COSY H-H
H-H COSY (二維同核相關光譜)
(Homonuclear COrrelation SpectroscopY)
1H - ACQU
1. Place the sample with a height of 4.0 cm into the spinner, wipe the lower part of the glass sample tube with a paper towel, and measure the
depth where the sample should be placed using a gauge (BBFO = 2.0 cm).
2. Press Lift to send air to the top of the Magnet, then slowly insert the sample attached to the spinner into the probe inside the Magnet.
3. edc Enter (filename) , (expno)
4. rpar bbfo_1h
5. getprosol
6. lock (Lock according to the solvent being used )
7. atmm ( tuning and matching - manually )
8. topshim (shimming )
9. Further adjust shimming in the x, y
10. rga (receiver gain adjust)
11. ns 16
12. zg (get a 1H spectrum - for use as a side plot in two-dimensional experiments )
COSY- ACQU
13. edc (edit the other expno)
14. rpar bbfo_1h_cosy , or rpar bbfo_cosy
15. getprosol
16. p0= (p1/2), (p1=90 pulse width , p0 =45 pulse width)
17. ns 4
18. rga
19. zg
20. expt (experiment time )
COSY - PROC
21. xfb ( Execute the two-dimensional Fourier transformation )
22. sym ( Perform symmetry correction.Both dimensions represent the same type of nucleus. )
23. abs2D (Conduct baseline correction in both dimensions , abs2, abs1)
24. calibration (F1 domain and F2 domain)
(identifying specific chemical shifts, such as those of solvent peaks, along the diagonal and using them as reference points. )
25. nlev (24 ~ 48) (number of contour levels ) , levcalc ,
edlev (edit level) , Choose positive and level increment to values such as 1.3 to 2.2.
Then, press "Fill" and "Apply"
安置側圖法 (Projection placement )
Method (一) edc2
(Fill in the table with 1H file-related information, such as expno, procno, hard disk, directory, etc.)
Use "rep 1" to repeat the process. (re procno 1 can update the screen).
Method (二)
Move the cursor to the frame above the 2D Projection.
Right-click (first button), choose External Projection.
Fill in the 1H file-related information, such as Name, expno, procno, directory.
Move the cursor to the frame on the left side of the 2D Projection and proceed accordingly.
COSY - PLOT
Select "PLOT"
Choose "Layout".
Select "Export" from Menu 3, then save as .pdf.
Note: Commands are indicated in blue, while actions are indicated in red.
H-H COSY (二維同核相關光譜)
(Homonuclear COrrelation 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)
8. topshim (勻場)
9. 再加 shim x, y
10. rga (receiver gain adjust)
11. ns 16
12. zg (get a 1H spectrum - 當二維之側圖用)
COSY- ACQU
13. edc (edit the other expno)
14. rpar bbfo_1h_cosy , 或 rpar bbfo_cosy
15. getprosol
16. p0= (p1/2), (p1=90 pulse width , p0 =45 pulse width)
17. ns 4
18. rga
19. zg
20. expt (實驗時間)
COSY - PROC
21. xfb ( 執行二維的傅立葉轉換)
22. sym ( 進行對稱化, 二維都是相同核種)
23. abs2D (2個維度之基線調整, abs2, abs1)
24. calibration (F1 domain 及F2 domain)
(於對角線上找出特定化學位移例如溶劑加以標定)
25. nlev (24 ~ 48) (contour level 圈數) , levcalc ,
edlev (edit level) , 選擇 positive , level increment 可設 1.3 ~ 2.2
再按 Fill, Apply
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
COSY - PLOT
挑選 PLOT
挑選 Layout ,
挑選 Menu 三 的 Export , 存成 .pdf
註: 藍色字表指令 紅色字表按鍵