1、Designation: E 1979 04Standard Practice forUltrasonic Extraction of Paint, Dust, Soil, and Air Samplesfor Subsequent Determination of Lead1This standard is issued under the fixed designation E 1979; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers an ultrasonic extraction procedurefor the extraction of lead from en
3、vironmental 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 determination o
4、f 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 as thestandard.1.6 This practice does not purport to address all of
5、 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 use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for
6、Reagent WaterD 5438 Practice for Collection of Floor Dust for ChemicalAnalysisD 6785 Test Method for Determination of Lead in Work-place AirE 631 Terminology of Building ConstructionsE 1605 Terminology Relating to Lead in BuildingsE 1613 Test Method for Determination of Lead by Induc-tively Coupled
7、Plasma Atomic Emission Spectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Spec-trometry (GFAAS) TechniquesE 1726 Practice for Preparation of Soil Samples by HotPlate Digestion for Subsequent Lead AnalysisE 1727 Practice for Field Collection of So
8、il Samples forLead Determination by Atomic Spectrometry TechniquesE 1728 Practice for Collection of Settled Dust SamplesUsing Wipe Sampling Methods for Subsequent LeadDeterminationE 1729 Practice for Field Collection of Dried Paint Samplesfor Lead Determination by Atomic Spectrometry Tech-niquesE 17
9、75 Guide for Evaluating the Performance of On-SiteExtraction and Field-Portable Electrochemical or Spectro-photometric Analysis for LeadE 1792 Specification for Wipe Sampling Materials for Leadin Surface DustE 1973 Provisional Practice for the Collection of SurfaceDust by Air Sampling Pump Vacuum Te
10、chnique for Sub-sequent Lead Determination3. Terminology3.1 Definitions: For definitions of terms relating to thispractice that do not appear in this section, refer to Terminolo-gies E 631 and E 1605.3.1.1 extractionthe dissolution of target analytes from asolid matrix into a liquid form.3.1.1.1 Dis
11、cussionDuring sample digestion or extraction,target analytes are extracted (solubilized) into solution toenable subsequent determination by analytical techniques (forexample, see Test Method E 1613).3.1.2 ultrasonic extractionthe use of ultrasonic energyand acidic or basic solution to extract target
12、ed 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 collection meth-ods (see Specification E 17
13、29; Practice E 1728, Practice1This 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, 2004. Published October 2004. Formerly PS8797. Ori
14、ginally adopted by Committee E06 in 1998. Last previous editionapproved in 1998 as E 1979 98.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document
15、Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D 5438 and Practice E 1973; Practice E 1727, respectively),are subjected to ultrasonic extraction in dilute nitric acid for adelineated time period.4.2 P
16、aint samples are ground, homogenized and weighed, ifnecessary, prior to ultrasonic extraction.4.3 Soil and bulk dust vacuum samples are sieved, homog-enized, and weighed prior to ultrasonic extraction.4.4 If applicable, dust filter samples are weighed prior toultrasonic extraction.4.5 Sample extract
17、s are diluted with ASTM Type I water(see Specification D 1193) in preparation for subsequent deter-mination of lead by analytical techniques (for example TestMethod E 1613, Guide E 1775, and NIOSH methods 7082,7105, and 7300 (1)3).4.6 This practice was developed based on an EPA standardoperating pro
18、cedure (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 dilute nitric acid is a simplerand easier method for
19、 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/high temperature digestion methods(for example, se
20、e Ref (1) and Test Method E 1613), providedthat the performance is demonstrated using accepted criteria asdelineated in Guide E 1775.5.2 In contrast with hot plate or microwave digestiontechniques, ultrasonic extraction is field-portable, which allowsfor on-site sample analysis.6. Apparatus and Mate
21、rials6.1 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 to60.002 g.6.4 Mortar and Pestle, pug mill, or wiggle
22、bug.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 Tweezers.6.10 Class A Pipets, 5 or 10 mL or both,
23、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 Tray.6.15 Rubber Mallet.6.16 Nylon Brush.6.17 A
24、luminum 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 Pencil7. Reagents7.1 ASTM Type I Water, in accordance with SpecificationD 1193.NOTE 2Commercially available distilled or deionized w
25、ater 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 extraction,while all other sample matrices require 25
26、% 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 instrument manufac-turer.8.1.1.2 Insert the tip of a
27、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 procedure:8.1.2.1 Fill the sonicator bath with
28、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 a size conformingto12 to34 of the area of the bo
29、ttom 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 shall be parallel andcentered to the bottom of the s
30、onicator.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 andbumps, and may be torn apart. Also, the perforation observedshould be uniform; that is, all portions of the foil should beo
31、bserved 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 Dry Paint Film Samples:3The boldface numbers given in parentheses refer to a list of references at theend of the tex
32、t.E1979042NOTE 4This practice assumes paint samples collected in accordancewith Practice E 1729.8.2.1 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 theestimated sample mass is greater than or equal to 0.25 g,
33、 thenquantitatively transfer the entire sample to an analytical bal-ance and weigh to the nearest 60.002 g. Under these circum-stances, do quantitative transfer and sample weighing prior togrinding and homogenization as described later in this practice.8.2.1.2 If the desired reporting units of lead
34、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 a mortar and pestleor a labeled 50 mL centrifuge tub
35、e. 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, pug mill, or wigglebug.Quantitatively transfer the
36、 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 following grind-ing, and then dry.8.2.2.2 Alternatively, place paint film sample in a clean, dry50 mL centri
37、fuge 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 condensation of water onto the sample by sealingthe sample a
38、nd 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 to 0.25g, or if the total sample mass is less than 0.25 g and the des
39、iredreported lead concentration is to be in units of mass of lead perunit mass of sample, weigh 0.05 to 0.25 g of ground andhomogenized paint sample to the nearest 60.002 g, and recordthe sample mass.NOTE 6If the desired reporting units are to be in terms of mass of leadper unit area of sample, and
40、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 reported lead concentration is to be in terms of mass
41、 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 mLpolypropylene centrifuge tube. To ensure quantitative sampl
42、etransfer, 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 and homogenizedpaint sample. Shake the centrifuge tu
43、be 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 place in an uprightposition in the sonicator bath.8.
44、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 the number of samples.NOTE 7Depending on the size of
45、 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 ultrasonic energy to the crushed and acidifiedsamples
46、 within the immersed centrifuge tubes for at least 30min.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 diluteacidified extracts to the 50 mL mark with ASTM Type
47、 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 Dust Wipe Samples:NOTE 9This procedure assumes dust
48、wipe samples were collected inaccordance with Practice E 1728 using wipes that conform to Specifica-tion E 1792.8.3.1 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 witha pair of clean tweezers, and place it in a l
49、abeled 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 needed, add more diluted 25 % HNO3in 5 mL aliquots
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