ASTM E1979-21

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation: E1979 − 17 E1979 − 21
Standard Practice for
Ultrasonic Extraction of Paint, Dust, Soil, and Air Samples
for Subsequent Determination of Lead
This standard is issued under the fixed designation E1979; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice covers an ultrasonic extraction procedure for the extraction of lead from environmental samples of interest in
lead abatement and renovation (or related) work, for analytical purposes.
1.2 Environmental matrices of concern include dry paint films, settled dusts, soils, and air particulates.
1.3 Samples subjected to ultrasonic extraction are prepared for subsequent determination of lead by laboratory analytical methods.
1.4 This practice includes, where applicable, descriptions of procedures for sample homogenization and weighing prior to
ultrasonic extraction.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This practicestandard does not purport to address all of the safety concerns, if any, associated with its use. It is the
responsibility of the user of this practicestandard to establish appropriate safety safety, health, and healthenvironmental practices
and determine the applicability of regulatory limitationlimitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D5438 Practice for Collection of Floor Dust for Chemical Analysis
D6785 Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furnace Atomic Absorption
Spectrometry
D7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Determination of Metals and
Metalloids
D8358 Guide for Assessment and Inclusion of Wall Deposits in the Analysis of Single-Stage Samplers for Airborne Particulate
Matter
This practice is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.12 on Sampling and
Analysis,Analysis of Lead,Lead for Exposure and Risk Assessment.
Current edition approved March 1, 2017Nov. 1, 2021. Published March 2017January 2023. Formerly PS 87–97. Originally adopted by Committee E06 in 1998. Last
previous edition approved in 20162017 as E1979-12(2016).E1979 – 17. DOI: 10.1520/E1979-17.10.1520/E1979-21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1979 − 21
E631 Terminology of Building Constructions
E1605 Terminology Relating to Lead in Buildings
E1613 Test Method for Determination of Lead by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES),
Flame Atomic Absorption Spectrometry (FAAS), or Graphite Furnace Atomic Absorption Spectrometry (GFAAS) Techniques
(Withdrawn 2021)
E1726 Practice for Preparation of Soil Samples by Hotplate Digestion for Subsequent Lead Analysis
E1727 Practice for Field Collection of Soil Samples for Subsequent Lead Determination
E1728 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Lead Determination
E1729 Practice for Field Collection of Dried Paint Samples for Subsequent Lead Determination
E1775 Guide for Evaluating Performance of On-Site Extraction and Field-Portable Electrochemical or Spectrophotometric
Analysis for Lead
E1792 Specification for Wipe Sampling Materials for Lead in Surface Dust
3. Terminology
3.1 Definitions:Definitions For —For definitions of terms relating to this practice that do not appear in this section, refer to
Terminologies E631 and E1605.
3.1.1 extraction—extraction, n—the dissolution of target analytes from a solid matrix into a liquid form.
3.1.1.1 Discussion—
During sample digestion or extraction, target analytes are extracted (solubilized) into solution to enable subsequent determination
by analytical techniques (for example, see Test Method E1613).
3.1.2 ultrasonic extraction—extraction, n—the use of ultrasonic energy and acidic or basic solution to extract targeted analytes
from samples.
3.1.2.1 Discussion—
The extract solution is subsequently analyzed for the determination of targeted analytes.
4. Summary of Practice
4.1 Samples of paint, settled dust (wipe or vacuum), soil, or airborne particles, obtained by ASTM sample collection methods (see
Practice E1729; Practice E1728, Practice D5438 and Practice D7144; Practice E1727, respectively), are subjected to ultrasonic
extraction in dilute nitric acid for a delineated time period.
4.2 Paint samples are ground, homogenized and weighed, if necessary, 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, airborne particulate and settled dust filter samples are weighed prior to ultrasonic extraction.
4.4.1 Preweighed filters assembled into closed-face cassettes as in NIOSH methods 0500 or 0600 (1) are used to collect airborne
particulate according to Test Method D6785 or to collect settled dust according to Practice D7144.
4.4.2 Closed-face cassettes using internal capsules as in NIOSH methods 0501, 5100, or 7306 (2) are used to collect airborne
particulate according to Test Method D6785 or to collect settled dust according to Practice D7144.
4.5 Sample extracts are diluted with ASTM Type I water (see Specification D1193) in preparation for subsequent determination
of lead by analytical techniques (for example Test Method E1613, Guide E1775, and NIOSH methods 7082, 7105, and 7300 (13) ).
4.6 This practice was developed based on an EPA standard operating procedure (ultrasonic extraction followed by colorimetric
lead analysis (24)) and published protocols (ultrasonic extraction followed by anodic stripping voltammetric determination of lead)
(35) (46).
The last approved version of this historical standard is referenced on www.astm.org.
The boldface numbers given in parentheses refer to a list of references at the end of the text.
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5. Significance and Use
5.1 Ultrasonic extraction using dilute nitric acid is a simpler and easier method for extracting lead from environmental samples
than are traditional digestion methods that employ hot plate or microwave digestion with concentrated acids (13), (35), (57), (68).
Hence, ultrasonic extraction may be used in lieu of the more rigorous strong acid/high temperature digestion methods (for example,
see Ref (13) and Test Method E1613), provided that the performance is demonstrated using accepted criteria as delineated in Guide
E1775.
5.2 In contrast with hot plate or microwave digestion techniques, ultrasonic extraction is field-portable, which allows for on-site
sample analysis.
6. Apparatus and Materials
6.1 Sonicator, 50 W minimum power; proper operation of the sonicator shall be confirmed prior to initial use and periodically
thereafter.
6.2 Plastic Centrifuge Tubes, 50 mL, with screw caps.
6.3 Analytical Balance, accuracy better than or equal to
60.002 g.
6.4 Mortar and Pestle, pug mill, or wigglebug.
6.5 Dry Ice (CO (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 shape of 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, and other volumes as needed.
NOTE 1—Precision digital mechanical pipettors using replaceable tips meet 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 μm.
6.14 Collection Tray.
6.15 Rubber Mallet.
6.16 Nylon Brush.
6.17 Aluminum Pie Tins.
E1979 − 21
6.18 Dust Mask.
6.19 Glass or Plastic Stirring Rods.
6.20 Aluminum Foil (conventional thickness for household use, that is, not heavy duty).
6.21 Graphite Pencil.
7. Reagents
7.1 ASTM Type I Water, in accordance with Specification D1193.
NOTE 2—Commercially available distilled or deionized water meets ASTM Type I water specifications.
7.2 Extraction Solution, 10 % or 25 % v/v HNO /H O; prepared from reagent grade concentrated nitric acid (70 to 71 % HNO )
3 2 3
and ASTM Type I water.
NOTE 3—Air filter samples require 10 % nitric acid (v/v) for extraction, while all other sample matrices require 25 % v/v HNO /H O.
3 2
8. Procedure
8.1 Testing of Sonicator:
8.1.1 Before use, ensure proper operation of the sonicator by employing the following diagnostic test.
8.1.1.1 Turn on the sonicator and allow for a reasonable warm-up period, as recommended by the instrument manufacturer.
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, graphite in solution will be observed streaming off the tip of the pencil.
8.1.2 Alternatively, demonstrate proper operation of the sonicator according to the following procedure:
8.1.2.1 Fill the sonicator bath with warm water (ca. 45 °C) to a level about half-full, and add a small amount (for example, three
drops) of surfactant
8.1.2.2 Turn on the sonicator for a minimum of 5 min to degas the solution. Turn off the sonicator.
1 3
8.1.2.3 Place aluminum foil (that is cut to a size conforming to ⁄2 to ⁄4 of the area of the bottom of the sonicator bath) on the
bottom of the sonicator bath. Lower the foil at an angle to prevent the trapping of air beneath the foil. Ensure that a narrow layer
of solution remains between the foil and the bottom of the sonicator bath. The foil shall be parallel and centered 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 foil should be observed to contain a myriad of small holes and bumps,
and may be torn apart. Also, the perforation observed should be uniform; that is, all portions of the foil should be observed to have
a high density of holes and perhaps tears. If the foil is not affected in this manner, then the sonicator performance is inadequate
for the purposes of this practice.
8.2 Dry Paint Film Samples:
NOTE 4—This practice assumes paint samples collected in accordance with Practice E1729.
8.2.1 Don a pair of gloves.
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8.2.1.1 If the desired reported lead concentration units are to be in terms of lead mass per unit area of sample, and the estimated
sample mass is greater than or equal to 0.25 g, then quantitatively transfer the entire sample to an analytical balance and weigh
to the nearest 60.002 g. Under these circumstances, do quantitative transfer and sample weighing prior to grinding and
homogenization as described later in this practice.
8.2.1.2 If the desired reporting units of lead concentration are to be in terms of lead mass per unit mass of sample, or if the desired
reporting units are to be in terms of lead mass per unit area and the estimated mass of the sample is less than 0.25 g, then
quantitatively transfer the sample to a mortar and pestle or a labeled 50 mL centrifuge tube. Use tweezers if necessary for
quantitative sample transfer. Clean tweezers before and after use with laboratory wipes.
8.2.2 Sample Grinding and Homogenization:
8.2.2.1 Grind and homogenize paint film sample to a fine powder using a mortar and pestle, pug mill, or wigglebug. Quantitatively
transfer the ground and homogenized a paint sample to a weighing vessel or weighing paper (see below). Thoroughly clean mortar
and pestle, wigglebug, or pug mill with moistened laboratory wipes prior to and following grinding, and then dry.
8.2.2.2 Alternatively, place paint film sample in a clean, dry 50 mL centrifuge tube, and place the tube in dry ice. Using a plastic
or metal rod, grind and homogenize the super-cooled, brittle paint sample to a fine powder. Thoroughly clean rod with laboratory
wipes prior to and following grinding procedure. Avoid condensation of water onto the sample by sealing the sample and allowing
it to warm to ambient temperature before weighing.
NOTE 5—The use of dry ice as described assists greatly in the grinding and homogenization of dry paint film samples.
8.2.3 If the total sample mass is greater than or equal to 0.25 g, or if the total sample mass is less than 0.25 g and the desired
reported lead concentration is to be in units of mass of lead per unit mass of sample, weigh 0.05 to 0.25 g of ground and
homogenized paint sample to the nearest 60.002 g, and record the sample mass.
NOTE 6—If the desired reporting units are to be in terms of mass of lead per unit area of sample, and the sample mass is estimated to be less than 0.25
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 the desired reported lead concentration is to be in terms of mass of lead per
unit area of collected sample, then the sample need not be weighed. However, the entire ground and homogenized sample must
be placed in the tube for extraction as described below.
8.2.5 Place the sample in a clean, dry, labeled 50 mL polypropylene centrifuge tube. To ensure quantitative sample transfer, rinse
materials used for transferring samples with a minimum of dilute (5 %) nitric acid, and direct the rinsate into the centrifuge tube.
8.2.6 Using a class A pipet, introduce 5 mL of 25 % HNO to the centrifuge tube containing the ground and homogenized paint
sample. Shake the centrifuge tube briefly to ensure that no solid paint material remains stuck to the bottom of the tube. Rinse the
inside of the centrifuge tube with a minimum quantity of 5 % HNO in order to ensure immersion of all solid material.
8.2.7 Cap the centrifuge tube, and place in an upright position in the sonicator bath.
8.2.8 Ensure that the bath of the sonicator contains enough water so that the water level is at least 2.5 cm above the level of liquid
within the centrifuge tube.
8.2.9 Repeat steps 8.2.1 – 8.2.8 as needed, depending on the size of the ultrasonic bath and the number of samples.
NOTE 7—Depending on the size of the sonicator, many centrifuge tubes may be immersed in the bath at one time. A custom rack for the centrifuge tubes
may be purchased or constructed to allow for the regular and orderly placement of multiple tubes in the sonicator bath.
8.2.10 Apply ultrasonic energy to the crushed and acidified samples within the immersed centrifuge tubes for at least 30 min.
8.2.11 Remove centrifuge tubes from the bath. Keep tubes in upright position.
E1979 − 21
8.2.12 Remove caps from centrifuge tubes that contain samples that were subjected to ultrasonic agitation, and dilute acidified
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, and allow the contents to settle. The samples are now ready for analysis for
lead content.
NOTE 8—The sample solutions may require filtration or centrifugation prior to analysis.
8.3 Settled Dust Wipe Samples:
NOTE 9—This procedure assumes dust wipe samples were collected in accordance with Practice E1728 using wipes that conform to Specification E1792.
8.3.1 Don a pair of gloves.
8.3.2 If not already placed in a labeled 50 mL centrifuge tube, remove the wipe sample from the sample container with a pair of
clean tweezers, and place it in a labeled clean and dry 50 mL centrifuge tube. Shove the wipe to the bottom of the tube with a clean
glass or plastic rod. Rinse the original sample container (if applicable), tweezers and rod with a minimum of dilute (5 %) nitric
acid to ensure quantitative sample transfer; make sure that the rinsate falls into the centrifuge tube. Clean tweezers and rods before
and after use with laboratory wipes.
8.3.3 Using a class A pipet, introduce 15 mL of 25 % HNO to the centrifuge tube containing the wipe sample, and cap the tube.
If needed, add more diluted 25 % HNO in 5 mL aliquots to ensure that the wipe is completely covered by acid extraction solution.
If bubbles are observed inside of the immersed wipe, apply pressure to the wipe with a clean stirring rod in order to force the
bubbles up and out.
8.3.4 Place centrifuge tube (containing wipe sample immersed in dilute acid) upright in the sonicator bath, and ensure that the
water level in the bath is at least 2.5 cm above the liquid level within the tube.
8.3.5 Repeat 8.3.1 – 8.3.4 for successive samples as needed, depending on the size of the ultrasonic bath.
NOTE 10—Depending on the size of the sonicator, many centrifuge tubes may be immersed in the bath at one time. A custom rack for the centrifuge tubes
may be purchased or constructed to allow for the regular and orderly placement of multiple tubes in the sonicator bath.
8.3.6 Apply ultrasonic energy to the acid-immersed wipe sample for at least 20 min.
8.3.7 Turn off the sonicator.
8.3.8 Carefully uncap each centrifuge tube.
8.3.9 Using a clean glass or plastic stirring rod for each sample, push down on each wipe within each centrifuge tube in order to
force bubbles (formed during sonication) up and out.
8.3.10 Recap the tubes.
8.3.11 Apply ultrasonic energy again for a minimum of 20 min.
NOTE 11—Longer extraction periods may be required for wipe samples. Quantitative recoveries from spiked w
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