1、Designation: D7202 11D7202 14Standard Test Method forDetermination of Beryllium in the Workplace Using Field-Based by Extraction and Optical Fluorescence Detection1This standard is issued under the fixed designation D7202; the number immediately following the designation indicates the year oforigina
2、l 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 is intended for use in the determination of beryl
3、lium by sampling workplace air and surface dust.1.2 This test method assumes that air and surface samples are collected using appropriate and applicable ASTM Internationalstandard practices for sampling of workplace air and surface dust. These samples are typically collected using air filter samplin
4、g,vacuum sampling or wiping techniques. See Guide E1370 for guidance on air sampling strategies, and Guide D7659 for guidanceon selection of surface sampling techniques.1.3 Determination of beryllium in soil is not within the scope of this test method. See Test Method D7458 for determinationof beryl
5、lium in soil samples.1.4 This test method includes a procedure for on-site extraction (dissolution) of beryllium in weakly acidic medium (pH of 1 %aqueous ammonium bifluoride is 4.8), followed by field analysis of aliquots of the extract solution using a beryllium-specific-optically fluorescent dye.
6、1.5 The procedure is targetedsuitable for on-site use in the field for occupational and environmental hygiene monitoringpurposes. The method is also applicable for use in fixed-site laboratories.1.6 No detailed operating instructions are provided because of differences among various makes and models
7、 of suitablefluorometric instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particularinstrument. This test method does not address comparative accuracy of different devices or the precision between instruments ofthe same make and model.1.7 The values
8、 stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.8 This test method contains notes that are explanatory and not part of mandatory requirements of the standard.1.9 This standard does not purport to address all of the safety concerns, if
9、 any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1356 Termino
10、logy Relating to Sampling and Analysis of AtmospheresD4840 Guide for Sample Chain-of-Custody ProceduresD5337 Practice for Flow Rate Adjustment of Personal Sampling PumpsD6966 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Determination of MetalsD7035 Test
11、Method for Determination of Metals and Metalloids in Airborne Particulate Matter by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)D7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationD7296 Practice for Collection of Settled Dust
12、Samples Using Dry Wipe Sampling Methods for Subsequent Determination ofBeryllium and Compounds1 This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality.Current edition approved Oct. 1, 2011April
13、1, 2014. Published October 2011May 2014. Originally approved in 2005. Last previous edition approved in 20062011 asD7202 - 06.D7202 11. DOI: 10.1520/D7202-11.10.1520/D7202-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For
14、Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not
15、 be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Dr
16、ive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D7458 Test Method for Determination of Beryllium in Soil, Rock, Sediment, and Fly Ash Using Ammonium BifluorideExtraction and Fluorescence DetectionD7659 Guide for Strategies for Surface Sampling of Metals and Metalloids for Worker Pr
17、otectionD7707 Specification for Wipe Sampling Materials for Beryllium in Surface DustE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE882 Guide for Accountability and Quality Co
18、ntrol in the Chemical Analysis LaboratoryE1370 Guide for Air Sampling Strategies for Worker and Workplace ProtectionE1792 Specification for Wipe Sampling Materials for Lead in Surface Dust3. Terminology3.1 DefinitionsFor definitions of terms not appearing here, see Terminology D1356.3.2 Definitions
19、of Terms Specific to This Standard:3.2.1 wipe, na disposable towelette that is moistened with a wetting agent such as water (water.E1792; D6966). E1792;D69663.2.1.1 DiscussionThese towelettes are used for collecting samples of dust, potentially containing beryllium, from surfaces.3.2.2 wipe sample,
20、nsample collected by wiping a representative surface of known area, as determined by Practice D6966,or equivalent method, with an acceptable wipe material as defined in PracticeSpecification D7707.4. Summary of Test Method4.1 Particles potentially containing beryllium from workplace air or surfaces,
21、 or both, are collected in the field using proceduresdescribed in ASTM International standards. To extract (or dissolve) beryllium in the collected samples, the media in or on whichthe samples are collected (that is, air sample, vacuum sample or wipe) are treated on-site using an acidic extraction s
22、olution(containing dilute ammonium bifluoride, NH4HF2 (1).)3. The presence of active fluoride ions (HF by dissociation of ammoniumbifluoride in acidic medium) enables dissolution of refractory materials such as “high-fired” beryllium oxide. The extractionsolution produced from each sample is then fi
23、ltered and an aliquot of this extract is added to a pH-adjusted detection solution whichcontains a beryllium-specific optical fluorescence reagent (1, 2).). The fluorescence exhibited by this final solution is thenmeasured on a calibrated field-portable fluorometer to quantify the amount of berylliu
24、m in the sample (3).).5. Significance and Use5.1 Exposure to beryllium can cause a potentially fatal disease, and occupational exposure limits for beryllium in air and onsurfaces have been established to reduce exposure risks to potentially affected workers (4, 5). Sampling and analytical methodsfor
25、 beryllium are needed in order to meet the challenges relating to exposure assessment and risk reduction. Field-portablesampling Sampling and analysis methods, such as the procedure described in this test method, are desired in order to facilitateon-site and fixed-site laboratory measurement of trac
26、e beryllium. On-site beryllium Beryllium analysis results can then be used asa basis for management of exposure assessment and protection of human health.6. Interferences6.1 This test method is highly specific for beryllium. Other solvated metal ions are either bound by ethylenediaminetetraaceticaci
27、d (EDTA) in the detection solution, or they precipitate out due to the high alkalinity of the detection solution (1).). In case thesample is suspected of having fluorescent organic contaminants that are suspected to be present, then their presence can be checkedand removed (6).).NOTE 1If the samples
28、 are suspected of having ana contaminant that fluoresces and has excitation and emission spectra that overlap with that of thesignal produced by the fluorescent dye bound to beryllium, then this contaminant needs to be removed. The presence of such ana contaminant can beverified by subjecting the fi
29、ltered sample to fluorescence excitation after the extraction step (without adding the fluorescent dye). If a fluorescence signalis detected, then that signal is dueascribed to the presence of a fluorescent contaminant. To remove the contaminant, high purity high-purity activatedcharcoal is added to
30、 the beryllium extraction solution and the extraction procedure is carried out at elevated temperature (80 to 90C for at least 45minutes). If the beryllium extraction procedure has already been performed, then after the addition of activated charcoal, the extraction process is repeatedat the elevate
31、d temperature. The solution is filtered to remove the activated charcoal before making the measurement solution. The measurement solutionis made by the addition of the fluorescent dye solution to an aliquot of the extraction solution. Details of this process have been published (6).).6.2 If iron is
32、present in high excess in the sample (typically more than 20 M), the resulting measurement solution may appeargolden-yellow. In this case the solution should be left for an hour or more for the iron to precipitate. The solution should then bere-filtered using the same procedure as for filtering the
33、dissolution solution (after the dissolution step), prior to fluorescencemeasurement.3 The boldface numbers in parentheses refer to a list of references at the end of this standard.D7202 1427. Apparatus7.1 Sampling EquipmentEquipment:7.1.1 Air SamplingUse air samplers and filters for collecting perso
34、nal air samples as described in Test Method D7035.7.1.2 Wipe SamplingUse wipe sampling apparatus for collecting surface dust samples as described in Practice D6966, (orPractice D7296 in special cases), using wipes meeting the specifications described in Specification D7707.7.1.3 Vacuum SamplingIf wi
35、pe sampling is not advisable, advisable for surface sample collection, use vacuum samplingapparatus for collecting surface dust samples as described in Practice D7144.7.2 InstrumentationInstrumentation:7.2.1 Ultraviolet/Visible (UV/Vis) Fluorometer, with irradiance excitation lamp (excitation = 380
36、nm) and time-integratingvisible detector (400-700(400700 nm, max 475 nm)nm).7.2.2 Mechanical Agitator or Heating Source, shaker, rotator,rotator or ultrasonic bath; or heat block block, oven or heatingbath.NOTE 2For routine samples, a shaker, rotator, or ultrasonic bath is adequate. To achieve highe
37、r recoveries from beryllium oxide (especially“high-fired” BeO), a heat block block, oven or heating bath is required.7.3 Laboratory SuppliesSupplies:7.3.1 Centrifuge tubes, plastic, 15-mL (plus 50-mL, if necessary)necessary).7.3.2 Syringe filters, 0.2 to 0.45-m nylon, polyethersulfone or hydrophilic
38、 polypropylene, 13- or 25-mm diameter, in plastichousingshousings.7.3.3 Syringes, plastic, 5-mL or 10-mL10-mL.7.3.4 Pipetters, mechanical, of assorted sizes as neededneeded.7.3.5 Pipet tips, plastic, disposable, of assorted sizes as neededneeded.7.3.6 Fluorescence cuvettes, disposable, low fluoresce
39、nce, 10-mm path length, transparent to UV/Vis radiationradiation.7.3.7 Labware, plastic (for example, beakers, flasks, graduated cylinders, etc.), of assorted sizes as neededneeded.7.3.8 Forceps, plastic or plastic-coatedplastic-coated.7.3.9 Personal protective wear, for example, respirators, masks,
40、 gloves, lab coats, safety eyewear, etc.etc., as neededneeded.7.3.10 Thermometer, to at least 100C.7.3.11 Other general laboratory suppliesapparatus, as needed.7.4 ReagentsReagents:7.4.1 WaterUnless otherwise indicated, references to water shall be understood to mean reagent as defined by Type I ofS
41、pecification D1193 (ASTM Type I Water: minimum resistance of 18 M-cm or equivalent)7.4.2 Calibration Stock Solution1000 ppm beryllium in dilute nitric acid or equivalent.7.4.3 Ethylenediaminetetraacetic acid (EDTA) disodium salt dihydratedihydrate.7.4.4 L-lysine monohydrochloridemonohydrochloride.7.
42、4.5 10-hydroxybenzohquinoline-7-sulfonate(10-HBQS).7.4.6 Sodium hydroxidehydroxide.7.4.7 Extraction (or Dissolution) Solution1 % 1 % ammonium bifluoride (NH4HF2) solution (aqueous) for dissolution ofberyllium in collected particulate matter. (WarningAmmonium bifluoride will etch glass, so it is esse
43、ntial that all NH4HF2solutions be contained in plastic labware.)7.4.8 Detection Solution63.4 M 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS) / 2.5 mM ethylenediaminetetraaceticacid (EDTA)/50.8 mM lysine monohydrochloride (pH adjusted to 12.8 with NaOH): The aqueous detection reagent is preparedby
44、the addition of 12.5 mL of 10.7 mM ethylenediaminetetraacetic acid (EDTA) disodium salt dihydrate and 25 mL of 107 mML-lysine monohydrochloride to 3 mL of 1.1 mM 10-hydroxybenzohquinoline-7-sulfonate (10-HBQS). The pH is adjusted to12.85 with addition of sodium hydroxide and water added to a total o
45、f 50 mL (1(1-3).).NOTE 3It For on-site analysis, it is recommended that the extraction and detection solutions be prepared in a fixed-site laboratory or other suchcontrolled environment prior to transport to the field.8. Procedure8.1 SamplingSampling:8.1.1 Air SamplesCollect workplace air samples fo
46、r beryllium in accordance with Test Method D7035, using personalsampling pumps calibrated in accordance with Practice D5337.8.1.2 Wipe SamplesCollect surface wipe samples for beryllium in accordance with Practices D6966 and D7296 using wipematerials that comply with Specification D7707.NOTE 4Practic
47、e D7296 should only be used when wetted wipe sampling is not physically feasible (for example, if the surface to be wiped wouldbe compromised by use of wetted wipes). Otherwise, Practice D6966 should be used.D7202 1438.1.3 Vacuum SamplesIf wipe sampling is inadvisable for surface dust sampling, coll
48、ect surface vacuum samples forberyllium in accordance with Practice D7144.8.1.4 Sample TransportIf applicable (that is, if samples are transported to a different location prior to sample preparation andanalysis), follow sampling chain-of-custody procedures to document sample traceability. Ensure tha
49、t the documentation thataccompanies the samples is suitable for a chain of custody to be established in accordance with Guide D4840.8.2 Sample PreparationWear appropriate personal protection during sample preparation and analysis activities. Performsample preparation and analysis in a clean area that is well removed from any possible beryllium contamination.8.2.1 Extraction of Air Filter Samples or Vacuum Samples:8.2.1.1 Don clean gloves and open the samplers. Using forceps, remove theUse either technique (1 filters from) or (2 the cas
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