ASTM D6785-02
(Test Method)Standard Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furnace Atomic Absorption Spectrometry
Standard Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furnace Atomic Absorption Spectrometry
SCOPE
1.1 This standard specifies flame and graphite furnace atomic absorption spectrometric methods for the determination of the time-weighted average mass concentration of particulate lead and lead compounds in workplace air.
1.2 The method is applicable to personal sampling of the inhalable fraction of airborne particles, as defined in ISO 7708, and to static (area) sampling.
1.3 The sample dissolution procedure specifies hot plate or microwave digestion, or ultrasonic extraction (11.2). The sample dissolution procedure is not effective for all lead compounds (see Section 5). The use of an alternative, more vigorous dissolution procedure is necessary when it is desired to extract lead from compounds present in the test atmosphere that are insoluble using the dissolution procedures described herein. For example if it is desired to determine silicate lead, a hydrofluoric acid dissolution procedure is required.
1.4 The flame atomic absorption method is applicable to the determination of masses of approximately 1 to 200 μg of lead per sample, without dilution (1). The graphite furnace atomic absorption method is applicable to the determination of masses of approximately 0.01 to 0.5 μg of lead per sample, without dilution (1).
1.5 The ultrasonic extraction procedure has been validated for the determination of masses of approximately 20 to 100 μg of lead per sample, for laboratory-generated lead fume air filter samples (2).
1.6 The concentration range for lead in air for which this procedure is applicable is determined in part by the sampling procedure selected by the user (see Section 10).
1.7 Anions that form precipitates with lead may interfere, but this potential interference is overcome by the addition of the disodium salt of ethylenediamine tetraacetic acid (EDTA) when necessary.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6785–02
Standard Test Method for
Determination of Lead in Workplace Air Using Flame or
Graphite Furnace Atomic Absorption Spectrometry
This standard is issued under the fixed designation D 6785; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This standard specifies flame and graphite furnace
bility of regulatory limitations prior to use.
atomic absorption spectrometric methods for the determination
of the time-weighted average mass concentration of particulate
2. Referenced Documents
lead and lead compounds in workplace air.
2.1 ASTM Standards:
1.2 The method is applicable to personal sampling of the
D 4840 Guide for Sample Chain-of-Custody Procedures
inhalable fraction of airborne particles, as defined in ISO 7708,
E 882 Guide for Accountability and Quality Control in the
and to static (area) sampling.
Chemical Analysis Laboratory
1.3 The sample dissolution procedure specifies hot plate or
E 1370 Guide for Air Sampling Strategies for Worker and
microwave digestion, or ultrasonic extraction (11.2). The
Workplace Protection
sample dissolution procedure is not effective for all lead
2.2 Other Standards:
compounds (see Section 5). The use of an alternative, more
ISO 648:1977, Laboratory Glassware—One-Mark Pipettes
vigorous dissolution procedure is necessary when it is desired
ISO 1042:1983, Laboratory Glassware—One-Mark Volu-
to extract lead from compounds present in the test atmosphere
metric Flasks
that are insoluble using the dissolution procedures described
ISO 3585:1991, Glass Plant, Pipelines and Fittings—
herein. For example if it is desired to determine silicate lead, a
Properties of Borosilicate Glass 3.3
hydrofluoric acid dissolution procedure is required.
ISO 3696:1987, Water for Laboratory Use—Specifications
1.4 The flame atomic absorption method is applicable to the
and Test Methods
determination of masses of approximately 1 to 200 µg of lead
ISO 6879:1983, Air Quality—Performance Characteristics
per sample, without dilution (1). The graphite furnace atomic
and Related Concepts For Air Quality Methods
absorption method is applicable to the determination of masses
ISO 6955:1982, Analytical Spectroscopic Methods—Flame
of approximately 0.01 to 0.5 µg of lead per sample, without
Emission, Atomic Absorption, and Atomic
dilution (1).
Fluorescence—Vocabulary
1.5 The ultrasonic extraction procedure has been validated
ISO 7708:1995, Particle Size Definitions for Health Related
for the determination of masses of approximately 20 to 100 µg
Sampling
of lead per sample, for laboratory-generated lead fume air filter
ISO15202-2:2001, WorkplaceAir—DeterminationofMet-
samples (2).
als and Metalloids in Airborne Particulate Matter by
1.6 The concentration range for lead in air for which this
Inductively Coupled Plasma Atomic Emission
procedure is applicable is determined in part by the sampling
Spectrometry—Part 2: Sample Preparation
procedure selected by the user (see Section 10).
EN 689:1995, Workplace Atmospheres—Guidance for the
1.7 Anions that form precipitates with lead may interfere,
AssessmentofExposuretoChemicalAgentsforCompari-
but this potential interference is overcome by the addition of
son with Limit Values and Measurement Strategy
the disodium salt of ethylenediamine tetraacetic acid (EDTA)
EN 1232:1997, Workplace Atmospheres—Pumps for Per-
when necessary.
sonal Sampling of Chemical Agents—Requirements and
1.8 This standard does not purport to address all of the
Test Methods
safety concerns, if any, associated with its use. It is the
EN 1540:1998, Workplace Atmospheres—Terminology
1 3
This test method is under the jurisdiction of ASTM Committee D22 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mittee D22.04 on Workplace Atmospheres. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 10, 2002. Published June 2002. the ASTM website.
2 4
The boldface numbers in parentheses refer to the list of references at the end of Available from American National Standards Institute, 25 W. 43rd St., 4th
this standard. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6785–02
EN 12919: 1999, Workplace Atmospheres—Pumps for Threshold Limit Values for Chemical Substances and Physical
SamplingofChemicalAgentswithaVolumeFlowRateof Agents; Biological Exposure Indices (3).
Over 5 L/Min—Requirements and Test Methods
3.1.9 workplace—the defined area or areas in which the
EN 13205: 2001, Workplace Atmospheres—Assessment of
work activities are carried out. EN 1540
Performance of Instruments for Measurement ofAirborne
3.2 Particle Size Fraction Definitions:
Particle Concentrations
3.2.1 inhalable convention—a target specification for sam-
EN ISO 8655-1, Piston-Operated Volumetric Instruments—
pling instruments when the inhalable fraction is of interest.
Part 1: Terminology, General Requirements and User
ISO 7708
Recommendations
3.2.2 inhalable fraction—the mass fraction of total airborne
EN ISO 8655-2 Piston-Operated Volumetric Instruments—
particles which is inhaled through the nose and mouth.
Part 2: Piston Pipettes
3.2.2.1 Discussion—The inhalable fraction depends on the
EN ISO 8655-5 Piston-Operated Volumetric Instruments—
speed and direction of air movement, on breathing rate and
Part 5: Dispensers
other factors. ISO 7708
EN ISO 8655-6 Piston-Operated Volumetric Instruments—
3.2.3 respirable convention—a target specification for sam-
Part 6: Gravimetric Test Methods
pling instruments when the respirable fraction is of interest.
ISO 7708
3. Terminology
3.2.4 respirable fraction—the mass fraction of inhaled par-
3.1 General Definitions:
ticles penetrating to the unciliated airways. ISO 7708
3.1.1 breathing zone—the space around the worker’s face
3.2.5 total airborne particles—all particles surrounded by
from where he or she takes his or her breath. For technical
air in a given volume of air.
purposes a more precise definition is as follows: hemisphere
3.2.5.1 Discussion—Because all measuring instruments are
(generally accepted to be 0.3 m in radius) extending in front of
size-selective to some extent, it is often impossible to measure
the human face, centered on the midpoint of a line joining the
the total airborne particles concentration. ISO 7708
ears;thebaseofthehemisphereisaplanethroughthisline,the
3.3 Sampling Definitions:
top of the head and the larynx. The definition is not applicable
3.3.1 personal sampler—a device attached to a person that
when respiratory protective equipment is used. EN 1540
samples air in the breathing zone. EN 1540
3.1.2 chemical agent—any chemical element or compound,
3.3.2 personal sampling—The process of sampling carried
on its own or admixed as it occurs in the natural state or as
out using a personal sampler. EN 1540
produced, used or released including release as waste, by any
3.3.3 sampling instrument; sampler—for the purposes of
work activity, whether or not produced intentionally and
this standard, a device for collecting airborne particles.
whether or not placed on the market. EN 1540
3.3.3.1 Discussion—Instruments used to collect airborne
3.1.3 exposure (by inhalation)—a situation in which a
particles are frequently referred to by a number of other terms,
chemical agent is present in air which is inhaled by a person.
for example, sampling heads, filter holders, filter cassettes etc.
3.1.4 limit value—reference figure for concentration of a
3.3.4 static sampler; area sampler—a device, not attached
chemical agent in air.
to a person, used in static (area) sampling.
3.1.4.1 Discussion—An example is the Threshold Limit
Value (TLV) for a given substance in workplace air, as 3.3.5 static sampling; area sampling—the process of air
established by the ACGIH (3). sampling carried out in a particular location.
3.1.5 measuring procedure—procedure for sampling and
3.4 Analytical Definitions:
analyzing one or more chemical agents in the air and including
3.4.1 sample dissolution—the process of obtaining a solu-
storage and transportation of the sample.
tioncontainingtheanalytesofinterestfromasample.Thismay
3.1.6 operating time—the period during which a sampling
or may not involve complete dissolution of the sample.
pump can be operated at specified flow rate and back pressure
3.4.2 sample preparation—all operations carried out on a
without recharging or replacing the battery. EN 1232
sample, after transportation and storage, to prepare it for
3.1.7 reference period—the specified period of time stated
analysis, including transformation of the sample into a mea-
for the limit value of a specific chemical agent.
surable state, where necessary.
3.1.7.1 Discussion—Examples of limit values for different
3.4.3 sample solution—solution prepared by the process of
referenceperiodsareshort-termandlong-termexposurelimits,
sample dissolution, but possibly needing to be subjected to
such as those established by the ACGIH (3).
further operations in order to produce a test solution that is
3.1.8 time weighted average (TWA) concentration—the
ready for analysis.
concentration of a chemical agent in the atmosphere, averaged
3.4.4 test solution—solution prepared by the process of
over the reference period.
sample dissolution and, if necessary, having been subjected to
3.1.8.1 Discussion—A more detailed discussion of TWA
any further operations required to bring it into a state in which
concentrations and their use can be found in the American
it is ready for analysis.
Conference of Government Industrial Hygienists publication
3.5 Statistical Terms:
3.5.1 analytical recovery—ratio of the mass of analyte
measured when a sample is analyzed to the known mass of
To be published. analyte in that sample, expressed as a percentage.
D6785–02
3.5.2 bias—consistent deviation of the results of a measure- made at 283.3 nm with background correction, and results are
ment process from the true value of the air quality character- obtained by the analytical curve technique (see 6.1 of ISO
istic itself. ISO 6879 6955).
4.5 Theresultsmaybeusedfortheassessmentofworkplace
3.5.3 overall uncertainty—(of a measuring procedure or of
exposures to airborne particulate lead (see EN 689).
an instrument) quantity used to characterize as a whole the
uncertainty of a result given by an apparatus or measuring
5. Reactions
procedure.Itisexpressed,asapercentage,byacombinationof
bias and precision, usually in accordance with the formula: 5.1 In general, the overwhelming majority of particulate
lead compounds that are commonly found in samples of
–
2+
|[x 2 x # | 1 2s
ref
workplace air are converted to water-soluble lead ions (Pb
)
3 100
x
ref
by the sample dissolution procedures described in 11.2. How-
ever, certain lead compounds, for example lead silicate, might
where:
not be dissolved. If necessary, a dissolution procedure employ-
–
= mean value of results of a number (n) of repeated
x
ing hydrofluoric acid should be used to dissolve silicate lead. If
measurements,
there is any doubt about the effectiveness of these procedures
x = true or accepted reference value of concentration,
ref
for the dissolution of particulate lead compounds that may be
and
present in the test atmosphere, then this shall be investigated
s = standard deviation of repeated measurements.
before proceeding with the method (see Section 11).
EN 482
3.5.4 precision—the closeness of agreement of results ob-
6. Significance and Use
tained by applying the method several times under prescribed
6.1 The health of workers in many industries, for example,
conditions. ISO 6879
mining, metal refining, battery manufacture, construction, etc.,
3.5.4.1 Discussion—Precisionisoftenexpressedintermsof
is at risk through exposure by inhalation of particulate lead and
the relative standard deviation.
lead compounds. Industrial hygienists and other public health
3.5.5 true value—the value which characterizes a quantity
professionals need to determine the effectiveness of measures
perfectly defined in the conditions which exist when that
taken to control workers’ exposure, and this is generally
quantity is considered. ISO 3534-1
achieved by making workplace air measurements. This stan-
3.5.5.1 Discussion—The true value of a quantity is a theo-
dard has been published in order to make available a method
retical concept and, in general, cannot be known exactly.
for making valid exposure measurements for lead. It will be of
EN 1540
benefit to: agencies concerned with health and safety at work;
industrial hygienists and other public health professionals;
4. Summary of Test Method
analytical laboratories; industrial users of metals and metal-
4.1 A known volume of air is drawn through a filter to loids and their workers, etc. It has been assumed in the drafting
collect particulate lead and lead compounds. For personal of this standard that the execution of its provisions, and the
sampling, a sampler designed to collect the inhalable fraction interpretation of the results obtained, is entrusted to appropri-
of airborne particles may be used. ately qualified and experienced people.
6.2 The measuring procedure shall comply with any rel-
NOTE 1—The inhalable convention may not be the regulated sampling
evant International, European or National Standard that speci-
convention in all countries where this standard may be applicable. In the
fies performance requirements for procedures for measuring
USA, for example, limit values promulgated by the Occupational Safety
chemical agents in workplace air (for example, EN 482).
and HealthAdministration (OSHA) (29 CFR 1910.1025) are based on the
use of samplers that were not specifically designed to meet the inhalable
7. Reagents
convention.
NOTE 2—During the analysis, use only reagents of recognized analyti-
4.2 The filter and collected sample are subjected to a
cal grade, and only water as specified in 7.1.
dissolution procedure in order to extract lead. The sample
7.1 Water, complying with the requirements for ISO 3696
dissolution procedure may use one of three techniques: hot
grade 2 water (electrical conductivity less than 0.1 mS/m and
plate digestion, microwave digestion or ultraso
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.