ASTM D3614-07(2021)

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: D3614 − 07 (Reapproved 2021)
Standard Guide for
Laboratories Engaged in Sampling and Analysis of
Atmospheres and Emissions
This standard is issued under the fixed designation D3614; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
The utilization of well tested and uniform laboratory practices is essential to the production of
reliable and defensible environmental data whose validity can be demonstrated at a later date through
theuseofwrittenfieldandlaboratoryrecords.Thisdocumentisintendedtoprovidegeneralguidelines
for the elements of laboratory practices that are considered to be basic to the performance of
laboratories that provide services in the sampling and analysis of atmospheres and emissions. This
document is intended to stimulate an awareness of good laboratory and field practices.
1. Scope 1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This guide covers criteria to be used by those respon-
ization established in the Decision on Principles for the
sible for the selection, evaluation, operation, and control of
Development of International Standards, Guides and Recom-
laboratory organizations engaged in sampling and analysis of
mendations issued by the World Trade Organization Technical
environmental atmospheres, including ambient, work space,
Barriers to Trade (TBT) Committee.
and source emissions, as well as atmospheric deposition
samples. For details specific to stack gases, see Practice
2. Referenced Documents
D7036, which covers administrative issues in full; several
2.1 ASTM Standards:
specifics in this guide regarding laboratory operations may yet
D1356Terminology Relating to Sampling and Analysis of
be helpful and do not overlap with Practice D7036.
Atmospheres
1.2 This guide presents features of organizations, facilities,
D1357Practice for Planning the Sampling of the Ambient
resources, and operations which by their selection and control
Atmosphere
affect the reliability and credibility of the data generated.
D3249Practice for General Ambient Air Analyzer Proce-
1.3 This guide presents the criteria for the selection and dures
control of the features listed in 1.2 so that acceptable perfor- D3670Guide for Determination of Precision and Bias of
mancemaybeattainedandsustained.Also,thisguidepresents Methods of Committee D22
recommendations for the correction of unacceptable perfor- D7036Practice for Competence of Air Emission Testing
Bodies
mance.
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. The values given in parentheses after SI units are
3.1 Definitions—For definitions of terms used in this guide,
providedforinformationonlyandarenotconsideredstandard.
see Terminology D1356.
1.5 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 accrediting authority, n—a body that evaluates the
responsibility of the user of this standard to establish appro-
capabilityofatestingagency,oraninspectionagency,orboth,
priate safety, health, and environmental practices and deter-
in certain specific fields of activity.
mine the applicability of regulatory limitations prior to use.
3.2.2 agency, n—an organization or part of an organization,
engaged in the activities of testing or inspection, or both.
This guide is under the jurisdiction of ASTM Committee D22 on Air
Qualityand is the direct responsibility of Subcommittee D22.01 on Quality
Control. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved March 1, 2021. Published March 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1977. Last previous edition approved in 2013 as D3614–07 (2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D3614-07R21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3614 − 07 (2021)
3.2.3 generic criteria, n—common characteristics pertain- 5.3 Laboratories that produce environmental sampling and
ing to organization, human resources, material resources, and analysisdataandthosewhohavetheresponsibilityofselecting
quality systems which provide a basis for assessing the a laboratory to perform air quality studies need to know what
qualifications of testing or inspection agencies. criteria, practices, and recommendations have been accepted
by consensus within this field of endeavor.
3.2.4 human resources, n—those elements of support or
capability that are provided by humans using their mental and
5.4 Demonstration and documentation by a laboratory that
physical capabilities.
there is judicious selection and control of organizational
factors, facilities, resources, and operations enhance the reli-
3.2.5 inspection, n—the process of measuring, examining,
testing, gauging, or otherwise evaluating materials, products, ability of the data produced and promote the acceptance of
these data.
services, systems, or environments.
3.2.6 organizational component, n—a portion of an organi-
6. Responsibilities and Duties of the Laboratory
zationwithspecifictasksandactivitiesthatconstitutesapartof
the total effort and accomplishment of the organization.
6.1 The purpose of the laboratory is to provide information
3.2.7 quality, n—the totality of features and characteristics
that is factual, accurate, reliable, and adequate for its purpose.
of a product or service that bear on its ability to satisfy a given The procedure by which this is to be achieved is by the
need. effectiveadministrationofaqualityassurance(QA)planbythe
management of the organization. The elements of a quality
3.2.8 quality assurance, n—a system of activities whose
assurance plan are described in 6.1.1 – 6.1.6.1.
purpose is to provide assurance that the overall quality control
6.1.1 Organization—Atableoforganizationwhichindicates
job is in fact being done effectively. The system involves a
the organizational structure and the lines of authority, areas of
continuing evaluation of the adequacy and effectiveness of the
responsibility, and job descriptions should be available. Key
overall quality control program (see quality control) with a
personnel, including their workplace locations and phone
view to having corrective measures initiated where necessary.
numbers, should be identified for each organizational entity.
For a specific product or service, this involves verifications,
Separateorganizationalchartsforsubcontractorsmightalsobe
audits, and the evaluation of the quality factors that affect the
needed. QA managers should be identified along with their
specification, production, inspection, and use of the product or
relationships to other project personnel. The QA managers
service.
shouldbeorganizationallyindependentofprojectmanagement
3.2.9 quality control, n—the overall system of activities
so that the risk of conflict of interest is minimized.
whosepurposeistoprovideaqualityofproductorservicethat
6.1.1.1 Human Resources—The key personnel of the orga-
meets the needs of users; also, the use of such a system. The
nization should be described by means of personal résumés
aim of quality control is to provide quality that is satisfactory,
presenting the applicable education and work experience
adequate, dependable, and economic. The overall system
relative to his or her position in the table of organization and
involves integrating the quality aspects of several related steps
the requirements of that position.
including: (1)the proper specification of what is wanted;
(2)production to meet the full intent of the specification; 6.1.1.2 Physical Resources—The laboratory facilities
(3)inspection to determine whether the resulting product or should provide a working environment that is clean, air-
service is in accord with the specifications; and (4)review of conditioned, heated, well-lighted, and safe. The instrumenta-
usage to provide for revision of specification. tion and equipment should be appropriate to the operational
needs of the laboratory.
3.2.10 testing, n—the determination by technical means of
6.1.2 Methodology—Written procedures should be readily
properties, performance, or elements of materials, products,
available to all personnel.
services, systems, or environments which involve application
of established scientific principles and procedures.
6.1.2.1 Sample collection and handling procedures, and
storage requirements should be written.
4. Summary of Guide
6.1.2.2 Calibration and standardization procedures should
be written.
4.1 This guide describes the criteria, practices, and recom-
mendations for the physical resources, data validation, and 6.1.2.3 Standard operating procedures (SOPs) and analyti-
mode of operation of the laboratory.
cal methods should be written.
6.1.2.4 Thereshouldbeadocumentcontrolsystemtoassure
5. Significance and Use
that the written procedures are current and complete.
5.1 Data on the composition and characteristics of environ- 6.1.2.5 All of the above should be periodically subjected to
mental atmospheres, such as ambient or work space air, are performance and system audits.
frequently used to evaluate the health and safety of humans.
6.1.3 Metrology Systems—Allsystemsformakingmeasure-
Dataonthecompositionofatmosphericdepositionsamplesare
ments should have the following features:
often used for environmental impact assessment.
6.1.3.1 Calibration and standardization procedures, includ-
5.2 These data are frequently used to ascertain compliance ing a description of a procedure for establishing traceability,
with regulatory statutes that place limits on acceptable com- description of calibration standards, and a schedule for
positions and characteristics of these atmospheres. calibration,
D3614 − 07 (2021)
6.1.3.2 Preventative maintenance procedures including a 7.2.1.1 Selection and approval of methods of sampling and
schedule for maintenance intervals and documentation of their analysis,
proper completion, and
7.2.1.2 Implementation of a quality assurance program to
6.1.3.3 Records of modification of configuration that may describe the quality of technical data,
occur in any measurement system due to repair and servicing
7.2.1.3 Development of standards of performance and
of equipment, replacement of components or reagents, or
evaluation of personnel by these standards, and
change of procedures.
7.2.1.4 Training of personnel.
6.1.4 Data Recording—The laboratory should keep records
NOTE 1—The equivalent requirement is for the purpose of recognizing
of submitted samples and completed analyses in a manner that
those persons who may have a comparable educational background that
provides for the retrievability, preservation and traceability of
has been obtained through recognized and qualified educational resources
the sample source, the procedures used, and the person or
but does not result in the award of a baccalaureate degree.The use of this
term will necessarily require the judgement of the user of this guide.
persons responsible for the sampling and analysis.
Certification by acknowledged professional boards is encouraged.
6.1.4.1 All laboratory data sheets should be dated and
signed by the analyst. 7.2.2 The Laboratory Supervisor—The laboratory supervi-
6.1.4.2 A policy for the use of computers for data sor should be a full time employee of the organization that
acquisition, archiving, and mathematical calculations should
operates the laboratory, and should have a minimum of an
be implemented. earned baccalaureate degree in science or engineering from an
6.1.5 Data Validation—The laboratory should keep records
accredited college, university, or the equivalent (see Note 1),
of analytical performance by means of audit procedures, and a minimum of one year analytical responsibility.
reference sample programs, and interlaboratory tests. Where
7.2.3 The Senior Staff—The senior staff of the laboratory
applicable, quality control charts should be used to report
should conduct the difficult and nonroutine sampling and
results from these validation activities. Quality control proce-
analysesandshoulddirectlysupervisethetechnicalstaff.Each
dures found in most current methods should be followed (1).
member of the senior staff should have a minimum of a
6.1.6 Deficiency Correction—The organizational system
baccalaureatedegreeinscienceorengineeringfromanaccred-
should provide the authority and the responsibility for a
ited college or university or the equivalent (see Note 1).
designated person or persons to investigate out of control
7.2.4 The Technical Staff—The technical staff will normally
procedures and to inform the laboratory management of the
consist of qualified personnel who conduct routine sampling
problems that occur. This is often the responsibility of the QA
and analyses and may also include highly trained and qualified
manager.
people who specialize in difficult procedures.
6.1.6.1 Acurrentlogshouldbemaintainedofsuchdeficien-
7.2.4.1 Each member of the technical staff should have
cies and the action taken to correct them.
formal, on-the-job training in the analyses and areas of
assigned responsibility. Training should be provided on-site,
7. Organization
and in many cases should be supplemented by short courses
offered by equipment manufacturers, professional
7.1 The production of reliable data is dependent upon the
organizations,universities,orotherqualifiedtrainingfacilities.
conscientiouseffortofeveryonewhohasanyinvolvementwith
7.2.4.2 After appropriate training, the staff member must
the service. Therefore, it is important that each member of the
demonstrate acceptable results in the analysis of an applicable
organizationhaveaclear-cutunderstandingofhisorherduties
quality control or performance evaluation sample.
and responsibilities, and their relationship to the total effort.
7.2.5 The Support Staff—The support staff will normally
Themanagementofthelaboratoryhasaprimeresponsibilityin
consist of personnel who perform routine services such as:
defining the policy goals in relation to the quality of perfor-
cleaning glassware, transportation and handling samples and
mance and assigning the specific areas of responsibility to the
equipment, maintenance of sampling equipment, and clerical
individual. The human resources that are required for the
and secretarial services.
operationofthelaboratorywillvarywiththespecificfunctions
7.2.5.1 Each member of the support staff should have
that are to be served, but the minimum personnel and their
qualifications should generally be as follows: sufficient on-the-job training for his or her level of responsi-
bility as defined by the laboratory director.
7.2 Human Resources (2):
7.2.1 The Director—The laboratory director should be a 7.3 Physical Resources:
full-time employee of the organization that operates the labo- 7.3.1 The laboratory environment can affect the results of
ratory. He or she should have a minimum of an earned
analyses which are intended to describe the character of
baccalaureatedegreeinscienceorengineeringfromanaccred- atmospheres and emissions; therefore, the laboratory facility
ited college or university or the equivalent (see Note 1) with a
should be carefully considered.
minimum of 5 years experience in sampling and analysis of
7.3.2 Thespecificitemsofequipmentandapparatusthatare
atmospheres or in a related field. The director should have the
needed for the performance of standard methods are described
following responsibilities:
in those standards. If the laboratory proposes to perform a
procedure, it should possess the specified items of equipment
and apparatus.
7.3.3 The laboratory should be kept as free from interfer-
The boldface numbers in parentheses refer to the references at the end of this
standard. ence as is necessary to avoid contamination of the samples.
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This may require such precautions as sweeping the floor 7.3.9 The laboratory should be supplied with the following:
carefully with a compound to suppress dust, periodically (1) Class ABC type fire extinguishers, (2) spill control mate-
rials for acids, bases, and flammable materials, (3) eye wash
coating the floor with an inert material, vacuuming or scrub-
bing walls, floors, benches, and equipment, and wearing andsafetyshowerfacilities, (4)eyeprotection,andothersafety
devices that may be consistent with the particular laboratory
lint-free laboratory clothing. Care should be taken to avoid
operation. The facility should provide for the safe disposal of
introducing potential contaminants when choosing cleaning
reagents and samples with written instructions for the use of
products.
these procedures by utility or support personnel. The labora-
7.3.4 Samples that have been protected against the labora-
tory may be subject to national, regional, or local regulations
tory environment should be compared against samples that
for the generation and disposal of generated wastes, for
have been exposed to the laboratory environment.
example, in the United States, the laboratory may be required
7.3.5 In order for the hoods to be effective in removing
to have an EPA waste generator number as required by the
noxious, harmful, or interfering fumes and aerosols from the
Resource Conservation and Recovery Act (6).
laboratory environment, the hoods must be operating at their
7.3.10 The physical conditions in the laboratory shall com-
designed capacity. They should not be located in areas of
ply with applicable national, regional, or local regulations to
countervailing winds, such as between two open doors. Under
ensure safe working conditions, for example, in the United
usual operating conditions, hoods will require from
States,requirementsoftheOccupationalSafetyandHealthAct
3 3 2 3
0.0236m /s to 0.059m /s (50–125ft /min) per 0.093m of
may be applicable (7).
face area. Face velocities should be checked routinely by
qualified personnel for compliance with specifications.
8. Methodology
7.3.5.1 For a more detailed treatment of ventilation consult
8.1 The use of written procedures that should be periodi-
Ref (3).
cally reviewed is essential to the systematic performance of
7.3.6 In order to minimize the generation of noxious,
operations.Procedureshaveatendencytoundergoaprocessof
harmful, or interfering fumes in the laboratory environment,
evolution over a period of time. Modifications of the proce-
potentially troublesome samples and reagents should be
dures may be needed periodically and they should be noted.
handled in properly operating hoods. Sinks should not be used
Such notations should be explicit, dated, and signed with the
for some sample or reagent disposal. The disposal area should
initials of the person responsible.
bewellseparatedfromthelaboratoryareaandmeetapplicable
8.2 Although the laboratory should maintain a library of
safetystandards.Thespecificdisposalmethodsarenotcovered
references for its methodology, it is inconvenient to use a
in this guide. In some standards the disposal method for the
reference book at the bench. Therefore, it is desirable to
reagent and sample will be defined. When this information is
establishSOPsforthelaboratory.Eachsetofdirectionsshould
not supplied in the standard, useful information may be
be identified on each page, and contain the date of the
obtained from guides to control hazardous chemical spills, and
document, date of the revision, if applicable, and the page
manuals of laboratory safety which are available from various
number out of the total number of pages. This is to serve the
laboratorysupplyfirms(seeRef (4)).Disposaltothemunicipal
purposeofprovidingadocumentcontrolprocedureorameans
sewersshouldbeinaccordancewithapplicablelocal,state,and
of maintaining the procedures in a complete and current
federal regulations.
condition.
7.3.7 The mix-up of samples and the cross-contamination
8.3 A readily accessible office file of methods used should
hazards are more easily avoided when there is adequate bench
be maintained and kept current.
spaceorworkingareaperanalyst.Asageneralguidelinethere
2 2
8.4 The detailed procedures of formerly used methods
should be 14 to 28 m (150 to 300 ft ) per analyst or 3.6 to
should be archived for reference and documentation of prior
7.3m(12to24linealft)ofbenchspaceperanalyst.Thespace
procedures.
requirement per analyst depends upon the equipment or appa-
ratus that is being used, the number of samples the analyst is
9. Metrology Systems
expected to handle at any one time, and the number of
operations that are to be performed by a single analyst. The
9.1 The basic system of weights and measurements for a
laboratory may also have a requirement for specialized
laboratory should be as comprehensive as required to conduct
facilities, such as a perchloric acid hood. The lighting level
all the necessary measurements. Mass standards traceable to
may vary from 50 to 100 fc (538 to 1076 lx) depending upon
the National Institute of Standards and Technology (NIST) or
the tasks being performed in the area (5).
othernationalstandardslaboratoryprovidethestandardagainst
7.3.8 The reliability of the instruments is sometimes af-
which the laboratory balances may be checked. This also
fectedbyelectricalsupplyfactorsincludingvoltage,frequency, provides the basic method of volumetric calibration of glass-
and electrical fields. Some instruments may require a separate
ware. A thermometer traceable to NIST or other national
grounded circuit or a regulated power supply for stable standards laboratory provides a check on the temperature
operation.Suchasupplyisrecommendedasagoodlaboratory
measurement systems.Aset of color standards may be used to
practice. A battery powered back-up supply is recommended, check the wavelength calibration and the stray light character-
especially for computer controlled equipment and data acqui-
istics of a spectrometer or colorimeter. These systems should
sition devices. be common to most analytical laboratories. Many of these
D3614 − 07 (2021)
systems, such as balances and spectrometers, may be main- encouraged for conformation of the adequacy of the technique
tained and certified under an annual service contract. and the analyst. This is also a useful tool for trouble-shooting
deficiencies.
9.2 Atmospheric sampling oft
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