1、Designation: E1775 07 (Reapproved 2016)Standard Guide forEvaluating Performance of On-Site Extraction and Field-Portable Electrochemical or Spectrophotometric Analysisfor Lead1This standard is issued under the fixed designation E1775; the number immediately following the designation indicates the ye
2、ar 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.1. Scope1.1 This guide provides guidelines for determining theperf
3、ormance of field-portable quantitative lead analysis instru-ments.1.2 This guide applies to field-portable electroanalytical andspectrophotometric (including reflectance and colorimetric)analyzers.1.3 Sample matrices of concern herein include paint, dust,soil, and airborne particles.1.4 This guide a
4、ddresses the desired performance character-istics of field-based sample extraction procedures for lead, aswell as on-site extraction followed by field-portable analysis.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility o
5、f 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. Referenced Documents2.1 ASTM Standards:2D5438 Practice for Collection of Floor Dust for ChemicalAnalysisD6785 Test Method for Determination of
6、Lead in WorkplaceAir Using Flame or Graphite Furnace Atomic AbsorptionSpectrometryD6966 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 In
7、ductivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)D7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationE1605 Terminology Relating to Lead in BuildingsE1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emi
8、ssion Spectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE1644 Practice for Hot Plate Digestion of Dust WipeSamples for the Determination of LeadE1645 Practice for Preparation of Dried Paint Samples byHotplate or M
9、icrowave Digestion for Subsequent LeadAnalysisE1726 Practice for Preparation of Soil Samples by HotplateDigestion for Subsequent Lead AnalysisE1727 Practice for Field Collection of Soil Samples forSubsequent Lead Determination (Withdrawn 2014)3E1729 Practice for Field Collection of Dried Paint Sampl
10、esfor Subsequent Lead Determination (Withdrawn 2014)3E1792 Specification for Wipe Sampling Materials for Leadin Surface DustE1864 Practice for Evaluating Quality Systems of Organi-zations Conducting Facility and Hazard Assessments forLead in Paint, Dust, Airborne Particulate, and Soil in andaround B
11、uildings and Related Structures (Withdrawn2011)32.2 U.S. EPA Documents:4EPA 600/R-93/200 Standard Operating Procedure for theField Analysis of Lead in Paint, Bulk Dust, and Soil byUltrasonic,Acid Digestion and Colorimetric Measurement(1993)EPA 747-R-92-001 Laboratory Accreditation Guidelines:Measure
12、ment of Lead in Paint, Dust, and Soil (1992)1This guide is under the jurisdiction of ASTM Committee E06 on Performanceof Buildings and is the direct responsibility of Subcommittee E06.23 on LeadHazards Associated with Buildings.Current edition approved Jan. 1, 2016. Published January 2016. Originall
13、yapproved in 1996. Last previous edition approved in 2007 as E1775 07. DOI:10.1520/E1775-07R16.2For 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 Documen
14、t Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from United States Environmental ProtectionAgency (EPA), WilliamJefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.Copyright ASTM
15、International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 For definitions of terms not listed here, see TerminologyE1605.3.2 anodic stripping voltammetryan electroanalyticaltechnique in which the concentration of analyte metal speciesdissolv
16、ed in solution is determined in the following manner:The analyte is first deposited (preconcentrated) electrochemi-cally by reducing the dissolved ion in solution to immobilizedmetal species at an electrode surface (such as mercury orbismuth). The metal is deposited at an applied potential(voltage)
17、which is negative of the standard oxidation potentialfor the metal/ion redox couple. After deposition, the precon-centrated metal species is then stripped from the electrode byapplying a positive potential sweep, which causes anodicoxidation of the analyte metal species to dissolved ion. Thecurrent
18、associated with this reoxidation is measured. The peakcurrent is proportional to the original concentration of dis-solved analyte species over a wide range of concentrations.3.3 colorimetryan analytical technique that is similar tospectrophotometry (see 3.5), except that ultraviolet-visiblelight of
19、a single, narrow wavelength range is passed through asample cell containing dissolved analyte, and the absorptionmeasured.3.4 reflectancea measurement technique (subset of spec-trophotometry; see 3.5) in which light is reflected off of areflecting surface and measured by a detector. The amount ofref
20、lected light may be a function of analyte concentration.3.5 spectrophotometryan analytical technique in which aspectrum of analyte species is obtained and used to determinethe analyte concentration in the following manner. Light isdirected onto or through analyte species, and the absorption ofthis l
21、ight across a range of wavelengths is measured by adetector. The amount of absorbed light is a function of theconcentration of analyte species.4. Significance and Use4.1 This guide is intended for use in evaluating the perfor-mance of field-portable electroanalytical or spectrophotometricdevices for
22、 lead determination, or both.4.2 Desired performance criteria for field-based extractionprocedures are provided.4.3 Performance parameters of concern may be determinedusing protocols that are referenced in this guide.4.4 Example reference materials to be used in assessing theperformance of field-por
23、table lead analyzers are listed.4.5 Exhaustive details regarding quality assurance issues areoutside the scope of this guide. Applicable quality assuranceaspects are dealt with extensively in references that are cited inthis guide.5. Performance Evaluation Materials5.1 Certified Reference Materials
24、(CRMs)These may con-sist of NIST Standard Reference Materials (SRMs) and are alsoknown as Primary and Secondary Reference Materials:5.1.1 PaintExamples are NIST paint SRMs, for example,NIST SRMs 2582, 2583, and numerous other CRMs.5.1.2 DustExamples are NIST 1648 (urban particulatematter), other NIS
25、T dust SRMs, and other CRMs.5.1.3 SoilExamples are NIST 2704 (river sediment) andNIST soil standards: SRMs 2709, 2710, and 2711 and numer-ous other CRMs.5.1.4 Airborne Particulate MatterAn example is NISTSRM 2783, which is available for airborne particulate mattercollected on filters. Other CRMs are
26、 also available.5.2 Real-World Materials:5.2.1 Paint, collected using Practice E1729 (or equivalent).To obtain reference values, determine lead concentration usingTest Method E1613 and Practice E1645 (or equivalent).5.2.2 Dust Wipes, collected using Practice D6966, withwipes meeting the requirements
27、 of Specification E1792.Toobtain reference values, determine lead concentration usingTest Method E1613 and Practice E1644 (or equivalent).5.2.3 Vacuumed Dust, collected using Practices D7144 orD5438. To obtain reference values, determine lead concentra-tion using Test Method E1613 and Practice E1726
28、 (or equiva-lent).5.2.4 Soil, collected using Practice E1727. To obtain refer-ence values, determine lead concentration using Test MethodE1613 and Practice E1726 (or equivalent).5.2.5 Airborne Particulate Matter, collected using TestMethod D6785 (or equivalent). To obtain reference values,determine
29、lead concentration using Test Method E1613 andeither Test Methods D6785 or D7035 (or equivalent).5.3 Secondary Reference MaterialsExamples of theseCRMs include samples from the Environmental Lead Profi-ciency Analytical Testing (ELPAT) program (paints, dustsspiked on wipes, and soils) and the Profic
30、iency AnalyticalTesting (PAT) program (air filters).5Other examples includesecondary reference materials (for example, bag house dust,sludge, and solid waste).65.3.1 PaintExamples include ELPAT paint samples.5.3.2 DustExamples include ELPAT wipe samples spikedwith lead-containing dusts.5.3.3 SoilExa
31、mples include ELPAT soil samples.5.3.4 Air FiltersExamples include PAT air filter samples.6. Performance Criteria6.1 Extraction ProceduresThe extraction procedure cho-sen shall have a demonstrated recovery of at least 80 % for thematrix of concern, and shall be compatible with the leadanalysis techn
32、ique used (EPA 600/R-93/200). (Reference ex-traction and analytical techniques include those ASTM stan-dards listed in 2.1.)6.2 Field-Portable Analysis:6.2.1 AccuracyOverall measurement accuracy of thefield-portable analytical technique following field-based ex-traction: within 25 % of the values ob
33、tained by the applicableASTM extraction procedure (see 2.1) and Test Method E1613.5Available from American Industrial Hygiene Association (AIHA), 3141 Fair-view Park Drive, Suite 777, Falls Church, VA 22042, http:/www.aiha.org.6Available from Fisher Scientific and Resource Technology Corp., Laramie,
34、 WY.E1775 07 (2016)26.2.2 PrecisionFor field-based extraction followed byfield-portable analysis, total uncertainties for standard refer-ence materials: 25 % relative standard deviation (RSD) (EPA747-R-92-001); for real-world materials: 25 % RSD (EPA747-R-92-001); for secondary reference materials:
35、25 % RSD.6.2.3 Working RangeMinimum working concentrationrange for the overall method shall extend from 0.1 times theapplicable action level to 2 times the applicable action level(NIOSH SOP 018)7for the sample matrix of concern.6.3 Sample SizeFollow applicable ASTM sample collec-tion and sample prep
36、aration practices listed in 2.1.NOTE 1Performance data from interlaboratory testing of a portableanodic stripping voltammetric procedure have been published.87. Quality Assurance (QA) and Quality Control (QC)7.1 Field and Laboratory QA/QCFollow QA/QC proce-dures delineated in the applicable ASTM sam
37、ple preparationpractices for the pertinent sample matrix (2.1) and in TestMethod E1613.7.2 QA SystemFollow the requirements delineated inPractice E1864.NOTE 2Participation in proficiency testing programs, for example,ELPAT and other similar round robin schemes, is recommended.8. Keywords8.1 electroa
38、nalysis; extraction; lead; portable analysis; spec-trophotometryASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any suc
39、h patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invite
40、d either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a
41、fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this
42、standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Dri
43、ve, Danvers, MA 01923, Tel: (978) 646-2600; http:/ National Institute for Occupational Safety and Health (NIOSH), “Guide-lines for Air Sampling and Analysis,” available from NIOSH Publications, 4676Columbia Parkway, Cincinnati, OH 45226, www.cdc.gov/niosh.8Ashley, K., Song, R., Esche, C.A., Schlecht, P. C., Baron, P.A., and Wise, T.J.,“Ultrasonic extraction and protable anodic stripping volumetric measurement oflead in pain, dust wipes, soil, and airAn interlaboratory evaluation,” Journal ofEnvironmental Monitoring, Vol. 1, pp. 459464 (1999).E1775 07 (2016)3
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