Introduction and History of Mass Spectrometry. Only the stable isotope bit counts!
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1 Introduction and History of Mass Spectrometry Only the stable isotope bit counts!
2 The People 1 Joseph John Thomson Parabolas of Wien (deflected Kanalstrahlen by strong superimposed M-E field) blurred -> collision with residual gas molecules Metal plate with slit (low pressure problem with photo plates) Variation of magnetic field Plot Magnet field vs. Ion current -> First Mass Spectrometer (1905)
3 The People 2 Francis W. Aston Tandem Electric field Magnet field Resolution ~ 130 (1919) Stable Isotopes Arthur J. Dempster (1918) 180 magnetic sector Josef Mattauch / Richard Herzog (1934) Double focusing mass spectrometer Alfred Nier / Edgar G. Johnson (1953) Double focusing mass spectrometer with corrected second order aberrations Double inlet
4 The People 3 Ludolf Jenckel (1947) 60 magnetic sector Build in a rented hospital cellar in Bremen Built his first mass spectrometer on a shoestring budget Early comments on mass spectrometers t machine that doesn t quite work there s got to be an easier way to make a living
5 Aston s First Instrument A Positive Ray Spectrograph. By F.W. Aston, M.A., D.Sc,. Clerk Maxwell Student of the University of Cambridge. 1919
6 1 st Results No magnetic field Hydrogen No diaphragm Hydrogen CH 2, CH 3, CH 4
7 Isotopes Everywhere
8 Commercial Manufacturers 1 Consolidated Engineering Corporation - CEC 1942, single collector, used in petrochemical industry Mass range 150 Daltons 1960 > Bell and Howell 1975 > dupont Nuclide (1961 to 1992) 180 magnetic sector Founded by Len Herzog at Penn State Selected by NASA to analyze the first moon rocks > Spectrumedix Corp Westinghouse Westinghouse Double focusing mass spectrometer
9 Commercial Manufacturers 2 GE Double focusing mass spectrometer with corrected second order aberrations Metropolitan Vickers > Associated Electrical Industries AEI > Kratos Vacuum Generators Started in 1962 by Bernard Eastwell and Vic Treasure to sell the CR38 vacuum valve > VG > Micromass > GV > GVI > IsoPrime/Elementar
10 Commercial Manufacturers VG offshoots Vacuum Generators > Vacuum Science Workshops (deceased) > Europa > Europa PDZ > Sercon > Turner Scientific > Thermo > DLT Ltd. > Thermo > Compact Science Systems HTX Instruments > Analytical Precision (with DLT Scientific) > CJS Science > Provac > Nu Instruments > At least a dozen others
11 Commercial Manufacturers - Bremen Atlas Werke AG > Atlas Werke AG MAT (Mes und Analysen Technik) > Varian MAT > Finnigan > Thermo MS1 60 sector instrument
12 Commercial Manufacturers - MAT
13 Commercial Manufacturers MAT isotope Isotope Ratio and Elemental Analyses New Generation THQ New Generation 1. Thermionic i Ionization (solids) CH5 TH TH Triton Triton Plus 281 Uranus 250 UF 2. Electron Impact Ionization (gases) 511 (UF) UF5 CH4 CH3 M GD Delta E 251HDT Delta S 252 BreathMAT Delta C Plus Plus Delta Delta XP Plus Delta V 3. Inductively coupled plasma ionization (solids, liquids) Element-XR Element Element2 Element-GD Element-GD Plus 4. Multi-collector ICP (solids, liquids) 5. Nobel gases (static vacuum) Neptune Helix SFT Argus VI Neptune Plus Helix MC
14 Ionization sources Gas Discharge Glow discharge Inductively coupled plasma Vacuum Spark Spark Source Surface Ionization o Thermal ionization Electron Ionization Nier 1947 with collimating magnet and focus plates Chemical Ionization SIMS Secondary Ion FAB Fast Atom Bombardment Field Ionization MALDI Matrix-assisted laser desorption/ionization Electrospray Ionization
15 Separation techniques Magnetic Sector Separates by mass to charge ratio Electrostatic Sector Separates by ion energy (velocity) Quadrupole Filters by mass to charge ratio Time of Flight Tandem MS (MS-MS) MS) Ion Trap Fourier Transform Orbitrap
16 Detection techniques Photographic plate Break vacuum to retrieve plate Electrical plate collector Vibrating read Faraday Collector High gain amplifier Daly detector Daly detector Secondary Electron Multiplier SEM Channeltrons
17 Vacuum techniques Diaphagm Rotary Diffusion Mercury Polyphenyl Ether oil (Santovac) Cryopump Tubomolecular Holweg stage for high compression of light gases Ion Getter Sublimation On-Tool booster
18 Sample Preparation Timeline
19 Dual Inlet
20 Early Commercial GIRMS
21 Dual Inlet Analysis
22
23 Delta Equations Delta equation δ sam = (R sam R ref ) / R ref * 1000 Correction to standard d δ corr = δ sam + δ std + (δ sam x δ std )/ 1000 corr sam std sam std
24 17 O Corrections Craig correction for PDB referenced analysis only δ 13 = x δ x δ 18 δ 18 = x δ x δ 13 Santrock and Hayes 17 R= 18 R a x K a = and K =
25 International Standards
26 Multiport
27 Microvolume
28
29 Open split
30 Open split devices Prep CSI 13 C 15 N 34 S HD 18 O 37 Cl 81 Br Simultaneous Device A Dual inlet x x x x x EA x x x x TC/EA x x x GCC x x x GC/TC x x x GasBench x x x x GC x x LC C x x
31 Continuous Flow Linearity
32 EA Continuous Flow
33 GC Continuous Flow
34 GasBench Continuous Flow
35 LC Continuous Flow
36 It behaves at times in the most capricious and unaccountable manner...when by good fortune, all is well, the arrangement is capable of good performances. Thus, after a favourable setting of the apparatus, six elements were successfully analysed in as many days. On the other hand, after dismantling became imperative and it had to be cleaned and rebuilt, exactly as before as far as one could tell, no results of any value were obtained during weeks of work. Francis William Aston
37 #140, Street S.W., SW Calgary, Alberta T2H 3A9 isomass@isomass.com Tel: (403) Fax: (403) Toll Free:
Introduction and History of Mass Spectrometry. Isotope measurements are really stable!
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