Espectroscopia no Infra-vermelho (IV) Espectrometria de ... RMN IV.pdf · Espectrometria de Massas...
Transcript of Espectroscopia no Infra-vermelho (IV) Espectrometria de ... RMN IV.pdf · Espectrometria de Massas...
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Espectroscopia no Infra-vermelho (IV)
Espectrometria de Massas (MS)
Ressonância Magnética Nuclear (RMN)
Marcos N Eberlin
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Symmetrical
stretching
Antisymmetrical
stretching
Scissoring Rocking Wagging Twisting
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http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/Spectrpy/InfraRed/infrared.htm
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Espectrometria de Massas (MS)
The Cavendish Laboratory, Cambridge,
England.
When the Duke of Devonshire offered to pay for building the
laboratory in 1870, the idea of a laboratory devoted to experimental
physics was considered an innovation.
~1870
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JJ Thomson's 'Plum Pudding Model' of the atom, a sphere
of positive charge containing electrons
The father of MS and the first mass
spectrometrist to win the Nobel Prize.
Pure species and mixtures
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"in recognition of the great
merits of his theoretical and
experimental investigations on
the conduction of electricity by
gases"
The Nobel Prize in Physics 1906
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Mass spectra and isotopes
The Nobel Prize in Chemistry 1922 "for his discovery, by means of his mass spectrograph, of isotopes, in a large
number of non-radioactive elements, and for his enunciation of the whole-
number rule"
Francis William Aston At the end of 1909 he accepted the invitation of Sir J.J.Thomson to work as his assistant at the Cavendish Laboratory, Cambridge, on studies of positive rays. It was during this period that he obtained definite evidence for the existence of two isotopes of the inert gas neon.
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12C/13C varies in nature
238U, 235U, 234 U = few mg of pure 235U
Alfred Nier
~1940 University of Minessota
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Bomba Atômica
Calutron “Racetracks” at
Oak Ridge produced
enriched 235U for the
world´s first atomic
weapons
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EI : Electron Ionization 70 eV
(Dempster & Nier)
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A Dupla Dinâmica!
Espécies Moleculares e Fragmentos
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y
z
x +
+
-
-
Quadrupolos Lineares : Q / q
Paul & Steinwedel 1953
A varredura é feita variando simultaneamente U (DC) e V0 (AC) mas
mantendo constante a relação U/V0.
Wolfgang Paul
Prêmio Nobel 1989
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Tempos de Vôo “TOF”
Cameron 1948
Através de um tubo de comprimento L (~ 1m) sob alto vácuo, íons formados
por ionização pulsada (~0.25 a 1 ms) são acelerados pela aplicação de uma
voltagem V (~1-10 KV), e adquirem velocidades proporcionais as suas m/z's.
Ocorre dispersão em tempo, e íons de diferentes m/z's chegam ao detector em
tempos diferentes :
t = (m / 2zeV)1/2 L
Princípio básico: Dispersão no tempo de íons por aceleração seguida da
medidas de seus tempos de vôo "livre".
O patinho feio
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Massa Exata = Composição Elementar
Defeitos de Massas
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CH3CH2CH2+
Reading the mass spectrum: Propyl bromide !
Br
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As “Pequenas” Moléculas
Produtos Naturais, Síntese, VOCs, ....
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As “Pequenas” Moléculas
O casal perfeito !
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ESI-MS “Ion Fishing”
Flying Molecular Elephants
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ESI-MS
HPLC/MS
“The Perfect Couple”
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MS
220 240 260 280 300 320 340 360 380 400m/z0
100
%
30JULYCAP_04 13 (0.440) Sm (Mn, 2x1.00); Cm (12:15) Scan ES- 1.46e5321
283257255
323
325
357 384
ESI-MS/MS
MS/MS CE = 12
120 140 160 180 200 220 240 260 280 300 320m/z0
100
%
30JULYCAP_03 2 (0.068) Sm (Mn, 2x1.00); Cm (2:32) Daughters of 321ES- 6.50e5321
257
152
194
176 249237
ESI-MS
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Olive Oil
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“Grape juice : must”
Wine
Wine characterization by direct infusion electrospray ionization mass spectrometry
Rodrigo R. Catharino a, Ildenize B. S. Cunha a, Aline O. Fogaça c, Elizete M. P. Facco b, Helena T. Godoy b,
Carlos E. Daudt c Marcos N. Eberlina and Alexandra C. H. F. Sawaya a*
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Isótopos
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Ressonância Magnética Nuclear (RMN)
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