Condense - University of Maryland
Contents
1. Condensed NMR Hands on Operation Manual Supplement and suitable ony or raining by TA or Senior Peer Full version is available at hitp chem umd edu nmr I 7 J You are working very close to several strong super canducting magnets in the NUR ab Folow al safety procedures and policesy as disclosed fo you atthe safely orientation To reserve spectrometer Go to hp chem umd edu nmr PLANNING Your NMR measurements Contac sta or atonal assistance Apporiment s highly recommended for project Basle sample preparation NMR Tube Sr OD 7 ong Quay rade at eas for 400M ld sven Amount ot compound assisning WL c 1000 oubie arco tempera and puro Seldcompounde 1 AmgtorH t 10 401mg fr 013 Ligideompounds 0102 Volume 000038008 Sor CH Volume of Solvent 051206 mi Deutecated savant 1009400 80 sonans Prior to NMR measurement gt Insert NMR sample tube into Selecta bue paste sample hoger Follow he recommended procede Adjust proper poston othe sample Improper adjustment leads to no detectable signals or breaking the NMI tube inside the shown te salty venation rt iei gt Insertion of NMR sample with spinner to the magnet Pres UFT btn on ihe keypad se design beu any sari ny so ie to he ool e maga Apache sie wih por Ger reci tenure o be amp epi ave supper by e preset i tun e ag eny pot inthe LPT tuo ag bn Jor sare rb ve qua The Keypad2. Far comprehensive let det willbe engined inthe PLOT seein RS ee he ge Frecessing se ak pk pen regt FR Poser tanto FD spk Automated reset phase Dk por corecitn vales PHD and PHC td wih ha ae Ue when ens scd ran ed A gt Ack your paertaner or MUR TA or demo You willbe tet is procedure on your check bm opiate 0 0 manly Chemical shit calibration select and click eter circled icone as shown in the figure DES MRM A Pecan ter Ct CSE ieee o mese e XU remit on nk arte prre rene lI 200 WF Verne re du teres ip ah s MS uae ri epe mend POO henalihn auem ie cme sone a yo se i trou fon ru ns por eal atom he ETE Peak Picking ran Chena Erato rus card abo an Foro User anal rdc a TTT hain ashy canbe maid wh Integration iura This s on tue when the processing 6 done prope suet fava dle he Coen e da o cote Procedure 7 Reo iUe aal ir sen ste Auto Integrate Chek he Integrate eon ype abe Spm Spi Were Top Tung fans Feces Opies Daye 7 BE etree ver ere pn COC RET EE eee STEP 2 Modification and calibration trees cask Toon sor rey terga Slope and bias on a particular Integral
3. 30 Beer repo Place he mosse on here ol eet lt ch an pp up mena appear ick Sted beaut ene The ieglragan hes yon gem uence Mr pm SAVEINTEGRATION ers sirens and roses compie vate he PLOT Before printing RETE UE e rece oir Sele measures Ci save wen adir i uen Plot print In top row of main window File gt gt gt click Print po puel Wnt is e LAYOUT tis triste t deines Pe prope lets ina T ec cane eran dieat ue 1D Hew or prt 10_BBLwp er ode Sack wp rich pec Plot editor wil automaticaly pori ha curent spect as the main object defined inthe layout coda Sanat cae Secon pace he mse nee Wa CEA ok aor Fa Select the 1D 20 ltor The Edtoplon how tele ove Te 10 20 option such esr aur eae ost etre Spc othe When you eh madi ath oec ck Fe an prr win he Pied D s hei pira o za MMH ar ino ABOUT THE Basic level NMR CHECK OUT Open book Last update ox as Dead Line for your check ou Name and signature of trainer gt Basie expectation 3 Able to lg on with your gun User ID to actuate the spectometar A Abe to compie al base ade procadun no icee meal obecis proper sample inseron wien working he NR a Able tocatec properly shimmed HY spectrum wihin on minutes FTP au FID det pone othe woastalone nthe NMR Lab Al datas obe processed an plot wit TOP
4. Locaes nest to be console Compute The you conss oa mati ot buttons B pressing a spoctie buon a cet tuncton can be mood b ring mo wheel zb The LED thes ta select uncon tal The value of austment is shown an he center LED bar Tee major etal wil be described ltr inthe T7 Mechanical coni on NMR sample 2 Reldcontals eck suco 3 Shim orden scien els see Aspen A To stat ToPSPIN double cick AU on PC desitop NUR Data ut custom eons an pl own mena Toss commen sop D ctor c wa te esl nes en c SS terree UB oh Fee Sean ere reer m aw a Shoat ta oan Sra pec Sim eri tole ee ans Mi pn aja a nc es tintin o ere ote emm dn Vix i re ein eee 3 Mame 06 ve name 6509 yer sample carpit paint nner Any lager Sehen ad dei he serio your sap 3 Mandstoryto keep the neri toe a shown nthe os i Experiment Dies XCHBnkerTOPSPINept rr bartsa Experiment Use core pra Basic Setup procedur Ate you rate ate and wt your sample proper incerta in ne magnet FG empl Aston Clk on UM Setup to sees and load standard expecment Fon ns emat wid ed presents any characters Set rat D ee par a tot aera an s Mo nti ay referee irre and puse value speci er h
5. SPIN sofware and ne worksatens in MMR acy atin TEN mites sfondi ell chan ti PR PO gt Bast understanding You a expected to know he function ofthe essential tems Di NS SW emt als cy Manual ores gt Print o copies spectra wih TOPSPIN sofware 3 The est plot ust conan he fotowingems selet aye 10_1 Acguiston amp processing parameters sted Fal spocral ange Noinegraton and peak Erase hem ey appears nthe plot seen Yur name and USER D ncded nthe te The second plat based onthe st iot delete the at of parameters but dd back the sing of shits and legates using ha 1D20 Ear Make fa use of he long o he chat paper forthe pat Tre signis and he regal are expended sufciaty large corosponding bu the integrals are nat overlapping tv basa ino fhe specum Pay panicuar tenion on ntaratens over mutple signa proper slope bas and Tangs o negras study Manual fo dea Basic reference vo 0 00 und edulome
6. e scale Sa aes par het snows a pation nih Me atone El Breen decode ia rave aig ee cnet aie et Basic procedure for a select NMR measurement et Feadnetucton er e scd messurarent Ores you ree tan on maj elas e covert reek ne el jel pane sen nag vem an em EET Optimization and data acquisition Adjust and Acquire ment Execute eps sequence ton opto EES NUT T atom fect acim tea Hoo pane nan fe ST immer om ete Skip Step 3 for routine spectrometer 2 asin Tune probe wa Noaptea or nce nn ooh stre spent west oc go na Venter eiii sete ene sng enn Optimization and data acquisition Conn Mania we egg Step 4 Manual Shim Esset to 2 eta ih resoution sharp NMR signal advance 400 60 ops 5 jst S s 4 Sick gei ruote ry feme The precy te base TFs chock i msde oso hg sed aU cy a ure sari colct doa ag TE hey e ane 2 90 Aways check the ne shape wh a uk ste scan to obra a Ht spectrum after Eu iir UP ung the cours of shim adustment the deck nil estende re anny sen duce hr ck oer Toke ate teak lovin ih ck pay he il lore Totes wie resin you shal charge Z eae en te yn yb 00 St nani i aud annt o eres a Rov afew segments Va haz thm a ened in hy pa coda eas ordre ber idee cee tbe Reverses satel at Z Nine lease he 7 si vai hy 20 to Suns
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