1、Designation: E2914 14E2914/E2914M 19Standard Practice forUltrasonic Extraction of Lead from Composited WipeSamples1This standard is issued under the fixed designation E2914;E2914/E2914M; the number immediately following the designation indicatesthe year of original adoption or, in the case of revisi
2、on, 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 covers the extraction of lead (Pb) using ultrasonication, heat and nitric acid from a co
3、mposited sample of upto 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 digestio
4、n 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 standard.
5、 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 Except
6、ionInch-pound units are provided in Note 6 and Note 8 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 healthenvironmenta
7、l 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, Guides
8、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 Methods f
9、or 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 Furnac
10、eAtomicAbsorption Spectrometry (GFAAS) TechniquesE1728 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Lead DeterminationE1792 Specification for Wipe Sampling Materials for Lead in Surface DustE1979 Practice for Ultrasonic Extraction of Paint, Dust, Soil, a
11、nd Air Samples for Subsequent Determination of LeadE2051 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
12、 for Clearance Examinations Following Lead Hazard Reduction Activities in Multifamily Dwellings1 This practice is under 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
13、approved May 1, 2014Jan. 1, 2019. Published June 2014February 2019. Originally approved in 2014. Last previous edition approved in 2014 as E291414.DOI: 10.1520/E2914-1410.1520/E2914_E2914M19.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at servi
14、ceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on 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 u
15、ser 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 appropriate. In all cases only the current versionof the standard
16、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 States1E3074/E3074M Practice for Clearance Examinations Following Lead Hazard Reduction Activities in Single Family Dwellings,in I
17、ndividual Units of Multifamily Dwellings, and in Other Child-Occupied Facilities2.2 ISO Standards:4ISO 3585 Borosilicate Glass 3.3 Properties Third EditionISO/IEC 17025:200517025:2017 General Requirements for the Competence of Testing and Calibration LaboratoriesISO 3585 Borosilicate Glass 3.3 Prope
18、rties 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 Terminology E1605.3.2 Definitions of Terms Specific to This
19、 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 of objective evidence that the particularrequirements for
20、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 Standardization (ISO), 1, ch. de la Voie-Creuse, CP 56, CH-1211
21、 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, (GPO), 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401,http:/www.access.gpo.gov.
22、http:/www.gpo.gov.E2914/E2914M 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 and modifications of standard methods to confirm that themethods are fit f
23、or 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 validation, and a statement asto whether the method is fit for the intended use.NO
24、TE 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 Practice4.1 Up to four wipes, meeting the requirements of Specification E1792, are
25、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 then extracted using ultrasonication, heat and nitric acid. Theresulting e
26、xtract solution 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 collected from equally-sized areas in the samespace combined to form a composited sample for subsequent determination
27、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 preparing s
28、amples 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 to
29、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 sepa
30、rately validated.6. Apparatus and Materials6.1 Borosilicate Glass (conforming to ISO 3585) or Plastic Labware:6.1.1 Bottles, 125 mL, polypropylene or equivalent, with screw caps, or equivalent,6.1.2 Graduated Cylinders, 100 mL, and,6.1.3 Stirring Rods, sized to reach the bottom of the bottles.6.2 Tw
31、eezers, non-metallic tweezers sized to remove wipes from sample shipping containers.6.3 Ultrasonic Bath, 53 watts or greater output, 1 L or greater capacity, capable of heating to at least 60C.60 C.6.4 Thermometer, calibrated, non-mercury thermometer that covers the range from 0C0 C to at least 110C
32、.110 C.6.5 Disposable Plastic Gloves, impermeable and powder free, to avoid the possibility of contamination, and to protect fromcontact with toxic and corrosive substancessubstances.6.6 Pencil, with graphite tip.6.7 Aluminum Foil. Aluminum Foil.6.8 Surfactant, liquid.7. Reagents7.1 Purity of Reagen
33、tsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available (5). Other grades may be used provide
34、d that it can be demonstrated that they are of sufficientlyhigh purity to permit their use without decreasing the accuracy of the determinations.6 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 Sampl
35、ing andAnalytical Method Development, 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,
36、 EURACHEM Guide 1st Ed, 1998.6 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.E2914/E2914M 1937.2 Re
37、agent WaterASTM Type I water as given in Unless otherwise indicated, reference to water shall be understood to meanType 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 spect
38、rometric analysis, such as spectroscopic grade.E2914/E2914M 194NOTE 3Suitable purity means having undetectable lead content in the extracted composited sample blanks.7.3.2 Dilute 35 % (v/v). Prepare by first adding 500 mL of reagent water to a 1 L volumetric flask and then carefully adding350 mL con
39、centrated nitric acid. Make to volume with reagent water.8. Sample Preparation Procedure8.1 Testing of Sonicator (Practice E1979):8.1.1 Before use, ensure proper operation of the sonicator by employing one of the following diagnostic tests:8.1.1.1 Turn on the sonicator and allow for a reasonable war
40、m-up period, as recommended by the instrument manufacturer.(1) Insert the tip of a graphite pencil into the bath.(2) If the sonication device is operating properly, graphite in solution will be observed streaming off the tip of the pencil.8.1.1.2 Alternatively, demonstrate proper operation of the so
41、nicator according to the following procedure:(1) Fill the sonicator bath with warm water (ca. 45C)45 C) to a level about half-full, and add a small amount (for example,three drops) of surfactant.(2) Turn on the sonicator for a minimum of 5 min to degas the solution. Turn off the sonicator.(3) Place
42、aluminum foil (that is cut to a size conforming to 12 to 34 of the area of the bottom of the sonicator bath) on the bottomof the sonicator bath. Lower the foil at an angle to prevent the trapping of air beneath the foil. Ensure that a narrow layer of solutionremains between the foil and the bottom o
43、f the sonicator bath. The foil shall be parallel and centered to the bottom of the sonicator.(4) Turn on the sonicator for a period of at least 45 s.(5) Examine the aluminum foil after sonication. The foil should be observed to contain a myriad of small holes and bumps,and may be torn apart.Also, th
44、e perforation observed should be uniform; that is, all portions of the foil should be observed to havea high density of holes and perhaps tears. If the foil is not affected in this manner, then the sonicator performance is inadequatefor the purposes of this practice.8.2 Sample Handling:8.2.1 Don a p
45、air of impermeable gloves.8.2.2 Using clean tweezers and a clean stirring rod as needed, remove the wipes from the sample shipping container and placethe wipes in a clean 125 mL bottle.8.2.3 Using 15 mL 35 % (v/v) nitric acid, wash the inside of the sample shipping container, the tweezer tips, and t
46、he stirringrod into the bottle containing the wipes. Add the remainder of the acid to the bottle, ensuring that the wipes are immersed in theacid. Clean the tweezers and rods before and after use with laboratory wipes.8.2.4 Cap the bottle and shake to assure that the wipes are well wetted with the a
47、cid. If bubbles are observed inside of theimmersed wipe, apply pressure to the wipes with a clean stirring rod in order to force the bubbles up and out.8.2.5 Repeat 8.2.1 to 8.2.4 for successive samples as needed, depending on the size of the ultrasonic bath.NOTE 4Depending on the size of the sonica
48、tor, many bottles may be immersed in the bath at one time.Acustom rack for the bottles may be purchasedor constructed to allow for the regular and orderly placement of multiple bottles in the sonicator bath.8.2.6 Preheat water in the sonicator bath to at least 60C.60 C.8.2.7 Place the bottle (contai
49、ning the wipes immersed in dilute acid) upright in the sonicator bath, and ensure that the water levelin the bath is approximately 2.5 cm above the liquid level within the bottle.8.2.8 Sonicate for at least 30 min at 60C60 C or warmer.8.2.9 Remove the bottles from sonicator bath and allow to cool.8.2.10 When cool, use a clean glass or plastic stirring rod for each sample to push down on the wipes to force bubbles (formedduring sonication) up and out.8.2.11 Add 35 mL of reagent water to each bottle.8.2.12 Recap and shake to mix.8.2.13 Place
