1、Designation: E1775 07 (Reapproved 2016)E1775 16Standard 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 indicate
2、s the year 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
3、 the performance of field-portable quantitative lead analysis instruments.1.2 This guide applies to field-portable electroanalytical and spectrophotometric (including reflectance and colorimetric)analyzers.1.3 Sample matrices of concern herein include paint, dust, soil, and airborne particles.1.4 Th
4、is guide addresses the desired performance characteristics of field-based sample extraction procedures for lead, as wellas on-site extraction followed by field-portable analysis.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the respo
5、nsibilityof 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:2D5438 Practice for Collection of Floor Dust for Chemical AnalysisD6785 Test Method for Determina
6、tion of Lead in Workplace Air Using Flame or Graphite Furnace Atomic AbsorptionSpectrometryD6966 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Determination of MetalsD7035 Test Method for Determination of Metals and Metalloids in Airborne Particulate Matt
7、er by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)D7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationD7439 Test Method for Determination of Elements in Airborne Particulate Matter by Inductively Coupled PlasmaMassSpectrometry
8、E1605 Terminology Relating to Lead in BuildingsE1613 Test Method for Determination of Lead by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES),FlameAtomicAbsorption Spectrometry (FAAS), or Graphite FurnaceAtomicAbsorption Spectrometry (GFAAS) TechniquesE1644 Practice for Hot Plate D
9、igestion of Dust Wipe Samples for the Determination of LeadE1645 Practice for Preparation of Dried Paint Samples by Hotplate or Microwave Digestion for Subsequent Lead AnalysisE1726 Practice for Preparation of Soil Samples by Hotplate Digestion for Subsequent Lead AnalysisE1727 Practice for Field Co
10、llection of Soil Samples for Subsequent Lead DeterminationE1729 Practice for Field Collection of Dried Paint Samples for Subsequent Lead DeterminationE1792 Specification for Wipe Sampling Materials for Lead in Surface DustE1864 Practice for Evaluating Quality Systems of Organizations Conducting Faci
11、lity and HazardAssessments for Lead in Paint,Dust, Airborne Particulate, and Soil in and around Buildings and Related Structures (Withdrawn 2011)31 This guide is under the jurisdiction of ASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead H
12、azardsAssociated with Buildings.Current edition approved Jan. 1, 2016March 1, 2016. Published January 2016April 2016. Originally approved in 1996. Last previous edition approved in 20072016 asE1775 07.E1775 07 (2016). DOI: 10.1520/E1775-07R16.10.1520/E1775-16.2 For referencedASTM standards, visit th
13、eASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document i
14、s 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 be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as approp
15、riate. 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 Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 U.S. EPA Documents:4EPA 600/R-93/200 Standard Operating Pro
16、cedure for the Field Analysis of Lead in Paint, Bulk Dust, and Soil by Ultrasonic,Acid Digestion and Colorimetric Measurement (1993)EPA 747-R-92-001 Laboratory Accreditation Guidelines: Measurement of Lead in Paint, Dust, and Soil (1992)2.3 ISO Document:5ISO Guide 30 Reference materials - Selected t
17、erms and definitions3. Terminology3.1 For definitions of terms not listed here, see Terminology E1605.3.2 anodic stripping voltammetryan electroanalytical technique in which the concentration of analyte metal species dissolvedin solution is determined in the following manner: The analyte is first de
18、posited (preconcentrated) electrochemically by reducingthe dissolved ion in solution to immobilized metal species at an electrode surface (such as mercury or bismuth). The metal isdeposited at an applied potential (voltage) which is negative of the standard oxidation potential for the metal/ion redo
19、x couple.After deposition, the preconcentrated metal species is then stripped from the electrode by applying a positive potential sweep,which causes anodic oxidation of the analyte metal species to dissolved ion. The current associated with this reoxidation ismeasured. The peak current is proportion
20、al to the original concentration of dissolved analyte species over a wide range ofconcentrations.determined.3.2.1 DiscussionThe analyte is first deposited (preconcentrated) electrochemically by reducing the dissolved ion in solution to immobilized metalspecies at an electrode surface (such as mercur
21、y or bismuth). The metal is deposited at an applied potential (voltage) which isnegative of the standard oxidation potential for the metal/ion redox couple. After deposition, the preconcentrated metal species isthen stripped from the electrode by applying a positive potential sweep, which causes ano
22、dic oxidation of the analyte metal speciesto dissolved ion. The current associated with this reoxidation is measured. The peak current is proportional to the originalconcentration of dissolved analyte species over a wide range of concentrations.3.3 colorimetryan analytical technique that is similar
23、to spectrophotometry (see in which 3.5), except that ultraviolet-visiblelight of a single, narrow wavelength range is passed through a sample cell containing dissolved analyte, and the absorptionmeasured.3.4 reflectancea measurement technique (subset of spectrophotometry; see 3.5) in which light is
24、reflected off of a reflectingsurface and measured by a detector. The amount of reflected light may be a function of analyte concentration.surface containingthe analyte of interest is measured by a detector.3.5 spectrophotometryan analytical technique in which a spectrum of analyte species a sample c
25、ontaining the analyte ofinterest is obtained and used to determine the analyte concentration in the following manner. Light is directed onto or throughanalyte species, and the absorption of this light across a range of wavelengths is measured by a detector. The amount of absorbedlight is a function
26、of the concentration of analyte species.concentration.3.5.1 DiscussionLight is directed onto or through analyte species, and the absorption of this light across a range of wavelengths is measured bya detector. The amount of absorbed light is a function of the concentration of analyte species.4. Sign
27、ificance and Use4.1 This guide is intended for use in evaluating the performance of field-portable electroanalytical or spectrophotometricdevices for lead determination, or both.4.2 Desired performance criteria for field-based extraction procedures are provided.4.3 Performance parameters of concern
28、may be determined using protocols that are referenced in this guide.4.4 Example reference materials to be used in assessing the performance of field-portable lead analyzers are listed.4.5 Exhaustive details regarding quality assurance issues are outside the scope of this guide. Applicable quality as
29、suranceaspects are dealt with extensively in references that are cited in this guide.4 Available from United States Environmental Protection Agency (EPA), William Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.5 Available from International Organization f
30、or Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,Switzerland, http:/www.iso.org.E1775 1625. Performance Evaluation Materials5.1 Certified Reference Materials (CRMs)These may consist of NIST Standard Reference Materials (SRMs) and are al
31、soknown as Primary and Secondary Reference Materials:Reference material accompanied by a certificate, one ore more of whoseproperty values are certified by a procedure which establishes its traceability to an accurate realization of the unit in which theproperty values are expressed: each certified
32、value is accomplished by an uncertainty at a stated level of confidence (ISO Guide30).5.1.1 PaintExamples are NIST paint SRMs, for example, NIST SRMs 2582, 2583, and numerous other CRMs.NOTE 1These may consist of NIST Standard Reference Materials (SRMs) and are also known as Primary and Secondary Re
33、ference Materials:(1) PaintExamples are NIST paint SRMs, for example, NIST SRMs 2582, 2583, and numerous other CRMs.(2) DustExamples are NIST 1648a (urban particulate matter), other NIST dust SRMs, and other CRMs.(3) SoilExamples are NIST 8704 (river sediment) and NIST soil standards: SRMs 2709a, 27
34、10a, and 2711a and numerousother CRMs.(4) Airborne Particulate MatterAn example is NIST SRM 2783, which is available for airborne particulate matter collectedon filters. Other CRMs are also available.5.1.2 DustExamples are NIST 1648 (urban particulate matter), other NIST dust SRMs, and other CRMs.5.
35、1.3 SoilExamples are NIST2704 (river sediment) and NISTsoil standards: SRMs 2709, 2710, and 2711 and numerous otherCRMs.5.1.4 Airborne Particulate MatterAn example is NIST SRM 2783, which is available for airborne particulate matter collectedon filters. Other CRMs are also available.5.2 Real-World M
36、aterials:5.2.1 Paint, collected using Practice E1729 (or equivalent). To obtain reference values, determine lead concentration using TestMethodMethods D7439 and E1613 and Practice E1645 (or equivalent).5.2.2 Dust Wipes, collected using Practice D6966, with wipes meeting the requirements of Specifica
37、tion E1792. To obtainreference values, determine lead concentration using Test MethodMethods D7439 and E1613 and Practice E1644 (or equivalent).5.2.3 Vacuumed Dust, collected using Practices D7144 or D5438. To obtain reference values, determine lead concentrationusing Test MethodMethods D7439 and E1
38、613 and Practice E1726 (or equivalent).5.2.4 Soil, collected using Practice E1727. To obtain reference values, determine lead concentration using Test MethodMethodsD7439 and E1613 and Practice E1726 (or equivalent).5.2.5 Airborne Particulate Matter, collected using Test Method D6785 (or equivalent).
39、 To obtain reference values, determinelead concentration using Test MethodMethods D7439 and E1613 and either Test Methods D6785 or D7035 (or equivalent).5.3 Secondary Reference MaterialsExamples of these CRMs include samples from the Environmental Lead ProficiencyAnalytical Testing (ELPAT) program (
40、paints, dusts spiked on wipes, and soils) and the Proficiency Analytical Testing (PAT)program (air filters).6 Other examples include secondary reference materials (for example, bag house dust, sludge, and solidwaste).75.3.1 PaintExamples include ELPAT paint samples.5.3.2 DustExamples include ELPAT w
41、ipe samples spiked with 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 procedure chosen shall have a demonstrated recovery of at least 80 % for the matrixof co
42、ncern, and shall be compatible with the lead analysis technique used (EPA 600/R-93/200). (Reference extraction andanalytical techniques include those ASTM standards listed in 2.1.)6.2 Field-Portable Analysis:6.2.1 AccuracyOverall measurement accuracy of the field-portable analytical technique follow
43、ing field-based extraction:within 25 % of the values obtained by the applicable ASTM extraction procedure (see 2.1) and Test Method E1613.6.2.2 PrecisionFor field-based extraction followed by field-portable analysis, total uncertainties for standard referencematerials: 25 % relative standard deviati
44、on (RSD) (EPA747-R-92-001); for real-world materials: 25 % RSD (EPA747-R-92-001);for secondary reference materials: 25 % RSD.6.2.3 Working RangeMinimum working concentration range for the overall method shall extend from 0.1 times the applicableaction level to 2 times the applicable action level (NI
45、OSH SOP 018)8 for the sample matrix of concern.6 Available from American Industrial Hygiene Association (AIHA), Proficiency Analytical Testing Programs, LLC (AIHA-PATP), 3141 Fairview Park Drive, Suite 777,Falls Church, VA 22042, http:/www.aiha.org.7 Available from Fisher Scientific and Resource Tec
46、hnology Corp., Laramie, WY.8 The National Institute for Occupational Safety and Health (NIOSH), “Guidelines for Air Sampling and Analysis,” available from NIOSH Publications, 4676 ColumbiaParkway,1150 Tusculum Ave., Cincinnati, OH 45226, www.cdc.gov/niosh.Mail Stop C14, http:/www.cdc.gov/niosh.E1775
47、 1636.3 Sample SizeFollow applicable ASTM sample collection and sample preparation practices listed in 2.1.E1775 164NOTE 2Performance data from interlaboratory testing of a portable anodic stripping voltammetric procedure have been published.97. Quality Assurance (QA) and Quality Control (QC)7.1 Fie
48、ld and Laboratory QA/QCFollow QA/QC procedures delineated in the applicableASTM sample preparation practicesfor the pertinent sample matrix (2.1) and in Test Method E1613.7.2 QA SystemFollow the requirements delineated in Practice E1864.NOTE 3Participation in proficiency testing programs, for exampl
49、e, 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 mentionedin 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 respo
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