E01.22 - Laboratory Quality

SIGNIFICANCE AND USE
5.1 This guide is intended for use by developers of RMs and CRMs for the metals and mining industries.  
5.2 The guidance is related to uniform procedures and requirements and is intended to prevent the proliferation of widely varying documentation practices, definitions, and terminology. Where the statements in this guide are made as imperatives, it is because the stated practices are fundamental to chemical metrology, not to CRM/RM development.  
5.3 The material in this guide is intended to supplement and to clarify the contents of ISO Guide 31 and to provide guidance specific to the needs of the metals and mining industries.  
5.4 The documents described in this guide are intended to contain the minimum amount of information required for a user to understand the material, to help a user judge the quality of the product, and to help a user employ it in appropriate ways. Neither this guide nor resultant documents are meant to be encyclopedic.  
5.5 Because this document is a standard guide, it is intended to educate those who are involved in laboratory operation, quality system development and maintenance, reference material development, and accreditation of laboratory operations within the scope of a quality system. It must be understood by all parties that the elements of this guide discuss optional practices having numerous choices for accomplishment and documentation. However, this guide does not constitute requirements for assessment and accreditation. An obvious example is statistical evaluation for consensus value and uncertainty calculations, which can take many forms with no single, correct choice for any given case.  
5.6 When using this guide, CRM developers will set goals for the material under development, such as target uncertainties for homogeneity and for overall coverage intervals for assigned values. These choices are based on the intended uses of a CRM. The material, property values, and their uncertainties may or may not meet the set goals...
SCOPE
1.1 This guide is designed to explain and to clarify documentation that accompanies an RM or a certified reference material (CRM). It explains the contents of certificates of analysis for CRMs and product information documents for RMs, based on existing international standards and guides. It briefly touches on the minimum requirements for a label attached to the CRM/RM unit or unit container and to the package containing the unit or unit container.  
1.2 This guide provides some basic guidance on calculation of consensus values and uncertainty estimates for CRMs and RMs with examples of approaches commonly used by national metrology institutes and suggestions for sources of information.  
1.3 Units—The values stated in SI units are to be regarded as the standard, whenever applicable. Values can be traceable to other higher-order reference systems, including Rockwell Hardness, pH, and other systems defined by an international standard or peer-reviewed publication.  
1.4 Contents—Sections and topics within this guide are enumerated below:    
Section  
Title  
1  
Scope  
2  
Referenced Documents  
3  
Terminology  
4  
Summary of Guide  
5  
Significance and Use  
6  
Contents of a Certificate of Analysis or Reference Material Documentation  
7  
Labels  
8  
Technical and Statistical Evaluations  
9  
Procedures for Consensus Value Calculations  
10  
Estimation of Uncertainty  
11  
Reporting Values and Uncertainty Estimates  
12  
International System of Units  
13  
Keywords  
Appendix X1  
Working Near Zero  
Appendix X2  
Working Near 100 %  
Appendix X3  
Censored Values  
Appendix X4  
Examples of Language for Sections of a Certificate of Analysis  
1.5 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 enviro...

SIGNIFICANCE AND USE
4.1 Method validation is a process of demonstrating that the method meets the required performance capabilities. International standards such as ISO/IEC 17025, certifying bodies, and regulatory agencies require evidence that analytical methods are capable of producing valid results. This applies to laboratories using published standard test methods, modified standard test methods, and in-house test methods.  
4.2 Although a collaborative study is part of this guide, this guide may be used by a single laboratory for method validation when a formal collaboration study is not practical. This guide may also be applied before a full collaboration study to predict the reliability of the method.  
4.3 The use of multiple validation techniques described in this guide increases confidence in the validity or application of the method.  
4.4 It is beyond the scope of this guide to describe fully the fundamental considerations in Section 5. For a more descriptive definition of these concepts, refer to the International Union of Pure and Applied Chemistry (IUPAC) technical report, “Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis” (1), the IUPAC Compendium of Analytical Nomenclature (Orange Book) (2), and the Eurachem publication, The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics (3).
SCOPE
1.1 This guide describes procedures for the validation of chemical and spectrochemical analytical test methods that are used by a metals, ores, and related materials analysis laboratory.  
1.2 This guide may be applied to the validation of laboratory developed (in-house) methods, addition of analytes to an existing standard test method, variation or scope expansion of an existing standard method, or the use of new or different laboratory equipment.  
1.3 The suggested approaches in this guide may also be used to validate the implementation of standard test methods used routinely by laboratories of the mining, ore processing, and metals industry.  
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 Ideally, interlaboratory testing of a method is conducted by a randomly chosen group of laboratories that typifies the kind of laboratory that is likely to use the method. In actuality, this ideal is only approximated by the laboratories that are available and willing to undertake the test work. The coordinator of the program must ensure that every participating laboratory has appropriate facilities and personnel and performs the method exactly as written. If this goal is achieved, the statistics developed during the ILS will be adequate for determining if the method is capable of producing satisfactory precision in actual use. If the program includes certified reference materials, the test data also provide information concerning the bias of the method. The statistics provide a general guide to the expected performance of the method.
SCOPE
1.1 This practice covers procedures and statistics for an interlaboratory study (ILS) of the performance of an analytical method. The study provides statistical values which are useful in determining if a method is satisfactory for the purposes for which it was developed. These statistical values may be incorporated in the method's precision and bias section. This practice discusses the meaning of the statistics and what users of analytical methods may learn from them.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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
4.1 This document provides guidance for the implementation of procedures for the preparation, testing, and documentation of an in-house reference material (hereafter called an iRM) to be used for a number of purposes, enumerated in the following document, associated with development, validation, and control of chemical and physical measurement processes.  
4.2 This guide is primarily concerned with characterization of the chemical compositions of metals, ores, and related materials. For all these materials, there is a continuing, strong demand for reference materials (RMs) that is difficult for metrology institutes and private certified reference material (CRM) developers to meet because CRM development requires substantial investments of time and money. The metals and mining industries consume RMs and create new product and by-product compositions at high rates. They use analytical methods that provide rapid and accurate determinations, and both quality assurance and quality control can be maintained using efficient procedures provided appropriate iRMs are available.  
4.3 The user of this guide must recognize that development of an iRM for any purpose carries with it the responsibility to design and execute the development process correctly, and to document the process thoroughly. In addition, the user of an iRM bears the responsibility for correct use of the iRM material within its design limitations.  
4.4 This guide contains discussions on material selection and sampling for RMs with some attention given to conversion to the final forms.  
4.5 The use of iRMs is appropriate for control chart procedures to demonstrate that chemical measurement processes are under statistical control. This function requires demonstration of sufficient homogeneity of a material, but it does not require assignment of chemical and physical property values with associated, exhaustively evaluated uncertainties.  
4.6 The use of iRMs is appropriate for calibration of test methods ...
SCOPE
1.1 This document provides guidance for the implementation of procedures for preparation of in-house reference materials for analytical testing of metals, ores, slags, and other materials encountered within the metals and mining industries.  
1.2 This guide is applicable to the production of reference materials only (usually for internal use) and does not apply to the production of certified reference materials (CRMs). Materials may include metals, alloys, minerals, geological materials, manufacturing intermediates, and byproducts. Samples may be in a number of physical forms including blocks, disks, rods, wires, chips, granules, powders, and liquids.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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
4.1 Many competent analytical laboratories comply with accepted quality system requirements. When using standard test methods, their test results on the same sample should agree with those from other similar laboratories within the reproducibility estimates index (R) published in the standard. Reproducibility estimates are generated as part of the interlaboratory studies (ILS), of the type described in Practice E1601. Competent laboratories participate in proficiency tests, such as those conducted in accordance with Practice E2027, to confirm that they perform consistently over time. In both ILS and proficiency testing protocols, it is generally assumed that only one work station is used to generate the data.  
4.2 Many laboratories have workloads, or logistical requirements, or both, that dictate the use of multiple work stations. Some have multiple stations in the same area (central laboratory format). Other stations are scattered throughout a facility (at-line laboratory format) and in some cases may even reside at different facilities. Often, analysis reports do not identify the workstation used for the testing, even if workstations differ in their testing uncertainties. Problems can arise if clients mistakenly attribute variation in report values to process rather than workstation variability. These problems can be minimized if the laboratory organization determines the overall uncertainty associated with results reported from multiple workstations and assesses the significance of the analytical uncertainty to the production process.  
4.3 This guide describes a protocol for efficiently optimizing and controlling variability in test results from different workstations used to perform the same test. It harmonizes calibration and control protocols, thereby providing the same level of measurement traceability and control to all workstations. It streamlines documentation and training requirements, thereby facilitating flexibility in personnel assignments. Finally...
SCOPE
1.1 This guide describes a protocol for optimizing, controlling, and reporting test method uncertainties from multiple workstations in the same laboratory organization. It does not apply when different test methods, dissimilar instruments, or different parts of the same laboratory organization function independently to validate or verify the accuracy of a specific analytical measurement.  
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.

SIGNIFICANCE AND USE
4.1 An accountability and quality control system is established by laboratory management to improve the quality of its results. It provides documented records which serve to assure users of the laboratory's services that a specified level of precision is achieved in the routine performance of its measurements and that the data reported were obtained from the samples submitted. The system also provides for: early warning to analysts when methods or equipment begin to develop a bias or show deterioration of precision; the protection and retrievability of data (results); traceability and control of samples as they are processed through the laboratory; good communication of sample information between submitters, analysts, and supervision; and information on sample processing history. This guide describes such a system. Other accountability and quality control programs can be developed. Such programs can be equivalent to the program in this guide if they provide all of the benefits mentioned above.
SCOPE
1.1 This guide covers the essential aspects of an accountability and quality control program for a chemical analysis laboratory. The reasons for establishing and operating such a program are discussed.  
1.2 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
4.1 Method validation is a process of demonstrating that the method meets the required performance capabilities. International standards such as ISO/IEC 17025, certifying bodies, and regulatory agencies require evidence that analytical methods are capable of producing valid results. This applies to laboratories using published standard test methods, modified standard test methods, and in-house test methods.  
4.2 Although a collaborative study is part of this guide, this guide may be used by a single laboratory for method validation when a formal collaboration study is not practical. This guide may also be applied before a full collaboration study to predict the reliability of the method.  
4.3 The use of multiple validation techniques described in this guide increases confidence in the validity or application of the method.  
4.4 It is beyond the scope of this guide to describe fully the fundamental considerations in Section 5. For a more descriptive definition of these concepts, refer to the International Union of Pure and Applied Chemistry (IUPAC) technical report, “Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis” (1), the IUPAC Compendium of Analytical Nomenclature (Orange Book) (2), and the Eurachem publication, The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics (3).
SCOPE
1.1 This guide describes procedures for the validation of chemical and spectrochemical analytical test methods that are used by a metals, ores, and related materials analysis laboratory.  
1.2 This guide may be applied to the validation of laboratory developed (in-house) methods, addition of analytes to an existing standard test method, variation or scope expansion of an existing standard method, or the use of new or different laboratory equipment.  
1.3 The suggested approaches in this guide may also be used to validate the implementation of standard test methods used routinely by laboratories of the mining, ore processing, and metals industry.  
1.4 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
4.1 Method validation is a process of demonstrating that the method meets the required performance capabilities. International standards such as ISO/IEC 17025, certifying bodies, and regulatory agencies require evidence that analytical methods are capable of producing valid results. This applies to laboratories using published standard test methods, modified standard test methods, and in-house test methods.  
4.2 Although a collaborative study is part of this guide, this guide may be used by a single laboratory for method validation when a formal collaboration study is not practical. This guide may also be applied before a full collaboration study to predict the reliability of the method.  
4.3 The use of multiple validation techniques described in this guide increases confidence in the validity or application of the method.  
4.4 It is beyond the scope of this guide to describe fully the fundamental considerations in Section 5. For a more descriptive definition of these concepts, refer to the International Union of Pure and Applied Chemistry (IUPAC) technical report, “Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis,”5 the IUPAC Compendium of Analytical Nomenclature (Orange Book),6 and the Eurachem publication, The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics.7
SCOPE
1.1 This guide describes procedures for the validation of chemical and spectrochemical analytical test methods that are used by a metals, ores, and related materials analysis laboratory.  
1.2 This guide may be applied to the validation of laboratory developed (in-house) methods, addition of analytes to an existing standard test method, variation or scope expansion of an existing standard method, or the use of new or different laboratory equipment.  
1.3 The suggested approaches in this guide may also be used to validate the implementation of standard test methods used routinely by laboratories of the mining, ore processing, and metals industry.  
1.4 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
4.1 This practice sets the basic requirements for proficiency test programs in the chemical analysis of metals, ores, and related materials. It does not set specific procedural requirements, but does establish a framework for particular programs, including those with either small or large numbers of participants.  
4.2 The data from proficiency testing programs can be used for value assignments for in-house reference materials developed in accordance with Guide E2972.  
4.3 Most accreditation bodies require that laboratories participate regularly in proficiency testing programs that they have accepted for this purpose. Therefore, it is essential that each program comply with accepted principles including technical requirements, statistical procedures (see Annex A1), and quality management (see Annex A2).
SCOPE
1.1 This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO/IEC 17043 and Guide E1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.  
1.2 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
4.1 An accountability and quality control system is established by laboratory management to improve the quality of its results. It provides documented records which serve to assure users of the laboratory's services that a specified level of precision is achieved in the routine performance of its measurements and that the data reported were obtained from the samples submitted. The system also provides for: early warning to analysts when methods or equipment begin to develop a bias or show deterioration of precision; the protection and retrievability of data (results); traceability and control of samples as they are processed through the laboratory; good communication of sample information between submitters, analysts, and supervision; and information on sample processing history. This guide describes such a system. Other accountability and quality control programs can be developed. Such programs can be equivalent to the program in this guide if they provide all of the benefits mentioned above.
SCOPE
1.1 This guide covers the essential aspects of an accountability and quality control program for a chemical analysis laboratory. The reasons for establishing and operating such a program are discussed.

SIGNIFICANCE AND USE
4.1 Method validation is a process of demonstrating that the method meets the required performance capabilities. International standards such as ISO/IEC 17025, certifying bodies, and regulatory agencies require evidence that analytical methods are capable of producing valid results. This applies to laboratories using published standard test methods, modified standard test methods, and in-house test methods.  
4.2 Although a collaborative study is part of this guide, this guide may be used by a single laboratory for method validation when a formal collaboration study is not practical. This guide may also be applied before a full collaboration study to predict the reliability of the method.  
4.3 The use of multiple validation techniques described in this guide increases confidence in the validity or application of the method.  
4.4 It is beyond the scope of this guide to describe fully the fundamental considerations in Section 5. For a more descriptive definition of these concepts, refer to the International Union of Pure and Applied Chemistry (IUPAC) technical report, “Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis,”5 the IUPAC Compendium of Analytical Nomenclature (Orange Book),6 and the Eurachem publication, The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics.7
SCOPE
1.1 This guide describes procedures for the validation of chemical and spectrochemical analytical methods of analysis that are used by a metals, ores, and related materials analysis laboratory.  
1.2 This guide may be applied to the validation of laboratory developed (in-house) methods, addition of analytes to an existing standard test method, variation or scope expansion of an existing standard method, or the use of new or different laboratory equipment.  
1.3 This guide may also be used to validate the implementation of standard test methods used routinely by laboratories of the mining, ore processing, and metals industry.

SIGNIFICANCE AND USE
4.1 This document provides guidance for the implementation of procedures for the preparation, testing, and documentation of an in-house reference material (hereafter called an iRM) to be used for a number of purposes, enumerated in the following document, associated with development, validation, and control of chemical and physical measurement processes.  
4.2 This guide is primarily concerned with characterization of the chemical compositions of metals, ores, and related materials. For all these materials, there is a continuing, strong demand for reference materials (RMs) that is difficult for metrology institutes and private certified reference material (CRM) developers to meet because CRM development requires substantial investments of time and money. The metals and mining industries consume RMs and create new product and by-product compositions at high rates. They use analytical methods that provide rapid and accurate determinations, and both quality assurance and quality control can be maintained using efficient procedures provided appropriate iRMs are available.  
4.3 The user of this guide must recognize that development of an iRM for any purpose carries with it the responsibility to design and execute the development process correctly, and to document the process thoroughly. In addition, the user of an iRM bears the responsibility for correct use of the iRM material within its design limitations.  
4.4 This guide contains discussions on material selection and sampling for RMs with some attention given to conversion to the final forms.  
4.5 The use of iRMs is appropriate for control chart procedures to demonstrate that chemical measurement processes are under statistical control. This function requires demonstration of sufficient homogeneity of a material, but it does not require assignment of chemical and physical property values with associated, exhaustively evaluated uncertainties.  
4.6 The use of iRMs is appropriate for calibration of test methods ...
SCOPE
1.1 This document provides guidance for the implementation of procedures for preparation of in-house reference materials for analytical testing of metals, ores, slags, and other materials encountered within the metals and mining industries.  
1.2 This guide is applicable to the production of reference materials only (usually for internal use) and does not apply to the production of certified reference materials (CRMs). Materials may include metals, alloys, minerals, geological materials, manufacturing intermediates, and byproducts. Samples may be in a number of physical forms including blocks, disks, rods, wires, chips, granules, powders, and liquids.  
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.

SIGNIFICANCE AND USE
5.1 The purpose of this practice is to evaluate the homogeneity of a lot of material selected as a candidate for development as a reference material or certified reference material, or for a L/B selected for some other purpose (see Appendix X1-Appendix X4 for examples).  
5.2 This practice is applicable to the testing of samples taken at various stages during production. For example, continuous cast materials, ingots, rolled bars, wire, etc., could be sampled at various stages during the production process and tested.
SCOPE
1.1 This practice is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical Principles. It is primarily intended for use in the development of reference materials but may be used in any other application where a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity of such a L/B.  
1.2 This practice is designed primarily to test for elemental homogeneity of a metal L/B by Spark-AES. However, it can be adapted for use with other instrumental techniques such as X-ray fluorescence spectrometry (XRF) or atomic absorption spectrometry (AAS).Note 1—This practice is not limited to elemental analysis or techniques. This practice can be applied to any property that can be measured, for example, the property of hardness as measured by the Rockwell technique.  
1.3 The criteria for acceptance of the test specimens must be previously determined. That is, the maximum acceptable level of heterogeneity must be determined on the basis of the intended use of the L/B.  
1.4 It is assumed that the analyst is trained in Spark-AES techniques including the specimen preparation procedures needed to make specimens ready for measurements. It is further assumed that the analyst is versed in and has access to computer-based data capture and analysis. The methodology of this practice is best utilized in a computer based spreadsheet.  
1.5 This practice can be applied to one or more elements in a specimen provided the signal-to-background ratio is not a limiting factor.  
1.6 This practice includes methods to correct for systematic drift of the instrument with time. (Warning—If drift occurs, erroneous conclusions will be obtained from the data analysis.)  
1.7 This practice also includes methods to refine estimates of composition and uncertainty through the use of a type standard or multiple calibrants.  
1.8 It further provides a means of reducing a nonhomogeneous set to a homogeneous subset.  
1.9 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.

SIGNIFICANCE AND USE
5.1 Ideally, interlaboratory testing of a method is conducted by a randomly chosen group of laboratories that typifies the kind of laboratory that is likely to use the method. In actuality, this ideal is only approximated by the laboratories that are available and willing to undertake the test work. The coordinator of the program must ensure that every participating laboratory has appropriate facilities and personnel and performs the method exactly as written. If this goal is achieved, the statistics developed during the ILS will be adequate for determining if the method is capable of producing satisfactory precision in actual use. If the program includes certified reference materials, the test data also provide information concerning the accuracy of the method. The statistics provide a general guide to the expected performance of the method.
SCOPE
1.1 This practice covers procedures and statistics for an interlaboratory study (ILS) of the performance of an analytical method. The study provides statistical values which are useful in determining if a method is satisfactory for the purposes for which it was developed. These statistical values may be incorporated in the method's precision and bias section. This practice discusses the meaning of the statistics and what users of analytical methods may learn from them.  
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.

SIGNIFICANCE AND USE
Many competent analytical laboratories comply with accepted quality system requirements. When using standard test methods, their test results on the same sample should agree with those from other similar laboratories within the reproducibility estimates index (R) published in the standard. Reproducibility estimates are generated as part of the interlaboratory studies (ILS), of the type described in Practice E1601. Competent laboratories participate in proficiency tests, such as those conducted in accordance with Practice E2027, to confirm that they perform consistently over time. In both ILS and proficiency testing protocols, it is generally assumed that only one work station is used to generate the data.
Many laboratories have workloads, or logistical requirements, or both, that dictate the use of multiple work stations. Some have multiple stations in the same area (central laboratory format). Other stations are scattered throughout a facility (at-line laboratory format) and in some cases may even reside at different facilities. Often, analysis reports do not identify the workstation used for the testing, even if workstations differ in their testing uncertainties. Problems can arise if clients mistakenly attribute variation in report values to process rather than workstation variability. These problems can be minimized if the laboratory organization determines the overall uncertainty associated with results reported from multiple workstations and assesses the significance of the analytical uncertainty to the production process.
This guide describes a protocol for efficiently optimizing and controlling variability in test results from different workstations used to perform the same test. It harmonizes calibration and control protocols, thereby providing the same level of measurement traceability and control to all workstations. It streamlines documentation and training requirements, thereby facilitating flexibility in personnel assignments. Finally, it offers an...
SCOPE
1.1 This guide describes a protocol for optimizing, controlling, and reporting test method uncertainties from multiple workstations in the same laboratory organization. It does not apply when different test methods, dissimilar instruments, or different parts of the same laboratory organization function independently to validate or verify the accuracy of a specific analytical measurement.
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.

SIGNIFICANCE AND USE
Method validation is a process of demonstrating that the method meets the required performance capabilities. International standards such as ISO/IEC 17025, certifying bodies, and regulatory agencies require evidence that analytical methods are capable of producing valid results. This applies to laboratories using published standard test methods, modified standard test methods, and in-house test methods.  
Although a collaborative study is part of this guide, this guide may be used by a single laboratory for method validation when a formal collaboration study is not practical. This guide may also be applied before a full collaboration study to predict the reliability of the method.
The use of multiple validation techniques described in this guide increases confidence in the validity or application of the method.
It is beyond the scope of this guide to describe fully the fundamental considerations in Section 5. For a more descriptive definition of these concepts, refer to the International Union of Pure and Applied Chemistry (IUPAC) technical report, “Harmonized Guidelines for Single Laboratory Validation of Methods of Analysis,” the IUPAC Compendium of Analytical Nomenclature (Orange Book), and the Eurachem publication, The Fitness for Purpose of Analytical Methods, A Laboratory Guide to Method Validation and Related Topics.
SCOPE
1.1 This guide describes procedures for the validation of chemical and spectrochemical analytical methods of analysis that are used by a metals, ores, and related materials analysis laboratory.
1.2 This guide may be applied to the validation of laboratory developed (in-house) methods, addition of analytes to an existing standard test method, variation or scope expansion of an existing standard method, or the use of new or different laboratory equipment.
1.3 This guide may also be used to validate the implementation of standard test methods used routinely by laboratories of the mining, ore processing, and metals industry.

SIGNIFICANCE AND USE
A result must be stated to a sufficient number of digits so that a user receives both quantitative information and a measure of the variability of the value reported.
The range of application of most methods of chemical analysis is based upon the presumption that the quantitative results produced are to be used to compare the analyte content of the test material with specified limiting values. However, analytical results may be used legitimately for other purposes. If the same material is analyzed a number of times or a product is analyzed periodically during an interval of production, each set of results may be averaged to yield an average result having improved reliability, provided nothing has been done between analyses to modify the composition of the analyzed material. Results that fall below the lower limit, although not quantitative individually, contain compositional information and may be reported. The reporting system in this practice permits the analyst to indicate which values are likely to be rendered quantitative by averaging and which are not.
The system is simple enough to be used routinely in reporting results from standard methods and assists those untrained in statistics to apply results appropriately.
SCOPE
1.1 This practice covers the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provides selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.
1.2 Specifically excluded is consideration of report forms and the associated informational content of reports in which results are tabulated or transmitted. It is assumed that the reporting laboratory has established a report format to ensure proper identification of the materials tested, the nature and conditions of the test, the responsible personnel, and other related information in accordance with existing regulations and good laboratory practices.

SIGNIFICANCE AND USE
An accountability and quality control system is established by laboratory management to improve the quality of its results. It provides documented records which serve to assure users of the laboratory's services that a specified level of precision is achieved in the routine performance of its measurements and that the data reported were obtained from the samples submitted. The system also provides for: early warning to analysts when methods or equipment begin to develop a bias or show deterioration of precision; the protection and retrievability of data (results); traceability and control of samples as they are processed through the laboratory; good communication of sample information between submitters, analysts, and supervision; and information on sample processing history. This guide describes such a system. Other accountability and quality control programs can be developed. Such programs can be equivalent to the program in this guide if they provide all of the benefits mentioned above.
SCOPE
1.1 This guide covers the essential aspects of an accountability and quality control program for a chemical analysis laboratory. The reasons for establishing and operating such a program are discussed.

SIGNIFICANCE AND USE
Ideally, interlaboratory testing of a method is conducted by a randomly chosen group of laboratories that typifies the kind of laboratory that is likely to use the method. In actuality, this ideal is only approximated by the laboratories that are available and willing to undertake the test work. The coordinator of the program must ensure that every participating laboratory has appropriate facilities and personnel and performs the method exactly as written. If this goal is achieved, the statistics developed during the ILS will be adequate for determining if the method is capable of producing satisfactory precision in actual use. If the program includes certified reference materials, the test data also provide information concerning the accuracy of the method. The statistics provide a general guide to the expected performance of the method.
SCOPE
1.1 This practice covers procedures and statistics for an interlaboratory study (ILS) of the performance of an analytical method. The study provides statistical values which are useful in determining if a method is satisfactory for the purposes for which it was developed. These statistical values may be incorporated in the method's precision and bias section. This practice discusses the meaning of the statistics and what users of analytical methods may learn from them.
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.

SIGNIFICANCE AND USE
This practice sets the basic requirements for proficiency test programs in the chemical analysis of metals, ores, and related materials. It does not set specific procedural requirements, but does establish a framework for particular programs, including those with either small or large numbers of participants. (Warning—The data from proficiency testing programs must never be used to assign certification values to the materials used in the program. The elements of a properly conceived and implemented certification program are described in detail in Guide E1724.)
Most accreditation bodies require that laboratories participate regularly in proficiency testing programs that they have accepted for the purpose. Therefore, it is essential that each program comply with accepted principles including technical requirements, statistical procedures (see Annex A1), and quality management (see Annex A2).
SCOPE
1.1 This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO Guide 43 and Guide E1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.

SIGNIFICANCE AND USE
The purpose of this practice is to evaluate the homogeneity of a lot of material selected as a candidate for development as a reference material or certified reference material, or for a L/B selected for some other purpose (see Appendix X1-Appendix X4 for examples).
This practice is applicable to the testing of samples taken at various stages during production. For example, continuous cast materials, ingots, rolled bars, wire, etc., could be sampled at various stages during the production process and tested.
SCOPE
1.1 This practice is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical Principles. It is primarily intended for use in the development of reference materials but may be used in any other application where a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity of such a L/B.
1.2 This practice is designed primarily to test for elemental homogeneity of a metal L/B by Spark-AES. However, it can be adapted for use with other instrumental techniques such as X-ray fluorescence spectrometry (XRF) or atomic absorption spectrometry (AAS).
Note 1—This practice is not limited to elemental analysis or techniques. This practice can be applied to any property that can be measured, for example, the property of hardness as measured by the Rockwell technique.
1.3 The criteria for acceptance of the test specimens must be previously determined. That is, the maximum acceptable level of heterogeneity must be determined on the basis of the intended use of the L/B.
1.4 It is assumed that the analyst is trained in Spark-AES techniques including the specimen preparation procedures needed to make specimens ready for measurements. It is further assumed that the analyst is versed in and has access to computer-based data capture and analysis. The methodology of this practice is best utilized in a computer based spreadsheet.
1.5 This practice can be applied to one or more elements in a specimen provided the signal-to-background ratio is not a limiting factor.
1.6 This practice includes methods to correct for systematic drift of the instrument with time. (Warning—If drift occurs, erroneous conclusions will be obtained from the data analysis.)
1.7 This practice also includes methods to refine estimates of composition and uncertainty through the use of a type standard or multiple calibrants.
1.8 It further provides a means of reducing a nonhomogeneous set to a homogeneous subset.
1.9 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.

SCOPE
1.1 This practice is suitable for testing the homogeneity of metals, either in solid or powdered form, and finely ground oxide materials that are intended for use as reference materials in X-ray emission, or optical emission spectroscopy, or both. The criteria for acceptance of the test specimens as reference materials, however, must be previously determined by the user for meeting his specific requirements.  
1.2 The procedure is designed primarily for testing specimens by X-ray emission spectrometry or optical emission spectroscopy, or both. However, the practice could be easily adapted for use with other instrumental techniques such as atomic absorption spectrophotometry.  
1.3 This procedure can be applied to one or more elements in a specimen provided the signal-to-background ratio is not a limiting factor.  
1.4 This practice includes one method, if desired, to correct for systematic or periodic (sinusoidal) drift in the instrument with time through the use of a control reference material.  Note 1-Caution: If serious drift occurs (for example, unstable power supply, X-ray tube, etc.) erroneous conclusions may be obtained from the data analysis.
1.5 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 is suitable for testing the homogeneity of metals, either in solid or powdered form, and finely ground oxide materials that are intended for use as reference materials in X-ray emission, or optical emission spectroscopy, or both. The criteria for acceptance of the test specimens as reference materials, however, must be previously determined by the user for meeting his specific requirements.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in May 2005 in accordance with section 10.5.3.1 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.

SCOPE
1.1 This guide describes a protocol for optimizing, controlling, and reporting test method uncertainties from multiple workstations in the same laboratory organization. It does not apply when different test methods, dissimilar instruments, or different parts of the same laboratory organization function independently to validate or verify the accuracy of a specific analytical measurement.
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.

SIGNIFICANCE AND USE
This practice sets the basic requirements for proficiency test programs in the chemical analysis of metals, ores, and related materials. It does not set specific procedural requirements, but does establish a framework for particular programs, including those with either small or large numbers of participants.
4.1.1 WARNING: The data from proficiency testing programs must never be used to assign certification values to the materials used in the program. The elements of a properly conceived and implemented certification program are described in detail in Guide E 1724.
Most accreditation bodies require that laboratories participate regularly in proficiency testing programs that they have accepted for the purpose. Therefore, it is essential that each program comply with accepted principles including technical requirements, statistical procedures (see Annex A1), and quality management (see Annex A2).
SCOPE
1.1 This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO/IEC Guide 43 and Guide E 1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.

SIGNIFICANCE AND USE
Consistency in analysis depends on being aware of a significant change in instrumental response, such as that caused by drift or changes in analytical precision, or both, and taking corrective action. The usual corrective action for drift is standardization. Standardization, however, when there is no real need, can only broaden the spread of subsequent analyses. One purpose of this practice is to set guidelines that will avoid “ overstandardization.”
To control manufacturing processes, there must be confidence that a consistent material is being produced and that the analysis of the material is reliable. For assurance that the material meets specification, a purchaser may require the supporting record of control charts to assess that proper analytical control has been maintained.
Ideally, variations in analytical results may be held to chance causes. The concept of a confidence interval or limits on a control chart is based on what can be expected when all normal precautions are exercised. When results appear to go out of control, the analyst should consider and correct what might be an assignable cause. As experience is accumulated, however, it may not seem unusual for readings to drift with time as optics degrade, detector response changes, or excitations modify as, for example, when deposits build up on a counter electrode (a correctable assignable cause), or the longer range effects as an X-ray tube deteriorates.
SCOPE
1.1 This practice covers procedures for determining if a spectrochemical analysis is under statistical control.
1.2 Criteria are presented for determining when corrective action is required.
1.3 Control will be effected by using verifiers to test instrument response. It is recommended, although not required, that this be accompanied by the plotting of control charts.
1.4 The preparation of control charts is described.
1.5 Limitations—The procedures that are described do not apply to analyses that require a calibration each time a set of analyses is run. Reference is made specifically to optical emission spectroscopy, but the practice has a more general application.
1.6 This practice does not apply to validation procedures that monitor the correctness of calibration.

SCOPE
1.1 This document covers terms and concepts used in developing and evaluating the performance of methods for determining chemical composition. Although useful with many types of methods, they are dealt with in this document in the context of chemical analysis of metals and related materials.

SIGNIFICANCE AND USE
An accountability and quality control system is established by laboratory management to improve the quality of its results. It provides documented records which serve to assure users of the laboratory’services that a specified level of precision is achieved in the routine performance of its measurements and that the data reported were obtained from the samples submitted. The system also provides for: early warning to analysts when methods or equipment begin to develop a bias or show deterioration of precision; the protection and retrievability of data (results); traceability and control of samples as they are processed through the laboratory; good communication of sample information between submitters, analysts, and supervision; and information on sample processing history. This guide describes such a system. Other accountability and quality control programs can be developed. Such programs can be equivalent to the program in this guide if they provide all of the benefits mentioned above.
SCOPE
1.1 This guide covers the essential aspects of an accountability and quality control program for a chemical analysis laboratory. The reasons for establishing and operating such a program are discussed.

SIGNIFICANCE AND USE
A result should be stated to a sufficient number of digits so that a user receives both quantitative information and a measure of the variability of the value reported.
The range of application of most methods of chemical analysis is based upon the presumption that the quantitative results produced are to be used to compare the analyte content of the test material with specified limiting values. However, analytical results may be used legitimately for other purposes. If the same material is analyzed a number of times or a product is analyzed periodically during an interval of production, each set of results may be averaged to yield an average result having improved reliability. Results that fall below the lower limit, although not quantitative individually, contain compositional information and shall be reported. The reporting system in this practice permits the analyst to indicate which values are likely to be rendered quantitative by averaging and which are not.
The system is simple enough to be used routinely in reporting results from standard methods and assists those untrained in statistics to apply results appropriately.
SCOPE
1.1 This practice covers the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provides selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.
1.2 Specifically excluded is consideration of report forms and the associated informational content of reports in which results are tabulated or transmitted. It is assumed that the reporting laboratory has established a report format to ensure proper identification of the materials tested, the nature and conditions of the test, the responsible personnel, and other related information in accordance with existing regulations and good laboratory practices.

SCOPE
1.1 This guide covers procedures to help a task group interpret interlaboratory study (ILS) statistics to state precision and accuracy of a test method and make judgments concerning its range of use.
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.

SIGNIFICANCE AND USE
Ideally, interlaboratory testing of a method is carried out by a randomly chosen group of laboratories that typifies the kind of laboratory that is likely to use the method. In actuality, this ideal is only approximated by the laboratories that are available and willing to undertake the test work. The coordinator of the program must ensure that every participating laboratory has appropriate facilities and personnel and performs the method exactly as written. If this goal is achieved, the statistics developed during the ILS will be adequate for determining if the method is capable of producing satisfactory precision in actual use. If the program includes certified reference materials, the test data also provide information concerning the accuracy of the method. The statistics provide a general guide to the expected performance of the method in the laboratories of those who will use it.
SCOPE
1.1 This practice presents procedures and statistics for an interlaboratory study (ILS) of the performance of an analytical method. The study provides statistical values which are useful in determining if a method is satisfactory for the purposes for which it was developed. These statistical values may be incorporated in the method's precision and bias section. This practice discusses the meaning of the statistics and what users of analytical methods may learn from them.
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.

SCOPE
1.1 This guide sets the minimum requirements which an analytical chemistry laboratory should meet to be recognized as competent to carry out specific analytical procedures.  
1.2 Additional requirements and information which have to be disclosed for assessing competence or for determining compliance with other criteria may be specified by the organization or authority granting the accreditation, depending upon the specific character of the task of the laboratory.  
1.3 This standard does not purport to address all of the safety problems, 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.

SCOPE
1.1 This practice covers procedures for determining if a spectrochemical analysis is under statistical control.
1.2 Criteria are presented for determining when corrective action is required.
1.3 Control will be effected by using verifiers to test instrument response. It is recommended, although not required, that this be accompanied by the plotting of control charts.
1.4 The preparation of control charts is described.
1.5 Limitations---The procedures which are described do not apply to analyses which requires a calibration each time a set of analyses is run. Reference is made specifically to optical emission spectroscopy, but the practice has a more general application.
1.6 This practice does not apply to validation procedures that monitor the correctness of calibration.

SCOPE
1.1 This guide describes a protocol for optimizing, controlling, and reporting test method uncertainties from multiple workstations in the same laboratory organization. It does not apply when different test methods, dissimilar instruments, or different parts of the same laboratory organization function independently to validate or verify the accuracy of a specific analytical measurement.
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.

SCOPE
1.1 This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO/IEC Guide 43 and Guide E 1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.

SCOPE
1.1 This guide covers procedures to help a task group interpret interlaboratory study (ILS) statistics to state precision and accuracy of a test method and make judgments concerning its range of use.  
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.

SCOPE
1.1 This practice presents procedures and statistics for an interlaboratory study (ILS) of the performance of an analytical method. The study provides statistical values which are useful in determining if a method is satisfactory for the purposes for which it was developed. These statistical values may be incorporated in the method's precision and bias section. This practice discusses the meaning of the statistics and what users of analytical methods may learn from them.
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.

SCOPE
1.1 This practice covers the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provides selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.

SCOPE
1.1 This guide describes the essential aspects of an accountability and quality control program for a chemical analysis laboratory. The reasons for establishing and operating such a program are discussed.

SCOPE
1.1 This document covers terms and concepts used in developing and evaluating the performance of methods for determining chemical composition. Although useful with many types of methods, they are dealt with in this document in the context of chemical analysis of metals and related materials.

SIGNIFICANCE AND USE
4.1 A result must be stated to a sufficient number of digits so that a user receives both quantitative information and a measure of the variability of the value reported.  
4.2 The range of application of most methods of chemical analysis is based upon the presumption that the quantitative results produced are to be used to compare the analyte content of the test material with specified limiting values. However, analytical results may be used legitimately for other purposes. If the same material is analyzed a number of times or a product is analyzed periodically during an interval of production, each set of results may be averaged to yield an average result having improved reliability, provided nothing has been done between analyses to modify the composition of the analyzed material. Results that fall below the lower limit, although not quantitative individually, contain compositional information and may be reported. The reporting system in this practice permits the analyst to indicate which values are likely to be rendered quantitative by averaging and which are not.  
4.3 The system is simple enough to be used routinely in reporting results from standard methods and assists those untrained in statistics to apply results appropriately.
SCOPE
1.1 This practice covers the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provides selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.  
1.2 Specifically excluded is consideration of report forms and the associated informational content of reports in which results are tabulated or transmitted. It is assumed that the reporting laboratory has established a report format to ensure proper identification of the materials tested, the nature and conditions of the test, the responsible personnel, and other related information in accordance with existing regulations and good laboratory practices.  
1.3 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.
WITHDRAWN RATIONALE
This practice covered the approximate number of digits required to express the expected precision of results reported from standard methods of chemical analysis. This practice provided selection criteria and proper form and symbols for coding results when necessary to indicate the relative reliability of results having small values.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in November 2023. This standard is being withdrawn without replacement due to it now being obsolete.

SIGNIFICANCE AND USE
5.1 The purpose of this practice is to evaluate the homogeneity of a lot of material selected as a candidate for development as a reference material or certified reference material, or for a L/B selected for some other purpose (see Appendix X1 – Appendix X4 for examples).  
5.2 This practice is applicable to the testing of samples taken at various stages during production. For example, continuous cast materials, ingots, rolled bars, wire, etc., could be sampled at various stages during the production process and tested.
SCOPE
1.1 This practice is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical Principles. It is primarily intended for use in the development of reference materials but may be used in any other application where a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity of such a L/B.  
1.2 This practice is designed primarily to test for elemental homogeneity of a metal L/B by Spark-AES. However, it can be adapted for use with other instrumental techniques such as X-ray fluorescence spectrometry (XRF) or atomic absorption spectrometry (AAS).Note 1—This practice is not limited to elemental analysis or techniques. This practice can be applied to any property that can be measured, for example, the property of hardness as measured by the Rockwell technique.  
1.3 The criteria for acceptance of the test specimens must be previously determined. That is, the maximum acceptable level of heterogeneity must be determined on the basis of the intended use of the L/B.  
1.4 It is assumed that the analyst is trained in Spark-AES techniques including the specimen preparation procedures needed to make specimens ready for measurements. It is further assumed that the analyst is versed in and has access to computer-based data capture and analysis. The methodology of this practice is best utilized in a computer based spreadsheet.  
1.5 This practice can be applied to one or more elements in a specimen provided the signal-to-background ratio is not a limiting factor.  
1.6 This practice includes methods to correct for systematic drift of the instrument with time. (Warning—If drift occurs, erroneous conclusions will be obtained from the data analysis.)  
1.7 This practice also includes methods to refine estimates of composition and uncertainty through the use of a type standard or multiple calibrants.  
1.8 It further provides a means of reducing a nonhomogeneous set to a homogeneous subset.  
1.9 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 is suitable for testing the homogeneity of a metal lot or batch (L/B) in solid form by spark atomic emission spectrometry (Spark-AES). It is compliant with ISO Guide 35—Certification of Reference Materials: General and Statistical Principles. It is primarily intended for use in the development of reference materials but may be used in any other application where a L/B is to be tested for homogeneity. It is designed to provide a combined study of within-unit and between-unit homogeneity of such a L/B.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in January 2023 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.

SIGNIFICANCE AND USE
4.1 This practice sets the basic requirements for proficiency test programs in the chemical analysis of metals, ores, and related materials. It does not set specific procedural requirements, but does establish a framework for particular programs, including those with either small or large numbers of participants.  
4.2 The data from proficiency testing programs can be used for value assignments for in-house reference materials developed in accordance with Guide E2972.  
4.3 Most accreditation bodies require that laboratories participate regularly in proficiency testing programs that they have accepted for this purpose. Therefore, it is essential that each program comply with accepted principles including technical requirements, statistical procedures (see Annex A1), and quality management (see Annex A2).
SCOPE
1.1 This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO/IEC 17043 and Guide E1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.  
1.2 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.
WITHDRAWN RATIONALE
This practice provides direction for organizing and conducting proficiency test programs in analytical chemistry for metals, ores, and related materials. It is consistent with ISO/IEC 17043 and Guide E1301. It does not address the selection and use of proficiency testing schemes by accrediting bodies.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in November 2022. This standard is being withdrawn without replacement due to its limited use by industry.

SIGNIFICANCE AND USE
Consistency in analysis depends on being aware of a significant change in instrumental response, such as that caused by drift or changes in analytical precision, or both, and taking corrective action. The usual corrective action for drift is standardization. Standardization, however, when there is no real need, can only broaden the spread of subsequent analyses. One purpose of this practice is to set guidelines that will avoid “unnecessary standardization.”
To control manufacturing processes, there must be confidence that a consistent material is being produced and that the analysis of the material is reliable. For assurance that the material meets specification, a purchaser may require the supporting record of control charts to assess that proper analytical control has been maintained.
Ideally, variations in analytical results may be held to chance causes. The concept of a confidence interval or limits on a control chart is based on what can be expected when all normal precautions are exercised. When results appear to go out of control, the analyst should consider and correct what might be an assignable cause. As experience is accumulated, however, it may not seem unusual for readings to drift with time as optics degrade, detector response changes, or excitations conditions change, for example, when deposits build up on a counter electrode (a correctable assignable cause), or the longer range effects as an X-ray tube deteriorates.
SCOPE
1.1 This practice covers procedures for determining if a spectrochemical analysis is under statistical control.
1.2 Criteria are presented for determining when corrective action is required.  
1.3 Control will be effected by using verifiers to test instrument response. It is recommended, although not required, that this be accompanied by the plotting of control charts.
1.4 The preparation of control charts is described.
1.5 Limitations—The procedures that are described do not apply to analyses that require a calibration each time a set of analyses is run. Reference is made specifically to atomic emission spectrometry, but the practice has a more general application.
1.6 This practice does not apply to validation procedures that monitor the correctness of calibration.
WITHDRAWN RATIONALE
This practice covered procedures for determining if a spectrochemical analysis is under statistical control.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in January 2019 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.

ABSTRACT
This practice covers the use of terms and concepts relating to the development and evaluation of method performance in determining the chemical composition of metals and related materials. Analytical science deals with the development and use of methods for chemical composition determination of materials. Chemical analysis is the application of written analytical methods. Analytical method development consists of selecting chemical and physical systems that respond to a specific analyte in a defined suite of material types which shall have the following desirable properties: accuracy and precision. Statistics deals with the collection, analysis, interpretation, and presentation of numerical data sets. Statistical terms include: arithmetic average or mean; standard deviation; precision; B-value; total error which is the statistical sum of random and systematic errors; detection limit; interlaboratory study which is a statistically designed demonstration of the actual performance of an analytical method; analysis of variance; and repeatability and reproducibility indices.
SCOPE
1.1 This document covers terms and concepts used in developing and evaluating the performance of methods for determining chemical composition. Although useful with many types of methods, they are dealt with in this document in the context of chemical analysis of metals and related materials.
WITHDRAWN RATIONALE
This document covered terms and concepts used in developing and evaluating the performance of methods for determining chemical composition.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this practice was withdrawn in January 2016 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.

SIGNIFICANCE AND USE
A written test method is subjected to an ILS to evaluate its performance. The ILS produces a set of statistical estimates that depend upon the method, but also are influenced by the laboratories and test materials involved in the study. For that reason, the ILS task group must interpret these estimates, aided by this guide and using analytical judgment, to decide if the method is suitable to be balloted for publication as a standard. The task group may use this guide to help them prepare the precision and bias statements that are a required part of the method.
SCOPE
1.1 This guide covers procedures to help a task group interpret interlaboratory study (ILS) statistics to state precision and accuracy of a test method and make judgments concerning its range of use.
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 guide covered procedures to help a task group interpret interlaboratory study (ILS) statistics to state precision and accuracy of a test method and make judgments concerning its range of use.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this guide was withdrawn in January 2015 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.

SCOPE
1.1 This practice describes a model for use by analytical chemistry laboratories in implementing standard performance-based test methods, such as those developed in accordance with Practice E 2437.
1.2 The principles in these practices can also be used by ISO 17025 compliant laboratories that need to implement other performance-based test methods or need to document and validate extensions of standard test methods, or non-standard test methods.
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.
WITHDRAWN RATIONALE
This practice described a model for use by analytical chemistry laboratories in implementing standard performance-based test methods.
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.

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.

SIGNIFICANCE AND USE
This guide describes the suggested procedures for the preparation, testing, and certification of reference materials (RMs) to be used in the calibration, verification, and control of methods used to characterize the chemical composition of metals, ores, and related materials.
Certified reference materials are frequently rare and valuable commodities requiring investment of considerable cost and production time. They are frequently available for only a limited portion of a user’ range of interest.
When comparative analytical methods are employed, appropriate CRMs are often unavailable for calibration. In this case, the use of RMs is indicated as the alternative choice.
The use of uncertified homogeneous materials is appropriate for control chart programs where relative data consistency is being monitored. The use of CRMs for such purposes is often a misuse of valuable CRM stocks, especially when uncertified materials of suitable homogeneity are available. For information on the use and misuse of CRMs, see ISO Guide 33 and NBS Special Publication 260-100.5  
Use CRMs and RMs with caution in the validation of analytical methods. The danger involves a potential for undetected systematic error, since the same methodology being validated may have been used to establish the values for the CRMs or RMs. For more information on the use of CRMs in the validation of analytical methods, see NIST Special Publication 829.6
SCOPE
1.1 This guide describes procedures to be considered for the testing and certification of metal, ore, and metal-related reference materials in the form of blocks, disks, rods, wires, chips, and powders.
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 guide describes procedures to be considered for the testing and certification of metal, ore, and metal-related reference materials in the form of blocks, disks, rods, wires, chips, and powders.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this guide was withdrawn in February 2010 in accordance with section 10.5.3.1 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.

SCOPE
1.1 This practice describes a model for establishing ISO 17025-compliant uncertainty budgets for the chemical analysis of metals, ores, and related materials. It is based on applying the Horwitz function to widely accepted, diverse interlaboratory test programs, such as interlaboratory testing of standard test methods and proficiency testing programs. This function expresses the interlaboratory standard deviations that can be expected for any concentration level as competent laboratories use optimized test procedures to analyze any matrix for any analyte. It may be used to set aim uncertainties against which to plan new standard test methods and to assess the performance of existing test methods.
1.2 An optimized test procedure is one in which the final test results are at least equivalent to alternative, state-of-the-art procedures. In the analytical chemistry community, this means that calibrations are carried out, verified, and controlled such that the final test results have no systematic, detectable bias. The elimination of sources of bias is a key responsibility of any person who designs analytical test methods. Hence, an analytical test method that contains systematic, measurable sources of bias would probably not be accepted as an ASTM test method and its performance data would probably not be in compliance with the procedures described in this practice.
1.3 The uncertainty budget model described in this practice is based on the assumption that, in a normally distributed, bias-free environment, measurement uncertainty will improve by the square root of two with each removal of a significant source of variation. Conversely, it is assumed that measurement uncertainty will worsen by the same amount with each addition of a significant source of variation. Furthermore, this model assumes that the hierarchy of increasing variation in any composition-based measurement system begins with calibration and progresses through control to intralaboratory standard deviation to interlaboratory standard deviation to product sampling for conformity assessment. Therefore, aim values for the expected uncertainties at any process step can be predicted using this model.
1.4 When using this model, the aim values generated using this model must then be validated, verified, and documented as part of the development and interlaboratory testing of any new test method, sampling practice, and product specification, as appropriate. It is also expected that each laboratory that elects to use that standard test method will generate data to show that the standard test method complies with the published uncertainties developed during interlaboratory testing of the standard test method. The principles in this practice can also be applied to the development of test methods used to determine the composition of other materials.
1.5 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 describes a model for establishing ISO 17025-compliant uncertainty budgets for the chemical analysis of metals, ores, and related materials. It is based on applying the Horwitz function to widely accepted, diverse interlaboratory test programs, such as interlaboratory testing of standard test methods and proficiency testing programs. This function expresses the interlaboratory standard deviations that can be expected for any concentration level as competent laboratories use optimized test procedures to analyze any matrix for any analyte. It may be used to set aim uncertainties against which to plan new standard test methods and to assess the performance of existing test methods.
Formerly under the jurisdiction of Committee E 01 on Analytical Chemistry for Metals, Ores, and Related Materials, t...

SCOPE
1.1 This guide sets the minimum requirements which an analytical chemistry laboratory should meet to be recognized as competent to carry out specific analytical procedures.  
1.2 Additional requirements and information which have to be disclosed for assessing competence or for determining compliance with other criteria may be specified by the organization or authority granting the accreditation, depending upon the specific character of the task of the laboratory.  
1.3 This standard does not purport to address all of the safety problems, 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 guide sets the minimum requirements which an analytical chemistry laboratory should meet to be recognized as competent to carry out specific analytical procedures.
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry of Metals, Ores, and Related Materials, this guide was withdrawn in August 2007.