JJG 705-2002 液相色谱仪

中华人民共和国国家计量检定规程

JJG705-2002

液相色谱仪

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2002一05一24发布2002一08一24实施

国家质量监督检验检疫总局发布

JJG705-2002

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液相色谱仪检定规程

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本规程经国家质量监督检验检疫总局于2002年05月24日批准，并自

2002年08月24日起施行。

归口单位:全国物理化学计量技术委员会

起草单位:国家标准物质研究中心

本规程委托全国物理化学计量技术委员会负责解释

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JJG705-2002

本规程主要起草人:

赵敏(国家标准物质研究中心)

参加起草人:

吴方迪(国家标准物质研究中心)

何雅娟(国家标准物质研究中心)

dJG705-2002

目录

1范围·(1)

2概述··························································································，··…(1)

3计量性能要求··············································································……(1)

3.1输液系统·················································································……(1)

3.2柱温箱···························，··························································，…(1)

3.3检测器···················································································……(1)

3.4整机性能·················································································……(2)

4通用技术要求··············································································……(2)

4.1仪器外观·················································································……(2)

4.2仪器电路系统···········································································……(2)

5计量器具控制··············································································……(3)

5.1检定条件·················································································……(3)

5.2检定项目和检定方法··································································……(3)

5.3检定结果的处理········································································……(9)

5.4检定周期·················································································……(9)

附录A色谱柱性能测试··································································……(10)

附录B检定证书(内页)格式·························································……(12)

附录C液相色谱仪检定记录格式······················································……(13)

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.T.TG705-2002

液相色谱仪检定规程

范围

本规程适用于配有紫外一可见光检测器、二极管阵列检测器、荧光检测器和示差折

光率检测器的液相色谱仪的首次检定、后续检定和使用中检验。液相色谱仪样机试验和

定型鉴定中有关计量性能试验可参照本规程进行。

2概述

液相色谱仪(以下简称仪器)是由输液系统、进样器、色谱柱(柱温箱)、检测器

和数据记录处理装置等部分组成的分析仪器，图1是其组成的方框图。液相色谱仪利用

试样中各组分在色谱柱内固定相和流动相间分配或吸附特性的差异，由流动相将试样带

人色谱柱中进行分离，经检测器检测，依据组分的保留时间和响应值(峰面积或峰高)

进行定性和定量分析。

图1液相色谱仪组成方框图

3计量性能要求

3.1输液系统

3.1.1输液管路接口紧密牢固，在规定的压力范围内无泄漏。

3.1.2流量设定值误差S、和流量稳定性误差S、应符合表1的要求。

3.1.3梯度误差‘:不超过士3%a

3.2柱温箱

3.2.1柱箱温度设定值误差△T:不超过士20Co

3.2.2温度稳定性T,:不超过1℃。

3.3检测器

液相色谱仪检测器的主要技术指标见表2.

JJG705-2002

表1流It设定值误差S:和流As定性误差S,的要求

流量设定值/(m1/min)0.51.02.0

测量次数333

流动相收集时间/min1055

S,5%3%2%

允许误差

SR3%2%2%

注:①最大流量的设定值可根据用户使用情况而定。

②对特殊的、流量小的仪器，流量的设定可根据用户使用情况选大、中、小三个流量，

流动相的收集时间则根据情况适当缩短或延长。

表2液相色谱仪检测器的主要技术指标

3.4整机性能

仪器的整机性能用定性定量测量重复性表示。

3.4.1‘定性测量重复性((6次测量)RSD6:不超过1.5%0

3.4.2‘定量测量重复性(6次测量)RSD6:不超过3.0%.

注:*与检定结果的处理有关，详见5.3条。

4通用技术要求

4.1仪器外观

仪器上应有仪器的名称、型号、制造厂名、产品系列号、出厂日期等内容的标牌，

国产仪器应有制造计量器具许可证砚巨弓标志。

4.2仪器电路系统

仪器电源线、信号线等插接紧密，各开关、旋钮、按键等功能正常，指示灯灵敏，

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2

JdG705-2002

显示器清晰。

5计f器具控制

计量器具控制包括:首次检定、后续检定和使用中检验。

5.1检定条件

5.1.1环境条件

检定室应清洁无尘，无易燃、易爆和腐蚀性气体，排风良好。

室温在15-30℃，检定过程中温度变化不超过3℃(对示差折光率检测器，

室温变化不超过29C)，室内湿度在20%一85%RH范围内。

仪器应平稳地放在工作台上，周围无强烈机械震动和电磁干扰源，仪器接地

良好。

电源电压为(220士22)V，频率为(50土0.5)Hz.

5.1.2检定设备

秒表:分度值不大于0.1so

分析天平:最大称量不小于100g，最小分度不大于1mgo

数字温度计:测量范围为0一100℃，最小分度不大于0.1℃。

注射器:10[L和50yL各一支。

以上计量器具需经计量检定合格。

10mL注射器一支。

游标卡尺:15cm/0.02mm.

容量瓶:50mL,10个。

5.1.3标准物质:

1x10一<g/mL,1x10一'g/.L的蔡/甲醇溶液;

1x10-6g/mL,1/10-'g/mL的硫酸奎宁/高氯酸水溶液;

1x10-'创mL,1x10-5g/mL的丙三醇1水溶液;

紫外波长标准溶液。

5.1.4其他要求

检定用试剂:HPLC用甲醇、纯水，分析纯的丙酮和异丙醇等。

其他玻璃器皿等

52检定项目和检定方法

5.2.1检定项目

检定项目见表30

表3检定项目一览表

序号检定项目首次检定后续检定使用中检验