OMCL Network of the Council of Europe

QUALITY ASSURANCE DOCUMENT

质量保证文件

PA/PH/OMCL (06) 86 DEF

QUALIFICATION OF EQUIPMENT

仪器确认

ANNEX 2: QUALIFICATION OF GC EQUIPMENT

附件2：气相色谱仪的确认

Full document title and reference 文件全名和索引号	Qualification of Equipment Annex 2: Qualification of GC Equipment PA/PH/OMCL(06)86DEF
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 首次发行日期	May 2006
Date of original entry into force 首次执行日期	June 2007
Date of entry into force of revised document 修订后执行日期	October 2006
Previous titles/other references 原文件名/其它索引号	This document replaces part of document PA/PH/OMCL(06)46 DEF
Custodian Organisation 保管机构	The present document was elaborated by the OMCL Network/EDQM of the Council of Europe
Concerned Network 相关网络	GEON

ANNEX 2 OF THE OMCL NETWORK GUIDELINE

“QUALIFICATION OF EQUIPMENT”

OMCL网络指南“仪器确认”附件2

QUALIFICATION OF GC EQUIPMENT

气相色谱仪的确认

Introduction 介绍

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

本文件是核心文件“仪器确认”的第二个附件，在计划、实施和记录气相色谱仪的确认时，应将本文件与核心文件联合使用。

The core document contains the general introduction and the Level I and II of qualification, common to all type of instruments, and the present annex contains GC instrument-related recommendations on parameters to be checked and the corresponding typical acceptance limits, as well as practical examples on the methodology that can be used to carry out these checks.

核心文件包括了一般介绍和第一级与第二级确认，适用于所有类型的仪器，本附件包括了气相色谱仪相关的建议，包括哪些参数需要检查，相应的典型可接受标准，以及用来进行这些检查的实践方法学例子。

The tests proposed in the Level III and IV of qualification are based on an overall approach, in which several parameters are checked at the same time in a combined test procedure, to obtain information on the overall system performance (e.g. peak area precision, retention time precision, temperature programme reproducibility, etc).

在第三级和第四级确认所建议的检查是基于一种全面检查的方法，在其中同一个联合测试可以检查几个不同参数，得到全面的系统性能信息（例如峰面积精密度、保留时间精密度、温度程序重复性等）

Nevertheless, it should be noted that it is also acceptable to check these parameters individually by using other well-defined procedures.

另外，需要注意如果采用其它界定很好的程序对这些参数进行单独确认也是可以接受的。

TABLE III表3

Level III. Periodic and motivated instrument checks

第三级 周期主动仪器检查

Examples of requirements for GC instruments with FID

配备FID检测器的气相色谱仪的要求举例

Instrument module 仪器模块	Parameter to be checked 需要检查的参数	Typical tolerance limit 典型可接受限度
1 Inlet system 进样系统	1.1 Injector leak test    进样器泄漏检查 1.2 Pressure/flow accuracy and stability    压力/流速准确性和稳定性 1.3 Repeatability of injection (overall test 1) -- in split mode 分流模式 --In split less mode 分流较少模式 1.4 Injector temperature ands accuracy and stability 进样器温度 准确度和稳定性 1.5 Carry-over (overall test 3)    残留（全面检查3）	Pressure drop≤15kPa Within 5 min 5分钟内压降≤15kPa Covered by overall test 1 包括在全面检查1中 RSD≤3.0% RSD≤3.0% Covered by overall test 2 包括在全面检查2中 ≤0.2%
2. Oven 柱温箱	2.1 Repeatability of oven temperature characteristics 柱温箱温度重复性	Covered by overall test 2 包括在全面检查2中
3. FID detector FID检测器	3.1. Linearity (overall test 3) 线性（全面检查3） 3.2. Constant detector response     检测器响应恒定性 3.3 Noise噪声 3.3. Drift 漂移	r2≥0.999 covered by overall test 1 or 2 包括在全面检查1或2中 see annex 1 见附件1 See Annex 1 见附件2

TABLE IV 表四

Level IV. In-use instrument checks 第四级：在用仪器检查

Examples of requirements for GC instruments with FID 配置FID检测器的气相色谱仪为例

Parameter to be checked 需要检查的参数	Typical tolerance limits 典型可接受限度
1.       System suitability check for the method 方法系统稳定性检查	According to Ph. Eur. Or MAH dossier or validated in-house method 根据EP或MAH相关文件，或内部已验证的方法
2.       Peak area precision 峰面积精密度	RSD≤3.0% unless otherwise prescribed* 除另有规定外RSD≤3.0%
3.       Retention time repeatability 保留时间重复性	RSD≤2.0%
4.       Sensitivity (where relevant, e.g. for related substances tests) 灵敏度（如果相关，例如对于有关物质）	According to Ph. Eur. or MAH dossier or validated in-house method 根据EP或MAH相关文件，或内部已验证的方法

* This is to be defined in conjunction with the target concentration of the analyte

这要与分析物的目的浓度联系起来确定。

All parameters given here should be checked when performing analyses under the working conditions for the actual sample determinations. Normally, the test and reference solutions to be prepared for this purpose are given as a part of the method.

这里给出的所有参数应在工作状态下进行实际样品检查分析时进行检查。一般来说，供试液和对照溶液应根据此目的作为方法的一部分进行准备。

ANNEX I 附件1

Level III. Periodic and motivated instrument checks

第三级 仪器周期主动检查

Practical examples of tests and their associated tolerance limits for several parameters related to the performance of the different modules of a GC are presented below.

下面是与不同GC模块的性能相关的几个参数检查的实践例子和其相关的允许限度

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”.

这些例子可以认为是OMCL可以使用的进行第三级仪器确认“周期主动的仪器检查”的方法

Several tests are proposed to check various parameters at the same time (overall tests). In order to run the tests in a more economical way, other suitable solutions can be used, as for example, the “Grob Test” mixture, available from different suppliers (e.g. Alltech, Sigma, Thames Restek). This commercial solution should be appropriate to the column material used.

建议同时检查几个参数（全面检查）。为了采用更经济的检查式，也可以使用其它合适的溶液，例如“Grob Test”混合物，可以从几个供应商处采购（例如Alltech, Sigma, Thames Restek）。这个商业化溶液应适用于色谱柱材料。

It is recommended to run the overall test by using always the same test column, exclusively dedicated to qualification purposes, to guarantee reproducible conditions. 建议一直采用同一根色谱柱进行全面检查，该色谱柱专用于仪器确认，以保证条件的可重复性

1. INLET SYSTEM 进样系统

The following tests are proposed for the periodic and motivated check of the GC Inlet System.

建议对GC进样系统周期主动检查实施以下内容

1.1. INJECTOR LEAK TEST 进器器泄漏检查

Method:方法

If not otherwise specified by the instrument manufacturer, the leak test is carried out according to the procedure laid down in the instrument manual or by the built in automatic leak check procedure of the instrument.

如果仪器供应商未另行指明，泄漏检查应根据操作手册指定的程序来进行，或者由仪器的内置泄漏自动检测程序进行。

Otherwise use the test described below:

否则采用以下所述检查

Disconnect the column from the injector and close the injector outlet with a sealed cap.

断开柱子与进样器连接，封闭进样器出口

Close the septum purge and the bypass.

关闭隔垫吹扫和旁路吹扫

Adjust the flow and pressure controller to the maximal possible value of the pressure gauge.

调整流速和压力控制器至可能的压力最大值

Adjust the flow controller to zero.

调整流速并控制在0

Read the pressure after 1 minute and record the value.

在1分钟后读取压力值并记录

Record the pressure after 5 minutes.

在5分钟后记录压力值

Limits:限度

Pressure drop ≤ 15 kPa within 5 minutes.

5分钟内压降≤ 15 kPa

1.2. INLET PRESSURE/FLOW ACCURACY AND STABILITY 进样压力/流速准确性和稳定性

A direct measurement of these parameters was not deemed practical or necessary, but the optimal conditions of flow/pressure can be verified by the overall test 1.

直接对这些参数进行测量在实际中不可行或没有必要，但流速/压力的最好条件可以在全面检查1中进行确认。

Limits: refer to overall test 1.

限度：参见全面检查1

1.3. REPEATABILITY OF INJECTION 进样重复性

The verification of this parameter is covered by the overall test 1.

本参数的确认可以包括在全面检查1中

This test is to be performed in both split and split less mode.

检查应针对分流和少分流两种模式

Limits: refer to overall test 1.

限度：参见全面检查1

1.4. INJECTOR TEMPERATURE ACCURACY AND STABILITY 进样器温度准确性和稳定性

Due to the fact that the temperature cannot be reliably measured without opening and modifying the system and due to the difficulties of introducing a probe inside this module, the verification of this parameter is considered to be covered by the overall test 2.

由于在不打开柱温箱和调整系统条件的情况下很难可靠地对温度进行测量，并且探头很难放入本模块中，因此本参数包括在全面检查2A和2B中。

Limits: refer to overall test 2.

限度：参见全面检查2

1.5. INJECTOR CARRY OVER 进样器残留

After having injected the solutions for the linearity test of the FID detector, in increasing order, inject the blank and measure the peaks that correspond to the major peaks (= analytes) in the linearity solutions.

在FID检测器线性检查进样后，按浓度增加的顺序，进线性溶液空白并测量主峰（被分析物）。

The verification of this parameter is covered by the overall test 3.

本参数的确认可以包括在全面检查3中

Limits: refer to overall test 3.

限度：参见全面检查3

2. OVEN 柱温箱

2.1. REPEATABILITY OF THE OVEN TEMPERATURE CHARACTERISTICS 柱温箱温度的重复性

Due to the fact that the temperature cannot be reliably measured without opening and modifying the system conditions and that even when introducing a probe inside the oven, its location would not reflect the real temperature conditions at all points, the verification of this parameter is covered by the overall tests2Aand 2B.

由于在不打开柱温箱和调整系统条件的情况下很难可靠地对温度进行测量，即使将探头放入柱温箱中，其放置的位置也无法反映所有点的真实温度情况，因此本参数包括在全面检查2A和2B中。

Limits: refer to overall test 2.

限度：参见全面检查2

3. FID DETECTOR FID检测器

The following tests are proposed for the periodic and motivated check of the GC FID detector.

下列检查目的是对GC的FID检测器进行周期主动性检查

3.1. FID DETECTOR LINEARITY FID检测器线性

Increasing amounts of analyte are injected and a linear response should be obtained.

注入一系列不断增加数量的被分析物，所得的响应值应呈线性。

The verification of this parameter is covered by the overall test 3.

本参数的确认包括在全面检查3中

Limits: refer to overall test 3.

限度：参见全面检查3

3.2. CONSTANT FID DETECTOR RESPONSE 恒定FID检查器响应

The proper and reproducible functioning of the FID can be demonstrated by checking the peak areas obtained from a pre-defined standard solution.

FID检测器的功能正确性及重复性可以通过检查预设定的标准溶液的峰面积得到。

The verification of this parameter is covered by the overall test 1 or 2.

本参数的确认可以包括在全面检查1或2中

Limits: refer to overall test 1 or 2.

限度：参见全面检查1或2

3.3. FID DETECTOR NOISE AND DRIFT  FID检测器噪声和漂移

If the instrument has a built-in automatic system for the verification of the noise and drift, follow the manufacturer’s instructions and apply the defined acceptance criteria. Otherwise, use the test described below:

如果仪器有一个内置的自动系统进行噪声和飘移确认，应根据供应商的指示进行，并采用供应商的可接受标准。如无，则采用以下检查

Settings:设置

Column installed 色谱柱

Suitable flow, depending on column length/diameter

合适的流速，取决于柱长度/直径

No injection

无进样

Oven temperature:40°C

柱温：40°C

Detector on and heated at working temperature (270-300°C)

开检测器，加热至工作温度（270-300°C）

Method:方法

After stabilisation of the system, record the signal for 15 minutes.

系统平衡后，记录15分钟信号

Noise: evaluate 10 periods of 1 minute and calculate the mean value.

噪声：评价一分钟内十次噪声，计算平均值

Drift: evaluate the slope of the baseline over the 15 minutes.

飘移：评价15分钟内的基线飘移

Limits:限度

The acceptance criteria for these parameters have to be chosen in accordance with the instrument vendor’s instructions and the intended use of the instrument. If no instructions are given, the user has to pre-define these acceptance criteria by taking into account the previous experience and the intended use of the instrument.

这些参数的可接受标准应根据仪器供应商的指示以及仪器的使用目的来选择。如果供应商没有给出指示，使用者应在根据之前的经验以及仪器的使用目的预先确定可接受标准。

No fixed values can be pre-defined in this guideline due to the high variety of integration systems used and consequently the acceptance criteria may be expressed in different units (voltage, current, arbitrary units per time).

由于使用的积分系统差异很大，因而可接受标准可能表达为不同的单位（电压、电流、单位时间内任意单位），所以在本指南中，没有给出预定的固定值。

OVERALL TEST 1 全面检查1

The overall test 1 covers the following parameters:

全面检查1包括以下参数

—     Pressure/flow accuracy and stability in the inlet system: Retention time repeatability

—     进样系统压力/流速准确度和稳定性：保留时间重复性

—     Repeatability of injection: peak area precision

—     进样准确性：峰面积精密度

—     In split mode

—     分流模式

—     In split less mode

—     较少分流模式

The test may be combined with overall test 3.

检查可以与全面检查3一起进行

Split mode: 分流模式

Test solution: 供试液

1-octanol in n-hexane 1% (v/v).

1%正辛醇的正乙烷溶液（V/V）

Settings: 设置

Column: SPB-1 (30mx0.32mmID x 0.25μm film)

色谱柱：SPB-1 (30mx0.32mmID x 0.25μm 膜)

Carrier gas: He

载气：氦气

Velocity:25cm/sec

流速：25cm/sec

Split: 1:100

分流比：1：100

Injection: 1μl

进样量：1ul

Injector temperature:220°C

进样器温度：220°C

Oven temperature:100°Cisotherm

柱温箱温度：100°C等温

Detector temperature:300°C

检测器温度：300°C

Runtime: 8 min

运行时间：8分钟

Retention time of 1-octanol: about 5 min

正辛醇保留时间：约5分钟

Split less mode:分流较少模式

Stock solution: 1-octanol in n-hexane 1% (v/v)

贮备液：1%的正辛醇正己烷溶液（V/V）

Test solution: Dilute 10 ml of the stock solution with n-hexane to 100 ml (corresponds to 1μl/ml of 1-octanol in n-hexane)

供试液：取10ml贮备液用正己烷稀释至100ml（1μl/ml的正辛醇的正己烷溶液）

Settings:设置

Column: SPB-1,30m,0.32mmID, 0.25μm film

色谱柱：SPB-1,30m,0.32mmID, 0.25μm film

Carrier: He

载气：氦气

Velocity:30cm/sec

流速：30 cm/sec

Split less injection: purge valve closed during 2 min

分流较少模式进样：进样阀在2分钟内关闭

Injection: 0.2μl of the test solution

进样量：0.2ul供试液

Injector Temperature:220°C

进样器温度：220°C

Oven Temperature: Initial60°Cfor 4 min,15°C/min. up to135°C, final time 1min

柱温箱温度：起始温度60°C，维持4分钟，以15°C/min速率升温至135°C，保持1分钟

Detector temperature:300°C

检测器温度：300°C

Runtime: 9.5 min

运行时间：9.5分钟

Retention time of 1-octanol: about 8 min

正辛醇保留时间：约8分钟

Method:方法

Carry out 6 consecutive injections of the test solution and calculate the RSD of the different peak areas and retention times.

连续进6针供试液，计算各峰面积和保留时间的RSD

Limits:限度

Retention time repeatability: the RSD of the retention times should be ≤ 2.0%

保留时间重复性：保留时间RSD≤ 2.0%

Peak area precision (split and split less mode): the RSD of the peak areas should be ≤ 3.0%

峰面积精密度（分流模式和分流较少模式）峰面积RSD≤ 3.0%

OVERALL TEST 2 全面测试2

The overall test 2 covers the following parameters: 全面测试2包括以下参数

-          Injector, oven and detector temperature accuracy and stability: retention time repeatability

-          进样器、柱温箱和检测器温度准确性和稳定性：保留时间重复性

Two alternative tests are proposed: 建议采用两个可相互替代的方法之一

Overall test2A全面测试2A

Test solution:供试液

0.035 ml 1-octanol （正辛醇）

0.035 ml 2-octanone（2-正辛酮）

0.035 ml 2,6-dimethylanilin （2.6-二甲基苯胺）

0.035 ml n-tridecane（正十三烷）

0.035 ml n-tetradecane（正十四烷）

35 mg n-eicosane（正二十烷）

dissolved in 50 ml Dichloromethane

溶于50ml二氯甲烷

Settings:设置

Column: SPB-1 (30mx0.32mmID x 0.25μm film)

色谱柱：SPB-1 (30mx0.32mmID x 0.25μm film)

Carrier gas: Helium

载气：氦气

Velocity:25 cm/s

流速：25 cm/s

Split: 1:100

分流比：1：100

Injection volume: 1 μl

进样量：1ul

Injector temperature:220°C

进样器温度：220°C

Detector: FID

检测器：FID

Detector temperature:300°C

检测器温度：300°C

Gradient programme:60°C(4 min),5°C/min,270°C(3 min)

程序升温程序：60°C (4 min),5°C/min,270°C(3 min)

Method:方法

Inject the solution twice and calculate the relative retention times in relation to n-eicosane (RRT = 1)

进样2针，计算对正二十烷（RRT=1）的相对保留时间

The following table shows the approximately expected relative retention times.

下表为大概的期望相对保留时间

Analyte 分析物	1-octanol	2-octanone	2,6-dimethylaniline	n-tridecane	n-tetradecane
RRT	0.30	0.22	0.37	0.52	0.60

Limits:限度

The RSD of each RRT from two consecutive injections should be ≤ 1.0%

每个物质2针RRT的RSD应≤ 1.0%

Overall test 2B 全面测试2B

Test Solution:供试液

1.0% (W/W) n-Nonane and Hexadecane in Tetradecane.

1.0%（W/W）正壬烷和十六烷溶于正十四烷中

Settings:设置

Column: Ultra-1 (25mx0.32mmID x 0.52μm film)

色谱柱：Ultra-1 (25mx0.32mmID x 0.52μm film)

Injection volume: 1 μl

进样量：1 μl

Solvent: Tetradecane

溶剂：正十四烷

Oven temperature:110°C

柱温箱温度：110°C

Gradient programme:110°C,20°C/min,180°C(final time: 3.5 min)

升温程序：110°C,20°C/min,180°C(final time: 3.5 min)

Detector temperature:250°C

检测器温度：250°C

Injector temperature:200°C

检测器温度：200°C

Detector: FID

检测器：FID

Flow rates: Carrier gas (Helium): 2 ± 0.2 ml/min

流速：载气（氦气）：2 ± 0.2 ml/min

Hydrogen: 30 ± 1.0 ml/min

氢气：30 ± 1.0 ml/min

Air: 400 ± 20.0 ml/min

空气：400 ± 20.0 ml/min

Makeup (Nitrogen): 28 ± 1.0 ml/min

尾吹（氮气）：28 ± 1.0 ml/min

Split ratio: 15

分流比：15

Split vent: 30 ± 3.0 ml/min

分流排空：30 ± 3.0 ml/min

Septum purge: 3-5 ml/min

隔垫吹扫：3-5 ml/min

Method:方法

Allow the system to equilibrate. 将系统平衡

Injection sequence: 进样序列

1) blank (Tetradecane) 空白（正十四烷）

2) 6 replicates of the test solution. Calculate the mean of the retention times and peak areas and the relative standard deviation of n-Nonane and n-Hexadecane.

6针供试液，计算正壬烷和十六烷保留时间、峰面积的平均值和相对标准偏差，

Limits:限度

Retention time repeatability: RSD of the peak retention times of the 6 replicates ≤ 2%

保留时间重复性：6次进样峰保留时间RSD≤ 2%

Retention time (Rt) accuracy: for this example, the retention time ranges shown in the table below are proposed. Nevertheless, individual ranges should be predefined by the laboratory depending on the column used (e.g. Rt ± 0.2 min).

保留时间准确度：对于这个例子，建议了下表中保留时间范围。无论如何，单个范围应该由化验室根据所使用的色谱柱来预先定义（例如Rt ± 0.2 min）

Compound 化合物	Rt(min)
n-Nonane (C9) 正壬烷	1.3-1.7
Tetradecan (C14) 十四烷	4.0-4.7
Hexadecane (C16)十六烷	5.1-6.0

OVERALL TEST 3 全面测试3

This test is a modified version of the overall test 1 to be used for the verification of:

本检查是全面检查1的修订版本，用于以下确认

—     Detector linearity: linearity of the areas recorded

—     检测器线性：记录的面积的线性

—     Injector carry-over: area recorded in the blank run

—     进样器残留：空白进样中记录的峰面积

It is described for both split and split less mode and may be combined with overall test 1.

对于分流模式和分流较少模式均可以与全面检查1一起进行

Split mode: 分流模式

Test solution: 1-octanol in n-hexane 1% (v/v)

供试液：正辛醇的正己烷1%溶液（V/V）

Prepare further reference solutions by diluting the test solution as described below.

按下述要求稀释供试溶液进一步制备参比溶液

Settings: see overall test 1

设置：见全面测试1

Injection sequence:进样序列

5.0 ml of the test solution diluted to 25.0 ml with n-hexane (2 μl/ml): 2 injections

取5.0ml供试液用正己烷稀释至25.0ml（2 μl/ml）：进样2针

10.0 ml of the test solution diluted to 25.0 ml with n-hexane (4 μl/ml): 2 injections

取10.0ml供试液用正己烷稀释至25.0ml（4μl/ml）：进样2针

15.0 ml of the test solution diluted to 25.0 ml with n-hexane (6 μl/ml): 2 injections

取15.0ml供试液用正己烷稀释至25.0ml（6μl/ml）：进样2针

20.0 ml of the test solution diluted to 25.0 ml with n-hexane (8 μl/ml): 2 injections

取20.0ml供试液用正己烷稀释至25.0ml（8μl/ml）：进样2针

if combined with overall test 1 for repeatability: test solution (10 μl/ml): 6 injections

如果与全面检查1一起做重复性：供试液（10 μl/ml）：进样6针

n-hexane as blank (carry over) 正己烷作为空白（残留）

Split less mode: 分流比

Stock solution: 1-octanol in n-hexane 1% (v/v)

贮备液：1%的正辛醇正己烷溶液（V/V）

Test solution: Dilute 10 ml of the stock solution with n-hexane to 100 ml (corresponds to 1μl/ml of 1-octanol in n-hexane).

供试液：取10ml贮备液用正己烷稀释至100ml（1μl/ml的正辛醇正己烷溶液）

Prepare further reference solutions by diluting the test solution with n-hexane.

用正己烷稀释供试液制备对照溶液

Settings: see overall test 1

设置：见全面检查1

Injection sequence:进样序列

5.0 ml of the test solution diluted to 25.0 ml with n-hexane (0.2 μl/ml): 2 injections

取5.0ml供试液用正己烷稀释至25.0ml（0.2 μl/ml）：进样2针

10.0 ml of the test solution diluted to 25.0 ml with n-hexane (0.4 μl/ml): 2 injections

取10.0ml供试液用正己烷稀释至25.0ml（0.2 μl/ml）：进样2针

15.0 ml of the test solution diluted to 25.0 ml with n-hexane (0.6 μl/ml): 2 injections

取15.0ml供试液用正己烷稀释至25.0ml（0.6 μl/ml）：进样2针

20.0 ml of the test solution diluted to 25.0 ml with n-hexane (0.8 μl/ml): 2 injections

取20.0ml供试液用正己烷稀释至25.0ml（0.8 μl/ml）：进样2针

if combined with overall test 1 for repeatability: test solution (1 μl/ml): 6 injections

如果与全面检查一起做重复性：供试液（1 μl/ml）：进样6针

n-hexane as blank (carry over)

正己烷作为空白 （残留）

Limits:限度

Linearity: coefficient of correlation of the calibration line obtained with the reference solutions and the test solution: r2 ≥ 0.999.

线性：用对照溶液和供试液所得的校正数值的线性 r2 ≥ 0.999

Carry-over: the percentage of the peak area corresponding to the analyte in the blank solution should be ≤ 0.2% of the peak area of this analyte in the chromatogram obtained with the solution with the highest concentration within the sequence.

残留：在空白中被分析物的峰面积百分比与最高浓度试液中被分析物的峰面积比值应≤ 0.2%