NMR 測定マニュアル(改訂版）

Size: px

Start display at page:

Download "NMR 測定マニュアル(改訂版）"

ひろみおとじま
5 years ago
Views:

1 NMR Manual for NMR Caution When you enter the C-4007 room, you must not take any items, for examples magnetic cards, watches, portable phones and metal items. Don t enter the NMR room with your shoes on. 4 cm The height of samples is ca. 4 cm The spinner-rotor must not be dropped. (Its charge is yen) The bottom of a spinner-rotor is not touched with your bare hands. Whenever you set the sample in the spinner-rotor, you have to clarify the sample tube with kimwipes. NMR Whenever you set the sample in the NMR machine, you have to check that air is flowed. 50 Don t break your sample tube in the NMR machine. The fee for repair of it is 500 thousand yen. When you have some problems and troubles, you have to ask managers (Yoshimura). 1

2 You are responsible for taking NMR. ( ) NMR connect (fig. 1) The person who takes NMR at first on the day have to turn on the drier followed by the compressor and connect between the spectrometer and PC (fig. 1). (fig. 1) Connect icon No Current Link Spectrometer Control Connect No Current Link (fig. 2) spectrometer control You have to click Connect icon in the Stectrometer Control window and No Current Link icon turn to yellow as (fig. 2). (fig. 2) 2

(fig. 3) The person who go home at last on the day have to turn off the compressor followed by the drier and disconnect between the spectrometer and PC (fig. 3). (fig. 3) Free (fig.

3 (fig. 3) The person who go home at last on the day have to turn off the compressor followed by the drier and disconnect between the spectrometer and PC (fig. 3). (fig. 3) Free (fig. 1) After you click Free icon, connection between the spectrometer and PC is free and you can find the window as (fig. 1). NMR Next, methods (one-clicked) taking NMR is described. You set your sample on the magnet. Caution) You have to check that air is flowed!!!! Spectrometer control Auto (fig. 4) You click the Auto icon on the Spectrometer control window. (fig. 4) (fig. 4) sample icon Auto icon 3

4 Automation fig. 5 You can find the Automation window (fig. 5) (fig. 5) Automation window Proton icon 4

5 Filename Yoshimura/TY You have to write your name/sample name in the Filename box in English, for example Yoshimura/TY You must not use special letters and slash is only used between your name and sample name. Comment If you need to any comments in the spectrum, you write your comments in the Comment box. Slot You don t touch the Slot box. delta automation auto2 You have to select the method that you want to take NMR in the delta~automation auto2. Generally, you use the following methods, i) Proton 1D H-NMR ii) Carbon 13C 1D 13C-NMR decoupled complete iii) Carbon and Dept135 13C dept 135 1D 13C-NMR decoupled complete and dept135 iv) Edited DEPT 13C dept135 dept90 dept45 1D 13C-NMR decoupled complete, dept135, dept90 and dept45 v) Gradient COSY H-H COSY H-H COSY can be taken in a short time. vi) Gradient TOCSY TOCSY TOCSY can be taken in a short time. vii) Gradient HMQC C-H COSY C-H COSY can be taken in a short time. viii) Gradient HMBC C-H long range C-H long range can be taken in a short time. ix) Gradient PS NOESY NOESY 2D n.o.e. can be taken in a short time. 5

6 H NMR case 1. H-NMR Proton fig. 5 You click the Proton icon. (see fig. 5) Set parameters for Proton fig. 6 You can find the Set Parameters for Proton window. (see fig. 6) i) Parameter box Select the solvent Run with Changes fig. 6 6

7 solvent (fig. 6) You have to select the solvent from the Solvent. MeOH DMF THF EtOH Gradient SIM option Gradient Shim Caution) When you use as solvents, which is deuterized MeOH, toluene, DMF, pyridine, THF, EtOH, glyme and nitrobenzene, you have to select Gradient Shim in Option and delete the check mark. Parameter box fig. 6 You can change some parameters in Parameter box (fig. 6) List of parameters in Parameter box i) auto gain Don t change ii) force tune When you change solvents and nuclei, you have to change iii) spin state (Don t change) iv) scans You can change. v) relaxtime delay (Don t change) vi) process (Don t change) vii) process copy (Don t change) viii) automatic (Don t change) ix) X offset You can change 7

8 x) X sweep You can change X offset X sweep X offset and X sweep are changed when you want to change the range of irradiation pulse. 13C sn-ratio In 13C NMR Parameter box has these parameters and sn-ratio. You have to write 0 in the sn-ratio NMR sample Autoshim When you take 2 D NMRs, you have to be free Autoshim placed in sample window. Run with Changes Go (fig. 6) After you click the Run with Change icon, you can find another window including Go icon. You have to click it immediately. NMR is running automatically from loading sample to saving datum. (How to open the files) delta Processors Process 1D (fig. 7) You have to select the Process 1D from Processors in the delta window.(see fig. 7) 8

9 (fig. 7) open file (fig. 8) You have to click the open file icon and you select your datum that you have to process.(fig. 8) (fig. 8) open file icon 1H icon Process icon 9

10 You have to process the Fourier transformation. ( ) i) 1H Process After you click the 1H icon, you have to click the Process icon. ii) 13C 13C Process In 13C case after you click the 13C icon, you have to click the Process icon. Spectrometer control (fig. 4) sample sample eject (fig. 10) After you finish to analyze your data, you eject your sample by clicking eject icon located in Sample window, which can be opened by clicking sample icon in Spectrometer control. (fig. 10) eject icon 10

11 delta sample Spectrometer control Finally, you have to close except for delta, sample and Spectrometer control 1 1 You have to save your data at your own file. If you save other folder, these data are deleted monthly. FID ( ) You should save your data in FID files. CD-R You have to save your own data in your CD-Rs. 11

GP05取説.indb

GP05取説.indb E -G V P 05D L V E -G P 05D W Ni-MH + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + + 1 + 2 + 3 + 4 + 5 + 6 1 2 3 4 5 6 + + + 1 + + + + + + + + + + + + + + + + + + 1 A B C + D + E