NMR數(shù)據(jù)處理流程

1、第一章 T1/T2實(shí)驗(yàn)數(shù)據(jù)處理1.1 前言樣品： T1/T2實(shí)驗(yàn)使用樣品為變壓器油，溶劑為CCl4,氘代標(biāo)準(zhǔn)樣品為TMS，幅度對比樣品為1,4-Dioxane(C4H8O2)。1.2 數(shù)據(jù)格式轉(zhuǎn)換1. 點(diǎn)擊主菜單 File/Open2. 找到原始NMR數(shù)據(jù)3.設(shè)置新數(shù)據(jù)文件名，實(shí)驗(yàn)序列號，主目錄，及用戶名4. 保存 File/Save 全點(diǎn)擊1.3 處理1選擇FID注意：步驟1 僅僅用來描述T2 實(shí)驗(yàn)為衰減函數(shù)。2 選擇ProcPars3 點(diǎn)擊顯示處理參數(shù)4 做出如下改變SI(F1) = 16PH_mod(F1) = noPH_mod(F2) = pk5 鍵入xf26 鍵入abs27 鍵入se

2、tdiffparm8 選擇Spectrum3.1.5 計(jì)算T2弛豫系數(shù)注意：如果采樣如下步驟，將會(huì)彈出具有重要介紹的信息窗口。請細(xì)細(xì)閱23讀介紹內(nèi)容。1 點(diǎn)擊主菜單的Analysis2 選擇T1/T2 Relaxation3點(diǎn)擊提取部分FID4點(diǎn)擊5鍵入16點(diǎn)擊7. 調(diào)相位8. 調(diào)基線7點(diǎn)擊定義范圍8點(diǎn)擊9點(diǎn)擊定義區(qū)域10利用鼠標(biāo)左鍵和光標(biāo)定義區(qū)域11點(diǎn)擊12點(diǎn)擊13選擇Export Region To Relaxation Module15在指南窗口中，點(diǎn)擊弛豫窗口16啟用Intensity17在指南窗口中，點(diǎn)擊擬合函數(shù)18點(diǎn)擊19在Fitting Function 部分，選擇uxnmrt2

3、 和vdlist20點(diǎn)擊21在指南窗口中，點(diǎn)擊開始計(jì)算22點(diǎn)擊23在數(shù)據(jù)窗口中，點(diǎn)擊計(jì)算所有數(shù)據(jù)點(diǎn)的擬合參數(shù)。注意：所有計(jì)算值顯示在數(shù)據(jù)窗口的簡介中。24在指南窗口中，點(diǎn)擊顯示報(bào)告。Dataset : C:BrukerTOPSPIN/data/pengsl/nmr/D20_T2/1/pdata/1INTENSITY fit : It= P*exp(-t/T2)16 points for Peak 1, Peak Point at 7.127 ppmResults Comp. 1 P = 9.441e-001T2 = 6.941sSD = 6.171e-002 tau ppm integral

4、intensity 2.000m 7.127 -1.6399e+006 1.324e+006 16.000m 7.127 -1.6347e+006 1.0845e+006 80.000m 7.127 -1.7485e+006 1.1653e+006 160.000m 7.127 -1.7617e+006 1.2251e+006 320.000m 7.127 -1.7016e+006 1.2774e+006 480.000m 7.127 -1.2727e+006 1.1777e+006 640.000m 7.127 -1.0013e+006 1.1873e+006 800.000m 7.127

5、-4.651e+005 1.2293e+006 960.000m 7.127 3.1215e+005 1.1478e+006 1.200s 7.127 7.9016e+005 1.0709e+006 1.480s 7.127 8.1055e+005 9.7672e+005 1.600s 7.127 8.6186e+005 9.0807e+005 2.000s 7.127 8.3397e+005 8.3684e+005 3.200s 7.127 7.5662e+005 7.71e+005 6.400s 7.127 6.2275e+005 6.306e+005 8.000s 7.127 58941

6、 3.1195e+00516 points for Peak 2, Peak Point at 1.270 ppmResults Comp. 1 P = 1.095e+000T2 = 1.411sSD = 8.582e-002 tau ppm integral intensity 2.000m 1.269 8.3123e+007 3.8776e+007 16.000m 1.269 8.1277e+007 3.8207e+007 80.000m 1.269 8.6909e+007 3.7916e+007 160.000m 1.269 8.9102e+007 3.7728e+007 320.000

7、m 1.269 9.412e+007 3.691e+007 480.000m 1.269 8.0176e+007 3.4291e+007 640.000m 1.269 7.2473e+007 3.3355e+007 800.000m 1.269 6.001e+007 2.9343e+007 960.000m 1.269 3.54e+007 2.1562e+007 1.200s 1.269 1.8724e+007 1.5121e+007 1.480s 1.269 1.2183e+007 1.1971e+007 1.600s 1.269 7.8246e+006 9.5146e+006 2.000s

8、 1.269 3.9297e+006 6.7795e+006 3.200s 1.269 9.0273e+005 3.8742e+006 6.400s 1.269 -1.3786e+005 2.2636e+006 8.000s 1.269 -4.4636e+005 1.9266e+00516 points for Peak 3, Peak Point at 0.883 ppmResults Comp. 1 P = 1.073e+000T2 = 1.770sSD = 8.594e-002 tau ppm integral intensity 2.000m 0.883 1.7282e+008 1.8

9、157e+007 16.000m 0.883 1.6741e+008 1.8552e+007 80.000m 0.883 1.5808e+008 1.8823e+007 160.000m 0.883 1.5379e+008 1.8855e+007 320.000m 0.883 1.348e+008 1.8835e+007 480.000m 0.884 1.2978e+008 1.7552e+007 640.000m 0.884 1.2009e+008 1.7105e+007 800.000m 0.884 1.0185e+008 1.5205e+007 960.000m 0.884 7.1128

10、e+007 1.1613e+007 1.200s 0.884 4.685e+007 8.8601e+006 1.480s 0.883 3.5891e+007 7.4629e+006 1.600s 0.883 2.7577e+007 6.3334e+006 2.000s 0.883 1.8885e+007 4.9117e+006 3.200s 0.883 1.0139e+007 3.174e+006 6.400s 0.883 5.6487e+006 2.1229e+006 8.000s 0.883 3.7839e+005 3.095e+005第二章 二維J-譜實(shí)驗(yàn)數(shù)據(jù)處理1.1 前言樣品： T1

11、/T2實(shí)驗(yàn)使用樣品為變壓器油，溶劑為CCl4,氘代標(biāo)準(zhǔn)樣品為TMS，幅度對比樣品為1,4-Dioxane(C4H8O2)。1.2 數(shù)據(jù)格式轉(zhuǎn)換1. 點(diǎn)擊主菜單 File/Open2. 找到原始NMR數(shù)據(jù)3.設(shè)置新數(shù)據(jù)文件名，實(shí)驗(yàn)序列號，主目錄，及用戶名4. 保存 File/Save 全點(diǎn)擊1.3 處理1選擇FID2 選擇ProcPars3 點(diǎn)擊顯示處理參數(shù)4 做出如下改變SI(F2) = 16kSI(F1) = 32PH_mod(F1) = mcPH_mod(F2) = pkWDW(F2) = SINEWDW(F1) = SINESSB(F2) 2SSB(F1) = 25 鍵入xfb6 鍵入a

12、bs28 選擇Spectrum20調(diào)整投影水平標(biāo)準(zhǔn)布魯克參數(shù)設(shè)置可以在使用AU 程序的條件下自動(dòng)進(jìn)行并優(yōu)化。在采樣(eda)和處理(edp)參數(shù)表中AU 程序的名字為AUNM。開始采樣使用xaua 命令。處理數(shù)據(jù)，鍵入xaup 命令4鍵入xaupAU 處理程序包含二維傅立葉變換，相位校正，基線校正和出圖。HMBC實(shí)驗(yàn)使用強(qiáng)度模式處理數(shù)據(jù)，因此只顯示正相關(guān)3.1.1 準(zhǔn)備實(shí)驗(yàn)1遵循基本實(shí)驗(yàn)用戶指南一維氫譜實(shí)驗(yàn)采集一維氫譜圖 3.12鍵入wrpa 23鍵入re 24拓展6ppm 到2ppm 間的圖譜5點(diǎn)擊，設(shè)置掃描寬度和O1 頻率圖 3.2186點(diǎn)擊7鍵入td 16k8鍵入si 8k9點(diǎn)擊zg 開

13、始采樣10鍵入ef11鍵入apk12鍵入abs圖 3.33.1.2 參數(shù)設(shè)置1鍵入iexpno2選擇AcquPars3點(diǎn)擊顯示脈沖序列參數(shù)4做出如下改動(dòng)PULPROG = stebpgp1s1dGPZ6% = 2GPZ% = -17.13D20s = 0.1P30us = 18005 鍵入rga6 鍵入zg7 加入ef8 鍵入apk9 鍵入abs19圖 3.410鍵入iexpno11選擇AcquPars12點(diǎn)擊顯示脈沖序列參數(shù)13做出如下改動(dòng)GPZ6% = 9514鍵入zg15鍵入ef16鍵入apk17鍵入abs圖 3.518點(diǎn)擊打開多重顯示窗口19拖動(dòng)前面實(shí)驗(yàn)到多重顯示窗口或鍵入re 320圖 3.6注意：兩個(gè)圖譜的強(qiáng)度差應(yīng)該在50 之間。如果差異小于50，改變P30 或D20值。3.1.3 采樣