1、Designation: D 7202 06Standard Test Method forDetermination of Beryllium in the Workplace Using Field-Based Extraction and Fluorescence Detection1This standard is issued under the fixed designation D 7202; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 sampling
3、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 sampling
4、 or wiping techniques.1.3 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 fluorescent dye.1.4 The pr
5、ocedure is targeted for on-site use in the field foroccupational and environmental hygiene monitoring purposes.1.5 No detailed operating instructions are provided becauseof differences among various makes and models of suitablefluorometric instruments. Instead, the analyst shall follow theinstructio
6、ns provided 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.1.6 The values stated in SI units are to be regarded asstandard.1.7 This test method contains notes
7、 that are explanatory andnot part of mandatory requirements of the standard.1.8 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 determi
8、ne the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 4840 Guide for Sample Chain-of-Custody ProceduresD 5337 Practice for Flow Rate Calibration
9、 of PersonalSampling PumpsD 6966 Practice for Collection of Settled Dust SamplesUsing Wipe Sampling Methods for Subsequent Determi-nation of MetalsD 7035 Test Method for Determination of Metals and Met-alloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emission Spectrometry (
10、ICP-AES)D 7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationD 7296 Practice for Collection of Settled Dust SamplesUsing Dry Wipe Sampling Methods for Subsequent De-termination of Beryllium and CompoundsE 691 Practice for Conducting an Interlabor
11、atory Study toDetermine the Precision of a Test MethodE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1792 Specification for Wipe Sampling Materials for Leadin Surface Dust3. Terminology3.1 DefinitionsFor definitions of terms not appearinghere, see Terminology
12、D 1356.3.2 Definition of Term Specific to This Test Method:3.2.1 wipe, na disposable towelette that is moistened witha wetting agent such as water (E 1792; D 6966).1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.04
13、on WorkplaceAtmospheres.Current edition approved Oct. 1, 2006. Published November 2006. Originallyapproved in 2005. Last previous edition approved in 2005 as D 7202 - 05.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annu
14、al 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.3.2.1.1 DiscussionThese towelettes are used for collect-ing samples of dust,
15、 potentially containing beryllium, fromsurfaces.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 s
16、amples, themedia in or on which the samples are collected (that is, airsample, vacuum sample or wipe) are treated on-site using anacidic extraction solution. The presence of active fluoride ions(HF by dissociation of ammonium bifluoride in acidic medium)enables dissolution of refractory materials su
17、ch as “high-fired”beryllium oxide. The extraction solution produced from eachsample is then filtered and an aliquot of this extract is added toa pH-adjusted detection solution which contains a beryllium-specific fluorescence reagent. The fluorescence of this finalsolution is then measured on a calib
18、rated field-portable fluo-rometer to quantify the amount of beryllium in the sample.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 exposure risksto potentially
19、 affected workers (1, 2). 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 in order tofacilitate on-s
20、ite 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-raacetic acid (EDTA) in the d
21、etection solution, or they precipi-tate out due to the high alkalinity of the detection solution.6.2 If iron is present in high excess in the 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
22、the iron to precipitate. The solutionshould then be re-filtered using the same procedure as forfiltering the dissolution solution (after the dissolution step),prior to fluorescence measurement.7. Apparatus7.1 Sampling Equipment7.1.1 Air SamplingUse air samplers and filters for collect-ing personal a
23、ir samples as described in Test Method D 7035.7.1.2 Wipe SamplingUse wipe sampling apparatus forcollecting surface dust samples as described in PracticesD 6966 and D 7296.7.1.3 Vacuum SamplingIf wipe sampling is not advisable,use vacuum sampling apparatus collecting surface dustsamples as described
24、in Practice D 7144.7.2 Instrumentation7.2.1 Ultraviolet/Visible (UV/Vis) Fluorometer, 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 blo
25、ck or heating bath.NOTE 1For routine samples, a shaker, rotator, or ultrasonic bath 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, ifnecess
26、ary)7.3.2 Syringe filters, 0.45-m nylon, 13- or 25-mm diam-eter, in plastic housings7.3.3 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
27、,10-mm path length, transparent to UV/Vis radiation7.3.7 Labware, plastic (for example, beakers, flasks, gradu-ated cylinders, etc.), of assorted sizes as needed7.3.8 Forceps, plastic or plastic-coated7.3.9 Personal protective wear, for example, respirators,masks, gloves, lab coats, safety eyewear,
28、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 D 1193 (ASTM Type I Water: minimum resis-tance of 18
29、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 hydroxide7.4.7 Extraction (or
30、 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 Solution63.4 M 10-hydroxybenz
31、ohquinoline-7-sulfonate (10-HBQS) (3) / 2.5mM ethylenediaminetetraacetic 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 dihydrate and 25 mL
32、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.NOTE 2It is recommended to prepare the extraction and detectionsolutions in a fixed-site laboratory p
33、rior to transport to the field.D72020628. Procedure8.1 Sampling8.1.1 Air SamplesCollect workplace air samples for be-ryllium in accordance with Test Method D 7035, using per-sonal sampling pumps calibrated in accordance with PracticeD 5337.8.1.2 Wipe SamplesCollect surface wipe samples forberyllium
34、in accordance with Practices D 6966 and D 7296.8.1.3 Vacuum SamplesIf wipe sampling is inadvisable forsurface dust sampling, collect surface vacuum samples forberyllium in accordance with Practice D 7144.8.1.4 Sample TransportIf applicable (that is, if samplesare transported to a different location
35、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 D 4840.8.2 Sample PreparationWear appropr
36、iate 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 samplers. Usingforceps, remove
37、 the filters from the cassette and place theminto 15-mL centrifuge tubes.NOTE 3If 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 the centrifugetube. Alter
38、natively, the extraction can be carried out within the samplingcassette (see Test Method D 7035).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 agitate or heat thesamples.(1
39、) 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 4Extraction is an example of a dissolution and solvatingprocess. Method evaluation might indicate that for c
40、omplete 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 inertn
41、ess 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 shall be cooled to ambient temperature before aliquots areremoved prior to
42、addition of the detection solution.8.2.2 Extraction of Wipe Samples8.2.2.1 Don clean gloves and, using forceps, place the wipesinto 15- or 50-mL centrifuge tubes.NOTE 5The size of the wipes used for sampling (8.1.2) will determinethe size of the centrifuge tubes to use for extraction. Small wipe mat
43、erials,such as 47-mm diameter filters, can be placed into 15-mLcentrifuge tubes.Larger wipes, however, will require the use of larger tubes such as 50-mLvolume. Use of 15-mL centrifuge tubes will facilitate achievement of thelower detection limit.8.2.2.2 Pipet 5 mL or 10 mL of 1 % ammonium bifluorid
44、eextraction solution (see 7.4.7) into the centrifuge tubes con-taining the wipe samples.NOTE 6The size of the wipes used for sampling (8.1.2) and the sizeof the centrifuge tubes used for extraction will determine the volume ofextraction solution to add. Small wipes in 15-mL tubes will require only5
45、mL of extraction solution, but larger wipes in 50-mL tubes will requirea minimum of 10 mL of extraction solution to ensure complete wettingand effective extraction. Use of a 15-mL centrifuge tube and 5 mL ofextraction solution will result in a lower detection limit than with use ofthe larger centrif
46、uge tube and a larger extraction solution volume.8.2.2.3 Cap the centrifuge tubes, and agitate or heat thesamples.(1) Activate the mechanical shaker, agitator, or ultrasonicbath, and agitate the samples for a minimum of 30 minutes; or(2) Preheat the heat block or heating bath to 85C (65C),and heat t
47、he samples for a minimum of 30 minutes.NOTE 7Extraction is an example of a dissolution and solvatingprocess. Method evaluation might indicate that for complete dissolution ofberyllium, it may be necessary for the dissolution process to be assisted byultrasonic energy, heat or longer treatment period
48、s 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”beryl
49、lium oxide.8.2.2.4 If the samples are heated during the extraction step,they shall be cooled to ambient temperature before aliquots areremoved prior to addition of the detection solution.8.2.3 FiltrationFilter aliquots (for example, 5 mL) ofextract solution through inert microfilters.NOTE 80.45-micrometre filters are acceptable. Preferred filters aremade out of nylon.NOTE 9The filtration process can be carried out by attaching a 25-mmdiameter syringe filter to a 5- or 10-mL Luer lock syringe and pouring theliquid contents into the syringe. The
