Pulsed lasers. To induce new chemistry, different from that initiated by conventional sources

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1 Pulsed lasers As part of a method to study photoinitiated chemical reactions To induce new chemistry, different from that initiated by conventional sources As a light source, to initiate the same chemistry as with conventional sources 1

2 Pulsed nanosecond lasers LASER WAVELENGTH, nm PULSE Nitrogen Excimer Ruby Nd/YAG Diode Dye (Ar/F) 248 (Kr/F) 308 (Xe/Cl) 351 (Xe/F) (x2) (x2) 355 (x3) 266 (x4) > 700 nm > 300 nm 8 ns, 10 mj 5-50 ns, 300 mj 5-50 ns, 1J 5-50 ns, 500 mj 5-50 ns, 300 mj 10 ns, 1 J 10 ns, 300 mj 5-10 ns, J 5-10 ns, 500 mj 5-10 ns, 300 mj 5-10 ns, 150 mj low 5-20 % of pump 2

3 Lindqvist's 1966 laser set-up Lamp Filter Monochromator PMT Amplifier Laser at 337 nm 1 mj Scope Lindqvist, L. (1966). Utilisation d'un Laser à Émission Ultraviolette Pulsé en Photolyse-Éclairs: Étude de l'état Triplet de l'acridine. Hebd. Seances Acad. Sci., Ser. C. 263,

4 PMT output Determining transient absorbances 0 Io Signal PMT output = P mt = Io - S ignal T = P mt Io O.D. = -log T = log 1 - Signal Io 4

5 Laser flash photolysis technique Typically 266, , 355 nm Laser Detector Lamp 5

6 Laser photolysis sequence LASER SHUTTER OPEN PRE PULSE PULSE POST PULSE TIME (ns) MONITORING SHUTTER OPENS A/D DETECTION LASER MONITORING SHUTTER CLOSES PMT OUTPUT (mv) SIGNAL 60 Hz AC SINE WAVE (From Line Synchronizer) 1 Hz LASER PULSES TIME 10 (ns) 6

7 Conditions and capabilities of laser flash photolysis FAST PRECURSOR PROCESSES SLOW DECAY OF PRODUCTS Process under study A B Reagents hν fast A A B 10 ns µs slow B final products 7

8 Kinetic analysis for visible systems Bu t O Bu t O + solvent-h Bu t O + Ph 2 CHOH CH 3 COCH 3 + CH 3 Bu t OH + (solvent) Bu t OH + P h 2 COH k 0 k rxn k growth = k 0 + k rxn [Ph 2 CHOH] PROBLEM: Most systems of interest do not involve reactants or products that can be readily detected in the UV-Vis region Bu t O + E.g.: Bu t OH + 8

9 The probe technique Bu t O CH 3 COCH 3 + CH 3 k 0 Bu t O + solvent-h Bu t O + Ph 2 CHOH Bu t OH + (solvent) Bu t OH + P h 2 COH k probe Bu t O + Bu t OH + k rxn OH signal carrier λ max 540 nm k growth = k 0 + k probe [probe] + k rxn [XH] k growth = k 0 ' + k rxn [XH] The technique allows the determination of the absolute rate constant for a reaction where all the reagents and all the products are invisible to the technique employed 9

10 The technique allows the determination of the absolute rate constant for a reaction where all the reagents and all the products are invisible to the technique employed Is there a catch? The method provides no information on the nature of the reaction; for example the mode or site of attack cannot be established by this method. The signals observed get weaker as the reactant is added. The rates are largely derived from conditions where the growth is fast and the signal weak. It is essential to select probes that overcome the second problem by giving intense, readily detectable signals. OH 10

11 The significance of growth rates All products from a reaction grow-in with a lifetime that is identical to the decay lifetime of their precursor. It is this characteristic that makes the probe technique possible This characteristic also implies that when two spectral bands grow-in with the same kinetics they have the same precursor. It does not mean that the two bands necesarily belong to the same species. 11

12 RCHBr-CH 2 Br hν Br + RCH-CH 2 Br RCH-CH 2 Br Br + RCH=CH 2 Br + Br Br 2 Time O.D. O.D. 0.2 µs Wavelength, nm 12

13 Analysis of the growth kinetics for Br 2 k growth = k 0 + k rxn [Rt 4 NBr] 8 k obs, 10 6 s k Q = 1.6x10 10 M -1 s [Et NBr], mm 4 13

14 The kinetics for invisible reactions can be determined by using the absorption from Br 2 as a probe k growth = k 0 + k Br [Br ] + k X [X] 7 k obs, 10 6 s k X = 3.9x10 7 M -1 s -1 3 [Br - ]= 50µM [2-propanol], M 14

15 Reate constants for reactions of bromine atoms Quencher k, 10 M s Q Methanol 0.93 Ethanol 16 1-Pentanol 11 1-Octanol 12 2-Octanol 35 2-Propanol 39 3-Pentanol 12 2-Methil-1-propanol 17 Dioxane 1.2 Ether 17 Toluene 66 Triethilamina p-cresol

16 Time resolved diffuse reflectance an alternate approach for opaque samples Laser Monochromator Sample PMT Detector Lamp Digitizer Computer 16

17 Decay of diphenylmethyl on silicagel Ph Diffuse reflectance under nitrogen Ph Ph O hν -CO 2 H A Ph J/J µs µs + B Time 17

18 Pulsed lasers As part of a method to study photoinitiated chemical reactions To induce new chemistry, different from that initiated by conventional sources As a light source, to initiate the same chemistry as with conventional sources 18

19 Photochemical source A laser and a lamp can give different products even if two photon processes do not occur hν CH x 10 5 s -1 (laser) 1 2 (lamp) 3 19

20 The photochemistry of tetraphenylacetone gives different products depending on the light source Ph Ph Ph O hν CCl 4 Ph Ph Ph Ph LAMP Ph Ph Ph CHCl LASER solvent CCl 4 20

21 Laser initiated two-photon processes Ground state reactants Excited state reactants Reaction Intermediates Ground state products hn hn Upper excited state reactants Excited Reaction Intermediates New chemistry 21

22 Halogen abstraction reactions of excited diphenylmethyl radicals are quite common. They are known to involve a charge transfer mechanism * H H Cl CCl x 10 8 M -1 s -1 H + ; CCl 4 22

23 Laser Flash Photolysis Employing two-color two-laser techniques Laser 1 Laser 2 Lamp Detector 23

24 The Laser Beam - Liquid Jet Argon Ion Laser 2 - Laserbeam 3 - Lens on Motor Positioner 4 - Capillary 5 - Glass Bulb 6 - Jet Stream 7 - Collecting Flask Filter 9 - Inert Gas Supply 10 - Low Pressure Tubing 11 - High Pressure Tubing 12 - HPLC Pump 13 - Projection Screen 24

25 The The laser-drop technique An An approach for for preparative multiphoton experiments in in organic chemistry 25

26 SINGLET OXYGEN EMISSION O 2 ( 1 g ) O 2 ( 3 Σ g ) 1269 nm 1588 nm O 2 ( 1 g ) + O 2 ( 1 g ) O 2 ( 3 Σ g ) + O 2 ( 3 Σ g ) "dimol emission" 634 nm 703 nm 26

27 Singlet oxygen time resolved detection Laser Attenuator preamp Sample Ge diode Si filter energy monitor Amplifier Digitizer Computer 27

28 CONDUCTIVITY SET-UPS V V beam beam blank Io + I V R L Vo + V R L R L ' 28

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