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by: Michelle Gulgowski DVM


Michelle Gulgowski DVM
GPA 3.91


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Class Notes
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This 27 page Class Notes was uploaded by Michelle Gulgowski DVM on Friday October 23, 2015. The Class Notes belongs to CHE 532 at University of Kentucky taught by Staff in Fall. Since its upload, it has received 24 views. For similar materials see /class/228304/che-532-university-of-kentucky in Chemistry at University of Kentucky.




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Date Created: 10/23/15
Mass Spectrometers Building a Mass Spectrometer Ionization Accelerate a Chamber Detector Ion source Mass Filter Separation by Velocity Ion Behavior in E or gt DeteCtOr B field Other methods M11M2 r gt Can be or or radical ions Neutral species are left behind Mass Analyzers Sector Timeof Flig ht Quadrupole Ion Trap All of these select or filter ions based on the mass etacharge ratio me or mz M2 is detected as 72 M Magnetic Sector Venerable simple capable of very high resolution when multiple sectors are linked 19988MTissue Ion source magnet wwscimediaoom counter or electrometer ion detector Time of Flight TOF gt Flight tube fied free G For a given accelerating voltage heavy ions reach a lower velocity than light ions Mass is related to arrival time at detector light ions arrive first heavy ions later No mass limit Requires fast electronics but othenvise simple Quadrupole Mass Filter Detector resonant ion dc and ac voltages WP Chem 1 gammaquot 7 Compact simple inexpensive Common in LCMS and GCMS systems mnTmp Ions can be held circulating in trap Ions can be ejected from trap as function of me and rf frequency 1 Detector Very compact High sensitivity Long ion lifetimes Facile MS experiments Ion SOUrces 39 Dozens of different ion sources out there often integrated with inlet systems GCMS LCMS ICPMS El 5 CI 2 MALDI FAB ESI Direct ProbeElectron Impact El Mass analyzer Only useful for samples With reasonable vapor pressme IOW only g ery simple Heating the probe can 39 e Xpe n39S39Ve decompose the sample Violent 10 s of eV Mquot often breaks up immediately A Simple El Spectrum HR 1 39 MQWZL a y 0quot F u r5 4 V El blasts lactose into pieces 39E 53 124 a f in LH o g 103 1 131 1 1m Ml l llH lIIIJ llll l llulll l L 191 ll lull NIHHJH 50 100 150 200 mz 250 300 350 itte tiny pieces m 7 73 pA O Lllllllll 57 60 U1 0 Illllllll O 100 150 U Q Chemical Ionization Mass analyzer GOG An39alyte molecules collide with ionized reagent gas to make MH ions as well as M15 and others Laser Desorption and MatrixAssisted Laser Desorption MALDI Sample in Matrix absorbs most of the matrix energy from laser pulse Analytematrix erupts into gas phase matrix peaks can interfere Ions in form of MHy M Na others Excellent for high masses Electrospray Ionization skimmer cone Nebulizer gas O IMass O gt O 39 analyzer kV III Vacuum evaporates solvent rapidly from small droplets Soft ionizat ion method excellent for delicatequot nonvolatile analytes Typically ions are MH or MNa39 not M t and multiply Charged ions are common Remember Lactose 57 739 6O 85 1 103 7 of Base Peak n w 1 III llllll ll 1 quotII 31 191 HIIIIIIII IIIIxI lIIIIIIIHIAIHIIIIIllwllylxll lllnlnmWullllu 50 100 150 200 mz 250 300 350 HO OH H OH 365 HO O I H H M23 Na gt H0 T HO r 0 H OH I H H H H quotquot on u I Lactose 012142201 1 Mol Wt 342 CH of Base Peak M 200l 251 3427 llIIwllH41IquotxII39IIIllIIIIIxIIwinHIIIIlllnlllnlmlwlmlullyllll 10 150 200 mZ 250 300 350 Electrospray Ionization of Myoglobin M1539113132 M16968 httpwwwchmbrisracukm stheoryeshion isfationrhtml Note little fragmentation Lots of39different multiply charged ions esolution and Sensitivity Maxi m u m me Analyzer Resolution roughly Sensitivity 1 5000 00001 39110000 Low No limit 00001 High 5 000 1 High 50070 1 High Much higher with multiply charged ions to 10 s of k Parent ion of Benzene Mz 78 M1 MZ 79 67 of 78 Due to 11 73C 3711 6 carbons Isotope lines Mass Intensity 100 0 68 318 Due to 35C 370 Mass Intensity 1 1570 44 1580 599 Due to 798r 87Br What about HIGH resolution Molecular Formula C4H602 C4H10N2 M 860 860 Precise Mass 860845 860368 See table 84 in PLKV Differ by 00477 mass units 0055 Sample Spectra m5 08 m om mm gi IUm r me NEE Io 216 mm mm N m fofofofofo K 0 0 x8 Ansuewy eAnmeg fofofofo ND om fofofo mv 2me 08 C6vm LGGC m I mcmom Bromobutane Re c ve ntensity 1007 nermrnxs4 125 M 136 06 138 06 mz ln cengitg 1 W is 1 33 43 SCI E43 T II 133 Spectrum 1 M is doubled Prominent me 91 from loss of 81 and loss of 79 Few other fragments RetGUve ntens tty 106 Mz 56 Loss of 18 Mermrs4ss Spectrum 2 Weak parent M1 M18 M43 is prominent Loss of 43 M1 mm 55 t mmm m wm m 15 20 25 60 65 7o 75 Mz 31 peak indicates that this39is the 1isomer not the 2isomer


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