NMR D-溶劑使用問題

NMR D-Solvent Usage:

When using a mixed solvent:

Please use manual shimming: z1, z2, x, y.

Sample Pre-treatment:

Samples should be prepared in suitable NMR tubes.

If there are any insoluble components in the sample, solid substances will affect field homogeneity and need to be filtered beforehand.

Use NMR-specific D-solvent for the sample.

Sample Preparation:

The sample solvent should be filled to a height of 4.0 cm (approximately 0.62 ml ~ 0.65 ml).

When the sample solvent is too little, field homogeneity is affected, which impacts peak shape and resolution.

When the sample solvent is too much, it becomes too heavy, affecting the performance of the pneumatic loader.

Excessive sample solvent dilutes the concentration, so be careful when filling the solvent.

When the solvent reaches a height of 3 cm, add slowly and in small amounts (drop by drop) until it reaches 4 cm.

For diluted samples, it's difficult to detect 13C because its natural abundance is only 1%.

The cost of 13C measurement depends on the duration of the measurement; the longer the measurement, the higher the cost, so if possible, prepare concentrated samples.

In the era of user payment, both self-testing and testing by others incur charges.

Because the fees cover the operating costs of the instrument (liquid helium, liquid nitrogen, electricity (instrument + compressed air), air conditioning, and maintenance).

Note:

All 400MHz NMR instruments (Agilent + Bruker) in the department charge by the hour, with longer logins incurring higher fees



NMR D-溶劑用途

(1)   D-solvent 是用來鎖定磁場，FT-NMR 一定得使用D-溶劑

(2)   D-solvent 是用來去除背景　

(3)   D-solvent 是用來勻場

(4)  D-solvent  是用來定標準


當使用mix-solvent 時

請使用manual shimming： z1,　z2,　x,　y


樣品前處理

樣品需配製在合宜的NMR管中

樣品若有其它不溶物，固體物會影響勻場效果，需要預先過濾

樣品需要使用 NMR 專用 D­-solvent

 

樣品配製

樣品溶劑請配 4.0 cm高 (約 0.62ml ~ 0.65ml)

樣品溶劑太少時，勻場差，影響峰型及解析度

樣品溶劑太多時太重，影響氣動裝置承載之效能

樣品溶劑太多時會稀釋濃度，所以填充溶劑時請用心填，

待溶劑達 3 cm高時， 需緩慢且少量 (一滴一滴)添加至  4 cm 高 

樣品稀時，13C不容易測出，因為它的自然豐率只有1% 

13C計價是以測定時間之長短而定，測的越久所支付費用越多，可以的話，儘量配濃


使用者付費之時代，使用者自測或找人代測都需要計費。

因為所付費用為儀器運作成本費(液氦、液氮、電費(儀器+壓縮空氣)、冷氣費及維修費)。

Note:

系上NMR 所有 400MHz NMR ( Agilent + Bruker ) 一律採按時收費，Log in 越久付費越多。