1、Designation: E 1775 07Standard Guide forEvaluating Performance of On-Site Extraction and Field-Portable Electrochemical or Spectrophotometric Analysisfor Lead1This standard is issued under the fixed designation E 1775; the number immediately following the designation indicates the year oforiginal ad
2、option or, in 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 standard provides guidelines for determining theperformance of f
3、ield-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 addresses the
4、 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 of the user o
5、f 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:2D 5438 Practice for Collection of Floor Dust for ChemicalAnalysisD 6785 Test Method for Determination of Lead in Wo
6、rk-place Air Using Flame or Graphite Furnace Atomic Ab-sorption SpectrometryD 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 Induct
7、ivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)D 7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationE 1605 Terminology Relating to Lead in BuildingsE 1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emis
8、sion Spectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE 1644 Practice for Hot Plate Digestion of Dust WipeSamples for the Determination of LeadE 1645 Practice for Preparation of Dried Paint Samples byHotplate or
9、Microwave Digestion for Subsequent LeadAnalysisE 1726 Practice for Preparation of Soil Samples by HotplateDigestion for Subsequent Lead AnalysisE 1727 Practice for Field Collection of Soil Samples forSubsequent Lead DeterminationE 1729 Practice for Field Collection of Dried Paint Samplesfor Subseque
10、nt Lead DeterminationE 1792 Specification for Wipe Sampling Materials for Leadin Surface DustE 1864 Practice for Evaluating Quality Systems of Organi-zations Conducting Facility and Hazard Assessments forLead in Paint, Dust, Airborne Particulate, and Soil in andaround Buildings and Related Structure
11、s2.2 U.S. EPA Documents:3EPA 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:Measurement of Lead in Paint, Dust, and Soil (1992)3.
12、Terminology3.1 For definitions of terms not listed here, see TerminologyE 1605.3.2 anodic stripping voltammetryan electroanalyticaltechnique in which the concentration of analyte metal speciesdissolved in solution is determined in the following manner:1This guide is under the jurisdiction of ASTM Co
13、mmittee E06 on Performanceof Buildings and is the direct responsibility of Subcommittee E06.23 on LeadHazards Associated with Buildings.Current edition approved Aug. 1, 2007. Published August 2007. Originallyapproved in 1996. Last previous edition approved in 2001 as E 1775 01.2For referenced ASTM s
14、tandards, 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.3Available from United States Environmental Protection Agency (EPA), ArielRios Bldg
15、., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http:/www.epa.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.The analyte is first deposited (preconcentrated) electrochemi-cally by reducing the dissolved ion in solution to i
16、mmobilizedmetal species at an electrode surface (such as mercury orbismuth). The metal is deposited at an applied potential(voltage) 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 ele
17、ctrode byapplying a positive potential sweep, which causes anodicoxidation of the analyte metal species to dissolved ion. Thecurrent associated with this reoxidation is measured. The peakcurrent is proportional to the original concentration of dis-solved analyte species over a wide range of concentr
18、ations.3.3 colorimetryan analytical technique that is similar tospectrophotometry (see 3.5), except that ultraviolet-visiblelight of a single, narrow wavelength range is passed through asample cell containing dissolved analyte, and the absorptionmeasured.3.4 reflectancea measurement technique (subse
19、t of spec-trophotometry; see 3.5) in which light is reflected off of areflecting surface and measured by a detector. The amount ofreflected light may be a function of analyte concentration.3.5 spectrophotometryan analytical technique in which aspectrum of analyte species is obtained and used to dete
20、rminethe analyte concentration in the following manner. Light isdirected onto or through analyte species, and the absorption ofthis light 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
21、.1 This guide is intended for use in evaluating the perfor-mance of field-portable electroanalytical or spectrophotometricdevices for lead determination, or both.4.2 Desired performance criteria for field-based extractionprocedures are provided.4.3 Performance parameters of concern may be determined
22、using protocols that are referenced in this guide.4.4 Example reference materials to be used in assessing theperformance of field-portable lead analyzers are listed.4.5 Exhaustive details regarding quality assurance issues areoutside the scope of this guide. Applicable quality assuranceaspects are d
23、ealt with extensively in references that are cited inthis guide.5. Performance Evaluation Materials5.1 Certified Reference Materials (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
24、SRMs, for example,NIST SRMs 2582, 2583, and numerous other CRMs.5.1.2 DustExamples are NIST 1648 (urban particulatematter), other NIST 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
25、 Particulate MatterAn example is NISTSRM 2783, which is available for airborne particulate mattercollected on filters. Other CRMs are also available.5.2 Real-World Materials:5.2.1 Paint, collected using Practice E 1729 (or equivalent).To obtain reference values, determine lead concentration usingTes
26、t Method E 1613 and Practice E 1645 (or equivalent).5.2.2 Dust Wipes, collected using Practice D 6966, withwipes meeting the requirements of Specification E 1792.Toobtain reference values, determine lead concentration usingTest Method E 1613 and Practice E 1644 (or equivalent).5.2.3 Vacuumed Dust, c
27、ollected using Practices D 7144 orD 5438. To obtain reference values, determine lead concentra-tion using Test Method E 1613 and Practice E 1726 (orequivalent).5.2.4 Soil, collected using Practice E 1727. To obtain refer-ence values, determine lead concentration using Test MethodE 1613 and Practice
28、E 1726 (or equivalent).5.2.5 Airborne Particulate Matter, collected using TestMethod D 6785 (or equivalent). To obtain reference values,determine lead concentration using Test Method E 1613 andeither Test Methods D 6785 or D 7035(or equivalent).5.3 Secondary Reference MaterialsExamples of theseCRMs
29、include samples from the Environmental Lead Profi-ciency Analytical Testing (ELPAT) program (paints, dustsspiked on wipes, and soils) and the Proficiency AnalyticalTesting (PAT) program (air filters).4Other examples includesecondary reference materials (for example, bag house dust,sludge, and solid
30、waste).55.3.1 PaintExamples include ELPAT paint samples.5.3.2 DustExamples include ELPAT wipe samples spikedwith lead-containing dusts.5.3.3 SoilExamples include ELPAT soil samples.5.3.4 Air FiltersExamples include PAT air filter samples.6. Performance Criteria6.1 Extraction ProceduresThe extraction
31、 procedure cho-sen shall have a demonstrated recovery of at least 80 % for thematrix of concern, and shall be compatible with the leadanalysis technique 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:
32、6.2.1 AccuracyOverall measurement accuracy of thefield-portable analytical technique following field-based ex-traction: within 25 % of the values obtained by the applicableASTM extraction procedure (see 2.1) and Test Method E 1613.6.2.2 PrecisionFor field-based extraction followed byfield-portable a
33、nalysis, total uncertainties for standard refer-ence materials: 25 % relative standard deviation (RSD)(EPA 747-R-92-001); for real-world materials: 25 % RSD(EPA 747-R-92-001); for secondary reference materials: 25 %RSD.6.2.3 Working RangeMinimum working concentrationrange for the overall method shal
34、l extend from 0.1 times the4Available from the American Industrial Hygiene Association (AIHA), 2700Prosperity Ave., Suite 250, Fairfax, VA 220315Available from Fisher Scientific and Resource Technology Corp., Laramie, WY.E1775072applicable action level to 2 times the applicable action level(NIOSH SO
35、P 018)6for the sample matrix of concern.6.3 Sample SizeFollow applicable ASTM sample collec-tion and sample preparation practices listed in 2.1.NOTE 1Performance data from interlaboratory testing of a portableanodic stripping voltammetric procedure have been published77. Quality Assurance (QA) and Q
36、uality Control (QC)7.1 Field and Laboratory QA/QCFollow QA/QC proce-dures delineated in the applicable ASTM sample preparationpractices for the pertinent sample matrix (2.1) and in TestMethod E 1613.7.2 QA SystemFollow the requirements delineated inPractice E 1864.NOTE 2Participation in proficiency
37、testing programs, for example,ELPAT and other similar round robin schemes, is recommended.8. Keywords8.1 electroanalysis; extraction; lead; portable analysis;spectrophotometryASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentio
38、nedin this standard. Users of this standard are expressly advised that determination of the validity of any such 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 an
39、d must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited 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 o
40、f theresponsible technical committee, which you may attend. If you feel that your comments have not received a 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
41、 C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this 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).6Natio
42、nal Institute for Occupational Safety and Health (NIOSH), “Guidelinesfor Air Sampling and Analysis,” available from NIOSH Publications, 4676Columbia Parkway, Cincinnati, OH 45226, www.cdc.gov/niosh.7Ashley, 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).E1775073
