NMR spectroscopy in non deuterated solvents.

E. Alvarado, U of Michigan, 8/2/06, 08/19/10

The acquisi ion of !M" s#ec ra in non deu era ed solven s is no ver$ differen fro% regular acquisi ions in deu era ed solven s. The %os no icea&le difference is ha $ou 'on( &e a&le o loc) he %agne or o shi% as usual &$ loo)ing a he loc) signal(s s reng h. Af er #lacing $our sa%#le in he %agne , loading a##ro#ria e #ara%e ers, and selec ing he solven *choose fro% he lis he deu era ed solven equivalen o $our #ro ona ed solven + load he shi%s as usual 'i h setlock. This %acro also se s ,0 * he %agne ic field(s s reng h+ o a value a##ro#ria e o $our solven . !o ice ha he -Find Z0. &u on 'ill no 'or) as i relies on he #resence of a deu era ed solven . Then urn he loc) off in he Start, Lock #ara%e er #anel. To shi% using he signal of $our #ro ona ed solven , firs %a)e sure he #ro&e is uned o de ec #ro ons, hen selec fro% he %ain %enu/ Acquisition > Do Gradient Shimming > Use 1H/gradient ma . This #rocedure 'or)s &es 'i h solven s ha #roduce onl$ one %a0or #ea). 1i h o her solven s, li)e T23, i %a$ no &e co%#le el$ successful, &u re#ea ing he shi%%ing #rocess a second or hird i%e can hel#. 4f he resul ing s#ec ru% is unacce# a&le, or if $our solven doesn( have an$ h$drogen a o%s, follo' he ins ruc ions in he 'ri eu# 5Gradient shimming non deuterated solvents6 availa&le in our 'e& si e. 4f $our solven does no have an$ h$drogen a o%s, he onl$ 'a$ o shi% is &$ %oni oring he sha#e of a signal in $our s#ec ru%. 4n he case of #ro on !M" in solven s con aining h$drogen a o%s, he solven (s signal can &e oo s rong for he receiver, even a gain=0 and $ou %a$ ge an error %essage si%ilar o 5"eceiver overflo', reduce #ulse 'id h6. 4f his ha##ens 0us do as $ou are old and reduce he #ulse 'id h *se pw=1+ and r$ again. 4f $our sa%#le is sufficien l$ concen ra ed, $ou %a$ ge an acce# a&le s#ec ru% des#i e he ver$ large solven #ea)*s+. !o ice ha close o he &ase of $our solven #ea)s so%e signals %a$ a##ear ha loo) li)e s#inning side &ands7 i.e. he$ are s$%%e rical around he %ain #ea). 2o'ever, he$ a##ear a frequencies ha do no corres#ond o he s#inning ra e or even he #ro on8car&on cou#ling cons an and he$ are usuall$ ou of #hase. The$ arise fro% an un&alanced s#inner *due o user a&use+. 9hanging he s#inner or urning he s#inning off 'ill eli%ina e hese ar ifac s. :lease don( dro# he s#inners; 4f $our sa%#le is dilu e or if $ou have a ver$ large solven #ea), $our s#ec ru% 'ill loo) 5nois$6. 4n his case, fur her accu%ula ion of scans 'ill no hel#. The #ro&le% is no of #oor signal o noise &u of li%i ed d$na%ic range/ $our 'ea) signal is #oorl$ digi i<ed 'hen a ver$ s rong signal is #resen . The &es course of ac ion is o eli%ina e he offending #ea)s using a solven su##ression echnique. The easies echnique is presaturation. 4 gives acce# a&le su##ression in %os cases, &u 'hen a %ore effec ive and selec ive %e hod is required, or 'hen $ou need o su##ress %ul i#le #ea)s as is he case 'i h T23, he &es %e hod is wet1D. This is a %ore so#his ica ed #ulse sequence ha e%#lo$s sha#ed #ulses and %agne ic field gradien s o #erfor% he su##ression. =o h 'e 1> and #resa ura ion are e?#lained in a se#ara e a##lica ion no e.