ASTM C1068-96e1
(Guide)Standard Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
Standard Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Industry
SCOPE
1.1 This guide provides guidance for selecting, validating, and qualifying measurement methods when qualification is required for a specific program. The recommended practices presented in this guide provide a major part of a quality assurance program for the laboratory data (see Fig. 1). Qualification helps to assure that the data produced will meet requirements established for those data.
1.2 The activities intended to assure the quality of analytical laboratory measurement data are diagrammed in Fig. 1. Discussion and guidance related to some of these activities appear in the following sections: Section Selection of Measurement Methods 5 Validation of Measurement Methods 6 Qualification of Measurement Methods 7 Control 8 Personnel Qualification 9
1.3 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.
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e1
Designation: C 1068 – 96
Standard Guide for
Qualification of Measurement Methods by a Laboratory
Within the Nuclear Industry
This standard is issued under the fixed designation C 1068; 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.
e NOTE—Editorial changes were made throughout in March 1997.
1. Scope
1.1 This guide provides guidance for selecting, validating,
and qualifying measurement methods when qualification is
required for a specific program. The recommended practices
presented in this guide provide a major part of a quality
assurance program for the laboratory data (see Fig. 1). Quali-
fication helps to assure that the data produced will meet
established requirements.
1.2 The activities intended to assure the quality of analytical
laboratory measurement data are diagrammed in Fig. 1. Dis-
cussion and guidance related to some of these activities appear
in the following sections:
Section
Selection of Measurement Methods 5
Validation of Measurement Methods 6
Qualification of Measurement Methods 7
Control 8
Personnel Qualification 9
1.3 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 appro-
FIG. 1 Quality Assurance of Analytical Laboratory Data
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
C 1210 Guide for Establishing a Measurement System
Quality Control Program for Analytical Chemistry Labo-
2. Referenced Documents
ratories Within the Nuclear Industry
2.1 ASTM Standards:
C 1297 Guide for Laboratory Analysts for the Analysis of
C 986 Guide for Developing Training Programs in the
Nuclear Fuel Cycle Materials
Nuclear Fuel Cycle
C 1009 Guide for Establishing a Quality Assurance Pro-
3. Terminology
gram for Analytical Chemistry Laboratories Within the
3.1 Definitions of Terms Specific to This Standard:
Nuclear Industry
3.1.1 qualification—a formal process to provide a desired
C 1128 Guide for Preparation of Working Reference Mate-
level of confidence that measurement methods used will
rials for Use in the Analysis of Nuclear Fuel Cycle
produce data suitable for their intended use. The methods must
Materials
meet established criteria prior to use and must be used under
C 1156 Guide for Establishing Calibration for a Measure-
conditions established for qualifications.
ment Method Used to Analyze Nuclear Fuel Cycle Mate-
rials
4. Significance and Use
4.1 Because of concerns for safety and the protection of
nuclear materials from theft, stringent specifications are placed
This guide is under the jurisdiction of ASTM Committee C-26 on Nuclear Fuel
Cycle and is the direct responsibility of Subcommittee C26.08 on Quality Assurance
on chemical processes and the chemical and physical proper-
Applications.
ties of nuclear materials. Strict requirements for the control and
Current edition approved Dec. 10, 1996. Published January 1997. Originally
accountability of nuclear materials are imposed on the users of
published as C 1068 – 86. Last previous edition C 1068 – 91.
Annual Book of ASTM Standards, Vol 12.01. those materials. Therefore, when analyses are made by a
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
C 1068
laboratory to support a project such as the fabrication of sound technology. This means that proven laboratory and
nuclear fuel materials, various performance requirements may instrumental techniques are used in ways recognized and
be imposed on the laboratory. One such requirement is often accepted by the community of users.
the use of qualified methods. Their use gives greater assurance 5.2.2 Interferences—The method should not be adversely
that the data produced will be satisfactory for the intended use affected by components in the matrix of the material to be
of those data. A qualified method will help assure that the data analyzed. Knowledge about the method’s limitations and about
produced will be comparable to data produced by the same the composition of the material should be used to determine if
qualified method in other laboratories. the analysis will be affected by interferences. Other potential
4.2 This guide provides guidance for qualifying measure- interferences such as environmental or electrical/electronic
ment methods and for maintaining qualification. Even though conditions should be considered in the selection process.
all practices would be used for most qualification programs, 5.2.3 Range—The method should be capable of responding
there may be situations in which only a selected portion would adequately across the range of concentration levels that will be
be required. Care should be taken, however, that the effective- encountered for the constituent to be measured. This require-
ness of qualification is not reduced when applying these ment is most often of concern for methods used to measure
practices selectively. The recommended practices in this guide impurities in materials since impurity concentrations may
are generic; based on these practices, specific actions should be fluctuate to a greater extent than other constituents. It is
developed to establish a qualification program. important that the measurement technique used discriminates
adequately between concentration levels encountered. The
5. Selection of Measurement Methods
lowest concentration level that can be measured reliably should
5.1 General:
be clearly established (detection limit).
5.1.1 Before qualifying a method for a specific application,
5.2.4 Reliability of Method—The method must be capable
there should be assurance that the method has been properly
of producing data that will meet the bias and precision
selected for that application. The guidance given in this section
requirements established for the required analysis under the
can be used to assess the adequacy of the method’s application.
expected conditions of use. The requirements are usually
The guidance can also be used to select a new method when a
established by the user of the data and they should be based on
new measurement capability is required within a laboratory.
the concentration levels of the constituents to be measured and
5.1.2 Measurement methods generally can be classified as
on specification limits set for the constituents.
one of three types as follows:
6. Validation of Measurement Methods
5.1.2.1 Those published as national or international consen-
sus standards,
6.1 There are occasions when it is desirable to investigate
5.1.2.2 Those established as acceptable for a specific appli- the applicability of a method to a particular use. This may be
cation based on long-term and wide usage, and
the case when the method has had limited use or it is being
5.1.2.3 Those having limited use, for example, those used
considered for a new or unique application. To provide some
only by a few laboratories or those that are relatively new.
confidence that a qualification effort would be successful, it
5.1.3 For some applications, there is a choice available of
may be desirable to validate the application of the method.
two or more acceptable methods. In those cases, one method is
Validation is not a mandatory step in the selection and
usually recognized as the reference method, particularly if it is
qualification process, but it can prevent wasted effort from
a published standard or if it is capable of producing the least
attempts to qualify inadequate methods.
bias and best precision.
6.2 Validation of a method is usually done by an analyst
5.1.4 When choosing a method, the four technical factors
under controlled conditions. Basically, validation involves
affecting its application should be evaluated as follows:
investigating any or all of the selection criteria in 5.2. The
5.1.4.1 Is the method actually capable of providing the
intent is to define method capability and to determine if the
specific analysis required?
method can be properly applied as intended. If modification of
5.1.4.2 Is the method free of adverse effects from the matrix
the method is required for it to be applicable, validation will
of the particular material requiring analysis?
provide the technical information needed for modification.
5.1.4.3 Does the method have the sensitivity and range to
Validation also provides the experience and information to
cover adequately the concentration levels that will be encoun-
write a detailed procedure if necessary. The result of the
tered? validation process will be either the rejection of a proposed
5.1.4.4 Is the method capable of producing data that will
method or confidence that it is acceptable for use as intended.
meet established bias and precision requirements?
7. Qualification of Measurement Methods
5.1.4.5 Each question must be answered in the affirmative
for a method to be acceptable. Although cost is not recognized 7.1 General:
as a criterion affecting selection, it could be of concern. 7.1.1 Although a method is selected based on the criteria in
5.1.5 The selection of a method should be based on the 5.2 of this guide, there is no assurance that a laboratory can
criteria in 5.2. In situations where a reference method and one actually obtain the performance expected from the method. In
or more acceptable methods are available, there should be no addition, there may not be sufficient assurance that the method
technical restrictions placed on which method is used. is in fact adequate for its intended use. To provide those
5.2 Recommended Practices: assurances, demonstration is included in the qualification
5.2.1 Technical Basis—The method should be based on process.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
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C 1068
7.1.2 Qualification requires having a laboratory demonstrate same criteria given in 7.2.3.1 of this guide. Another should be
that a method can produce acceptable data under specified used to demonstrate the detection limit of the method. When
conditions of qualification. Demonstration must be done under possible, the detection limit should be sufficiently below the
actual operating conditions and not under ideal test conditions. specification limit to determine whether or not the concentra-
A specified material is analyzed to produce a specified amount tion level of the impurity is within specification. Both test
of data. These data are evaluated by the person or organization materials would serve to demonstrate the range of the method.
that is responsible for approving qualification. The procedure When a method requires one or more standards for calibration,
established for demonstration should include provisions for the calibration standard(s) that will be used should be specified.
handling failures in the demonstration and for repeating the See Guide C 1156.
demonstration should the method not be used for a specified
7.2.4 Qualification Requirements—A procedure to be fol-
period of time. Demonstration could also include producing
lowed during demonstration should be established. The proce-
other evidence such as appropriate literature references that the
dure that will govern qualification should include the following
method is in fact applicable to the material to be analyzed.
criteria:
7.2 Recommended Practices:
7.2.4.1 Bias—A statistical sampling and hypothesis testing
plan should be developed such that the risk of qualifying a
7.2.1 Procedures—The use of a method to make a labora-
tory measurement involves taking discrete actions in a specific method is acceptably small when the true bias exceeds the
stated requirement and the risk of not qualifying the method is
order. Any change in an action or in the order may produce
unsatisfactory data. To minimize potential problems, written, acceptably small when the true bias is zero. The plan would
include the number of analyses of a test standard required to
stepwise procedures should be provided within the methods. It
is important that procedures are well-written, complete, and control these risks at acceptably small levels and would express
the requirement for qualifying based on bias as a statistical
correct. They should receive technical and editorial reviews,
and should be approved by appropriate management. Approval hypothesis testing procedure.
by the user of the data to be produced also may be required.
7.2.4.2 Precision—The precision requirement should state a
Procedures prepared in accordance with Guide C 1009 will
value of the true standard deviation (larger than zero) that is
meet these criteria.
both desirable and practical to maintain together with an upper
limit, above which the true standard deviation would be
7.2.2 Method Performance Requirements—To provide ac-
unacceptable. A statistical sampling and hypothesis testing plan
ceptable data, the method must be capable of meeting perfor-
should then be developed such that: the risk of qualifying a
mance requirements for bias, precision, and range. Before a
method is acceptably small when the true standard deviation
laboratory demonstrates its capability, these requirements
should be clearly established (this should be done even before exceeds the specified upper limit, and the risk of not qualifying
the method is acceptably small when the true standard devia-
a method is selected for use; see 5.2). Specifications estab-
lished for a process or material are the primary source of tion is less than or equal to the desired value. The plan would
include the number of analyses of a test material required to
information on which the performance requirements are based.
The performance requirements should be used to establish control these risks at acceptably small levels and would express
the requirement for qualifying based on precision as a statis-
conditions required for qualification. Such conditions may
require a statistically designed experiment to allow for other tical hypothesis testing procedure.
sources of variability such as the number of analysts or
7.2.4.3 Range—A requirement, such as the following,
instruments, or both, as well as the concentration range of
should be stated when range is of concern: “Data obtained from
interest.
the analysis of test materials, including calibration standards,
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