最近NMR打出的谱本来单峰的变双峰（注匀场噪音不大，0.001以下），有时又是好的单峰，看不到分裂。同个样品也是这样。混合溶剂打时匀场匀速会自动变慢。用3%CDCl3于Acetone的标样计算机匀场的结果CDCl3是双峰，不知道什么原因，怎么消除。请各位大虾帮忙解决一下。还有一点不明的是计算机匀场老出现Spinning not OK:13Hz对话横框,不知道旋转不行是什么原因，13Hz是什么意思？
最近NMR打出的谱本来单峰的变双峰（注匀场噪音不大，0.001以下），有时又是好的单峰，看不到分裂。同个样品也是这样。混合溶剂打时匀场匀速会自动变慢。用3%CDCl3于Acetone的标样计算机匀场的结果CDCl3是双峰，不知道什么原因，怎么消除。请各位大虾帮忙解决一下。还有一点不明的是计算机匀场老出现Spinning not OK:13Hz对话横框,不知道旋转不行是什么原因，13Hz是什么意思？
* r- S/ H0 V6 L & u; A. b" t+ V; K3 Z$ R
It sounds like you had problem with sample spinning. The regular spinning rate for 5mm tube is 20Hz. Check your spinner first to see if it is dirty or damaged and try a new spinner if you have any. This problem might also be caused by a weak airflow or gas leakage. Check the air pressure inside the console first to see what pressure you had. It is usually set between 4 to 6 bar. Also check the hose connection to see if there is any air leak. You may want to run spin calibration if you know how to do it. The other possibilities could be broken glassware inside the probe or slcb board inside the BSMS is in trouble.
发表于 2009-2-19 23:30:07
