1、Designation: E2913 14Standard Practice forHotplate Digestion of Lead from Composited Wipe Samples1This standard is issued under the fixed designation E2913; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、 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 is similar to Practice E1644 and covers thehot, nitric acid digestion of lead (Pb) from a compositedsample of up to fo
3、ur individual wipe samples of settled dustcollected from 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 procedures
4、used 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-p
5、ound units are provided in Note 7and Note 9 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-b
6、ility 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 Sp
7、ectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE1644 Practice for Hot Plate Digestion of Dust WipeSamples for the Determination of LeadE1728 Practice for Collection of Settled Dust Samples UsingWipe Sampling Meth
8、ods for Subsequent Lead Determi-nationE1792 Specification for Wipe Sampling Materials for Leadin Surface DustE2051 Practice for the Determination of Lead in Paint,Settled Dust, Soil and Air Particulate by Field-PortableElectroanalysis (Withdrawn 2010)3E2239 Practice for Record Keeping and Record Pre
9、servationfor Lead Hazard Activities2.2 ISO Standards:4ISO 1042 Laboratory Glassware One-mark VolumetricFlasksISO/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
10、Lead-Based Paint Poisoning Prevention 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 resulti
11、ng fromthe combination of individual 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 un
12、der the jurisdiction of ASTM Committee 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/E2913-142For referenced ASTM standards, visit the ASTM webs
13、ite, www.astm.org, orcontact ASTM 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 Internationa
14、l Organization for Standardization (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 AST
15、M International, 100 Barr Harbor 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 modifica
16、tions of standard methods to con-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 sta
17、tement as to whether the method is 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
18、wipes, meeting the requirements of 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 thendigested using heat and nitric acid. The resulting extractsolution is analyzed ac
19、cording to Test Method E1613 orPractice 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
20、 and should not 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
21、matrices not soluble 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 vali
22、datedfor use and 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 Glassware:6.1.1 Volumetric F
23、lasks, 400 mL, borosilicate, withStoppers, 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 Stirring Rods, sized to reach the bottom of the GriffinBeakers.6.2 Funnels, plastic, porcela
24、in or borosilicate funnels sizedto deliver filtrate into a 400 mL volumetric flask.6.3 Tweezers, non-metallic tweezers sized to remove wipesfrom sample shipping containers.6.4 Filter Paper, fast filtering, suitable for metals analysis.6.5 Electric Hotplates, suitable for operation at tempera-tures t
25、hat allow digestion of nitric acid and hydrogen peroxidesolutions encountered 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 Disposable Gloves, impermeable and powder free, toavoid the possibility of contamination, and t
26、o protect fromcontact with toxic and corrosive substances.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 suitable purity for atomic spectro-metric analysis, such as spect
27、roscopic grade.NOTE 3Suitable purity means having undetectable lead content in theextracted composited sample blanks.7.2.2 Dilute 1:1 (v/v); prepared by carefully pouring avolume of concentrated acid into an equal volume of reagentwater.7.3 Hydrogen Peroxide30 % (w/w), suitable for atomicspectrometr
28、ic analysis, such as spectroscopic grade. See Note3.8. Sample Preparation Procedure8.1 Don a new pair of impermeable gloves. Treat eachcomposited sample in a batch equally.8.2 Quantitatively transfer the contents of the dust-wipesample containers to a labeled beaker as follows:8.2.1 Carefully open e
29、ach container, remove wipes using aclean tweezers and a clean stirring rod as needed, and place allthe wipes comprising the composited sample into a clean 250mL beaker.8.2.2 If the sample containers are hard-walled, rigid con-tainers such as a plastic centrifuge tubes, using a minimumvolume of solut
30、ion, wash the inside of the sample shippingcontainer, the tweezer tips and the stirring rod with 1:1 (v/v)nitric acid into the beaker containing the wipes.8.2.3 If the sample containers are flexible plastic bags andmaterial appears to be left behind after wipe removal, attemptto transfer the residua
31、l material into the beaker by shaking orusing mechanical removal with a clean laboratory spatula or6Kennedy, 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 (NIOS
32、H), Publication 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 f
33、or Single Laboratory Validation of Methods ofAnalysis (IUPAC Technical Report) Pure Appl. Chem., Vol. 74, No. 5, pp. 835855,2002.E2913 142similar tool. Document observations of potential loss of sampledue to any residue in the container for later reporting with theresults of the lead analysis.8.3 Sl
34、owly add 60 mL of concentrated nitric acid to thebeaker. Assuring that all wipes are immersed, gently swirl tomix, and cover with a clean watch glass. Digest on a hotplateto a solution volume of about 8 mL. Do not digest to dryness.(WarningSome wipes break down into a gelatinous residuethat readily
35、bumps or spatters, or both. Heating should beslowed with these materials.)8.4 Remove from the hotplate and allow to cool.8.5 When cool, carefully remove the watch glass and slowlyadd 40 mL of 30 % (w/w) hydrogen peroxide, assuring that allwipes are immersed.NOTE 4Exercise care when removing the watc
36、h glass. Avoid leadcontamination problems by placing it upside down on new clean labora-tory wipes.8.6 Cover the beaker with the watchglass and return thecovered beaker to the hot plate. Take care to ensure that lossesdo not occur due to vigorous effervescence during heating.Heat until effervescence
37、 subsides and then digest to a solutionvolume of about 8 mL. Do not digest to dryness.8.7 Remove the digestate from the hotplate and allow tocool.8.8 Assemble funnels, filter paper and volumetric flasks asneeded to allow filtering of digestates into 400 mL volumetricflasks.NOTE 5Do not attempt to po
38、ur the undiluted digestate through thefilter paper as the filter paper will dissolve in strong acid solutions.8.9 When cool, use reagent water to wash the bottom of thewatch glass, the inside walls of the beaker, and any remainingwipe material to the bottom of the beaker. Use about 80 mL ofreagent w
39、ater to accomplish the washing. Pour the diluteddigestate through 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 inthe bottom of the beaker three times. Use enough reagent watereach time to at least cover the remaini
40、ng wipe material in thebeaker. Use about 150 mL to accomplish the washing. Pour thefirst two washings through the filter paper, and use the third towash any remaining wipe material from the beaker and ontothe filter paper.8.11 Using reagent water, wash the glass stirring rod and thebeaker at least t
41、hree times. Pour the washings through the filterpaper.8.12 Using reagent water, wash the filter paper, any remain-ing wipe material on the filter paper, the funnel, and the funnelstem into the volumetric flask.8.13 Add reagent water to the volumetric flask to the mark,cap and invert to mix. The resu
42、lting digestate solution is about2 % (v/v) nitric acid. Calibration standards used for instrumen-tal measurement should be made with this level of nitric acid.NOTE 6The wipe material may or may not be completely solubilized.Many types of wipes contain materials that do not dissolve in nitric acid.8.
43、14 Analyze the digestate according to Test Method E1613or Practice E2051.9. Calculations9.1 To report the total lead found, calculate the total leadeddust found on the surfaces sampled, g Pb.gPb# 5C!400! (1)where:C = digestate lead concentration analytically found; inmicrograms of lead per millilitr
44、e, g Pb/mL400 = final digestate volume, in millilitres, 400 mLg Pb = total leaded dust found on the surfaces sampled; inmicrograms of lead, 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
45、 individual areas sampled.All measurements are to be done in centimetres, cm, withresulting areas 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 w
46、ipes is four (n 4)9.2.2 Divide the mass of lead found g Pb by the total areasampledATto determine 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-pos
47、ited wipe samplingNOTE 7To determine the average leaded dust loading for the areassampled, the individual areas sampled must be the same size, for example,929 cm2(1 ft2) each. The use of English units is for informationalpurposes.NOTE 8Consult the laws, regulations and requirements of the localautho
48、rity having jurisdiction for any required method of calculation oflead loading.NOTE 9In the United 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 wi
49、th each collected from a 929 cm2(1 ft2) area, dividethe reported results in units g Pb/cm2 by 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 sig
