1、Designation: E1979 12 (Reapproved 2016)Standard Practice forUltrasonic Extraction of Paint, Dust, Soil, and Air Samplesfor Subsequent Determination of Lead1This standard is issued under the fixed designation E1979; the number immediately following the designation indicates the year oforiginal adopti
2、on 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 last revision or reapproval.1. Scope1.1 This practice covers an ultrasonic extraction procedurefor the extraction
3、of lead from environmental samples ofinterest in lead abatement and renovation (or related) work, foranalytical purposes.1.2 Environmental matrices of concern include dry paintfilms, settled dusts, soils, and air particulates.1.3 Samples subjected to ultrasonic extraction are preparedfor subsequent
4、determination of lead by laboratory analyticalmethods.1.4 This practice includes, where applicable, descriptions ofprocedures for sample homogenization and weighing prior toultrasonic extraction.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are includ
5、ed in thisstandard.1.6 This practice does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this practice to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitation prior to u
6、se.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD5438 Practice for Collection of Floor Dust for ChemicalAnalysisD6785 Test Method for Determination of Lead in WorkplaceAir Using Flame or Graphite Furnace Atomic AbsorptionSpectrometryD7144 Practice for Collection of
7、 Surface Dust by Micro-vacuum Sampling for Subsequent Metals DeterminationE631 Terminology of Building ConstructionsE1605 Terminology Relating to Lead in BuildingsE1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emission Spectrometry(ICP-AES), Flame Atomic Absorption
8、 Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE1726 Practice for Preparation of Soil Samples by HotplateDigestion for Subsequent Lead AnalysisE1727 Practice for Field Collection of Soil Samples forSubsequent Lead DeterminationE1728 Practice for Collection
9、 of Settled Dust Samples UsingWipe Sampling Methods for Subsequent Lead Determi-nationE1729 Practice for Field Collection of Dried Paint Samplesfor Subsequent Lead DeterminationE1775 Guide for Evaluating Performance of On-Site Extrac-tion and Field-Portable Electrochemical or Spectrophoto-metric Ana
10、lysis for LeadE1792 Specification for Wipe Sampling Materials for Leadin Surface Dust3. Terminology3.1 Definitions: For definitions of terms relating to thispractice that do not appear in this section, refer to Terminolo-gies E631 and E1605.3.1.1 extractionthe dissolution of target analytes from aso
11、lid matrix into a liquid form.3.1.1.1 DiscussionDuring sample digestion or extraction,target analytes are extracted (solubilized) into solution toenable subsequent determination by analytical techniques (forexample, see Test Method E1613).3.1.2 ultrasonic extractionthe use of ultrasonic energyand ac
12、idic or basic solution to extract targeted analytes fromsamples.3.1.2.1 DiscussionThe extract solution is subsequentlyanalyzed for the determination of targeted analytes.4. Summary of Practice4.1 Samples of paint, settled dust (wipe or vacuum), soil, orairborne particles, obtained by ASTM sample col
13、lection meth-ods (see Practice E1729; Practice E1728, Practice D5438 and1This practice is under 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 Oct. 1, 2016.
14、Published October 2016. Formerly PS8797. Originally adopted by Committee E06 in 1998. Last previous editionapproved in 2012 as E1979-12. DOI: 10.1520/E1979-12R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book
15、of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1Practice D7144; Practice E1727, respectively), are subjected toultrasonic extraction
16、in dilute nitric acid for a delineated timeperiod.4.2 Paint samples are ground, homogenized and weighed, ifnecessary, prior to ultrasonic extraction.4.3 Soil and bulk dust vacuum samples are sieved,homogenized, and weighed prior to ultrasonic extraction.4.4 If applicable, dust filter samples are wei
17、ghed prior toultrasonic extraction.4.5 Sample extracts are diluted with ASTM Type I water(see Specification D1193) in preparation for subsequent deter-mination of lead by analytical techniques (for example TestMethod E1613, Guide E1775, and NIOSH methods 7082,7105, and 7300 (1)3).4.6 This practice w
18、as developed based on an EPA standardoperating procedure (ultrasonic extraction followed by colori-metric lead analysis (2) and published protocols (ultrasonicextraction followed by anodic stripping voltammetric determi-nation of lead) (3)(4).5. Significance and Use5.1 Ultrasonic extraction using di
19、lute nitric acid is a simplerand easier method for extracting lead from environmentalsamples than are traditional digestion methods that employ hotplate or microwave digestion with concentrated acids (1), (3),(5), (6). Hence, ultrasonic extraction may be used in lieu of themore rigorous strong acid/
20、high temperature digestion methods(for example, see Ref (1) and Test Method E1613), providedthat the performance is demonstrated using accepted criteria asdelineated in Guide E1775.5.2 In contrast with hot plate or microwave digestiontechniques, ultrasonic extraction is field-portable, which allowsf
21、or on-site sample analysis.6. Apparatus and Materials6.1 Sonicator, 50 W minimum power; proper operation ofthe sonicator shall be confirmed prior to initial use andperiodically thereafter.6.2 Plastic Centrifuge Tubes, 50 mL, with screw caps.6.3 Analytical Balance, accuracy better than or equal to60.
22、002 g.6.4 Mortar and Pestle, pug mill, or wigglebug.6.5 Dry Ice (CO2(s).6.6 Cooler, for storage of dry ice.6.7 Plastic or Glass Rods, 0.6 to 1.0 cm diameter,15 to 20 cm length; tapered at one end to conform to the shapeof the bottoms of the 50 mL centrifuge tubes.6.8 Powderless Plastic Gloves.6.9 Tw
23、eezers.6.10 Class A Pipets, 5 or 10 mL or both, and other volumesas needed.NOTE 1Precision digital mechanical pipettors using replaceable tipsmeet Class A requirements.6.11 Laboratory Wipes, wet or dry, or both.6.12 Power Source for Sonicator.6.13 Sieves, Number 10 (1.9 mm) and 250 m.6.14 Collection
24、 Tray.6.15 Rubber Mallet.6.16 Nylon Brush.6.17 Aluminum Pie Tins.6.18 Dust Mask.6.19 Glass or Plastic Stirring Rods.6.20 Aluminum Foil (conventional thickness for householduse, that is, not heavy duty).6.21 Graphite Pencil.7. Reagents7.1 ASTM Type I Water, in accordance with SpecificationD1193.NOTE
25、2Commercially available distilled or deionized water meetsASTM Type I water specifications.7.2 Extraction Solution, 10 % or 25 % v/v HNO3/H2O;prepared from reagent grade concentrated nitric acid (70 to71 % HNO3) and ASTM Type I water.NOTE 3Air filter samples require 10 % nitric acid (v/v) for extrac
26、tion,while all other sample matrices require 25 % v/v HNO3/H2O.8. Procedure8.1 Testing of Sonicator:8.1.1 Before use, ensure proper operation of the sonicatorby employing the following diagnostic test.8.1.1.1 Turn on the sonicator and allow for a reasonablewarm-up period, as recommended by the instr
27、ument manufac-turer.8.1.1.2 Insert the tip of a graphite pencil into the bath.8.1.1.3 If the sonication device is operating properly, graph-ite in solution will be observed streaming off the tip of thepencil.8.1.2 Alternatively, demonstrate proper operation of thesonicator according to the following
28、 procedure:8.1.2.1 Fill the sonicator bath with warm water (ca. 45C) toa level about half-full, and add a small amount (for example,three drops) of surfactant8.1.2.2 Turn on the sonicator for a minimum of 5 min todegas the solution. Turn off the sonicator.8.1.2.3 Place aluminum foil (that is cut to
29、a size conformingto12 to34 of the area of the bottom of the sonicator bath) onthe bottom 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 sonicator bath. The foil shal
30、l be parallel andcentered to the bottom of the sonicator.8.1.2.4 Turn on the sonicator for a period of 45 s.8.1.2.5 Examine the aluminum foil after sonication. The foilshould be observed to contain a myriad of small holes and3The boldface numbers given in parentheses refer to a list of references at
31、 theend of the text.E1979 12 (2016)2bumps, 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 inadeq
32、uate for the purposes of this practice.8.2 Dry Paint Film Samples:NOTE 4This practice assumes paint samples collected in accordancewith Practice E1729.8.2.1 Don a pair of gloves.8.2.1.1 If the desired reported lead concentration units are tobe in terms of lead mass per unit area of sample, and thees
33、timated sample mass is greater than or equal to 0.25 g, thenquantitatively transfer the entire sample to an analytical bal-ance and weigh to the nearest 60.002 g. Under thesecircumstances, do quantitative transfer and sample weighingprior to grinding and homogenization as described later in thisprac
34、tice.8.2.1.2 If the desired reporting units of lead concentrationare to be in terms of lead mass per unit mass of sample, or ifthe desired reporting units are to be in terms of lead mass perunit area and the estimated mass of the sample is less than 0.25g, then quantitatively transfer the sample to
35、a mortar and pestleor a labeled 50 mL centrifuge tube. Use tweezers if necessaryfor quantitative sample transfer. Clean tweezers before andafter use with laboratory wipes.8.2.2 Sample Grinding and Homogenization:8.2.2.1 Grind and homogenize paint film sample to a finepowder using a mortar and pestle
36、, pug mill, or wigglebug.Quantitatively transfer the ground and homogenized a paintsample to a weighing vessel or weighing paper (see below).Thoroughly clean mortar and pestle, wigglebug, or pug millwith moistened laboratory wipes prior to and followinggrinding, and then dry.8.2.2.2 Alternatively, p
37、lace paint film sample in a clean, dry50 mL centrifuge tube, and place the tube in dry ice. Using aplastic or metal rod, grind and homogenize the super-cooled,brittle paint sample to a fine powder. Thoroughly clean rodwith laboratory wipes prior to and following grinding proce-dure. Avoid condensati
38、on of water onto the sample by sealingthe sample and allowing it to warm to ambient temperaturebefore weighing.NOTE 5The use of dry ice as described assists greatly in the grindingand homogenization of dry paint film samples.8.2.3 If the total sample mass is greater than or equal to0.25 g, or if the
39、 total sample mass is less than 0.25 g and thedesired reported lead concentration is to be in units of mass oflead per unit mass of sample, weigh 0.05 to 0.25 g of groundand homogenized paint sample to the nearest 60.002 g, andrecord the sample mass.NOTE 6If the desired reporting units are to be in
40、terms of mass of leadper unit area of sample, and the sample mass is estimated to be less than0.25 g, a larger sample may be collected in order to obtain more mass(thereby enabling the sample to be treated as described in 8.2.1.1).8.2.4 If the total sample mass is less than 0.25 g and thedesired rep
41、orted lead concentration is to be in terms of mass oflead per unit area of collected sample, then the sample need notbe weighed. However, the entire ground and homogenizedsample must be placed in the tube for extraction as describedbelow.8.2.5 Place the sample in a clean, dry, labeled 50 mLpolypropy
42、lene centrifuge tube. To ensure quantitative sampletransfer, rinse materials used for transferring samples with aminimum of dilute (5 %) nitric acid, and direct the rinsate intothe centrifuge tube.8.2.6 Using a class A pipet, introduce 5 mL of 25 % HNO3to the centrifuge tube containing the ground an
43、d homogenizedpaint sample. Shake the centrifuge tube briefly to ensure thatno solid paint material remains stuck to the bottom of the tube.Rinse the inside of the centrifuge tube with a minimumquantity of 5 % HNO3in order to ensure immersion of all solidmaterial.8.2.7 Cap the centrifuge tube, and pl
44、ace in an uprightposition in the sonicator bath.8.2.8 Ensure that the bath of the sonicator contains enoughwater so that the water level is at least 2.5 cm above the levelof liquid within the centrifuge tube.8.2.9 Repeat steps 8.2.1 8.2.8 as needed, depending on thesize of the ultrasonic bath and th
45、e number of samples.NOTE 7Depending on the size of the sonicator, many centrifuge tubesmay be immersed in the bath at one time. A custom rack for the centrifugetubes may be purchased or constructed to allow for the regular and orderlyplacement of multiple tubes in the sonicator bath.8.2.10 Apply ult
46、rasonic energy to the crushed and acidifiedsamples within the immersed centrifuge tubes for at least30 min.8.2.11 Remove centrifuge tubes from the bath. Keep tubesin upright position.8.2.12 Remove caps from centrifuge tubes that containsamples that were subjected to ultrasonic agitation, and dilutea
47、cidified extracts to the 50 mL mark with ASTM Type I water.8.2.13 Re-cap and then shake the tubes for 5 to 10 s, andallow the contents to settle. The samples are now ready foranalysis for lead content.NOTE 8The sample solutions may require filtration or centrifugationprior to analysis.8.3 Settled Du
48、st Wipe Samples:NOTE 9This procedure assumes dust wipe samples were collected inaccordance with Practice E1728 using wipes that conform to SpecificationE1792.8.3.1 Don a pair of gloves.8.3.2 If not already placed in a labeled 50 mL centrifugetube, remove the wipe sample from the sample container wit
49、ha pair of clean tweezers, and place it in a labeled clean and dry50 mL centrifuge tube. Shove the wipe to the bottom of thetube with a clean glass or plastic rod. Rinse the original samplecontainer (if applicable), tweezers and rod with a minimum ofdilute (5 %) nitric acid to ensure quantitative sample transfer;make sure that the rinsate falls into the centrifuge tube. Cleantweezers and rods before and after use with laboratory wipes.8.3.3 Using a class A pipet, introduce 15 mL of 25 % HNO3to the centrifuge tube containing the wipe sample, and cap thetube. If ne
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