ASTM E1644-04(2016)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
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 E1728 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 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 Method E1613), 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.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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´1
Designation: E1644 − 04 (Reapproved 2016)
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—Caution statement changed to a warning in 8.1.4 and editorial changes made throughout in November 2016.
1. Scope Wipe Sampling Methods for Subsequent Lead Determi-
nation
1.1 This practice covers the acid digestion of surface dust
E1792 Specification for Wipe Sampling Materials for Lead
samples (collected using wipe sampling practices) and associ-
in Surface Dust
ated quality control (QC) samples for the determination of
E2051 Practice for the Determination of Lead in Paint,
lead.
Settled Dust, Soil and Air Particulate by Field-Portable
1.2 The values stated in SI units are to be regarded as
Electroanalysis (Withdrawn 2010)
standard. No other units of measurement are included in this
E2239 PracticeforRecordKeepingandRecordPreservation
standard.
for Lead Hazard Activities
1.2.1 Exception—Informational inch-pound units are pro-
2.2 Other Documents:
vided in Note 3.)
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
and processing conditions that are applied to field samples
within a batch are also applied to the method blanks.)
This practice is under the jurisdiction of ASTM Committee E06 on Perfor-
3.2.3.1 Discussion—Analysis results from method blanks
manceofBuildingsandisthedirectresponsibilityofSubcommitteeE06.23onLead
provide information on the level of potential contamination
Hazards Associated with Buildings.
Current edition approved Oct. 1, 2016. Published November 2016. Originally
ɛ1
approved in 1994. Last previous edition approved in 2012 as E1644–04(2012) .
DOI: 10.1520/E1644-04R16E01.
2 3
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
´1
E1644 − 04 (2016)
resulting from the laboratory and sampling medium sources 5.6 This practice is not capable of determining lead bound
that are experienced by samples processed within the batch. within matrices, such as silica, that are not soluble in nitric
acid.
3.2.4 non-spiked sample—a portion of a homogenized
sample that was targeted for the addition of analyte but is not
5.7 This practice is capable of determining lead bound
fortified with the target analytes before sample preparation.
within paint.
3.2.4.1 Discussion—Forwipesamples,anon-spikedsample
is equivalent to a method blank. Analysis results for this
6. Apparatus and Materials
sample are used to correct for background levels in the blank
6.1 Borosilicate Glassware:
wipes used for spiked and spiked duplicate samples.
6.1.1 Class A Volumetric Flasks with Stoppers, 100 mL and
3.2.5 reagent blank—a digestate that reflects the maximum
other sizes needed to make serial dilutions,
treatment given any one sample within a sample batch except
6.1.2 Griffın Beakers, 150 mL or 250 mL,
that it has no sample placed into the digestion vessel. (The
6.1.3 Watch Glasses, sized to cover Griffin beakers,
same reagents and processing conditions that are applied to
6.1.4 Class A Pipets, as needed to make serial dilutions, and
field samples within a batch are also applied to the reagent
6.1.5 Glass Rods.
blank.)
6.2 Funnels—Plastic or porcelain or borosilicate funnels
3.2.5.1 Discussion—Analysis results from reagent blanks
sized to fit into a 100-mL volumetric flask.
provide information on the level of potential contamination
6.3 Filter Paper—Fast filtering, suitable for metals analysis.
resulting from only laboratory sources that are experienced by
samples processed within the batch.
6.4 Thermometers—Red alcohol or thermocouple, that cov-
3.2.6 spiked sample and spiked duplicate sample—a blank ers a range of 0 to 150°C.
wipe that is spiked with a known amount of analyte (that is,
6.5 Electric Hot Plate—Suitable for operation at tempera-
lead) before hot plate digestion and subsequent lead analysis.
tures up to at least 100°C (see Note 3).
3.2.6.1 Discussion—Analysis results for these samples are
NOTE 3—Provided that the hot plate is capable of handling the extra
used to provide information on accuracy and precision of the
heating required, use of a 12- to 25-mm (0.5- to 1-in.) thick aluminum
overall analysis process.
plate placed on the burner head can help reduce the presence of hot spots
common to electric hot plates.
4. Summary of Practice
6.6 Vinyl Gloves—Powderless.
4.1 A dust wipe sample is digested using hot plate type
6.7 Micropipettors with Disposable Plastic Tips—Sizes
heating with nitric acid and hydrogen peroxide. The digestate
needed to make reagent additions, and spike standards. In
is diluted to final volume prior to lead measurement.
general, the following sizes should be readily available: 1 to
NOTE 1—The procedure in this practice is based on U.S. EPA SW846
5 mL adjustable, 100 µL, 500 µL, 250 µL, and 1000 µL.
Method 3050, NIOSH 7082, and NIOSH 7105.
7. Reagents
5. Significance and Use
7.1 Purity of Reagents—Reagent grade chemicals shall be
5.1 This practice is intended for the digestion of lead in dust
used in this practice. Unless otherwise indicated, it is intended
wipe samples collected during various lead hazard activities
thatallreagentsconformtothespecificationsoftheCommittee
performed in and around buildings and related structures.
on Analytical Reagents of the American Chemical Society,
5.2 This practice is also intended for the digestion of lead in
where such specifications are available. Other grades may be
dust wipe samples collected during and after building renova-
used, provided it is first ascertained that the reagent is of
tions.
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
7.2 Nitric Acid—Concentrated, suitable for atomic spec-
with Practice E1728 using wipes that may or may not conform
trometry analysis such as spectroscopic grade.
to Specification E1792.
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
7.4 Purity of Water—Unless otherwise indicated, references
such as 50-mL centrifuge tubes or flexible plastic bags.
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. (USP), Rockville,
electrochemica
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1 ´1
Designation: E1644 − 04 (Reapproval 2012) E1644 − 04 (Reapproved 2016)
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 Caution statement changed to a warning in 28.1.4 in April 2012.and edito-
rial changes made throughout in November 2016.
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
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
E1728 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
2.2 Other Documents:
EPA SW 846, Method 3050, “Acid Digestion of Sediments, Sludges, and Soils.” This method is found in Test 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 and E1605.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 blank wipe—an unused, unspiked dust wipe that is only removed from its packaging immediately before use.
This practice is under the jurisdiction of ASTM Committee E06 on Performance of Buildings and is the direct responsibility of Subcommittee E06.23 on Lead Hazards
Associated with Buildings.
Current edition approved April 1, 2012Oct. 1, 2016. Published May 2012November 2016. Originally approved in 1994. Last previous edition approved in 20042012 as
ɛ1
E1644 – 04.E1644–04(2012) . DOI: 10.1520/E1644-04R12.10.1520/E1644-04R16E01.
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.
Available from National Technical Information Service (NTIS), 5301 Shawnee 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
´1
E1644 − 04 (2016)
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—surface dust collected on a wipe.
3.2.3 method blank—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. (The same reagents and processing
conditions that are applied to field samples 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 resulting from the laboratory and
sampling medium sources that are experienced by samples processed within the batch.
3.2.4 non-spiked sample—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—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. (The same reagents and processing conditions that are applied to field samples
within a batch are also applied to the reagent blank.)
3.2.5.1 Discussion—
Analysis results from reagent blanks 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—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.
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, 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 E1728 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 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 Method E1613), 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.
´1
E1644 − 04 (2016)
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. 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 for metals analysis.
6.4 Thermometers—Red alcohol or thermocouple, that covers a range of 0 to 150°C.
6.5 Electric Hot Plate—Suitable for operation at temperatures up to at least 100°C (see Note 3).
NOTE 3—Provided that the hot plate is capable of handling the extra heating required, use of a 1212- to 25-mm (0.5(0.5- 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—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 mL 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, suitable for atomic spectrometry analysis such as spectroscopic grade.
7.3 Hydrogen Peroxide—30 % (w/w), 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.
8. Sample Preparation Procedure
8.1 Sample Extraction:
8.1.1 Treat each
...
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