AOJA.1I1 7U7 ALI-ITA IJNIV EUp40NION DEPTOF CHEMI'STPY F/G 7/4VR AT IONA L S PECTRO! 0,COP, 0~ THE LECTODE-SOLUTION INTERPHA S F.;--ETC('l

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REPORT DOMUENTATIO14 PAGE

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Depertuent of Chemletry M-Vibrational Spectroeloly 01 t"o Elnctrodtt-Solutio Intorphah.V. Ulvit o Albt and 248k 202 RM-1

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Office Of INaval Rsnearch NoS 15r- YChemistry Pregra - CWIstry Cede 472 ~ ~ '

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*D"Werteent of Cheitryft. University

a.- ~~~Sootb.to. U.K.* 6ON5So . -

alcvchSty ISntrulctecuSml"~, matfltetl Sesctroscopy. WIN

The. *s~avfimet- dAosl for tbs 9etbsrirl of hi*h Iuality, lsirnlGiow Nis tle

fy, puEpo of the UiMt"d States owceot

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The *x1petkmentex Consideration$ ft"essary to afftect

successful recording of in situ vibrational spectrocopy~ at the

Oectcode-solution iuter9ic* Wve described. In this Work. the

Fourier transform infrared .ect.cmter is wsed.

IV. ~l1P3AI TPSSVAe 1MFAM~ 5p&Cy*AgCO#.t

Stanley Pos'an 1. D~do

DePArtesut at Chemistry W

University of AlbertaEdeaeton, Alberta, CanadeM96

MG 262

amd

A. Mewief 1,kbtU.

Department of cheistry &~lblt ~'The University D/1

Southampton I "apshtc

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although the use of Infrared etroacopy as an in siti meto of spectra with eubsequent subtraction gives the deaired

probe for observing interfacial phenomena during electrochemical result.

*apartments has been attempted any times In the last 20 years.

it ha only been in the last three years that high quality

reproducible spectra have been routinely obtained. This has been spectrometer

because of Wa the successful coupling of electrode modulation The instrument used in our recent Work has beem the Nicalat

techniques to the optical signal (1).* (b) the exploitation of the 'l Oir tranafoasicaed. spectrometer. TO perform these

multiptes advantage and high throughput of Fourier transform caper imentse the machine Should have the following featureas

spectrometers i2). and 4c) the use of more sophisticated 11) the ability to store. aml signet. average subequent spectra.

techniques such an polarisation modulation (33. As a result. in at least three separate data file. The software should

Investigations such as the study of adsorbed hydrogen an platinum b e flexible enough to specify which files is to be sue" for a

and rhodiM (4.5). the structure of Internediates in Igiven spectrum.

electrocatalytic osidatione (6i. the study of organic ion radical i 2) An output trigger Pulse (Preferably itL.aor CWW omatibles

intermediates 471. the adsorption of strylomittile it). th designating the beginning ad data osilectios by the A/D

planum. Interf ace is organic electrolytee (2.91). and the Iconverter of the instrument on sach scas.

structure ot water at various electrodesurf aces (1.10) have been (33 spectral ratiolIg and subtraction capability.

4 reprted. 441 Capability to handle mid-in fat detectors With stains

it to of Purpse at this paper to define the experimental values of I a 1910. such as 77cf-edimtelrd 11

t*ebAiqom 2 apparatus required to obtain mush results by using solid state units.

reotrer trawelers Infrared metheds. hlthouA* ties resolved is$ sample comartment mives lare sough to hold comparatively

spostresw is pessible using the techniques described herein, large cells mounted on adjustable reflection 4ttiachA&~

m e Will limit 60r dieueiom so sea9 steady-state meesuremns. Optical tables.

The the basic approach Is tA apply a potastial stop to an (6) Reasonably fast data collection time.

elect~os wit f9W Steady state Conditione to develop, and take (73 Sesolution of a cm-1 or better.

retu1ned to a Mas genestiel * asd the @Cdabdue repeated. The The moat convenient. fore in which to present spectra is an a

entie Ccleto opet" se te secta ae sinalwwwoge todifference in Infrared transmission of tie cell at ach Of thethe desired simlt-ielevel, Appropriate ratioiag of the a

a " a M a r r a i d W .

." C t r

. " p o t n t i l i s t h e

D a t C L V

<at t i '

A9V

two electrode plariXationk status. This diffterence will then to mae" to butt a rubber gasket against the fixed sleeve by a not at

due to changes in the iaterphame brougt about by the dti fereces the and of the assembly to seal icnl't %t cell barrel, The

in potetial, the optical PCoprties of the rest of the cell brans rod was cowered with a thin layer of eposy betore sealiny

remaining constant. to term of the measured coliectivitias at it into the Eel-F &leeve to prevent any Chace of leakage of

the two potentials, *I and 22u. this difference in tiransision solution between the electrode and the sleeve. RIltrden

can be written a 3/l l a quantity which is readily obtained prepared in this sanner are very stable menchanically and

using software Normally provided with commercial WTIR chemically in most solvents and electrolytes for several

spectrometers. in practice, it Is mst convenient to calculate m onths. For instance, we have sed I fl sulfuric acid, I IS

&2/21-1 em 81/111 - R1/R1. This ltter quantity in simply the perebloric acid, stonitrile, mathylene chloride.

difference between two single bean spectra, each of which has Idinethylforeanide, dinethylacetamide. and dioblocoethene for

been ratioed to the ohosene reference state Rl. Presentation off etended periods without degradation of electrd performance.

the spectra in thin foae in them equivalent to the Lie/S C lectrodes are typically polishe by nountime in a sturdy

presentation ued is MUiM (as/f is equivalent to tN21ml aleMinvon 319 to amiamin perpendicular contact with the polishing

I pad. or on a commrcial polishing machine. With reasonable mace.alecochemical inetta~tatio'

the potential. we ootolied at the working mirror electrodeelcrdsfatrtnA/atS&rm robasaevlu

these rather simple techniques.by a ai-Tek iatrmnta Y1GA potentiostat driven by a PP21

wavesex geeraor.ghm loas& omptersuppieda IL pt" oEves though the electrode arae reasonably flat, it is

aw cnnecor a th sawpass an achNewceaneasry to take additional care to assure that the tace is

mitiste. 'hispal& Mewoo tot~iW te weelom gnertorparallel to the optical winnow, so that a vmiforim solution layer

via 7496 % a-doa e~matc. *andis~sin.)thickness will exist there, this is accomplished by allowinge the

optical windo to be bonded to Its grommed glass sleeve with both

Electrodes a"d Cell sleeve and electrode An plae in the cell and with the window

Electrodes (Ceical E1letics Associates, 133 Smouth resting an the face at the meoted electrode, pressure being

Coenty RDm". P.O. amw 313. PNAm beach, Pie.) were oestructed maintained against the window sinultameewesly to keep it

f rem a 2 me thick - I me diamter disk 0f the desired material absolutely flat against this electrode face Itigae II). the

ffimed to the Md of a 7mis - 135 a brass cod which had bee, electrode, Window cap, am cell body weerhdto maintaint

heat/ressm aitted into a s.1-F sleeve (o.0. - 9 mi.* A looms reproducible realignment in abeequent experiments. When the

fitting Eel-P sleeve at the rear of the electrode assembly was window was prepared in this mNannr. typical fluctuations is gap

:n1

~V

AA I

7

size of 6S.US MicOrowae obtained in WOMMOss re ts ErOn side to reflect Iran the electrode surf ace at a dt.- ged mPAle.

side aroa the electrode foa using the Integrated atiiwtiom Subsequently. the boomseaat he gatugasdto its original path a

* Coetfficient of the acetonitgile C&M stretch fundamental closely "s possible so ad not to affect the purpose of the

aborption hend as a masure of the gaP thckness, focussing optics of the Output detector sectios of the

The Call IChemical Electronics Asociate.. Inc.) was similar Spectrmter. Several designs for a apparatus to perform this

to that described by Sewick at &I fog use in electrochemaically gefnction are possible. Wie have Used a modified versica of as

modulated Infrared ref lectance spectroscopy 1101210) 111). It WAS apparatus described by Merrick 412).

125 Us ia overall length without the electrode mounted. and held polarization of the radiation was effected by mouting a Met

10 cm3 of solution. iTh, optical window was mounted on a T 24 substrate transmission polarizer (Cmridge Phyical Seienes.

female ground glass joiat. When in place, the working electrode jCambridge, Bogland, "yp 105225) in the bass either in freat of

disk Say be pushed up flush to the window. A Leggjin reference orbehind the call. The polarizer vas Mounted in & calibrated

Capillary was mounted with itn tip close to the window where the housing that could be rotated so that a" polarization a"s

electrode face rest&. The Lwugia is connected through a ground coud be conveniently chosen.

*glass stopcok to the reference electrode *department. ASolvents and Chemicals

platinum wiv, loop was mounted soch that the loop was cosialDlue to the estramely high Sensitivity of the method. it IS

with the Mounted working electrode to serve as the secondaryelecrod. Puge as nletcmioutet cnnetios wae - atnecessary to use very pure solventsa m electrolytes fot routineelinvstigaions Pue have folnd mwa thele useo wag mom grad

the bottam and top af the main cell body. md the working inestigatolntsw ae suithat for mas lowmi igadedi

electrode mnurtimg tuba was located at the Me.comrilslet *suabefr atgam Iemdae

A mnall p~ation wire to be used as a subsidiary reference, tde 7.wie9tbCprfcto fUM %P81

electrode say be mounted through the Luggin tubs just helow usalteurdfrsestvhdopinerdul ae tde

stopcockL to provide a low impedance path MM reduce high* frqueny iterfrenc. Wam ued. t ws Ociteced hrouh aThe, drying of suppotimg electrolytes suoh as lithiwa

firemoc Intrfeenc. whn g". t wa 000aced trouh aPerchalorateato tetraalkylinonliue salts should be effected with a6.1 or capacitor to the Ngema refaeenc electrode,vaumdnfo tlst4hurathe09 Fsie

Ilflostonce attaubmeat temperatures. Transfer* of electrolytes O abslutions he the

the onaverging heom ot radiation through the sample Call should he ade in a dry atmoseuere.

CO~prtbeft of the Spectrot Set he Intercepted sad made to

"WhU.TlI AND DIliCUlSRI fte the counter. i.e. every 16 scee" of the spectrometer. The

he an eseaple of a tyV&cal experimst. It was desiced toaeom uertr~r~ur

reodtespectrum 09the bensophenteme ketyl species formedbydrtolaetIscnlngrhntesptomerC te o

the me l~cnm rdacionof hnsabanme a a latnumsean I spectra) such that the electrode potential wstaken.t

elecrod. A10 N soutin o betelbeftme & dgamed 2-50 V OAg/Ag reference) for 9 a then returned to the base

anhydrous 0.16 1 tetrahutylesnfim tOt tlmURVOLOrate value of416 a -1. 70 - until the spctrm"ter initiated te7th scanThe lecrod Wa, Pace flsh gatAL he ellWL , .MW ad the Complete sequence was reputed.

all 0s to reins a&elnt the tubber gasket on the otrod A softwre progamw writtoo to perform eight sas. of

assembly. Using the 30 coo- acetooitrile bond. te sotution wichd only tihe last fout ware ca-eddsd mo saved is a reference

thi~WAS Wonto* tobe aoutS M~g .M dterir~dby hefit. this or oration allowed about lour seconds (the first four

r t inu m to h . te i heun sd Sce@) for the C ll to CUMs to A Steady State. The

I progrom ha celled for eight *emmoto bemade, again

d 9MS!! discarding the HMrs four, bet this tie storing the oo-adddG ~last four in a sompt filu. This "seration us repeated lv times

d is the molust" thickness. A Vt M- 'soniiance. a ia the so that a total of forty co-added Spectra resulted in the

entittiim CHIC404.C i theCOM~ttei*ROf te aoarbngreference file ad the same in the Simle, file. Tis program was

mrsc". nd istheange a lot a th relecinginterfaced synchronously to the Wae~form generator through thespecies @n pus isd the angle coute circiderc. at tbrflctn

surface. t polariser us set to pass the oneomenot of lightben cnpneadte710ontricur.Thsilspetra wers gathered at the approsisate points indicated in

that had Its electric field vector parallel, to the IncidenceFie 2.AOMPGothalt"cmpedemtisaaplane, so that the field would have a earn-into sugnitude at the iu 2.A apeo h pcrscmue o hsdt

I in the momenr described in the experimental section is sowos inelectrede surface.

The 'begin a"* WI. pulse available f rom the computer ad Fiue,()

the 116specromteruse eed- inut o a741Wbinry aically, the peaks ettending usnierde correspond to thetheenve ofI Seectroeeter subtrte ate the eInput to the0bnayu

cousac Whose binary output bed Initially been preet, to binary rmvlo -abmm usrt.a h SOMO b

output 11 (1111). the "Moutput of the counter uas connected to fraino ey 1 oetn~gpas.ACl

the *Start TM! input at the 5551 waefceom generator so that tedescription of this spectrum Dhas bees repeden 47).

latter esecuad OWe waveform sequence M every 0 1 transition " pcr sFgrs()md()wg bandI

similar meaner. Details are provided io the figure Igna

AN--

.;7n

* ~. Maim4

-- r .4 el

712

Nigher sensitivity Was needed to obsreve changes In the Zt~3I

population of spec ie as the double lay.. structure was changed

at a platinum electrode. A thinner aolution layer 10.75 micr-ons)1.ASei, . unat.adS.Is.Eero i.Aca2

amd 160 averaged spectra at each potential state was utilised. I(1950) 465. A. Bewick and K. Kunktae Surf. Sci. 101

The electrolyte "a 0.106M tatrabutylammonius 15111

tetrafluaoroborate. The resulting difference spectra are OHMw in.7 eisn .inA Mwc.md91 t~~. 3

F'~iur (3. The affect at added water for the nase eaperiment is Blectroatel. Chem. 12% (19411 237.

shown In Figure (71. These spectra have been Interpreted 3. .W. Russell. a3. Owereed. R. Scenlc.. X.M. Severson. end A.

2lsewhere (63. 1 Sewick. J1. thys. Chem., in press.

It is clear f rom the spectra shown that the technique has 4 A. Newick, S. Munimatsm. J1. Robinson. and .3. Russell. ..

the sensitivity to detect Changes approaching 10-6 A",Iin Electroasal. Chem. 132 (19S21 320.

expegimP-s collecting data frome ISS scene at each potential, the S. A. Renick end ... Russell, Ji. Slectroamal. die. is pess.

total esperisental tim being about 10 win. ?bus the method 6. a. Baen. A. Sewick. a. auaimatsu, sad C. Lamy. .

seem wall suited for the obtaining of vibrational spectra at the Blectroanal. Chem. 121 (19311 243.

eleCtrode-eolatioa isterf ace In Situ, and Should be Sitable for 7. 5. Posts. 1. Davides. savid A. Remick. J1. Blectroem. Soc.,

the structural detereination of a variety of catalytic, adsorbed. submitted.

aOW short-lived soletice-f rae Intermediates focreed at such 6 .Swc.C iieo 3 lcrea.de.*sbitd

interface*. a. S. Pons. P. Davidson. andl A. Renick. J1. 3Slectroesal. Che..

submitted.

La. A. "wuick and 9. Kifasasu J3. Klectroastal. dRIM..

Part of this work was supported by. the office of Naval sbitd

Chem.. submitted.

12. M. Herrick. Apol. optics 10 11~ 2344.

f72

4.4

.. ....

13

(1) Cell cap and electrode tip configuration.

121 Timing foe s ectra asuisition. Points (dI represent I i

sectra ttat are discarded. points (al represent spectra

that act a ade and 0c-addod. Diagram is for Case Where more

absorbing apsna see presnt at high sampling potential.

£3) a) Transmission spectrum of bensophenune. (b) Difference br WOMAN

spectm between -V.?S V and -2.50 V 41.V a benzophnone in PI

0.10 A VDAF In ftetonitrile). Downwacd estendig leaks are P20

few the ketyl anion.I 0

(41 a) Transmission spectrum of athracens. fbi Difference i+

spectrum between -1.54 V and -2.S0 V. -'

151 a) transmission spectrum of tetcacysnoetbyiene. (b) am beitjDifference spectrum betweem 40.S and -0.2 V.

(6) Difference spectra of amydrous 0.10 tetreutylamLu

teorafluoroborato.

(7) Soms am Figure 4, cept. 0.10 x umo include.

TI .-.

... .. + + .... I N 4 ....... ++ + . ~~~~~ ~~~.... ... " + " +a:++ ' +'+

cbO' 36bO 32bo aabo 24bo zobo i 6bo 120 0bW*ENUMBERS

IZkoi7i

'TJ

*000 36bo .32bo 2abo 2tbo 2zbo 1 600 1200 -aboWqV~ENUM3ERS

b

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