Spectrochimica Acta Part A 55 (1999) 1337 – 1345

Resonance Raman excitation profile for uranyl acetate in

dimethyl sulfoxide
Takeshi Soga *, Ken Ohwada
Department of Material Science, Japan Atomic Energy Research Institute, Tokai-mura, Ibaraki-ken 319 -11, Japan

Received 14 February 1998; accepted 5 October 1998

Abstract

The intensity of Raman lines of uranyl acetate/UO2(CH3COO)2 in dimethyl sulfoxide has been measured as a
function of excitation energy in the region of the Laport-forbidden f – f electronic transitions, using ten output lines
of an argon-ion laser. The resonance Raman excitation profile of the totally symmetric stretching vibration of the
uranyl observed at 829 cm − 1 shows vibrational fine structure, which resembles the vibronic structure of the electronic
absorption spectrum but does not completely coincide. Experimental excitation profile is compared to that calculated
using transform theory with parameters derived from the observed absorption spectrum of the resonant electronic
state of interest. The non-Condon model (generalized B, C-term source of scattering) gives relatively good agreement
with experimental results. The disagreement between the experimental data and the calculated resonance Raman
excitation profile may be ascribed to interference between the weak scattering from the neighboring forbidden
electronic states and strong preresonance scattering from allowed electronic states at higher level. The change in the
UO equilibrium bond length resulting from the 1Sg+ “ 1Fg electronic transition is found to be 0.068 Å. © 1999
Elsevier Science B.V. All rights reserved.

Keywords: Excitation; Raman; Resonance; Uranyl acetate

1. Introduction high intensity overtone progressions for the same

fundamental vibration, especially in the case of an
Resonance Raman spectra are obtained when a electric-dipole-allowed transition. In such studies,
molecule is excited with a laser beam whose fre- it has been realized that the dependence of the
quency corresponds or closely corresponds to an Raman intensity on the wavelength of exciting
electronic transition frequency of the molecule. light, i.e. the Raman excitation profile (REP) for
Such spectra are frequently characterized by an the scattered mode, as well as the electronic ab-
enormous intensity enhancement of the band aris- sorption spectrum (ABS), can provide useful in-
ing from a totally symmetric fundamental vibra- formation on the character of resonant excited
tion of the molecule, together with appearance of states. Therefore, the analysis of the REP is indis-
pensable for understanding the resonant excited
* Corresponding author. electronic state of interest. Existence of a close

1386-1425/99/$ - see front matter © 1999 Elsevier Science B.V. All rights reserved.
PII: S 1 3 8 6 - 1 4 2 5 ( 9 8 ) 0 0 3 0 6 - 0
1338 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345

theoretical relation between the ABS and the Tokyo, Japan) was dissolved in DMSO of ana-
REP, which are the quite different experimental lytical reagent grade without further purification.
observations, has been known for many years, The 0.48 and 0.048 M UO2(CH3COO)2 –DMSO
and the relation emerged recently in the form of solutions were used in the Raman spectral and
useful transform methods for determining REPs the electronic (vibronic) absorption measure-
from observed ABSs. By introducing the adia- ments, respectively.
batic approximation along only one normal co-
ordinate identified with the vibrational state
2.2. Raman scattering measurements
being examined in the Raman experiment, Stal-
lard et al. [1] derived a powerful transform law
The Raman spectra were recorded within the
for the Stokes scattering of a totally symmetric
region of 4000 cm − 1 using the excitation lines
vibration. The great advantage of the transform
at 528.7, 514.5, 501.7, 496.5, 488.0, 476.5, 472.7,
method is that, despite the fact that the Raman
465.8, 457.9, and 454.5 nm with an argon ion
excitation profile is a multimode-dependent
laser (Spectra Physics Model 168-11/265). The
function, only parameters associated with the
laser power ranged from 100 to 150 mW. The
particular vibrational mode under consideration
beam was passed through the sample solution
are used. The transform technique have been
contained in the 5 ml single-path quartz cell
proven very useful in analyzing the resonance
(10×10×50 mm) at room temperature. Scat-
Raman spectra of molecules and crystals that
tered light was collected in some small solid an-
contain many modes of vibrations [2 – 5].
gle around an observation direction at 90° to
Recently, we have obtained the REP of the
that of the incident light using an f/1.2 lens and
uranyl symmetric stretching vibration at 835
focused on the entrance slit of a 1 m double
cm − 1 of uranyl nitrate in dimethyl sulfoxide
monochromator (Japan Spectroscopic CT-
and have found that the REP resembles the vi-
1000D), equipped with holographic gratings and
bronic structure of the electronic absorption
a scanning control unit (Japan Spectroscopic
spectrum [6]. In this paper, we shall pay atten-
SMD-80). Detection was carried out by a pho-
tion to the uranyl acetate-dimethyl sulfoxide sys-
tomultiplier tube (Hamamatsu Photonics R-464),
tem to examine the ligand effect on the REP in
coupled with a two-phase lock-in amplifier (NF
comparison with the uranyl nitrate-dimetyl sul-
Electronic Instruments 5610B). The frequencies
foxid system [6] (the bond between CH3COO −
quoted are accurate to 1 cm − 1. The Raman line
group and uranyl is less ionic than that between
at 1044 cm − 1 of DMSO was used as an internal
NO3− and uranyl) and to estimate the equi-
intensity reference for Raman scattering of the
librium conformation of the uranyl ion in the
uranyl symmetric stretching vibration, because
excited state 1Fg. Transform methods are ap-
DMSO does not decompose with long exposure
plied to analysis of the observed REP obtained
to the laser beam and shows no resonance Ra-
in resonance with the excited electronic state.
man effect [6].

2. Experimental 2.3. Electronic absorption spectral measurements

2.1. Preparation of sample solutions The absorption spectra of the solution con-
tained in the 5-ml quartz cell (10 ×10× 50 mm)
Dimethyl sulfoxide (DMSO) was chosen as were measured at room temperature in the re-
the solvent for the spectral measurements, be- gion from 300 to 700 nm with a spectrophoto-
cause its Raman lines can be conveniently used meter (Japan Spectroscopic Ubest-50). No
as internal intensity standards. The stoichiomet- change was observed in the UV and visible ab-
ric amounts of uranyl acetate, UO2(CH3COO)2 sorption spectra before or after long exposure to
(guaranteed reagent grade, Koso Chemical, the laser beam.
 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345 1339

Fig. 1. Electronic absorption spectrum of the uranyl acetate – dimethyl sulfoxide system at room temperature. Peaks at 492.5, 476.0
and 460.5 are attributed to the 1Sg+ “ 1Fg transition. The vertical arrows indicate the laser lines used for excitation of Raman
spectra.

3. Results and discussion categories [7]: (I) the absorption situated between
500 and 445 nm consists of three well resolved
The ABS of uranyl acetate in dimethyl sulfox- peaks at 492.5, 476.5, and 460.5 nm attributed to
ide measured at room temperature is shown in the 1Sg+ “ 1Fg transition, and; (II) the absorption
Fig. 1, together with the wave lengths of laser situated between 445 and 370 nm consists of
lines indicated by arrows. In the ABS, the uranyl unresolved peaks of the 1Sg+ “ 1Dg transition.
ion has an intense structureless (electric-dipole-al- The intensity of the Raman lines of uranyl
lowed electronic transition) absorption band in acetate, UO2(CH3COO)2 in the DMSO solution
the shorter wavelength region (330 – 375 nm) and has been measured as a function of exciting ener-
a series of medium intensity bands, Laport-forbid- gies (ten output lines of argon-ion laser) in the
den f–f electronic transition in the wavelength vicinity of vibronically allowed electronic transi-
region from 370 to 500 nm. These are changed by tions ranging from 500 to 445 nm (1Sg+ “ 1Fg
the host matrices around the uranyl ion, such as transition). The Raman spectrum observed with
CH3COO − , NO3− , and DMSO. The vibronic the 514 nm line of an argon-ion laser, which is the
structure of the latter band is subdivided into two most frequently used exciting source, at room
1340 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345

Fig. 2. Resonance Raman spectrum of uranyl acetate in dimethyl sulfoxide below 2000 cm − 1, observed with exciting light of 514.5
nm. The Raman lines due to the uranyl ion are indicated with arrows in the figure. The weak broad band (asterisked) around 1600
cm − 1 may be assigned to the bound acetate group, the remaining lines to DMSO.

temperature is shown in Fig. 2. The Raman lines 476.5, and 514.5 nm). From this one can see that
due to the uranyl ion, in the UO2(CH3COO)2 – the intensity of the Raman line at 829 cm − 1,
DMSO system, are indicated with arrows in the change markedly depending on the wavelength of
figure. The linear uranyl group, OUO would of excitation light. The REP for the uranyl symmet-
course be expected to show two Raman active ric mode is a convenient means of showing this
fundamental frequencies at about 830 and 200 correlation qualitatively. In order to obtain the
cm − 1 which have been assigned to the totally accurate experimental REP, one needs to know
symmetric stretching and bending vibrations re- accurate scattering intensities of an objective
spectively [8]. The two bands at 829 and 206 Raman mode. However, the experimental deter-
cm − 1 can be readily assigned to the two Raman mination of such intensities is commonly difficult,
active modes of the uranyl symmetric stretching particularly when the resulting intensities are to
and bending vibrations, respectively [6]. The weak be placed on an absolute scaler. For this reason,
broad band around 1600 cm − 1 (indicated by an we here employed relative intensities of the uranyl
asterisk) may be assigned to the bound acetate totally symmetric stretching mode (829 cm − 1) to
group and the remaining lines to DMSO. No the internal standard of DMSO (1044 cm − 1),
Raman band was observed in the overtone and which show no resonance Raman effect. The
combination regions. This point will be discussed closely spaced peaks at 1044 and 954 cm − 1 (due
later in relation to the resonance interaction be- to DMSO) and 829 cm − 1 (due to uranyl) were
tween the exciting laser line and the vibrational well resolved (Fig. 3) and their band intensities
levels in the excited electronic state. were determined as the products of peak height
Fig. 3 illustrates the enlarged view of the uranyl and full-width-at-half-maximum. The relative in-
symmetric stretching vibration at 829 cm − 1 for tensity was determined as the average of five runs
three different wavelengths of excitation (454.5, for each excitation line. The absorption of excit-
 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345 1341

Fig. 3. The enlarged view of the resonance Raman scattering in the UO2(CH3COO)2 – DMSO system around the uranyl symmetric
stretching vibration at 829 cm − 1. The line at 1044 cm − 1 due to DMSO can be used as an internal intensity standard.

ing light and reabsorption of scattered Raman systems of UO2(NO3)2 –DMSO [6] and
light by the sample solution itself were not taken RbUO2(NO3)3 –DMSO [8]. This phenomenon
into account, as it is rather difficult to evaluate may be explained by the interference effect which
these effect accurately. The REP for the uranyl has been pointed out by Friedman and Hoch-
symmetric mode was obtained by plotting the strasser [9].
values of such relative intensities against the excit- It is seen from Fig. 4 that the relative intensity
ing wavelengths, and shown in Fig. 4 as filled change in the REP, ranging from 0.3 to 0.9, is not
circles. It is found from Figs. 1 and 4 that the so large in comparison with that of the
observed REP of the uranyl totally symmetric UO2(NO3)2 –DMSO system (0.25–1.25) [6]. This
stretching line has similar structure to the vibronic suggests that the REP of the uranyl–DMSO sys-
structure of the ABS, but does not superimpose tem depends considerably upon the ligands bound
on it. The same tendency is also found in the to the uranyl group. But, the ligand effect on the
1342 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345

Fig. 4. Resonance Raman excitation profile for the 829 cm − 1 fundamental vibration. Filled circles give relative scattering intensities
for the 0.48 M UO2(CH3COO)2 –DMSO solution with respect to the DMSO 1044 cm − 1 mode. The solid line gives the best
transform fit with the experimental data within the non-Condon model using excited state frequency of 705 cm − 1.

observable Raman shift is small, i.e. there is a problem, intrinsic to the theory of the resonance
little difference (6 cm − 1) between UO2(NO3)2 – Raman effect of polyatomic molecules. In this
DMSO and UO2(CH3COO)2 – DMSO. While, the respect, the transform method allows one to cir-
REP of RbUO2(NO3)3 – DMSO, in which three cumvent this difficulty by transferring the multi-
NO3− are bonded around the uranyl ion, displays mode information contained in the ABS directly
a similar change (0.25 – 0.8) with that of to the REPs [5]. For convenience the transform
UO2(CH3COO)2 – DMSO, and little difference (5 method as outlined by Stallard et al. [1] is used,
cm − 1) is seen in the observed Raman shifts be- though any other variant of the transform would
tween them. These results are summarized in be equally valid. The basis for the transform
Table 1. relation between ABS and a given REP lies in the
It is of interest to interpret the observed REP Kramers–Heisenberg formulation for the off-di-
from a theoretical point of view. The interpreta- agonal molecular polarizability. In general, it is
tion of REPs is complicated in general, since a not easy to calculate the resonance Raman scat-
large number of phenomena can influence their tering tensor because of many modes which par-
behavior. One of the most serious difficulties in ticipate in the nuclear motions. Stallard et al. have
the calculation of REPs is so-called multimode derived a transform relation directly from the
 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345 1343

Table 1
The wave number (cm−1) of the Raman active vibration of the OUO totally symmetric stretching mode in both the ground (gv\)
and excited (ev\) states and the change in the REP (DREP) for uranyl compounds in DMSO

Complex gv\ (cm−1) ev\ (cm−1) DREP Reference

UO2(NO3) 835 703 0.25–1.25 [6]

RbUO2(NO3)3 834 740 0.25–0.80 [8]
a
UO2(CH3COO)2 829 703 0.30–0.90

a
Present work.

frequency domain Kramers – Heisenberg expres- the experimental REP. Sa = (kaDQa/2F( a)2 is the
sion. Their approach is based on the recursion Franck–Condon coupling parameter (FC), where
relation for Raman Franck – Condon factors and ka is the force constant, DQa is the displacement
introduces the relaxation of several of the stan- of the excited potential from that of the ground
dard constraint. In particular, a limited adiabatic state, and F( a is the root mean squared zero point
approach is used in which only the mode being force. Sr (Rrr )IO is the vibronic coupling parame-
examined in the Raman experiment is assumed to ter. Eq. (1) as outlined above is appropriate to the
be factorized from the molecular eigenstate space, description of resonance Raman scattering inten-
and the following useful transform equation for sities of totally symmetric vibrational modes for
the Stokes scattering of a totally symmetric vibra- excitation to an electric-dipole-allowed transition.
tion has been derived: In the present case, the definition Ca can not be

   
d sR
−
4 d sR
used because the electronic transition (1Sg+ “ 1Fg)
we are dealing with is mostly vibronic. Introduc-
d V  3 d V Þ ing an assumption that Sr(Rrr)IOˆSa1/2, one may
(v− va)4 modify Eq. (1) as follows [8].
= S (1 + Ca)fv −(1 −Ca)f(v − va)2
16C 2p 2 a
(1)
   
d sR
−
4 d sR
d V  3 d V
 
Þ

where, (v− va)4 2

= % (R rr ) IO
f(v)+f(v−va)2
16C 2p 2 r
% (Rrs )IO (2)
r
Ca = .
S 1/2 The Kramers–Kronig transform of the ABS gives
   
a
the real part of the polarizability, while the optical
d sR d sR
Here, and denote the orienta- theorem shows how the absorption function itself
d V  dV Þ represents the imaginary part [18]. Thus the com-
tionally averaged total resonance-Raman differen- plex linear polarizability f(v) at the frequency v
tial cross-section for totally symmetric modes with can be calculated from the measured ABS
the scattered light polarized parallel () and per- through the Hilbert transform:

&
pendicular (Þ) to the polarization of the incident
light, respectively. v is a particular laser excita- 1 +
sABS(x) sABS(v)
tion frequency and va the vibrational frequency in f(v)= P d x+ i (3)
p − x(x− v) v
the excited electronic state. The dimensionless rel-
ative non-Condon parameter Ca, a pure real num- Where, P denotes the Caushy principal value of
ber, represents the ratio at the amplitude level of the integral. The expected REP is now fully deter-
the generalized B, C-term to A-term sources of mined by the observed ABS and the excited elec-
scattering for the single factored vibration [13]. tronic excited state fundamental vibrational
This parameter can be varied to provide a fit to frequency of interest through Eqs. (2) and (3).
1344 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345

We calculated the REP for the uranyl symmet- Using Eqs. (2) and (3), we have calculated the
ric stretching mode at 829 cm − 1 of REP for the OUO stretching mode at 829
UO2(CH3COO)2 in DMSO by use of this trans- cm − 1, in which the intensities are adjusted to
form method and compared it with the experi- those of the experimental REP. In Eq. (3), though
mental REP (Fig. 4). For the calculation, we have the limits of the integration extend over all fre-
here assumed that the line shape function for the quencies, the finite extent of the ABS allows trun-
ABS in Eq. (3), sABS(v) may be expressed as cation, 18.5–22.5 ×103 cm − 1. In Fig. 4, the
some linear combination of Lorentzians, L(v)n, calculated REP for the 829 cm − 1 mode is com-
sABS(v)=m n = 1 gnL(v)n where the coefficients gn
pared with the experimental REP within the re-
are determined so as to give the best agreement gion of the electronic transition 1Sg+ “ 1Fg
between the calculated and experimental ABSs. In (550–450 nm; 18.5–22.5 ×103 cm − 1). In this
the present case, the number of Lorentzian is figure, filled circles indicate the experimentally
m = 13. observed relative intensities and the solid line
The only adjustable parameter in Eq. (2) for gives the best transform fit in the non-Condon
resonance exciting Raman line shape fitting is the model using the excited state frequency of 705
excited electronic state fundamental vibrational cm − 1. One can see from the figure that an excited
frequency of interest, va. It may be varied within frequency of 705 cm − 1 in the non-Condon model
a limited range of the known ground state fre- gives relatively good agreement with experiment
quency, if the excited value is not independently except for the low frequency region below 20.5×
103 cm − 1. The discrepancy between the experi-
available. We could properly estimate this
mental and calculated REPs are ascribed to
parameter from consideration of the observed
interference between the scattering from a neigh-
ABS (Fig. 1) as shown below.
boring vibronic resonance electronic state (1Sg+ “
The maxima in the electronic absorption spec- 1
Dg) and strong preresonance scattering from
trum of the uranyl ion can be expressed by the
allowed electronic states of higher energy, situated
following equation [10]: nabs =nE +nsns + nAnA +
between 27 and 30× 103 cm − 1. Considering the
nBnB + Sinini, where nE refers to the wavenumber
experimental ABS in Fig. 1, one can see that the
of the pure electronic transition, nS to the symmet-
intensity of resonance Raman scattering in the
ric stretching vibration, nA to the antisymmetric region of Sg+ “ 1Dg may be more strongly en-
one and nB to the bending vibration. ni concerns hanced than in the region of the 1Sg+ “ 1Fg elec-
all ligand or crystal lattice vibrations coupled to tronic transition. The preresonance scattering due
the electronic transition. The number nS, nA, nB, to the allowed transition may also be stronger
and ni give the number of quanta of the various than that of these two forbidden electronic states.
vibrations involved. According to this formula, a In order to understand the experimentally ob-
uranyl spectrum should be very complex. It has served REP correctly, we will have to investigate
however been established experimentally that the the REP resulting from these three electronic
spectrum is simplified because one vibration is states.
predominantly coupled to the electronic transi- In the case of an electric-dipole-allowed transi-
tions of the uranyl ion. Several authors [11] have tion, the Albrecht’s A-term predominantly con-
identified it as the symmetric stretching vibration tributes to a Raman spectrum, and the high
nS, and have described the ABS by nabs = nE + intensity totally symmetric fundamental mode and
nSnS. From the observed ABS (Fig. 1), we can see its overtone progressions are expected to be ob-
that intervals between these vibronic maxima are served. The fact that there are no overtone and
separated with almost regular intervals, 704 and combination bands at all in this system means
707 cm − 1 in the electronic transition region of that the resonance Raman intensities of the uranyl
Sg “ 1Fg. The only adjustable parameter, va
1 +
symmetric stretching mode depend mainly on the
was chosen as 705 cm − 1, the mean value for two generalized B, C-term (non-Condon term) source
intervals. of scattering [12].
 T. Soga, K. Ohwada / Spectrochimica Acta Part A 55 (1999) 1337–1345 1345

The scattering intensities of the uranyl totally the O–U–O stretching mode is similar to the
symmetric stretching vibration at 829 cm − 1 de- vibronic progression of the observed ABS and
pend on the wavelengths of exciting laser lines. displays maxima in the wavelength region of in-
Application of an empirical rule of Hirakawa and terest. The intensity change in the observed REP
Tsuboi [13– 15] to the present case suggest that is not so large as that of the UO2(NO3)2 –DMSO
the uranyl ion in the excited electronic state has system. Transform methods have been applied to
an equilibrium conformation linearly distorted the analysis of the observed REP. The non-Con-
along the symmetric stretching mode. don model gives relatively good agreement with
It is of importance to examine the equilibrium the experimental REP. Differences between the
geometrical change in the uranyl bond length in experimental REP and the transform predictions
the excited electronic state of interest. In order to may have resulted from the coalescence of the
evaluate the change in the uranyl bond length in neighboring vibronic resonance state and the pre-
going from the ground to the excited electronic resonance scattering due to allowed electronic
states, 1Sg+ “ 1Fg, a simple rule presented by Bad- transition located in the shorter wavelength of
ger [16], which relates a bond length with its visible spectrum. Elongation of the OUO bond
stretching force constant, was employed. This arising from the 1Sg+ “ 1Fg electronic transition
simple rule has been proven very useful for ana- was estimated.
lyzing the UO bond length RUO in the ground
state uranyl compounds from their stretching
force constant KU − O determined by normal coor- References
dinate analysis: RU − O =1.08K − 1/3
U − O +1.17 [17]. If
we would expect this relation be applicable to the [1] B.R Stallard, P.M. Champion, P.R. Callis, A.C. Albrecht,
J. Chem. Phys. 78 (1983) 712.
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[2] D.L. Tonks, J.B. Page, Chem. Phys. Lett. 66 (1979) 449.
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DRU − O = rU − O −RU − O =1.08(k − 1/3 − 1/3
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where rUO and kUO denote the UO bond length Chem. 90 (1986) 2347.
and the symmetric stretching force constant in the [5] P.M. Champion, A.C. Albrecht, Ann. Rev. Phys. Chem.
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[9] J. Friedman, R.M. Hochstrasser, Chem. Phys. Lett. 32
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705 cm − 1 from the vibronic progression of the [10] G.H. Dieke, A.B.F. Duncan, Spectroscopic Properties of
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the UO bond length is about 0.068 Å. [11] E. Rabinowitch, R.L. Belford, Spectroscopy and Photo-
chemistry of Uranyl Compounds, Pergamon, Oxford,
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[12] A.C. Albrecht, J. Chem. Phys. 34 (1961) 1476.
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4. Summary [14] M. Tsuboi, A.Y. Hirakawa, S. Muraishi, J. Mol. Spec-
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75.
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[16] R.M. Badger, J. Chem. Phys. 2 (1934) 128.
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ten output lines of an argon ion laser at room [18] S. Hassing, O.S. Mortensen, J. Chem. Phys. 73 (1980)
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