ASTM E1613-2012 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:E161304 Designation: E1613 12Standard 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 t

2、he fixed designation E1613; 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 () indicates an editorial change since the l

3、ast revision or reapproval.1. Scope1.1 This test method is intended for use with extracted or digested 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 sample ext

4、racts or digestates (for example, extracted or digested paint, soil, dust,and airborne particulate) using inductively coupled plasma atomic emission spectrometry (ICP-AES), flame atomic absorptionspectrometry (FAAS), or graphite furnace atomic absorption spectrometry (GFAAS).1.3 This test method con

5、tains directions for sample analysis, as well as quality assurance (QA) and quality control (QC), andmay be used for purposes of laboratory accreditation and certification.1.4 No detailed operating instructions are provided because of differences among various makes and models of suitableinstruments

6、 Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument.1.5The values stated in SI units are to be regarded as the standard.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this stan

7、dard.1.6 This practice contains notes which are explanatory and not part of the mandatory requirements of this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropr

8、iate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption SpectrophotometryD4210 Pra

9、ctice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level DataD4697 Guide for Maintaining Test Methods in the Users LaboratoryD4840 Guide for Sample Chain-of-Custody ProceduresD6785 Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furn

10、ace Atomic AbsorptionSpectrometryD7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationE456 Terminology Relating to Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE1188 Practic

11、e for Collection and Preservation of Information and Physical Items by a Technical InvestigatorE1605 Terminology Relating to Lead in BuildingsE1644 Practice for Hot Plate Digestion of Dust Wipe Samples for the Determination of LeadE1645 Practice for Preparation of Dried Paint Samples by Hotplate or

12、Microwave Digestion for Subsequent Lead AnalysisE1726 Practice for Preparation of Soil Samples by Hotplate Digestion for Subsequent Lead AnalysisE1727 Practice for Field Collection of Soil Samples for Subsequent Lead DeterminationE1728 Practice for Collection of Settled Dust Samples Using Wipe Sampl

13、ing Methods for Subsequent Lead Determination1This test method is under the jurisdiction ofASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead HazardsAssociated with Buildings.Current edition approved August 1, 2004.July 15, 2012. Published

14、August 2004.2012. Originally approved in 1994. Last previous edition approved in 19992004 asE161399.E1613 04. DOI: 10.1520/E1613-04.10.1520/E1613-12.2For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standar

15、dsvolume information, refer to the standards Document Summary page on the ASTM website.1This 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 be technically possible t

16、o 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 Drive, PO Box C700, West Con

17、shohocken, PA 19428-2959, United States.E1729 Practice for Field Collection of Dried Paint Samples for Subsequent Lead DeterminationE1741 Practice for Preparation of Airborne Particulate Lead Samples Collected During Abatement and Construction Activitiesfor Subsequent Analysis by Atomic Spectrometry

18、E1775 Guide for Evaluating Performance of On-Site Extraction and Field-Portable Electrochemical or SpectrophotometricAnalysis for LeadE1792 Specification for Wipe Sampling Materials for Lead in Surface DustE1864 Practice for Evaluating Quality Systems of Organizations Conducting Facility and Hazard

19、Assessments for Lead inPaint, Dust, Airborne Particulate, and Soil in and around Buildings and Related Structures E1973Practice for Collection ofSurface Dust by Air SamplingPump Vacuum Technique forSubsequent Lead Determina-tionE1979 Practice for Ultrasonic Extraction of Paint, Dust, Soil, and Air S

20、amples for Subsequent Determination of LeadE2239 Practice for Record Keeping and Record Preservation for Lead Hazard Activities3. Terminology3.1 Definitions: For definitions of terms not appearing here, see Terminology E1605.3.2 Definitions of Terms Specific to This Standard:3.2.1 analysis runa peri

21、od of measurement time on a given analytical instrument during which data are calculated from asingle calibration curve (or single set of curves).3.2.1.1 DiscussionRecalibration of a given instrument produces a new analysis run.3.2.2 calibration standardssolutions of known analyte concentrations use

22、d to calibrate instruments.3.2.2.1 DiscussionCalibration standards must be matrix matched to the acid content present in sample digestates or extractsand must be measured prior to analyzing samples.3.2.3 continuing calibration blank (CCB)a solution containing no analyte that is used to verify blank

23、response and freedomfrom carryover.3.2.3.1 DiscussionThe CCB must be analyzed after the CCV (see 3.2.4) and after the ICkS (see 3.2.9). The measured valueis to be (at most) less than five times the instrumental detection limit (IDL) (see 3.2.7).3.2.4 continuing calibration verification (CCV)a soluti

24、on (or set of solutions) of known analyte concentration used to verifyfreedom from excessive instrumental drift; the concentration is to be near the mid-range of a linear calibration curve.3.2.4.1 DiscussionThe CCV must be matrix matched to the acid content present in sample digestates or extracts.

25、The CCVmust be analyzed before and after all samples and at a frequency of not less than every ten samples. The measured value is to fallwithin 610 % (620 % for GFAA) of the known value.3.2.5 initial calibration blank (ICB)a standard containing no analyte that is used for the initial calibration and

26、 zeroing of theinstrument response.3.2.5.1 DiscussionThe ICB must be matrix matched to the acid content of sample extracts and digestates. The ICB must bemeasured during and after calibration. The measured value is to be (at most) less than five times the IDL (see 3.2.7).3.2.6 initial calibration ve

27、rification (ICV)a solution (or set of solutions) of known analyte concentration used to verifycalibration standard levels; the concentration of analyte is to be near the mid-range of the linear curve that is made from a stocksolution having a different manufacturer or manufacturer lot identification

28、 than the calibration standards.3.2.6.1 DiscussionThe ICV must be matrix matched to the acid content of sample extracts or digestates. The ICV must bemeasured after calibration and before measuring any sample digestates or extracts. The measured value is to fall within 610 %of the known value.3.2.7

29、instrumental detection limit (IDL)the lowest concentration at which the instrumentation can distinguish analyte contentfrom the background generated by a minimal matrix.3.2.7.1 DiscussionThe IDL is usually determined by the manufacturer. The IDL can be determined from blank, acidified,deionized, or

30、ultrapure water as the matrix and from the same calculation methods used to determine a method detection limit(MDL) (see 3.2.12). Typical lead (Pb) IDLs for FAAS, ICP-AES, and GFAAS are 0.05, 0.03, and 0.002 g/mL, respectively.3.2.8 instrumental QC standardsthese provide information on measurement p

31、erformance during the instrumental analysisportion of the overall analyte measurement process. They include CCBs, CCVs, ICBs, ICVs, and ICkSs.3.2.9 interference check standard (ICkS)a solution (or set of solutions) of known analyte concentrations used for ICP-AESto verify an accurate analyte respons

32、e in the presence of possible spectral interferences from other analytes that may be presentin samples; the concentration of analyte is to be less than 25 % of the highest calibration standard, and concentrations of theinterferences will be 200 g/mL of aluminum, calcium, iron, and magnesium.3.2.9.1

33、DiscussionThe ICkS must be matrix matched to the acid content of sample digestates or extracts. The ICkS must beanalyzed at least twice, once before and once after the analysis of all sample extracts or digestates. The measured analyte valueis expected to be within 620 % of the known value.3.2.10 me

34、thod blanka digestate or extract that reflects the maximum treatment given any one sample within a sample batch,except that no sample is placed into the digestion or extraction vessel. (The same reagents and processing conditions that areE1613 122applied to field samples within a batch are also appl

35、ied to the method blank.)3.2.10.1 DiscussionAnalysis results from method blanks provide 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) or the IDL (see 3.2.7), depending on the context.3.2.12 met

36、hod detection limit (MDL)the minimum concentration of analyte that, in a given matrix and with a specifiedanalytical method, has a 99 % probability of being identified and 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 smalle

37、st measurable (that is, nonzero) concentration of lead within the paintsample as determined by the validated extraction and analysis method used. Note that there would be a different MDL for differentsample matrices (such as dust wipes, air filters, and soils), even if the sample preparation and ana

38、lysis process is the same for alltypes of matrices. Thus each sample matrix has a unique MDL, given in units specific to the matrix, even if the analyte contentis the same for each.NOTE 1For instance, for dust wipe samples, different brands of wipes could have different MDLs. Dust wipes and paint sa

39、mples would have leadcontents expressed in different units.(b) There are thus four component inputs to defining an MDL: (1) the analyte of interest (that is, lead (Pb) for our purposes here);(2) the sample matrix (for example: paint, dust or brand x wipe, soil, or air particulate collected on type x

40、 filter); (3) theextraction/digestion procedure used; and (4) the analysis procedure (includes the type of instrument) used for quantification ofanalyte content. The MDL must be established prior to reporting analysis data.3.2.13 quantitative analysisan analysis run on sample digestates or extracts

41、or serial dilutions thereof) that includesinstrumental QC standards.3.2.13.1 DiscussionData from this analysis run are used to calculate and report final lead analysis results.3.2.14 quantitation limitan instrumental measurement value that is used to provide a lower concentration limit for reportin

42、gquantitative analysis data for a given analytical method.3.2.14.1 DiscussionAny sample that generates a lead measurement below the quantitation limit is reported as a less-than valueusing the quantitation limit value multiplied by the appropriate dilution factors resulting from preparation of the s

43、ample forinstrumental analysis.3.2.15 semiquantitative analysisan analysis run that is performed on highly diluted sample digestates or extracts for thepurpose of determining the approximate analyte level in the digest.3.2.15.1 DiscussionThis analysis run is generally performed without inserting ins

44、trumental QC standards except forcalibration standards. Data from this run are used for determining serial dilution requirements for sample digestates or extracts tokeep them within the linear range of the instrument.3.2.16 serial dilutiona method of producing a less-concentrated solution through on

45、e or more consecutive dilution steps.3.2.16.1 DiscussionA dilution step for a standard or sample solution is performed by volumetrically placing a small aliquot(of known volume) of a higher concentrated solution into a volumetric flask and diluting to volume with water containing the sameacid levels

46、 as those found in original sample digestates or extracts.3.2.17 spiked samplea sample portion (split from an original sample) that is spiked with a known amount of analyte.3.2.17.1 DiscussionAnalysis results for spiked samples are used to provide information on the precision and bias of theoverall

47、analysis process.3.2.18 spiked duplicate sampleTwo portions of a homogenized sample that were targeted for addition of analyte and fortifiedwith all the target analytes before preparation.3.2.18.1 DiscussionAnalysis results for these samples are used to provide information on the precision and bias

48、of the overallanalysis process.3.2.19 un-spiked samplea portion of a homogenized sample that was targeted for the addition of analyte but is not fortifiedwith target analytes before sample preparation.3.2.19.1 DiscussionAnalysis results for this sample are used to correct for native analyte levels i

49、n the spiked and spikedduplicate samples.4. Summary of Test Method4.1 A sample digestate or extract is analyzed for lead content using ICP-AES, FAAS, or GFAAS techniques (4, 1, 2).3.Instrumental QC samples are analyzed along with sample digestates or extracts in order to ensure adequate instrumentalperformance.NOTE 2Digestion is an example of an extraction process. Other examples of extraction processes are ultrasonic extraction (3) and leaching.5. Significance and Use5.1 This test method is intended for use with other standards (see 2.1) th