ASTM E2437-05
(Practice)Standard Practice for Designing and Validating Performance-Based Test Methods for the Analysis of Metals, Ores, and Related Materials (Withdrawn 2014)
Standard Practice for Designing and Validating Performance-Based Test Methods for the Analysis of Metals, Ores, and Related Materials (Withdrawn 2014)
SCOPE
1.1 This practice covers a model for designing and validating performance-based, ISO 17025-compliant, standard test methods for the instrumental chemical analysis of metals, ores, and related materials. The principles in this practice can also be applied to the development of test methods used to determine the composition of other materials.
1.2 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.
WITHDRAWN RATIONALE
This practice covered a model for designing and validating performance-based, ISO 17025-compliant, standard test methods for the instrumental chemical analysis of metals, ores, and related materials.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in January 2014 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E2437 − 05
StandardPractice for
Designing and Validating Performance-Based Test Methods
for the Analysis of Metals, Ores, and Related Materials
This standard is issued under the fixed designation E2437; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 ISO Standards
ISO 17025 General Requirements for the Competence of
1.1 This practice covers a model for designing and validat-
Testing and Calibration Laboratories
ing performance-based, ISO 17025-compliant, standard test
ISOGuide31 ReferenceMaterials—ContentsofCertificates
methods for the instrumental chemical analysis of metals, ores,
and Labels
andrelatedmaterials.Theprinciplesinthispracticecanalsobe
ISO Guide 32 Calibration in Analytical Chemistry and Use
applied to the development of test methods used to determine
of Certified Reference Materials
the composition of other materials.
ISO Guide 34 General Requirements for the Competence of
1.2 This standard does not purport to address all of the
Reference Material Producers
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 Definitions—For definitions of terms used in this
bility of regulatory limitations prior to use.
practice, refer to Terminology E135.
3.2 Definitions of Terms Specific to This Standard:
2. Referenced Documents
3.2.1 aim interlaboratory uncertainty, n— the maximum
2.1 ASTM Standards:
deviation (95 % confidence) to be allowed in the design of the
E135 Terminology Relating to Analytical Chemistry for
total interlaboratory uncertainty of a test method, beginning
Metals, Ores, and Related Materials
withthepreparationofahomogeneoussampleandendingwith
E305 Practice for Establishing and Controlling Atomic
a final report value to the client.
Emission Spectrochemical Analytical Curves
3.2.2 aim uncertainty budget, n—during the development of
E691 Practice for Conducting an Interlaboratory Study to
astandardperformance-basedtestmethod,thetargetallocation
Determine the Precision of a Test Method
of interlaboratory measurement uncertainty among specific
E1329 Practice for Verification and Use of Control Charts in
components of a measurement process that contribute signifi-
Spectrochemical Analysis
cantly to the overall deviation.
E1601 Practice for Conducting an Interlaboratory Study to
3.2.2.1 Discussion—The target allocation is made by the
Evaluate the Performance of an Analytical Method
task group as described in Practice E2165 and serves as
E1621 Guide for X-Ray Emission Spectrometric Analysis
guidance for interlaboratory test participants during method
E2027 Practice for Conducting Proficiency Tests in the
testing.
ChemicalAnalysis of Metals, Ores, and Related Materials
3.2.3 interlaboratory uncertainty, n—in a performance
E2165 Practice for Establishing an Uncertainty Budget for
based standard test method, the precision (95 % confidence)
the Chemical Analysis of Metals, Ores, and Related
that participating laboratories achieved during interlaboratory
Materials (Withdrawn 2007)
studies, beginning with the preparation of a homogeneous
sample and ending with a final report value to the client.
This practice is under the jurisdiction of ASTM Committee E01 on Analytical 3.2.4 intralaboratory uncertainty, n—in a performance
Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
based standard test method, the precision (95 % confidence)
Subcommittee E01.22 on Laboratory Quality.
that a laboratory achieves when the method is used by more
Current edition approved May 1, 2005. Published July 2005. DOI: 10.1520/
than one operator. In test methods that establish maximum
E2437-05.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
allowable intralaboratory uncertainties, users must be able to
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.
3 4 rd
The last approved version of this historical standard is referenced on Available from American National Standards Institute (ANSI), 25 W. 43 St.,
th
www.astm.org. 4 Floor, New York, NY 10036 (www.ansi.org).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2437 − 05
demonstrate compliance with those uncertainties in order to tainedduringbothmethoddevelopmentandproficiencytesting
report that a given test result was produced using the named using existing methods is a function of concentration, per
method. Practice E2165, it follows that the interlaboratory testing of a
new test method should perform no worse than its predeces-
3.2.5 performance based method, n—a test method that
sors. Practice E2165 describes how historical interlaboratory
defines (1) the general approaches for sampling, sample
test results can be used to set aim data quality objectives for
preparation, and making measurements on a specified type of
new test methods. This practice incorporates those aim data
material, and (2) defines maximum allowable uncertainties for
quality objectives in developing uncertainty budgets used in
each measured constituent over its validated concentration
the design, development, and testing of performance-based
range.
methods. This approach ensures that interlaboratory test data
3.2.6 uncertainty budget, n—the allocation of intralabora-
included in Precision and Bias statements are consistent with
tory measurement uncertainty among specific components of a
that associated with the other standard test methods.
measurementprocessthatcontributesignificantlytotheoverall
deviation.
5. Summary of Practice
5.1 The remaining parts of this practice provide instructions
4. Significance and Use
for planning a performance-based method development
4.1 This practice provides guidance for methods-writing
project, conducting the necessary validation and interlabora-
task group leaders and members in planning, drafting, and
tory precision tests, and documenting the results.
testing performance-based test methods. It also guides users of
5.2 The organization of the rest of the practice guides the
performance-based methods in interpreting and applying them
task group through the following steps:
properly.
5.2.1 Section 6—Sets overall objectives for the project,
4.2 Standard test methods, particularly those that cover the
detailed only to the extent needed to convince the task group
instrumental analysis of commercial materials by specific
that the project can be accomplished as planned.
measurement techniques, such as point-to-plane atomic
5.2.2 Section 7—Sets the technical parameters to be incor-
emission, x-ray fluorescence, inductively-coupled plasma, and
porated in the new test method. Establishes details needed to
atomic absorption spectroscopy, need sufficient flexibility to
facilitate organizing and drafting a test method.
accommodate the various applicable makes and models of
5.2.3 Section 8—Addresses writing the first draft of the test
instrumentation.At the same time, these standard test methods
method.
must be capable of generating commercially-useful results that
5.2.4 Section 9—Describes how to verify the draft method
aresufficientlyaccurateandprecise.Theseneedscanbemetby
before entering into more extensive interlaboratory testing.
the use of performance-based test methods that rely more on
5.2.5 Section 10—Discusses writing the interlaboratory
the demonstrated quality of the test results than on strict
protocol plan so that all of the needed data is available in a
adherence to specific procedural steps. One model for devel-
form that is easily processed.
oping these methods is described in this practice.
5.2.6 Section 11—Describes task group work in conducting
4.3 It is expected that laboratories using performance-based
the interlaboratory test.
standard test methods developed in accordance with this
5.2.7 Section 12—Describes performance-based method in-
practice will prepare their own detailed work instructions.
formation to be included in the Research Report.
Theseworkinstructionswillincludedetailedoperatinginstruc-
5.2.8 Section 13—Addresses finalizing the text of the test
tionsforthespecificlaboratory,thespecificreferencematerials
method after interlaboratory testing is satisfactorily completed.
(RMs) employed, and performance acceptance criteria to be
applied in that laboratory. It is also expected that those
6. Setting Objectives
laboratories will document their own performance data using
6.1 For the material to be tested, identify and list applicable
their work instruction to show that their data are consistent
national and international product specifications, sampling
with the standard test method’s Precision and Bias statement.
practices, and standard test methods. Be sure to reference these
Over time, it is also expected that, when applicable, an
documents appropriately in the new test method.
individual laboratory’s proficiency test results will also be
consistent with its documented performance. 6.2 List the elements and concentration ranges to be in-
cludedinthematerialstobeanalyzedusingthemethodandlist
4.4 TraditionalASTM Precision and Bias statements, devel-
the subset of those elements and concentration ranges to be
oped during interlaboratory testing in accordance with Prac-
incorporated as analytes in the new test method.
ticesE691andE1601,provideinformationontheperformance
achieved by participating laboratories. Intralaboratory preci- 6.3 Determine how measurement uncertainty and data qual-
sion can be estimated by dividing the Repeatability index, r, in ity objectives will be handled.
the Precision and Bias Table by the square root of 2, at any 6.3.1 To comply with ASTM requirements, plan to prepare
tested concentration. Proficiency test programs, such as those a precision and bias statement. To comply with ISO 17025
following Practice E2027, periodically provide interlaboratory requirements, plan to identify all significant sources of mea-
performance data from larger numbers of laboratories, using a surement uncertainty and to calculate the intralaboratory un-
variety of test methods, at many different concentrations over certainty (3.2.3) from the information in the precision and bias
an extended time period. Since interlaboratory precision ob- statement.
E2437 − 05
6.3.2 To help laboratories use the new performance-based 7.2.3 Calibration and Calibrants:
test method more effectively, the task group should consider 7.2.3.1 For each element and concentration range, ensure
developing an uncertainty budget (3.2.5). That budget may be the availability of sufficient numbers of acceptable calibrants.
developed as suggested in this practice, or in a different way, Sufficient numbers of calibrants must be available to define the
provided that the minimum requirements in 6.3.1 are met. shape of each calibration curve over the concentration range of
6.3.3 If the task group elects to develop an uncertainty interest and to allow compensation for interelement effects.
budget as described in this practice, it should attempt to Refer to Practice E305 or Guide E1621 for additional back-
establish each component of its aim uncertainty budget as ground information. An acceptable calibrant is a CRM that is
defined in Practice E2165. In some cases, the method of choice compliant with ISO Guide 34, or an RM that is traceable to a
may not be optimum for each analyte to be covered. In those CRM or the appropriate SI unit, and has an estimated uncer-
cases, if the anticipated performance meets applicable specifi- tainty small enough to make it possible to meet the aim data
cation requirements, the task group should set its data quality quality objectives of the method. Some methods may be
objectives in a way that is compliant with specifications calibrated directly with CRMs used in the as-received condi-
(commercial needs) and attainable performance. The compo- tion. Others may require the dissolution of chip or solid CRMs
nents of uncertainty will be useful in planning and developing or the use of CRM spectrometric solutions that must be
the performance-based test method. combined with other reagents or materials in order to provide
suitable calibrants. In cases where CRMs are combined with
7. Setting Technical Parameters
other reagents to make calibrants, the standard test method
7.1 Select the Approach to Make the Measurements: must provide strict specifications on those reagents to ensure
7.1.1 Select a measurement technique that represents an that the calibrants’ assigned quantity values are accurate and
optimum choice based on: (1) wide acceptance and use have correct uncertainty estimates.
throughout the industry, (2) anticipated ability to measure all 7.2.3.2 Set aim uncertainty limits for all calibration curves
elements and concentration ranges in conformance with the and calibrants. See X1.2.2.2 and X1.2.2.3 for a suggested
aimuncertaintybudget,(3)anticipatedsustainedavailabilityof approach.
Certified Reference Materials (CRMs) for achieving traceable 7.2.4 Verifiers—Ensure the availability of traceable refer-
calibrations (Note 1) of all elements and concentration ranges, ence materials that comply with the requirements of 7.2.3, but
and (4) anticipated sustained availability of homogeneous
are reserved for use to independently verify the calibration
materials needed for statistical control of the method. function.
7.2.5 Quality Control—For each element and concentration
NOTE 1—This practice assumes the use of a Type III calibration as
range to be determined, ensure the availability of material that
defined in ISO Guide 32. Types I and II do not require the use of CRMs.
can be used for control in accordance with ISO 17025, clause
7.1.2 Select the sampling equipment and procedure. Re-
5.9. For planning purposes, consider the availability of at least
solve any questions about the adequacy of the sampling
two concentrations for each calibration range, one at about
process. Ensure its acceptability to users. If a new or revised
20 % and one at about 80 % of the maximum values. Avail-
sampling practice is needed, arrange for the development of
ability means that a typical laboratory can acquire the needed
that practice and establish acceptability with those who are
materialsinareasonableway,eithercommerciallyorin-house.
responsible for performing the sampli
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