ASTM E1979-98

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Designation: E 1979 – 98
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 E 1979; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 1727 Practice for Field Collection of Soil Samples for
Lead Determination
1.1 This practice covers an ultrasonic extraction procedure
E 1728 Practice for Field Collection of Settled Dust
for the extraction of lead from environmental samples of
Samples Using Wipe Sampling Methods for Lead Deter-
interest in lead abatement and renovation (or related) work, for
mination
analytical purposes.
E 1729 Practice for Field Collection of Dried Paint Samples
1.2 Environmental matrices of concern here include dry
for Lead Determination
paint films, settled dusts, soils, and air particulates.
E 1775 Guide for Evaluating the Performance of On-Site
1.3 Samples subjected to ultrasonic extraction are prepared
Extraction and Field-Portable Electrochemical or Spectro-
for subsequent determination of lead by laboratory analytical
photometric Analysis for Lead
methods.
E 1792 Specification for Wipe Sampling Materials for Lead
1.4 This practice includes, where applicable, descriptions of
in Surface Dust
procedures for sample homogenization and weighing prior to
PS 46 Provisional Practice for the Collection of Surface
ultrasonic extraction.
Dust by Air Sampling Pump Vacuum Technique for Sub-
1.5 The values stated in SI units are to be regarded as the
sequent Lead Determination
standard.
1.6 This practice does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions: For definitions of terms relating to this
responsibility of the user of this practice to establish appro-
practice that do not appear in this section, refer to Terminology
priate safety and health practices and determine the applica-
E 1605.
bility of regulatory limitation prior to use.
3.1.1 extraction—the dissolution of target analytes from a
2. Referenced Documents solid matrix into a liquid form.
3.1.1.1 Discussion—During sample digestion or extraction,
2.1 ASTM Standards:
2 target analytes are extracted (solubilized) into solution to
D 1193 Specification for Reagent Water
enable subsequent determination by analytical techniques (for
D 5438 Practice for Collection of Floor Dust for Chemical
3 example, see Test Method E 1613).
Analysis
3.1.2 ultrasonic extraction—the use of ultrasonic energy
E 1553 Practice for Collection of Airborne Particulate Lead
4 and acidic or basic solution to extract targeted analytes from
During Abatement and Construction Activities
samples.
E 1605 Terminology Relating to Abatement of Lead Haz-
4 3.1.2.1 Discussion—The extract solution is subsequently
ards
analyzed for the determination of targeted analytes.
E 1613 Test Method for the Analysis of Digested Samples
for Lead Determination by Atomic Spectrometry
4. Summary of Practice
E 1726 Practice for Sample Digestion of Soils for Lead
4.1 Samples of paint, settled dust (wipe or vacuum), soil, or
Determination
air particulate, obtained by ASTM sample collection methods
(see Specification E 1729; Practice E 1728, Practice D 5438
This practice is under the jurisdiction of ASTM Committee E-6 on Performance and Provisional Practice PS 46; Practice E 1727; and Practice
of Buildings and is the direct responsibility of Subcommittee E06.23 on Abatement
E 1553, respectively), are subjected to ultrasonic extraction in
of Lead Hazards.
dilute nitric acid for a delineated time period.
Current edition approved Sept. 10, 1998. Published March 1999. Formerly PS
4.2 Paint samples are ground, homogenized and weighed, if
87–97.
Annual Book of ASTM Standards, Vol 11.01.
necessary, prior to ultrasonic extraction.
Annual Book of ASTM Standards, Vol 11.03.
Annual Book of ASTM Standards, Vol 04.07.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1979
meet Class A requirements.
4.3 Soil and bulk dust vacuum samples are sieved, homog-
enized and weighed prior to ultrasonic extraction.
6.13 Laboratory Wipes, wet or dry, or both.
4.4 If applicable, dust filter samples are weighed prior to
6.14 Power Source for Sonicator.
ultrasonic extraction.
6.15 Sieves, Number 10 (1.9 mm) and 250 μm.
4.5 Sample extracts are diluted with ASTM Type I water
6.16 Collection Tray.
(see Specification D 1193) in preparation for subsequent deter-
6.17 Rubber Mallet.
mination of lead by analytical techniques (for example Test
6.18 Nylon Brush.
Method E 1613, Guide E 1775, and NIOSH methods 7082,
6.19 Aluminum Pie Tins.
7105, and 7300 (1) ).
6.20 Dust Mask.
4.6 This practice was developed based on an EPA standard
6.21 Glass or Plastic Stirring Rods.
operating procedure (ultrasonic extraction followed by colori-
6.22 Aluminum Foil (conventional thickness for household
metric lead analysis (2)) and published protocols (ultrasonic
use, that is, not heavy duty).
extraction followed by anodic stripping voltammetric determi-
nation of lead) (3)(4).
7. Procedure
5. Significance and Use
7.1 Testing of Sonicator:
5.1 Ultrasonic extraction using dilute nitric acid is a simpler
7.1.1 Quarterly Testing—Before initial use and at least
and easier method for extracting lead from environmental
quarterly thereafter, test ultrasonic extraction of lead from a
samples than are traditional digestion methods that employ hot
bulk solid performance evaluation material that is traceable to
plate or microwave digestion with concentrated acids (1), (3),
a primary standard (for example, National Institute of Stan-
(5), (6). Hence, ultrasonic extraction may be used in lieu of the
dards and Technology Standard Reference Materials, NIST
more rigorous strong acid/high temperature digestion methods
SRMs) using the sonicator in the following manner:
(for example, see Ref (1) and Test Method E 1613), provided
7.1.1.1 Add a weighed amount of performance evaluation
that the performance is demonstrated using accepted criteria as
material (0.05 to 0.5 6 0.002 g) to a minimum of six 50 mL
delineated in Guide E 1775.
centrifuge tubes. Wear gloves while weighing is conducted.
5.2 In contrast with hot plate or microwave digestion
7.1.1.2 Introduce nitric acid, either 5 mL of 25 % nitric acid
techniques, ultrasonic extraction is field-portable, which allows
or 10 mL of 10 % to 25 % HNO , to each centrifuge tube
for on-site sample preparation.
containing weighed performance evaluation material, and the
tubes capped.
6. Apparatus and Materials
7.1.1.3 Shake the centrifuge tubes briefly to ensure that no
6.1 Sonicator, 50 W minimum power; proper operation of
solid material remains stuck to the bottom of the tubes.
the sonicator shall be confirmed prior to initial use and
7.1.1.4 Place the centrifuge tubes in the sonicator in an
periodically thereafter.
upright position, and add water to the sonicator bath to a level
6.2 Plastic Centrifuge Tubes, 50 mL, with screw caps.
at least 2.5 cm above the level of liquid within the tubes.
6.3 Analytical Balance, accuracy better than or equal to
7.1.1.5 Turn on the sonicator for a period of at least 30 min
6 0.002 g.
to effect ultrasonic extraction of lead from the performance
6.4 Mortar and Pestle, pug mill, or wigglebug.
evaluation materials immersed in diluted nitric acid.
6.5 Dry Ice (CO (s)).
7.1.1.6 Then remove the centrifuge tubes from the sonicator
6.6 Cooler, for storage of dry ice.
bath.
6.7 Plastic or Glass Rods, 0.6 to 1.0 cm diameter,
7.1.1.7 Uncap the centrifuge carefully, and add ASTM Type
15 to 20 cm length; tapered at one end to conform to the shape
I water to effect a final volume within the tubes of 50 mL.
of the bottoms of the 50 mL centrifuge tubes.
Shake tubes and allow to settle. The performance evaluation
6.8 ASTM Type I Water, in accordance with Specification
samples are now ready for the contents.
D 1193.
NOTE 3—The sample solutions may require filtration or centrifugation
NOTE 1—Commercially available distilled or deionized water meets
prior to analysis.
ASTM Type I water specifications.
6.9 Extraction Solution,10to25% v/v HNO /H 0; pre- 7.1.1.8 Determine lead in the performance evaluation
3 2
pared from reagent grade concentrated nitric acid (70 to 71 %
samples according to Test Method E 1613 or an equivalent
HNO ) and ASTM Type I water. method.
6.10 Powderless Plastic Gloves.
7.1.1.9 The lead concentration as determined in 7.1.1.8
6.11 Tweezers.
must be within 100 6 20 % of the certified lead concentration
6.12 Class A Pipets, 5 or 10 mL or both, and other volumes
in the performance evaluation material (see Guide E 1775). If
as needed.
the lead recovery determined is outside this range, the sonica-
tor performance does not meet the requirements of this
NOTE 2—Precision digital mechanical pipettors using replaceable tips
standard.
7.1.2 Monthly Testing—At least monthly, demonstrate
proper operation of the sonicator according to the following
The boldface numbers given in parentheses refer to a list of references at the
end of the text. procedure:
E 1979
7.1.2.1 Fill the sonicator bath with warm water (ca. 45°C) to 7.2.3 If the total sample mass is greater than or equal to 0.25
a level about half-full, and add a small amount (for example, g, or if the total sample mass is less than 0.25 g and the desired
three drops) of surfactant reported lead concentration is to be in units of mass of lead per
7.1.2.2 Turn on the sonicator for a minimum of 5 min to unit mass of sample, weigh 0.05 to 0.25 g of ground and
degas the solutions. Turn off the sonicator. homogenized paint sample to the nearest 6 0.002 g, and record
7.1.2.3 Place aluminum foil (that is cut to a size conforming the sample mass.
1 3
to ⁄2 to ⁄4 of the area of the bottom of the sonicator bath) on
NOTE 6—If the desired reporting units are to be in terms of mass of lead
the bottom of the sonicator bath. Lower the foil at an angle to
per unit area of sample, and the sample mass is estimated to be less than
prevent the trapping of air beneath the foil. Ensure that a
0.25 g, a larger sample may be collected in order to obtain more mass
narrow layer of solution remains between the foil and the (thereby enabling the sample to be treated as described in 7.2.1.1).
bottom of the sonicator bath. The foil shall be parallel and
7.2.4 If the total sample mass is less than 0.25 g and the
centered to the bottom of the sonicator.
desired reported lead concentration is to be in terms of mass of
7.1.2.4 Turn on the sonicator for a period of 45 s.
lead per unit area of collected sample, then the sample need not
7.1.2.5 Examine the aluminum foil after sonication. The foil
be weighed. However, the entire ground and homogenized
should be observed to contain a myriad of small holes and
sample must be placed in the tube for extraction as described
bumps, and may be torn apart. Also, the perforation observed
below.
should be uniform; that is, all portions of the foil should be
7.2.5 Place sample in a clean, dry, labeled 50 mL polypro-
observed to have a high density of holes and perhaps tears. If
pylene centrifuge tube. To ensure quantitative sample transfer,
the foil is not affected in this manner, then the sonicator
rinse materials used for transferring samples with a minimum
performance is inadequate for the purposes of this practice.
of dilute (5 %) nitric acid, and direct the rinsate into the
7.2 Dry Paint Film Samples:
centrifuge tube.
NOTE 4—This practice assumes paint samples collected in accordance
7.2.6 Using a class A pipet, introduce 10 mL of 10 to 25 %
with Practice E 1729.
HNO or5mLof25 %HNO to the centrifuge tube containing
3 3
7.2.1 Don a pair of gloves. the ground and homogenized paint sample. Shake the centri-
7.2.1.1 If the desired reported lead concentration units are to fuge tube briefly to ensure that no solid paint material remains
be in terms of lead mass per unit area of sample, and the
stuck to the bottom of the tube. Rinse the insides of the
estimated sample mass is greater than or equal to 0.25 g, then centrifuge tube with a minimum quantity of 5 % HNO in order
quantitatively transfer the entire sample to an analytical bal-
to ensure immersion of all solid material.
ance and weigh to the nearest 6 0.002 g. Under these 7.2.7 Cap the centrifuge tube, and place in an upright
circumstances, do quantitative transfer and sample weighing
position in the sonicator bath.
prior to grinding and homogenization as described later in this
7.2.8 Ensure that the bath of the sonicator contains enough
practice.
water so that the water level is at least 2.5 cm above the level
7.2.1.2 If the desired reporting units of lead concentration of liquid within the centrifuge tube.
are to be in terms of lead mass per unit mass of sample, or if
7.2.9 Repeat steps 7.2.1-7.2.8 as needed, depending on the
the desired reporting units are to be in terms of lead mass per
size of the ultrasonic bath and the number of samples.
unit area and the estimated mass of the sample is less than 0.25
NOTE 7—Depending on the size of the sonicator, many centrifuge tubes
g, then quantitatively transfer the sample to a mortar and pestle
may be immersed in the bath at one time. A custom rack for the centrifuge
or a labeled 50 mL centrifuge tube. Use tweezers if necessary
tubes may be purchased or constructed to allow for the regular and orderly
for quantitative sample transfer. Clean tweezers before and
placement of multiple tubes in the sonicator bath.
after use with laboratory wipes.
7.2.10 Apply ultrasonic energy to the crushed and acidified
7.2.2 Sample Grinding and Homogenization:
samples within the immersed centrifuge tubes for at least 30
7.2.2.1 Grind and homogenize paint film sample to a fine
min.
powder using a mortar and pestle, pug mill, or wigglebug.
7.2.11 Remove centrifuge tubes from the bath. Keep tubes
Quantitatively transfer the ground and homogenized paint
in upright position.
sample to a weighing vessel or weighing paper (see below).
7.2.12 Remove caps from centrifuge tubes that contain
Thoroughly clean mortar and pestle, wigglebug, or pug mill
samples that were subjected to ultrasonic agitation, and dilute
with moistened laboratory wipes prior to and following grind-
acidified extracts to the 50 mL mark with ASTM Type I water.
ing, and then dry.
7.2.13 Re-cap and then shake the tubes for 5 to 10 s, and
7.2.2.2 Alternatively, place paint film sample in a clean, d
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