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) Techniques1
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:2
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
1.2 This test method contains directions for sample analysis, Graphite Furnace Atomic Absorption Spectrophotometry
as well as quality assurance (QA) and quality control (QC), and D4210 Practice for Intralaboratory Quality Control Proce-
may be used for purposes of laboratory accreditation and dures and a Discussion on Reporting Low-Level Data
certification. (Withdrawn 2002)3
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 Instead, the analyst shall follow the Laboratory (Withdrawn 2009)3
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
standard. No other units of measurement are included in this Spectrometry
standard. D6966 Practice for Collection of Settled Dust Samples
1.4.1 Exception—The SI and inch-pound units shown for Using Wipe Sampling Methods for Subsequent Determi-
wipe and micro-vacuuming sampling data are to be individu- nation of Metals
ally regarded as standard for wipe and micro-vacuuming D7035 Test Method for Determination of Metals and Met-
sampling data. alloids in Airborne Particulate Matter by Inductively
1.5 This test method contains notes which are explanatory Coupled Plasma Atomic Emission Spectrometry (ICP-
and not part of the mandatory requirements of this standard. AES)
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.

2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction of ASTM Committee D22 on Air contact ASTM Customer Service at [email protected]. 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.
3
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

1
 D8568 − 24
E1583 Practice for Evaluating Laboratories Engaged in De- 2.2 ISO/IEC Standard:4
termination of Lead in Paint, Dust, Airborne Particulates, ISO/IEC 17025 General requirements for the competence of
and Soil Taken From and Around Buildings and Related testing and calibration laboratories
Structures
3. Terminology
E1605 Terminology Relating to Lead in Buildings
E1644 Practice for Hot Plate Digestion of Dust Wipe 3.1 Definitions—For definitions of terms not appearing here,
Samples for the Determination of Lead see Terminologies D1356, E456, and E1605.
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-
E1727 Practice for Field Collection of Soil Samples for strument produces a new analysis run.
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)3 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)3 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 4
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.

2
 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
3.2.7 method detection limit (MDL), n—the minimum con- sample digestates or extracts.
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
type x sampling media); (3) the extraction/digestion procedure 4. Summary of Test Method
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).5 Quality control (QC) samples are analyzed
value that is used to provide a lower Pb concentration limit for along with sample digestates or extracts in order to ensure
reporting quantitative analysis data for a given analytical adequate instrumental performance.
method. NOTE 2—Digestion is an example of an extraction process. Other
3.2.8.1 Discussion—Any sample that generates a lead mea- examples of extraction processes are ultrasonic extraction (4) and leaching
(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
sample for instrumental analysis. 5.1 Environmental (including workplace) samples obtained
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 5
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.

3
 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 D2 or H2 continuum background correction preferably in a fume hood. Commercial, automatic systems are
(7). available that perform a similar process.
6.1.2 High concentrations (for example, 100- to 1000-fold
excess compared to lead concentration) of calcium, sulfate, 9.2 Alternatively, soak glassware and plastic equipment in
phosphate, iodide, fluoride, or acetate can interfere with lead volume fraction 35 % (volume/volume 1+1) nitric acid and
determination by GFAAS (7, 8). These interferences can be water in a plastic tub preferably in a working hood with the
corrected by standard addition techniques (9). hood sash down, rinse three times with ASTM Type I Water,
6.1.3 Other sources of interference may be found for various and allowed to dry preferably in a fume hood.
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
7.1 Analytical Instrumentation—The instrumentation used appropriate to the matrix of interest, using Test Method D4532,
shall consist of one or more of the following apparatus: Practices D6966, D7144, E1727, E1728, E1729, E2271/
7.1.1 Graphite Furnace Atomic Absorption Spectrometer E2271M, E3074/E3074M, or Guide D8358, or combinations
(GFAAS), equipped with background correction, lead hollow thereof.
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
NOTE 3—For lead, the 283.3 nm line is normally preferred over the E2914/E2914M.
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.
7.3 Vinyl Gloves, powderless. NOTE 6—In the United States of America, laboratories performing
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
8.1 Water—Unless otherwise indicated, references to water information when reporting the results.
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

4
 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
using the same final nitric acid concentration present in the the specifications for these instrumental QC standards requires
sample digestates/extracts. complete recalibration. Sample digestates or extracts cannot be
12.3.3 The ICV is used to assess the accuracy of the measured under these conditions. It is recommended that
calibration standards. It shall therefore be made from a standards be prepared anew prior to re-calibration.
different original source of stock solutions than the stock used 12.5.2 High-Calibration Standard Rerun—Failure to meet
to make the calibration standards. Use of a different serial specifications for this instrumental QC standard requires com-
dilution of the same original stock solution is not acceptable. plete re-calibration. Sample digestates/extracts cannot be mea-
12.4 Procedure for Calibration and Instrumental sured under conditions where these specifications are not met.
Measurement—Perform the calibration and quantitative lead It is recommended that the standard range be reduced prior to
measurement of sample digestates or extracts and instrumental recalibration.
QC samples in the sequential order outlined in Table 2. 12.5.3 CCV—Failure to meet the specifications for these
12.4.1 It is generally recommended to perform a semiquan- instrumental QC standards indicates excessive instrumental
titative screen prior to quantitative analysis for sample drift. Sample digestates or extracts cannot be measured under
digestates/extracts containing unknown levels of lead. The these conditions, and any sample digestates or extracts mea-
purpose of this screen is to determine the serial dilution sured since the last passing CCV shall be reanalyzed. This
requirements of each sample digestate/extract necessary to situation requires either reanalysis of the standard until speci-
keep the instrumental response within the calibration curve. All fications are met or re-calibration. All measurements on sample
digestates are diluted to a constant large value (1 to 1000 for digests or extracts shall be bracketed by a CCV that meets
GFAAS) during a semiquantitative screen. The instrument is specifications.
calibrated, and diluted digestates/extracts are analyzed without 12.5.4 CCB—Failure to meet the specifications for these
inserting the instrumental QC used for a quantitative analysis instrumental QC standards suggests the presence of possible
run. Data from this screen are then reviewed to calculate the instrumental carryover or baseline shift. Such a failure will
optimum serial dilution required for each digestate or extract have the most impact on sample digestates or extracts having
sample solution. The optimum dilution is one that achieves the lead concentrations in the low range of the calibration line at
maximum lead response that is still within the calibration the lower end of the calibration curve. The first corrective
curve. action is to reanalyze the CCB. The rinse time between the

TABLE 1 Instrumental QC Standards and Specifications

Name Use Specification
Initial calibration blank (ICB) initial calibration and zeroing calibration standard containing no analyte
instrument measured before and after calibration
measured value shall be less than five times method
detection limit (MDL)

Calibration standards instrument calibration matrix matched to digestates/extracts

high standard rerun used to check measured prior to measuring any sample digestates or
for carryover and instrumental drift extracts
correlation coefficient of $0.995, as measured using
linear regression on instrument response versus
concentration
highest level calibration standard is measured after
calibration; measured value within ±10 % of known value

Initial calibration verification (ICV) verify calibration standard levels analyte concentration near mid-range of calibration line
made from stock solution from different lot or vendor
than calibration standards
measured after calibration and before measuring sample
digestates/extracts
measured value within ±10 % of known value

Continuing calibration verification verify freedom from excessive analyte concentration near mid-range of calibration line
(CCV) instrumental drift analyzed before and after all sample digestates/extracts,
and at a frequency not less than once every ten samples
measured value within ±10 % of known value

Continuing calibration blank verify blank response and calibration standard containing no analyte
(CCB) freedom from carryover analyzed after the CCV
measured value less than five times MDL

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 D8568 − 24
TABLE 2 Example Recommended Analysis Run Order
Run Order No. Sample Identification Comments
1 ICB calibration blank instrument calibration
2 to 4 low, med, high, calibration standards
standards
5 ICB calibration blank calibration verification
6 ICV made from different stock, level
near midpoint of curve
7 high standard calibration standard linearity check
8 CCB same as calibration blank
9 CCB continuing calibration blank carryover check
10 CCV carryover check drift check; same as near
midpoint
calibration standard
11 CCB carryover check
*** start repeating cycle of samples—instrumental QC here ***
12 to 20 sample IDs sample digestates/extracts maximum of 10 samples
21 to 22 CCV, CCB drift check + carryover check see run Nos. 9 to 10
23 to 32 sample IDs sample digestates/extracts maximum of 10 samples
33 to 34 CCV, CCB drift check + carryover check see run Nos. 9 to 10
*** end repeating cycle of samples—QC standards here ***

samples should be increased and the analysis run continued if Ni = the number of times an unknown sample is to be
the CCB passes. If the instrument response remains elevated analyzed (usually one), and
and has not changed significantly, the instrument can be Nb = the number of blank media digestates/extracts
re-zeroed. This shall be followed by a CCV-CCB and reanaly- analyzed, which is greater than or equal to seven.
sis of all samples since the last passing CCB that are within five
times the response of the failed CCB. 13.1.2.1 When Ni = 1 and Nb = 7, Eq 2 is simplified to:
MDL = 3.360 S (3)
13. Calculations
13.2 GFAAS Calibration Curve—Prepare a calibration
13.1 Estimation of Method Detection Limit—The MDL shall curve to convert the instrument response (absorbance) to
be calculated at least annually. There are many ways to concentration of lead (µg/mL) using a linear regression fit.
estimate an MDL. Each involves the use of sampling media Convert all instrumental measurements on instrumental QC
digestates/extracts at low analyte concentration. The two meth- standards and sample digests or extracts to lead concentrations
ods discussed in 13.1.1 and 13.1.2 are in common use. Liquid (in µg/mL) using the calibration line.
standard spiking of clean matrix material is allowed for the
determination of an MDL. 13.3 Calculation of Lead Concentration in Sample
13.1.1 To estimate an MDL extract/digest, a minimum of Digestate/Extract—Calculate the lead concentration in the
seven spiked samples with concentration of no more than five sample digest or extract after instrumental analysis as follows:
times the expected MDL (this necessitates making an educated measured lead in sample solution, µg/mL = ~ A i !~ D ! (4)
guess as to the MDL) and determine the standard deviation of where:
the results (10). The MDL is the standard deviation multiplied
Ai = instrumentally measured lead concentration, µg/mL,
by 3.143, a factor from the Tables of Student “t” Values for
and
seven samples at the 99 % confidence limit:
D = dilution factor, mL/mL, required during instrumental
MDL = 3.143 S (1) analysis to produce a measured lead level within the
13.1.2 Another method that may be used to estimate an calibration curve.
MDL but does not require an estimate of the (actual) MDL can 13.4 Calculation of Lead Concentration in Original
be found in example references (Test Method D6785; 11). The Samples—Calculation of the lead levels in the originally
process involves analysis of the digestates or extracts from a digested or extracted samples is dependent upon the sample
minimum of seven samples of the blank matrix. The standard matrix (dust, soil, airborne particulate, or paint) and sample
deviation of the results is calculated and entered into a preparation procedure. For sample digestates or extracts gen-
relationship that considers the degrees of freedom of the erating lead measurements falling below the quantitation limit,
process: the value of the quantitation limit is used for performance
MDL 5 tS @ ~ N i 1 N b ! ⁄ ~ N i N b ! # 0.5 (2) calculations. A less than sign (<) is used on lead analysis results
from such calculations to indicate the uncertainty of these
where: values. The following subsections describe calculations for
MDL = the method detection limit, each of these matrices:
T = the Student T statistic for n = 7 (t = 3.143), 13.4.1 Airborne Particulate—Airborne particulate samples
S = the standard deviation of the analyte concentration
should be collected using Test Method D4532 or Guide D8358.
found in the blank media digestates/extracts,
Calculate the airborne concentration of lead as follows:

6
 D8568 − 24
Lead concentration, µg/m 3 5 @ ~ C !~ v ! 2 B # ⁄ V (5) where:
where: A = measured lead concentration in sample digestate or
extract from 13.3,
C = measured lead concentration in sample digestate or
B = final dilution volume, mL, and
extract, µg/mL, C = collection area, cm2.
v = final dilution volume, mL,
B = total lead in the blank, µg, and 13.4.5.2 Lead Mass per Unit Mass of Sample:
V = air volume collected, m3. lead content, µg/cm 2 5 @ ~ A ! ~ B ! # ⁄ @ ~ C ! ~ 1000! # (11)
13.4.2 Lead in Dust Wipes—Dust wipe samples should be where:
collected using Practices D6966, E1728, E2271/E2271M, A = measured lead content in sample digestate or extract
E3074/E3074M, or Guide E2115, or combinations thereof, from 13.3,
with wipes meeting Specification E1792. Wipes should be B = final dilution volume, mL, and
prepared for subsequent analysis following Practices E1644, C = sample mass, g.
E1979, E2913/E2913M, or E2914/E2914M.
13.4.5.3 Lead Mass per Sample:
lead concentration, µg/cm 2 5 @ ~ A ! ~ B ! # ⁄ ~ C ! (6)
lead concentration, µg/filter 5 @ ~ A ! ~ B ! # (12)
where: where:
A = measured lead concentration in sample digestate or A = measured lead content in sample digestate or extract
extract from 13.3, from 13.3, and
B = final dilution volume, mL, and B = final dilution volume, mL.
C = collection area, cm2.
13.5 Calculation of the lead levels in the originally digested
13.4.2.1 Lead Mass per Sample: QC samples is dependent on the sample matrix (dust, soil, or
lead content, µg/wipe = @ ~ A !~ B ! # (7) paint) and sample preparation procedure. The previous calcu-
lations in 13.3 are examples of each of these matrices.
where:
A = measured lead concentration in sample digestate or 14. Quality Assurance (QA)
extract from 13.3, and
B = final dilution volume, mL. 14.1 Analysis Procedures—The performance of the lead
analysis procedures on QC samples shall meet the specifica-
13.4.3 Lead in Dust by Micro-vacuuming—Settled dust tions listed in Tables 1 and 2.
should be collected by means of micro-vacuum sampling using 14.1.1 Performance criteria for lead analyses of environ-
Practice D7144. mental samples have been recommended (12). Performance
lead content, µg/m 2 or µg/ft2 5 @ ~ A ! ~ B ! # ⁄ ~ C ! (8) criteria for measurement accuracy, precision, sample size, and
working range for lead analyses have been delineated in
where: Practice E1775. Although this test method does not deal
A = measured lead concentration in sample digestate or specifically with sample preparation aspects of the overall
extract, µg/mL, from 14.3, analysis, the performance of the overall analytical method
B = final dilution volume, mL, and should meet the minimum performance criteria stated in
C = collection area, cm2 or ft2. Practice E1775.
13.4.4 Lead in Soil—Soil samples should be collected 14.2 QA System—The QA system shall meet the require-
following Practices E1727, E2271/E2271M, E3074/E3074M, ments of Practice E1864. Before and during analyses, follow
or Guide E2115, or combinations thereof, and they should be QA/QC procedures delineated in Practices D4210 and E1188
prepared for subsequent analysis in accordance with Practices and Guides D4697 and D4840.
E1726 or E1979. 14.3 External Quality Assessment—For laboratories that
lead concentration, µg/g 5 @ ~ A ! ~ B ! # ⁄ ~ C ! (9) carry out lead in air analysis on a regular basis, it is strongly
recommended to participate in relevant external quality assess-
where: ment or proficiency testing schemes.
A = measured lead concentration in sample digestate or
extract, from 13.3, 15. Record Keeping
B = final dilution volume, mL, and
15.1 Records shall be maintained in accordance with Prac-
C = sample mass, g.
tice E2239, and shall include a copy of the field collection
13.4.5 Lead in Paint—Paint samples should be collected report.
following Practice E1729 or Guide E2115, or both, and they
should be prepared for subsequent analysis using Practices 16. Report
E1645 or E1979. 16.1 Data to report include sample receipt information, all
13.4.5.1 Lead Mass per Unit Sample Area: final field sample analysis results, and instrument QC data.
lead concentration, mg/cm 2 5 @ ~ A ! ~ B ! # ⁄ @ ~ C ! ~ 1000! # (10) 16.2 The test report shall contain the following information:

7
 D8568 − 24
16.2.1 A statement that the laboratory conforms to Practice applicable analytical range was reported to be 0.01 µg to 0.5 µg
E1583, or is recognized for lead analysis as promulgated by an Pb per sample, without dilution.
authority having jurisdiction, or both; 17.4 Microwave Digestion—Interlaboratory analysis of lead
16.2.2 A statement to indicate the confidentiality of the in various reference materials (paint, dust, and soil) has
information supplied, if appropriate; demonstrated the equivalence of microwave digestion and hot
16.2.3 A reference to this test method; plate digestion followed by GFAAS determination of lead (14).
16.2.4 The type(s) of instrument(s) used for sample prepa-
17.5 Ultrasonic Extraction—Ultrasonic extraction with
ration and analysis, and unique identifier(s);
electrochemical detection of lead was evaluated against hot
16.2.5 The estimated detection limit under the working
plate extraction and GFAAS for air samples collected from
analytical conditions;
construction sites (15). For air filter and bulk CRMs, the test
16.2.6 Any operation not specified in this test method, or
procedure using ultrasonic extraction was found to be equiva-
regarded as optional;
lent to that using hot plate digestion. While alternative,
16.2.7 The name of the analyst(s) (or other unique identifi- equivalent analysis methods have been evaluated (16), interla-
er(s)); boratory data are not yet available for this extraction procedure
16.2.8 The date of the analysis; and followed by GFAAS analysis.
16.2.9 Any inadvertent deviations, unusual occurrences, or
other notable observations. 17.6 Bias—For lead determinations by GFAAS, bias de-
pends on both the sample preparation procedure and analysis
16.3 QC analysis data to report shall include results for procedures used. Biases for analytical methods used in proce-
method blanks, spike and spike duplicate recoveries, and range dures that are equivalent to ASTM sample preparation and
of duplicate percent recoveries. analysis procedures are typically less than 65 % (14, 15, 16);
the principal contributor to overall method bias ordinarily
17. Precision and Bias arises from the sample preparation procedure. In some
17.1 The precision and bias for this analysis method are instances, hot plate digestion of environmental CRMs by
dependent on both the choice of GFAAS analytical instrumen- procedures that are equivalent to Practices E1644, E1645,
tation and components, the sample type, sampling media (if E1726, and E1741 can yield recoveries that are significantly
applicable), and the sample digestion or extraction procedures less than 100 % (17). For example, some soil CRMs have been
used for preparing the samples. found to give lead recoveries of 80 % to 85 % (15, 16). This is
due to the possible presence of refractory compounds that are
17.2 Precision—Practice E691 (or an equivalent procedure) insoluble when using the reference sample preparation proce-
was used to estimate method precision as applied to a lead in dures; the use of hydrofluoric acid (HF) is needed to achieve
various certified reference material (CRM) matrices. Practice 100 % recovery from such samples (see, for example, Test
E691 specifies interlaboratory analysis using a minimum of six Method D7035). However, the use of HF in occupational
laboratories, at least four concentration or loading levels, and at hygiene laboratories is generally discouraged for safety rea-
least two determinations for each of the four sample loading sons. During spectrometric analysis, matrix matching is crucial
levels. to minimizing bias.
17.3 Hot Plate Digestion—The precision of the GFAAS
measurement procedure after hot plate digestion was found to 18. Keywords
be less than 0.05 for airborne particulate CRMs in the range 18.1 hazard assessment; instrumental analysis; quantitative
0.1 µg to 4.5 µg per sample (13). No bias was identified. The measurement

REFERENCES

(1) HSE MDHS 6/3, Lead and Inorganic Compounds of Lead in Air – (5) U.S. EPA, Hazardous Waste Test Methods / SW-846; Method 1311.
Laboratory Method Using Flame Atomic Absorption Spectrometry or U.S. Environmental Protection Agency: Washington, DC, 1992.
Electrothermal Atomic Absorption Spectrometry; in Methods for the (6) Slavin, W., Atomic Absorption Spectroscopy, 2nd ed. Wiley: New
Determination of Hazardous Substances. Health and Safety Executive York, 1978.
(HSE): London, UK, 1998; ISBN: 0–7176–1517–0. (7) M. T.C. de Loos-Vollebregt, Background Correction Methods in
(2) NIOSH Method 7105, Lead by GFAAS; in NIOSH Manual of Atomic Absorption Spectrometry; in Encyclopedia of Analytical
Analytical Methods, 4th ed., Eller, P. M., Cassinelli, M.E., Eds. Chemistry. Wiley: New York, 2013; doi: 10.1002/
National Institute for Occupational Safety and Health (NIOSH): 9780470027318.a5104.pub2.
Cincinnati, OH, 1994. (8) Smith, S. B., and Hieftje, G. M., A New Background-Correction
(3) Borges, D. L. B., Graphite Furnace Atomic Absorption Spectrometry; Method for Atomic Absorption Spectrometry. Spectroscopy, Vol. 37,
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Instrumentation. Wiley: New York, 2022; doi:10.1002/ (9) Skoog, D., West, D. M., and Holler, F.J., Fundamentals of Analytical
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(4) Ashley, K., Ultrasonic extraction of heavy metals from environmental (10) Kennedy, E. R., Fischbach, T. J., Song, R., Eller, P. M. and Shulman,
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(11) U.S. EPA, Definition and Procedure for the Determination of the Journal, 1996, Vol. 57, p. 1035.
Method Detection Limit, Revision 2. U.S. Environmental Protection (15) Ashley, K., Mapp, K. J., and Millson, M., Ultrasonic Extraction and
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Agency: Washington, DC, 1992; EPA 747-R-92-001. (16) Ashley, K., Schlecht, P. C., Song, R., Feng, A., Dewalt, G., and
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