Monday (March 28)- Mass spectrometry Tuesday (March 29)- Experiment 6: Separa>ons ICP-MS calcula>ons
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1 LOOKING AHEAD Monday (March 28)- Mass spectrometry Tuesday (March 29)- Experiment 6: Separa>ons ICP-MS calcula>ons Thursday (March 31)- Poster crea>on? Hayes on travel Monday (April 4)- Chromatographic instrumenta>on LEARNING CHECK 1
2 LEARNING CHECK What is the purpose of chromatography? PARTITIONING Mobile phase (M) a AM a AS StaRonary phase (S) DistribuRon constant K c >1 staronary phase favored K c <1 mobile phase favored 2
3 LEARNING CHECK From the chromatogram shown below, es>mate the frac>on of the >me the solute spends in the mobile phase. LEARNING CHECK Describe a theore>cal plate? Roughly how many theore>cal plates are in an HPLC column? Which column shown below contains more theore>cal plates? 3
4 Column 1 Column 2 Column 1 neither Compound B Compound B γ=1.25 The following data are for a liquid chromatographic column: length= 24.7 cm flow rate= ml min -1 V m = 1.37 ml V s = ml A chromatogram of a mixture of species A, B, C, D provided the following data: Species reten>on >me (min) width of peak (FWHM; min) t m 3.1 A B C D Calculate the amount of >me species B spends in the solid phase. Calculate the number of theore>cal plates and plate height for Species A. For species C and D, calculate the resolu>on. Is quan>ta>ve separa>on achieved? 4
5 MASS SPECTROMETRY CHAPTERS 11, 20 OBJECTIVES Label, diagram and describe a generalized mass spectrometer Compare and contrast the ioniza>on methods described in class. How do they work? How are they applied? Describe three methods for separa>ng analyte ions on the basis of mass to charge ra>o. Diagram an electron mul>plier and channeltron. Explain how each generates a current. Label, diagram, and describe an ICP-MS 5
6 MASS SPECTROMETRY I IONIZATION METHODS IonizaRon and ion acceleraron selecron of ions detecron Mass Spectrometry Separates and detects ions based on their mass to charge raro. Elemental composiron Organic & inorganic structures ComposiRon of mixtures Structure and composiron of surfaces Isotopic raros 6
7 HISTORY Pre 1940s 1940s frac>onal dis>lla>on widespread use in petroleum industry Characterize hydrocarbon mixture generated through cataly>c cracking 1950s widespread use of commercial MS for organic ID 1980s applica>on of MS to biomolecules 1984 Electrospray ioniza>on first described 1988 MALD first described 1990 Biological MS explosion! Due to new ioniza>on techniques pep>des, polymers, proteins and other high MW biopolymers 2002 Nobel Prize given for Electrospray ioniza>on APPLICATIONS Iden>fica>on of pure compounds: Molecular masses Molecular formula from exact molar masses Molecular formula from isotopic ra>os Structural informa>on from fragmenta>on pacerns Compound iden>fica>on based on comparison of spectra 7
8 BOX DIAGRAM OF A MASS SPECTROMETER IonizaRon and ion acceleraron selecron of ions detecron 8
9 IONIZATION METHODS Electron ioniza>on Chemical ioniza>on Field ioniza>on and desorp>on MALDI Electrospray ELECTRON IONIZATION 70 ev ~55 ev, 0.1 ev h7p:// 9
10 FRAGMENTATION Interac>ons with high energy electrons leave the molecules in a vibra>onal and rota>onal excited states. Relaxa>on frequently results in fragmenta>on DESCRIBING A FRAGMENTATION PATTERN Molecular ion- Is an ionized radical with the same molecular mass as the original molecule. Also called parent ion. Base peak- The most intense peak in the chromatogram. Intensity is normalized to 100 m/z. Daughter Ions- Lower mass ions 10
11 ELECTRON IONIZATION CHEMICAL IONIZATION h7p:// 11
12 METHANE CHEMICAL IONIZATION 90% of methane exists as CH 4 + and CH 3 + and can react rapidly with other methane molecules: These species collide with analyte molecules: This generates (M+1) +, (M-1) + Also used for CI: Propane, isobutane, and ammonia MASS SPECTRUM OF OF 1-DECANOL Electron Ioniza>on Chemical Ioniza>on 12
13 MASS SPECTRUM OF OF PENTOBARBITAL Electron Ioniza>on Chemical Ioniza>on Electron Ioniza>on Chemical Ioniza>on 13
14 FIELD AND DESORPTION IONIZATION Very sog ioniza>on method Developed in Filament with >ny whiskers dipped into sample or in contact with gaseous sample. 2. Electric field applied across filament (5-20 kv) 3. This ionizes sample at emicer >ps 4. Ions accelerated into the MS FIELD AND DESORPTION IONIZATION Electron Ioniza>on Field Ioniza>on Field Desorp>on 14
15 MALDI MATRIX- ASSISTED LASER DESORPTION/ IONIZATION h7p:// MALDI MATRIX- ASSISTED LASER DESORPTION/ IONIZATION 15
16 MALDI MATRIX- ASSISTED LASER DESORPTION/ IONIZATION ELECTROSPRAY IONIZATION Good for high MW > 100kD 16
17 ELECTROSPRAY IONIZATION h7p:// Iceman Lab Electrospray IonizaRon cone into MS capillary 17
18 ELECTROSPRAY MASS SPECTRA Typical spectra have major peaks differing by charges on molecules (indicated by numbers in spectra) 18
19 SUMMARY h7p:// SEPARATION AND SELECTION OF IONS Instruments: MagneRc sector Quadropole Time of flight Resolu>on of Mass Spectrometers: R = resoluron m= mean mass of two closely spaced peaks Δm= mass difference between two barely resolvable peaks. 19
20 MAGNETIC SECTOR Pressure: bar R= 10 3 MAGNETIC SECTOR The kine>c energy of a charged analyte par>cle entering the magnet: The forces ac>ng upon the analyte ion are the magne>c force and the centripedal force, which must be equal: KE= kinerc energy m = mass z= charge V= voltage difference v= velocity parrcle e = charge of e - B= strength of magnet r= radius of curvature This can be rearranged to give: Using which, the m/z that will pass through the magnet to the detector can be calculated for a given B. 20
21 DOUBLE FOCUSING MS Pressure: bar R= 10 5 Nier- Johnson ElectrostaRc sector- passes a DC voltage between two curved metallic plates Limits KE range of ions reaching the magnerc sector since ions with different KE strike the ESA plane at a locaron other than the slit DOUBLE FOCUSING MS Ma7auch-Herzog 21
22 QUADRUPOLE Pressure: 10-9 bar R= 10 3 QUADRUPOLE 22
23 TIME OF FLIGHT Pressure: bar R=
24 TIME OF FLIGHT MASS SPECTROMETERS CAN ALSO BE USED IN SERIES 24
25 MASS SPECTROMETRY ION DETECTION IonizaRon and ion acceleraron selecron of ions detecron DETECTION: ELECTRON MULTIPLIER 25
26 DETECTION: CHANNELTRON 10 5 AMPLIFICATION INDUCTIVELY COUPLED PLASMA Atomic Emission Spectroscopy (AES) OpRcal Emission Spectroscopy (OES) Mass Spectrometry (MS) 26
27 ICP-MS HYDRIDE GENERATION 27
28 INDUCTIVELY COUPLED PLASMA (ICP) Argon carrier gas- high temp, stable, inert environment High ioniza>on energy (15.8 ev)- If Ar is ionizing, so is everything else Piezo crystal Atomiza>on- ICP INDUCTIVELY COUPLED PLASMA (ICP) NEBULIZER Piezo crystal- nebuliza>on Oscilla>ng at 1 MHz Condenser and desolvator remove solvent 28
29 INDUCTIVELY COUPLED PLASMA (ICP) ATOMIZER RF induc>on coil 27 or 41 MHz Plasma- Ar + e - + analyte ions 6-10K temp ICP-MS Sampling and skimmer cones- sample only a small volume of plasma and start genera>ng vacuum. Skimmer cone- held at a nega>ve poten>al to acract plasma ions 29
30 ICP-MS Octapole collision cell - contains H 2 or He to reduce isobaric interferences Dynamic reac>on cell- facilitates thermodynamically favorable reac>ons to reduce isobaric interferences. Eg: NH 3, CH 4, N 2 O, CO, O Ar + + NH 3 à NH Ar ICP-MS Electrosta>c collima>on of ions Deflector Plates- Ions deflected into quadrupole MS separates photons and ions 30
31 ICP-MS Quadrupole MS- Ions separated on the basis of m/z Detector- electron mul>plica>on can quan>fy elements in the low ppt range Max is ~100 ppb ISOBARIC INTERFERENCES Isobaric interferences- interferences by ions with a similar mass to charge ra>o Ar + is rarely generated, but highly reac>ve with other elements Mass/ charge 56: ArO + and 56 Fe + 80: Ar 2+ and 80Se + 69: 138 Ba 2+ and 69 Ga + Solu>ons: High resolu>on instruments Measure another or mul>ple isotopes Use collision cell 31
32 32
33 33
34 MOLECULAR ION- M/Z 106 Is an ionized radical with the same molecular mass as the original molecule Also called parent ion BASE PEAK- M/Z 91 The most intense peak in the chromatogram Intensity is normalized to 100 m/z 34
35 DAUGHTER IONS Lower mass ions 35
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