核磁共振变温实验和注意事项（英文版）
NotesonVariableTemperature
INANEMERGENCY:
Ifthepowerfails,thegassupplyisinterrupted,younoticeaburningsmell,etc.,IMMEDIATELYSTOPALLVTACTIVITIES:
1.Immediatelytypetemp='n'su
2.ImmediatelysettheFTSpre-conditioningunitto20C.
3.Immediatelyremovetheliquidnitrogenbucketifyouareusingit.
4.ImmediatelycontacttheNMRFacilitystaff.
5.Immediatelyremoveyoursample.
6.Inextremeemergencies:
A.WalkaroundthemagnettothebackoftheI-400console.DONOTwalkbetweenthemagnetandconsolethroughthecables&circuits.
B.TurnOFFthepowertotheVTunitbypressingthebigred"POWER"buttonontheconsoleVTunit(theconsoleVTunithasablackpanelwithaPOWERbutton,STATUSlight,andLEDdisplayofthetemperature).
核磁共振变温实验和注意事项（英文版）
TroubleshootingtheVTunit.
1.Ifyoutypetemp=25suandtheVTdisplayontheremotestatusmoduledoesNOTrespondafterafewminutes,typesethw('vt','reset')temp=25su(thisONLYworksonINOVAspectrometers)
2.Ifthereisnochange,
A.WalkaroundthemagnettothebackoftheI-400console.DONOTwalkbetweenthemagnetandconsolethroughthecables&circuits.
B.TurnOFFthepowertotheVTunitbypressingthebigred"POWER"buttonontheconsoleVTunit(theconsoleVTunithasablackpanelwithaPOWERbutton,STATUSlight,andLEDdisplayofthetemperature).
C.Wait10seconds,thenpressthebigred"POWER"buttonagaintoturnONthepowertotheconsoleVTunit.
D.Typetemp=25su.TheVTdisplayontheremotestatusmoduleshouldrespond.
3.CheckthatthereisNOCONSTRICTIONinallVThosesandthatallhoseconnectionsaresealedtightlywithnogasleaks.Themostlikelyplaceforthisconstrictionisbetweenthepre-conditioningunit(orliquidnitrogenbucket)andtheprobe.BECAREFULwhenyoucheckthehoseconnecteddirectlytotheprobe:thisconnectionmaybefrozenandtheprobeisVERYFRAGILE---begentle,oryouwillbreaktheprobe!
核磁共振变温实验和注意事项（英文版）
ToperformVTexperimentsbetween+25Cand+90C:
1.MAKESUREthatyoursampleisstableatthelowestandhighesttemperaturethatyouwilluseonthespectrometer.Ifyoursampleexplodesinthemagnetanddestroystheprobe,youwillberesponsibleforthecostofequipmentrepair.
2.Typetemp=25sutoregulateyoursampleat25C.
3.MakesurethattheFTSpre-conditioningunitissetat20C.
4.Afterthetemperaturedisplayontheremotestatusmodulehasstabilizedforafewminutes,typetemp=temp+10su.Donotincreasethetemperaturebymorethan10degreeincrements.Ifyourdesiredtemperatureiswithin10CofthecurrentVTtemperature,typetemp=##where##isyourdesiredtemperature.
5.Repeatstep#4untilyoureachthedesiredtemperature
6.Performyourexperiment(s).
7.WhenyouarefinisheddoingVTexperiments,typetemp=temp-10su.Donotdecreasethetemperaturebymorethan10degreeincrements.
8.Waitforthetemperaturedisplayontheremotestatusmoduletostabilizeforafewminutes.Repeatstep#7untilthetemperatureis15C.
9.SettheFTSpre-conditioningunitto20C.Waituntilthedisplayonthepre-conditioningunitreachesthesettemperature.
10.Typetemp='n'sutoturnofftheVTregulation.
ToperformVTexperimentsbetween+90and+150C
1.MAKESUREthatyoursampleisstableatthelowestandhighesttemperaturethatyouwilluseonthespectrometer.Ifyoursampleexplodesinthemagnetanddestroystheprobe,youwillberesponsibleforthecostorequipmentrepair.
2.InformtheNMRFacilitystaffatleasttwodaysinadvancethatyouwillneedN2gasfromtheN2boil-offtanksinthewetlab.
3.PurgetheVTsystemwithN2gasfor20minutes.
4.Typetemp=25sutoregulateyoursampleat25C.
5.Thedifferencebetweenthepre-conditioningunitandthesampletemperatureshouldnotbegreaterthan60C.Ifthenextstepincreasestempmorethan60degreesabovethepre-conditioningunittemperature,firstincreasethetemperatureofthepre-conditioningunit.DONOTincreasethepre-conditioningunittemperatureabovetheVTtemperature.DONOTincreasethepre-conditioningunitabove+90C.
6.Afterthetemperaturedisplayontheremotestatusmodulehasstabilizedforafewminutes,typetemp=temp+10su.Donotincreasethetemperaturebymorethan10degreeincrements.Ifyourdesiredtemperatureiswithin10CofthecurrentVTtemperature,typetemp=##where##isyourdesiredtemperature.
7.Repeatsteps#5&6untilyoureachthedesiredtemperature.
8.Performyouexperiment(s).
9.WhenyouarefinisheddoingVTexperiments,typetemp=temp-10su.Donotdecreasethetemperaturebymorethan10degreeincrements.Decreasethetemperatureofthepre-conditioningunitifthetemperatureofthisunitishigherthantemp.
10.Waitforthetemperaturedisplayontheremotestatusmoduletostabilizeforafewminutes.Repeatstep#9untilthetemperatureis0C.
11.RemovethelN2bucketwhenthetemperatureissetto0Corhigher.ContinuetowarmtheVTunitbyfollowingstep#9.
12.Whentemperatureequals>15C,typetemp='n'sutoturnofftheVTregulation.
13.SwitchtheVTsystemfromN2gastoair.
ToAccuratelyMeasuretheTemperature:
ThetemperaturedisplayontheremotestatusmoduleisNOTNECESSARILYthetemperatureofyoursample.SeealsoImportantNotesaboutVT:note#1.Whilethedifferencebetweenrealtempanddisplayedtempisusuallysmall,thisdifferenceislargeratextremelyloworextremelyhightemperaturesettings.Toaccuratelymeasurethetemperatureofyoursample,dothefollowingbeforeorafter(orbeforeANDafter)youperformyourexperiment:
Tomeasuretemperaturesbetween+20Cand+90C:
1.Puttheethyleneglycoltemperaturecalibrationsampleinthemagnet.TurnthelockOFF.
2.Bringthesampletothedesiredtemperature.
3.Equilibratefor10minutes.
4.Obtaina1D1Hspectrum.
5.Displaytwocursorsandalignthemonthetworesonancesinthespectrum
6.typetempcal('e')ortempcalc('e','####.#').
tempcalcalculatesthetemperaturebaseduponthecursorpositiononthescreen.
tempcalccalculatesthetemperaturebaseduponanumber(typeanumberinplaceof####.#inthecommand).Therearethreevariationsoftempcalcfortheethyleneglycolsample:
●tempcalc('e','####.#')calculatestemperatureofethyleneglycol,chemicalshiftdifferenceinHz
●tempcalc('e','####.#','h')calculatestemperatureofethyleneglycol,chemicalshiftdifferenceinHz
●tempcalc('e','####.#','p')calculatestemperatureofethyleneglycol,chemicalshiftdifferenceinPPM
7.Therealtemperatureisdisplayed.RecordthistemperatureANDtheVTgasflow.
Tomeasuretemperaturesbetween-90Cand+40C:
1.Putthemethanoltemperaturecalibrationsampleinthemagnet.TurnthelockOFF.
2.Bringthesampletothedesiredtemperature.
3.Equilibratefor10minutes.
4.Obtaina1D1Hspectrum.
5.Displaytwocursorsandalignthemonthetworesonancesinthespectrum
6.typetempcal('m')ortempcalc('m','####.#').
tempcalcalculatesthetemperaturebaseduponthecursorpositiononthescreen.
tempcalccalculatesthetemperaturebaseduponanumber(typeanumberinplaceof####.#inthecommand).Therearethreevariationsoftempcalcforthemethanolsample:
●tempcalc('m','####.#')calculatestemperatureofmethanol,chemicalshiftdifferenceinHz
●tempcalc('m','####.#','h')calculatestemperatureofmethanol,chemicalshiftdifferenceinHz
●tempcalc('m','####.#','p')calculatestemperatureofmethanol,chemicalshiftdifferenceinPPM
7.Therealtemperatureisdisplayed.RecordthistemperatureANDtheVTgasflow.ImportantNotesaboutVT:
1.Insidetheprobe,thegasflowspasttheheater,thenpastthethermocouple,thenpastyoursample
A.IfgasisNOTflowingpasttheheaterandtheheateristurnedON,therewillbeaVERYRAPIDbuild-upofheatinsidetheprobe.Thishastwoeffects:
1.Theprobecouldsufferdamage.
2.Yousamplewillstarttoincreaseintemperature.However,thisincreasewillnotbeveryrapiduntilthegasflowstartsagain.Oncethegasflowstartsagain,thegaswillflowpasttheVERYHOTheater,andthenflowuptoyoursample,andyoursamplewillrapidlyincreaseintemperature.THEREFORE,ifthegasflowisinterrupted,immediatelyturnofftheheater,especiallybeforeturningonthegasflow.
B.Becausetheheaterisbelowthesample,everysampleexperiencesatemperaturegradientfromthebottomofthetubetothetopofthetube.
1.Limityoursampleheightfrom28to32mmtoreducethisgradient.
2.Thisgradientmayalsocauserefluxingorconvectionofyoursolvent,whichwilldegradethelockstabilityandresolution.ConsulttheNMRFacilitystaffaboutvortexplugs,whichwillreducetherefluxingofyoursolvent.
3.Increasethegasflowatextremetemperaturestoreducethechangeingastemperaturebetweentheheater,thermocouple,andsample.(Caution:Ifyouincreasethegasflowtoomuch,samplespinningmaynotworkand/oryoursamplemayriseoutoftheprobehead,asifthesamplewaspartiallyejected).
C.Becausethethermocoupleisbelowthesample,thetemperaturedisplayedontheremotestatusmoduleandtherealtemperatureofthesampleareNOTNECESSARILYthesame.Whilethedifferencebetweenrealtempanddisplayedtempisusuallysmall,thisdifferenceislargeratextremelyloworextremelyhightemperaturesettings.Increasetheairflowtoreducethisdifference,especiallyatextremelyloworhightemperatures.(Caution:Ifyouincreasethegasflowtoomuch,samplespinningmaynotworkand/oryoursamplemayriseoutoftheprobehead,asifthesamplewaspartiallyejected).
2.Thenormalflowofgasshouldbe10LPM
3.ThisconnectionbetweentherubberhoseandtheprobeisVERYFRAGILE!BECAREFULifyoumoveanythingaroundthisconnection.Donotremovetherubbertubefromtheprobeiftherubberisfrozen---firstthawtherubberwithyourhand.
4.Theliquidnitrogenusuallylasts1to2hours.DonotrunlN2esperimentsunattendedformorethan1hour.
5.Iftin='y'andVTbecomesunregulatedduringtheexperiment,thedataacquisitionisautomaticallystopped.TheacquisitionwillNOTautomaticallyresumeiftheVTbecomesregulatedagain.
6.vtwaitdeterminesthelengthoftimetowaitforVTregulationbeforetheexperimentwillstart.Thedefaultvalueforvtwaitis180seconds.IfVTregulationisnotachievedaftervtwait,then"VTFAILURE"willbedisplayedontheSunmonitor.
7.Withproperchoicesforpadandatemparray,aseriesofexperimentscanbeautomaticallycollectedwithchangesintemperaturebetweenexperiments.
8.High-powerdecouplingcanheatyoursample,whichdecrerasesyourVTstabilityand
accuracy.ConsulttheNMRFacilitystaffaboutmethodstoreduceheatingbythedecoupler.
9.Thepre-conditioningVTunithasthefollowingcontrols:
TheUParrowincreasesthetemperaturesetpoint
TheDOWNarrowdecreasesthetemperaturesetpoint
TheRUNkeytogglesthecontrolleron/off.TheunitisregulatedonlywhentheRUNlightison.IftheRUNlightisoff,presstheRUNbuttontoturniton.
Toturnoffthepre-conditioningunit:
A.turnthetemperaturecontrollerto-60C.
B.Turnofftherefridgerationswitch
C.Letaircontinuetoflowthroughthesystemuntiltheexitairreaches+20C
D.TurnofftheFTS"regulation"unit.
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