第一部分 介绍..........................................................................................................................................1-1 1.1 概述 .........................................................................................................1-1 1.2 PFPD描述............................................ .............................................................................1-1 1.2.1 PFPD基本部件.......................................... ...................................................1-1 1.2.2 PFPD组件的特点............................. ........... ................................1-2 1.2.3 PFPD电路板的特点............................. ........... ..................................1-4 1.3 PFPD操作理论................................................................. ........... ...............................1-4 1.3.1 PFPD火焰脉冲步骤.............................. .......................... ..........................1-5 1.3.2 PFPD火焰脉冲步骤操作................. ........... .................................1-6 1.3.3 PFPD怎样提高灵敏度和选择性.................... ........... .................................1-6 1.3.4 PFPD气体流路............................. ........... .................................1-10 1.3.5 参考文献........................ .................. .......................................................1-10 1.4 PFPD指标................................................................. ........... ................................1-11 1.5 氮或其它元素的操作.................................................. ........... ................................1-11 第二部分 设定PFPD ........................................................................................2-1 2.1 概述 ..........................................................................................................2-1 2.2 PFPD检查...................................................................... ........... ................................2-1 2.3 PFPD配件工具包的内容................................................... ........... ................................2-2 2.4 PFPD扩展工具包的内容................................................ ......... ................................2-3 第三部分 操作 ........................................................................................3-1 1.1 概述 .........................................................................................................3-1 3.2 安装色谱柱................................................................ ........... ................................3-1 3.2.1 柱安装.......................................................... ...............................................3-1 3.2.2 准备色谱柱头............................. ........... .................................3-2 3.2.3 PFPD装配.....................................................................................................3-3 3.2.4 PFPD的分解............................. ........... .................................3-3 3.2.6 插入柱子....................... ..........................................................................3-5 3.2.6 重新装配PFPD............................. ........... .................................3-6 3.3 调节气体流速................................................................. ........... ................................3-7 3.3.1 分流阀. ......................... ..............................................................................3-7 3.3.2 PFPD气路图........................................... ...................................................3-8 3.3.3 调节气体流速............................. ........... .................................3-9 3.4 校正流量控制器................................................................. ......... ................................3-10 3.5 优化PFPD ..........................................................................................................3-11 3.5.1 检测限...................................... .................................................................3-12 3.5.2 选择性....................................................... ........... .................................3-12 3.5.3 生产率............................ ................................... ..................................3-12 3.5.4 燃气流速建议值......... ............................................ ...................................3-13 3.5.5 PFPD调节建议值.................................................... .................................3-13 3.5.6 优化要点............................. ........... .................................3-14 3.5.7 建立Tick-Tock.............................................................................................3-17 3.5.8 光电倍增管高压............................. ........... .................................3-20 3.5.9 调节光电倍增管(PMT)电压................ ........... ........... .............................3-20 3.5.10 优化PFPD................................................. ....... ......................................3-21 3.5.11 重复进标样.....................................................................................3-22 3.5.12 标准的连续扩散.......................... ........... .................................3-23 3.6 测试PFPD 性能..........................................................................................................3-25 3.6.1 测试PFPD 性能..........................................................................................3-25 3.6.2 PFPD测试谱图(S性能)......... ..................... ........... ................................3-25 3.6.3 PFPD测试谱图(P性能)........... ................. ........... ..................................3-27 3.6.4 检测限.......... .................................................... ......................................3-28 3.6.5 PFPD测试谱图(S检测限).... ........... .......... ........... .................................3-29 3.6.6 PFPD测试谱图(P检测限).... ......... ............ ........... .................................3-30 3.7 使用门延迟和门宽度参数.................................... ......... ..................................................3-30 3.7.1 设定触发电位..............................................................................................3-31 3.7.2 设定门延迟和门宽度............... ....... ................ ........... ..............................3-34 3.7.3 设定门宽度........ .... .. ......... .................. ........... ..................................3-35 3.8 建立一个GC方法 ........................................................................................................3-35 3.9 建立一个GC工作站方法.................................................... .......... ................................3-36 3.10 定量.......................................... ........... ................ .......... ........... ................................3-37 3.10.1 用PFPD进行定量......................................................................................3-37 3.10.2 峰面积定量............................. ........... .................................3-38 3.10.3 峰高定量...................................................................................................3-38 3.10.4 使用PFPD的峰分辨率............................. .......... ................................3-38 3.10.5 硫模式定量.......... .......... ..................... .................. ........... ..................3-38 3.10.6 平方根功能............................. ........... .................................3-39 第四部分 高级操作 ........................................................................................4-1 4.1 概述 ..........................................................................................................4-1 4.2 操作理论................................................................ ........... ................................4-1 4.2.1 优化的流速表............................. ........... .................................4-2 4.3 N模式部件的安装............................................................. ......... ................................4-2 4.4 N模式操作................................................................. ........... ................................4-4 4.5 P模式操作 ..........................................................................................................4-5 4.6 S模式操作 ..........................................................................................................4-5 4.7 部件和消耗品..........................................................................................................4-5 4.8 砷选择性检测..........................................................................................................4-5 4.8.1 发射波长.......................................................................................................4-5 4.8.2发射时间........................... ........... .................................4-6 4.8.3火焰组成............................. ........... ..................................4-6 4.8.4滤光片............................ ........... .................................4-6 4.9 硒选择性检测........................................................................................................4-7 4.9.1发射波长........................................................................................................4-7 4.9.2发射时间........................... ............................ ...............................................4-7 4.9.4火焰组成............................. ........... ..................................4-7 4.9.4滤光片............................ ........... .................................4-7 4.10 锡选择性检测..........................................................................................................4-8 4.10.1发射波长........................ ...................................... ......................................4-8 4.10.2发射时间........................... ........... .................................4-8 4.10.3火焰组成............................. ........... ..................................4-8 4.10.4滤光片............................ ........... .................................4-9 4.11 锰选择性检测..........................................................................................................4-9 4.11.1发射波长...................... ................................................................................4-9 4.11.2发射时间........................... ........... .................................4-10 4.11.4火焰组成............................. ........... ..................................4-10 4.11.4滤光片............................ ........... .................................4-10 第五部分 PFPD维护 ........................................................................................5-1 5.1 概述 ..........................................................................................................5-1 5.2 更换光学滤光片............................................................... ........... ................................5-1 5.3 更换燃烧室............................................................. ........... ................................5-3 5.4 换掉污染的燃烧室............................................................ ........... ................................5-3 5.5 定购PFPD的部件及消耗品.............................................. ........... ................................5-4 第六部分 故障排除 ........................................................................................6-1 6.1 概述 ..........................................................................................................6-1 6.1.1 不能点火.... .............................. ........... .................................6-2 6.1.2 基线噪声太高............................. ........... ..................................6-3 6.1.3 基线不稳定(TICK-TOCK).................................... .................................6-6
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