ASTM E1613-99
(Test Method)Standard 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
Standard 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
SCOPE
1.1 This test method is intended for use with digested samples that were collected originally during the abatement of lead hazards from buildings and related structures.
1.2 This test method covers the lead analysis of sample digestates (for example, digested paint, soil, dust, and airborne particulate) using inductively coupled plasma atomic emission spectrometry (ICP-AES), flame atomic absorption spectrometry (FAAS), and graphite furnace atomic absorption spectrometry (GFAAS) techniques.
1.3 No detailed operating instructions can be provided because of differences among various makes and models of satisfactory instruments. Instead, the analyst should follow the instructions provided by the manufacturer of the particular instrument.
1.4 This test method contains directions for sample analysis as well as quality assurance (QA) and quality control (QC) and may be used for purposes of laboratory accreditation and certification.
1.5 The use of analytical instrumentation other than ICP-AES, FAAS, and GFAAS is not within the scope of this test method.
1.6 The values stated in SI units are to be regarded as the standard.
1.7 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: E 1613 – 99
Standard 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
This standard is issued under the fixed designation E 1613; 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 D 3919 Practice for Measuring Trace Elements in Water by
Graphite Furnace Atomic Absorption Spectrophotometry
1.1 This test method is intended for use with extracted or
D 4210 Practice for Intralaboratory Quality Control Proce-
digested samples that were collected originally during the
dures and a Discussion on Reporting Low-Level Data
assessment, management, or abatement of lead hazards from
D 4697 Guide for Maintaining Test Methods in the User’s
buildings, structures, or other locations.
Laboratory
1.2 This test method covers the lead analysis of sample
D 4840 Guide for Sampling Chain of Custody Procedures
extracts or digestates (for example, extracted or digested paint,
E 456 Terminology Relating to Quality and Statistics
soil, dust, and airborne particulate) using inductively coupled
E 691 Practice for Conducting an Interlaboratory Study to
plasma atomic emission spectrometry (ICP-AES), flame
Determine the Precision of a Test Method
atomic absorption spectrometry (FAAS), or graphite furnace
E 1188 Practice for Collection and Preservation of Informa-
atomic absorption spectrometry (GFAAS).
tion and Physical Items by a Technical Investigator
1.3 This test method contains directions for sample analysis
E 1553 Practice for Collection of Airborne Particulate Lead
as well as quality assurance (QA) and quality control (QC) and
During Abatement and Construction Activities
may be used for purposes of laboratory accreditation and
E 1605 Terminology Relating to Abatement of Hazards
certification.
from Lead-Based Paint in Buildings and Related Struc-
1.4 No detailed operating instructions can be provided
tures
because of differences among various makes and models of
E 1644 Practice for Hot Plate Digestion of Dust Wipe
satisfactory instruments. Instead, the analyst should follow the
Samples for Subsequent Determination of Lead by Atomic
instructions provided by the manufacturer of the particular
Spectrometry
instrument.
E 1645 Practice for Preparation of Dried Paint Samples for
1.5 The use of analytical instrumentation other than ICP-
Subsequent Lead Analysis by Atomic Spectrometry
AES, FAAS, and GFAAS is not within the scope of this test
E 1726 Practice for Sample Digestion of Soils for the
method.
Determination of Lead by Atomic Spectrometry
1.6 The values stated in SI units are to be regarded as the
E 1727 Practice for Field Collection of Soil Samples for
standard.
Lead Determination by Atomic Spectrometry Techniques
1.7 This standard does not purport to address all of the
E 1728 Practice for Field Collection of Settled Dust
safety concerns, if any, associated with its use. It is the
Samples Using Wipe Sampling Methods for Lead Deter-
responsibility of the user of this standard to establish appro-
mination by Atomic Spectrometry Techniques
priate safety and health practices and determine the applica-
E 1729 Practice for Field Collection of Dried Paint Samples
bility of regulatory limitations prior to use.
for Determination by Atomic Spectrometry Techniques
2. Referenced Documents
E 1741 Practice for Preparation of Airborne Particulate
Lead Samples Collected During Abatement and Construc-
2.1 ASTM Standards:
tion Activities for Subsequent Analysis by Atomic Spec-
D 1193 Specification for Reagent Water
trometry
This test method is under the jurisdiction of ASTM Committee E-6 on
Performance of Buildings and is the direct responsibility of Subcommittee E06.23
on Lead Hazards Associated with Buildings.
Current edition approved Oct. 10, 1999. Published December 1999. Originally Annual Book of ASTM Standards, Vol 07.02.
published as E 1613 – 94. Last previous edition E 1613 – 94. Annual Book of ASTM Standards, Vol 14.02.
2 5
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 04.11.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1613
E 1775 Guide for Evaluating Performance of On-Site Ex- 3.1.6 digestate—an acidified aqueous solution that results
traction and Field-Portable Electrochemical or Spectropho- from digestion of the sample.
tometric Analysis for Lead 3.1.7 digestion—a high temperature sample preparation
E 1792 Specification for Wipe Sampling Materials for Lead process that solubilizes targeted analytes that may be present in
in Surface Dust the sample and results in an acidified aqueous solution called
E 1864 Practice for Evaluating Quality Systems of Organi- the digestate (see 3.1.6).
zations Engaged in Conducting Facility and Hazard As- 3.1.7.1 Discussion—Digestion normally entails the use of a
sessments to Determine the Presence and Extent of Lead in hot plate or microwave oven for subjecting the acidified sample
Paint, Dust, Airborne Particulate, and Soil in Buildings and solution to high temperatures. Digestion is a type of extraction
Related Structures (see 3.1.8).
E 1973 Practice for Collection of Surface Dust by Air 3.1.8 extraction—the dissolution of target analytes from a
Sampling Pump Vacuum Technique for Subsequent Lead solid matrix into a liquid form, and results in a solution called
Determination the extract.
E 1979 Practice for Ultrasonic Extraction of Paint, Dust, 3.1.8.1 Discussion—Target analytes are extracted (solubi-
Soil, or Air Samples for Subsequent Determination of lized) into a solution during sample extraction. Digestion (see
Lead 3.1.7) is an example of an extraction process. Apart from
2.2 Federal Documents: digestion, other examples of extraction processes include
ultrasonic extraction (1) and leaching (for example, 40 CFR
40 CFR 261 Appendix II-Method 1311 Toxic Characteristic
Leaching Procedure (TCLP) 261 Appendix II Method 1311).
3.1.9 initial calibration blank (ICB)—a standard containing
40 CFR 136 Guidelines Establishing Test Procedures for the
Analysis of Pollutants no analyte that is used for the initial calibration and zeroing of
the instrument response.
3.1.9.1 Discussion—The ICB must be matrix matched to
3. Terminology
the acid content of sample extracts and digestates. The ICB
3.1 Definitions—For definitions of related terms not appear-
must be measured during and after calibration. The measured
ing here, see Terminology E 1605.
value is to be (at most) less than five times the IDL (see 3.1.11).
3.1.1 analysis run—a period of measurement time on a
3.1.10 initial calibration verification (ICV)—a solution (or
given analytical instrument during which data are calculated
set of solutions) of known analyte concentration used to verify
from a single calibration curve (or single set of curves).
calibration standard levels; the concentration of analyte is to be
Recalibration of a given instrument produces a new analysis
near the mid-range of the linear curve that is made from a stock
run.
solution having a different manufacturer or manufacturer lot
3.1.2 batch—a group of field or QC samples that are
identification than the calibration standards.
processed together using the same reagents and equipment.
3.1.10.1 Discussion—The ICV must be matrix matched to
3.1.3 calibration standards—solutions of known analyte
the acid content of sample extracts or digestates. The ICV must
concentrations used to calibrate instruments.
be measured after calibration and before measuring any sample
3.1.3.1 Discussion—Calibration standards must be matrix
digestates or extracts. The measured value is to fall within
matched to the acid content present in sample digestates or
610 % of the known value.
extracts and must be measured prior to analyzing samples.
3.1.11 instrumental detection limit (IDL)—the lowest con-
3.1.4 continuing calibration blank (CCB)—a solution con-
centration at which the instrumentation can distinguish analyte
taining no analyte that is used to verify blank response and
content from the background generated by a minimal matrix.
freedom from carryover.
3.1.11.1 Discussion—The IDL is usually determined by the
3.1.4.1 Discussion—The CCB must be analyzed after the
manufacturer for use in advertising and promotion. The IDL
CCV (see 3.1.5) and after the ICkS (see 3.1.13). The measured
can be determined from blank, acidified deionized, or ultrapure
value is to be (at most) less than five times the instrumental
water as the matrix and from the same calculation methods
detection limit (IDL) (see 3.1.1).
used to determine a method detection limit (MDL) (see 3.1.15).
3.1.5 continuing calibration verification (CCV)—a solution
Typical IDLs for FAAS, ICP-AES, and GFAAS are 0.05, 0.03,
(or set of solutions) of known analyte concentration used to
and 0.002 μg Pb/mL, respectively.
verify freedom from excessive instrumental drift; the concen-
3.1.12 instrumental QC standards—these provide informa-
tration is to be near the mid-range of a linear calibration curve.
tion on measurement performance during the instrumental
3.1.5.1 Discussion—The CCV must be matrix matched to
analysis portion of the overall analyte measurement process.
the acid content present in sample digestates or extracts. The
They include CCBs, CCVs, ICBs, ICVs, and ICkSs.
CCV must be analyzed before and after all samples and at a
3.1.13 interference check standard (ICkS)—a solution (or
frequency of not less than every ten samples. The measured
set of solutions) of known analyte concentrations used for
value is to fall within 610 % (620 % for GFAA) of the known
ICP-AES to verify an accurate analyte response in the presence
value.
of possible spectral interferences from other analytes that may
6 7
Available from Superintendent of Documents, U.S. Government Printing The boldface numbers in parentheses refer to a list of references at the end of
Office, Washington, DC 20402. this standard.
E 1613
be present in samples; the concentration of analyte is to be less 3.1.19 quantitation limit—an instrumental measurement
than 25 % of the highest calibration standard, and concentra- value that is used to provide a lower concentration limit for
tions of the interferences will be 200 μg/mL of aluminum, reporting quantitative analysis data for a given analytical
calcium, iron, and magnesium. method.
3.1.13.1 Discussion—The ICkS must be matrix matched to 3.1.19.1 Discussion—Any sample that generates a lead
the acid content of sample digestates or extracts. The ICkS measurement below the quantitation limit is reported as a
must be analyzed at least twice, once before and once after the less-than value using the quantitation limit value multiplied by
analysis of all sample extracts or digestates. The measured the appropriate dilution factors resulting from preparation of
analyte value is expected to be within 620 % of the known the sample for instrumental analysis.
value. 3.1.20 semiquantitative analysis—an analysis run that is
3.1.14 method blank—a digestate or extract that reflects the performed on highly diluted sample digestates or extracts for
maximum treatment given any one sample within a sample the purpose of determining the approximate analyte level in the
batch, except that no sample is placed into the digestion or digest.
extraction vessel initially. (The same reagents and processing 3.1.20.1 Discussion—This analysis run is generally per-
conditions that are applied to field samples within a batch are formed without inserting instrumental QC standards except for
calibration standards. Data from this run are used for deter-
also applied to the method blank.)
3.1.14.1 Discussion—Analysis results from method blanks mining serial dilution requirements for sample digestates or
extracts to keep them within the linear range of the instrument.
provide information on the level of potential contamination
experienced by samples processed within the batch. 3.1.21 serial dilution—a method of producing a less-
concentrated solution through one or more consecutive dilution
3.1.15 limit of detection (LOD)—the MDL (see 3.1.16) or
the IDL (see 3.1.11), depending on the context. steps.
3.1.21.1 Discussion—A dilution step for a standard or
3.1.16 method detection limit (MDL)—the minimum con-
sample solution is performed by volumetrically placing a small
centration of analyte that, in a given matrix and with a specified
aliquot (of known volume) of a higher concentrated solution
analytical method, has a 99 % probability of being identified
into a volumetric flask and diluting to volume with water
and is reported to be greater than zero concentration.
containing the same acid levels as those found in original
3.1.16.1 Discussion:
sample digestates or extracts.
(a) As an example, the MDL for lead in paint is the
3.1.22 spiked sample—a sample portion (split from an
smallest measurable (that is, nonzero) concentration of lead
original sample) that is spiked with a known amount of analyte.
within the paint sample as determined by the validated extrac-
3.1.22.1 Discussion—Analysis results for spiked samples
tion and analysis method used. Note that there would be a
are used to provide information on the precision and bias of the
different MDL for different sample matrices (such as dust
overall analysis process.
wipes, air filters, and soils), even if the sample preparation and
3.1.23 spiked duplicate sample—Two portions of a homog-
analysis process is the same for all types of matrices. Thus each
enized sample that were targeted for addition of analyte and
sample matrix has a unique MDL, given in units specific to the
fortified with all the target analytes before preparation.
matrix, even if the analyte content is the same for each.
3.1.23.1 Discussion—Analysis results for these samples are
NOTE 1—For instance, for dust wipe samples, different brands of wipes
used to provide information on the precision and bias of the
could have different MDLs. Dust wipes and paint samples would have
overall analysis process.
lead contents expressed in different units.
(b) There are thus four component inputs to defining an
4. Summary of Test Method
MDL: (1) the analyte of interest (that is, lead (Pb) for our
4.1 A sample digestate or extract is analyzed for lead
purposes here); (2) the sample matrix (for example: paint, dust
content using ICP-AES, FAAS, or GFAAS tec
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