1、Designation: D3267 12Standard Test Method forSeparation and Collection of Particulate and Water-SolubleGaseous Fluorides in the Atmosphere (Filter and ImpingerMethod)1This standard is issued under the fixed designation D3267; the number immediately following the designation indicates the year oforig
2、inal 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.1. Scope1.1 This test method provides a procedure for separationand collect
3、ion on a chemically treated filter and in an impingerof particulate and water-soluble gaseous fluoride in the atmo-sphere. The sampling rate may vary from 30 L/min (1.0ft3/min) to 15 L/min (0.5 ft3/min) for longer sampling periodsdepending on the atmospheric fluoride concentration. This testmethod i
4、s not intended to be applied to gaseous fluorinecompounds that are not water-soluble1.2 There are several limitations of the test method:1.2.1 Although the acid-treated, medium retentive, prefilterhas been shown to allow passage of HF, it will restrict passageof particulate matter only as small as a
5、bout 1 m. Thus, smallerparticulate matter may pass through the filter and be collectedin or pass through the impingers.1.2.2 The maximum sample volume to be taken using thistest method prior to changing the acid-treated prefilter isrecommended as 12 m3. This recommendation is made tominimize any eff
6、ects due to particulate matter build-up.1.3 The values stated in SI units are to be regarded as thestandard. The inch-pound units given in parentheses are forinformation only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibi
7、lity 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.For specific precau-tionary statements, see 7.2 and 7.4.6.2. Referenced Documents2.1 ASTM Standards:2D1071 Test Methods for Volumetric Measu
8、rement of Gas-eous Fuel SamplesD1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtmospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphereD2009 Practice for Collection by Filtration and Determina-tion of Mass, Number, and Optical Sizing of
9、AtmosphericParticulates3D3268 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)
10、3D3270 Test Methods for Analysis for Fluoride Content ofthe Atmosphere and Plant Tissues (SemiautomatedMethod)E337 Test Method for Measuring Humidity with a Psy-chrometer (the Measurement of Wet- and Dry-Bulb Tem-peratures)3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod
11、, 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 prefilter toremove particulate matter that may contain fluoride and thenthrough an impinger to remove water-soluble fluorides.4.2 The prefi
12、lter and impinger solution are removed fromthe sampling system at the end of the selected sampling periodand taken to an analytical work area and analyzed by either apotentiometric or photometric method (1, 2, 3, 4).4See TestMethods D3269 and D3270.1This test method is under the jurisdiction of ASTM
13、 Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.03 on AmbientAtmospheres and Source Emissions.Current edition approved April 1, 2012. Published May 2012. Originallyapproved in 1973. Last previous edition approved in 2005 as D3267 - 91(2005).DOI: 10.1520/D3267-12.2Fo
14、r referenced ASTM standards, visit the ASTM website, www.astm.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.3Withdrawn.4The boldface numbers in parentheses refer to the ref
15、erences at the end of thisstandard.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This test method provides a means of separation andcollection of particulate and water soluble gaseous fluoride andprovides
16、 samples that are convenient to analyze.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 the water-soluble gaseousfluoride on the prefilter. If interfering quantities of suchparticulate
17、metallic salts are present, the use of Test MethodD3268 is recommended because the acidic fluoride gases arecollected prior to the filter.6.2 Aluminum or certain other metals or phosphates caninterfere with subsequent analyses by photometric or electro-metric methods. These potential interferences a
18、re discussed inTest Methods D3269 and D3270.7. Apparatus7.1 Standard Impinger,(Fig. 2C) for sampling coveringperiods up to 3 h. When sampling is initiated, the collectingimpinger shall contain 75 to 150 mLof reagent water (see 8.2).7.2 Impinger, Modified, Standard, Smith-Greenburg (Fig.1). For sampl
19、ing periods from 3 to 72 h, see Fig. 1 and Fig. 3C.(WarningIf a different size impinger is used, the recovery ofthe sample should be determined.)7.3 Water Level Control Device, for use with long-termsampling train (Fig. 3).7.3.1 Liquid Level Controller. (See Fig. 3G and H.)7.3.2 Control Valve, solen
20、oid-activated. (See Fig. 3D.)7.3.3 Water Reservoir, equipped with a guard tube contain-ing an alkaline reagent to prevent fluoride contamination. (SeeFig. 3E and F.)7.4 Sampling Equipment (see Fig. 1, Fig. 2, and Fig. 3 fordimensions and details).7.4.1 Sampling Tube (see Fig. 2A), constructed of a12
21、25-mm (4-ft) length of a material that is inert to theatmosphere being sampled. (See Note 1.)NOTE 1Stainless steel coated with plastic material is preferred be-cause of its rigidity and permanence. Plastic materials which have beenshown to have a low absorbance for gaseous fluorides are polytetraflu
22、o-roethylene, polyethylene, polypropylene and polychlorotrifluoroethylene.However, high air velocities through some types of plastic tubing maycreate a static charge and cause deposition of particulate matter. Conse-quently, if plastic is selected for use, it should be tested to demonstrate thatthis
23、 effect does not occur to a significant degree.7.4.2 Filter Holder, stainless steel or polypropylene, (Fig.2B), to hold the acid-treated prefilter. (See Note 2.)NOTE 2Note that filter changes are recommended after 12 m3aresampled.7.4.3 Mercury Manometer (Fig. 2E), for the determinationof pressure in
24、 the metered sampling line. A calibrated vacuumgage is also satisfactory.7.4.4 Dry Test Meter (Fig. 2F), for measuring the totalvolume sampled.7.4.5 ThermometerTemperature measuring devices suchas RTDs (Resistance Temperature Devices), thermistors andorganic liquid-in-glass thermometers meeting the
25、requirementsof specific applications may be used.7.4.6 Control Valve (Fig. 2H), to adjust the sample ratethrough a dry test meter. (See 7.4.4.) (WarningExercise careto see that all sampling apparatus is clean and free ofcontamination. Clean with a detergent low in fluoride andphosphate, followed by
26、thorough rinsing with water (see 8.2.)7.4.7 Vacuum Pump (see Fig. 2J), capable of a 30 L/min (1ft3/min) sampling rate and capable of continuous operationover the maximum sample period selected under the environ-mental conditions imposed by the sampling location.8. Reagents8.1 Purity of ReagentsReage
27、nt grade chemicals shall beused in all tests.All reagents shall conform to the specificationsof the Committee on Analytical Reagents of the AmericanChemical Society, where such specifications are available.58.2 Purity of WaterWater shall be Type II reagent waterconforming to Specification D1193.Addi
28、tionally, test the waterwith a specific ion electrode or by concentration and photo-metric analysis to demonstrate that it contains less than 0.005g/mL of fluoride.8.3 Alcoholic Citric Acid Solution (0.1 N)Dissolve 4.203g of citric acid monohydrate in 200 mL of 95 % ethyl alcohol.8.4 Chemically trea
29、ted filters are used as the prefilter. (See10.1.)8.5 Sodium Hydroxide Solution (5N)Dissolve 200 g ofsodium hydroxide (NaOH) in 250 mL of water in a 1-Lvolumetric flask, swirl to mix, cool and dilute to 1000 mL withwater. Mix thoroughly.5Reagent Chemicals, American Chemical Society Specifications, Am
30、ericanChemical Society, Washington, DC. For suggestions on the 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. (U
31、SPC), Rockville,MD.FIG. 1 Modified Standard ImpingerD3267 1228.6 Sodium Hydroxide Solution (1.0 N)Dissolve 40.0 g ofNaOH in 250 mL of reagent water in a 1000-mL volumetricflask. Swirl to mix, cool, and dilute to 1000 mL with reagentwater. Mix thoroughly.8.7 Sulfuric Acid (1.0 N)Add 28.0 mL of concen
32、tratedH2SO4(sp gr 1.84) to 250 mL of reagent water in a 1000-mLvolumetric flask. Swirl to mix, cool, and dilute to 1000 mLwith reagent water. Mix thoroughly.8.8 Total Ionic Strength Adjustment Buffer (TISAB)Add57 mL of glacial acetic acid, 58 g of sodium chloride (NaCl)and 4.0 g of CDTA (1,2-cyclohe
33、xylene-dinitrilo)tetraaceticacid) to 500 mL of distilled water. Stir and add 5 NNaOHsolution (see 8.5) slowly until the pH is between 5.0 and 5.5.Cool and dilute to 1 L.8.9 TISAB (1:1)Dilute the full strength TISAB (see 8.8)1:1 with an equal amount of water.9. Calibration9.1 Calibrate the dry test m
34、eter (see 7.4.4) in accordancewith Test Methods D1071.10. Procedure10.1 Treatment of Prefilter:10.1.1 Immerse medium retentive prefilter (WarningExercise care to see that all sampling apparatus is clean andfree of contamination. Clean with a detergent low in fluorideand phosphate, followed by thorou
35、gh rinsing with water (see8.2.) in the alcoholic citric acid solution (0.1 N) (see 8.3) andplace under an infrared lamp to dry. After drying and prior touse, store the treated filter in a sealed container to preventcontamination.NOTE 3If the person using this test method demonstrates a require-ment
36、for prefilter of higher retentivity, other filters may be used.Membrane filters, if used, require reduction of the alcohol content of thealcoholic citric acid solution to 65 % to prevent deformation of the pores.10.2 Sampling:10.2.1 Test the System for Leaks:10.2.1.1 Fill the impinger with the requi
37、red volume ofreagent water (see 8.2) that will be utilized during sampling.10.2.1.2 Turn on the vacuum pump (see 7.4.7) and developa vacuum slightly greater than that required for the desiredsampling rate.NOTE 4For short term sampling (3 h or less), utilize a flow rate of 30L/min (1 ft3/min). For lo
38、ng-term sampling (24 to 72 h), a flow rate of 15L/min (0.5 ft3/min) shall be used with the modified standard impinger (see7.2) and the water level controller (see 7.3) to compensate for solutionevaporation.10.2.2 During the sampling period, record the time,vacuum, and meter reading at the beginning
39、and end of thesampling period. Also record barometric pressure in accor-dance with Test Method D3270 and the ambient temperature atintervals during the sampling period.A Sampling tube F MeterB Filter holder G ThermometerC Standard impinger H Metering valveD Deminster (dry-impinger) J Vacuum pumpE Ma
40、nometerSI Equivalentsin.91634 45836mm 14 19 102 127 203 914FIG. 2 Diagram of a Sample Train for Short-Term Sampling of Atmospheric FluoridesD3267 12310.2.3 Use field blanks with each sample. (See Note 4.)NOTE 5Take two filters to the field and use one for sampling. Use thesecond filter as a field bl
41、ank. Carry an impinger containing 150 mL ofdeionized water to the sampling site and treat in the same manner as thesample impingers except do not connect into a sample train. Use thisimpinger as a field blank.10.2.4 At the end of the sampling period, transfer the filterand impinger contents to suita
42、ble containers for transporting tothe work area where analyses are to be performed.10.3 See Practice D1357 for guidance on sampling.11. Preparation of Samples for Fluoride Analysis11.1 Carry out the analysis in a work area with an atmo-sphere free of contamination by fluorides.11.2 Preparation of Im
43、pinger Solutions for Fluoride Analy-sis:11.2.1 Measure the volume of liquid in the impinger byweight if a tare weight is available on the impinger or bytransferring to a tared polyethylene bottle and weighing thetotal contents after transfer. Record the weight of the liquidcontents. Mix the contents
44、 thoroughly.11.2.2 For Potentiometric Analysis:(Note 5 and Note 6).11.2.2.1 Transfer 10.0 mL of the sample into a cleanpolyethylene (or polypropylene or TFE-fluorocarbon) beakerand dilute an equal amount with TISAB buffer. (8.9)11.2.2.2 Analyze the aliquot using the potentiometric TestMethod D3269.N
45、OTE 6If the fluoride levels in the impinger solutions are lower thanthe sensitivities of the prescribed methods, then the solutions may beconcentrated for analysis as described in Test Methods D3269 or analyzedas described in Note 6.NOTE 7In the potentiometric method, the sample may be spiked withan
46、 exactly measured amount of fluoride (for example: 0.4-mL of 0.01 mgF/mL standard NaF solution in 40 mL of final volume). This additionwould be used if required to raise the concentration to a more favorablepart of the response curve of the fluoride specific ion electrode. Theconcentration added wil
47、l be deducted from the concentration determined.11.2.3 For Semiautomated Analyses:11.2.3.1 Transfer the solution to an 8.5-mL sample cup.11.2.3.2 Analyze the sample using Method D3270.11.3 Preparation of the Prefilter Used to Collect Particulatefor Fluoride Analysis:11.3.1 For Potentiometric Analysi
48、s:11.3.1.1 Place the filter in a clean polyethylene (or polypro-pylene or TFE-fluorocarbon) beaker. Add 10.0 mL of 1 NH2SO4(see 8.7), mix for a minimum of 5 min with a magneticstirrer, and allow to stand for 5 min.11.3.1.2 Add an equal volume of 1 NNaOH solution (see8.6) and mix. (See Note 7.)NOTE 8
49、In any specific sampling program, confirm the quantitativerecovery of the fluoride content of the filter extraction with 1 N H2SO4(seeA Sampling tube F Guard tubeB Filter holder G Water level controllerC Modified standard impinger H Water level sensorD Control valve J Refer to Fig. 2 for Remainder of Sam-E Water-reservoir pling train following impinger CSI Equivalentsin.91634 45836mm 14 19 102 127 203 914FIG. 3 Diagram of a Modified Standard Impinger for Long-Term Sampling of Atmospheric FluoridesD3267 1248.7) (see Test Methods D3269.)11.3.1.3 Add 20
