Triple TOF 5600 基础，使用入门与维护 胡浩咏 2013年11月

内容 仪器概况与工作过程 仪器使用入门 仪器各部分的维护周期与方法

仪器概况与工作过程

AB SCIEX TripleTOF™ 5600+ 仪器外观

AB SCIEX TripleTOF™ 5600+ 离子通道 离子源 QJet Q1质量分析器 加速器 Q0 检测器 Curtain Plate 1 Torr 10-3 Torr 10-5 Torr Q2 碰撞室 760 Torr Orifice Plate 飞行管 10-7 Torr 双层离子反射镜 5

四极杆工作原理——离子飞行轨迹

四极杆工作原理——离子聚焦 B A B A = ions End View B A RF 180° phase shift B A B A = ions RF only-A rods & B rods are 180 out of phase 180° phase shift RF End View RF For general presentation- Animation can be turned off. 1. Ions are attracted to a “B” pole. 2. RF voltage reversed, all ions attracted to an ‘A’ pole. 3. RF voltage reversed, all ions attracted to other ‘B’ pole. 4. RF voltage reversed, all ions attracted to other ‘A’ pole. Q0, Q2 & Stubbies always RF only. Q3 RF only if selecting in Q1. Q1 RF only if selecting in Q3 RF 180° phase shift

四极杆工作原理

四极杆工作原理

离子轴向飞行的动力——LENS电压

TOF 原理

TOF 原理——离子反射镜 However, a better way to reduce the effect of spatial spread is by using an Ion Mirror. The ion motion begins as before, with the corresponding time focusing in the focal plane. After the focal plane, ions start to depart again until they enter the Ion Mirror. The Ion Mirror is a relatively large gap with a homogeneous repelling electric field . More energetic ions get deeper into the mirror and therefore stay longer in it. In other senses the Ion Mirror works as a usual mirror: ions are reflected from it, and continue their motion in the opposite direction. If all parameters are adjusted properly, time focusing will happen again at the detector, and ions will hit the detector simultaneously. The technique was invented in Russia in the late 60’s by Mamyrin. Due to the wide use of Ion Mirrors in TOFs today, Mamyrin will receive this year’s ASMS award for Distringuished Contributiont in Mass Spectrometry. With Mirrors, mass resolution increased from a few hundeds to many thousands.

TOF 原理——直角注入 This is a simplified scheme of TOF with orthogonal injection. Ions enter the extraction region slowly and orthogonally to the TOF axis. When the extraction region is filled with ions, a voltage pulse is applied to the Pusher plate. Ions are accelerated into the drift space towards the Ion Mirror. The rest of the trajectory is the same as before: ions are reflected in the Mirror, travel through the second leg of the drift space and are recorded at the detector. While the first portion of ions is being recorded, the next portion is entering and filling the extraction region Ions fill the extraction region and are then pushed (accelerated) into the TOF

ESI工作原理 Liquid sample from LC is vaporized by nebulizer gas High voltage applied to spray tip creates charged droplets Desolvation of charged droplets leads to creation of ions

TOF with Orthogonal Injection This is a simplified scheme of TOF with orthogonal injection. Ions enter the extraction region slowly and orthogonally to the TOF axis. When the extraction region is filled with ions, a voltage pulse is applied to the Pusher plate. Ions are accelerated into the drift space towards the Ion Mirror. The rest of the trajectory is the same as before: ions are reflected in the Mirror, travel through the second leg of the drift space and are recorded at the detector. While the first portion of ions is being recorded, the next portion is entering and filling the extraction region Ions fill the extraction region and are then pushed (accelerated) into the TOF

APCI（又名Heated Nebulizer ）工作原理 Reaction with analyte molecules Corona Discharge Needle (NC) Ionization of solvent molecules Orifice (DP) Mass Analyzer X = Solvent Molecule M = Analyte Curtain Gas (CUR) Vacuum Atmospheric Pressure LC Flow Formation of clusters Heated Nebulizer (TEM) Nebulizing Gas (GS1) APCI is a three step ionization process: Corona Discharge needle charges N2 or O2 in the source N2 or O2 pass charge to vaporized solvent Charged and vaporized solvent passes charge to analyte

仪器使用入门

仪器外部 一 CDS(calibrant delivery system) 校正液输送系统 DuoSprayTM 离子源：ESI和 APCI整合离子源 Syringe Pump: 注射泵 状态灯

仪器外部 二 TDC 卡连接口：数据采集 USB连接口：连接USB-GPIB卡， 仪器通讯控制。 RS232连接口：控制注射泵

仪器外部 三 机械泵真空管接口 CDS控制接口 LC同步接口 （保留） 离子源接口（部分离子源） CURTAIN GAS 供气口 GAS1/ GAS2供气口 EXHAUST GAS供气口 CAD供气口 离子源废气排出口

仪器外部 四 仪器电源开关：用于仪器 开关机。 带盖断路器：分子泵的磁 悬浮电路供电（分子泵完 全停止前，一直打开）。 电源线插头。仪器主机供 电（分子泵完全停止前， 不能拔出） 。

仪器状态灯

CDS状态灯

TIS APCI DuoSpray

Turbo V Probes

注射泵 一 注射器的活塞 基座释放按钮：按压此按扭， 可上下调节基座的位置

注射泵 二 保护钮：压按该钮，注射泵 停止运行； 保护柱：注射器内溶液接近 推完，保护柱刚好压到保护 钮，保护注射器和注射泵不 会损坏； 保护杆固定螺丝：调节和固 定保护杆。

仪器供气 GAS1/ GAS2: 零级空气或高纯氮气，105 psi； CURTAIN GAS: 高纯氮气， 60 psi； CAD GAS: 高纯氮气， 60 psi； EXHAUST GAS：零级空气，无油空气或高纯氮气，55 – 105 psi;

仪器关机一般顺序 停止LC或注射泵的流速； 停止正在进行的扫描，deactivate硬件profile； 关闭仪器电源开关 关闭机械泵 等待至少15分钟，至真空舱内气压回复至大气压

仪器开机一般顺序 打开机械泵电源 确认带盖断路器处于打开状态； 15分钟后，打开仪器电源开关； 仪器真空度同时满足以下条件时，真空状态灯停止闪动 Q1 VACUUM GAUGE: 小于2*10-5 TORR TOF VACUUM GAUGE: 小于2*10-6 TORR 继续等待直至真空度稳定；

仪器各部分的维护周期与方法

仪器维护项目及周期

离子源的清洁——喷雾针与内腔 周期：建议每周一次 方法：用无尘纸蘸溶剂清洁 按以下溶剂按顺序清洁 1、甲醇 – 水（50：50） 2、甲醇

Curtain Plate 和 Orifice的清洁 周期：建议每周一次 方法：用无尘纸蘸溶剂清洁 按以下溶剂按顺序清洁 1、甲醇 – 水（50：50） 2、甲醇

QJET的清洁 周期：当需要时 现象：用Tuning solution检查，信号明显下降，分辨率明显变差，且优化参数不能恢复到正常状态 方法：泡沫棒蘸溶剂清洁 按以下溶剂按顺序清洁 1、甲醇 – 水（50：50） 2、甲醇

QJET的清洁 周期：当需要时 现象：用Tuning solution检查，信号明显下降，分辨率明显变差，且优化参数不能恢复到正常状态 方法：泡沫棒蘸溶剂清洁 按以下溶剂按顺序清洁 1、甲醇 – 水（50：50） 2、甲醇

机械泵油的更换 周期：6-12个月 操作： 1、关质谱主机和关机机械泵电源 2、等待30分钟以上 3、拧开泵油入口 4、专用的六角扳手打开泵油出口，废油完全放空。 5、加入新油至刻度（加入量约2升）

Questions and Answers

仪器的扫描模式

扫描模式 – Q1 MS Q1 MS Used to tune and calibrate Q1 TOF in DC mode

扫描模式 – TOF MS TOF MS Similar to a Q1 scan on a triple quad instrument Used to obtain molecular weight information

扫描模式 – Product Ion Product Ion Q1 filters a precursor m/z Precursors are fragmented in Q2 Fragments (products) are analyzed in the TOF Used for structural information gathering and identification of product ions

Product Ion

Product Ion

扫描模式 – Precursor Ion Precursor Ion Q1 sweeps a given mass range Computer looks at fixed product m/z in TOF Used to determine the “origin” of particular product

Precursor Ion

Questions and Answers