tape38-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
43、shall be used to remove acidic gaseous fluorides.8.5 Citric Acid, Alcoholic, Solution (0.1 M)Dissolve4.203 g of citric acid monohydrate in 200 mL of 95 % ethylalcohol.8.6 Sodium Hydroxide, Alcoholic Glycerin Solution (0.5N)Dissolve 4.000 g of NaOH pellets in 200 mLof 95 % ethylalcohol containing 5 %
44、 glycerol.8.7 Total Ionic Strength Adjustment Buffer (TISAB)Add57 mL of glacial acetic acid, 58 g of NaCl and 4.0 g of CDTA(1,2-cyclohexylenedinitrilo)tetraacetic acid) to 500 mL ofdistilled water. Stir and add 5 N NaOH solution (8.11) slowlyuntil pH is between 5.0 and 5.5. Cool and dilute to 1 L.8.
45、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 concentratedH2SO4(sp gr 1.84) to 250 mL of reagent water in a 1-Lvolumetric flask. Swirl to mix, cool, and dilute to 1 L withreagent water. Mix thoroughly.8.10 Sodium
46、 Hydroxide Solution (1.0 N)Dissolve 40.0 gof NaOH in 250 mL of reagent water in a 1000-mL volumetricflask. Swirl to mix, cool, and dilute to 1000 mL with reagentwater. Mix thoroughly.8.11 Sodium Hydroxide Solution(5.0 N)Dissolve 200.0 g ofNaOH in a 1-L volumetric flask. Swirl to mix, cool, and dilut
47、eto 1 L with water. Mix thoroughly.8.12 Hydrogen Fluoride Permeation Tube200 ng/min at35C is satisfactory.89. Sampling9.1 See Practice D1357 for general sampling guidelines.9Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the
48、testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.FIG. 3 Inlet Flow Calibration SchematicD3266
49、 91 (2018)49.2 Carefully align the sample block assembly to minimizeleakage.9.3 Adjust temperature controller for a temperature of 54C(130F).9.4 Adjust flow rate to 15 L/min (0.5 ft3/min).9.5 Adjust timer to required sample time.9.6 When temperature of inlet is stable at 54C, at a flowrate of 15 L/min, advance tape, and commence sampling.9.7 Record the reading of the inlet pressure gauge, M5, formeasurement of the air flow through the inlet tube. The air flowshould remain reasonably constant over the sampling periodselected.9.8 Prior to r
