ASTM E3193-23
(Test Method)Standard Test Method for Measurement of Lead (Pb) by Flame Atomic Absorption Spectrophotometry (FAAS)
Standard Test Method for Measurement of Lead (Pb) by Flame Atomic Absorption Spectrophotometry (FAAS)
SIGNIFICANCE AND USE
5.1 This test method is intended for use with other standards that address the collection and preparation of samples (airborne particulate, dusts by wipe and micro-vacuuming, dried paint chips, and soils) that are obtained during the assessment or mitigation of lead hazards from buildings and related structures.
5.2 Laboratories analyzing samples obtained during the assessment or mitigation of lead hazards from buildings and related structures shall conform to Practice E1583, or shall be recognized for lead analysis as promulgated by authorities having jurisdiction, or both.
Note 2: In the United States of America, laboratories performing analysis of samples collected during lead-based paint activities are required to be accredited to ISO/IEC 17025 and to other requirements promulgated by the Environmental Protection Agency (EPA).
5.3 This test method may also be used to analyze similar samples from other environments such as toxic characteristic extracts of waste sampled using Guide E1908, and soil and sludge as prepared for analysis using U.S. EPA SW-846 Test Method 1311.
SCOPE
1.1 This test method covers the determination of lead (Pb) in airborne particulate, dust by wipe and micro-vacuuming, paint, and soil collected in and around buildings and related structures by flame atomic absorption spectrophotometry (FAAS) and is derived from Test Methods D4185 and E1613.
1.2 The sensitivity, detection limit, and optimum working concentration for lead (Pb) are given in Table 1.
1.3 The values stated in SI units are to be regarded as standard. No other values of measurement are included in this standard.
1.3.1 Exception—The SI and inch-pound units shown for wipe and micro-vacuuming sampling data are to be individually regarded as standard for wipe and micro-vacuuming sampling data (14.4.2 and 14.4.3).
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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.
General Information
- Status
- Published
- Publication Date
- 31-Oct-2023
- Technical Committee
- D22 - Air Quality
- Drafting Committee
- D22.12 - Sampling and Analysis of Lead for Exposure and Risk Assessment
Relations
- Effective Date
- 01-Nov-2023
- Effective Date
- 01-Apr-2024
- Effective Date
- 01-Apr-2024
- Effective Date
- 01-Apr-2024
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Apr-2022
- Effective Date
- 01-Apr-2022
- Effective Date
- 01-Sep-2020
- Effective Date
- 01-Sep-2020
- Effective Date
- 01-Sep-2020
- Referred By
ASTM E1792-20 - Standard Specification for Wipe Sampling Materials for Lead in Surface Dust - Effective Date
- 01-Nov-2023
- Effective Date
- 01-Nov-2023
- Effective Date
- 01-Nov-2023
Overview
ASTM E3193-23: Standard Test Method for Measurement of Lead (Pb) by Flame Atomic Absorption Spectrophotometry (FAAS) establishes the procedures for accurately determining lead concentration in various environmental samples, including airborne particulate, dust (by wipe and micro-vacuuming), paint, and soil. Developed by ASTM International, this standard is crucial for professionals involved in environmental assessment, remediation, and occupational safety, particularly during the evaluation or mitigation of lead hazards in and around buildings and related structures.
By providing a robust framework for the precise measurement of lead using FAAS, ASTM E3193-23 supports compliance with regulatory requirements, enhances laboratory quality assurance, and ensures public and occupational health.
Key Topics
Sample Collection and Preparation
The method works in conjunction with other ASTM standards that specify proper procedures for collecting and preparing samples such as dust wipes, micro-vacuumed particulates, paint chips, and soil.Analytical Procedure
Samples are digested or extracted and analyzed for lead using flame atomic absorption spectrophotometry. Calibration with standards and periodic verification ensure analytical accuracy.Quality Control
The method incorporates rigorous quality control procedures, requiring analysis of blanks, calibration checks, and ongoing verification to maintain data integrity. Laboratories must comply with ASTM E1583 or equivalent authority-recognized protocols.Detection Limits and Sensitivity
The detection limit for lead (Pb) is 0.02 µg/mL, with an optimum linear range up to 10 µg/mL under ideal conditions, facilitating precise analysis across a variety of sample types.Accreditation Requirements
Laboratories conducting lead analysis must have proper accreditation, such as ISO/IEC 17025 and, in the United States, certification through relevant Environmental Protection Agency (EPA) programs.Interferences and Corrections
The method addresses possible spectral, background, chemical, and physical interferences encountered during FAAS lead measurement and prescribes techniques for minimizing or correcting these effects.
Applications
ASTM E3193-23 is widely used in the following contexts:
Lead Hazard Assessment and Abatement
Essential for environmental professionals assessing lead contamination prior to renovation, repair, or demolition of buildings. It supports risk evaluation and clearance examination processes.Regulatory Compliance Testing
Required for meeting local and federal standards such as the U.S. EPA’s 40 CFR 745, especially in lead-based paint hazard control and workplace air monitoring.Soil, Waste, and Paint Analysis
Applicable to lead determination in soil samples near structures, debris and waste streams subject to EPA’s Toxicity Characteristic Leaching Procedure, and dried paint chip analysis.Laboratory Accreditation and Quality Assurance
Laboratories can leverage this standard to adhere to industry best practices, assure clients of data quality, and support international recognition of analytical competence.
Related Standards
Understanding and implementing ASTM E3193-23 often involves referencing these key related standards and regulations:
Sample Collection and Preparation
- ASTM D6966, E1727, E1728, E1729, E2271, D7144: Field collection protocols for dust, soil, and paint
- ASTM E1644, E1645, E1726, E1979, E2913, E2914: Sample digestion and preparation methods
Analytical Support and Laboratory Practices
- ASTM E1583: Practice for evaluating laboratories for lead analysis
- ISO/IEC 17025: Accreditation for testing and calibration laboratories
- EPA SW-846 Test Method 1311: Toxicity Characteristic Leaching Procedure
Regulatory Guidance
- 40 CFR 745: U.S. regulations on lead-based paint hazards
- EPA National Lead Laboratory Accreditation Program (NLLAP)
For comprehensive lead hazard identification and mitigation, practitioners should utilize ASTM E3193-23 in combination with these referenced standards to ensure accurate, reliable, and compliant results in environmental lead testing.
Keywords: ASTM E3193-23, lead measurement, flame atomic absorption spectrophotometry (FAAS), environmental lead testing, dust wipe sampling, laboratory accreditation, lead hazard assessment, EPA 40 CFR 745, ISO/IEC 17025, lead in paint, lead in soil, building renovation, lead abatement, quality control in laboratories.
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Frequently Asked Questions
ASTM E3193-23 is a standard published by ASTM International. Its full title is "Standard Test Method for Measurement of Lead (Pb) by Flame Atomic Absorption Spectrophotometry (FAAS)". This standard covers: SIGNIFICANCE AND USE 5.1 This test method is intended for use with other standards that address the collection and preparation of samples (airborne particulate, dusts by wipe and micro-vacuuming, dried paint chips, and soils) that are obtained during the assessment or mitigation of lead hazards from buildings and related structures. 5.2 Laboratories analyzing samples obtained during the assessment or mitigation of lead hazards from buildings and related structures shall conform to Practice E1583, or shall be recognized for lead analysis as promulgated by authorities having jurisdiction, or both. Note 2: In the United States of America, laboratories performing analysis of samples collected during lead-based paint activities are required to be accredited to ISO/IEC 17025 and to other requirements promulgated by the Environmental Protection Agency (EPA). 5.3 This test method may also be used to analyze similar samples from other environments such as toxic characteristic extracts of waste sampled using Guide E1908, and soil and sludge as prepared for analysis using U.S. EPA SW-846 Test Method 1311. SCOPE 1.1 This test method covers the determination of lead (Pb) in airborne particulate, dust by wipe and micro-vacuuming, paint, and soil collected in and around buildings and related structures by flame atomic absorption spectrophotometry (FAAS) and is derived from Test Methods D4185 and E1613. 1.2 The sensitivity, detection limit, and optimum working concentration for lead (Pb) are given in Table 1. 1.3 The values stated in SI units are to be regarded as standard. No other values of measurement are included in this standard. 1.3.1 Exception—The SI and inch-pound units shown for wipe and micro-vacuuming sampling data are to be individually regarded as standard for wipe and micro-vacuuming sampling data (14.4.2 and 14.4.3). 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 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.
SIGNIFICANCE AND USE 5.1 This test method is intended for use with other standards that address the collection and preparation of samples (airborne particulate, dusts by wipe and micro-vacuuming, dried paint chips, and soils) that are obtained during the assessment or mitigation of lead hazards from buildings and related structures. 5.2 Laboratories analyzing samples obtained during the assessment or mitigation of lead hazards from buildings and related structures shall conform to Practice E1583, or shall be recognized for lead analysis as promulgated by authorities having jurisdiction, or both. Note 2: In the United States of America, laboratories performing analysis of samples collected during lead-based paint activities are required to be accredited to ISO/IEC 17025 and to other requirements promulgated by the Environmental Protection Agency (EPA). 5.3 This test method may also be used to analyze similar samples from other environments such as toxic characteristic extracts of waste sampled using Guide E1908, and soil and sludge as prepared for analysis using U.S. EPA SW-846 Test Method 1311. SCOPE 1.1 This test method covers the determination of lead (Pb) in airborne particulate, dust by wipe and micro-vacuuming, paint, and soil collected in and around buildings and related structures by flame atomic absorption spectrophotometry (FAAS) and is derived from Test Methods D4185 and E1613. 1.2 The sensitivity, detection limit, and optimum working concentration for lead (Pb) are given in Table 1. 1.3 The values stated in SI units are to be regarded as standard. No other values of measurement are included in this standard. 1.3.1 Exception—The SI and inch-pound units shown for wipe and micro-vacuuming sampling data are to be individually regarded as standard for wipe and micro-vacuuming sampling data (14.4.2 and 14.4.3). 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.5 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.
ASTM E3193-23 is classified under the following ICS (International Classification for Standards) categories: 13.040.20 - Ambient atmospheres; 91.010.01 - Construction industry in general. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM E3193-23 has the following relationships with other standards: It is inter standard links to ASTM E3193-21, ASTM E1729-24, ASTM E1792-24, ASTM E3074/E3074M-24, ASTM E2239-24, ASTM E1908-24, ASTM E1727-24, ASTM E456-13a(2022)e1, ASTM E456-13a(2022), ASTM E1908-20, ASTM E3074/E3074M-20, ASTM E2239-20, ASTM E1792-20, ASTM D7439-21, ASTM E1727-20. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM E3193-23 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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: E3193 − 23
Standard Test Method for
Measurement of Lead (Pb) by Flame Atomic Absorption
Spectrophotometry (FAAS)
This standard is issued under the fixed designation E3193; 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 D4185 Test Method for Measurement of Metals in Work-
place Atmospheres by Flame Atomic Absorption Spectro-
1.1 This test method covers the determination of lead (Pb)
photometry
in airborne particulate, dust by wipe and micro-vacuuming,
D4210 Practice for Intralaboratory Quality Control Proce-
paint, and soil collected in and around buildings and related
dures and a Discussion on Reporting Low-Level Data
structures by flame atomic absorption spectrophotometry
(Withdrawn 2002)
(FAAS) and is derived from Test Methods D4185 and E1613.
D4532 Test Method for Respirable Dust in Workplace At-
1.2 The sensitivity, detection limit, and optimum working
mospheres Using Cyclone Samplers
concentration for lead (Pb) are given in Table 1.
D4697 Guide for Maintaining Test Methods in the User’s
Laboratory (Withdrawn 2009)
1.3 The values stated in SI units are to be regarded as
standard. No other values of measurement are included in this D4840 Guide for Sample Chain-of-Custody Procedures
D6785 Test Method for Determination of Lead in Workplace
standard.
1.3.1 Exception—The SI and inch-pound units shown for Air Using Flame or Graphite Furnace Atomic Absorption
Spectrometry
wipe and micro-vacuuming sampling data are to be individu-
ally regarded as standard for wipe and micro-vacuuming D6966 Practice for Collection of Settled Dust Samples
Using Wipe Sampling Methods for Subsequent Determi-
sampling data (14.4.2 and 14.4.3).
nation of Metals
1.4 This standard does not purport to address all of the
D7035 Test Method for Determination of Metals and Met-
safety concerns, if any, associated with its use. It is the
alloids in Airborne Particulate Matter by Inductively
responsibility of the user of this standard to establish appro-
Coupled Plasma Atomic Emission Spectrometry (ICP-
priate safety, health, and environmental practices and deter-
AES)
mine the applicability of regulatory limitations prior to use.
D7144 Practice for Collection of Surface Dust by Micro-
1.5 This international standard was developed in accor-
vacuum Sampling for Subsequent Determination of Met-
dance with internationally recognized principles on standard-
als and Metalloids
ization established in the Decision on Principles for the
E456 Terminology Relating to Quality and Statistics
Development of International Standards, Guides and Recom-
E631 Terminology of Building Constructions
mendations issued by the World Trade Organization Technical
E691 Practice for Conducting an Interlaboratory Study to
Barriers to Trade (TBT) Committee.
Determine the Precision of a Test Method
E1188 Practice for Collection and Preservation of Informa-
2. Referenced Documents
2 tion and Physical Items by a Technical Investigator
2.1 ASTM Standards:
E1583 Practice for Evaluating Laboratories Engaged in De-
D1193 Specification for Reagent Water
termination of Lead in Paint, Dust, Airborne Particulates,
D1356 Terminology Relating to Sampling and Analysis of
and Soil Taken From and Around Buildings and Related
Atmospheres
Structures
E1605 Terminology Relating to Lead in Buildings
This test method is under the jurisdiction of ASTM Committee D22 on Air
E1613 Test Method for Determination of Lead by Induc-
Quality and is the direct responsibility of Subcommittee D22.12 on Sampling and
tively Coupled Plasma Atomic Emission Spectrometry
Analysis of Lead for Exposure and Risk Assessment.
(ICP-AES), Flame Atomic Absorption Spectrometry
Current edition approved Nov. 1, 2023. Published November 2023. Originally
approved in 2019. Last previous edition approved in 2021 as E3193 – 21. DOI: (FAAS), or Graphite Furnace Atomic Absorption Spec-
10.1520/E3193-23.
trometry (GFAAS) Techniques (Withdrawn 2021)
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3193 − 23
TABLE 1 FAAS Instrumental Detection Limit and Optimum Working Concentration for Lead (Pb)
Detection Limit, μg/mL
Optimum Linear Range Upper Limit, Elements, Compound Classes,
Element (approximately three times
μg/mL and Oxides
A
standard deviation of blank)
Inorganic compounds, airborne particulate, paint, dust by
Pb 0.02 10
wipe and micro-vacuuming, soil
A
Detection limit represents ideal laboratory conditions; variability due to sampling, digestion, reagents, and sample handling has not been taken into account.
E1644 Practice for Hot Plate Digestion of Dust Wipe 2.2 Code of Federal Regulations:
Samples for the Determination of Lead 40 CFR 745 Lead-Based Paint Poisoning Prevention in
E1645 Practice for Preparation of Dried Paint Samples by Certain Residential Structures
Hotplate or Microwave Digestion for Subsequent Lead
2.3 Governmental Agency Guidance:
Analysis
U.S. Environmental Protection Agency National Lead Labo-
E1726 Practice for Preparation of Soil Samples by Hotplate
ratory Accreditation Program (NLLAP)
Digestion for Subsequent Lead Analysis U.S. Environmental Protection Agency SW-846 Test Method
E1727 Practice for Field Collection of Soil Samples for 1311: Toxicity Characteristic Leaching Procedure
Subsequent Lead Determination
2.4 ISO Standard:
E1728 Practice for Collection of Settled Dust Samples Using
ISO/IEC 17025 General requirements for the competence of
Wipe Sampling Methods for Subsequent Lead Determi-
testing and calibration laboratories
nation
E1729 Practice for Field Collection of Dried Paint Samples
3. Terminology
for Subsequent Lead Determination
3.1 Definitions—For definitions of terms used in this test
E1741 Practice for Preparation of Airborne Particulate Lead
method, refer to Terminologies D1356, E456, E631, and
Samples Collected During Abatement and Construction
E1605.
Activities for Subsequent Analysis by Atomic Spectrom-
3.2 Definitions of Terms Specific to This Standard:
etry (Withdrawn 2009)
3.2.1 analysis run, n—a period of measurement time on a
E1792 Specification for Wipe Sampling Materials for Lead
given analytical instrument during which data are calculated
in Surface Dust
from a single calibration curve (or single set of curves).
E1864 Practice for Evaluating Quality Systems of Organi-
3.2.1.1 Discussion—Recalibration of a given instrument
zations Conducting Facility and Hazard Assessments for
produces a new analysis run.
Lead in Paint, Dust, Airborne Particulate, and Soil in and
3.2.2 calibration standards, n—solutions of known analyte
around Buildings and Related Structures (Withdrawn
3 concentrations used to calibrate instruments.
2011)
3.2.2.1 Discussion—Calibration standards must be matrix
E1908 Practice for Sample Selection of Debris Waste from a
matched to the acid content present in sample digestates or
Building Renovation or Lead Abatement Project for Tox-
extracts and must be measured prior to analyzing samples.
icity Characteristic Leaching Procedure (TCLP) Testing
3.2.3 initial calibration blank (ICB), n—a standard contain-
for Leachable Lead (Pb)
ing no analyte that is used for the initial calibration and zeroing
E1979 Practice for Ultrasonic Extraction of Paint, Dust,
of the instrument response.
Soil, and Air Samples for Subsequent Determination of
3.2.3.1 Discussion—The ICB must be matrix matched to the
Lead
acid content of sample extracts and digestates. The ICB must
E2115 Guide for Conducting Lead Hazard Assessments of
be measured during and after calibration. The measured value
Dwellings and of Other Child-Occupied Facilities
is to be (at most) less than five times the IDL.
E2239 Practice for Record Keeping and Record Preservation
3.2.4 initial calibration verification (ICV), n—a solution (or
for Lead Hazard Activities
set of solutions) of known analyte concentration used to verify
E2271/E2271M Practice for Clearance Examinations Fol-
calibration standard levels; the concentration of analyte is to be
lowing Lead Hazard Reduction Activities in Multifamily
near the mid-range of the linear curve that is made from a stock
Dwellings
E2913/E2913M Practice for Hotplate Digestion of Lead
from Composited Wipe Samples
Available from U.S. Government Publishing Office, 732 N. Capitol St., NW,
E2914/E2914M Practice for Ultrasonic Extraction of Lead
Washington, DC 20401, http://www.gpo.gov.
from Composited Wipe Samples
Available from United States Environmental Protection Agency (EPA), William
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
E3074/E3074M Practice for Clearance Examinations Fol-
http://www.epa.gov.
lowing Lead Hazard Reduction Activities in Single Fam-
Available from International Organization for Standardization (ISO), ISO
ily Dwellings, in Individual Units of Multifamily
Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
Dwellings, and in Other Child-Occupied Facilities Geneva, Switzerland, http://www.iso.org.
E3193 − 23
solution having a different manufacturer or manufacturer lot formed without inserting instrumental QC standards except for
identification than the calibration standards. calibration standards. Data from this run are used for deter-
3.2.4.1 Discussion—The ICV must be matrix matched to the mining serial dilution requirements for sample digestates or
acid content of sample extracts or digestates. The ICV must be extracts to keep them within the linear range of the instrument.
measured after calibration and before measuring any sample
3.2.12 serial dilution, n—a method of producing a less
digestates or extracts. The measured value is to fall within
concentrated solution through one or more consecutive dilution
610 % of the known value.
steps.
3.2.5 instrumental detection limit (IDL), n—the lowest con- 3.2.12.1 Discussion—A dilution step for a standard or
centration at which the instrumentation can distinguish analyte sample solution is performed by volumetrically placing a small
content from the background generated by a minimal matrix. aliquot (of known volume) of a higher concentrated solution
3.2.5.1 Discussion—The IDL is usually determined by the into a volumetric flask and diluting to volume with water
manufacturer. The IDL can be determined from blank, containing the same acid levels as those found in original
acidified, deionized, or ultrapure water as the matrix and from sample digestates or extracts.
the same calculation methods used to determine a method
3.2.13 spiked duplicate sample, n—two portions of a ho-
detection limit (MDL). Typical lead (Pb) IDL for FAAS is
mogenized sample that were targeted for addition of analyte
0.05 μg ⁄mL.
and fortified with all the target analytes before preparation.
3.2.6 instrumental QC standards, n—these provide informa- 3.2.13.1 Discussion—Analysis results for these samples are
tion on measurement performance during the instrumental used to provide information on the precision and bias of the
analysis portion of the overall analyte measurement process. overall analysis process.
They include CCBs, CCVs, ICBs, and ICVs.
3.2.14 spiked sample, n—a sample portion (split from an
3.2.7 method blank, n—a digestate or extract that reflects the original sample) to which an additional known amount of
maximum treatment given any one sample within a sample analyte has been added.
batch, except that no sample is placed into the digestion or 3.2.14.1 Discussion—Analysis results for spiked samples
extraction vessel. (The same reagents and processing condi- are used to provide information on the precision and bias of the
tions that are applied to field samples within a batch are also overall analysis process.
applied to the method blank.)
3.2.15 un-spiked sample, n—a portion of a homogenized
3.2.7.1 Discussion—Analysis results from method blanks
sample that was targeted for the addition of analyte but is not
provide information on the level of potential contamination
fortified with target analytes before sample preparation.
experienced by samples processed within the batch.
3.2.15.1 Discussion—Analysis results for this sample are
3.2.8 quantitation limit, n—an instrumental measurement used to correct for native analyte levels in the spiked and
value that is used to provide a lower concentration limit for spiked duplicate samples.
reporting quantitative analysis data for a given analytical
4. Summary of Test Method
method.
3.2.8.1 Discussion—Any sample that generates a lead mea-
4.1 A sample digestate or extract is analyzed for lead
surement below the quantitation limit is reported as a less-than
content using FAAS. Instrumental QC samples are analyzed
value using the quantitation limit value multiplied by the
along with sample digestates or extracts in order to ensure
appropriate dilution factors resulting from preparation of the
adequate instrumental performance.
sample for instrumental analysis.
NOTE 1—Digestion is an example of an extraction process. Other
3.2.9 quantitative analysis, n—an analysis run on sample
examples of extraction processes are ultrasonic extraction and leaching.
digestates or extracts (or serial dilutions thereof) that includes
4.2 Samples and standards are aspirated into the flame of an
instrumental QC standards.
absorption spectrophotometer. A lead (Pb) hollow cathode or
3.2.9.1 Discussion—Data from this analysis run are used to
electrodeless discharge lamp provides the characteristic radia-
calculate and report final lead analysis results.
tion energy for lead. The absorption of this characteristic
3.2.10 reporting limit, n—the lowest concentration of ana- energy by lead atoms in the flame is related to the concentra-
lyte in a sample that can be reported with a defined, reproduc-
tion of lead in the aspirated sample. The flame and operating
ible level of certainty. conditions for lead are listed in Table 2.
3.2.10.1 Discussion—This value is usually based on the low
5. Significance and Use
standard used for instrument calibration. For analyses in the
United States of America subject to 40 CFR 745 and the
5.1 This test method is intended for use with other standards
National Lead Laboratory Accreditation Program (NLLAP),
that address the collection and preparation of samples (airborne
the reporting limit for a specific sample matrix must be at least
particulate, dusts by wipe and micro-vacuuming, dried paint
twice the MDL for that same sample matrix.
chips, and soils) that are obtained during the assessment or
mitigation of lead hazards from buildings and related struc-
3.2.11 semiquantitative analysis, n—an analysis run that is
tures.
performed on highly diluted sample digestates or extracts for
the purpose of determining the approximate analyte level in the
digest. 7
The boldface numbers in parentheses refer to a list of references at the end of
3.2.11.1 Discussion—This analysis run is generally per- this standard.
E3193 − 23
TABLE 2 FAAS Flame and Operating Conditions for Lead (Pb)
Analytical Wavelength,
A A
Element Type of Flame Interferences Remedy Reference
nm
217.0 Ca, high concentration
B
Pb Air-C H (oxidizing) (1)
2 2 –2
283.3 SO
A
High concentrations of silicon in the sample can cause an interference and may cause aspiration problems. If large amounts of silica are extracted from the samples,
the samples should be allowed to stand for several hours and centrifuged or filtered to remove the silica.
B
Samples are periodically analyzed by the method of additions to check for chemical interferences. If interferences are encountered, determinations must be made by
the standard additions method or, if the interferent is identified, it may be added to the standards.
5.2 Laboratories analyzing samples obtained during the controlled by the addition of a high concentration of another
assessment or mitigation of lead hazards from buildings and easily ionized element which will buffer the electron concen-
related structures shall conform to Practice E1583, or shall be tration in the flame.
recognized for lead analysis as promulgated by authorities
6.5 Chemical interferences occur in FAAS when species
having jurisdiction, or both.
present in the sample cause variations in the degree to which
NOTE 2—In the United States of America, laboratories performing atoms are formed in the flame, or when different valence states
analysis of samples collected during lead-based paint activities are
of a single element have different absorption characteristics.
required to be accredited to ISO/IEC 17025 and to other requirements
Such interferences may be controlled by adjusting the sample
promulgated by the Environmental Protection Agency (EPA).
matrix or by the method of standard additions (3). Also, the use
5.3 This test method may also be used to analyze similar
of lanthanum as a releasing element minimizes the interference
samples from other environments such as toxic characteristic
from the formation of nonvolatile compounds in the flame.
extracts of waste sampled using Guide E1908, and soil and
Lanthanum forms nonvolatile compounds preferentially with
sludge as prepared for analysis using U.S. EPA SW-846 Test
the interferent so that the analyte remains free.
Method 1311.
6.6 Physical interferences may result if the physical prop-
erties of the samples vary significantly. Changes in viscosity
6. Interferences
and surface tension can affect the sample aspiration rate and
6.1 In FAAS, the occurrence of interferences is less com-
thus cause erroneous results. Sample dilution or the method of
mon than in many other analytical techniques. Interferences
standard additions, or both, are used to correct such interfer-
can occur, however, and when encountered are corrected as
ences. High concentrations of silica in the sample can cause
indicated in the following sections. The known interferences
aspiration problems. If large amounts of silica are extracted
and correction methods for lead are indicated in Table 2. The
from the samples, they shall be allowed to stand for several
methods of standard additions and background monitoring and
hours and centrifuged or filtered to remove the silica.
correction (2-5) are used to identify the presence of an
6.7 This procedure references matrix-specific methods for
interference. Insofar as possible, the matrix of sample and
sample preparation.
standard are matched to minimize possible interference.
6.2 Background or nonspecific absorption can occur from
7. Apparatus
particles produced in the flame, which can scatter light and
produce an apparent absorption signal. Light scattering may be
7.1 Analytical Apparatus:
encountered when solutions of high salt content are being
7.1.1 Flame Atomic Absorption Spectrophotometer,
analyzed. They are most severe when measurements are made
equipped with air/acetylene burner head.
at shorter wavelengths (for example, below about 250 nm).
7.1.2 Lead (Pb) Hollow Cathode or Electrodeless Dis-
Background absorption may also occur as the result of the
charge Lamp.
formation of various molecular species which can absorb light.
7.1.3 Deuterium Continuum Lamp.
The background absorption can be accounted for by the use of
7.1.4 Compressed Air—Appropriate pressure-reducing
background correction techniques (2).
regulator with base connections (see instrument manufacturer’s
6.3 Spectral interferences are those interferences which instructions).
result from an atom different from the one being measured that
7.1.5 Acetylene Gas and Regulator—A cylinder of acety-
absorbs a portion of the radiation. Such interferences are
lene equipped with a two-gauge, two-stage pressure-reducing
extremely rare in FAAS. In some cases, multi-element hollow
regulator with hose connections (see instrument manufactur-
cathode lamps may cause a spectral interference by having
er’s instructions).
closely adjacent emission lines from two different elements. In
7.1.6 Beakers, Phillips or Griffin, 125 mL, borosilicate
general, the use of multi-element hollow cathode lamps is
glass.
discouraged.
7.1.7 Centrifuge Tubes, 15 mL, graduated, plastic or boro-
silicate glass; or, tubes to fit the autosampler in use.
6.4 Ionization interference occurs when easily ionized at-
oms are being measured. The degree to which such atoms are 7.1.8 Miscellaneous Borosilicate Glassware (Pipets and
ionized is dependent upon the atomic concentration and the Volumetric Flasks)—All pipets and volumetric flasks shall be
presence of other easily ionized atoms. This interference can be calibrated Class A volumetric glassware.
E3193 − 23
8. Reagents 10. Safety Precautions
10.1 Hazards to personnel exist in the operation of the flame
8.1 Purity of Reagents—Reagent grade chemicals shall be
atomic absorption spectrophotometer. Do not operate any
used in all tests. Unless otherwise indicated, it is intended that
FAAS unit until the manufacturer’s instruction manual has
all reagents shall conform to the specifications of the Commit-
been read and completely understood. Follow all safety in-
tee on Analytical Reagents of the American Chemical Society,
structions in the manual and the safety requirements pertaining
where such specifications are available. Other grades may be
to the handling, storage, and use of compressed gases.
used provided that it can be demonstrated that they are of
sufficiently high purity to permit their use without decreasing
10.2 Hazards to personnel exist in all operations in which
the accuracy of the determinations.
hot, concentrated mineral acids are used. The appropriate
laboratory procedures for working with reagents of this nature
8.2 Purity of Water—Unless otherwise indicated, reference
shall be observed.
to water shall be understood to mean Type II reagent water
conforming to Specification D1193.
10.3 Lead and lead compounds are hazardous to health and
shall be handled in a manner consistent with the danger they
8.3 Hydrochloric Acid (HCl)—Concentrated hydrochloric
present.
acid, 12 N, specific gravity 1.19.
10.4 The instrument exhaust gases contain the combustion
8.4 Nitric Acid (HNO )—Redistilled, concentrated nitric
products of the flame as
...
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.
Designation: E3193 − 21 E3193 − 23
Standard Test Method for
Measurement of Lead (Pb) in Dust by Wipe, Paint, and Soil
by by Flame Atomic Absorption Spectrophotometry (FAAS)
This standard is issued under the fixed designation E3193; 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
1.1 This test method covers the determination of lead (Pb) in airborne particulate, dust by wipe, wipe and micro-vacuuming, paint,
and soil collected in and around buildings and related structures by flame atomic absorption spectrophotometry (FAAS) and is
derived from Test Methods D4185 and E1613. For determination of lead (Pb) and other metals in air by FAAS, see Test Method
D4185.
1.2 The sensitivity, detection limit, and optimum working concentration for lead (Pb) are given in Table 1.
1.3 The values stated in SI units are to be regarded as standard. No other values of measurement are included in this standard.
1.3.1 Exception—The SI and inch-pound units shown for wipe and micro-vacuuming sampling data are to be individually regarded
as standard for wipe and micro-vacuuming sampling data (14.4.114.4.2 and 14.4.3).
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D4185 Test Method for Measurement of Metals in Workplace Atmospheres by Flame Atomic Absorption Spectrophotometry
D4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data (Withdrawn
2002)
D4532 Test Method for Respirable Dust in Workplace Atmospheres Using Cyclone Samplers
D4697 Guide for Maintaining Test Methods in the User’s Laboratory (Withdrawn 2009)
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.12 on Sampling and Analysis
of Lead for Exposure and Risk Assessment.
Current edition approved Sept. 1, 2021Nov. 1, 2023. Published September 2021November 2023. Originally approved in 2019. Last previous edition approved in 20202021
as E3193E3193 – 21. – 20. DOI: 10.1520/E3193-21.DOI: 10.1520/E3193-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E3193 − 23
TABLE 1 FAAS Instrumental Detection Limit and Optimum Working Concentration for Lead (Pb)
Detection Limit, μg/mL
Optimum Linear Range Upper Limit, Elements, Compound Classes,
Element (approximately three times
μg/mL and Oxides
A
standard deviation of blank)
Pb 0.02 10 Inorganic compounds, paint, dust by wipe, soil
TABLE 1 FAAS Instrumental Detection Limit and Optimum Working Concentration for Lead (Pb)
Detection Limit, μg/mL
Optimum Linear Range Upper Limit, Elements, Compound Classes,
Element (approximately three times
μg/mL and Oxides
A
standard deviation of blank)
Inorganic compounds, airborne particulate, paint, dust by
Pb 0.02 10
wipe and micro-vacuuming, soil
A
Detection limit represents ideal laboratory conditions; variability due to sampling, digestion, reagents, and sample handling has not been taken into account.
D4840 Guide for Sample Chain-of-Custody Procedures
D6785 Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furnace Atomic Absorption
Spectrometry
D6966 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Determination of Metals
D7035 Test Method for Determination of Metals and Metalloids in Airborne Particulate Matter by Inductively Coupled Plasma
Atomic Emission Spectrometry (ICP-AES)
D7144 Practice for Collection of Surface Dust by Micro-vacuum Sampling for Subsequent Determination of Metals and
Metalloids
E456 Terminology Relating to Quality and Statistics
E631 Terminology of Building Constructions
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1188 Practice for Collection and Preservation of Information and Physical Items by a Technical Investigator
E1583 Practice for Evaluating Laboratories Engaged in Determination of Lead in Paint, Dust, Airborne Particulates, and Soil
Taken From and Around Buildings and Related Structures
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
(Withdrawn 2021)
E1644 Practice for Hot Plate Digestion of Dust Wipe Samples for the Determination of Lead
E1645 Practice for Preparation of Dried Paint Samples by Hotplate or Microwave Digestion for Subsequent Lead Analysis
E1726 Practice for Preparation of Soil Samples by Hotplate Digestion for Subsequent Lead Analysis
E1727 Practice for Field Collection of Soil Samples for Subsequent Lead Determination
E1728 Practice for Collection of Settled Dust Samples Using Wipe Sampling Methods for Subsequent Lead Determination
E1729 Practice for Field Collection of Dried Paint Samples for Subsequent Lead Determination
E1741 Practice for Preparation of Airborne Particulate Lead Samples Collected During Abatement and Construction Activities
for Subsequent Analysis by Atomic Spectrometry (Withdrawn 2009)
E1792 Specification for Wipe Sampling Materials for Lead in Surface Dust
E1864 Practice for Evaluating Quality Systems of Organizations Conducting Facility and Hazard Assessments for Lead in Paint,
Dust, Airborne Particulate, and Soil in and around Buildings and Related Structures (Withdrawn 2011)
E1908 Practice for Sample Selection of Debris Waste from a Building Renovation or Lead Abatement Project for Toxicity
Characteristic Leaching Procedure (TCLP) Testing for Leachable Lead (Pb)
E1979 Practice for Ultrasonic Extraction of Paint, Dust, Soil, and Air Samples for Subsequent Determination of Lead
E2115 Guide for Conducting Lead Hazard Assessments of Dwellings and of Other Child-Occupied Facilities
E2239 Practice for Record Keeping and Record Preservation for Lead Hazard Activities
E2271/E2271M Practice for Clearance Examinations Following Lead Hazard Reduction Activities in Multifamily Dwellings
E2913/E2913M Practice for Hotplate Digestion of Lead from Composited Wipe Samples
E2914/E2914M Practice for Ultrasonic Extraction of Lead from Composited Wipe Samples
E3074/E3074M Practice for Clearance Examinations Following Lead Hazard Reduction Activities in Single Family Dwellings,
in Individual Units of Multifamily Dwellings, and in Other Child-Occupied Facilities
2.2 Code of Federal Regulations:
40 CFR 745 Lead-Based Paint Poisoning Prevention in Certain Residential Structures
Available from U.S. Government Publishing Office, 732 N. Capitol St., NW, Washington, DC 20401, http://www.gpo.gov.
E3193 − 23
2.3 Governmental Agency Guidance:
U.S. Environmental Protection Agency National Lead Laboratory Accreditation Program (NLLAP)
U.S. Environmental Protection Agency SW-846 Test Method 1311: Toxicity Characteristic Leaching Procedure
2.4 ISO Standard:
ISO/IEC 17025 General requirements for the competence of testing and calibration laboratories
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminologies D1356, E456, E631, and E1605.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 analysis run, n—a period of measurement time on a given analytical instrument during which data are calculated from a
single calibration curve (or single set of curves).
3.2.1.1 Discussion—
Recalibration of a given instrument produces a new analysis run.
3.2.2 calibration standards, n—solutions of known analyte concentrations used to calibrate instruments.
3.2.2.1 Discussion—
Calibration standards must be matrix matched to the acid content present in sample digestates or extracts and must be measured
prior to analyzing samples.
3.2.3 initial calibration blank (ICB), n—a standard containing no analyte that is used for the initial calibration and zeroing of the
instrument response.
3.2.3.1 Discussion—
The ICB must be matrix matched to the acid content of sample extracts and digestates. The ICB must be measured during and after
calibration. The measured value is to be (at most) less than five times the IDL.
3.2.4 initial calibration verification (ICV), n—a solution (or set of solutions) of known analyte concentration used to verify
calibration standard levels; the concentration of analyte is to be near the mid-range of the linear curve that is made from a stock
solution having a different manufacturer or manufacturer lot identification than the calibration standards.
3.2.4.1 Discussion—
The ICV must be matrix matched to the acid content of sample extracts or digestates. The ICV must be measured after calibration
and before measuring any sample digestates or extracts. The measured value is to fall within 610 % of the known value.
3.2.5 instrumental detection limit (IDL), n—the lowest concentration at which the instrumentation can distinguish analyte content
from the background generated by a minimal matrix.
3.2.5.1 Discussion—
The IDL is usually determined by the manufacturer. The IDL can be determined from blank, acidified, deionized, or ultrapure water
as the matrix and from the same calculation methods used to determine a method detection limit (MDL). Typical lead (Pb) IDL
for FAAS is 0.05 0.05 μg μg/mL.⁄mL.
3.2.6 instrumental QC standards, n—these provide information on measurement performance during the instrumental analysis
portion of the overall analyte measurement process. They include CCBs, CCVs, ICBs, and ICVs.
3.2.7 method blank, n—a digestate or extract that reflects the maximum treatment given any one sample within a sample batch,
except that no sample is placed into the digestion or extraction vessel. (The same reagents and processing conditions that are
applied to field samples within a batch are also applied to the method blank.)
3.2.7.1 Discussion—
Analysis results from method blanks provide information on the level of potential contamination experienced by samples processed
within the batch.
Available from United States Environmental Protection Agency (EPA), William Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov.
Available from International Organization for Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Switzerland, http://www.iso.org.
E3193 − 23
3.2.8 quantitation limit, n—an instrumental measurement value that is used to provide a lower concentration limit for reporting
quantitative analysis data for a given analytical method.
3.2.8.1 Discussion—
Any sample that generates a lead measurement below the quantitation limit is reported as a less-than value using the quantitation
limit value multiplied by the appropriate dilution factors resulting from preparation of the sample for instrumental analysis.
3.2.9 quantitative analysis, n—an analysis run on sample digestates or extracts (or serial dilutions thereof) that includes
instrumental QC standards.
3.2.9.1 Discussion—
Data from this analysis run are used to calculate and report final lead analysis results.
3.2.10 reporting limit, n—the lowest concentration of analyte in a sample that can be reported with a defined, reproducible level
of certainty.
3.2.10.1 Discussion—
This value is usually based on the low standard used for instrument calibration. For analyses in the United States of America
subject to 40 CFR 745 and the National Lead Laboratory Accreditation Program (NLLAP), the reporting limit for a specific sample
matrix must be at least twice the MDL for that same sample matrix.
3.2.11 semiquantitative analysis, n—an analysis run that is performed on highly diluted sample digestates or extracts for the
purpose of determining the approximate analyte level in the digest.
3.2.11.1 Discussion—
This analysis run is generally performed without inserting instrumental QC standards except for calibration standards. Data from
this run are used for determining serial dilution requirements for sample digestates or extracts to keep them within the linear range
of the instrument.
3.2.12 serial dilution, n—a method of producing a less concentrated solution through one or more consecutive dilution steps.
3.2.12.1 Discussion—
A dilution step for a standard or sample solution is performed by volumetrically placing a small aliquot (of known volume) of a
higher concentrated solution into a volumetric flask and diluting to volume with water containing the same acid levels as those
found in original sample digestates or extracts.
3.2.13 spiked duplicate sample, n—two portions of a homogenized sample that were targeted for addition of analyte and fortified
with all the target analytes before preparation.
3.2.13.1 Discussion—
Analysis results for these samples are used to provide information on the precision and bias of the overall analysis process.
3.2.14 spiked sample, n—a sample portion (split from an original sample) to which an additional known amount of analyte has
been added.
3.2.14.1 Discussion—
Analysis results for spiked samples are used to provide information on the precision and bias of the overall analysis process.
3.2.15 un-spiked sample, n—a portion of a homogenized sample that was targeted for the addition of analyte but is not fortified
with target analytes before sample preparation.
3.2.15.1 Discussion—
Analysis results for this sample are used to correct for native analyte levels in the spiked and spiked duplicate samples.
4. Summary of Test Method
4.1 A sample digestate or extract is analyzed for lead content using FAAS. Instrumental QC samples are analyzed along with
sample digestates or extracts in order to ensure adequate instrumental performance.
NOTE 1—Digestion is an example of an extraction process. Other examples of extraction processes are ultrasonic extraction and leaching.
4.2 Samples and standards are aspirated into the flame of an absorption spectrophotometer. A lead (Pb) hollow cathode or
E3193 − 23
electrodeless discharge lamp provides the characteristic radiation energy for lead. The absorption of this characteristic energy by
lead atoms in the flame is related to the concentration of lead in the aspirated sample. The flame and operating conditions for lead
are listed in Table 2.
5. Significance and Use
5.1 This test method is intended for use with other standards that address the collection and preparation of samples (dusts by wipe,
(airborne particulate, dusts by wipe and micro-vacuuming, dried paint chips, and soils) that are obtained during the assessment or
mitigation of lead hazards from buildings and related structures.
5.2 Laboratories analyzing samples obtained during the assessment or mitigation of lead hazards from buildings and related
structures shall conform to Practice E1583, or shall be recognized for lead analysis as promulgated by authorities having
jurisdiction, or both.
NOTE 2—In the United States of America, laboratories performing analysis of samples collected during lead-based paint activities are required to be
accredited to ISO/IEC 17025 and to other requirements promulgated by the Environmental Protection Agency (EPA).
5.3 This test method may also be used to analyze similar samples from other environments such as toxic characteristic extracts
of waste sampled using Guide E1908, and soil and sludge as prepared for analysis using U.S. EPA SW-846 Test Method 1311.
6. Interferences
6.1 In FAAS, the occurrence of interferences is less common than in many other analytical techniques. Interferences can occur,
however, and when encountered are corrected as indicated in the following sections. The known interferences and correction
methods for each metal lead are indicated in Table 2. The methods of standard additions and background monitoring and correction
(2-5) are used to identify the presence of an interference. Insofar as possible, the matrix of sample and standard are matched to
minimize possible interference.
6.2 Background or nonspecific absorption can occur from particles produced in the flame, which can scatter light and produce an
apparent absorption signal. Light scattering may be encountered when solutions of high salt content are being analyzed. They are
most severe when measurements are made at shorter wavelengths (for example, below about 250 nm). Background absorption may
also occur as the result of the formation of various molecular species which can absorb light. The background absorption can be
accounted for by the use of background correction techniques (2).
6.3 Spectral interferences are those interferences which result from an atom different from the one being measured that absorbs
a portion of the radiation. Such interferences are extremely rare in FAAS. In some cases, multi-element hollow cathode lamps may
cause a spectral interference by having closely adjacent emission lines from two different elements. In general, the use of
multi-element hollow cathode lamps is discouraged.
6.4 Ionization interference occurs when easily ionized atoms are being measured. The degree to which such atoms are ionized is
dependent upon the atomic concentration and the presence of other easily ionized atoms. This interference can be controlled by
the addition of a high concentration of another easily ionized element which will buffer the electron concentration in the flame.
TABLE 2 FAAS Flame and Operating Conditions for Lead (Pb)
Analytical Wavelength,
A A
Element Type of Flame Interferences Remedy Reference
nm
217.0 Ca, high concentration
B
Pb Air-C H (oxidizing) (1)
2 2 –2
283.3 SO
A
High concentrations of silicon in the sample can cause an interference for many of the elements in this table and may cause aspiration problems. No matter what elements
are being measured, if If large amounts of silica are extracted from the samples, the samples should be allowed to stand for several hours and centrifuged or filtered to
remove the silica.
B
Samples are periodically analyzed by the method of additions to check for chemical interferences. If interferences are encountered, determinations must be made by
the standard additions method or, if the interferent is identified, it may be added to the standards.
The boldface numbers in parentheses refer to a list of references at the end of this standard.
E3193 − 23
6.5 Chemical interferences occur in FAAS when species present in the sample cause variations in the degree to which atoms are
formed in the flame, or when different valence states of a single element have different absorption characteristics. Such
interferences may be controlled by adjusting the sample matrix or by the method of standard additions (3). Also, the use of
lanthanum as a releasing element minimizes the interference from the formation of nonvolatile compounds in the flame.
Lanthanum forms nonvolatile compounds preferentially with the interferent so that the analyte remains free.
6.6 Physical interferences may result if the physical properties of the samples vary significantly. Changes in viscosity and surface
tension can affect the sample aspiration rate and thus cause erroneous results. Sample dilution or the method of standard additions,
or both, are used to correct such interferences. High concentrations of silica in the sample can cause aspiration problems. If large
amounts of silica are extracted from the samples, they shall be allowed to stand for several hours and centrifuged or filtered to
remove the silica.
6.7 This procedure references matrix-specific methods for sample preparation.
7. Apparatus
7.1 Analytical Apparatus:
7.1.1 Flame Atomic Absorption Spectrophotometer, equipped with air/acetylene burner head.
7.1.2 Lead (Pb) Hollow Cathode or Electrodeless Discharge Lamp.
7.1.3 Deuterium Continuum Lamp.
7.1.4 Compressed Air—Appropriate pressure-reducing regulator with base connections (see instrument manufacturer’s instruc-
tions).
7.1.5 Acetylene Gas and Regulator—A cylinder of acetylene equipped with a two-gauge, two-stage pressure-reducing regulator
with hose connections (see instrument manufacturer’s instructions).
7.1.6 Beakers, Phillips or Griffin, 125 mL, borosilicate glass.
7.1.7 Centrifuge Tubes, 15 mL, graduated, plastic or borosilicate glass; or, tubes to fit the autosampler in use.
7.1.8 Miscellaneous Borosilicate Glassware (Pipets and Volumetric Flasks)—All pipets and volumetric flasks shall be calibrated
Class A volumetric glassware.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall 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 that it can be demonstrated that they are of sufficiently high
purity to permit their use without decreasing the accuracy of the determinations.
8.2 Purity of Water—Unless otherwise indicated, reference to water shall be understood to mean Type II reagent water conforming
to Specification D1193.
8.3 Hydrochloric Acid (HCl)—Concentrated hydrochloric acid, 12 N, specific gravity 1.19.
8.4 Nitric Acid (HNO )—Redistilled, concentrated nitric acid, 16 N, specific gravity 1.42.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
E3193 − 23
8.5 Lead (Pb) Stand
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