HMBC
Two-dimensional Heteronuclear Multiple Bond Correlation Spectroscopy
HMBC - ACQU
Insert the sample, lock the field, shim, and perform tuning and matching (atmm) for all relevant nuclei (carbon and hydrogen).
Measure the 90-degree pulse width for 1H.
Measure the 1D 1H spectrum -> For plotting, use it as a side plot for F2 projection (use 13C spectrum experiment for F1 projection).
Use either rpar bbfo_13C_hmbc or rpar bbfo_c13hmbcet (choose one to load) all.
getprosol for 1H (90pw) (pl).
Run rga.
Set ns to 16-64 (depending on concentration).
expt
Acquire zg.
Run the experiment again to check the required time(expt).
HMBC - PROC
Execute Fourier transform of both dimensions (xfb).
If there are no negative peaks, skip this step (xf2m: magnitude mode).
Calibration (choose an independent signal for calibration; correct F2 domain with 1H chemical shift; correct F1 domain with 13C chemical shift).
Perform baseline correction of both dimensions: abs2, abs1.
Enter edc2:
Data Set2 = (filename of 1H)
Data Set3 = (filename of 13C)
Select the printer icon, Layout: +2D_CH_ntu.xwp
Note: HMBCET has positive and negative phase differences; perform xfb first, then xf2m.
二維碳氫異核長距離化學位移相關光譜
HMBC – ACQU
1. 置入樣品,鎖場、勻場及 atmm 所有相關核種(碳及氫)
2. 量測1H之90度脈寬
3. 量測一維之1H譜 -> 製圖時,當側圖使用- for F2 projection (另外F1 projection 請用1 3C譜實驗)
4. rpar bbfo_13C_hmbc
或rpar bbfo_c13hmbcet (擇一讀入) all
5. getprosol 1h (90pw) (pl)
6. rga
7. ns 16~64 (視濃度而定)
8. expt
9. zg
10. expt (檢查實驗所需之時間)
HMBC - PROC
1. xfb (execute fourier transform of both dimensions)
2. xf2m (若沒有負峰, 跳過此步 , m : magnitude mode)
3. calibration ( 定標:擇一獨立訊號, F2 domain 以1H的化學位移訂正;F1 domain 以13C的化學位移訂正)
4. abs2, abs1 (baseline correction of both dimension : 2個維度的基線調整)
5. edc2
Data Set2 = ( filename of 1H )
Data Set3 = ( filename of 13C)
6. 選擇printer icon ,Layout:+2D_CH_ntu.xwp
註:HMBCET 有正負相位之別,xfb 後再 xf2m