ASTM D8568-24

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.
Designation: D8568 − 24
Standard Test Method for
Determination of Lead by Graphite Furnace Atomic
Absorption Spectrometry (GFAAS) Techniques
This standard is issued under the fixed designation D8568; 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 2. Referenced Documents
1.1 This test method covers the determination of lead (Pb) 2.1 ASTM Standards:
in airborne particulate, dust by wipe and micro-vacuuming, D1193 Specification for Reagent Water
paint, and soil collected in and around buildings and related D1356 Terminology Relating to Sampling and Analysis of
structures using graphite furnace atomic absorption spectrom- Atmospheres
etry (GFAAS). D3919 Practice for Measuring Trace Elements in Water by
Graphite Furnace Atomic Absorption Spectrophotometry
1.2 This test method contains directions for sample analysis,
D4210 Practice for Intralaboratory Quality Control Proce-
as well as quality assurance (QA) and quality control (QC), and
dures and a Discussion on Reporting Low-Level Data
may be used for purposes of laboratory accreditation and
(Withdrawn 2002)
certification.
D4532 Test Method for Respirable Dust in Workplace At-
1.3 No detailed operating instructions are provided because
mospheres Using Cyclone Samplers
of differences among various makes and models of suitable
D4697 Guide for Maintaining Test Methods in the User’s
GFAAS instruments. Instead, the analyst shall follow the
Laboratory (Withdrawn 2009)
instructions provided by the manufacturer of the particular
D4840 Guide for Sample Chain-of-Custody Procedures
instrument.
D6785 Test Method for Determination of Lead in Workplace
1.4 The values stated in SI units are to be regarded as Air Using Flame or Graphite Furnace Atomic Absorption
Spectrometry
standard. No other units of measurement are included in this
standard. D6966 Practice for Collection of Settled Dust Samples
Using Wipe Sampling Methods for Subsequent Determi-
1.4.1 Exception—The SI and inch-pound units shown for
nation of Metals
wipe and micro-vacuuming sampling data are to be individu-
ally regarded as standard for wipe and micro-vacuuming D7035 Test Method for Determination of Metals and Met-
alloids in Airborne Particulate Matter by Inductively
sampling data.
Coupled Plasma Atomic Emission Spectrometry (ICP-
1.5 This test method contains notes which are explanatory
AES)
and not part of the mandatory requirements of this standard.
D7144 Practice for Collection of Surface Dust by Micro-
1.6 This standard does not purport to address all of the
vacuum Sampling for Subsequent Determination of Met-
safety concerns, if any, associated with its use. It is the
als and Metalloids
responsibility of the user of this standard to establish appro-
D8358 Guide for Assessment and Inclusion of Wall Deposits
priate safety, health, and environmental practices and deter-
in the Analysis of Single-Stage Samplers for Airborne
mine the applicability of regulatory limitations prior to use.
Particulate Matter
1.7 This international standard was developed in accor-
E456 Terminology Relating to Quality and Statistics
dance with internationally recognized principles on standard-
E691 Practice for Conducting an Interlaboratory Study to
ization established in the Decision on Principles for the
Determine the Precision of a Test Method
Development of International Standards, Guides and Recom-
E1188 Practice for Collection and Preservation of Informa-
mendations issued by the World Trade Organization Technical
tion and Physical Items by a Technical Investigator
Barriers to Trade (TBT) Committee.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D22 on Air contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Quality and is the direct responsibility of Subcommittee D22.12 on Sampling and Standards volume information, refer to the standard’s Document Summary page on
Analysis of Lead for Exposure and Risk Assessment. the ASTM website.
Current edition approved April 1, 2024. Published April 2024. DOI: 10.1520/ The last approved version of this historical standard is referenced on
D8568-24. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8568 − 24
E1583 Practice for Evaluating Laboratories Engaged in De- 2.2 ISO/IEC Standard:
termination of Lead in Paint, Dust, Airborne Particulates, ISO/IEC 17025 General requirements for the competence of
testing and calibration laboratories
and Soil Taken From and Around Buildings and Related
Structures
3. Terminology
E1605 Terminology Relating to Lead in Buildings
3.1 Definitions—For definitions of terms not appearing here,
E1644 Practice for Hot Plate Digestion of Dust Wipe
see Terminologies D1356, E456, and E1605.
Samples for the Determination of Lead
E1645 Practice for Preparation of Dried Paint Samples by
3.2 Definitions of Terms Specific to This Standard:
Hotplate or Microwave Digestion for Subsequent Lead 3.2.1 analysis run, n—a period of measurement time on a
Analysis
given analytical instrument during which data are calculated
E1726 Practice for Preparation of Soil Samples by Hotplate from a single calibration curve (or single set of such curves).
Digestion for Subsequent Lead Analysis 3.2.1.1 Discussion—Recalibration of a given GFAAS in-
strument produces a new analysis run.
E1727 Practice for Field Collection of Soil Samples for
Subsequent Lead Determination
3.2.2 calibration standards, n—solutions of known analyte
E1728 Practice for Collection of Settled Dust Samples Using
(Pb) concentrations used to calibrate instruments.
Wipe Sampling Methods for Subsequent Lead Determi-
3.2.2.1 Discussion—Calibration standards are matrix
nation
matched to the acid content present in sample digestates or
E1729 Practice for Field Collection of Dried Paint Samples extracts and are measured prior to analyzing samples.
for Subsequent Lead Determination
3.2.3 initial calibration blank (ICB), n—a standard contain-
E1741 Practice for Preparation of Airborne Particulate Lead
ing no analyte (Pb) that is used for the initial calibration and
Samples Collected During Abatement and Construction
zeroing of the instrument response.
Activities for Subsequent Analysis by Atomic Spectrom-
3.2.3.1 Discussion—The ICB is matrix matched to the acid
etry (Withdrawn 2009)
content of sample extracts and digestates. The ICB is measured
E1775 Guide for Evaluating Performance of On-Site Extrac-
during and after calibration. The measured Pb value is to be (at
tion and Field-Portable Electrochemical or Spectrophoto-
maximum) less than five times the IDL (see 3.2.7).
metric Analysis for Lead
3.2.4 initial calibration verification (ICV), n—a solution (or
E1792 Specification for Wipe Sampling Materials for Lead
set of solutions) of known analyte (Pb) concentration used to
in Surface Dust
verify calibration standard levels; the concentration of analyte
E1864 Practice for Evaluating Quality Systems of Organi-
is to be near the mid-range of the linear curve that is made from
zations Conducting Facility and Hazard Assessments for
a stock solution having a different manufacturer or manufac-
Lead in Paint, Dust, Airborne Particulate, and Soil in and
turer lot identification than the calibration standards.
around Buildings and Related Structures (Withdrawn
3.2.4.1 Discussion—The ICV is matrix matched to the acid
2011)
content of sample extracts or digestates. The ICV is measured
E1908 Practice for Sample Selection of Debris Waste from a
after calibration and before measuring any sample digestates or
Building Renovation or Lead Abatement Project for Tox-
extracts. The measured Pb value is to fall within 610 % of the
icity Characteristic Leaching Procedure (TCLP) Testing
known value.
for Leachable Lead (Pb)
3.2.5 instrumental detection limit (IDL), n—the lowest con-
E1979 Practice for Ultrasonic Extraction of Paint, Dust,
centration at which the instrumentation can distinguish analyte
Soil, and Air Samples for Subsequent Determination of
(Pb) content from the background generated by a minimal
Lead
matrix.
E2115 Guide for Conducting Lead Hazard Assessments of
3.2.5.1 Discussion—The IDL is usually determined by the
Dwellings and of Other Child-Occupied Facilities
instrument manufacturer. The IDL can be determined from
E2239 Practice for Record Keeping and Record Preservation
blank, acidified, deionized, or ultrapure water as the matrix and
for Lead Hazard Activities
from the same calculation methods used to determine a method
E2271/E2271M Practice for Clearance Examinations Fol-
detection limit (MDL) (see 3.2.10). Typical lead (Pb) IDLs for
lowing Lead Hazard Reduction Activities in Multifamily
GFAAS are near 0.002 μg Pb/mL.
Dwellings
3.2.6 method blank, n—a digestate or extract that reflects the
E2913/E2913M Practice for Hotplate Digestion of Lead
maximum treatment given to any one sample within a sample
from Composited Wipe Samples
batch, except that no sample is placed into the digestion or
E2914/E2914M Practice for Ultrasonic Extraction of Lead
extraction vessel.
from Composited Wipe Samples
3.2.6.1 Discussion—The same reagents and processing con-
E3074/E3074M Practice for Clearance Examinations Fol-
ditions that are applied to field samples within a batch are also
lowing Lead Hazard Reduction Activities in Single Fam-
ily Dwellings, in Individual Units of Multifamily
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Dwellings, and in Other Child-Occupied Facilities 4th Floor, New York, NY 10036, http://www.ansi.org.
D8568 − 24
applied to the method blank. Analysis results from method aliquot (of known volume) of a higher concentrated solution
blanks provide information on the level of potential contami- into a volumetric flask and diluting to volume with water
nation experienced by samples processed within the batch. containing the same acid levels as those found in original
sample digestates or extracts.
3.2.7 method detection limit (MDL), n—the minimum con-
centration of analyte (Pb) that, in a given matrix and with a 3.2.12 spiked duplicate sample, n—two portions of a ho-
specified analytical method, has a 99 % probability of being mogenized sample that were targeted for addition of analyte
identified and is reported to be greater than zero concentration. (Pb) and fortified with all the target analytes before prepara-
3.2.7.1 Discussion—As an example, the MDL for lead in tion.
paint is the smallest measurable (that is, nonzero) concentra- 3.2.12.1 Discussion—Analysis results for these samples are
tion of lead within the paint sample as determined by the used to provide information on the precision and bias of the
validated extraction and analysis method used. Note that there overall analysis process.
would be a different MDL for different sample matrices (such
3.2.13 spiked sample, n—a sample portion (split from an
as dust wipes, air particulates, and soils), even if the sample
original sample) that is spiked with a known amount of analyte
preparation and analysis process is the same for all types of
(Pb).
matrices. Thus each sample matrix has a unique MDL, given in
3.2.13.1 Discussion—Analysis results for spiked samples
units specific to the matrix, even if the analyte content is the
are used to provide information on the precision and bias of the
same for each.
overall analysis process.
NOTE 1—For instance, for dust wipe samples, different brands of wipe
3.2.14 un-spiked sample, n—a portion of a homogenized
media could have different Pb MDLs. Dust wipes and paint samples will
sample that was targeted for the addition of analyte (Pb) but is
have lead contents expressed in different units.
not fortified with target analytes before sample preparation.
3.2.7.2 Discussion—There are four component inputs to 3.2.14.1 Discussion—Analysis results for this sample are
defining an MDL: (1) the analyte of interest (that is, lead (Pb) used to correct for native analyte (Pb) levels in the spiked and
for our purposes here); (2) the sample matrix (for example: spiked duplicate samples.
paint, dust, or brand x wipe, soil, or air particulate collected on
4. Summary of Test Method
type x sampling media); (3) the extraction/digestion procedure
used; and (4) the analysis procedure (using the type of GFAAS
4.1 A sample digestate or extract of a sample of air
instrumentation and components) used for quantification of
particulate, dust (wipe or vacuum sample), paint or soil is
analyte content. The MDL is established prior to reporting
analyzed for lead content using graphite furnace atomic ab-
analysis data.
sorption spectrometric (GFAAS) instrumentation (Practice
3.2.8 quantitation limit, n—an instrumental measurement D3919; 1, 2, 3). Quality control (QC) samples are analyzed
along with sample digestates or extracts in order to ensure
value that is used to provide a lower Pb concentration limit for
reporting quantitative analysis data for a given analytical adequate instrumental performance.
NOTE 2—Digestion is an example of an extraction process. Other
method.
examples of extraction processes are ultrasonic extraction (4) and leaching
3.2.8.1 Discussion—Any sample that generates a lead mea-
(Guide E1908).
surement below the quantitation limit is reported as a less-than
value using the quantitation limit value multiplied by the
5. Significance and Use
appropriate dilution factors resulting from preparation of the
5.1 Environmental (including workplace) samples obtained
sample for instrumental analysis.
during the assessment or mitigation of lead hazards from
3.2.9 quantitative analysis, n—an analysis run on sample
buildings and related structures are analyzed to determine lead
digestates or extracts (or serial dilutions thereof) that includes
content in media of concern. This test method is intended for
instrumental QC standards.
use with other ASTM standards (see 2.1) that address the
3.2.9.1 Discussion—Data from this analysis run are used to
collection and preparation of samples (airborne particulate,
calculate and report final lead analysis results.
dusts by wipe and micro-vacuuming, dried paint chips, and
3.2.10 semiquantitative analysis, n—an analysis run that is
soils) that are obtained during the assessment or mitigation of
performed on highly diluted sample digestates or extracts for
lead hazards. This test method may be used to analyze samples
the purpose of determining the approximate analyte (Pb) level
collected from various environments, such as workplaces,
in the digest.
buildings, indoor or outdoor settings, construction sites,
3.2.10.1 Discussion—This analysis run is generally per-
housing, and so on.
formed without inserting instrumental QC standards except for
5.2 This test method may also be used to analyze similar
calibration standards. Data from this run are used for deter-
samples from other environments such as toxic characteristic
mining serial dilution requirements for sample digestates or
extracts of waste sampled using Guide E1908, and soil and
extracts to keep them within the linear range of the instrument.
sludge as prepared for analysis using U.S. EPA SW-846 Test
3.2.11 serial dilution, n—a method of producing a less-
Method 1311 (5).
concentrated solution through one or more consecutive dilution
steps.
3.2.11.1 Discussion—A dilution step for a standard or
The boldface numbers in parentheses refer to the list of references at the end of
sample solution is performed by volumetrically placing a small this standard.
D8568 − 24
5.3 This test method can be relied upon by laboratories different lot number (or manufacturer) than the calibration
seeking accreditation for lead analysis by means of GFAAS. stock solution (see 8.3).
6. Interferences 9. Preparation of Labware
6.1 Interferences for GFAAS can be manufacturer- and
9.1 Wash glassware and plastic equipment with laboratory
model-specific. The following are general guidelines:
detergent, rinse with tap water, soak for at least 4 h in volume
6.1.1 Molecular absorption is a potential interference in
fraction 35 % (volume/volume 1+1) nitric acid and water, rinse
GFAAS (6). These interferences can be minimized by using
three times with ASTM Type I Water, and allow to dry
techniques such as D or H continuum background correction
preferably in a fume hood. Commercial, automatic systems are
2 2
(7).
available that perform a similar process.
6.1.2 High concentrations (for example, 100- to 1000-fold
9.2 Alternatively, soak glassware and plastic equipment in
excess compared to lead concentration) of calcium, sulfate,
volume fraction 35 % (volume/volume 1+1) nitric acid and
phosphate, iodide, fluoride, or acetate can interfere with lead
water in a plastic tub preferably in a working hood with the
determination by GFAAS (7, 8). These interferences can be
hood sash down, rinse three times with ASTM Type I Water,
corrected by standard addition techniques (9).
and allowed to dry preferably in a fume hood.
6.1.3 Other sources of interference may be found for various
matrices; these are discussed in more detail elsewhere (6, 8).
10. Sample Collection and Preparation
7. Apparatus and Materials
10.1 Sample Collection—Samples should be collected, as
appropriate to the matrix of interest, using Test Method D4532,
7.1 Analytical Instrumentation—The instrumentation used
Practices D6966, D7144, E1727, E1728, E1729, E2271/
shall consist of one or more of the following apparatus:
E2271M, E3074/E3074M, or Guide D8358, or combinations
7.1.1 Graphite Furnace Atomic Absorption Spectrometer
thereof.
(GFAAS), equipped with background correction, lead hollow
cathode lamp, or discharge lamp without electrodes, and
10.2 Sample Preparation—Samples should be prepared for
capable of making lead absorption measurements at the
analysis, as appropriate to the matrix of interest, using Prac-
283.3 nm absorption line (see Practice D3919).
tices E1644, E1645, E1726, E1741, E1979, E2913/E2913M, or
E2914/E2914M.
NOTE 3—For lead, the 283.3 nm line is normally preferred over the
217.0 nm line because of the increased noise levels commonly observed at
217.0 nm for GFAAS.
11. Requirement for Laboratory Analysis
NOTE 4—GFAAS is sometimes referred to as electrothermal atomic
absorption spectrometry (ETAAS).
11.1 Laboratories analyzing samples obtained during the
NOTE 5—The operating parameters for graphite furnace atomic absorp-
assessment or mitigation of lead hazards from buildings and
tion can vary considerably between different instruments.
related structures shall conform to Practice E1583, or shall be
7.2 Argon, compressed, in grade specified by the manufac-
recognized for lead analysis as promulgated by authorities
turer of the GFAAS instrument used.
having jurisdiction, or both.
NOTE 6—In the United States of America, laboratories performing
7.3 Vinyl Gloves, powderless.
analysis of samples collected during lead-based paint activities are
7.4 Micropipettors with Disposable Plastic Tips, in sizes
required to be accredited to ISO/IEC 17025 and to other requirements
necessary to make reagent additions, serial dilutions, and
promulgated by the Environmental Protection Agency (EPA).
spiking standards. In general, the following sizes should be
readily available: 1 mL to 5 mL adjustable and 1000 μL, 12. Procedure
500 μL, 250 μL, and 100 μL.
12.1 Laboratory Records—Record all reagent sources (lot
7.5 Volumetric Flasks, in sizes necessary to make calibra-
numbers and vendors) used for sample preparation and analysis
tion standards, serial dilutions, and instrumental QC standards.
in a laboratory notebook. Record any inadvertent deviations,
unusual happenings, or observations on a real-time basis as the
8. Reagents
samples are processed. Use these records to add supplemental
information when reporting the results.
8.1 Water—Unless otherwise indicated, references to water
shall be understood to mean reagent water as defined by Type
12.2 Instrumental Setup:
I of Specification D1193. (ASTM Type I Water: minimum
12.2.1 Set the GFAAS spectrometer up for the analysis of
resistance of 16.67 MΩ-cm or equivalent.)
lead at 283.3 nm, in accordance with the instructions given by
8.2 Nitric Acid, concentrated, suitable for atomic spectrom-
the manufacturer. Allow an appropriate warm-up of the system
etry analysis (such as spectroscopic grade). prior to analysis.
8.3 Calibration Stock Solution, 100 μg/mL of lead in dilute
12.3 Preparation of Calibration and Instrumental QC Stan-
nitric acid or equivalent (such as a multielement stock contain-
dards:
ing lead).
12.3.1 Calibration Standards—Prepare a series of calibra-
8.4 Check Standard Stock Solution (for ICV), 100 μg/mL of tion standards (minimum of three) covering the linear range of
lead in dilute nitric acid or equivalent. This shall be from a the GFAAS instrumentation. Prepare these standards using
D8568 − 24
serial dilution from the calibration stock solutions and obtain- 12.5 Instrumental QC Evaluation and Corrective Action—
ing the same final nitric acid concentration present in the Examine the data generated from the analysis of calibration
sample digestates or extracts. Also prepare an ICB (see Table standards and instrumental QC standards. Evaluate the analysis
1). run using the criteria given in Table 1. Failure to achieve the
12.3.2 Instrumental QC Standards—Prepare instrumental specifications given in Table 1 will require corrective action to
QC standards as summarized in Table 1 using serial dilution be performed as described as follows:
from the required stock solutions. Prepare these standards
12.5.1 ICB, Calibration Standards, or ICV—Failure to meet
u
...