ASTM E1644-98
(Practice)Standard Practice for Hot Plate Digestion of Dust Wipe Samples for the Determination of Lead
Standard Practice for Hot Plate Digestion of Dust Wipe Samples for the Determination of Lead
SCOPE
1.1 This practice covers the acid digestion of settled dust samples (collected using wipe sampling practices) and associated quality control (QC) samples for the determination of lead using laboratory atomic spectrometry analysis techniques such as Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES), Flame Atomic Absorption Spectrometry (FAAS), and Graphite Furnace Atomic Absorption Spectrometry (GFAAS).
1.2 This practice is based on U.S. EPA SW846 Method 3050, NIOSH 7082 and NIOSH 7105.
1.3 This practice contains notes which are explanatory and not part of mandatory requirements of the standard.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E 1644 – 98
Standard Practice for
Hot Plate Digestion of Dust Wipe Samples for the
Determination of Lead
This standard is issued under the fixed designation E 1644; 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 3.1.1 batch—a group of field or quality control (QC)
samples that are processed together using the same reagents
1.1 This practice covers the acid digestion of settled dust
and equipment.
samples (collected using wipe sampling practices) and associ-
3.1.2 certified reference material (CRM)—reference mate-
ated quality control (QC) samples for the determination of
rial accompanied by a certificate, of which one or more of its
lead.
property values are certified by a procedure that establishes its
1.2 This practice is based on U.S. EPA SW846 Method
traceability to an accurate realization of the unit in which the
3050, NIOSH 7082 and NIOSH 7105.
property values are expressed. E 1724
1.3 This practice contains notes which are explanatory and
3.1.3 digestate—an acidified aqueous solution that results
not part of mandatory requirements of the standard.
from digestion of the sample.
2. Referenced Documents
3.1.4 digestion—the sample preparation process that solu-
bilizes (extracts) targeted analytes present in the sample and
2.1 ASTM Standards:
results in an acidified aqueous solution called the digestate;
D 1129 Terminology Relating to Water
equivalent to extraction.
D 1193 Specification for Reagent Water
3.1.5 dust wipe sample—a settled dust sample collected on
E 1605 Terminology Relating to Abatement of Hazards
a moistened disposable towellette (see wipe).
from Lead-Based Paint in Buildings and Related Struc-
3.1.6 extraction—the dissolution of target analytes from a
tures
solid matrix into a liquid form. During sample digestion, target
E 1724 Guide for Testing and Certification of Reference
analytes are extracted (solubilized) into an acid solution.
Materials
3.1.7 method blank—a digestate that reflects the maximum
E 1792 Specification for Wipe Sampling Materials for Lead
treatment given any one sample within a sample batch except
in Surface Dust
that only the sampling medium (such as a blank wipe) is
2.2 Other Documents:
initially placed into the digestion vessel. (The same reagents
EPA SW 846, Method 3050, “Acid Digestion of Sediments,
and processing conditions that are applied to field samples
Sludges, and Soils.” This method is found in Test Methods
within a batch are also applied to the method blanks.) Analysis
for Evaluating Solid Waste, Physical/Chemical Methods,
results from method blanks provide information on the level of
U.S. EPA SW 846, 3rd Edition, Revision 1, 1987
potential contamination resulting from the laboratory and
NIOSH Manual of Analytical Methods, NIOSH 7082 and
sampling medium sources that are experienced by samples
7105, Eller, P.M., Ed., 3rd ed., 1984
processed within the batch.
3. Terminology
3.1.8 non-spiked sample—a blank wipe sample that was
targeted for addition of analyte but was not fortified with all the
3.1 Definitions—For definitions of terms relating to this
target analytes before sample preparation.
practice that do not appear in this section, refer to Terminology
3.1.8.1 Discussion—For wipe samples, a non-spiked
D 1129 and E 1605.
sample is equivalent to a method blank. Analysis results for
this sample are used to correct for background levels in the
This practice is under the jurisdiction of ASTM Committee E-6 on Performance
blank wipes used for spiked and spiked duplicate samples.
of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead Paint
3.1.9 reagent blank—a digestate that reflects the maximum
Abatement.
treatment given any one sample within a sample batch except
Current edition approved June 10, 1998. Published March 1999. Originally
published as E 1644 – 94. Last previous edition E 1644 – 94. that it has no sample initially placed into the digestion vessel.
Annual Book of ASTM Standards, Vol 11.01.
(The same reagents and processing conditions that are applied
Annual Book of ASTM Standards, Vol 04.11.
to field samples within a batch are also applied to the reagent
Annual Book of ASTM Standards, Vol 03.06.
blank.)
Available from National Technical Information Service, 5285 Port Royal Rd.,
Springfield, VA 22161.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1644
3.1.9.1 Discussion—Analysis results from reagent blanks that all reagents conform to the specifications of the Committee
provide information on the level of potential contamination on Analytical Reagents of the American Chemical Society,
resulting from only laboratory sources that are experienced by where such specifications are available. Other grades may be
samples processed within the batch. used, provided it is first ascertained that the reagent is of
3.1.10 spiked sample and spiked duplicate sample—a sufficiently high purity to permit its use without lessening
spiked sample (or spiked duplicate sample) is a blank wipe that accuracy of the determination.
is spiked with a known amount of analyte before preparation. 7.2 Nitric Acid—Concentrated, suitable for atomic spec-
3.1.10.1 Discussion—Analysis results for these samples are trometry analysis such as spectroscopic grade.
used to provide information on accuracy and precision of the 7.3 Hydrogen Peroxide—30 % (w/w), suitable for atomic
overall analysis process. spectrometry analysis such as spectroscopic grade.
3.1.11 wipe—a disposable, porous paper (cellulosic) tow- 7.4 Purity of Water—Unless otherwise indicated, references
ellette that is moistened with a wetting agent. E 1792 to water shall be understood to mean reagent water as defined
by Type 1 of Specification D 1193.
4. Summary of Practice
7.5 Calibration Stock Solution—100 μg/mL of Pb in dilute
4.1 A dust wipe sample is digested using hot plate type
nitric acid.
heating with nitric acid and hydrogen peroxide. The digestate
is diluted for final volume prior to lead measurement.
8. Sample Preparation Procedure
8.1 Sample Extraction:
5. Significance and Use
8.1.1 Treat each sample in a batch equally.
5.1 This practice is intended for the determination of lead in
8.1.2 Quantitatively transfer the contents of the sample
dust wipe samples that have been collected during various
container to the labeled beaker as described as follows:
construction and renovation practices in and around buildings
8.1.2.1 For blank wipe targeted for spiking (see Section 9),
and related structures.
add the appropriate volume of a lead standard stock to the
5.2 This practice is not capable of determining lead bound
beaker (see Note 2). In the absence of other information, add
within matrices, such as silica, that are not soluble in nitric
200 μg of lead to each beaker containing the blank wipes
acid.
targeted for spike duplicates (2 mL of 100 μg/mL Pb stock
5.3 This practice is capable of determining lead bound
solution).
within paint.
NOTE 2—The appropriate volume will be dependent on the anticipated
6. Apparatus and Materials
average lead level in the wipe samples within a given batch. The optimum
spike addition is one that will match the average lead level in the batch of
6.1 Borosilicate Glassware:
wipes. Use of multiple spike levels such as 400 μg and 800 μg may also
6.1.1 Class A Volumetric Flasks with Stoppers, 100 mL and
be useful for sample batches containing a wide range of lead levels.
other sizes needed to make serial dilutions,
8.1.2.2 Carefully open the container containing the wipe
6.1.2 Griffın Beakers, 150 mL or 250 mL,
sample, remove the folded wipe using a new pair of plastic
6.1.3 Watch Glasses, sized to cover Griffin beakers,
gloves or plastic forceps, or both, and place it into a labeled
6.1.4 Class A Pipets, as needed to make serial dilutions, and
Griffin Beaker.
6.1.5 Glass Rods.
8.1.2.3 If the sample container is a plastic centrifuge tube,
6.2 Funnels—Plastic or porcelain or borosilicate funnels
then rinse out the inside of the container into the beaker with
sized to fit into a 100-mL volumetric flask.
two small volumes (2 to 3 mL) of water using a squirt bottle
6.3 Filter Paper—Fast filtering, suitable for metals analysis.
filled with ASTM Type I water.
6.4 Thermometers—Red alcohol or thermocouple, that cov-
8.1.2.4 If the sample container is a plastic bag and material
ers a range of 0 to 150°C.
appears to be left behind in the container and the sample
6.5 Electric Hot Plate—Suitable for operation at tempera-
container, then attempt to transfer the material into the beaker
tures up to at least 100°C as measured by a thermometer inside
using shaking or mechanical removal with a clean laboratory
a solution-filled container placed on the surface of the hot plate
tool such as a spatula. Document observations in laboratory
(see Note 1) or a hot plate surface temperature of up to 150°C.
records of
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