ASTM E1644-04(2012)e1
(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
SIGNIFICANCE AND USE
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.
This practice is also intended for the digestion of lead in dust wipe samples collected during and after building renovations.
This practice is applicable to the digestion of dust wipe samples that have or have not been collected in accordance with Practice E1728 using wipes that may or may not conform to Specification E1792.
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 for sample collection.
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 Method E1613), or using electrochemical techniques such as anodic stripping voltammetry (see Practice E2051).
This practice is not capable of determining lead bound within matrices, such as silica, that are not soluble in nitric acid.
This practice is capable of determining lead bound within paint.
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.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: E1644 − 04(Reapproval 2012)
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.
ε NOTE—Editorial corrections made to Section 2 in April 2012.
1. Scope E1792 Specification for Wipe Sampling Materials for Lead
in Surface Dust
1.1 This practice covers the acid digestion of surface dust
E2051 Practice for the Determination of Lead in Paint,
samples (collected using wipe sampling practices) and associ-
Settled Dust, Soil and Air Particulate by Field-Portable
ated quality control (QC) samples for the determination of
Electroanalysis (Withdrawn 2010)
lead.
E2239 PracticeforRecordKeepingandRecordPreservation
1.2 The values stated in SI units are to be regarded as
for Lead Hazard Activities
standard. No other units of measurement are included in this
2.2 Other Documents:
standard.
EPA SW 846, Method 3050, “Acid Digestion of Sediments,
1.3 This practice contains notes which are explanatory and
Sludges, and Soils.”This method is found in Test Methods
not part of mandatory requirements of the standard.
for Evaluating Solid Waste, Physical/Chemical Methods,
1.4 This standard does not purport to address all of the U.S. EPA SW 846, 3rd Edition, Revision 1, 1987
NIOSH Manual of Analytical Methods, NIOSH 7082 and
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 7105, Eller, P.M., Ed., 3rd ed., 1984
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 3. Terminology
3.1 Definitions—Fordefinitionsoftermsnotappearinghere,
2. Referenced Documents
refer to Terminologies D1129 and E1605.
2.1 ASTM Standards:
3.2 Definitions of Terms Specific to This Standard:
D1129 Terminology Relating to Water
3.2.1 blank wipe—an unused, unspiked dust wipe that is
D1193 Specification for Reagent Water
only removed from its packaging immediately before use.
E1605 Terminology Relating to Lead in Buildings
3.2.1.1 Discussion—Blank wipes are used to prepare non-
E1613 Test Method for Determination of Lead by Induc-
spiked,spiked,andspikedduplicatequalityassurancesamples.
tively Coupled Plasma Atomic Emission Spectrometry
3.2.2 dust wipe sample—surface dust collected on a wipe.
(ICP-AES), Flame Atomic Absorption Spectrometry
3.2.3 method blank—a digestate that reflects the maximum
(FAAS), or Graphite Furnace Atomic Absorption Spec-
treatment given any one sample within a sample batch except
trometry (GFAAS) Techniques
that only the sampling medium (such as a blank wipe) is
E1728 PracticeforCollectionofSettledDustSamplesUsing
initially placed into the digestion vessel. (The same reagents
Wipe Sampling Methods for Subsequent Lead Determi-
and processing conditions that are applied to field samples
nation
within a batch are also applied to the method blanks.)
3.2.3.1 Discussion—Analysis results from method blanks
provide information on the level of potential contamination
This practice is under the jurisdiction of ASTM Committee E06 on Perfor-
resulting from the laboratory and sampling medium sources
manceofBuildingsandisthedirectresponsibilityofSubcommitteeE06.23onLead
that are experienced by samples processed within the batch.
Hazards Associated with Buildings.
Current edition approved April 1, 2012. Published May 2012. Originally
approved in 1994. Last previous edition approved in 2004 as E1644 – 04. DOI:
10.1520/E1644-04R12.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM www.astm.org.
Standards volume information, refer to the standard’s Document Summary page on Available from National Technical Information Service (NTIS), 5301 Shawnee
the ASTM website. Rd., Alexandria, VA 22312, http://www.ntis.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E1644 − 04 (Reapproval 2012)
3.2.4 non-spiked sample—a portion of a homogenized 5.6 This practice is not capable of determining lead bound
sample that was targeted for the addition of analyte but is not within matrices, such as silica, that are not soluble in nitric
fortified with the target analytes before sample preparation. acid.
3.2.4.1 Discussion—Forwipesamples,anon-spikedsample
5.7 This practice is capable of determining lead bound
is equivalent to a method blank. Analysis results for this
within paint.
sample are used to correct for background levels in the blank
wipes used for spiked and spiked duplicate samples.
6. Apparatus and Materials
3.2.5 reagent blank—a digestate that reflects the maximum
6.1 Borosilicate Glassware:
treatment given any one sample within a sample batch except
6.1.1 Class A Volumetric Flasks with Stoppers, 100 mL and
that it has no sample placed into the digestion vessel. (The
other sizes needed to make serial dilutions,
same reagents and processing conditions that are applied to
6.1.2 Griffın Beakers, 150 mL or 250 mL,
field samples within a batch are also applied to the reagent
6.1.3 Watch Glasses, sized to cover Griffin beakers,
blank.)
6.1.4 Class A Pipets, as needed to make serial dilutions, and
6.1.5 Glass Rods.
3.2.5.1 Discussion—Analysis results from reagent blanks
provide information on the level of potential contamination
6.2 Funnels—Plastic or porcelain or borosilicate funnels
resulting from only laboratory sources that are experienced by
sized to fit into a 100-mL volumetric flask.
samples processed within the batch.
6.3 Filter Paper—Fast filtering, suitable for metals analysis.
3.2.6 spiked sample and spiked duplicate sample—a blank
6.4 Thermometers—Red alcohol or thermocouple, that cov-
wipe that is spiked with a known amount of analyte (that is,
ers a range of 0 to 150°C.
lead) before hot plate digestion and subsequent lead analysis.
6.5 Electric Hot Plate—Suitable for operation at tempera-
3.2.6.1 Discussion—Analysis results for these samples are
tures up to at least 100°C (see Note 3).
used to provide information on accuracy and precision of the
overall analysis process.
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.) thick aluminum plate
placed on the burner head can help reduce the presence of hot spots
4. Summary of Practice
common to electric hot plates.
4.1 A dust wipe sample is digested using hot plate type
6.6 Vinyl Gloves—Powderless.
heating with nitric acid and hydrogen peroxide. The digestate
6.7 Micropipettors with Disposable Plastic Tips—Sizes
is diluted to final volume prior to lead measurement.
needed to make reagent additions, and spike standards. In
NOTE 1—The procedure in this practice is based on U.S. EPA SW846
general, the following sizes should be readily available: 1 to 5
Method 3050, NIOSH 7082, and NIOSH 7105.
mL adjustable, 100 µL, 500 µL, 250 µL, and 1000 µL.
5. Significance and Use
7. Reagents
5.1 This practice is intended for the digestion of lead in dust
7.1 Purity of Reagents—Reagent grade chemicals shall be
wipe samples collected during various lead hazard activities
used in this practice. Unless otherwise indicated, it is intended
performed in and around buildings and related structures.
thatallreagentsconformtothespecificationsoftheCommittee
5.2 This practice is also intended for the digestion of lead in
on Analytical Reagents of the American Chemical Society,
dust wipe samples collected during and after building renova-
where such specifications are available. Other grades may be
tions.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening
5.3 This practice is applicable to the digestion of dust wipe
accuracy of the determination.
samples that have or have not been collected in accordance
with Practice E1728 using wipes that may or may not conform
7.2 Nitric Acid—Concentrated, suitable for atomic spec-
to Specification E1792. trometry analysis such as spectroscopic grade.
7.3 Hydrogen Peroxide—30 % (w/w), suitable for atomic
5.4 This practice is applicable to the digestion of dust wipe
spectrometry analysis such as spectroscopic grade.
samplesthatwereplacedineitherhard-walled,rigidcontainers
such as 50-mL centrifuge tubes or flexible plastic bags.
7.4 Purity of Water—Unless otherwise indicated, references
NOTE 2—Due to the difficulty in performing quantitative transfers of
to water shall be understood to mean reagent water as defined
some samples from plastic bags, hard-walled rigid containers such as
by Type 1 of Specification D1193.
50-mL plastic centrifuge tubes are recommended for sample collection.
5.5 Digestates prepared according to this practice are in-
tended to be analyzed for lead concentration using spectromet- 5
Reagent Chemicals, American Chemical Society Specifications, American
ric techniques such as Inductively Coupled Plasma Atomic
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Emission Spectrometry (ICP-AES) and FlameAtomicAbsorp-
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
tion Spectrometry (FAAS) (see Test Method E1613), or using
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
electrochemical techniques such as anodic stripping
...
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