OMCL Network of the Council of Europe

QUALITY ASSURANCE DOCUMENT

质量保证文件

PA/PH/OMCL (07) 12 DEF CORR

QUALIFICATION OF EQUIPMENT

仪器确认

ANNEX 4: QUALIFICATION OF IR SPECTROPHOTOMETERS

附件4 红外分光光度计的确认

Full document title and reference 文件全名和索引号	Qualification of Equipment 仪器确认 Annex 4: Qualification of IR sepctrophotometers 附件4：红外分光光度计确认 PA/PH/OMCL(07)12 DEF CORR
Document type 文件类型	Guideline
Legislative basis 立法基础	The present 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	May 2007
Date of original entry into force 首次生效日期	July 2007
Date of entry into force of revised document 修订生效日期	December 2007
Previous titles/other references 曾用文件名/其它索引号	This document replaces document PA/PH/OMCL(07) 12 DEF
Cutodian organisation 管理机构	The present document was elaborated by the OMCL Network/EDQM of the Council ofEurope
Concerned Network 相关网络	GEON

ANNEX 4 OF THE OMCL NETWORK GUIDELINE

“QUALIFICATION OF EQUIPMENT”

OMCL网络指南“仪器确认”附件4

QUALIFICATION OF IR SPECTROPHOTOMETERS

红外分光光度计的确认

Introduction 介绍

The present document is the fourth Annex of the core document “Qualification of Equipment”, and it should be used in combination with it when planning, performing and documenting the IR spectrophotometer qualification process.

本文件为“仪器确认”核心文件的第四个附件，在对红外分光光度计确认过程进行计划、实施和记录时，应结合该核心文件一起使用。

The core document contains the Introduction and general forms for Level I and II of qualification, which are common to all type of instruments.

核心文件包括了第一级和第二级确认的介绍和通用表格，该表格通用于各类型仪器。

For FTIR spectrometers, an example has been added to give instrument-specific proposals that may be used in combination with the general requirements presented in the core document “Qualification of Equipment”, when drawing up a Level I checklist.

对于傅立叶红外变换光度计，在本指南中给出一个仪器专用的方案，在起草第一级检查清单时，与“仪器确认”核心文件中的第一级通用表格一起使用。

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.

附件中包括了与仪器相关，在第三级和第四级确认中需要检查的参数，以及其相应的典型可接受限度，和用于实施这些检查的实用方法举例。

TABLE I 表一

Level I. Selection of instruments and suppliers

第一级 仪器和供应商选择

Example of check-list (non-exhaustive)

检查清单举例（未尽列举）

Manufacturer: 生产商

Provider/Distributor: 分销商/供货商

Name of instrument and type: 仪器名称和型号

Attribute 特征 (This list may be adapted if necessary) （本清单在需要时采用）	Specification 标准	Benefits 优点(Instrument/ supplier) （仪器/供应商）	Assessment 评价
			Pass 通过	Fails 不通过
Spectrophotometer 分光光度计
Detector range 检测器范围	The optical bench shall include a DTGS detector with a frequency range of 7400 to350cm-1 光具座应包括一个DTGS检测器，其频率范围为7400至350cm-1
It shall include a compressed air interferometer 应包括一个压缩空气干涉仪
The instrument shall come with an air-cooled standard infrared source 仪器应具有气冷标准红外源
Spectral resolution 光谱分辨率	The instrument shall have a spectral resolution not exceeding1.0cm-1
Wave number accuracy 波数准确度	Wave number accuracy shall be better than ±0.01cm-1
The interferometer shall have at least four basic velocity levels; software shall permit the selection of a greater number of velocities between the basic levels. 干涉仪应至少有四个基本速率水平；软件应允许在基本水平间选择较大值
The mirror’s greatest velocity shall allow a speed of at least five sweeps per second. 镜子最大速率应允许至少每秒5次清扫
The laser and infrared beams must be coaxial to enable rapid, easy alignment of the system, depending on the samples or accessories. 激光和红外光束必须同轴，可以根据样品或附件情况，迅速容易地调整定位
The instrument shall have a beam splitter with a range of 7400 to350cm-1 仪器应具有分光器，其范围为7400至350cm-1
The optical bench shall have a main experimentation module with a device to allow purging with nitrogen. 光具座应具有主实验模具，允许用氮气吹扫净化
At purchase, the main experimentation module shall be designed so it can receive 13 and5mmpotassium bromide pellets. 采购时，主实验夹具应设计为可以接受13和5mm溴化钾丸

Notes: 注

—     This check-list, containing examples of technical attributes that can be taken into account in the selection of an instrument and supplier, can be used in combination with the general check-list presented in Level I in the core document “Qualification of Equipment”.

—     本检查清单包括了技术特性举例，在选择仪器和生产商时可以进行考虑，可以与核心文件“仪器确认”中第一级通用检查清单结合使用。

—     For Table II (Level II of Equipment Qualification: Installation and release for use) please refer to the core document.

—     表二（第二级仪器确认 安装和使用放行）参见核心文件

TABLE III 表三

Level III. Periodic and motivated instrument checks

第三级 周期性主动仪器检查

Examples of requirements for IR spectrophotometers

红外分光光度仪的要求举例

Parameter to be checked 需要检查的参数	Typical tolerance limits 典型允许限度
1.       wave-number scale 波数刻度	See annex 1 见附件1
2.       Detector energy ratio 检测能量比	See manufacturer’s specification 见生产商标准
3.       Signal/Noise ratio 信噪比	See manufacturer’s specifications 见生产商标准
4.       Resolution 分辨率	See Annex 1 见附件1
5.       Zero test 零点检测	See manufacturer’s specification 见生产商标准
6.       Contamination check (only for ATR instruments) 污染检查（仅对ATR仪器）	See Annex I 见附件1
7. Throughput check (only for ATR instruments) 流量检查（仅对ATR仪器）	80%
8. Spectral library 图谱库	See Annex I 见附件1

TABLE IV 表四

Level IV. In-use instrument checks

第四级 在用仪器检查

Examples of requirements for IR spectrophotometers

红外分光光度计要求举例

Parameter to be checked 需要检查的参数	Typical tolerance limits 典型允许限度
1.       System suitability check 系统适用性检查	According to Ph. Eur. Or MAH dossier or validated in-house method 根据EP或MAH文件或验证过的内控方法

ANNEX I 附件1

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 an IR spectrophotometer.

本附件包括了红外分光光度计性能相关的几个参数的检查实例及其相关的允许限度

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”.

这些举例可以认为是OMCL在实施第三级检查“周期性主动仪器检查”时可能方法。

Note: If available and judged appropriate, the use of the automatic internal calibration function of the instrument is encouraged. Please refer to the manufacturer instructions.

注：如可能，且判断为适用，鼓励采用仪器内置校正功能。参见供应商指导手册。

1. WAVE-NUMBER SCALE 波数刻度

Method and Limits:方法和限度

The wave-number scale may be verified by recording the spectrum of a polystyrene film, which has transmission minima (absorption maxima) at the wave numbers (in cm-1) shown in the table below:

确认波数刻度时，记录聚苯乙烯薄膜的图谱，该图谱最小透过率（最大吸收）波数值（cm-1）列于下表。

Limits: 限度

Energy ratio test specifications vary for each spectrometer configuration. Refer to the manufacturer’s specification.

能量比测试标准根据各仪器参数不同，参见生产商标准。

3. SIGNAL/NOISE RATIO 信噪比

Method: 方法

Record the maximum noise level for each of the following regions:

记录以下波数区域最大噪声水平

Peak-to-peak noise between: 噪声波数区域

4050 cm-1 and3950 cm-1

2050 cm-1 and1950 cm-1

1050 cm-1 and950 cm-1

550 cm-1 and450 cm-1

(systems with DTGS detector only 仅适用于DTGS检测器系统)

RMS (root mean square) noise between: 在以下波数间的RMS（均方根）

4050 cm-1 and3950 cm-1

2050 cm-1 and1950 cm-1

1050 cm-1 and950 cm-1

550 cm-1 and450 cm-1

(systems with DTGS detector only 仅适用于DTGS检测器系统)

Limits (% T): 限度（%T）

Noise level test specifications vary for each spectrometer configuration. Refer to the manufacturer’s specifications.

信号水平测试标准根据每个光谱仪的参数不同而不同，参见生产商标准。

4. RESOLUTION 分辨率

Materials: 材料

Certified polystyrene film of approximately 35 μm in thickness.

Method: 方法

—     For instruments having a monochromator, record the spectrum of the polystyrene film.

—     单色器光谱仪记录聚苯乙烯薄膜的光谱

—     For Fourier-transform instruments, use suitable instrument resolution with the appropriate apodisation prescribed by the manufacturer. The resolution is checked by suitable means, for example by recording the spectrum of a polystyrene film approximately 35 μm in thickness.

—     对于傅立叶变换光谱仪，采用供应商描述的吸收器所适用的仪器分辨率。分辨率采用适当的方法进行检查，例如记录厚度红为35μm的聚苯乙烯薄膜的光谱图。

用于分辨率性能检查的聚苯乙烯的典型图谱

Limits: 限度

Monochromator instruments: 单色器仪器

—     Difference x between the percentage transmittance at the transmission maximum A at2870 cm-1 (3.48 μm) and that at the transmission minimum B at2849.5 cm-1 (3.51 μm) > 18.

—     在2870cm-1(3.48 μm)处最大透光A和在2849.5cm-1 (3.51 μm)处最小透光B差值X > 18

—     Difference y between the percentage transmittance at the transmission maximum C at1589 cm-1 (6.29 μm) and that at the transmission minimum D at1583 cm-1 (6.32 μm) > 10.

—     的1589cm-1(6.29 μm)处最大透光C和在1583cm-1(6.32 μm)处最小透光D差值Y > 10

Fourier-transform instruments: 富立叶变换仪器

—     Difference between the absorbances at the absorption minimum at2870 cm-1 and the absorption maximum at2849.5 cm-1 > 0.33.

—     在波长2870cm-1最小吸收和在2849cm-1最大吸收差值> 0.33

—     Difference between the absorbances at the absorption minimum at1589 cm-1 and the absorption maximum at1583 cm-1 > 0.08.

—     在1589cm-1处的最小吸收和在1583cm-1处的最大吸收差值> 0.08

5. ZERO TEST 零点测试

Method: 方法

When using a polystyrene film of approximately 35 μm in thickness as standard at the wavelength of2925 cm-1 and700 cm-1, almost complete absorption of the irradiated energy can be observed. With this test, the remaining transmission is measured. As the maximum absorption can be observed at700 cm-1 negative values may be observed. The objective of the test is to evaluate if, despite the fact that there is almost complete absorption, energy is still detectable.

当使用约35μm厚的聚苯乙烯薄膜作为标准时，在波长2925cm-1和700cm-1处，辐照能量几乎被完全吸收。在这个测试中，测量剩余的能量。由于在700cm-1处能观察到最大吸收，可能会测得负值。检查的目标是，测试是否还能检到能量，尽管事实上可能被会部吸收。

Non-valid results are an indication of a non-linear behaviour of the detector and the electronic system.

无效的结果表明检测器和电子系统呈非线性

Limits (%T): 限度

See manufacturer’s specification.

见供应商标准

6. CONTAMINATION TEST (only for Attenuated Total Reflection (ATR) instruments) Note: if an automated system is available, this test can be run more frequently or it can be transferred to Level IV, to be run before each analysis.

污染检查（仅用于衰减全反射（ATR）仪器） 注：如果使用的是自动系统，该检测频次可以更高，或者转至第四级，在每次分析前检查

Method:方法

This test checks the presence of peaks that signal a contamination problem.

本测试检查出现在峰信号是否有污染问题

Use the automated function of the instrument (if available) to perform this test. If not available, record a background spectrum.

如果有自动功能的话，采用自动功能实施检查，如果没有，记录背景图谱

Limits:限度

Wave-number 波数 (cm-1)	Upper limit  上限 (A)
3100.0-2800.0	0.1
1800.0-1600.0	0.1
1400.0-1100.0	0.2

7.       THROUGHPUT CHECK (only for Attenuated Total Reflection (ATR) instruments)

流量检查（仅针对衰减全反射（ATR）仪器）

Note: if an automated system is available, this test can be run more frequently or it can be transferred to Level IV, to be run before each analysis.

注：如果有自动系统，本测试可以按更高的频次进行，或者转入第四级，在每次分析前检查。

Method:方法

This test checks for an unexpected reduction of the transmittance. An instrument specific automated test can be used.

本项目用于检查非预期的传输衰减，可以采用系统自动测试。

A background spectrum is recorded and the transmittance is measured at 3 wave numbers e.g. 4000, 2600 and1000 cm-1.

记录背景图谱，在3个波数记录透光率，例如 4000，2600和1000cm-1

Limits:限度

The lower limit of the transmittance for the 3 wave numbers must be 80 %.

3个波数透光率最低限度应为80%

8. SPECTRAL LIBRARY 谱图库

It is recommended to record the spectrum of a newly acquired polystyrene film and to save it in a spectra library.

建议记录一个新扫描的聚苯乙烯薄膜的图谱，保存在图谱库中。

Electronic libraries for checking the identity of unknown substances should be examined from time to time by using selected examples of well-known reference substances.

对电子谱库应选用已知物质样品定期进行检查，以确认其能识别未知物质。

Requirements:要求

The substances are unambiguously identified by the electronic library search.

物质可以由电子谱库搜索进行准确识别。

ANNEX II 附件2

Level IV. In-use instrument checks

第四级 在用仪器检查

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

本附件包括一些测试实践举例，以及红外光谱仪性能相关的参数允许限度

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”.

这些举例可以认为是OMCL作为实施第四级检查“在用仪器检查”的可能的方法。

Note: If available and judged appropriate, the use of the automatic internal calibration function of the instrument is encouraged. Please refer to the manufacturer instructions.

注：如果有，并判断适当，鼓励使用自动内置校正功能。参见生产商指导

1. SYSTEM SUITABILITY TEST OF THE METHOD 方法系统适用性检查

Method:方法

This test should be performed according to Ph. Eur., the MAH dossier or a suitably validated in-house method.

本测试应根据EP，MAH文件或适用的验证过的内控方法进行。

Note: regeneration or replacement of the desiccant should be done in case of failure of the system suitability test (e.g. by drying it for 8-12h at250°C, then flushing with N2).

注：如果系统适用性试验失败，应更新或替换干燥剂（例如，在250°C干燥8-12小时，再用氮气吹洗）

REFERENCES 参考文献

(For all references, the latest version applies)

（所有参考文献以最新版本为准）

1)      Ph Eur.2.2.24, Absorption spectrophotometry, Infrared.

欧洲药典2.2.24，吸收光谱仪，红外