Designation: E 1644 – 98

Standard Practice for

Hot Plate Digestion of Dust Wipe Samples for the
Determination of Lead1
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)

1.1 This practice covers the acid digestion of settled dust samples that are processed together using the same reagents
samples (collected using wipe sampling practices) and associ- and equipment.
ated quality control (QC) samples for the determination of 3.1.2 certified reference material (CRM)—reference mate-
lead. rial accompanied by a certificate, of which one or more of its
1.2 This practice is based on U.S. EPA SW846 Method property values are certified by a procedure that establishes its
3050, NIOSH 7082 and NIOSH 7105. traceability to an accurate realization of the unit in which the
1.3 This practice contains notes which are explanatory and property values are expressed. E 1724
not part of mandatory requirements of the standard. 3.1.3 digestate—an acidified aqueous solution that results
from digestion of the sample.
2. Referenced Documents 3.1.4 digestion—the sample preparation process that solu-
2.1 ASTM Standards: bilizes (extracts) targeted analytes present in the sample and
D 1129 Terminology Relating to Water2 results in an acidified aqueous solution called the digestate;
D 1193 Specification for Reagent Water2 equivalent to extraction.
E 1605 Terminology Relating to Abatement of Hazards 3.1.5 dust wipe sample—a settled dust sample collected on
from Lead-Based Paint in Buildings and Related Struc- a moistened disposable towellette (see wipe).
tures3 3.1.6 extraction—the dissolution of target analytes from a
E 1724 Guide for Testing and Certification of Reference solid matrix into a liquid form. During sample digestion, target
Materials4 analytes are extracted (solubilized) into an acid solution.
E 1792 Specification for Wipe Sampling Materials for Lead 3.1.7 method blank—a digestate that reflects the maximum
in Surface Dust3 treatment given any one sample within a sample batch except
2.2 Other Documents: that only the sampling medium (such as a blank wipe) is
EPA SW 846, Method 3050, “Acid Digestion of Sediments, initially placed into the digestion vessel. (The same reagents
Sludges, and Soils.” This method is found in Test Methods and processing conditions that are applied to field samples
for Evaluating Solid Waste, Physical/Chemical Methods, within a batch are also applied to the method blanks.) Analysis
U.S. EPA SW 846, 3rd Edition, Revision 1, 19875 results from method blanks provide information on the level of
NIOSH Manual of Analytical Methods, NIOSH 7082 and potential contamination resulting from the laboratory and
7105, Eller, P.M., Ed., 3rd ed., 19845 sampling medium sources that are experienced by samples
processed within the batch.
3. Terminology 3.1.8 non-spiked sample—a blank wipe sample that was
3.1 Definitions—For definitions of terms relating to this targeted for addition of analyte but was not fortified with all the
practice that do not appear in this section, refer to Terminology target analytes before sample preparation.
D 1129 and E 1605. 3.1.8.1 Discussion—For wipe samples, a non-spiked
sample is equivalent to a method blank. Analysis results for
this sample are used to correct for background levels in the
1
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
Abatement.
3.1.9 reagent blank—a digestate that reflects the maximum
Current edition approved June 10, 1998. Published March 1999. Originally treatment given any one sample within a sample batch except
published as E 1644 – 94. Last previous edition E 1644 – 94. that it has no sample initially placed into the digestion vessel.
2
Annual Book of ASTM Standards, Vol 11.01. (The same reagents and processing conditions that are applied
3
Annual Book of ASTM Standards, Vol 04.11.
4
Annual Book of ASTM Standards, Vol 03.06.
to field samples within a batch are also applied to the reagent
5
Available from National Technical Information Service, 5285 Port Royal Rd., blank.)
Springfield, VA 22161.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

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 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.6 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 1193.7
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
5. Significance and Use 8.1 Sample Extraction:
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
6.1 Borosilicate Glassware: spike addition is one that will match the average lead level in the batch of
6.1.1 Class A Volumetric Flasks with Stoppers, 100 mL and wipes. Use of multiple spike levels such as 400 µg and 800 µg may also
be useful for sample batches containing a wide range of lead levels.
other sizes needed to make serial dilutions,
6.1.2 Griffın Beakers, 150 mL or 250 mL, 8.1.2.2 Carefully open the container containing the wipe
6.1.3 Watch Glasses, sized to cover Griffin beakers, sample, remove the folded wipe using a new pair of plastic
6.1.4 Class A Pipets, as needed to make serial dilutions, and gloves or plastic forceps, or both, and place it into a labeled
6.1.5 Glass Rods. Griffin Beaker.
6.2 Funnels—Plastic or porcelain or borosilicate funnels 8.1.2.3 If the sample container is a plastic centrifuge tube,
sized to fit into a 100-mL volumetric flask. then rinse out the inside of the container into the beaker with
6.3 Filter Paper—Fast filtering, suitable for metals analysis. two small volumes (2 to 3 mL) of water using a squirt bottle
6.4 Thermometers—Red alcohol or thermocouple, that cov- filled with ASTM Type I water.
ers a range of 0 to 150°C. 8.1.2.4 If the sample container is a plastic bag and material
6.5 Electric Hot Plate—Suitable for operation at tempera- appears to be left behind in the container and the sample
tures up to at least 100°C as measured by a thermometer inside container, then attempt to transfer the material into the beaker
a solution-filled container placed on the surface of the hot plate using shaking or mechanical removal with a clean laboratory
(see Note 1) or a hot plate surface temperature of up to 150°C. tool such as a spatula. Document observations in laboratory
records of potential lost sample remaining in the container for
NOTE 1—Provided that the hot plate is capable of handling the extra
later reporting with laboratory analysis results. Due to the
heating required, use of a 12 to 25-mm (0.5 to 1-in.) thick aluminum plate
placed on the burner head can help reduce the presence of hot spots difficulty in performing quantitative transfers from plastic bags
common to electric hot plates. for some samples, hard containers such as plastic 50-mL
centrifuge tubes are recommended for sample collection.
6.6 Vinyl Gloves—Powderless.
6.7 Micropipettors with Disposable Plastic Tips—Sizes
needed to make reagent additions, and spike standards. In
general, the following sizes should be readily available: 1 to 5 6
Reagent Chemicals, American Chemical Society Specifications, American
mL adjustable, 1000 µL, 500 µL, 250 µL, and 100 µL. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
7. Reagents Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
7.1 Purity of Reagents—Reagent grade chemicals shall be MD.
used in this practice. Unless otherwise indicated, it is intended 7
ASTM Type I Water: Minimum resistance of 16.67 megohm-cm, or equivalent.

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 E 1644
8.1.3 Add 25 mL of 1 : 1 nitric acid : water to each beaker, NOTE 6—The sample media (wipe material) may or may not be
gently swirl to mix, and cover with a watchglass. Gently heat completely solubilized. Many types of wipes contain materials that do not
the sample to 85°C to 100°C and reflux for 10 to 15 min dissolve in nitric acid. If a large amount of undissolved material remains,
rinse the solids as many times as possible to transfer solubilized lead into
without boiling. Monitor the temperature by having a ther- the volumetric flask.
mometer inside a beaker or flask containing a small volume of NOTE 7—Some wipes leave a significant amount of residue. It may be
water on the hot plate. necessary to filter the digestate before dilution in order to remove this
NOTE 3—A hot plate surface temperature of 120 to 140°C will yield a material.
sample digestate temperature of 85 to 100°C.
9. Quality Assurance
8.1.4 Using a glass rod, push the wipe down into the
digestion solution periodically to effect efficient extraction. 9.1 Quality Control Samples—Quality control samples to
CAUTION—Some wipes break down into a gelatinous residue process with each batch of samples are summarized in Table 1.
that readily bumps or spatters, or both. Heating should be 9.1.1 Reagent Blanks—Carry reagent blanks (water and
slowed with these materials. reagents) throughout the entire sample preparation and analyti-
8.1.5 Allow the sample to cool to near room temperature, cal process to determine if the samples are being contaminated
add 10 mL of concentrated nitric acid, replace the watch glass, from laboratory activities. Process reagent blanks according to
and reflux for 30 min without boiling. the frequency listed in Table 1.
8.1.6 Remove the watchglass and allow the solution to 9.1.2 Non-Spiked Samples, Spiked Samples and Spiked Du-
evaporate to approximately 10 mL without boiling (see Notes plicate Samples—Process non-spiked, spiked and spiked du-
4 and 5). Allow the sample to cool to near room temperature plicate samples on a routine basis to estimate method accuracy
after evaporation to approximately 10 mL. on the sample batch, expressed as percent recovery relative to
the true spiked value. Since wipe samples cannot be split
NOTE 4—Exercise care when removing watch glasses. Avoid lead
uniformly, blank wipes are used for non-spike, spikes and spike
contamination problems by placing them upside down on new clean
laboratory wipes. duplicates. The brand or type of wipe used should be the same
NOTE 5—Boiling of the sample should be avoided because of potential as that used for the collection of the samples. Field personnel
sample splattering losses and cross-contamination problems. The same should submit sufficient numbers of blank wipes to the labo-
problems can be experienced if samples are allowed to evaporate to ratory to permit generation of these QC samples at the
dryness. frequency listed in Table 1.
8.1.7 After the sample has cooled to near room temperature, 9.1.3 Certified Reference Materials—Process certified or
add 5 mL of water and 5 mL of 30 % hydrogen peroxide. Cover Standard Reference Materials (CRMs) on a routine basis to
the beaker with a watchglass and return the covered beaker to determine an estimate of method accuracy on the sample batch,
the hot plate for warming and to start the peroxide reaction. expressed as percent recovery relative to the certified value.
Take care to ensure that losses do not occur due to excessively Incorporate SRMs or CRMs into each analytical batch accord-
vigorous effervescence during heating. Heat until efferves- ing to the frequency listed in Table 1. Use a CRM that has a
cence subsides and cool the beaker to near room temperature. matrix similar or identical to dust with a certified lead
8.1.8 Remove the watchglass and continue heating the concentration level. Place a known quantity of the CRM into a
acid-peroxide digestate carefully until the volume has been blank wipe and process along with other samples. The brand or
reduced to approximately 10 mL (see Notes 4 and 5). type of wipe used should be the same as that used for the
8.1.9 Allow the digestates to cool to near room temperature, collection of the samples. Field personnel should submit
rinse the beaker walls and bottom of the watchglass with water, sufficient numbers of blank wipes to the laboratory to generate
and quantitatively transfer through a funnel equipped with a these QC samples.
fast filter into a 100-mL volumetric flask (see Note 6). Dilute 9.2 Laboratory Records—Record all information regarding
to volume with water and swirl to mix. The diluted digestate the preparation of samples (both QC samples and those
solution contains approximately 10 % (v/v) nitric acid. Cali- submitted to the analyst) as follows:
bration standards used for instrumental measurement should be 9.2.1 Record all reagent sources (lot numbers) used for
made with this level of nitric acid. sample preparation. For each entry, include the date(s) and

TABLE 1 Quality Control Samples

QC samples Definition Frequency
Method blank or Non-spiked sample A blank wipe carried through sample preparation along with other 1 per 20 samples, a minimum of 1
amples. Should reflect the maximum treatment given any one ample per batch
within the batch.
Reagent blank Type I water—digest as a sample with addition of all reagents. 1 per batch
Should reflect the maximum treatment given any one sample within
the batch.
Spiked sample A blank wipe fortified with all the target analytes before preparation. 1 per 20 samples, a minimum of 1
per batch
Spiked sample duplicate A blank wipe fortified with all the target analytes before preparation. 1 per 20 samples, a minimum of 1
per batch
Reference material A material of known composition where the analyte levels are 1 per batch of samples
certified by the manufacturer.

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 E 1644
identification and signature(s) of the person(s) making the incorrect entry, accompanied by the initials of the person
entry. Record any inadvertent deviations, unusual occurrences, making the correction, and the date of the correction.
or observations on a real-time basis as samples are processed.
Use the records to add supplemental information when report- 10. Keywords
ing results.
9.2.2 Laboratory notebooks must be bound with prenum- 10.1 digestion; lead; sample preparation; wipes
bered pages, and all entries must be made in ink. Any entry
errors must be corrected by using only a single line through the

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