1、Designation: E2913 14E2913/E2913M 19Standard Practice forHotplate Digestion of Lead from Composited Wipe Samples1This standard is issued under the fixed designation E2913;E2913/E2913M; the number immediately following the designation indicatesthe year of original adoption or, in the case of revision
2、, the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice is similar to Practice E1644 and covers the hot, nitric acid digestion of lead (Pb) from a
3、 composited sampleof up to four individual wipe samples of settled dust collected from equally-sized areas in the same space.1.2 This practice contains notes which are explanatory and not part of mandatory requirements of the practice.1.3 This practice should be used by analysts experienced in diges
4、tion techniques such as hot blocks. Like all procedures usedin an analytical laboratory, this practice needs to be validated for use and shown to produce acceptable results before being appliedto client samples.1.4 The values stated in either SI units or inch-pound units are to be regarded as standa
5、rd. No other units of measurement areincluded in this separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shallbe used independently of the other. Combining values from the two systems may result in non-conformance with the standard.1.4.1 Exc
6、eptionInch-pound units are provided in Note 7 and Note 9 for information.1.5 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 appropriate safety safety, health, and healthenvironme
7、ntal practices and determine theapplicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guid
8、es and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD6966 Practice for Collection of Settled Dust Samples Using Wipe Sampling Method
9、s for Subsequent Determination of MetalsE631 Terminology of Building ConstructionsE1605 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 Fur
10、naceAtomicAbsorption Spectrometry (GFAAS) TechniquesE1644 Practice for Hot Plate Digestion of Dust Wipe Samples for the Determination of LeadE1728 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Lead DeterminationE1792 Specification for Wipe Sampling Materi
11、als for Lead in Surface DustE2051 Practice for the Determination of Lead in Paint, Settled Dust, Soil and Air Particulate by Field-Portable Electroanalysis(Withdrawn 2010)3E2239 Practice for Record Keeping and Record Preservation for Lead Hazard ActivitiesE2271/E2271M Practice for Clearance Examinat
12、ions Following Lead Hazard Reduction Activities in Multifamily DwellingsE3074/E3074M Practice for Clearance Examinations Following Lead Hazard Reduction Activities in Single Family Dwellings,in Individual Units of Multifamily Dwellings, and in Other Child-Occupied Facilities1 This practice is under
13、the jurisdiction of ASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead HazardsAssociated with Buildings.Current edition approved May 1, 2014Jan. 1, 2019. Published June 2014February 2019. Originally approved in 2014. Last previous edition a
14、pproved in 2014 as E291314.DOI: 10.1520/E2913-1410.1520/E2913_E2913M19.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page o
15、n the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This 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 techn
16、ically possible to 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 B
17、ox C700, West Conshohocken, PA 19428-2959. United States12.2 ISO Standards:4ISO 1042 Laboratory Glassware One-mark Volumetric FlasksISO 3585 Borosilicate Glass 3.3 Properties Third EditionISO/IEC 17025:200517025:2017 General Requirements for the Competence of Testing and Calibration LaboratoriesISO
18、3585 Borosilicate Glass 3.3 Properties Third Edition2.3 Other Document:540 CFR Part 745 Lead-Based Paint Poisoning Prevention in Certain Residential Structures3. Terminology3.1 For definitions of terms not appearing here, refer to Terminology D1129, Specification D1193, and TerminologyTermi-nologies
19、 E631 and E1605.3.2 Definitions of Terms Specific to This Standard:3.2.1 composited samplesample, nthe single sample resulting from the combination of individual samples collected fromdifferent sections of the same area.3.2.2 validationvalidation, nthe confirmation by examination and the provision o
20、f objective evidence that the particularrequirements for a specific intended use are fulfilled ISO 17025:2005 (5.4.5.1).a given item fulfills specified requirements, wherethe specified requirements are adequate for an intended use. ISO 17025:20174 Available from International Organization for Standa
21、rdization (ISO), 1, ch. de la Voie-Creuse, CP 56, CH-1211 Geneva 20,ISO Central Secretariat, BIBC II, Chemin deBlandonnet 8, CP 401, 1214 Vernier, Geneva, Switzerland, http:/www.iso.org.5 Available from U.S. Government Printing Office Superintendent of Documents, Publishing Office (GPO), 732 N. Capi
22、tol St., NW, Mail Stop: SDE, Washington, DC20401, http:/www.access.gpo.gov.http:/www.gpo.gov.E2913/E2913M 1923.2.3 The laboratory is responsible for validating (1-4,),6, non-standard methods, laboratory-designed/developed methods,standard methods used outside their intended scope, and amplifications
23、 and modifications of standard methods to confirm that themethods are fit for the intended use. The validation shall be as extensive as is necessary to meet the needs of the given applicationor field of application. The laboratory shall record the results obtained, the procedure used for the validat
24、ion, and a statement asto whether the method is fit for the intended use.NOTE 1It is the responsibility of the laboratory to carry out its testing activities in such a way as to satisfy the needs of the client, the regulatoryauthorities, and organizations providing recognition.4. Summary of Practice
25、4.1 Up to four wipes, meeting the requirements of Specification E1792, are used according to PracticePractices D6966 or E1728to collect settled dust from equally-sized areas in the same space and composited as one sample. sample as in PracticesE2271/E2271M and E3074/E3074M. This composited sample is
26、 then digested using heat and nitric acid. The resulting extractsolution is analyzed according to Test Method E1613 or Practice E2051.5. Significance and Use5.1 This practice is for use in the preparation of no more than four wipe samples combined to form a composited sample forsubsequent determinat
27、ion of lead content.5.2 This practice assumes use of wipes that meet Specification E1792 and should not be used unless the wipes meetSpecification E1792.5.3 This practice is capable of preparing samples for determination of lead bound within paint dust.5.4 This practice may not be capable of prepari
28、ng samples for determination of lead bound within silica or silicate matrices,or within matrices not soluble in nitric acid.5.5 Adjustment of the nitric acid concentration or acid strength, or both, of the final extract solution may be necessary forcompatibility with the instrumental analysis method
29、 to be used for lead quantification.5.6 This sample preparation practice has not been validated for use and must be validated by the user prior to using the practicefor client samples.NOTE 2Each combination of wipes (two wipes, three wipes, and four wipes) constitutes a different matrix and must be
30、separately validated.6. Apparatus and Materials6.1 Borosilicate Glassware:6.1.1 Volumetric Flasks, 400 mL, borosilicate, with Stoppers, conforming to ISO 1042 and ISO 3585,6.1.2 Griffn Beakers, 250 mL,6.1.3 Watch Glasses, sized to cover the Griffin Beakers,6.1.4 Graduated Cylinder, 100 mL, and,6.1.5
31、 Stirring Rods, sized to reach the bottom of the Griffin Beakers.6.2 Funnels, plastic, porcelain or borosilicate funnels sized to deliver filtrate into a 400 mL volumetric flask.6.3 Tweezers, non-metallic tweezers sized to remove wipes from sample shipping containers.6.4 Filter Paper, fast filtering
32、, suitable for metals analysis.6.5 Electric Hotplates, suitable for operation at temperatures that allow digestion of nitric acid and hydrogen peroxide solutionsencountered in this practice.6.6 Wash Bottles, of suitable size and material to contain 1:1 (v/v) nitric acid solution or reagent water.6.7
33、 Disposable Gloves, impermeable and powder free, to avoid the possibility of contamination, and to protect from contactwith toxic and corrosive substances.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents
34、shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where6 Kennedy, Ph.D., Eugene R., Fischbach, Thomas J., Song, Ph.D., Ruiguang, Eller, Ph.D., Peter M., and Schulman, Ph.D., Stanley A., Guidelines for Air Sampling andAnalytical Method Develo
35、pment, DHHS (NIOSH), Publication No. 95-117, 1995.7 Green, J. Mark, A Practical Guide to Analytical Method Validation, Analytical Chemistry, 1996, (68) 305A-309A.8 The Fitness for Purpose of Analytical Methods-A Laboratory Guide to Method Validation and Related Topics, EURACHEM Guide 1st Ed, 1998.6
36、Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis (IUPAC Technical Report) Pure Appl. Chem., Vol. 74, No. 5, pp. 835855, 2002.Theboldface numbers in parentheses refer to a list of references at the end of this standard.E2913/E2913M 193such specifications are available (5)
37、. Other grades may be used, provided that it can be demonstrated that they are of sufficientlyhigh purity to permit their use without decreasing the accuracy of the determinations.7.2 Reagent WaterASTM Type I water as given in Unless otherwise indicated, reference to water shall be understood to mea
38、nType II reagent water conforming to Specification D1193 with minimum resistance of 16.67 megaohm-cm, or equivalent7.3 Nitric Acid:7.3.1 Concentrated, of suitable purity for atomic spectrometric analysis, such as spectroscopic grade.NOTE 3Suitable purity means having undetectable lead content in the
39、 extracted composited sample blanks.7.3.2 Dilute 1:1 (v/v); prepared by carefully pouring a volume of concentrated acid into an equal volume of reagent water.7.4 Hydrogen Peroxide30 % (w/w), suitable for atomic spectrometric analysis, such as spectroscopic grade. See Note 3.8. Sample Preparation Pro
40、cedure8.1 Don a new pair of impermeable gloves. Treat each composited sample in a batch equally.8.2 Quantitatively transfer the contents of the dust-wipe sample containers to a labeled beaker as follows:8.2.1 Carefully open each container, remove wipes using a clean tweezers and a clean stirring rod
41、 as needed, and place all thewipes comprising the composited sample into a clean 250 mL 250 mL beaker.8.2.2 If the sample containers are hard-walled, rigid containers such as a plastic centrifuge tubes, using a minimum volume ofsolution, wash the inside of the sample shipping container, the tweezer
42、tips and the stirring rod with 1:1 (v/v) nitric acid into thebeaker containing the wipes.8.2.3 If the sample containers are flexible plastic bags and material appears to be left behind after wipe removal, attempt totransfer the residual material into the beaker by shaking or using mechanical removal
43、 with a clean laboratory spatula or similartool. Document observations of potential loss of sample due to any residue in the container for later reporting with the results ofthe lead analysis.8.3 Slowly add 60 mL of concentrated nitric acid to the beaker. Assuring that all wipes are immersed, gently
44、 swirl to mix, andcover with a clean watch glass. Digest on a hotplate to a solution volume of about 8 mL. Do not digest to dryness.(WarningSome wipes break down into a gelatinous residue that readily bumps or spatters, or both. Heating should be slowedwith these materials.)8.4 Remove from the hotpl
45、ate and allow to cool.8.5 When cool, carefully remove the watch glass and slowly add 40 mL of 30 % (w/w) hydrogen peroxide, assuring that allwipes are immersed.NOTE 4Exercise care Care should be exercised when removing the watch glass.Avoid lead Lead contamination problems may be avoided by placingi
46、t the watch glass upside down on new clean laboratory wipes.8.6 Cover the beaker with the watchglass watch glass and return the covered beaker to the hot plate. Take care to ensure thatlosses do not occur due to vigorous effervescence during heating. Heat until effervescence subsides and then digest
47、 to a solutionvolume of about 8 mL. Do not digest to dryness.8.7 Remove the digestate from the hotplate and allow to cool.8.8 Assemble funnels, filter paper and volumetric flasks as needed to allow filtering of digestates into 400 mLvolumetric flasks.NOTE 5Do not attempt to pour the undiluted digest
48、ate through The undiluted digestate is a strong acid solution and may dissolve the filter paper asthe filter paper will dissolve in strong acid solutions.if poured through it.8.9 When cool, use reagent water to wash the bottom of the watch glass, the inside walls of the beaker, and any remaining wip
49、ematerial to the bottom of the beaker. Use about 80 mL of reagent water to accomplish the washing. Pour the diluted digestatethrough the filter paper.8.10 Using reagent water and a clean glass stirring rod, break up and wash the mass of any remaining wipe material in thebottom of the beaker three times. Use enough reagent water each time to at least cover the remaining wipe material in the beaker.Use about 150 mL to accomplish the washing. Pour the first two washings through the filter paper, and use the third to wash anyremaining wipe material from
