1、Designation: D7202 11Standard Test Method forDetermination of Beryllium in the Workplace Using Field-Based Extraction and Optical Fluorescence Detection1This standard is issued under the fixed designation D7202; the number immediately following the designation indicates the year oforiginal adoption
2、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 is intended for use in the determinationof beryllium by samp
3、ling workplace air and surface dust.1.2 This test method assumes that air and surface samplesare collected using appropriate and applicable ASTM Interna-tional standard practices for sampling of workplace air andsurface dust. These samples are typically collected using airfilter sampling, vacuum sam
4、pling or wiping techniques. SeeGuide E1370 for guidance on air sampling strategies, andGuide D7659 for guidance on selection of surface samplingtechniques.1.3 Determination of beryllium in soil is not within thescope of this test method. See Test Method D7458 fordetermination of beryllium in soil sa
5、mples.1.4 This test method includes a procedure for on-site ex-traction (dissolution) of beryllium in weakly acidic medium(pH of 1 % aqueous ammonium bifluoride is 4.8), followed byfield analysis of aliquots of the extract solution using aberyllium-specific-optically fluorescent dye.1.5 The procedur
6、e is targeted for on-site use in the field foroccupational and environmental hygiene monitoring purposes.1.6 No detailed operating instructions are provided becauseof differences among various makes and models of suitablefluorometric instruments. Instead, the analyst shall follow theinstructions pro
7、vided by the manufacturer of the particularinstrument. This test method does not address comparativeaccuracy of different devices or the precision between instru-ments of the same make and model.1.7 The values stated in SI units are to be regarded asstandard.1.8 This test method contains notes that
8、are explanatory andnot part of mandatory requirements of the standard.1.9 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
9、 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtmospheresD4840 Guide for Sample Chain-of-Custody ProceduresD5337 Practice for Flow Rate Calibration of Person
10、alSampling PumpsD6966 Practice for Collection of Settled Dust SamplesUsing Wipe Sampling Methods for Subsequent Determi-nation of MetalsD7035 Test Method for Determination of Metals and Met-alloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)D714
11、4 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationD7296 Practice for Collection of Settled Dust SamplesUsing Dry Wipe Sampling Methods for Subsequent De-termination of Beryllium and CompoundsD7458 Test Method for Determination of Beryllium in Soil,
12、Rock, Sediment, and Fly Ash Using Ammonium Bifluo-ride Extraction and Fluorescence DetectionD7659 Guide for Strategies for Surface Sampling of Metalsand Metalloids for Worker ProtectionD7707 Specification for Wipe Sampling Materials for Be-ryllium in Surface DustE691 Practice for Conducting an Inter
13、laboratory Study toDetermine the Precision of a Test MethodE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1370 Guide for Air Sampling Strategies for Worker andWorkplace Protection1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and
14、 is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved Oct. 1, 2011. Published October 2011. Originallyapproved in 2005. Last previous edition approved in 2006 as D7202 - 06. DOI:10.1520/D7202-11.2For referenced ASTM standards, visit the ASTM website, w
15、ww.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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E17
16、92 Specification for Wipe Sampling Materials for Leadin Surface Dust3. Terminology3.1 DefinitionsFor definitions of terms not appearinghere, see Terminology D1356.3.2 Definition of Term Specific to This Test Method:3.2.1 wipe, na disposable towelette that is moistened witha wetting agent such as wat
17、er (E1792; D6966).3.2.1.1 DiscussionThese towelettes are used for collect-ing samples of dust, potentially containing beryllium, fromsurfaces.3.2.2 wipe sample, nsample collected by wiping a repre-sentative surface of known area, as determined by PracticeD6966, or equivalent method, with an acceptab
18、le wipe materialas defined in Practice D7707.4. Summary of Test Method4.1 Particles potentially containing beryllium from work-place air or surfaces, or both, are collected in the field usingprocedures described in ASTM International standards. Toextract (or dissolve) beryllium in the collected samp
19、les, themedia in or on which the samples are collected (that is, airsample, vacuum sample or wipe) are treated on-site using anacidic extraction solution (1)3. The presence of active fluorideions (HF by dissociation of ammonium bifluoride in acidicmedium) enables dissolution of refractory materials
20、such as“high-fired” beryllium oxide. The extraction solution producedfrom each sample is then filtered and an aliquot of this extractis added to a pH-adjusted detection solution which contains aberyllium-specific optical fluorescence reagent (1, 2). Thefluorescence exhibited by this final solution i
21、s then measuredon a calibrated field-portable fluorometer to quantify theamount of beryllium in the sample (3).5. Significance and Use5.1 Exposure to beryllium can cause a potentially fataldisease, and occupational exposure limits for beryllium in airand on surfaces have been established to reduce e
22、xposure risksto potentially affected workers (4, 5). Sampling and analyticalmethods for beryllium are needed in order to meet thechallenges relating to exposure assessment and risk reduction.Field-portable sampling and analysis methods, such as theprocedure described in this test method, are desired
23、 in order tofacilitate on-site measurement of beryllium. On-site berylliumanalysis results can then be used as a basis for management ofprotection of human health.6. Interferences6.1 This test method is highly specific for beryllium. Othersolvated metal ions are either bound by ethylenediaminetet-ra
24、acetic acid (EDTA) in the detection solution, or they precipi-tate out due to the high alkalinity of the detection solution (1).In case the sample is suspected of having fluorescent organiccontaminants that are suspected to be present, then theirpresence can be checked and removed (6).NOTE 1If the s
25、amples are suspected of having an contaminant thatfluoresces and has excitation and emission spectra that overlap with thatof the signal produced by the fluorescent dye bound to beryllium, then thiscontaminant needs to be removed. The presence of such an contaminantcan be verified by subjecting the
26、filtered sample to fluorescence excitationafter the extraction step (without adding the fluorescent dye). If afluorescence signal is detected, then that signal is due to the presence ofa fluorescent contaminant. To remove the contaminant, high purityactivated charcoal is added to the beryllium extra
27、ction solution and theextraction procedure is carried out at elevated temperature (80 to 90C forat least 45 minutes). If the beryllium extraction procedure has alreadybeen performed, then after the addition of activated charcoal, theextraction process is repeated at the elevated temperature. The sol
28、ution isfiltered to remove the activated charcoal before making the measurementsolution. The measurement solution is made by the addition of thefluorescent dye solution to an aliquot of the extraction solution. Details ofthis process have been published (6).6.2 If iron is present in high excess in t
29、he sample (typicallymore than 20 M), the resulting measurement solution mayappear golden-yellow. In this case the solution should be leftfor an hour or more for the iron to precipitate. The solutionshould then be re-filtered using the same procedure as forfiltering the dissolution solution (after th
30、e dissolution step),prior to fluorescence measurement.7. Apparatus7.1 Sampling Equipment7.1.1 Air SamplingUse air samplers and filters for collect-ing personal air samples as described in Test Method D7035.7.1.2 Wipe SamplingUse wipe sampling apparatus forcollecting surface dust samples as described
31、 in Practice D6966,using wipes meeting the specifications described in Specifica-tion D7707.7.1.3 Vacuum SamplingIf wipe sampling is not advisable,use vacuum sampling apparatus collecting surface dustsamples as described in Practice D7144.7.2 Instrumentation7.2.1 Ultraviolet/Visible (UV/Vis) Fluorom
32、eter, with irradi-ance excitation lamp (excitation l = 380 nm) and time-integrating visible detector (400-700 nm, lmax 475 nm)7.2.2 Mechanical Agitator or Heating Source, shaker, rota-tor, or ultrasonic bath; or heat block or heating bath.NOTE 2For routine samples, a shaker, rotator, or ultrasonic b
33、ath isadequate. To achieve higher recoveries from beryllium oxide (especially“high-fired” BeO), a heat block or heating bath is required.7.3 Laboratory Supplies7.3.1 Centrifuge tubes, plastic, 15-mL (plus 50-mL, ifnecessary)7.3.2 Syringe filters, 0.45-m nylon, 13- or 25-mm diam-eter, in plastic hous
34、ings7.3.3 Syringes, plastic, 5-mL or 10-mL7.3.4 Pipetters, mechanical, of assorted sizes as needed7.3.5 Pipet tips, plastic, disposable, of assorted sizes asneeded7.3.6 Fluorescence cuvettes, disposable, low fluorescence,10-mm path length, transparent to UV/Vis radiation7.3.7 Labware, plastic (for e
35、xample, beakers, flasks, gradu-ated cylinders, etc.), of assorted sizes as needed3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.D7202 1127.3.8 Forceps, plastic or plastic-coated7.3.9 Personal protective wear, for example, respirators,masks, gloves, lab
36、coats, safety eyewear, etc. as needed7.3.10 Thermometer, to at least 100C.7.3.11 Other general laboratory supplies as needed.7.4 Reagents7.4.1 WaterUnless otherwise indicated, references to wa-ter shall be understood to mean reagent as defined by Type I ofSpecification D1193 (ASTM Type I Water: mini
37、mum resis-tance of 18 MV-cm or equivalent)7.4.2 Calibration Stock Solution1000 ppm beryllium indilute nitric acid or equivalent.7.4.3 Ethylenediaminetetraacetic acid (EDTA) disodiumsalt dihydrate7.4.4 L-lysine monohydrochloride7.4.5 10-hydroxybenzohquinoline-7-sulfonate(10-HBQS).7.4.6 Sodium hydroxi
38、de7.4.7 Extraction (or Dissolution) Solution1 % ammoniumbifluoride (NH4HF2) solution (aqueous) for dissolution ofberyllium in collected particulate matter. (WarningAmmonium bifluoride will etch glass, so it is essential that allNH4HF2solutions be contained in plastic labware.)7.4.8 Detection Solutio
39、n63.4 M 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS) / 2.5 mMethylenediaminetetraacetic acid (EDTA)/50.8 mM lysinemonohydrochloride (pH adjusted to 12.8 with NaOH): Theaqueous detection reagent is prepared by the addition of 12.5mL of 10.7 mM ethylenediaminetetraacetic acid (EDTA)disodium salt di
40、hydrate and 25 mL of 107 mM L-lysinemonohydrochloride to 3 mL of 1.1 mM 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS). The pH isadjusted to 12.85 with addition of sodium hydroxide and wateradded to a total of 50 mL (1).NOTE 3It is recommended that the extraction and detection solutionsbe prepared
41、in a fixed-site laboratory or other such controlled environmentprior to transport to the field.8. Procedure8.1 Sampling8.1.1 Air SamplesCollect workplace air samples for be-ryllium in accordance with Test Method D7035, using personalsampling pumps calibrated in accordance with Practice D5337.8.1.2 W
42、ipe SamplesCollect surface wipe samples forberyllium in accordance with Practices D6966 and D7296using wipe materials that comply with Specification D7707.NOTE 4Practice D7296 should only be used when wetted wipesampling is not physically feasible (for example, if the surface to be wipedwould be com
43、promised by use of wetted wipes). Otherwise, PracticeD6966 should be used.8.1.3 Vacuum SamplesIf wipe sampling is inadvisable forsurface dust sampling, collect surface vacuum samples forberyllium in accordance with Practice D7144.8.1.4 Sample TransportIf applicable (that is, if samplesare transporte
44、d to a different location prior to sample prepara-tion and analysis), follow sampling chain-of-custody proce-dures to document sample traceability. Ensure that the docu-mentation that accompanies the samples is suitable for a chainof custody to be established in accordance with Guide D4840.8.2 Sampl
45、e PreparationWear appropriate personal pro-tection during sample preparation and analysis activities.Perform sample preparation and analysis in a clean area that iswell removed from any possible beryllium contamination.8.2.1 Extraction of Air Filter Samples8.2.1.1 Don clean gloves and open the sampl
46、ers. Usingforceps, remove the filters from the cassette and place theminto 15-mL centrifuge tubes.NOTE 5If the entire contents of the sampler are regarded as part of thesample, the interior of the cassette should be rinsed with extractionsolution, or wiped with another clean filter, and included in
47、the centrifugetube. Alternatively, the extraction can be carried out within the samplingcassette (see Test Method D7035).8.2.1.2 Pipet 5 mL of 1 % ammonium bifluoride extractionsolution (see 7.4.7) into the centrifuge tubes containing the airfilter samples.8.2.1.3 Cap the centrifuge tubes, and agita
48、te or heat thesamples.(1) Activate the shaker, rotator, or ultrasonic bath, andagitate for a minimum of 30 minutes; or(2) Preheat the heat block or heating bath to 85C (65C).and heat for a minimum of 30 minutes.NOTE 6Extraction is an example of a dissolution and solvatingprocess. Method evaluation m
49、ight indicate that for complete dissolution ofberyllium, it may be necessary for the dissolution process to be assisted byultrasonic energy, heat or longer treatment periods to obtain acceptablerecoveries. This will be dependent upon the sample media, particlephysical characteristics (such as shape and size) and the inertness ofberyllium-containing compounds. Heating to between 80 and 90C isrequired for the dissolution of refractory compounds such as “high-fired”beryllium oxide.8.2.1.4 If the samples are heated during the extraction step,they sha
