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Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water 水中D19委员会适用测试方法精度和偏差的标准实践
发布日期: 2006-08-15
1.1本规程建立了统一标准,用于估算和表示D19水委员会适用试验方法的精度和偏差。 1.2除1.3、1.4和1.5中的规定外,本实践要求任务组提出一种新的测试方法,以进行协作研究,从中可以制定精度声明(总体和单操作员标准偏差估计)和偏差。该实践为任务组在规划和进行精度和偏差的确定方面提供了一般指导。 1.3如果由于试验方法的性质或样品的不稳定性,全面协作研究在技术上不可行,则应进行最大可行的缩小协作研究,以提供估计整体和单个- 操作员标准偏差。 1.3.1可接受的缩小研究的例子是由小组委员会D19.24进行的关于微生物方法的局部研究,因为固有的样品不稳定性。这些研究涉及六名或六名以上完全独立的本地分析师,他们可以在约定的时间开始分析均匀样本。 1.3.2如果均匀样本在任何情况下都不可行,则单操作员精度声明将符合本规程的要求。只要可能,该声明应根据独立多个操作员生成的数据编制,每个操作员对独立样本(特定基质类型)进行重复分析,这些样本通常在规定的浓度范围内(见( 3. )). 1.3.3本规程不适用于涉及对特定成分和特性进行连续采样或连续测量的方法。 1.3.4本规程也不适用于明渠流量测量。 1.4当进行研究时,满足本实施规程版本要求的合作研究将继续被视为每个试验方法中所需精度和偏差声明的充分基础。如果该研究不满足当前协作研究的最低要求,则应在精度和偏差声明中包含一份列出该研究缺陷的声明和对本段的引用,作为免除当前要求的依据。 1.5本段涉及根据或不明确接受的特殊豁免。在D19委员会根据结果顾问和D19委员会执行小组委员会技术操作科的建议批准后,一份声明将满足ASTM的两项要求,该声明给出了无法达到本规程所有或特定点的令人信服的理由 () 以及本规程的相关要求。此外,D19委员会可通过主要委员会投票批准发布“初步”标准方法,期限不超过5年。初步标准必须至少包含单操作员精度和偏差声明,以及基于单操作员数据的质量控制部分。初步标准的发布取决于该标准的完整D 2777合作研究设计的批准。本段授权的精度和偏差声明应包括D19委员会批准的日期。 1.6原则上,本规程涵盖所有试验方法。 1.7在第12节中,本规程展示了以下示例性精度和偏差声明格式:( 1. )产生数值测量的试验方法( 2. )根据程序中规定的标准,产生成功或失败的非数值报告的试验方法,以及( 3. )规定使用另一种ASTM试验方法中的程序的试验方法,仅需进行微不足道的修改。 1.8所有研究,即使是那些不符合或项下某些要求的研究,在进行前(见第节)和完成后(见第节)均应获得结果顾问的批准。 1.9本规程满足规程D 5847的质量控制要求。 1.10本实践的目的是,任务组尽一切努力保留其循环研究中的所有数据。除非有确凿证据表明价值被排除,否则不应排除价值。结果顾问应与任务组密切合作,以实现这一目标。 ====意义和用途====== 遵循这一实践应产生精度和偏差声明,任何实验室都可以通过适当使用所研究的测试方法来实现。这些精度和偏差声明为测试方法质量控制部分使用的通用限值提供了基础。 该方法规定了测试方法适用的矩阵。协作测试在测试设计的限制范围内证实了编写。广泛测试只能使用代表性矩阵,因此结果不能暗示普遍适用性。 协作研究的基本假设是,测试的基质、测试的浓度和参与实验室是对书面测试方法的范围和适用性的代表性和公平评估。
1.1 This practice establishes uniform standards for estimating and expressing the precision and bias of applicable test methods for Committee D19 on Water. 1.2 Except as specified in 1.3, 1.4, and 1.5, this practice requires the task group proposing a new test method to carry out a collaborative study from which statements for precision (overall and single-operator standard-deviation estimates) and bias can be developed. This practice provides general guidance to task groups in planning and conducting such determinations of precision and bias. 1.3 If a full-scale collaborative study is not technically feasible, due to the nature of the test method or instability of samples, the largest feasible scaled-down collaborative study shall be conducted to provide the best possible limited basis for estimating the overall and single-operator standard deviations. 1.3.1 Examples of acceptable scaled-down studies are the local-area studies conducted by Subcommittee D19.24 on microbiological methods because of inherent sample instability. These studies involve six or more completely independent local-area analysts who can begin analysis of uniform samples at an agreed upon time. 1.3.2 If uniform samples are not feasible under any circumstances, a statement of single-operator precision will meet the requirements of this practice. Whenever possible, this statement should be developed from data generated by independent multiple operators, each doing replicate analyses on independent samples (of a specific matrix type), which generally fall within specified concentration ranges (see ( 3 )). 1.3.3 This practice is not applicable to methodology involving continuous sampling or continuous measurement, or both, of specific constituents and properties. 1.3.4 This practice is also not applicable to open-channel flow measurements. 1.4 A collaborative study that satisfied the requirements of the version of this practice in force when the study was conducted will continue to be considered an adequate basis for the precision-and-bias statement required in each test method. If the study does not satisfy the current minimum requirements for a collaborative study, a statement listing the study's deficiencies and a reference to this paragraph shall be included in the precision-and-bias statement as the basis for an exemption from the current requirements. 1.5 This paragraph relates to special exemptions not clearly acceptable under or. With the approval of Committee D19 on the recommendation of the Results Advisor and the Technical Operations Section of the Executive Subcommittee of Committee D19, a statement giving a compelling reason why compliance with all or specific points of this practice cannot be achieved will meet both ASTM requirements () and the related requirements of this practice. In addition, Committee D19, through a Main Committee ballot, may approve publication of a "Preliminary" Standard Method for a period not to exceed 5 years. Preliminary Standards must contain a minimum of a single-operator precision-and-bias statement and a Quality Control section based on the single operator data. Publication of a Preliminary Standard is conditional on the approval of a full D 2777 collaborative study design for the standard. Precision-and-bias statements authorized by this paragraph shall include the date of approval by Committee D19. 1.6 In principle, all test methods are covered by this practice. 1.7 In Section 12 this practice shows exemplary precision-and-bias-statement formats for: ( 1 ) test methods yielding a numerical measure, ( 2 ) test methods yielding a non-numerical report of success or failure based on criteria specified in the procedure, and ( 3 ) test methods specifying that procedures in another ASTM test method are to be used with only insignificant modifications. 1.8 All studies, even those exempt from some requirements under or, shall receive approval from the Results Advisor before being conducted (see Section ) and after completion (see Section ). 1.9 This practice satisfies the QC requirements of Practice D 5847. 1.10 It is the intent of this practice that task groups make every effort to retain all the data from their round-robin studies. Values should not be eliminated unless solid evidence exists for their exclusion. The Results Advisor should work closely with the task groups to effect this goal. ====== Significance And Use ====== Following this practice should result in precision-and-bias statements that can be achieved by any laboratory properly using the test method studied. These precision-and-bias statements provide the basis for generic limits for use in the Quality Control section of the test method. The method specifies the matrices for which the test method is appropriate. The collaborative test corroborates the write-up within the limitations of the test design. An extensive test can only use representative matrices so that universal applicability cannot be implied from the results. The fundamental assumption of the collaborative study is that the matrices tested, the concentrations tested, and the participating laboratories are a representative and fair evaluation of the scope and applicability of the test method as written.
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归口单位: D19.02
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