1、Designation: D3266 91 (Reapproved 2011)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 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 and
4、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 are for informat
5、iononly.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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Refe
6、renced 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 ofAtmospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphereD3195 Practice for Rotamete
7、r CalibrationD3268 Test Method for Separation and Collection of Par-ticulate and Gaseous Fluorides in theAtmosphere (SodiumBicarbonate-Coated Glass Tube and Particulate FilterMethod)D3269 Test Methods for Analysis for Fluoride Content ofthe Atmosphere and Plant Tissues (Manual Procedures)3D3270 Test
8、 Methods for Analysis for Fluoride Content ofthe Atmosphere and Plant Tissues (SemiautomatedMethod)D3609 Practice for Calibration Techniques Using Perme-ation TubesD3614 Guide for Laboratories Engaged in Sampling andAnalysis of Atmospheres and Emissions3. Terminology3.1 DefinitionsFor definitions of
9、 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 an acid-treated prefilterpaper tape to remove particulate matter which may containfluoride and then through an alkali-treated
10、 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 prevent fluoride contamination of the paper tapes from theambient air.4.3 Automatically, at the end of the preset sampling period,
11、the vacuum pump is turned off, the tapes are indexed, and afterindexing the vacuum pump is turned on. Indexing results in a“dead time” of several seconds.1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.03 on Ambient
12、Atmospheres and Source Emissions.Current edition approved Oct. 1, 2011. Published October 2011. Originallyapproved in 1973. Last previous edition approved in 2005 as D3266 - 91(2005).DOI: 10.1520/D3266-91R11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custome
13、r Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO B
14、ox C700, West Conshohocken, PA 19428-2959, United States.4.4 The paper tapes are removed from the sampler after aselected period of operation and taken to an analytical workarea where the individual sample spots are cut out, treated todissolve the fluoride, and analyzed by potentiometric or pho-tome
15、tric methods.4,5,65. Significance and Use5.1 This test method provides a means of automaticallyseparating and collecting atmospheric particulate and acidicgaseous fluoride samples.5.2 Since the samples are collected on dry tapes, thesamples are in a form which allows elution of the fluoridecontent w
16、ith 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 metallic salts, such as those of aluminum,iron, calcium, magnesium or rare-earth elements, may reactwith and remove some or all of t
17、he acidic gaseous fluoride onthe prefilter. If interfering quantities of such particulate metal-lic salts are present, the use of Test Methods D3268 isrecommended because the acidic fluoride gases are collectedprior to the filter.6.2 Acid aerosols or gases might neutralize or acidify thealkali-treat
18、ed 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 extract(13.2.2.1) may provide relevant information.6.3 Aluminum or certain other metals or phosphates caninterfere with subsequent
19、 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 the test method thatcould possibly occur:6.4.1 Although the acid-treated medium retentive prefilterhas been shown to allow pa
20、ssage 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 on or pass through the alkali-treated second tape.6.4.2 The maximum sampling time recommended in themethod is 3 h. This time is
21、 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 a modification of andutilizes the basic principles of the sequential paper tapesampler used for dust collection. The commerci
22、ally 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) inlength, 9.5 mm (38 in.) (outside diameter), encased in a 9.5 mm(38 in.) (inside diameter) aluminum tube. See Fig. 1. Theal
23、uminum 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, RsConstructed of TFE-fluorocarbon.7.1.1.2 Proportional Temperature ControllerH1, withthermocouple reference point located at the b
24、ottom 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 placed between the intake tube and the sample block, andthe other side is connected to a TFE-fluorocarbon run teeplaced at the en
25、trance 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 block (Tp) has a cylindrical cavity 25.4 mm
26、 (1in.) in diameter with the inlet tube to the cavity perpendicular4Mandl, R. H., Weinstein, L. H., Weiskopf, G. J., and Major, J. L. “TheSeparation and Collection of Gaseous and Particulate Fluorides.” Paper CP-25A, 2DInternational Clean Air Congress, Washington, DC, 1970.5Weinstein, L. H., and Man
27、dl, R. H. “The Separation and Collection of Gaseousand Particulate Fluorides.” VDI Berichte Nr. Vol 164, 1971, pp. 53 to 63.6Lodge, 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 this a
28、pparatus known to the Committee isAnderson Samplers, Atlanta, GA. If you are aware of alternate suppliers, pleaseprovide this information to ASTM Headquarters, 100 Barr Harbor Drive, PO BoxC700, West Conshohocken, PA 194282959. Your comments will recieve carefulconsideration at a meeting of the resp
29、onsible technical committee, which you mayattend.8Zankel, K. L., McGirr, R., Romm, M. Campbell, Miller, R. “Measurement ofAmbient Ground-Level Concentrations of Hydrogen Fluoride,” Journal of The AirPollution Control Association, Vol 37: 11911196 (1987).FIG. 1 Dual Tape Sampler Flow SchematicD3266 9
30、1 (2011)2to 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 at a right angle into the pump compartment. The lowerblock shall be spring-loaded with a total for
31、ce 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 solenoidwhich counteracts the spring pressure.7.1.2.2 Capstans, positioned to guide the paper tapesth
32、rough 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 accomplished either by me-chanical or photoelectric means to provide even spacingbetween samples. Provision i
33、s 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 turn offthe vacuum pump during tape transport.7.1.2.4 Interval Timer, used to provide desired sampli
34、ngtimes.7.1.2.5 Carbon-Vane Vacuum Pump, to sample air, of nomi-nal 30 L/min (1 ft3/min) free-air capacity. This provides asampling 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 topres
35、surize the front compartment and prevent contamination byfluorides from the ambient air.FIG. 2 Schematic Drawing of Double Paper Tape SamplerD3266 91 (2011)37.1.2.6 Sample Flow Adjustment ValveAn inline needlevalve, V3.7.1.2.7 Flow Indicator030 L/min (01 ft3/min) M1.7.1.2.8 Paper Tape38-mm (1.5-in.)
36、 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 Calibration EquipmentSee Fig. 3.7.2.1 Inlet Calibration AdapterTo connect hose from flowcalibration equi
37、pment to sampler inlet.7.2.2 Flow MeterM4, 030 L/min (01 ft3/min), cali-brated in accordance with Practice D3195.7.2.3 Wet TestmeterM3, calibrated in accordance withTest Methods D1071.7.3 HF Permeation Tube CalibratorA permeation tubedevice, modified as described in Footnote 10. See also PracticeD36
38、09.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 thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society, where such specifications
39、 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 testing with a specific ion electrode or byconcentration and photometric analysis to contain less than0.00
40、5 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 shall be used to remove acidic gaseous fluorides.8.5 Citric Acid, Alcoholic, Solution (0.1 M)Dissolve4.20
41、3 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 mL of 95 %ethyl alcohol containing 5 % glycerol.8.7 Total Ionic Strength Adjustment Buffer (TISAB)Add57 mL of glacial acetic acid, 58 g of NaC
42、l 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.8.8 TISAB (1 + 1)Dilute the full strength TISAB (8.7)1 + 1 with an equal amount of reagent water.8.9 Sulfu
43、ric 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 Hydroxide Solution (1.0 N)Dissolve 40.0 gof NaOH in 250 mL of reagent water in a 1000-mL volumetricfla
44、sk. Swirl to mix, cool, and dilute to 1000 mL with reagentwater. Mix thoroughly.8.11 Sodium Hydroxide Solution (5.0 N) Dissolve 200.0 gof NaOH in a 1-L volumetric flask. Swirl to mix, cool, anddilute to 1 L with water. Mix thoroughly.8.12 Hydrogen Fluoride Permeation Tube200 ng/min at35C is satisfac
45、tory.89. Sampling9.1 See Practice D1357 for general sampling guidelines.9.2 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 t
46、emperature 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
47、 to removing the tapes, the reading of the staticpressure meter should again be recorded to provide an averageair flow measurement over the total operational period.9.9 Remove the paper tapes at convenient intervals andplace each in separate clean containers.9.10 Analyze the individual samples by ph
48、otometric orelectrometric methods as referenced below and described inTest Methods D3269 and D3270.9Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Anala
49、r 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 91 (2011)410. Preparation of Apparatus10.1 Treatment of Paper TapesTreat the paper tapes bypassing the tapes through the appropriate impregnating solu-tion and under a dryer and then rewinding. This is preferablydone with a continuous motor-driven system.10.1.1 Treatment of the Medium Retentive PrefilterTreatthis t
