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NMR Solvent

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showtheirdegreeofvariability.Occasionally,inorder

todistinguishbetweenpeakswhoseassignmentwasambiguous,afurther1-2μLofaspecificsubstratewere

addedandthespectrarun

again.Table1.1HNMRData

protonmultCDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3ODD2O

solventresidualpeak7.262.052.507.161.943.314.79

H2Os1.562.84a3.33a0.402.134.87

aceticacidCH3s2.101.961.911.551.961.992.08

acetoneCH3s2.172.092.091.552.082.152.22

acetonitrileCH3s2.102.052.071.551.962.032.06

benzeneCHs7.367.367.377.157.377.33

tert-butylalcoholCH3s1.281.181.111.051.161.401.24

OHcs4.191.552.18

tert-butylmethyletherCCH3s1.191.131.111.071.141.151.21

OCH3s3.223.133.083.043.133.203.22

BHTbArHs6.986.966.877.056.976.92

OHcs5.016.654.795.20

ArCH3s2.272.222.182.242.222.21

ArC(CH3)3s1.431.411.361.381.391.40

chloroformCHs7.268.028.326.157.587.90

cyclohexaneCH2s1.431.431.401.401.441.45

1,2-dichloroethaneCH2s3.733.873.902.903.813.78

dichloromethaneCH2s5.305.635.764.275.445.49

diethyletherCH3t,71.211.111.091.111.121.181.17

CH2q,73.483.413.383.263.423.493.56

diglymeCH2m3.653.563.513.463.533.613.67

CH2m3.573.473.383.343.453.583.61

OCH3s3.393.283.243.113.293.353.37

1,2-dimethoxyethaneCH3s3.403.283.243.123.283.353.37

CH2s3.553.463.433.333.453.523.60

dimethylacetamideCH3COs2.091.971.961.601.972.072.08

NCH3s3.023.002.942.572.963.313.06

NCH3s2.942.832.782.052.832.922.90

dimethylformamideCHs8.027.967.957.637.927.977.92

CH3s2.962.942.892.362.892.993.01

CH3s2.882.782.731.862.772.862.85

dimethylsulfoxideCH3s2.622.522.541.682.502.652.71

dioxaneCH2s3.713.593.573.353.603.663.75

ethanolCH3t,71.251.121.060.961.121.191.17

CH2q,7d3.723.573.443.343.543.603.65

OHsc,d1.323.394.632.47

ethylacetateCH3COs2.051.971.991.651.972.012.07

CH2CH3q,74.124.054.033.894.064.094.14

CH2CH3t,71.261.201.170.921.201.241.24

ethylmethylketoneCH3COs2.142.072.071.582.062.122.19

CH2CH3q,72.462.452.431.812.432.503.18

CH2CH3t,71.060.960.910.850.961.011.26

ethyleneglycolCHse3.763.283.343.413.513.593.65

“grease”fCH3m0.860.870.920.860.88

CH2brs1.261.291.361.271.29

n-hexaneCH3t0.880.880.860.890.890.90

CH2m1.261.281.251.241.281.29

HMPAgCH3d,9.52.652.592.532.402.572.642.61

methanolCH3sh3.493.313.163.073.283.343.34

OHsc,h1.093.124.012.16

nitromethaneCH3s4.334.434.422.944.314.344.40

n-pentaneCH3t,70.880.880.860.870.890.90

CH2m1.271.271.271.231.291.29

2-propanolCH3d,61.221.101.040.951.091.501.17

CHsep,64.043.903.783.673.873.924.02

pyridineCH(2)m8.628.588.588.538.578.538.52

CH(3)m7.297.357.396.667.337.447.45

CH(4)m7.687.767.796.987.737.857.87

siliconegreaseiCH3s0.070.130.290.080.10

tetrahydrofuranCH2m1.851.791.761.401.801.871.88

CH2Om3.763.633.603.573.643.713.74

tolueneCH3s2.362.322.302.112.332.32

CH(o/p)m7.177.1-7.27.187.027.1-7.37.16

CH(m)m7.257.1-7.27.257.137.1-7.37.16

triethylamineCH3t,71.030.960.930.960.961.050.99

CH2q,72.532.452.432.402.452.582.57

aInthesesolventstheintermolecularrateofexchangeisslowenoughthatapeakduetoHDOisusuallyalsoobserved;itappearsat

2.81and3.30ppminacetoneandDMSO,respectively.Intheformersolvent,itisoftenseenasa1:1:1triplet,with2JH,D)1Hz.

b2,6-Dimethyl-4-tert-butylphenol.cThesignalsfromexchangeableprotonswerenotalwaysidentified.dInsomecases(seenotea),the

couplinginteractionbetweentheCH2andtheOHprotonsmaybeobserved(J)5Hz).eInCD3CN,theOHprotonwasseenasamultiplet

atδ2.69,andextracouplingwasalsoapparentonthemethylenepeak.fLong-chain,linearaliphatichydrocarbons.Theirsolubilityin

DMSOwastoolowtogivevisiblepeaks.gHexamethylphosphoramide.hInsomecases(seenotesa,d),thecouplinginteractionbetween

theCH3andtheOHprotonsmaybeobserved(J)5.5Hz).iPoly(dimethylsiloxane).ItssolubilityinDMSOwastoolowtogivevisible

peaks.NotesJ.Org.Chem.,Vol.62,No.21,19977513Table2.13CNMRDataa

CDCl3(CD3)2CO(CD3)2SOC6D6CD3CNCD3ODD2O

solventsignals77.16(0.0629.84(0.0139.52(0.06128.06(0.021.32(0.0249.00(0.01

206.26(0.13118.26(0.02

aceticacidCO175.99172.31171.93175.82173.21175.11177.21

CH320.8120.5120.9520.3720.7320.5621.03

acetoneCO207.07205.87206.31204.43207.43209.67215.94

CH330.9230.6030.5630.1430.9130.6730.89

acetonitrileCN116.43117.60117.91116.02118.26118.06119.68

CH31.891.121.030.201.790.851.47

benzeneCH128.37129.15128.30128.62129.32129.34

tert-butylalcoholC69.1568.1366.8868.1968.7469.4070.36

CH331.2530.7230.3830.4730.6830.9130.29

tert-butylmethyletherOCH349.4549.3548.7049.1949.5249.6649.37

C72.8772.8172.0472.4073.1774.3275.62

CCH326.9927.2426.7927.0927.2827.2226.60

BHTC(1)151.55152.51151.47152.05152.42152.85

C(2)135.87138.19139.12136.08138.13139.09

CH(3)125.55129.05127.97128.52129.61129.49

C(4)128.27126.03124.85125.83126.38126.11

CH3Ar21.2021.3120.9721.4021.2321.38

CH3C30.3331.6131.2531.3431.5031.15

C34.2535.0034.3334.3535.0535.36

chloroformCH77.3679.1979.1677.7979.1779.44

cyclohexaneCH226.9427.5126.3327.2327.6327.96

1,2-dichloroethaneCH243.5045.2545.0243.5945.5445.11

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Solvent extraction

Solvent extraction

Unit Three 第3单元 Unit Operations and Transport Processes (II)

单元操作和传递过程

Lesson 9

第9课

Solvent Extraction

溶剂萃取

Separation of two or more components of a liquid solution溶液 is one of the commonest of chemical-engineering problems. 1、两种或两种以上组分溶液的分离是最常见的化学工程问题之

一。

The most usual常用的 procedures程序 are evaporation蒸发,

fractional crystallization部分结晶, and distillation精馏, in which

separation is accomplished by taking advantage of利用 the differing

solubilities溶解性 or volatilities挥发性 of the components.

2、最常用的程序是蒸发、分步结晶和精馏，其主要是利用不同

组分之间溶解性和挥发性的差异来是实现的。

Alternatively或者, it is often possible to accomplish the desired 要

求的separation by bringing the liquid in contact with a second liquid

which selectively选择性地 removes one or more of the components of the solution so treated'. 3、或是，让溶液和第二种液体相接触，其可以选择性的移除被

处理溶液中的一个或是更多的组分来实现所要求的分离经常也可以

NMR参数说明

NMR参数说明

Operating

the

Bruker Avance DRX-400

NMR

William D. Wheeler, Ph.D.Department of ChemistryUniversity of Wyoming

Revised September 7, 20062

University of Wyoming Department of Chemistry NMR FacilityINTRODUCTION

The procedures for the recording and processing of a routine proton or carbon NMRspectrum using a standard set of parameters are described here. The topicscovered are:

Starting the NMR ProgramSetting Up an ExperimentLoading, Locking and Shimming a SampleData AcquisitionData ProcessingExpanding the SpectrumThe XWinNMR ToolbarReferencing the SpectrumIntegrationPlottingExiting the programXWinNMR ParametersXWinNMR CommandsProbe Calibration Results

STATUS BAR

The status bar at the bottom of the screen displays both a short description of themenu item highlighted and the status of a the current command.

HELPThere is help available by choosing Help from the main menu and selecting eitherContents or Index.3

NMR溶剂峰化学位移表

NMR溶剂峰化学位移表

GlaxoSmithKline

NMR Chemical Shifts

for Residual Protons in Solvents Solvent CDCl3 (CD3)2SO D2O CD3OD

Acetic Acid 2.13 1.95 1.16 1.99

Acetone 2.17 2.12 2.22 2.15

Acetonitrile 1.98 2.09 2.05 2.03

Anisyl Alcohol 4.61, 3.79 4.44, 3.74 4.57, 3.81 -

Benzene 7.37 7.40 7.44 7.33

Bromoform 6.85 7.75 insol 7.42

n-Butanol 3.67(t) 0.94(t) 3.41(t) 0.89(t) 3.60(t) 0.89(t) 3.54(t) 0.93(t)

t-Butyl Alcohol 1.28 1.14 1.23 -

Chloroacetic Acid 4.14 4.28 4.25 -

Chloroform 7.27 8.35 insol 7.88

Cyclohexane 1.43 1.42 insol 1.45

1,2-Dibromoethane 3.63 3.84 3.79 3.72

Dichloroacetic Acid 5.98 6.68 6.21 -

1,2-Dichloroethane 3.73 3.93 3.92 3.78

Dichloromethane 5.30 5.79 Insol 5.48

Diethyleneglycol, dimethyl ether 3.60(m) 3.38 3.49(m) 3.28 3.63(m) 3.37 -

Diethyl Ether 3.48(q) 1.20(t) 3.42(q) 1.13(t) 3.56(q) 1.17(t) 3.48(q) 1.17(t)

实验室常用溶剂的化学位移

实验室常用溶剂的化学位移

NMRChemicalShiftsofCommon

LaboratorySolventsasTraceImpurities

HugoE.Gottlieb,*VadimKotlyar,and

AbrahamNudelman*

DepartmentofChemistry,Bar-IlanUniversity,Ramat-Gan52900,Israel

ReceivedJune27,1997

InthecourseoftheroutineuseofNMRasanaidfor

organicchemistry,aday-to-dayproblemistheidentifica-

tionofsignalsderivingfromcommoncontaminants

(water,solvents,stabilizers,oils)inless-than-analyti-

cally-puresamples.Thisdatamaybeavailableinthe

literature,butthetimeinvolvedinsearchingforitmay

beconsiderable.Anotherissueistheconcentration

dependenceofchemicalshifts(especially1H);results

obtainedtwoorthreedecadesagousuallyrefertomuch

moreconcentratedsamples,andrunatlowermagnetic

fields,thantoday’spractice.

Wethereforedecidedtocollect1Hand13Cchemical

shiftsofwhatare,inourexperience,themostpopular

“extrapeaks”inavarietyofcommonlyusedNMR

solvents,inthehopethatthiswillbeofassistanceto