Accepted Manuscript

Bismuth Electrodes in Contemporary Electroanalysis

Vasko Jovanovski , Samo B. Hočevar , Božidar Ogorevc

PII: S2451-9103(17)30035-2
DOI: 10.1016/j.coelec.2017.07.008
Reference: COELEC 77

To appear in: Current Opinion in Electrochemistry

Received date: 2 June 2017

Revised date: 14 July 2017
Accepted date: 18 July 2017

Please cite this article as: Vasko Jovanovski , Samo B. Hočevar , Božidar Ogorevc , Bismuth
Electrodes in Contemporary Electroanalysis, Current Opinion in Electrochemistry (2017), doi:
10.1016/j.coelec.2017.07.008

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 ACCEPTED MANUSCRIPT

Highlights
 Bismuth electrode as an attractive replacement for its mercury counterpart
 Bismuth is considered as a "green-element"
 Bismuth electrodes allow detection of numerous metal and organic analytes

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Bismuth Electrodes in Contemporary Electroanalysis

Vasko Jovanovski, Samo B. Hočevar* and Božidar Ogorevc

Department of Analytical Chemistry, National Institute of Chemistry, Hajdrihova 19, SI-1000

Ljubljana, Slovenia

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*Corresponding author. Tel.: +386 1 4760 230; fax: +386 1 4760 300.

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E-mail address: samo.hocevar@ki.si (S.B. Hocevar).

Abstract
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After the first introduction of bismuth film electrode in 2000 as an attractive alternative to its
mercury analogue for anodic stripping voltammetric detection of trace (heavy) metal ions, and
following the first few years of pioneering studies, the bismuth as a "green" electrode material
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gained a broader attention within the electrochemical community worldwide. These investigations
triggered intensive research of bismuth-based electrodes for detecting numerous important analytes
under different conditions, and the development of novel types of bismuth electrodes.
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Introduction
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Reliable, sensitive, selective and inexpensive electrochemical sensors and methods for detecting
(heavy) metal ions and other relevant substances continuously attract significant interest due to
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mostly the toxic character of these analytes, their extensive production, application and
consequently their widespread and growing occurrence in the environment, and ultimately in the
food chain.
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In the past six decades, different types of mercury electrodes had been most commonly used for
metal ion and other analyte detection despite a well-known toxicity of mercury and associated
occupational health hazards, inconvenience for application in flow systems, difficulties in its
handling, storage and waste. In the past, there were numerous attempts to replace mercury with
other less toxic electrode materials, but none of them has approached the exceptional
electroanalytical performance of mercury.

Eighteen years ago, in 2000, a bismuth film electrode (BiFE) was reported for the first time by J.
Wang and co-workers [1]. This introductory article described and demonstrated the capability of
BiFE for anodic stripping voltammetric detection of selected trace metal ions, and as an attractive
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replacement for its mercury counterpart. As it is well known, bismuth has a non-toxic character and
is generally recognized as a "green element", besides its electrochemically interesting insensitivity
towards dissolved oxygen. After this first revolutionary report on BiFE several following milestone
articles described the use of in-situ and ex-situ prepared BiFEs considering different conditions and
applications such as adsorptive cathodic stripping voltammetry of trace Ni(II) [2], studying the effect
of surface-active compounds upon its anodic stripping voltammetric performance [3], and direct
cathodic voltammetric detection of an organic compound 2-nitrophenol [4].

The appealing attributes of bismuth electrode has attracted numerous groups to investigate this
promising electrode material and to study its electroanalytical capabilities. We are exposing here

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briefly only the most exciting and introductory works reported in the beginning of the BiFE era; in
2002 the BiFE was investigated under potentiometric stripping regime [5], the bismuth film carbon

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paste electrode modified with Bi2O3 was studied [6], and electrically-heated bismuth coated carbon
paste electrode was examined [7]. In 2003, the ex-situ prepared BiFE was introduced for

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simultaneous adsorptive cathodic stripping voltammetric and constant current
chronopotentiometric stripping detection of Ni(II) and Co(II) [8]. Later, the bismuth bulk electrode
was presented for the first time in a study of measuring heavy metal ions and selected organic

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compounds [9]; in the same year an interesting study was reported on using bismuth-coated boron-
doped diamond electrode [10]. By that time, the bismuth-based electrodes had gained worldwide
recognition as one of the most suitable alternative to mercury electrodes and consequently
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hundreds of studies were reported that are well-summarized in the three review papers covering
the first decade of the BiFE’s life [11-13].

There are few other important moments in this impressive story of bismuth electrode. For example,
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in 2006 and 2007, the BiFE prepared in the presence of bromide ions was examined revealing a
beneficial effect of bromide upon its electrochemical performance/stability together with scanning
electrochemical microscopy and in-situ atomic force microscopy investigation (Fig 1), as well as
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detailed study of electrodeposition parameters was carried out [14, 15].

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Fig. 1. AFM recorded in-situ at different substrates; bare GCE (a), BiFE prepared without (b) and with
(c) bromide ions in the modification solution (ref. 14 - figure which needs permission).
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In 2008, a bismuth nanoparticle modified boron-doped diamond electrode was investigated. In-situ
atomic force microscopy was employed to examine the bismuth nanoparticle growth [16]. An
important study was carried out in 2012 which enabled the diagnostics of anodic stripping
voltammetric electrode processes at the BiFE from theoretical and experimental point of view [17].
More recently, an exciting work on the use of Janus-type bismuth-based particles for "wireless"
electrosampling followed by stripping voltammetric measurement of heavy metal ions was
described, as depicted schematically in Fig. 2 [18].

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Fig. 2. Schematic illustration of the bipolar electrodeposition of (a, b) bismuth film on a glassy
carbon bead and (c) Cd(II) and Pb(II) on the bismuth film modified glassy carbon bead (ref. 18 - figure
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which needs permission).

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Due to the great success of bismuth electrode, several attempts were undertaken in searching for
other similar metal-based electrodes that could possibly, in parallel with bismuth electrode, serve as
convenient replacements to mercury, such as lead [19], antimony [20], tin [21], copper [22] and
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various amalgams (e.g. with silver) [23, 24] etc. As the purpose of this review is to summarize mostly
the recent progress in the development of bismuth-based electrodes for environmental analysis, the
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following overview is further limited to achievements published in the last three years (from 2015).
In general, three main research and/or application areas are taking place: (i) application studies,
typically for detection of trace (heavy) metal ions and other inorganic compounds, (ii) research
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orientated toward determination of environmentally and/or biologically relevant organic species,

and (iii) development and characterization of novel types of bismuth-based electrodes
encompassing different bismuth precursors, surface modifications, integration of ionic liquids,
bismuth composites and examination of various bismuth morphologies.

(i) Detection of trace metals and other inorganic compounds:

Application studies of bismuth-based electrodes for measuring trace metal ions have been focused
mainly on the development of novel approaches typically employing anodic stripping voltammetry
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(ASV) when during the in-situ or ex-situ electrochemical accumulation of metallic analytes, the
surface formation of bismuth alloys/intermetallic compounds are possible. For example, ASV in
combination with BiFE was therefore developed for determination of trace mercury with the
introduction of a pre-stripping step that enabled very sensitive measurements in ng L- 1
concentration levels [25]. Mercury was also determined together with other analytes, e.g. with
copper using Bi-Au nanocomposite-modified carbon paste electrode [26] or with As(III) and Pb(II)
utilizing bismuth-modified exfoliated graphite electrode [27]. The enhanced sensitivity for measuring
Sn(IV) was achieved with a help of zinc mediator [28]. The applications of bismuth-based electrodes
in a variety of formats and in combination with ASV have been widely investigated using mostly
Cd(II) and Pb(II) as the model analytes, both well-recognized as severe environmental pollutants.

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These reports can be, for example, grouped based on the employed substrate electrodes, such as
glassy carbon electrode (GCE) [29- 33], screen-printed carbon electrode (SPCE) [34-37], carbon paste

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electrode (CPE) [38, 39], carbon thread [40] and others [41, 42]. The BiFE was originally found to be
optimally functioning in moderately acidic media at pH of ca. 4-5, among others, aimed at avoiding

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issues connected with hydrogen evolution when operating at more negative accumulation
potentials, e.g. for measuring Zn(II); however, an interesting approach was presented for the
detection of trace Zn(II) in more acidic medium with the addition of potassium sodium tartrate, as
shown in Fig. 3 [43].
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Fig. 3. ASVs for ten successive additions of Zn(II), Cd(II) and Pb(II) in the range of 10 to 90 g L-1
together with background responses obtained at the in-situ prepared BiFE in 0.01 mol L-1 HCl
containing 0.8 mg L-1 Bi(III) and 0.5 mmol L-1 tartrate. Insets depict corresponding calibration plots.
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(ref. 43 - figure which needs permission).

Trace Zn(II) detection was also investigated using the alkaline extraction from multivitamin
formulations [44] and, under less acidic conditions, in the presence of cell culture medium and ZnO
nanoparticles [45]. The BiFE prepared on the surface of SPCE employing magnetic field signal
amplification and dual bismuth precursor yielded a very low limit of detection (LOD), i.e. 0.05 g.L-1
Zn(II) [46], and a quite exotic approach featured a wearable skin sensor for real-time monitoring of
trace Zn(II) in human sweat [47]. BiFE associated with ASV and chemometric methods was also
implemented for simultaneous measurement of Sn(IV) and Pb(II) [48]. The detection of nanomolar
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concentrations of Fe(III) in coastal waters was studied either by using a tin-bismuth alloy electrode
or a bismuth nanosheet-coated graphene oxide electrode, in both cases combined with cathodic
stripping voltammetric protocol [49, 50]. Bismuth bulk annular band electrode was employed for
measuring Tl(I) using differential pulse ASV yielding exceptionally low LOD of 1 ng.L-1 [51]. In two
case studies, a bismuth bulk electrode was examined for measuring cadmium residues in bee
products [52] and a pencil-lead BiFE together with square wave ASV and chemometric tools was
employed for simultaneous determination of Zn(II), Cd(II), Pb(II) and Cu(II) in raw propolis samples
[53]. Released Pb(II) from ceramic dishes was detected by using CPE containing bismuth
nanostructures anchored on biochar [54], and two other studies presented the use of BiFE in
combination with ASV for tracing silver nanoparticle dissolution [55] and for examining the role of

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polyvinylpyrrolidone (PVP) in bioavailability of Ag(I) to terrestrial isopods released from PVP-
stabilized Ag-nanoparticle suspension [56]. An interesting study reported the use of cloud point

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extraction preconcentration at BiFE for the ASV detection of Cd(II) [57], and another voltammetric
approach was suggested using BiFE for the determination of size and particle concentration of Cd-

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based quantum dots [58]. The distribution of reduced sulfur species (sulfides) in wetland pore
waters was also investigated with BiFE [59]. Whenever the formation of alloys and/or intermetallic
compounds at the bismuth electrode surface during the electrochemical accumulation step is not

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feasible, metal ions are typically determined by means of accumulation of their complexes using
adsorptive cathodic stripping voltammetry (AdCSV). Depending on the metal analyte, several organic
ligands can be exploited for the coordination task. For example, dimethylglyoxime (DMG) ligand was
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used for simultaneous AdCSV determination of Ni(II) and Co(II) using either a macroporous bismuth
film deposited on SPCE [60] or a renewable bismuth bulk annular electrode [61], the latter electrode
being also employed for detection of Pd(II) via its DMG complex [62]. In an another study of this
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kind, Se(IV) was determined using 4-nitro-1,2-phenylenediamine ligand at the in-situ prepared BiFE
[63]. By adjusting optimal conditions and using an ex-situ prepared BiFE, trace amounts of Sb(III)
were measured via application of quercetin-5′-sulfonic acid as the chelating agent achieving
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excellent LOD below 1 g.L-1 [64]. For the purpose of speciation study a bismuth electrode was
utilized for monitoring trace Cr(VI) in combination with pyrocatechol violet ligand with good
selectivity even in the presence of less toxic Cr(III) [65]. In two similar investigations trace levels of
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Ga(III) [66] and In(III) [67] were successfully measured through their cupferron complexes using in-
situ prepared BiFE, whereas trace U(VI) was determined using the same ligand and employing a tin-
bismuth alloy electrode also combined with AdCSV [68]. A sequential voltammetric procedure for
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the determination of U(VI), Cd(II) and Pb(II) in phosphate fertilizers was investigated at the ex-situ
prepared BiFE [69]. As the first of bismuth-silver nanoparticle configuration sensor family, the
detection of Pt(II) in the presence of DMG was demonstrated [70]. In the following work, a bismuth-
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silver nanosensor was used in the voltammetric analysis of dust and soil samples for Pd(II), Pt(II) and
Rh(III) [71], and a bismuth-silver nanosensor was applied for the simultaneous determination of Pt-
Rh and Pd-Rh complexes with a remarkably low LODs for all three metal analytes below ng.L-1 level
[72].

(ii) Determination of environmentally and/or biologically relevant organic species:

Bismuth-based electrodes have also been widely investigated and applied in electroanalytical studies
of numerous organic compounds, a majority of which are considered pollutants by directly or
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indirectly entering certain environmental zones, such as surface waters and consequently drinking
water and food chain. These organic compounds can be divided into several categories of
electroactive species, e.g. harmful pesticides, also with their degradation products, selected
nutrients, hormones, aminoacids and amines, pharmaceuticals, DNA molecules, even
microorganisms, etc.

In the case of pesticides several studies tackled metribuzin degradation [73], detection of
neonicotinoids (Clothianidin, Imidacloprid, Thiamethoxam, Nitenpyram and Dinotefuran) [74],
Pendimethalin [75] and an endocrine disruptor Parathion [76]. Among essential nutrients,
measurements of folic acid using AdCSV at the BiFE [77, 78] and at the bismuth nanowires modified

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GCE [79] were demonstrated, as well as the detection of vitamin B2 (riboflavin) in the sub-
nanomolar range at the sparked-bismuth oxide screen-printed electrode and at the BiFE [80, 81]. In

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addition, glutathione detection at the BiFE [82] and ascorbic acid at the bismuth-silver nanosensor
[83] were also investigated. Low concentrations of hormone testosterone were determined using

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BiFE both in pharmaceutical and human urine samples in combination with AdCSV [84]. Hazardous
food additive Tartrazine was successfully detected with bismuth chitosan nanosheets-modified GCE
[85]. Bismuth nanostructured carbon paste ionic liquid electrode was studied for detection of amino

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acid cysteine [86], and carbon nano-fragments combined with bismuth oxide-coated GCE was
applied for electrochemical analysis of trace catechol [87]. The DNA detection was demonstrated
using a very sensitive bismuth-modified SPCE biosensor [88], a bismuth titanate nanoparticle-based
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amperometric biosensor [89], a bismuth-coated GCE combined with analytical approach
encompassing CdSe quantum dots as signal markers and endonuclease [90], and using an
impedimetric DNA biosensor based on a rod-like bismuth sulfide and polyaniline (PANI)
nanocomposite film modified ionic liquid-carbon paste electrode [91]. A bismuth oxide-based
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nanocomposite-coated electrode was exploited for sensitive and selective determination of

neurotransmitter epinephrine [92]. A variety of pharmaceutical formulations were successfully
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detected applying different bismuth-based electrodes, such as 5-nitroindazole, diazepam,

paracetamol, caffeine, sulfasalazine and valacyclovir [93-97]. An interesting research described a
highly sensitive electrochemical genosensor based on multiwalled carbon nanotubes–chitosan–
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bismuth and lead sulfide nanoparticles for the detection of pathogenic Aeromonas [98],
organosulfur compounds in fossil fuels were determined using cyclic voltammetry and in-situ
prepared BiFE [99] and Bi2O3-modified SPCE was employed for monitoring mycotoxin deoxynivalenol
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[100]. An electrochemical immunoassay of quantum dot-labelled proteins was successfully

implemented using the in-situ bismuth deposition into a disposable microfluidic platform [101] or
with the application of graphite screen-printed electrodes (SPEs) modified with bismuth citrate [102,
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103]. A novel electrochemical immunosensor for sensitive, specific and simple detection of anthrax
protective antigen toxin at picogram concentration levels was developed using bismuth
nanocomposite film and cadmium ion functionalized titanium phosphates [104].

(iii) Novel types of bismuth-based electrodes:

Similar to the early stage of the bismuth electrode era, also in the recent few years enormous efforts
were directed into further study and development of bismuth-based electrodes either from the pure
electrochemical point of view or in terms of their enhanced electroanalytical performance
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considering the electrode surface protection, electrode composition, shape, size etc. For example,
novel strategies for designing bismuth electrodes included the electrochemical deposition from
various bismuth precursors [29, 100, 105]. Another attractive direction of several research groups is
the development and characterization of diverse bismuth alloys [26, 28, 41, 49, 68, 71, 106]
employing a variety of metals such as Au, Zn, Sn, Sb, Ag etc. that have revealed appealing
electroanalytical properties. In order to further improve the electroanalytical performance of
bismuth-based sensors assorted composites were prepared using, e.g. graphene [31, 50, 92, 107-
112] or other carbon materials mainly differing in morphology/porosity [27, 30, 33, 35, 39, 54, 65,
87, 96, 98, 113, 114]. Surfaces of bismuth-based electrodes were modified with polymers, such as
polystyrene sulfonate [34], chitosan [85], polyaniline [91, 115], poly(1,8-diaminonaphthalene) [116],

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over-oxidized conductive polymers [117] or ionic liquids [42, 86, 118, 119]. There have been also
reports on preparation of different bismuth film morphologies aimed at improving detection

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characteristics [60, 74, 79, 120-124], and an interesting approach was presented including the Box–
Behnken design combined with the response surface methodology to investigate the influence of

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different parameters upon Cd(II) detection at BiFE [125].

Conclusion:
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This short overview, which mentions and lists numerous reports, apart from several hundreds of
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them published in the past 18 years since the introduction of bismuth film electrode, clearly
demonstrates the broad versatility, applicability and scientific importance of bismuth-based
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electrodes and justifies a still growing interest in their research and development. It can be well
concluded that after first several hundred reports addressing basic functional and operational
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parameter studies and applicability of bismuth-based sensors, together with a large number of
possible inorganic and organic analytes, known electroanalytical approaches, as well as simple (film,
bulk) and complex (composites of diverse (nano)materials) electrode configurations, still intensive
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investigations and other research directions can be foreseen. This includes numerous topics that still
need to be addressed, such as improved electrode surface protection and general robustness for
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long-term use, sensor miniaturization and adaptation for incorporation into sophisticated analytical
systems for in-vivo, biomedical and industrial monitoring, for decentralized environmental and
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security applications, etc. Novel concepts and applications associated with analytical
electrochemistry and related fields will therefore constantly be emerging. In this view, bismuth
electrodes undoubtedly exhibit a great potential and hence attract and deserve further attention.

Acknowledgement

Financial support from the Slovenian Research Agency (P1- 0034) is gratefully acknowledged.
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