仪器确认 附件5 自动滴定仪确认 中英文

PA/PH/OMCL (07) 108 4R - OMCL Guideline on automatic titrators (Annex 5) OMCL Network of the Council of Europe QUALITY MANAGEMENT DOCUMENT质量管理文件PA/PH/OMCL (07) 108 4RQUALIFICATION OF EQUIPMENT仪器的确认ANNEX 5: QUALIFICATION OF AUTOMATIC TITRATORSANNEX 5 OF THE OMCL NETWORK GUIDELINE“QUALIFICATION OF EQUIPMENT”OMCL网络指南“仪器确认”附件5QUALIFICATION OF AUTOMATIC TITRATORS自动滴定仪的确认Introduction 介绍The present document is the 5th Annex of the core do cument “Qualification of Equipment”, and it should be used in combination with it when planning, performing and documenting the qualification process of automatic titrators.本文件为核心文件“仪器的确认”的第5个附件，在对计划、实施和记录自动滴定仪的确认过程中，应将本文件与核心文件一起使用。

The core document contains the Introduction and general forms for Level I and II of qualification, which are common to all type of instruments.核心文件包括第一级和第二级确认的介绍和通用表格，适用于所有类型的仪器。

It is recommended, at Level II of qualification of the automatic titrators (Installation and release for use), to perform a gravimetric test of the volumes (10 selected volumes in a random way from 20 to 100% of the cylinder volume).建议在自动滴定仪的第二级确认中（安装和使用放行），对体积进行重量检测（滴定管20%-100%体积随机选择10个）。

The present annex contains instrument-related recommendations on parameters to be checked at Level III and IV of qualification and the corresponding typical acceptance limits, as well as practical examples on the methodology that can be used to carry out these checks.所附文件包括与仪器相关的推荐，在第三级和第四级确认应检查何各参数，以及典型的可接受标准，还有可以用于实施这些检查的实践举例。

TABLE 表III Level III. Periodic and motivated instrument checks第三级周期性主动仪器检查Examples of requirements for automatic titrators自动滴定仪要求举例1. POTENTIOMETRIC TITRATORS 电位滴定仪(Ph. Eur. 欧洲药典2.2.20)2. KARL FISCHER VOLUMETRIC TITRATORS used for semi-micro determination of water卡尔费休容量法滴定仪，用于半微量水分测定(Karl Fischer Titration, Ph. Eur. 卡尔费休滴定，欧洲药典2.5.12)TABLE表III (cont.续) Level III. Periodic and motivated instrument checks第三级周期性仪器检查Examples of requirements for automatic titrators (cont.)自动滴定仪要求举例3. KARL FISCHER COULOMETRIC TITRATORS used for micro determination of water卡尔费休库仑滴定仪，用于微量水分测定(Coulometric Titration, Ph. Eur. 2.5.32)（库仑滴定法，欧洲药典2.5.32）4. KARL FISCHER OVEN used for micro determination of water using an evaporation technique (Coulometric Titration, Ph. Eur. 2.5.32)卡尔费休炉，用于蒸发技术测定微量水，（库仑滴定，欧洲药典2.5.32）TABLE IVLevel IV. In-use instrument checks第四层次在用仪器检查Examples of requirements for automatic titrators自动滴定仪要求举例1. POTENTIOMETRIC TITRATORS自动电位滴定仪2. KARL FISCHER VOLUMETRIC TITRATORS 卡尔费休容量法滴定仪3. KARL FISCHER COULOMETRIC TITRATORS 卡尔费休库仑法滴定仪ANNEX 附件ILevel III. Periodic and motivated instrument checks第三级周期性主动仪器检查This Annex contains practical examples of tests and their associated tolerance limits for several parameters related to the performance of automatic titrators.本附件包括了检查的实践性例子，及其相关的几个与自动滴定仪性能相关的参数的可接受标准。

These examples can be considered by the OMCLs as possible approaches to perform the Level III of the equipment qualification process: “Periodic and motivated instrument checks”.这些例子可以被OMCL认为是仪器第三级别确认“周期性主动仪器检查”的方法。

GENERAL CONSIDERATIONS 总体考虑—Due to the fact that a holistic approach has been taken, the verification of temperature probes and burettes is not included in this guideline, as the performance of these items is indirectly checked during the accuracy test.—由于采用了整合功能的确认方法，本指南未包括温度探头和滴定管的确认，因为在准确度检查中，上述两项已经间接地被检查了。

—If available, the internal start-up test function may be used each time the instrument is switched on.—如果可以的话，仪器内置开机检查功能在每次开机时可以使用。

—If several exchange units are used for different titrants, all units should be tested at Level III.—如果有几个滴定单元用于不同的滴定剂，所有单元在第III级均需要检测。

—The limits and specifications of this guideline have been set according to Metrohm documentation. For other manufacturers (e.g. Mettler-Toledo, Mitsubishi, etc) the specifications may slightly differ.—本指南的限度和标准根据万通相关文献进行设定。

对于其它生产商（例如梅特勒-托利多、三菱等），标准可能稍有不同。

1. POTENTIOMETRIC TITRATORS 电位滴定仪1.1. PRECISION 精密度Materials:材料Suitable certified standard RV (highly pure, dried), e.g. Benzoic acid RV or tris(hydroxymethyl)- aminomethane (TRIS).合适的标准品RV（高纯，干燥），例如苯甲酸RV或三(羟甲基)氨基甲烷（TRIS）Fresh titrant, appropriate to titrate the selected standard.费休滴定剂，适宜滴定选择的标准Method:方法Perform a minimum of 3 titrations with 3 independent additions of certified standard (in random order if using different weights), which should result in a consumption of approx. 20 % to 90 % of the burette volume.独立加入3次计量过的标准物质（如果重量不同的话，顺序可以随机），进行至少3次滴定，消耗的滴定剂的体积应控制在一管体积的20%-90%。