Bruker NMR advanced 中文使用手册（适合于初学者）

仪器资料 · 发表于 2017-8-26 20:25:25

目录
目录.................................................................................................................................................3
1 简介.............................................................................................................................................７
1.1 可能的损害.......................................................................................................................７
1.1.1 软件版本及命令语法...........................................................................................８
2 安全注意事项...............................................................................................................................9
2.1 简述.....................................................................................................................................9
2.2 关于磁性的安全注意事项................................................................................................9
2.2.1 内部区域安全注意事项...............................................................................................10
2.2.2 外部区域安全注意事项...............................................................................................11
2.3 关于深冷液体的安全注意事项......................................................................................11
2.4 关于电气的安全注意事项..............................................................................................11
2.5 关于化学的安全注意事项..............................................................................................11
2.6 关于CE认证.....................................................................................................................11
3 理论及术语说明.........................................................................................................................13
3.1 简介..................................................................................................................................13
3.2 氯仿的NMR分析.............................................................................................................15
3.3 标样，赫兹，ppm...........................................................................................................17
3.4 质子NMR——化学位移.................................................................................................18
3.5 苯的质子频谱...................................................................................................................19
3.6 乙酸苄酯（Benzylacetate）的质子频谱........................................................................20
3.7 带自旋/自旋耦合的乙基苯质子频谱.............................................................................21
3.8 去耦..................................................................................................................................23
3.9 FID和频谱........................................................................................................................24
4 系统介绍.....................................................................................................................................27
4.1 简介..................................................................................................................................27
4.2 操作控制台及其连接......................................................................................................27
4.3 机柜..................................................................................................................................28
4.4 主机与AQS间的连接......................................................................................................29
4.5 磁体、匀场系统、HPPR和探头....................................................................................29
4.6 磁体和磁体杜瓦..............................................................................................................31
4.6.1 室温腔管..............................................................................................................32
4.6.2 液氦腔..................................................................................................................32
4.6.3 液氮腔..................................................................................................................33
4.7 锁场系统简介..................................................................................................................33
4.8 探头..................................................................................................................................34
4.8.1 双模13C/1H探头...............................................................................................36
4.8.2 更换探头..............................................................................................................38
5 NMR样品....................................................................................................................................39
5.1 简介..................................................................................................................................39
5.2 溶剂选择..........................................................................................................................39
5.3 样品管..............................................................................................................................40
5.4 样品处理..........................................................................................................................41
6 实验基本步骤.............................................................................................................................43
6.1 简介..................................................................................................................................43
6.2 BSMS键盘........................................................................................................................43
6.2.1 保存一组匀场值（wsh命令）............................................................................44
6.2.2 读取一组匀场值（rsh命令） ............................................................................44
6.2.3 BSMS功能...........................................................................................................45
6.2.4 样品控制功能......................................................................................................45
6.2.5 手动锁场功能......................................................................................................45
6.2.6 手动匀场功能......................................................................................................46
6.2.7 液氦高度功能......................................................................................................46
6.3 将样品管插入转子..........................................................................................................47
6.4 将带样品管的转子放入磁体..........................................................................................47
6.5 旋转样品..........................................................................................................................48
6.6 调谐和匹配探头..............................................................................................................49
6.6.1 使用wobble曲线进行调谐和匹配.....................................................................49
6.6.2 使用HPPR LED进行调谐和匹配......................................................................51
6.6.3 对多个核进行调谐和匹配..................................................................................52
6.7 锁定样品..........................................................................................................................53
6.7.1 锁场步骤..............................................................................................................54
6.8 匀场..................................................................................................................................55
6.8.1 初始匀场..............................................................................................................56
6.8.2 常规匀场..............................................................................................................56
7 准备采样——数据集， edasp、eda命令.................................................................................59
7.1 简介..................................................................................................................................59
7.2 数据集..............................................................................................................................59
7.3 创建数据集......................................................................................................................61
7.4 谱仪参数edasp.................................................................................................................62
7.4.1 edasp窗口布局....................................................................................................63
7.4.2 edasp窗口的一些特性........................................................................................65
7.5 基本采样参数：“eda”表..............................................................................................65
7.5.1 发射、基础和偏移频率的数学解释..................................................................72
8 脉冲程序 / ased命令.................................................................................................................75
8.1 脉冲程序“zg”和“zg30” ............................................................................................75
8.2 “zg30”程序详解.............................................................................................................75
8.3 命令“ased”.....................................................................................................................77
9 氢谱.............................................................................................................................................79
9.1 前言..................................................................................................................................79
9.2 创建新数据集..................................................................................................................79
9.3 读取标准参数集..............................................................................................................80
9.3.1 “getprosol”表.....................................................................................................80
9.4 设置接收机增益..............................................................................................................80
9.5 进行采样..........................................................................................................................81
9.6 傅立叶变换和谱图相位校正..........................................................................................83
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9.7 基本处理：傅立叶变换..................................................................................................85
9.8 相位校正..........................................................................................................................85
9.9 谱图的校准......................................................................................................................87
9.9.1 水平放大图谱......................................................................................................88
9.9.2 图谱校准..............................................................................................................88
9.10 使用SW-SFO1 功能调整谱宽......................................................................................89
9.10.1 调整cholesterylacetate谱图的SW.................................................................89
9.11 增加扫描次数................................................................................................................90
10 不去耦的13C谱.......................................................................................................................93
10.1 简介................................................................................................................................93
10.2 步骤................................................................................................................................93
11 去耦氢的13C谱.......................................................................................................................97
11.1 简介................................................................................................................................97
11.2 详细步骤........................................................................................................................97
11.3 确定去耦频率................................................................................................................98
11.4 调整去耦参数................................................................................................................99
11.5 脉冲程序zgpg30 ............................................................................................................99
12 基本故障排除.........................................................................................................................103
12.1 简介..............................................................................................................................103
12.2 打开和关闭谱仪..........................................................................................................103
12.3 谱仪开机......................................................................................................................103
12.4 谱仪关机......................................................................................................................104
12.4.1 在Windows系统运行Topspin........................................................................104