ASTM E1613-2004 Standard Test Method for Determination of Lead by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) Flame Atomic Absorption Spectrometry (FAAS) or GG.pdf

1、Designation: E 1613 04Standard Test Method forDetermination of Lead by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES), Flame AtomicAbsorption Spectrometry (FAAS), or Graphite FurnaceAtomic Absorption Spectrometry (GFAAS) Techniques1This standard is issued under the fixed designatio

2、n E 1613; the number immediately following the designation indicates 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 (e) indicates an editorial change since the last revision or r

3、eapproval.1. Scope1.1 This test method is intended for use with extracted ordigested samples that were collected during the assessment,management, or abatement of lead hazards from buildings,structures, or other locations.1.2 This test method covers the lead analysis of sampleextracts or digestates

4、(for example, extracted or digested paint,soil, dust, and airborne particulate) using inductively coupledplasma atomic emission spectrometry (ICP-AES), flameatomic absorption spectrometry (FAAS), or graphite furnaceatomic absorption spectrometry (GFAAS).1.3 This test method contains directions for s

5、ample analysis,as well as quality assurance (QA) and quality control (QC), andmay be used for purposes of laboratory accreditation andcertification.1.4 No detailed operating instructions are provided becauseof differences among various makes and models of suitableinstruments. Instead, the analyst sh

6、all follow the instructionsprovided by the manufacturer of the particular instrument.1.5 The values stated in SI units are to be regarded as thestandard.1.6 This practice contains notes which are explanatory andnot part of the mandatory requirements of this standard.1.7 This standard does not purpor

7、t 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 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 119

8、3 Specification for Reagent WaterD 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption SpectrophotometryD 4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level DataD 4697 Guide for Maintaining Test Methods in the Us

9、ersLaboratoryD 4840 Guide for Sampling Chain of Custody ProceduresD 6785 Test Method for Determination of Lead in Work-place AirE 456 Terminology Relating to Quality and StatisticsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 1188 Practice for Col

10、lection and Preservation of Informa-tion and Physical Items by a Technical InvestigatorE 1605 Terminology Relating to Abatement of Hazardsfrom Lead-Based Paint in Buildings and Related StructuresE 1644 Practice for Hot Plate Digestion of Dust WipeSamples for Subsequent Determination of Lead by Atomi

11、cSpectrometryE 1645 Practice for Preparation of Dried Paint Samples forSubsequent Lead Analysis by Atomic SpectrometryE 1726 Practice for Sample Digestion of Soils for theDetermination of Lead by Atomic SpectrometryE 1727 Practice for Field Collection of Soil Samples forLead Determination by Atomic

12、Spectrometry TechniquesE 1728 Practice for Field Collection of Settled DustSamples Using Wipe Sampling Methods for Lead Deter-mination by Atomic Spectrometry TechniquesE 1729 Practice for Field Collection of Dried Paint Samplesfor Determination by Atomic Spectrometry TechniquesE 1741 Practice for Pr

13、eparation of Airborne ParticulateLead Samples Collected During Abatement and Construc-tion Activities for Subsequent Analysis by Atomic Spec-trometryE 1775 Guide for Evaluating Performance of On-Site Ex-traction and Field-Portable Electrochemical or Spectropho-tometric Analysis for LeadE 1792 Specif

14、ication for Wipe Sampling Materials for Leadin Surface Dust1This test method is under the jurisdiction of ASTM Committee E06 onPerformance of Buildings and is the direct responsibility of Subcommittee E06.23on Lead Hazards Associated with Buildings.Current edition approved August 1, 2004. Published

15、August 2004. Originallyapproved in 1994. Last previous edition approved in 1999 as E 1613 99.2For 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 Document

16、Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E 1864 Practice for Evaluating Quality Systems of Organi-zations Engaged in Conducting Facility and Hazard As-sessments to Determine the Presence and Ext

17、ent of Lead inPaint, Dust,Airborne Particulate, and Soil in Buildings andRelated StructuresE 1973 Practice for Collection of Surface Dust by AirSampling Pump Vacuum Technique for Subsequent LeadDeterminationE 1979 Practice for Ultrasonic Extraction of Paint, Dust,Soil, orAir Samples for Subsequent D

18、etermination of LeadE 2239 Practice for Record Keeping and Record Preserva-tion for Lead Hazard Activities3. Terminology3.1 Definitions: For definitions of terms not appearing here,see Terminology E 1605.3.2 Definitions of Terms Specific to This Standard:3.2.1 analysis runa period of measurement tim

19、e on agiven analytical instrument during which data are calculatedfrom a single calibration curve (or single set of curves).3.2.1.1 DiscussionRecalibration of a given instrumentproduces a new analysis run.3.2.2 calibration standardssolutions of known analyteconcentrations used to calibrate instrumen

20、ts.3.2.2.1 DiscussionCalibration standards must be matrixmatched to the acid content present in sample digestates orextracts and must be measured prior to analyzing samples.3.2.3 continuing calibration blank (CCB)a solution con-taining no analyte that is used to verify blank response andfreedom from

21、 carryover.3.2.3.1 DiscussionThe CCB must be analyzed after theCCV (see 3.2.4) and after the ICkS (see 3.2.9). The measuredvalue is to be (at most) less than five times the instrumentaldetection limit (IDL) (see 3.2.7).3.2.4 continuing calibration verification (CCV)a solution(or set of solutions) of

22、 known analyte concentration used toverify freedom from excessive instrumental drift; the concen-tration is to be near the mid-range of a linear calibration curve.3.2.4.1 DiscussionThe CCV must be matrix matched tothe acid content present in sample digestates or extracts. TheCCV must be analyzed bef

23、ore and after all samples and at afrequency of not less than every ten samples. The measuredvalue is to fall within 610 % (620 % for GFAA) of the knownvalue.3.2.5 initial calibration blank (ICB)a standard containingno analyte that is used for the initial calibration and zeroing ofthe instrument resp

24、onse.3.2.5.1 DiscussionThe ICB must be matrix matched tothe acid content of sample extracts and digestates. The ICBmust be measured during and after calibration. The measuredvalue is to be (at most) less than five times the IDL (see 3.2.7).3.2.6 initial calibration verification (ICV)a solution (orse

25、t of solutions) of known analyte concentration used to verifycalibration standard levels; the concentration of analyte is to benear the mid-range of the linear curve that is made from a stocksolution having a different manufacturer or manufacturer lotidentification than the calibration standards.3.2

26、.6.1 DiscussionThe ICV must be matrix matched tothe acid content of sample extracts or digestates. The ICV mustbe measured after calibration and before measuring any sampledigestates or extracts. The measured value is to fall within610 % of the known value.3.2.7 instrumental detection limit (IDL)the

27、 lowest con-centration at which the instrumentation can distinguish analytecontent from the background generated by a minimal matrix.3.2.7.1 DiscussionThe IDL is usually determined by themanufacturer. The IDL can be determined from blank, acidi-fied, deionized, or ultrapure water as the matrix and f

28、rom thesame calculation methods used to determine a method detec-tion limit (MDL) (see 3.2.12). Typical lead (Pb) IDLs forFAAS, ICP-AES, and GFAAS are 0.05, 0.03, and 0.002g/mL, respectively.3.2.8 instrumental QC standardsthese provide informa-tion on measurement performance during the instrumentala

29、nalysis portion of the overall analyte measurement process.They include CCBs, CCVs, ICBs, ICVs, and ICkSs.3.2.9 interference check standard (ICkS)a solution (or setof solutions) of known analyte concentrations used for ICP-AES to verify an accurate analyte response in the presence ofpossible spectra

30、l interferences from other analytes that may bepresent in samples; the concentration of analyte is to be lessthan 25 % of the highest calibration standard, and concentra-tions of the interferences will be 200 g/mL of aluminum,calcium, iron, and magnesium.3.2.9.1 DiscussionThe ICkS must be matrix mat

31、ched tothe acid content of sample digestates or extracts. The ICkSmust be analyzed at least twice, once before and once after theanalysis of all sample extracts or digestates. The measuredanalyte value is expected to be within 620 % of the knownvalue.3.2.10 method blanka digestate or extract that re

32、flects themaximum treatment given any one sample within a samplebatch, except that no sample is placed into the digestion orextraction vessel. (The same reagents and processing condi-tions that are applied to field samples within a batch are alsoapplied to the method blank.)3.2.10.1 DiscussionAnalys

33、is results from method blanksprovide information on the level of potential contaminationexperienced by samples processed within the batch.3.2.11 limit of detection (LOD)the MDL (see 3.2.12)orthe IDL (see 3.2.7), depending on the context.3.2.12 method detection limit (MDL)the minimum con-centration o

34、f analyte that, in a given matrix and with a specifiedanalytical method, has a 99 % probability of being identifiedand is reported to be greater than zero concentration.3.2.12.1 Discussion:(a) As an example, the MDL for lead in paint is the smallestmeasurable (that is, nonzero) concentration of lead

35、 within thepaint sample as determined by the validated extraction andanalysis method used. Note that there would be a differentMDL for different sample matrices (such as dust wipes, airfilters, and soils), even if the sample preparation and analysisprocess is the same for all types of matrices. Thus

36、 each samplematrix has a unique MDL, given in units specific to the matrix,even if the analyte content is the same for each.NOTE 1For instance, for dust wipe samples, different brands of wipescould have different MDLs. Dust wipes and paint samples would haveE1613042lead contents expressed in differe

37、nt units.(b) There are thus four component inputs to defining anMDL: (1) the analyte of interest (that is, lead (Pb) for ourpurposes here); (2) the sample matrix (for example: paint, dustor brand x wipe, soil, or air particulate collected on type xfilter); (3) the extraction/digestion procedure used

38、; and (4) theanalysis procedure (includes the type of instrument) used forquantification of analyte content. The MDL must be estab-lished prior to reporting analysis data.3.2.13 quantitative analysisan analysis run on sampledigestates or extracts (or serial dilutions thereof) that includesinstrument

39、al QC standards.3.2.13.1 DiscussionData from this analysis run are usedto calculate and report final lead analysis results.3.2.14 quantitation limitan instrumental measurementvalue that is used to provide a lower concentration limit forreporting quantitative analysis data for a given analyticalmetho

40、d.3.2.14.1 DiscussionAny sample that generates a leadmeasurement below the quantitation limit is reported as aless-than value using the quantitation limit value multiplied bythe appropriate dilution factors resulting from preparation ofthe sample for instrumental analysis.3.2.15 semiquantitative ana

41、lysisan analysis run that isperformed on highly diluted sample digestates or extracts forthe purpose of determining the approximate analyte level in thedigest.3.2.15.1 DiscussionThis analysis run is generally per-formed without inserting instrumental QC standards except forcalibration standards. Dat

42、a from this run are used for deter-mining serial dilution requirements for sample digestates orextracts to keep them within the linear range of the instrument.3.2.16 serial dilutiona method of producing a less-concentrated solution through one or more consecutive dilutionsteps.3.2.16.1 DiscussionA d

43、ilution step for a standard orsample solution is performed by volumetrically placing a smallaliquot (of known volume) of a higher concentrated solutioninto a volumetric flask and diluting to volume with watercontaining the same acid levels as those found in originalsample digestates or extracts.3.2.

44、17 spiked samplea sample portion (split from anoriginal sample) that is spiked with a known amount of analyte.3.2.17.1 DiscussionAnalysis results for spiked samplesare used to provide information on the precision and bias of theoverall analysis process.3.2.18 spiked duplicate sampleTwo portions of a

45、 homog-enized sample that were targeted for addition of analyte andfortified with all the target analytes before preparation.3.2.18.1 DiscussionAnalysis results for these samples areused to provide information on the precision and bias of theoverall analysis process.3.2.19 un-spiked samplea portion

46、of a homogenizedsample that was targeted for the addition of analyte but is notfortified with target analytes before sample preparation.3.2.19.1 DiscussionAnalysis results for this sample areused to correct for native analyte levels in the spiked andspiked duplicate samples.4. Summary of Test Method

47、4.1 A sample digestate or extract is analyzed for leadcontent using ICP-AES, FAAS, or GFAAS techniques (4, 1,2)3. Instrumental QC samples are analyzed along with sampledigestates or extracts in order to ensure adequate instrumentalperformance.NOTE 2Digestion is an example of an extraction process. O

48、therexamples of extraction processes are ultrasonic extraction (3) and leach-ing.5. Significance and Use5.1 This test method is intended for use with other standards(see 2.1) that address the collection and preparation of samples(dried chips, dusts, soils, and air particulates) that are obtainedduri

49、ng the assessment or mitigation of lead hazards frombuildings and related structures.5.2 This test method may also be used to analyze similarsamples from other environments.6. Interferences6.1 Interferences for FAAS, GFAAS, and ICP-AES can bemanufacturer and model specific. The following are generalguidelines:6.1.1 Special interferences may be encountered in ICP-AESanalysis (5). These interferences can be minimized by properwavelength selection, interelement correction factors, andbackground correction (6).6.1.2 Molecular absorption is a potenti