《GCMS基础理论》PPT课件.ppt

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1、Slide title:Font:Myriad or Arial,36ptSub title(Author):Font:Myriad or Arial,18ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings.GCMSGCMS基础知识基础知识Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSub

2、head:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsGCMS的基本流路的基本流路图图GC接口MS数据处理真空系统Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptT

3、ext:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings气相色谱仪的流动相气相色谱仪的流动相-载气载气l高纯氦气（纯度高纯氦气（纯度99.999%99.999%以上）以上）Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial

4、28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsMSMSMSMS流程图流程图流程图流程图样品进样系统离子源真空系统质量分析器检测器数据处理GC进样进样 直接进样直接进样Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:Myriad

5、orArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings为什麽为什麽为什麽为什麽MSMSMSMS需要高真空需要高真空需要高真空需要高真空v提供足够的平均自由程提供足够的平均自由程v提供无碰撞的离子轨道提供无碰撞的离子轨道v减少离子减少离子-分子反应分子反应v减少背景干扰减少背景干扰v延长灯丝寿命延长灯丝寿命v消除放电消除放电v增加灵敏度增加灵敏度Headlin

6、eforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings真空系统确保离子由离子源转移至检测器真空系统确保离子由离子源转移至检测器+ionair,water etc.高真空低真空

7、为什麽为什麽为什麽为什麽MSMSMSMS需要高真空需要高真空需要高真空需要高真空Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings 压力压力 10 10-3

8、-3-10-10-4 4 Pa(Pa(平均自由路径平均自由路径 5m-50m)5m-50m)排气系统排气系统Ion sourceLens systemRod systemDetector主泵副泵Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Character

9、s should not be overlapped on global strings真空泵真空泵(主泵主泵)涡轮分子泵（Turbo molecular pump）旋转叶片使气体分子向下移动并 由 出口排出干净真空启动和关机时间短价格昂贵Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on th

10、e text length.Characters should not be overlapped on global strings 单泵排气系统和差动排气系统单泵排气系统和差动排气系统 l差动排气系统更有利于高流量分析差动排气系统更有利于高流量分析单泵排气系统差动排气系统高真空Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adj

11、usted depending on the text length.Characters should not be overlapped on global stringslInterface:GC 和和 MS的连接部件的连接部件接口色谱柱MS高真空使用石墨垫圈 密封（85%Vespel+15%石墨）加热块接口接口Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont si

12、ze:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsMS MS MS MS 的分类的分类的分类的分类v磁质谱v四极杆质谱v飞行时间质谱(TOF)v离子肼质谱Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont siz

13、e:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings四极杆质量分析器四极杆质量分析器Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on

14、the text length.Characters should not be overlapped on global stringsm1+m2+m3+m1+m1/z=kV1m2/z=kV2m3/z=KV3m2+m3+11m/zVm：mass numberz：charge(=1 in GCMS)k：constant V:voltage applied to QP四极杆质量分析器四极杆质量分析器Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:Myriad

15、orArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsQP/MSQP/MSQP/MSQP/MS的结构的结构的结构的结构 离子源透镜四极杆检测器气质联用使用的电离技术 电子轰击电离（EI）正化学电离（PCI）负化学电离（NCI）Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-line

16、s:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings电子轰击电离（电子轰击电离（EIEI）e-e-e-e-e-样品分子样品分子灯丝灯丝+碎片离子碎片离子QP电子轰击电离（电子轰击电离（EIEI）l热电子（子（7070eVeV）轰击分子，使其分子，使其电离离l丰富的碎片离子丰富的碎片离子=丰富

17、的丰富的结构信息构信息 “指指纹”俵e-Mm1m3m2EI spectrum硬酯酸甲酯 M.W.298Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings反应

18、气反应气灯丝灯丝e-e-e-e-e-QPCH4 CH5+C2H5+样品分子样品分子H+-CH4M+1-C2H4正化学电离（正化学电离（PCIPCI）正化学电离（正化学电离（PCIPCI）l首先首先电离反离反应气分子气分子样品分子主要品分子主要 由由质子子转移移电离离l容易容易产生准分子离子生准分子离子用于确定分子量用于确定分子量 +CH4eMC2H5MH+C2H4PCI spectrum硬酯酸甲酯 M.W.298Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhea

19、d:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings EIEIEIEIEIEI和和和和和和 PCI PCI PCI PCI PCI PCI的比较的比较的比较的比较的比较的比较EI 模式模式PCI 模式模式碎片碎片 分子量分子量Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseo

20、ftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings负化学电离负化学电离负化学电离负化学电离(NCI)NCI)NCI)NCI)灯丝灯丝e-e-e-e-反应气反应气样品样品 样品样品捕获电子形成负离子 lMX+e(015eV)-MX X:电负性强元素电负性强元素CH4e MX

21、MXCH4+CH3+HCH4CH4CH4e MXMX_ _负化学电离负化学电离(NCI)NCI)Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringslNCI

22、NCI 质谱图六氯苯 M.W.284负化学电离(NCI)Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsNCI NCI NCI NCI 的优点的优点的优点

23、的优点适合分析电负性强的元素 l高灵敏度高灵敏度 与与 GC-ECD灵敏度相当灵敏度相当l高选择性高选择性Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings

24、EIPCINCIMarthone(MW330)EI PCI NCI 的比较的比较Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings NCI-GC/MS 和和

25、 GC-ECD定量结果的比较定量结果的比较重量 5g萃取(丙酮/水=5/2)蒸发(除去丙酮)加盐正己烷萃取蒸发色谱柱蒸发并定容 (5mL)按 JP方法进行前处理KOUJIN中有机氯农药的定量结果（ppm）Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Char

26、acters should not be overlapped on global strings面积的重现性面积的重现性 Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on globa

27、l strings离子源结构离子源结构离子源结构离子源结构v电离室电离室v透镜透镜Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings电离室电离室v永久磁铁v

28、灯丝v靶v电子聚焦离子化过程：样品分子与电子相互作用，电子把能量给予样品。如果这个能量足够大，则化合物被活化，失去一个电子，产生一个正离子，我们称之为分子离子。电子的能量通常为70ev。如果样品分子离子含有剩余的能量，会导致离子进一步断裂，形成碎片，剩余的能量越多，生成的碎片越多。形成的中性碎片被真空泵抽走，负离子撞击到离子源的其他部件上。Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial

29、20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings透镜透镜透镜透镜v排斥极：排斥极：使带正电荷的离子碎片向质量分析器方向运动。排斥极位于离子化室使带正电荷的离子碎片向质量分析器方向运动。排斥极位于离子化室出口对面；它的极性与离子相同。排斥极帮助离子穿过透镜。出口对面；它的极性与离子相同。排斥极帮助离子穿过透镜。v拉出极：拉出极：帮助带正电荷的离子碎片向质量分析器方向运动。拉出极的电压比排帮助带正电荷的离子碎片向

30、质量分析器方向运动。拉出极的电压比排斥极负，吸引正电子向质量分析器方向运动。拉出极是一个中心带有小孔的圆片。斥极负，吸引正电子向质量分析器方向运动。拉出极是一个中心带有小孔的圆片。v离子聚焦：离子聚焦：如果没有其他部件，离子穿过拉出极后会发生散射，离子聚焦部如果没有其他部件，离子穿过拉出极后会发生散射，离子聚焦部件可以帮助离子成束状进入质量分析器。离子聚焦带负电，形成一个电场，即使件可以帮助离子成束状进入质量分析器。离子聚焦带负电，形成一个电场，即使离子聚成束，又防止聚焦部件捕获电子。离子聚成束，又防止聚焦部件捕获电子。v入口透镜：入口透镜：位置紧挨四极杆，作用是使离子加速，并且抑制四极杆的边

31、缘效位置紧挨四极杆，作用是使离子加速，并且抑制四极杆的边缘效应，防止离子外溢。应，防止离子外溢。Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings离子检测器

32、离子检测器电子倍增器：从质量分析器出来的离子轰击电子倍增管的阴极表面，使其发射出二次电子，再由二次电子依次轰击一系列电极，使二次电子获得不断倍增，最后由阳极接受电流，使离子束信号得到放大。Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters s

33、hould not be overlapped on global stringsMSMSMSMS调谐调谐调谐调谐v灵敏度调节灵敏度调节v分辨率调节分辨率调节v质量数修正质量数修正v相对强度修正相对强度修正Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Cha

34、racters should not be overlapped on global stringsMS MS MS MS MS MS 调谐标样调谐标样调谐标样调谐标样调谐标样调谐标样PFTBA(全氟三丁胺)稳定可挥发碎片涵盖质量范围宽仅有C-13和N-15同位素无质量缺陷Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjuste

35、d depending on the text length.Characters should not be overlapped on global stringsPFTBAPFTBAPFTBAPFTBAPFTBAPFTBA relative m/z intensity 69 100.0131 26.0219 32.0414 2.0502 2.0614 0.2CF3-CF2-CF2-CF2-N-C4F9 C4F9Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubh

36、ead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsMSMSMSMS自动调谐流程自动调谐流程自动调谐流程自动调谐流程v寻找质量峰v粗调EM电压和峰宽v调节离子源部件使502达到最佳v调节EM和峰宽达到最佳v质量轴校正Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftw

37、o-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsGC-MSGC-MSGC-MSGC-MS常用术语常用术语常用术语常用术语基峰：179分子离子：304质荷比（m/z)质谱图（棒图）Headlineforslide:Incaseofone-line:MyriadorArial32

38、ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsGC-MSGC-MSGC-MSGC-MS常用术语常用术语常用术语常用术语总离子流图（TIC)TIC和MC（质量色谱图）Headlineforslide:Incaseofone-line:MyriadorA

39、rial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsGC-MSGC-MSGC-MSGC-MS常用术语常用术语常用术语常用术语总离子流图（TIC)Headlineforslide:Incaseofone-line:MyriadorArial32p

40、tIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings数据采集模式数据采集模式数据采集模式数据采集模式vScan（扫描）扫描）vSIM(选择离子选择离子)mass numbermass numberTimeTimeScanSIM(定性定性定性定性)(定量定量定

41、量定量)Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsScan Scan Scan Scan 模式（定性）模式（定性）模式（定性）模式（定性）m/zRe

42、tention timeTIC:Scan 7254152MS 质谱图质谱图Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsSIM SIM SIM SIM

43、模式（定量）模式（定量）模式（定量）模式（定量）Retention timem/z=72 m/z=152 m/z=54灵敏度高于灵敏度高于 Scan模式模式Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be ove

44、rlapped on global stringsSIM(选择离子模式）选择离子模式）lSIM主要用于定量分析主要用于定量分析l只有特定质量数的离子被检测只有特定质量数的离子被检测l根据目标化合物选择合适的检测离子相当重要。l灵敏度取决于所选择的检测离子。TimeVm/z0.2secV112VVVSIM数据采集模式数据采集模式Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFon

45、t size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global stringsSIM SIM SIM SIM 模式（定量）模式（定量）模式（定量）模式（定量）SIM的优点：的优点：l提高灵敏度提高灵敏度l改善峰形改善峰形l改善精确度改善精确度应用应用l痕量分析痕量分析l复杂基质复杂基质l常规定量常规定量Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:Myriado

46、rArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings 原子质量和质量数原子质量和质量数l以以12C 质量质量12为单位来表示原子质量为单位来表示原子质量l质量数质量数:整数表示整数表示example mass mass number1H 1.00782522 12H 2.01410222 212C 12.00

47、000000 1213C 13.00335508 1314N 14.00307440 1416O 15.99491502 1618O 17.99915996 18示例:水的质量数(H2O)1x2+16=18更精确的分子量1.00782522x2+15.99491502=18.01056546Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can b

48、e adjusted depending on the text length.Characters should not be overlapped on global strings 分析方法分析方法 计算方法算方法方法的建立方法的建立Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSubhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on th

49、e text length.Characters should not be overlapped on global strings分析方法（仪器参数）分析方法（仪器参数）l分析参数分析参数选择分析系分析系统:进样方式、色方式、色谱柱柱等等GC参数参数:载气流量、分流比、温度条件气流量、分流比、温度条件等等MS参数参数:扫描模式：扫描模式：SCAN,SIM 离子源：离子源：EI,PCI,NCI 检测器电压等检测器电压等Headlineforslide:Incaseofone-line:MyriadorArial32ptIncaseoftwo-lines:MyriadorArial28ptSu

50、bhead:MyriadorArial28ptText:MyriadorArial20ptFont size:Sizes can be adjusted depending on the text length.Characters should not be overlapped on global strings进样口、色口、色谱柱、柱、检测器的温度器的温度设定定l进样口温度进样口温度考虑样品中各组分的沸点，设定温度使样品瞬间汽化。考虑样品中各组分的沸点，设定温度使样品瞬间汽化。l色谱柱温度色谱柱温度考虑样品中各组分的沸点，及希望的分析周期，考虑样品中各组分的沸点，及希望的分析周期，宽沸程