Noesy / Roesy
NOESY / ROESY (二維同核空間相關光譜)
( Nuclear Overhauser Effect SpectroscopY)
1H - ACQU
Mount the sample, a 4.0 cm high solution, on a spinner. Wipe the lower part of the glass sample tube with a tissue. Use a gauge to measure the depth where the sample should be placed (BBFO = 2.0 cm).
Use Lift to send air to the middle of the Magnet above. Slowly insert the sample with the mounted spinner into the probe inside the Magnet.
Enter (filename), (expno) for edc.
Use rpar bbfo_1h.
getprosol
Lock (lock according to the solvent used).
Perform tuning and matching manually (atmm)(This step is VIP).
Perform topshim (shimming).
Perform shim x, y (shimming up to quadratic is sufficient). You can revisit topshim once more.
Run receiver gain adjust (rga).
Set ns to 16-80.
Acquire zg (get a 1H spectrum, used as a side plot for 2D).
NOESY / ROESY - ACQU
Edit the other expno for edc.
Use either rpar bbfo_1h_roesy or rpar bbfo_noesy.
getprosol for 1H (pw) (pl).
Set ns to 4-8.
Set rg = (rg of 1H) /5.
Set ds to 32.
Acquire zg.
Run the experiment (set experiment time).
NOESY / ROESY - PROC
Execute Fourier transform of both dimensions (xfb).
Phase adjustment:
First adjust row, then adjust column.
Enter phase adjustment mode.
Along the middle and bottom of the diagonal line, select three peaks each (using add).
Then select R mode (row) and adjust the phase of these three peaks to negative, similar to one-dimensional phase adjustment method.
Then adjust C mode (column) using the same method.
Perform baseline correction of both dimensions (abs2D) (abs2, abs1).
Calibration (F1 domain and F2 domain):
Identify specific chemical shifts on the diagonal line (e.g., solvent peaks) for calibration.
Set nlev to 36-48 (number of contour levels).
Projection Placement
Method (1): edc2
Fill in both left and right columns with relevant information of the 1H file (e.g., expno, procno, hard disk, directory, etc.).
Run rep 1 to update the screen.
Method (2): Move the cursor to the frame of Projection above the 2D, right-click (first key), select External Projection, fill in the relevant information of the 1H file (e.g., Name, expno, procno, directory), then move the cursor to the frame of Projection on the left side of 2D, and follow the procedure.
NOESY / ROESY - PLOT
Choose PLOT.
Select Layout, 2D_hom.xwp.
Select Export from Menu three, save as .pdf.
NOESY / ROESY (二維同核空間相關光譜)
( Nuclear Overhauser Effect SpectroscopY)
1H - ACQU
1. 將 4.0cm高溶液的樣品套上轉子(spinner) 用紙巾擦拭玻璃樣品
管下半部, 用gauge量好樣品應置放之深度 (BBFO = 2.0 cm)
2. 按Lift 將空氣送達Magnet上方中, 將套好轉子的樣品緩緩送入
Magnet內的探頭中 ,
3. edc 鍵入 (filename) , (expno)
4. rpar bbfo_1h
5. getprosol
6. lock (依據使用的溶劑鎖場)
7. atmm ( tuning and matching - 手動調諧) (This step is VIP)
8. topshim (勻場)
9. 再加 shim x, y, ( 二次方以下都能勻), 可再回頭topshim 一次
10. rga (receiver gain adjust)
11. ns 16~ 80
12. zg (get a 1H spectrum - 當二維之側圖用)
NOESY / ROESY- ACQU
13. edc (edit the other expno)
14. rpar bbfo_1h_roesy , 或 rpar bbfo_noesy
15. getprosol 1H (pw) (pl)
16. ns 4~8
17. rg = ( rg of 1H) /5
18. ds 32
19. zg
20. expt (實驗時間)
NOESY / ROESY - PROC
21. xfb ( 執行二維的傅立葉轉換)
22. Phase
先調整row, 再調整column
首先進入相位調整模式，
沿著對角線上中下的位置，
分別各選三個峰（用add），
再選擇 R mode (row)，
類似一維相位調整法把這三個峰的相位都調成負相，
然後以同樣手法去調整 C mode (column)
23. abs2D (2 個維度之基線調整, abs2, abs1)
24. calibration (F1 domain 及F2 domain)
(在 對角線上找出特定化學位移 例如溶劑峰 加以標定)
25. nlev 36~48 (number of contour level 圈數)
安置側圖法 (Projection placement )
方法 (一) edc2
(表格左右欄都填入 1H 檔案相關訊息; 如 expno, procno, hard disk, directory 等)
rep 1 (re procno 1 ，可將螢幕更新)
方法 (二) 將游標移到 2D上方的 Projection 的框架內，按下右鍵（第一鍵），選擇External Projection，
填入 1H 檔案相關訊息; 如 Name, expno, procno, directory ，將游標移到 2D 左方的 Projection 的框架內，
依法泡製
NOESY / ROESY - PLOT
挑選 PLOT
挑選 Layout , 2D_hom.xwp
挑選 Menu 三 的 Export , 存成 .pdf