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自动滴定仪的确认指南
来源: | 作者:prodcc054 | 发布时间: 2017-08-17 | 1238 次浏览 | 分享到:
 

OMCL Network of the Council of Europe

QUALITY MANAGEMENT DOCUMENT

质量管理文件

PA/PH/OMCL (07) 108 4R

QUALIFICATION OF EQUIPMENT

仪器的确认

ANNEX 5: QUALIFICATION OF AUTOMATIC TITRATORS

附件5:自动滴定仪的确认

Full document title and reference

文件全名和参考文献

Qualification of Equipment 仪器的确认

Annex 5: Qualification of automatic titrators

附件5:自动滴定仪的确认

PA/PH/OMCL (07) 108 4R

Document type

文件类型

Guideline

指南

Legislative basis

立法基础

The previous version of this document was also accepted by EA as recommendation document to be used in the context of Quality Management System audits of OMCLs

Date of first adoption

首次采用日期

June 2008

Date of original entry into force 初版生效日期

August 2008

Date of entry into force of revised document

修订本生效日期

1st May 2012

Previous titles/other

References

曾用名/其它参考文献

This document replaces document PA/PH/OMCL (07) 108 3R

本文件替代文件PA/PH/OMCL (07) 108 3R

Custodian Organisation

管理机构

The present document was elaborated by the OMCL Network/

EDQM of the Council of Europe

Concerned Network

相关网络

GEON


ANNEX 5 OF THE OMCL NETWORK GUIDELINE

“QUALIFICATION OF EQUIPMENT”

OMCL网络指南“仪器确认”附件5

QUALIFICATION OF AUTOMATIC TITRATORS

自动滴定仪的确认

Introduction 介绍

The present document is the 5th Annex of the core document “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 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)

Parameter to be checked

要检查的参数

Typical tolerance limits

典型可接受限度

1.1. Precision 精密度

RSD ≤0.2%

1.2. Accuracy 准确度

drel  ≤ ±0.5 %

1.3. Linearity 线性

r2 ≥ 0.9990

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)

Parameter to be checked

需要检查的参数

Typical tolerance limits

典型可接受限度

2.1. Precision 精密度

RSD 1.0 %

2.2. Linearity (optional) 线性(可选项)

r2 ≥ 0.9990

2.3. Recovery (optional) 回收率(可选项)

97.5 % to 102.5 %


TABLE III (cont.)

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

Parameter to be checked

需检查的参数

Typical tolerance limits

典型可接受限度

3.1. Precision 精密度

Standard 标准1000μg/g H2O: RSD ≤2.0 %

Standard 标准100 μg/g H2O: RSD ≤5.0 %

3.2. Recovery 回收率

Standard 标准1000μg/g H2O: 97.5 % to 102.5 %

Standard 标准100μg/g H2O: 90.0 % to 110.0 %

3.3. Linearity (optional) 线性

r2 ≥ 0.990

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

Parameter to be checked

需要检查的参数

Typical tolerance limits

典型可接受限度

4.1. Temperature accuracy 温度准确性

±5.0

4.2. Temperature stability 温度稳定性

±0.5

4.3. Carrier gas flow rate 载气流速

±10 ml/min


TABLE IV

Level 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

Parameter to be checked

需要检查的参数

Typical tolerance limits

典型可接受标准

1.1. Precision精密度

RSD0.2 %

1.2. Accuracy准确度

drel≤±2 %

2. KARL FISCHER VOLUMETRIC TITRATORS 卡尔费休容量法滴定仪

Parameter to be checked

需要检查的参数

Typical tolerance limits

典型可接受标准

2.1. Precision 精密度

RSD 1.5%

2.2. Recovery 准确度

97.5 % to 102.5 %

3. KARL FISCHER COULOMETRIC TITRATORS 卡尔费休库仑法滴定仪

Parameter to be checked

需要检查的参数

Typical tolerance limits

典型可接受标准

3.1. Recovery回收率

Standard 标准1000 μg/g H2O: 97.5 % to 102.5 %

Standard 标准100 μg/g H2O: 90.0 % to 110.0 %


ANNEX 附件 I

Level 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%

Note: If necessary, for lower volume burettes, increase the molarity of the titrant (for example, from 0.1 to1.0M) to minimize the weighing error of the standard.

注:如有必要,对于小容量滴管,增加滴定剂的浓度(如从0.1增加到1.0M)以减少标准的称量误差。

Calculate the relative standard deviation of the titers obtained.

计算所得的滴定度的相对标准偏差(RSD)。

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

如果可以的话,该计算可以由仪器的内置统计功能计算得到。

Limits: RSD ≤ 0.2 %

限度:RSD ≤ 0.2 %


1.2. ACCURACY 准确度

Materials:材料

Refer to chapter 1.1. Precision.参照第1.1 精密度

The accuracy of the results obtained depends on the content of the certified standard guaranteed by its manufacturer.

所得结果的准确性依赖于标准物质供应商所保证的含量。

Calculation of the theoretical titer value as a function of temperature:

对滴定度受温度影响的计算

The theoretical titer value of the titrant solution at20is 1.000, with a reduction in the titer of 0.02 % per degree of temperature rise, according to the following formula:

滴定剂溶液在20℃时理论滴定度为1.000,根据以下公式进行计算,每升高一度,则滴定度会下降0.02%

Titertheoretical (at X) = 1.000 + 0.0002 (20 – x)

理论滴定度(在X度时) = 1.000 + 0.000220-X

Where:其中

x = mean of the initial and final temperature of the titrant solution (at the beginning and at the end of the measurement), in °C.

X = 滴定剂溶液起始和结束温度(在测量开始和结束时),

Note: The stated formula is only applicable for aqueous titrant solutions (see Application Bulletin No. 252, Metrohm). For example, the given reduction in the titer of Perchloric acid is 0.1% per degree of temperature rise.

注:所给定的公式只用于水相滴定溶液(见第252号应用公告,万通)。例如,高氯酸滴定液给定的温度膨胀系数为每升高一度,浓度降低0.1%

Method:方法

Perform a minimum of 3 titrations with 3 different weights of certified standard.

称量三份标准物质,进行至少三次滴定。

Note: Results from the precision test (see 1.1.) can be used.

注:可以采用精密度测试(见1.1)的数据。

Calculate the mean of the titers obtained.

计算滴定度的平均值。

Calculate the systematic deviation (drel) with the following formula:

用以下公式计算系统误差(drel

drel =

titer mean  titer theoretical

×100

titer theoretical

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

如果可以的话,该计算可以由仪器的内置统计功能计算得到。

Limits:限度

The systematic deviation (drel) should be maximum ≤±0.5 % (when using a freshly opened titrant container).

系统误差应≤±0.5 %(如果使用新开的滴定剂的话)

1.3. LINEARITY 线性

Materials:材料

Refer to chapter 1.1. Precision. 参见第1.1 精密度

Method: Linear regression volume/sample size

方法: 线性回归 体积/样品量

Calculate a linear regression of the titrant volume in ml (y-coordinate), versus the weight of the certified standard in g (x-coordinate) on a minimum of 5 weights.

以滴定体积(ml)为y轴,对标准品重量(g)为x轴计算线性回归方程式,至少需要五个重量数据。

Limits: r2 ≥ 0.9990.

限度:r2 ≥ 0.9990.

Note: In addition, using the same linearity data, systematic errors can be evaluated, as the y axis intercept of the linear regression Titrant volume in ml/Sample size in g (asys), and the slope of the linear regression Titer in M/Titrant volume in ml (bT/Vol).

注:另外,如果使用相同的线性数据,可以评估系统错误,因为y轴截距为滴定体积(ml/样品重量(g(asys),线性回归的斜率为滴定度(M/滴定体积(ml(bT/Vol)

Limits: 限度

asys < ±10 μl for 1 ml-burettes; asys <±50μl for 5, 10, 20 and 50 ml-burettes

1ml滴定管:asys < ±10 μl5102050ml滴定管:asys <±50μl

bT/Vol < ± 0.0010 ml-1

2. KARL FISCHER (KF) VOLUMETRIC TITRATORS 卡尔费休(KF)容量法滴定仪

GENERAL RECOMMENDATIONS FOR KF TITRATIONS 卡尔费休滴定常规推荐

     It is recommended to work with certified water standard solutions for water determination, with exactly known water contents, e.g. HYDRANAL®. Solid substances, such as disodium tartrate dihydrate, can also be used.

     推荐使用经过计量的水标准溶液来检测水含量,它们的水含量为准确已知,例如HYDRANAL®,也可以使用固体标准物质,例如酒石酸二钠二水合物。

     KF instruments should not be located in rooms that are subject to large variations of temperature, or close to refrigerators or radiators. A protection should be installed if they are located close to water baths or sinks, or in direct sunlight.

     卡尔费休仪器不应放置在温差较大的房间,或接近冰箱、有辐射源的地方。如果附近有水源、水池或直接光照,应加以保护。

2.1. PRECISION 精密度

Materials:材料

Certified water standard solution with a defined guaranteed water contents of 10 mg/g.

Karl Fischer reagents for volumetric water determination.

卡尔费休试剂:用于容量法测定水分

Note: The drying tube of the titration cell must be filled with fresh molecular sieve.

注:滴定单元需要干燥,充填新鲜分子筛。

Method:方法

Perform a minimum of 6 titrations with 6 independent additions of water standard solution (in random order if using different weights), which should result in a consumption of approx. 20 % to 90 % of the burette volume.

用至少6份独立的水标准溶液(如果重量不同的话顺序可以随机)进行至少六次滴定,控制消耗的滴定液体积为一管的20%90%

Calculate the relative standard deviation of the titers obtained.

计算所得滴定度的相对标准偏差(RSD)。

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

如果可以的话,该计算可以由仪器内置的统计功能直接计算得到。

Limits: RSD 1.0 %.

限度:RSD 1.0 %.

2.2. LINEARITY (optional) 线性(可选项)

Materials:材料

Refer to chapter 2.1. Precision.

参见第2.1章,精密度

Method: Linear regression volume/sample size

方法: 线性回归 体积/样品量

Calculate a linear regression of the titrant volume in ml (y-coordinate), versus the weight of the certified standard in g (x-coordinate) on a minimum of 5 weights.

以滴定体积(ml)为y轴,对标准品重量(g)为x轴计算线性回归方程式,至少需要五个重量数据。

Limits: r2 ≥ 0.9990.

限度:r2 ≥ 0.9990.

2.3. RECOVERY 回收率

Materials: 材料

Refer to chapter 2.1. Precision. 参见第2.1章, 精密度

Method: 方法

Perform a minimum of 3 injections with an accurately weighed amount of water standard and perform the titration. Calculate the mean percentage recovery (r) of water from the water standard, using the following formula:

用精密称量的水标准至少进3个样,滴定,用以下公式计算回收率的平均值。

Where:其中

r: percentage recovery. 百分比回收率

W1: amount of water added, in mg. 加入的水的重量mg

W2: amount of water found, in mg. 实测水的重量mg

Limits: 97.5 % to 102.5 %.

限度:97.5%102.5%

3. KARL FISCHER COULOMETRIC TITRATORS 卡尔费休库仑法滴定仪

3.1. PRECISION 精密度

Materials:材料

Certified standard solution (highly pure, stable) with exactly known water content: 1000 μg/g or 100 μg/g.

标准物质(高纯度,稳定),水含量已知为1000 μg/g100 μg/g

Karl Fischer reagents for coulometry.

用于库仑法的卡尔费休试剂

Method:方法

Perform a minimum of 6 determinations with 6 independent additions of water standard solution (in random order if using different weights), between 0.2 and2.0 gfor a water standard solution 1000 μg/g, and between 0.5 and5.0 gfor a water standard solution 100 μg/g.

用至少6份独立的水标准溶液(如果重量不同的话顺序可以随机)进行至少六次滴定,水标准溶液1000μg/g称样量0.2-2.0g,水标准1000μg/g称样量为0.5-5.0g

Calculate the relative standard deviation of the water contents found (in μg/g).

计算实测水含量(μg/g)相对标准偏差。

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

可以采用仪器内置的统计功能进行该项计算。

Limits: 限度

Water standard solution 1000μg/g: RSD2.0 %.

水标准溶液1000μg/g: RSD2.0 %.

Water standard solution 100μg/g: RSD5.0 %.

水标准溶液100μg/g: RSD5.0 %.

3.2. RECOVERY 回收率

The determination of the recovery is based upon the water content of the standard guaranteed by the manufacturer.

回收率的计算基于水标准供应商所申明的水含量。

Materials:材料

Refer to chapter 3.1. Precision. 参见第3.1 精密度

Method: 方法

Perform a minimum of 3 injections with an accurately weighed amount of water standard and perform the coulometric titration. Calculate the mean percentage recovery (r) of water from the water standard, using the following formula:

取水标准精密称定,进校至少3次,作库仑法滴定,用以下公式计算水标准的回收率的平均值。

r = 100 W2/W1

Where: 其中

r: percentage recovery. 百分比回收率

W1: amount of water added, in mg. 加入水的数量mg

W2: amount of water found, in mg. 实测得水的数量mg

Limits:限度

Water standard solution 1000 μg/g - Recovery: 97.5 % to 102.5 %.

水标准溶液1000 μg/g – 回收率: 97.5 % to 102.5 %

Water standard solution 100 μg/g - Recovery: 90.0 % to 110.0 %.

水标准溶液100 μg/g – 回收率: 90.0 % to 110.0 %

3.3. LINEARITY (optional) 线性 (可选项)

Materials:材料

Refer to chapter 3.1. Precision.参见第3.1章,精密度

Method:方法

Calculate the regression line of the amount of water found in μg (y-coordinate), versus the sample size in g (x-coordinate).

以实测水含量(μg)为y轴,对样品重量(g)为x轴计算线性回归系数。

Limits: 0.990

限度: 0.990

4. KARL FISCHER OVEN 卡尔费休高温炉

The following tests may be performed in case the Karl Fischer titrator (volumetric or coulometric) is coupled to an oven.

如果卡尔费休滴定仪(容量法或库仑法)配置了高温炉,应进行下列检查

4.1. TEMPERATURE ACCURACY 温度精密度

Materials:材料

Calibrated temperature probe.

经过校正的温度探头。

Method:方法

Set the oven temperature at150°C. Wait until the system is equilibrated.

将炉温设定为150℃,待系统平衡。

By means of the calibrated probe, measure the actual temperature in the oven (always in the same position) and compare it to the temperature displayed by the oven.

用校正过的温度探头,测量炉内实际温度(保持在同一位置),与高温炉的实际显示温度进行比较。

Limits:限度

The actual temperature may not differ more than ±5.0°C with respect to the set temperature.

实测温度与设定温度差值不应大于±5.0°C

4.2. TEMPERATURE STABILITY 温度稳定性

Materials:材料

Calibrated temperature probe.

校正过的温度探头。

Method:方法

Set the oven temperature at150°C. Wait until the system is equilibrated.

将炉温设定为150°C,待系统平衡。

Insert the calibrated temperature probe into the oven block (always in the same position). Read the initial temperature and repeat the reading after 20 minutes.

将校正过的温度探头插入炉内(保持总在同一位置)。读取初始温度,20分钟后再次读取温度。

Limits: 限度

The temperature after 20 minutes may not differ more than ±0.5°C with respect to the initial temperature.

20分钟后,实际温度与起始温度差异不得过±0.5°C

4.3. CARRIER GAS FLOW RATE 载气流速

Materials: 材料

Calibrated flowmeter or flow meter used in connection with a calibrated watch.

校正过的流量计或连接有校正过的秒表的流量计

Method: 方法

Set the carrier gas (air or N2) flow rate at 50 ml/min. By means of the calibrated flowmeter, measure the actual flow rate and compare it to the set value.

设定载气流速(空气或氮气)为50ml/min,用校正过的流量计测量实际流速,与设定值进行比较。

Limits:限度

The actual flow rate may not differ more than ±10 ml/min. with respect to the set flow rate.

实际流速与设定流速差异值不得过±10 ml/min


ANNEX II 附件2

Level IV. In-use instrument checks

第四级 在用仪器的检查

This Annex contains practical examples of tests and their associated tolerance limits for several parameters related to the performance of an automatic titrator.

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 IV of the equipment qualification process: “In-use instrument checks”.

这些例子可以被OMCL认为是仪器第四级别确认“在用仪器检查”的方法。

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).

适当的经过计量的标准物质(高纯,干燥),例如苯甲酸或三羟甲基甲胺(TRIS)。

Fresh titrant, appropriate to titrate the selected standard.

费休滴定剂,适合滴定所选择的标准。

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.

采用计量过的标准物质进行3次独立加样(如果使用的重量不同,顺序可以随机),进行至少3次滴定,滴定液消耗体积应为一管的20%-90%

Calculate the relative standard deviation of the titers obtained.

计算所得滴定度的相对标准偏差。

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

可以使用仪器内置的统计功能进行上述计算。

Limits: RSD 0.2 %

限度:RSD 0.2 %

1.2. ACCURACY 准确度

Materials: 材料

Refer to chapter 1.1. Precision. 参见第1.1章,精密度

Method:方法

Calculate the mean of the titers obtained in chapter 1.1. Precision.

计算在第1.1章,精密度中得到的滴定度的平均值。

For the calculation of the theoretical titer value of the titrant solution and the systematic deviation (drel), refer to Level III, chapter POTENTIOMETRIC TITRATORS; 1.2. ACCURACY.

对于滴定剂溶液的理论滴定度值和系统性偏差(drel)的计算,参见第III级,电位滴定仪第1.2章精密度。

Limits: 限度

The systematic deviation (drel) should be maximum ≤ ±2% of the theoretical titer (determined on a freshly opened titrant container).

系统偏差(drel)应最大不超过理论滴定度的±2%(以新开的滴定剂容器为准)。

Note: The implementation of the suggested limit depends on the quality of the used volumetric solution. The use of a new solution and/or the check of the titer are recommended.

注:所建议执行的可接受标准依赖于所用的定量溶液的质量。建议使用新溶液和/检查滴定度。

2. KARL FISCHER VOLUMETRIC TITRATORS

卡尔费休容量法滴定仪

2.1. PRECISION

准确度

Materials:

材料

Certified water standard solution with a defined guaranteed water contents of 10 mg/g.

经过标定的水标准溶液,水含量10mg/g

Karl Fischer reagents for volumetric water determination.

用于库仑法测定水分的卡尔费休试剂。

Method:

方法

Perform a minimum of 3 titrations with 3 independent additions of water standard solution (in random order if using different weights), which should result in a consumption of approx. 20 % to 90 % of the burette volume.

用水标准溶液3次独立进样,进行至少3次滴定(如果标准溶液重量不同,进样顺序可以随机),滴定消耗的滴定体积应为一管的20%-90%

Calculate the relative standard deviation of the titers obtained.

计算所得的滴定度的相对标准偏差。

If available, this calculation can be performed directly with the built-in statistics function of the instrument.

如果可以的话,该计算可以由仪器内置的统计功能直接计算得到。

Limits: RSD 1.5 %.

限度: RSD 1.5 %

2.2. RECOVERY 回收率

Materials and Method:

材料和方法

Refer to Recovery test in Level III.

参见第III级别 回收率测试

Limits限度: 97.5 % to 102.5 %.

限度: 97.5 % to 102.5 %

3. KARL FISCHER COULOMETRIC TITRATORS

卡尔费休库仑法滴定仪

3.1. RECOVERY

回收率

Materials and Method:

材料和方法

Refer to Recovery test in Level III.

参见第III级别 回收率测度

Limits:

限度

Water standard solution 1000μg/g - Recovery: 97.5 % to 102.5 %.

水标准溶液1000μg/g – 回收率: 97.5 % to 102.5 %.

Water standard solution 100μg/g - Recovery: 90.0 % to 110.0 %.

水标准溶液100μg/g – 回收率: 90.0 % to 110.0 %.

REFERENCES 参考文献

(For all references, the latest version applies 所有的参考文献均应采用现行版本)

1) Ph. Eur 欧洲药典. (2.5.12, 2.5.32).

2) Application Bulletin No. 255 - Validation of Metrohm KF Titrators according to GLP/ISO 9001. Metrohm. 应用期刊第255---万通卡尔费休滴定仪根据GLP/ISO9001的验证,万通

3) Application Bulletin No. 252 - Validation of Metrohm titrators (potentiometric) according to GLP/ISO 9001. Metrohm. 应用期刊第252---依据GLP/ISO 9001的万通滴定仪(电位滴定)的验证, 万通

4) Application Bulletin No. 273 - Validation of Metrohm KF coulometers using Standard Operating Procedures. Metrohm. 应用期刊第273---万通卡尔费休库仑法的标准操作程序,万通

5) Application Bulletin No. 283 – Validation of Metrohm burets. Metrohm. 应用期刊第283----万通滴定管的验证,万通