ASTM E1644-21

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of the standard as published by ASTM is to be considered the official document.
Designation: E1644 − 17 E1644 − 21
Standard Practice for
Hot Plate Digestion of Dust Wipe Samples for the
Determination of Lead
This standard is issued under the fixed designation E1644; 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 the acid digestion of surface dust samples (collected using wipe sampling practices) and associated quality
control (QC) samples for the determination of lead.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exception—Informational inch-pound units are provided in Note 3.
1.3 This practice contains notes which are explanatory and not part of mandatory requirements of the standard.
1.4 This standard 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 standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.5 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:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
E1583 Practice for Evaluating Laboratories Engaged in Determination of Lead in Paint, Dust, Airborne Particulates, and Soil
Taken From and Around Buildings and Related Structures
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(Withdrawn 2021)
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, 2017Sept. 1, 2021. Published March 2017October 2021. Originally approved in 1994. Last previous edition approved in 20162017 as
ɛ1
E1644–04(2016)E1644 . DOI: 10.1520/E1644-17. – 17. DOI: 10.1520/E1644-21.
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.
The last approved version of this historical standard is referenced on www.astm.org.
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E1644 − 21
E1728E1728/E1728M Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Lead
Determination
E1792 Specification for Wipe Sampling Materials for Lead in Surface Dust
E2051 Practice for the Determination of Lead in Paint, Settled Dust, Soil and Air Particulate by Field-Portable Electroanalysis
(Withdrawn 2010)
E2239 Practice for Record Keeping and Record Preservation for Lead Hazard Activities
E3193 Test Method for Measurement of Lead (Pb) in Dust by Wipe, Paint, and Soil by Flame Atomic Absorption
Spectrophotometry (FAAS)
E3203 Test Method for Determination of Lead in Dried Paint, Soil, and Wipe Samples by Inductively Coupled Plasma-Optical
Emission Spectroscopy (ICP-OES)
2.2 Other Documents:
EPA SW 846, Method 3050,3050 “AcidAcid Digestion of Sediments, Sludges, and Soils.” This method is found in SoilsTest
Methods for Evaluating Solid Waste, Physical/Chemical Methods, U.S. EPA SW 846, 3rd Edition, Revision 1, 1987
NIOSH Manual of Analytical Methods, NIOSH 7082 and 7105, Eller, P.M., Ed., 3rd ed., 1984
3. Terminology
3.1 Definitions—For definitions of terms not appearing here, refer to Terminologies D1129, D1356, and E1605.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 blank wipe—wipe, n—an unused, unspiked dust wipe that is only removed from its packaging immediately before use.
3.2.1.1 Discussion—
Blank wipes are used to prepare non-spiked, spiked, and spiked duplicate quality assurance samples.
3.2.2 dust wipe sample—sample, n—surface dust collected on a wipe.
3.2.3 method blank—blank, n—a digestate that reflects the maximum treatment given any one sample within a sample batch except
that only the sampling medium (such as a blank wipe) is initially placed into the digestion vessel.
3.2.3.1 Discussion—
The same reagents and processing conditions that are applied to field samples within a batch are also applied to the method blanks
so that analysis results provide information on the level of potential contamination resulting from the laboratory and sampling
medium sources that are experienced by samples processed within the batch.
3.2.4 non-spiked sample—sample, n—a portion of a homogenized sample that was targeted for the addition of analyte but is not
fortified with the target analytes before sample preparation.
3.2.4.1 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 blank wipes used for spiked and spiked duplicate samples.
3.2.5 reagent blank—blank, n—a digestate that reflects the maximum treatment given any one sample within a sample batch
except that it has no sample placed into the digestion vessel.
3.2.5.1 Discussion—
The same reagents and processing conditions that are applied to field samples within a batch are also applied to the reagent blank
so that analysis results provide information on the level of potential contamination resulting from only laboratory sources that are
experienced by samples processed within the batch.
3.2.6 spiked sample and spiked duplicate sample—sample, n—a blank wipe that is spiked with a known amount of analyte (that
is, lead) before hot plate digestion and subsequent lead analysis.
3.2.6.1 Discussion—
Analysis results for these samples are used to provide information on accuracy and precision of the overall analysis process.
This method is found in Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, U.S. EPA SW 846, 3rd Edition, Revision 1, 1987. Available from National
Technical Information Service (NTIS), 5301 Shawnee Rd., Alexandria, VA 22312, http://www.ntis.gov.
E1644 − 21
4. Summary of Practice
4.1 A dust wipe sample is digested using hot plate type heating with nitric acid and hydrogen peroxide. The digestate is diluted
to final volume prior to lead measurement.
NOTE 1—The procedure in this practice is based on U.S. EPA SW846, Method 3050, and NIOSH 7082, Manual of Analytical Methods, NIOSH 7082 and
NIOSH 7105.
5. Significance and Use
5.1 This practice is intended for the digestion of lead in dust wipe samples collected during various lead hazard activities
performed in and around buildings and related structures.
5.2 This practice is also intended for the digestion of lead in dust wipe samples collected during and after building renovations.
5.3 This practice is applicable to the digestion of dust wipe samples that have or have not been collected in accordance with
Practice E1728E1728/E1728M using wipes that may or may not conform to Specification E1792.
5.4 This practice is applicable to the digestion of dust wipe samples that were placed in either hard-walled, rigid containers such
as 50-mL centrifuge tubes or flexible plastic bags.
NOTE 2—Due to the difficulty in performing quantitative transfers of some samples from plastic bags, hard-walled rigid containers such as 50-mL plastic
centrifuge tubes are recommended in Practice E1728/E1728M for sample collection.
5.5 Digestates prepared according to this practice are intended to be analyzed for lead concentration using spectrometric
techniques such as Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) and Flame Atomic Absorption
Spectrometry (FAAS) (see Test MethodMethods E1613, E3193, and E3203), or using electrochemical techniques such as anodic
stripping voltammetry (see Practice E2051).
5.6 This practice is not capable of determining lead bound within matrices, such as silica, that are not soluble in nitric acid.
5.7 This practice is capable of determining lead bound within paint.
6. Apparatus and Materials
6.1 Borosilicate Glassware:
6.1.1 Class A Volumetric Flasks with Stoppers, 100 mL and other sizes needed to make serial dilutions,
6.1.2 Griffın Beakers, 150 mL or 250 mL,
6.1.3 Watch Glasses, sized to cover Griffin beakers,
6.1.4 Class A Pipets, as needed to make serial dilutions, and
6.1.5 Glass Rods.
6.2 Funnels—Plastic or porcelain or borosilicate funnels sized to fit into a 100-mL volumetric flask.
6.3 Filter Paper—Fast filtering, suitable Suitable for metals analysis.
6.4 Thermometers—Red alcohol or thermocouple, that covers a range of 0 to 150°C.°Cto 150 °C.
6.5 Electric Hot Plate—Suitable for operation at temperatures up to at least 100°C 100 °C (see Note 3).
Ashley, K., and O’Connor, P. F., eds., NIOSH Manual of Analytical Methods, 5th ed., National Institute for Occupational Safety and Health: Cincinnati, OH, 2017.
E1644 − 21
NOTE 3—Provided that the hot plate is capable of handling the extra heating required, use of a 12- to 25-mm (0.5- to 1-in.) 12 mm to 25 mm (0.5 in.
to 1 in.) thick aluminum plate placed on the burner head can help reduce the presence of hot spots common to electric hot plates.
6.6 Vinyl Gloves—Gloves, Powderless.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 mL to 5 mL adjustable, 100 μL, 500 μL, 250 μL, and 1000 μL.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in this practice. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening accuracy of the determination.
7.2 Nitric Acid—Concentrated, 16.0 M HNO , suitable for atomic spectrometry analysis such as spectroscopic grade.
7.3 Hydrogen Peroxide—30 % (w/w), mass fraction 30 %, suitable for atomic spectrometry analysis such as spectroscopic grade.
7.4 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type
1 of Specification D1193.
7.5 Calibration Stock Solution—100 μg/mL of Pb in dilute nitric acid.
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