1、Designation: E2914 14Standard Practice forUltrasonic Extraction of Lead from Composited WipeSamples1This standard is issued under the fixed designation E2914; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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 practice covers the extraction of lead (Pb) usingultrasonication, heat and nitric acid from a composited sampleof up to four
3、individual wipe samples of settled dust collectedfrom the same space.1.2 This practice contains notes which are explanatory andnot part of mandatory requirements of the practice.1.3 This practice should be used by analysts experienced indigestion techniques such as hot blocks. Like all proceduresuse
4、d in an analytical laboratory, this practice needs to bevalidated for use and shown to produce acceptable resultsbefore being applied to client samples.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4.1 ExceptionInch-poun
5、d units are provided in Note 6and Note 8 for information.1.5 This standard does not purport 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-bili
6、ty of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterE1605 Terminology Relating to Lead in BuildingsE1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emission Spect
7、rometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE1728 Practice for Collection of Settled Dust Samples UsingWipe Sampling Methods for Subsequent Lead Determi-nationE1792 Specification for Wipe Sampling Materials for L
8、eadin Surface DustE1979 Practice for Ultrasonic Extraction of Paint, Dust,Soil, and Air Samples for Subsequent Determination ofLeadE2051 Practice for the Determination of Lead in Paint,Settled Dust, Soil and Air Particulate by Field-PortableElectroanalysis (Withdrawn 2010)3E2239 Practice for Record
9、Keeping and Record Preservationfor Lead Hazard Activities2.2 ISO Standards:4ISO/IEC 17025:2005 General Requirements for the Compe-tence of Testing and Calibration LaboratoriesISO 3585 Borosilicate Glass 3.3 Properties Third Edition2.3 Other Document:540 CFR Part 745 Lead-Based Paint Poisoning Preven
10、tion inCertain Residential Structures3. Terminology3.1 For definitions of terms not appearing here, refer toTerminology D1129, Specification D1193 and TerminologyE1605.3.2 Definitions of Terms Specific to This Standard:3.2.1 composited samplethe single sample resulting fromthe combination of individ
11、ual samples collected from differentsections of the same area.3.2.2 validationthe confirmation by examination and theprovision of objective evidence that the particular requirementsfor a specific intended use are fulfilled ISO 17025:2005(5.4.5.1).1This practice is under the jurisdiction of ASTM Comm
12、ittee E06 on Perfor-mance of Buildings and is the direct responsibility of Subcommittee E06.23 on LeadHazards Associated with Buildings.Current edition approved May 1, 2014. Published June 2014. DOI: 10.1520/E2914-142For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
13、 Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from International Organization for Standardizatio
14、n (ISO), 1, ch. dela Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.5Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.Copyright ASTM International, 100 Barr Harbor
15、Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.3 The laboratory is responsible for validating6,7,8,9non-standard methods, laboratory-designed/developed methods,standard methods used outside their intended scope, andamplifications and modifications of standard methods to con-
16、firm that the methods are fit for the intended use. The validationshall be as extensive as is necessary to meet the needs of thegiven application or field of application. The laboratory shallrecord the results obtained, the procedure used for thevalidation, and a statement as to whether the method i
17、s fit forthe intended use.NOTE 1It is the responsibility of the laboratory to carry out its testingactivities 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 o
18、f Specifi-cation E1792, are used according to Practice E1728 to collectsettled dust from equally-sized areas in the same space andcomposited as one sample. This composited sample is thenextracted using ultrasonication, heat and nitric acid. Theresulting extract solution is analyzed according to Test
19、 MethodE1613 or Practice E2051.5. Significance and Use5.1 This practice is for use in the preparation of no morethan four wipe samples combined to form a composited samplefor subsequent determination of lead content.5.2 This practice assumes use of wipes that meet Specifica-tion E1792 and should not
20、 be used unless the wipes meetSpecification E1792.5.3 This practice is capable of preparing samples for deter-mination of lead bound within paint dust.5.4 This practice may not be capable of preparing samplesfor determination of lead bound within silica or silicatematrices, or within matrices not so
21、luble in nitric acid.5.5 Adjustment of the nitric acid concentration or acidstrength, or both, of the final extract solution may be necessaryfor compatibility with the instrumental analysis method to beused for lead quantification.5.6 This sample preparation practice has not been validatedfor use an
22、d must be validated by the user prior to using thepractice for client samples.NOTE 2Each combination of wipes (two wipes, three wipes, and fourwipes) constitutes a different matrix and must be separately validated.6. Apparatus and Materials6.1 Borosilicate Glass (conforming to ISO 3585) or PlasticLa
23、bware:6.1.1 Bottles, 125 mL, polypropylene or equivalent, withscrew 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 Tweezers, non-metallic tweezers sized to remove wipesfrom sample shipping containers.6.3 Ultrasonic Bath, 5
24、3 watts or greater output, 1 L orgreater capacity, capable of heating to at least 60C.6.4 Thermometer, calibrated, non-mercury thermometer thatcovers the range from 0C to at least 110C.6.5 Disposable Plastic Gloves, impermeable and powderfree, to avoid the possibility of contamination, and to protec
25、tfrom contact with toxic and corrosive substances6.6 Pencil, with graphite tip.6.7 Aluminum Foil.6.8 Surfactant, liquid.7. Reagents7.1 Reagent WaterASTM Type I water as given in Speci-fication D1193 with minimum resistance of 16.67 megaohm-cm, or equivalent.7.2 Nitric Acid:7.2.1 Concentrated, of sui
26、table purity for atomic spectro-metric analysis, such as spectroscopic grade.NOTE 3Suitable purity means having undetectable lead content in theextracted composited sample blanks.7.2.2 Dilute 35 % (v/v). Prepare by first adding 500 mL ofreagent water toa1Lvolumetric flask and then carefullyadding 35
27、0 mL concentrated nitric acid. Make to volume withreagent water.8. Sample Preparation Procedure8.1 Testing of Sonicator (Practice E1979):8.1.1 Before use, ensure proper operation of the sonicatorby employing one of the following diagnostic tests:8.1.1.1 Turn on the sonicator and allow for a reasonab
28、lewarm-up period, as recommended by the instrument manufac-turer.(1) Insert the tip of a graphite pencil into the bath.(2) If the sonication device is operating properly, graphitein solution will be observed streaming off the tip of the pencil.8.1.1.2 Alternatively, demonstrate proper operation of t
29、hesonicator according to the following procedure:(1) Fill the sonicator bath with warm water (ca. 45C) to alevel 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 degasthe solution. Turn off the sonicator.(3) Place alu
30、minum foil (that is cut to a size conforming to12 to34 of the area of the bottom of the sonicator bath) on thebottom of the sonicator bath. Lower the foil at an angle toprevent the trapping of air beneath the foil. Ensure that anarrow layer of solution remains between the foil and thebottom of the s
31、onicator bath. The foil shall be parallel andcentered to the bottom of the sonicator.6Kennedy, Ph.D., Eugene R., Fischbach, Thomas J., Song, Ph.D., Ruiguang,Eller, Ph.D., Peter M., and Schulman, Ph.D., Stanley A., Guidelines for AirSampling and Analytical Method Development, DHHS (NIOSH), Publicatio
32、n No.95-117, 1995.7Green, J. Mark, A Practical Guide to Analytical Method Validation, AnalyticalChemistry, 1996, (68) 305A-309A.8The Fitness for Purpose of Analytical Methods-A Laboratory Guide to MethodValidation and Related Topics, EURACHEM Guide 1st Ed, 1998.9Harmonized Guidelines for Single Labo
33、ratory Validation of Methods ofAnalysis (IUPAC Technical Report) Pure Appl. Chem., Vol. 74, No. 5, pp. 835855,2002.E2914 142(4) Turn on the sonicator for a period of at least 45 s.(5) Examine the aluminum foil after sonication. The foilshould be observed to contain a myriad of small holes andbumps,
34、and may be torn apart. Also, the perforation observedshould be uniform; that is, all portions of the foil should beobserved to have a high density of holes and perhaps tears. Ifthe foil is not affected in this manner, then the sonicatorperformance is inadequate for the purposes of this practice.8.2
35、Sample Handling:8.2.1 Don a pair of impermeable gloves.8.2.2 Using clean tweezers and a clean stirring rod asneeded, remove the wipes from the sample shipping containerand place the wipes in a clean 125 mL bottle.8.2.3 Using 15 mL 35 % (v/v) nitric acid, wash the inside ofthe sample shipping contain
36、er, the tweezer tips, and the stirringrod into the bottle containing the wipes. Add the remainder ofthe acid to the bottle, ensuring that the wipes are immersed inthe acid. Clean the tweezers and rods before and after use withlaboratory wipes.8.2.4 Cap the bottle and shake to assure that the wipes a
37、rewell wetted with the acid. If bubbles are observed inside of theimmersed wipe, apply pressure to the wipes with a cleanstirring rod in order to force the bubbles up and out.8.2.5 Repeat 8.2.1 to 8.2.4 for successive samples asneeded, depending on the size of the ultrasonic bath.NOTE 4Depending on
38、the size of the sonicator, many bottles may beimmersed in the bath at one time. A custom rack for the bottles may bepurchased or constructed to allow for the regular and orderly placement ofmultiple bottles in the sonicator bath.8.2.6 Preheat water in the sonicator bath to at least 60C.8.2.7 Place t
39、he bottle (containing the wipes immersed indilute acid) upright in the sonicator bath, and ensure that thewater level in the bath is approximately 2.5 cm above the liquidlevel within the bottle.8.2.8 Sonicate for at least 30 min at 60C or warmer.8.2.9 Remove the bottles from sonicator bath and allow
40、 tocool.8.2.10 When cool, use a clean glass or plastic stirring rodfor each sample to push down on the wipes to force bubbles(formed during 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 the bottle into the sonicator such that the w
41、aterin the sonicator bath is approximately 2.5 cm above the liquidlevel in the bottle.8.2.14 Sonicate for at least 30 min at 60C or warmer. Ifbubbles are observed inside of the immersed wipe, applypressure to the wipes with a clean stirring rod in order to forcethe bubbles up and out.8.2.15 Remove f
42、rom sonicator bath and allow to cool.8.2.16 When cool, shake to mix. The extract is about 10 %(v/v) nitric acid.NOTE 5Centrifuge a portion of the extract if it is excessively turbid orshows excess suspended solids, or both.8.2.17 Analyze the extract according to Test Method E1613or Practice E2051.9.
43、 Calculations9.1 To report the total lead found, calculate the total leadeddust found on the surfaces sampled, g Pb.gPb# 5C!50! (1)where:C = extract lead concentration analytically found; inmicrograms per millilitre, g Pb/mL50 = final digestate volume, in millilitres, 50 mLg Pb = total amount of lea
44、d found on the surfacessampled; in micrograms, g Pb9.2 To report the results as leaded dust loading per unit area:9.2.1 Determine the total area sampled (up to four areas percomposited sample) by summing the individual areas sampled.All measurements are to be done in centimetres, cm, withresulting a
45、reas in square centimetres, cm2.AT5 a11.1an(2)where:AT= total area sampled, in square centimetres, cm2a = area sampled by wipes to be composited, in squarecentimetres, cm2, where the maximum total numberof wipes is four (n 4)9.2.2 Divide the mass of lead found g Pb by the total areasampledATto deter
46、mine the leaded dust loading as determinedby composited wipe sampling.g Pb/ cm2# 5 gPb#/AT(3)where:g Pb = total leaded dust found on the surfacessampledg Pb/cm2 = leaded dust loading as determined by com-posited wipe samplingNOTE 6To determine the average leaded dust loading for the areassampled, th
47、e individual areas sampled must be the same size, for example,929 cm2(1 ft2) each. The use of English units is for informationalpurposes.NOTE 7Consult the laws, regulations and requirements of the localauthority having jurisdiction for any required method of calculation oflead loading.NOTE 8In the U
48、nited States of America (per 40 CFR Part 745), theaverage lead loading for a space is to be reported in units of microgramsof lead per square foot, g Pb/ft2. For example: For a three-wipecomposited sample with each collected from a 929 cm2(1 ft2) area, dividethe reported results in units g Pb/cm2 by
49、 2787 (= 3 x 929) since 929cm2=1ft2. The use of English units is for informational purposes.10. Records10.1 Each analyst and technician shall record their samplepreparation activities in a laboratory notebook or an electronicrecord.10.1.1 Laboratory notebooks, if not electronic records, shallbe bound with pre-numbered pages.10.1.2 All entries in laboratory notebooks, if not electronicrecords, shall be made using ink with signature and date ofentry.10.1.3 Any entry errors in laboratory notebooks shall becorrected
