Application of Time-Resolved Fourier-Transform Infrared Spectroscopy to Photodissociation Dynamics Application of Time-Resolved Fourier-Transform Infrared.

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Application of Time-Resolved Fourier-Transform Infrared Spectroscopy to Photodissociation Dynamics Application of Time-Resolved Fourier-Transform Infrared Spectroscopy to Photodissociation Dynamics Yuan-Pern Lee, Department of Applied Chemistry and Institute of Molecular Science National Chiao Tung University, Hsinchu, Taiwan

OutlineOutline Introduction of step-scan FTS Emission mode – slit-jet system Photolysis of Fluoro-compound Emission mode – flow system Cl + CH 3 SH, O( 1 D) + CO Absorption mode – White cell C 6 H 5 SO 2 and its reactions Introduction of step-scan FTS Emission mode – slit-jet system Photolysis of Fluoro-compound Emission mode – flow system Cl + CH 3 SH, O( 1 D) + CO Absorption mode – White cell C 6 H 5 SO 2 and its reactions

The Michelson Interferometer

Step-scan Data Acquisition t1t2t3t4t5t6 t1t2t3t4t5t6 x7x7 x1x1 x2x2 x3x3 x4x4 x5x5 x6x6 I time

Experimental Setup (Emission) 10 ns / 0.1  s 0.1 / 0.25 cm ns / 0.1  s 0.1 / 0.25 cm -1

Photolysis of Vinyl Chloride HCCH + HCl (4-center) C Cl h h + Cl HCCH + H C 2 H 2 Cl + H HCCH + Cl HCCCl + H 2 :CC + H 2 :CCH 2 + HCl (3-center) H H Cl H H H H H H

Rotational Distribution of HCl (v)

HCl-elimination from C 2 H 3 Cl Bimodal rotational distribution of HCl(v) high J (3-center) low J (4-center) T rot  10,000 K T rot  500 K T vib  16,000 K peaked at v' = 2 ratio 83: 17 Evidence of “kick” from vinylidene  acetylene Vibrational adiabaticity? J. Chem. Phys. 114, 160 (2001)

C Cl h F FH FCCCl + HF (4-center) :CCF 2 + HCl (3-center) :CCF 2 FCCF X Photolysis of CF 2 CHCl at 193 nm J. Chem. Phys. 117, 9785 (2002)

Configuration of twin slit jets

TR-FTS with Twin Slit Jets Slit-Jet

Comparison of rot. distribution jet theory flow REMPI

Photolysis of Fluorobenzene at 193 nm

HF Emission from C 6 H 5 F (jet) at 248 nm

Rotational populations of HF after photolysis of C 6 H 5 F/He ~30 mTorr at 248 nm

Vibrational population of HF  

Photolysis of C 6 H 5 F at 193 nm Nascent internal energy of HF E rot = 15  2 kJ mol -1 (17  2 kJ mol -1 ) E vib = 34  4 kJ mol -1 (37  4 kJ mol -1 ) E ava = 284 kJ mol -1 ; E trans = 96 kJ mol -1 ; E HF = 48 kJ mol -1 (54  6 kJ mol -1 ) E C6H4 = 140 kJ mol -1 (134  8 kJ mol -1 ?) Nascent internal energy of HF E rot = 15  2 kJ mol -1 (17  2 kJ mol -1 ) E vib = 34  4 kJ mol -1 (37  4 kJ mol -1 ) E ava = 284 kJ mol -1 ; E trans = 96 kJ mol -1 ; E HF = 48 kJ mol -1 (54  6 kJ mol -1 ) E C6H4 = 140 kJ mol -1 (134  8 kJ mol -1 ?)

Photolysis of CH 3 (C 6 H 4 )F at 193 nm

109.7 kcal mol kcal mol kcal mol kcal mol -1

PES for HF-elimination of o-Fluorotoluene

Transition States of CH 3 (C 6 H 4 )F Species R HF /Å E vib /kJ mol -1 Angle E rot (expt) /kJ mol -1 E rot (impulse) /kJ mol -1 CH 2 CHF (528 kJ) ±9 (0.157) 8.2  (219 kJ) CF 2 CHCl (458 kJ) ±6 (0.100) 17.0  (199 kJ) 20±416 C 6 H 5 F (284 kJ) ±6 (0.120) 32.8  (56 kJ) 15±414 CH 3 C 6 H 4 F (251 kJ) 1.08 ~26±5 (0.103) 27.0  (59 kJ) ~10±211

IR emission from C 6 H 5 F irradiation at 248 nm

Dynamics in Bimolecular Reactions

Products are not produced instantly –Needs collisions –Depends on rate coefficients Rotational quenching might be substantial –Non-negligible after 1  s Nascent vibrational populations –Less affected by quenching –Extrapolation to t = 0 might have errors Products are not produced instantly –Needs collisions –Depends on rate coefficients Rotational quenching might be substantial –Non-negligible after 1  s Nascent vibrational populations –Less affected by quenching –Extrapolation to t = 0 might have errors

Previous Derivation of Rot. Distrib.

Rotational Temperatures of HCl (v = 1) from Cl + H 2 S J. Chem. Phys. 119, 4229 (2003)

Temporal Profiles of HCl (v = 1, 2) Model of fitting Cl + H 2 S  HCl (v = 2) + HS k 2 Cl + H 2 S  HCl (v = 1) + HS k 1 HCl (v = 2)  HCl (v = 1) k q2 HCl (v = 1)  HCl (v = 0) k q1 Model of fitting Cl + H 2 S  HCl (v = 2) + HS k 2 Cl + H 2 S  HCl (v = 1) + HS k 1 HCl (v = 2)  HCl (v = 1) k q2 HCl (v = 1)  HCl (v = 0) k q1

Comparison of Cl + H 2 S and Cl +CH 3 SH Cl + H 2 SCl + CH 3 SH frfr 0.12   0.02 fvfv 0.33   0.10 H...Cl1.619 Å1.675 Å D-effectrate ~0.50little effect TS (adduct)longershort-lived J. Chem. Phys. 120, 1792 (2004)

Transition States of Cl + CH 3 SH

Dynamics of the O( 1 D) +CO reaction

E-V energy transfer Long-lived CO 2 * collision complex Harding/Weston.Flynn JCP 88, 3590 (1988)

Comparison of Literature Values on Efficiency E-V energy transfer efficiency E-V energy transfer efficiency 40 % Slanger et al. (1974) Expt. 40 % Slanger et al. (1974) Expt. 21 % Shortridge et al. (1976) Expt. 21 % Shortridge et al. (1976) Expt. 25 % Harding et al. (1988) Expt. 25 % Harding et al. (1988) Expt. 31 % Matsumi et al. (1994) Expt. 31 % Matsumi et al. (1994) Expt. 29 % Makoto et al. (1994) Expt. 29 % Makoto et al. (1994) Expt. 29 % Tully (1974) Theor. 29 % Tully (1974) Theor. 21 % Kinnersly (1979) Theor. 21 % Kinnersly (1979) Theor.

( ● ) experimental work; ( ○ ) trajectory calculation; (Δ) Harding et al. ( □ ) Shortridge et al. Comparison of CO Vibrational Distribution J. P. C. 1994, 98, Makoto Abe, Yousuke Inagaki, Larry L. Springsteen, Yutaka Matsumi, and Masahiro Kawasaki, Hiroto Tachikawa J. P. C. 1994, 98, Makoto Abe, Yousuke Inagaki, Larry L. Springsteen, Yutaka Matsumi, Masahiro Kawasaki, Hiroto Tachikawa

J. P. C. 1994, 98, Makoto Abe, Yousuke Inagaki, Larry L. Springsteen, Yutaka Matsumi, Masahiro Kawasaki, Hiroto Tachikawa CO Rotational Distribution

Infrared emission spectra of CO

Comparison with Abe et al.

Detection of Intermediates TR-FTS in absorption mode

Experimental Setup for TRS-Absorption

Absorption of Cl 2 SO irradiated at 248 nm resolution = 1.5 cm -1 ; laser fluence = 100 mJ cm -2 Cl 2 SO = 0.35, Ar = 24.4 TorrCl 2 SO = 0.35, Ar = 1.5 Torr J. Chem. Phys. 120, 3179 (2004)

Simulated spectrum of ClSO at 300 K - Simulated - Experiment Resolution = 0.3cm -1; A’/A”, B’/B”, C’/C” = , , a-type/b-type = 1/0.2; J max =120; temp. = 350 K

Photolysis of C 6 H 5 SO 2 Cl

C 6 H 5 SO 2 Cl irradiated at 248 nm in a static cell C 6 H 5 SO 2 Cl = ~140 mTorr after 248 nm irradiating for 2 min at 10 Hz R = 0.5 cm -1

Transient absorption upon photolysis of C 6 H 5 SO 2 Cl at 248 nm P : , , , cm -1 A1 : cm -1 A2 : cm -1 S : cm -1 (SO 2 s-str.) Temp.= 80  C R = 2 cm -1 7 expt. ave. 0-7  s static C 6 H 5 SO 2 Cl C 6 H 5 SO 2 Cl / N 2 = 1 / 240 at P = 72 Torr

Photolysis of C 6 H 5 SO 2 Cl  C 6 H 5 SO 2 Photolysis of C 6 H 5 SO 2 Cl  C 6 H 5 SO 2 Reaction of C 6 H 5 with SO 2  C 6 H 5 SO 2 Reaction of C 6 H 5 with SO 2  C 6 H 5 SO 2 C 6 H 5 Cl  C 6 H 5 + Cl C 6 H 5 Br  C 6 H 5 + Br C 6 H 5 Cl  C 6 H 5 + Cl C 6 H 5 Br  C 6 H 5 + Br

Reaction of C 6 H 5 and SO 2 A1 : cm -1 ; A2 : cm -1 B1 : / cm -1 ; B2 : cm -1 C 6 H 5 SO 2 Cl / N 2 C 6 H 5 Cl / SO 2 / N 2 = 1 / 14 / 100 at P = 59 Torr C 6 H 5 Br / SO 2 / N 2 = 1 / 10 / 150 at P = 63 Torr T= 80  C R = 2 cm -1 7 expt. Ave  s T = 25  C R = 4 cm  s T = 25  C R = 1.5 cm -1 8 expt. ave  s

Possible products: C 6 H 5 SO 2 C 6 H 5 OSO C 6 H 4 SO 2 Possible products: C 6 H 5 SO 2 C 6 H 5 OSO C 6 H 4 SO 2

Prediction of harmonic frequencies by DFT calculation C 6 H 5 SO 2 C 6 H 5 OSOC 6 H 4 SO 2 Exp. harmonic frequencies (5.0) / (13.6)986.5 (0.2)963.6 (0.03) (1.4) / (0.6) (0.1) (0.9) (8.3) / (24) (0.9) (1.7) (16) / (21.4) (9.8) (9.1) (93) / (56.8) (9.4) (0.5) (7.9) / (7.2) (170.9) (328) (0.1) / (0.2) (1.8) (33.8) (1.3) / (2.0) (14.0) (0.9) (111) / (106) (121.7) (203) (0.2) / (0.5) (0.2) (20.5) ?? (2.5) / (2.8) (0.8) (20.8) (12.2) / (10.8) (2.6) (23.3) B3P86 / P3LYP with aug-cc-pVTZB3P86 with aug-cc-pVTZB3P86 with G** C 6 H 5 SO 2 C 6 H 5 OSO C 6 H 4 SO 2 Exp (8.3) / (24) (0.9) (1.7) (16) / (21.4) (9.8) (9.1) (93) / (56.8) (9.4) (0.5) (7.9) / (7.2) (170.9) (328) (0.1) / (0.2) (1.8) (33.8) (1.3) / (2.0) (14.0) (0.9) (111)/ (106) (121.7) (203) (0.2) / (0.5) (0.2) (20.5) ? (2.5) / (2.8) (0.8) (20.8) (12) / (10.8) (2.6) (23.3) B3P86 / P3LYP B3P86 B3P86 with aug-cc-pVTZ with aug-cc-pVTZ with 6-311G**

Simulated spectrum of C 6 H 5 SO 2 simulation parameters A  = cm -1 B  = cm -1 C  = cm -1 A/A  = B/B  = C/C  = Temp. = 300K J max =130 b-type:c-type = 1 : 0.3 T 0 = cm -1

Reaction of C 6 H 5 Br + SO nm Reaction of C 6 H 5 Cl + SO nm C 6 H 5 + SO 2  (C 6 H 5 OSO)  C 6 H 4 OSOH  C 6 H 5 SO 2  C 6 H 5 SO 2 Br C 6 H 5 + SO 2  (C 6 H 5 OSO)  C 6 H 4 OSOH  C 6 H 5 SO 2  C 6 H 5 SO 2 Cl

 =4.6  10 3 s cm -1 Bn(3700) temporal profile of C 6 H 5 Br + SO 2 at 248 nm  =4.4  10 3 s -1 Bn  =1.3  10 4 s -1 An  =3.1  10 3 s -1 Cn C 6 H 5 SO 2 C 6 H 4 OSOH C 6 H 5 SO 2 B r

Summary Transient absorption bands at 1278 and 1088 cm -1, observed upon photolysis of C 6 H 5 SO 2 Cl at 248 nm, are assigned as the SO 2 stretching modes of C 6 H 5 SO 2. Same bands were observed from reactions of C 6 H 5 with SO 2 using C 6 H 5 Cl and C 6 H 5 Br as precursors. Additional transient absorption bands at 1203, 1408, and 3607 cm -1, observed upon reaction of C 6 H 5 with SO 2, might be due to C 6 H 4 SOH. Kinetics for formation of C 6 H 5 SO 2 and C 6 H 4 SOH are discussed.

SUMMARY Applications of Time-resolved FTIR Dynamics in Photolysis 4-center molecular elimination of HF Dynamics in Bimolecular Reactions Cl + H 2 S/CH 3 SH, O( 1 D) + CO Detection of Intermediates (absorption) ClSO, ClCS, C 6 H 5 SO 2 Multiplex advantage Applications of Time-resolved FTIR Dynamics in Photolysis 4-center molecular elimination of HF Dynamics in Bimolecular Reactions Cl + H 2 S/CH 3 SH, O( 1 D) + CO Detection of Intermediates (absorption) ClSO, ClCS, C 6 H 5 SO 2 Multiplex advantage

Chia-Yan Wu, Li-Kang Chu Sherry Liao, Shen-Kai Yang Chia-Yan Wu, Li-Kang Chu Sherry Liao, Shen-Kai Yang Ministry of Education National Science Council IAMS, Academia Sinica Ministry of Education National Science Council IAMS, Academia Sinica