Journal of Raman Spectroscopy

Cover image for Vol. 48 Issue 4

Early View (Online Version of Record published before inclusion in an issue)

Impact Factor: 2.395

ISI Journal Citation Reports © Ranking: 2015: 15/43 (Spectroscopy)

Online ISSN: 1097-4555

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  1. 1 - 65
  1. Research articles

    1. Pressure dependence of peak positions, half widths, and peak intensities of methane Raman bands (ν2, 2ν4, ν1, ν3, and 2ν2).

      Dmitry V. Petrov

      Version of Record online: 18 APR 2017 | DOI: 10.1002/jrs.5141

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      Results of investigation of changing peak positions, half widths, and peak intensities of Q-branches of the ν2, 2ν4, ν1, ν3, and 2ν2 methane Raman bands are presented at pressures in the range 1−55 bar and а temperature of 298 K. A set of data obtained will be useful for the Raman analysis of natural gas and can also be used for determination of the pressure of methane-containing media.

    2. High-pressure Raman study of nyerereite from Oldoinyo Lengai

      Sergey V. Rashchenko, Sergey V. Goryainov, Alexander V. Romanenko, Alexander V. Golovin, Andrey V. Korsakov, Bertrand N. Moine and Anastasia O. Mikhno

      Version of Record online: 17 APR 2017 | DOI: 10.1002/jrs.5152

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      Secondary melt inclusion in olivine xenocryst from the Udachnaya-East kimberlite.

    3. Raman optical activity of human α-synuclein in intrinsically disordered, micelle-bound α-helical, molten globule and oligomeric β-sheet state

      Carl Mensch, Albert Konijnenberg, Roos Van Elzen, Anne-Marie Lambeir, Frank Sobott and Christian Johannessen

      Version of Record online: 17 APR 2017 | DOI: 10.1002/jrs.5149

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      We report distinct Raman and Raman optical activity patterns of α-synuclein (α-syn) in disordered, α-helical and β-sheet conformation and identify a (pre-)molten globule intermediate in the aggregation pathway of α-syn induced by a fluorinated alcohol. Furthermore, by careful spectral subtraction, we isolated the spectral contribution of the disordered C-terminal tail in micelle-bound α-syn. These results demonstrate the unique sensitivity of these spectroscopies to study challenging proteins.

    4. High-pressure Raman spectroscopy of Ca(Mg,Co)Si2O6 and Ca(Mg,Co)Ge2O6 clinopyroxenes

      M. Tribaudino, I. Aliatis, D. Bersani, G. D. Gatta, E. Lambruschi, L. Mantovani, G. Redhammer and P. P. Lottici

      Version of Record online: 17 APR 2017 | DOI: 10.1002/jrs.5134

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      In situ high-pressure Raman spectra were collected on pyroxenes, with composition CaCoSi2O6, CaMgSi2O6, CaMgGe2O6 and CaCoGe2O6, up to P = 8.3 GPa. The peak wavenumbers υi increase almost linearly with pressure; the slope dυi/dP is more pronounced for the modes at higher wavenumbers, and higher in germanates than in silicates. The strong dependence of the higher energy stretching modes with pressure shows that Raman spectroscopy is best suited to detail subtle changes in the tetrahedra of germanates and silicates.

    5. Spectral restoration method for spatial heterodyne Raman spectrometer

      Guangxiao Hu, Wei Xiong, Haiyan Luo, Hailiang Shi, Zhiwei Li, Jing Shen, Xuejing Fang and Biao Xu

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5145

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      Spatial heterodyne Raman spectrometer (SHRS) is a new developing method to detect Raman spectra with many advantages over traditional instruments. The research focuses on the spectral restoration method of SHRS, which is the key part to remove the potential data defects. The processing results prove that the restoration method has a good performance for real Raman spectra achieved by an SHRS breadboard.

    6. SERS spectrum of red dyes in the Mapuche belts from the beginning of the XXth century

      M. M. Campos-Vallette, M. J. Rodríguez, M. A. Chapanoff, E. Clavijo, J. S. Gómez-Jeria, A. E. Aliaga, G. P. Jara, F. Celis, C. Paipa and P. Leyton

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5147

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      Red dyes in seven belts (trariwe) belonging to the Mapuche culture, dated as beginning of the XXth century and stored in Museo Regional de la Araucanía, Chile, were analysed by using ultraviolet-visible, liquid chromatography coupled to mass spectrometry, Raman and Surface Enhanced Raman Scattering spectroscopies. Red dyes were extracted and characterized; the spectral analysis allowed identifies a commercial synthetic aniline the azopigment PR57 as the principal red dye in five samples. Another monoazopigment, orange benzimidazolone, was identified in two samples.

    7. Effect of physiological factors on the biochemical properties of colon tissue – an in vivo Raman spectroscopy study

      Hao Ding, Andrew W. Dupont, Shashideep Singhal, Larry D. Scott, Sushovan Guha, Mamoun Younes, Yuanqing Ye and Xiaohong Bi

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5140

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      Raman spectra from healthy colon tissue were acquired in vivo through an endoscopic Raman system, and potential physiological factors affecting tissue biochemistry were evaluated. The results showed that gender, ethnicity, age, body mass index, and anatomical locations along the colon were significant sources of variability, resulting from different abundance in lipids and proteins.

    8. Raman imaging studies on the adsorption of methylene blue species onto silver modified linen fibers

      Sara Fateixa, Manon Wilhelm, Alípio M. Jorge, Helena I. S. Nogueira and Tito Trindade

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5136

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      Surface-enhanced resonance Raman scattering (SERRS) coupled with Raman imaging can be successfully used to identify distinct forms of organic dyes adsorbed within antimicrobial linen fibers enriched in Ag nanoparticles. The potential of this approach as a non-destructive characterization method of fabrics was evaluated with Raman studies performed on the molecular forms of methylene blue (MB), used here as the textile colorant. Our results demonstrate that by using SERRS imaging it is possible to identify the adsorbate species in distinct regions of the substrates.

    9. Raman spectra of nyerereite, gregoryite, and synthetic pure Na2Ca(CO3)2: diversity and application for the study micro inclusions

      A. V. Golovin, A. V. Korsakov, P. N. Gavryushkin, A. N. Zaitsev, V. G. Thomas and B. N. Moine

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5143

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      The strongest Raman bands for nyerereite, Na2Ca(CO3)2, and gregoryite occur at 1070–1090 cm−1 region. Raman spectra of the nyerereite (incommensurately modulated structure, space group Cmcm) can be divided into three types and are likely to be related to crystallographic orientations. Synthetic Na2Ca(CO3)2 (commensurately modulated structure, P21ca) has only one type of Raman spectrum, but intensity ratios of the bands vary significantly. The strongest Raman band of one type of the nyerereite can be erroneously interpreted as gregoryite, but later is always symmetrical.

    10. Spatially resolved Raman spectroscopy study of uniform and tapered InAs micro-nano wires: correlation of strain and polytypism

      Vandna K. Gupta, Alka A. Ingale, Suparna Pal, R. Aggarwal and V. Sathe

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5138

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      Polarization and wavelength-dependent Raman spectroscopy shows existence of polytypism in InAs micro-nanowires (MNWs) of all types.

      1. Wavenumber of TO phonon (zinc blende: ZB) and E2h phonon (wurtzite: WZ) are observed in the range of 216–218 and 212–215 cm−1 for diameters ranging from 500 nm to 2.2 μm and 400 nm to 2.2 μm, respectively.
      2. Phonon wavenumber variation in a tapered MNW, from base (2 μm) to tip (800 nm) is correlated to the variation in residual strain due to increase in the relative content of WZ structure w.r.t. ZB of InAs.
      3. Temperature-dependent Raman data further show that there is a measurable contribution of dω/dT due to stress to the total dω/dT, positive for ZB and negative for WZ phonons, which can be explained in terms of difference between their thermal expansion coefficients.
    11. Assessment of the Cr doping and size effects on the Raman-active modes of rutile TiO2 by UV/Visible polarized Raman spectroscopy

      G. Cristian Vásquez, David Maestre, Ana Cremades and Javier Piqueras

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5133

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      Size and Cr doping effects have been evaluated by the study of Raman spectra of different undoped and Cr-doped rutile TiO2 samples. Raman polarization effects have been also evaluated by modifying the orientation of the probed microstructures. It has been found that Cr incorporation increases vibration modes at 110, 154, 700 and 810 cm−1. The relation of these vibration modes with a possible doping-induced activation of the Raman-inactive B1u and A2u modes, as well as the influence of size effects, is evaluated and discussed.

    12. Quantitative detection using two-dimension shell-isolated nanoparticle film

      Jing-Liang Yang, Zhen-Wei Yang, Yue-Jiao Zhang, He Ren, Hua Zhang, Qing-Chi Xu, Rajapandiyan Panneerselvam, Kundan Sivashanmugan, Jian-Feng Li and Zhong-Qun Tian

      Version of Record online: 12 APR 2017 | DOI: 10.1002/jrs.5151

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      A highly uniform, reproducible, and stable shell-isolated Ag@SiO2 nanoparticle monolayer film was prepared. It was employed as a substrate for the quantitative determination of melamine in milk samples through shell-isolated nanoparticle-enhanced Raman spectroscopy, and showed ultrahigh sensitivity with a limit of detection down to 0.03 ppm.

    13. Identification of inorganic and organic inclusions in the subglacial antarctic Lake Vostok ice with Raman spectroscopy

      U. Böttger, S. A. Bulat, F. Hanke, S. G. Pavlov, M. Greiner-Bär and H.-W. Hübers

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5142

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      First results of Raman measurements of inclusions in accretion ice type I in a Vostok lake ice sample show that Raman spectroscopy is an appropriate method for the exploration of inclusions entrapped into lattice of any natural mono-crystalline ice. As Raman spectroscopy will be applied in upcoming space missions, a co-operation of the space science community with the Antarctic Lake Vostok community is suggested to test the space instrumentation under the extreme Antarctic environment and conditions of the subglacial Lake Vostok.

    14. A machine learning framework to analyze hyperspectral stimulated Raman scattering microscopy images of expressed human meibum

      Alba Alfonso-García, Jerry Paugh, Marjan Farid, Sumit Garg, James Jester and Eric Potma

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5118

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      A machine learning methodology for batch-level analysis of hyperspectral stimulated Raman of expressed human meibum is presented. A strategy based on clustering and classification of hyperspectral stimulated Raman scattering spectra in the CH-stretching region provides a high throughput, rapid quantitative analysis of the protein composition of meibum. This approach enables direct comparison among samples using a single set of reference spectra and reveals marked variation among samples that potentially correlate with meibum health quality.

    15. Raman microspectrometric study of pigments in melanized fungi from the hyperarid Atacama desert gypsum crust

      Adam Culka, Jan Jehlička, Carmen Ascaso, Octavio Artieda, Cristina M. Casero and Jacek Wierzchos

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5137

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      Microbial communities composed by eukaryotic microorganisms: melanized fungi and algae colonizing the interior of gypsum crusts in hyperarid zone of the Atacama desert were studied by Raman microspectroscopy. Melanin pigments present in fungi cell walls were identified directly in the colonized gypsum crust and on the cultivated culture of the fungi from Neocatenulostroma genus. Two signature broad bands located at wavenumbers 1605–1580 cm−1 and around 1350 cm−1 have been detected and confirmed melanin as a main fungal protective pigment.

    16. Geochemical study of the Northwest Africa 6148 Martian meteorite and its terrestrial weathering processes

      Imanol Torre-Fdez, Julene Aramendia, Leticia Gomez-Nubla, Kepa Castro and Juan M. Madariaga

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5148

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      In order to characterise the NWA 6148 Martian nakhlite Raman imaging, XRF imaging and SEM-EDS analysis has been performed. Augite and olivine have been found as the main mineral phases of the sample, and metal proportion quantification was performed by means of Raman bands position for both minerals. Moreover, several uncommon minerals were found, including the Co3O4, which is the first time that is observed in a Martian meteorite.

    17. Comparison of Raman-active crystals as a narrowband probe light source for picosecond three-color vibrational CARS thermometry

      Christian Meißner, Johannes W. Tröger, Dimitrii N. Kozlov, Frank Beyrau and Thomas Seeger

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5135

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      Solid-state Raman shifters are for the first time tested and employed as a probe light source in a three-color picosecond vibrational CARS approach for thermometry. The first results of temperature measurements under ambient conditions and in a sooting ethylene/air flame are presented. Therewith, temperature errors by N2 vibrational CARS measurements in sooting flames can be avoided.

    18. Portable Raman verification and quantification of jade in Olmec ceremonial axes from El Manatí, Veracruz, Mexico

      François Gendron, David C. Smith, Pierre Masson, María del Cármen Rodríguez Martínez and Ponciano Ortiz Ceballos

      Version of Record online: 11 APR 2017 | DOI: 10.1002/jrs.5122

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      A series of Olmec ceremonial stone axes from an archaeological site in Mexico have been analysed by hand-held portable Raman spectroscopy in order to verify physico-chemically which ones really are in jade. The recognised sodic aluminous clinopyroxenes were then quantified in terms of mol. % jadeite in the solid-solution series Jd–Di–Hd using an available calibration of the wavenumber shifts of their T–O–T vibration band. Problems with jade terminology, with correlating density measurements and with provenancing rock types are discussed.

    19. Label-free surface-enhanced Raman spectroscopy of lipid-rafts from hepatocyte plasma membranes

      Blanca Delgado-Coello, Danai Montalvan-Sorrosa, Armando Cruz-Rangel, Marcela Sosa-Garrocho, Beatriz Hernández-Téllez, Marina Macías-Silva, Rolando Castillo and Jaime Mas-Oliva

      Version of Record online: 7 APR 2017 | DOI: 10.1002/jrs.5101

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      Lipid rafts are sphingomyelin/cholesterol-rich domains present in the plasma membrane of eukaryotic cells. We propose a novel approach for the study of plasma membrane lipid rafts using SERS and PCA in correlation with conventional biochemical techniques. Our work using SERS/PCA shows a correlation between the composition of lipid rafts from the plasma cell membrane and the catalytic activity of the Ca2+-ATPase, and its direct association to the presence of specific lipids located in membrane lipid rafts.

    20. SERS detection of hepatitis B virus DNA in a temperature-responsive sandwich-hybridization assay

      Adem Zengin, Ugur Tamer and Tuncer Caykara

      Version of Record online: 5 APR 2017 | DOI: 10.1002/jrs.5109

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      A surface-enhanced Raman scattering (SERS) sensor was designed for detection of hepatitis B virus DNA in a temperature-responsive sandwich-hybridization assay. The SERS sensor can efficiently discriminate and detect a hepatitis B virus DNA target. The SERS sensor can be extended to ultrasensitive and selective detection of other analytes such as proteins, viruses, and explosives without any labeling.

    21. Quantum-chemical perspective of nanoscale Raman spectroscopy with the three-dimensional phonon confinement model

      Vitaly I. Korepanov and Hiro-o Hamaguchi

      Version of Record online: 4 APR 2017 | DOI: 10.1002/jrs.5132

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      We introduce a general quantitative approach to interpret the Raman spectra of nanoscale materials. We combine a quantum-chemical calculation with the 3D phonon confinement model to successfully reproduce the size-dependent Raman spectra of nano-diamonds.

    22. Automatic morphology-based cubic p-spline fitting methodology for smoothing and baseline-removal of Raman spectra

      Juan José González-Vidal, Rosanna Pérez-Pueyo and María José Soneira

      Version of Record online: 31 MAR 2017 | DOI: 10.1002/jrs.5130

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      We present a fully automated denoising methodology which enhances the Raman information with no user input. The proposed approach reduces the shot noise, rejects the fluorescence's baseline and does not modify the shapes of the Raman bands maintaining their intensity ratios. The reliable results that were obtained make the methodology a useful tool to help the analyst in the interpretation of Raman spectra.

    23. A SERS investigation of antimicrobial adsorption on silver nanoparticles as mediated by surface modifiers

      Aline Luciano Filgueiras, Tailine Mara Freire Dutra, Diego Paschoal, Hélio F. Dos Santos and Antonio Carlos Sant'Ana

      Version of Record online: 31 MAR 2017 | DOI: 10.1002/jrs.5131

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      Using SERS spectroscopy for understanding the adsorption of three antimicrobials and the surface chemistry of silver nanoparticles modified with 2-mercaptoethanol, chloride ions and polyvinyl alcohol. The control of the chemical properties of the silver surface led to different spectral patterns ascribed to different adsorption mechanisms.

    24. Prediction of viral loads for diagnosis of Hepatitis C infection in human plasma samples using Raman spectroscopy coupled with partial least squares regression analysis

      H. Nawaz, N. Rashid, M. Saleem, M. Asif Hanif, M. Irfan Majeed, I. Amin, M. Iqbal, M. Rahman, Ola Ibrahim, S. M. Baig, M. Ahmed, F. Bonnier and H. J. Byrne

      Version of Record online: 31 MAR 2017 | DOI: 10.1002/jrs.5108

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      Raman spectroscopy has been used to identify the biochemical changes associated with the presence of the Hepatitis C virus (HCV) in infected human blood plasma samples as compared with healthy samples, as control.

    25. Rapid 3D chemical-specific imaging of minerals using stimulated Raman scattering microscopy

      Marie-Andrée Houle, Robert C. Burruss, Andrew Ridsdale, Douglas J. Moffatt, François Légaré and Albert Stolow

      Version of Record online: 14 MAR 2017 | DOI: 10.1002/jrs.5098

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      We present the first applications of stimulated Raman scattering microscopy, a nonlinear optical Raman technique, to samples of mineralogical interest. Combined with second harmonic generation microscopy, stimulated Raman scattering offers a multimodal tool for rapidly imaging mineral samples having chemical specificity, structural sensitivity, and excellent three-dimensional resolution. In mineralogical applications, our wide-tuning range offers hyperspectral imaging of both trapped organics, via the CH region (~2900 cm−1), and the low-frequency (<1000 cm−1) modes important for mineral identification.

    26. Thermodynamic CoO–Co3O4 crossover using Raman spectroscopy in magnetic octahedron-shaped nanocrystals

      Beatriz Rivas-Murias and Verónica Salgueiriño

      Version of Record online: 8 MAR 2017 | DOI: 10.1002/jrs.5129

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      The thermodynamic crossover of octahedron-shaped nanocrystals of cobalt(II) oxide to oxidized Co3O4 normal spinel is studied using Raman spectroscopy. For that, the effect of the laser power from 0.3 (0.05%) to 69 (100%) mW and of the exposure time using different laser wavelengths was analyzed. Controlling both laser power and time exposure, the sample evolution from CoO rock salt to Co3O4 fcc spinel was attained, stemming from the energy transfer and consequent local heating.

    27. The effect of excitation wavelength and metallic nanostructure on SERS spectra of C60

      Miri Sinwani, Merav Muallem and Yaakov R. Tischler

      Version of Record online: 8 MAR 2017 | DOI: 10.1002/jrs.5126

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      In this study, we investigated the surface-enhanced Raman scattering spectra of Fullerene C60 evaporated on tapered Au thin films that contain several nanomorphologies with two excitation wavelengths: 532 and 784 nm. We show that each excitation wavelength reveals the strongest surface-enhanced Raman scattering signal at different regions in the tapered Au film. We explain these observations as a result of different Raman enhancement mechanisms.

    28. Raman spectral variation for human fingernails of postmenopausal women is dependent on fracture risk and osteoporosis status

      J. R. Beattie, M. C. Caraher, N. M. Cummins, O. M. O'Driscoll, R. Eastell, S. H. Ralston and M. R. Towler

      Version of Record online: 8 MAR 2017 | DOI: 10.1002/jrs.5123

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      Human nail protein structure and composition are affected by systemic factors that are associated with poor bone health. Fracture risk is associated with restructuring of nail keratin and compositional changes. Osteoporosis is associated with changes in the ionization of acid residues in the nail keratin.

    29. Ab initio simulations and experimental Raman spectra of Mg2SiO4 forsterite to simulate Mars surface environmental conditions

      C. Stangarone, U. Böttger, D. Bersani, M. Tribaudino and M. Prencipe

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5127

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      Comparison between a natural sample of forsterite (Fo#89) unpolarized Raman spectrum (bottom) and a calculated forsterite Mg2SiO4 by means of CRYSTAL14 (top). The box at the top on the left is an enlargement of wavenumbers from 150 to 500 cm−1 to emphasize peaks at low wavenumbers.

    30. Al4SiC4 vibrational properties: density functional theory calculations compared to Raman and infrared spectroscopy measurements

      L. Pedesseau, O. Chaix-Pluchery, M. Modreanu, D. Chaussende, E. Sarigiannidou, A. Rolland, J. Even and O. Durand

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5128

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      The nontoxic semiconductor Al4SiC4 has a huge potential for technological applications. First thorough experimental Raman and IR investigation of vibrational properties of Al4SiC4 single crystals are reported. The experimental results are compared with the full theoretical analysis of vibrational properties based on Density Functional Theory calculations that are revisited here.

  2. Rapid communications

    1. Conventional and standoff pulsed laser–Raman–echelle–time-gated (PRET) system

      Muhammed Shameem K. M., M. M. Tamboli, Praveen Devangad, Unnikrishnan V. K., Sajan D. George, V. B. Kartha and Santhosh C.

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5125

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      Time-gated Raman system has been developed using a pulsed laser and high-resolution intensified charge-coupled device echelle spectrograph. Echelle spectrograph provides broad spectral band-pass of 0–8500 cm−1 in a single scan with a resolution of 1.75 cm−1 for 532 nm at an extremely small slit width of 10 μm. Feasibility of echelle spectrograph for Raman measurements has been tested for both conventional and standoff distance of 5 m with all the external illumination sources on and discussed in detail.

  3. Research articles

    1. Novel VECSEL for short-wave infrared Raman spectroscopy applications

      I. P. Santos, A. van der Lee, X. Gu, P. J. Caspers, T. C. Bakker Schut, R. van Doorn, V. Noordhoek Hegt, S. Koljenović and G. J. Puppels

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5124

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      Vertical-external-cavity surface-emitting lasers (VECSELs) are an interesting alternative laser source for Raman spectroscopy. VECSELs offer a narrow linewidth, high power stability, good power efficiency, and circular beam profile. We developed a 986-nm VECSEL for a specific biomedical application (Raman measurements of pigmented skin lesions) and demonstrate that it fulfils the requirements for the selected application. Because of small size and good possibilities for mass-production, VECSELs are particularly interesting for low-cost compact hand-held Raman spectroscopy devices.

    2. Investigations of anharmonic effects via phonon mode variations in nanocrystalline Dy2O3, Gd2O3 and Y2O3

      Nita Dilawar Sharma, Jasveer Singh, Aditi Vijay, K. Samanta and Sugandha Dogra Pandey

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5120

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      The cubic nanocrystalline rare earth sesquioxides Dy2O3, Gd2O3 and Y2O3 have been investigated for anharmonic effects in the temperature range 80–440 K using Raman spectroscopy. The predominant Tg + Ag phonon modes of the samples primarily exhibited phonon softening. Three phonon or cubic anharmonicity dominates over quartic anharmonicity in all the samples. The true anharmonic term dominates over quasi-harmonic term in determining the total anharmonicity. The line width variations for these samples were found to display similar trends; however, their magnitudes were indicative of the factors that are expected to contribute to the variation in phonon behaviour.

    3. Standoff spatial heterodyne Raman spectrometer for mineralogical analysis

      Miles Jacob Egan, S. M. Angel and Shiv K. Sharma

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/jrs.5121

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      Traditionally, Raman spectra were acquired with grating-based dispersive spectrometers that require tens of micrometer-sized entrance slits and thus limited light throughput. We have used a new type of Fourier transform Raman spectrometer, the spatial heterodyne Raman spectrometer, that provides high spectral resolution in a compact system without limiting light throughout. In this work, we present time-resolved Raman spectra of carbonate, sulfate, and silicate minerals.

    4. You have full text access to this OnlineOpen article
      Feasibility of the quantification of respirable crystalline silica by mass on aerosol sampling filters using Raman microscopy

      Peter Stacey, Kerstin T. Mader and Christopher Sammon

      Version of Record online: 20 FEB 2017 | DOI: 10.1002/jrs.5113

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      Airborne respirable crystalline silica is hazardous, and more sensitive measurements are needed for exposure assessment. Limits of detection obtained on silver filters were ten times lower than reported by current Infrared or X-ray diffraction methods. Differences in median aerodynamic particle size of calibration dusts did not affect the Raman response. Respirable crystalline silica was measured in mixtures of 94% calcite and 80% hematite. Absorption of Raman response by opaque hematite particles occurred above a ‘critical’ loading.

    5. Violaxanthin cycle kinetics analysed in vivo with resonance Raman spectroscopy

      Matthias Koch, Serge Zagermann, Ann-Kathrin Kniggendorf, Merve Meinhardt-Wollweber and Bernhard Roth

      Version of Record online: 17 FEB 2017 | DOI: 10.1002/jrs.5102

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      A new approach to probe violaxanthin cycle kinetics in vivo using resonance Raman spectroscopy, baseline correction, and principal component analysis will be described, allowing studies with many more data points than possible with chemical analysis, as well as forgoing destructive sampling. Three experiments on the green alga Dunaliella salina will be shown, featuring both the light-to-dark and dark-to-light transition response kinetics.

  4. Short communications

    1. Determining alloy composition in MoxW(1 − x)S2 from low wavenumber Raman spectroscopy

      Tsachi Livneh, Dumitru O. Dumcenco and Iddo Pinkas

      Version of Record online: 16 FEB 2017 | DOI: 10.1002/jrs.5114

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      Mixed alloy MoxW(1-x)S2 (0 ≤ x ≤ 1) bulk samples are characterized by low wavenumber Raman spectroscopy. The absence of disorder effects in its interlayer motion (unlike for the intralayer motion) and the lack of Mo/W composition dependence of the shear mode force constants enables the facile employment of a reduced monoatomic linear chain model. The results provide a convenient and reliable means for systematically determining the sample Mo/W composition.

  5. Rapid communications

    1. In-situ Raman study of phengite compressed in water medium under simultaneously high P–T parameters

      S. V. Goryainov, A. S. Krylov, O. P. Polyansky and A. N. Vtyurin

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5112

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      In-situ method of Raman spectroscopy was used to study the layered phengite compressed in water under simultaneously high P–T (up to 373 °С and 12.5 GPa). The implemented conditions were typical of modeling the “cold” subduction zones in lithospheric slabs. Raman spectra have demonstrated a high Р–Т stability of the mineral. No non-quenchable phengite states were observed.

  6. Research articles

    1. Characterization of phosphorus compounds in soils by deep ultraviolet (DUV) Raman microspectroscopy

      Christian Vogel, Manfred Ramsteiner, Ryo Sekine, Ashlea Doolette and Christian Adam

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5115

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      Deep ultraviolet Raman microspectroscopy was successfully investigated as a new approach to analyze the chemical state of phosphorus compounds directly in soil. We demonstrate that ultraviolet excitation has the advantage to avoid the interference with the strong fluorescence, which occurs in the visible spectral range caused by organic matter in soils. For some organic phosphorus compounds, intensive sample cooling is found to strongly reduce the rate of degradation induced by the illumination with the ultraviolet excitation light.

    2. Raman spectra of gem-quality variscite and metavariscite

      Emmanuel Fritsch, Stefanos Karampelas and Jean-Yves Mevellec

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5117

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      Raman spectra on a set of five gems presented as variscite from the three major gem sources known were acquired, along with infrared spectra and chemical analysis. Surprisingly, four out of five samples are found to be metavariscite, which has been documented in gem quality only once before. Results of micro-FTIR in reflectance confirmed this result.

    3. Rapid quantification of total protein with surface-enhanced Raman spectroscopy using o-phthalaldehyde

      Merve Eryilmaz, Adem Zengin, Ismail Hakki Boyaci and Uğur Tamer

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5099

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      o-Phthalaldehyde (OPA) reagent with 2-mercaptoethanol was used as a SERS probe to quantify total protein in the presence of gold nanorod particles for the first time. The measurement time was 10 s, and the total analysis time was less than 5 min with a portable Raman reporter. The limit of detection was determined to be 0.08 mg/ml, and the ability of the developed method to quantify total protein in milk samples was investigated.

    4. Improved stopped-flow time-resolved resonance Raman spectroscopy device for studying enzymatic reactions

      Sachiko Yanagisawa, Megha Subhash Deshpande, Shun Hirota, Tatsuo Nakagawa and Takashi Ogura

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5100

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      An improved stopped-flow resonance Raman spectroscopy device was constructed using a stopped-flow mixer with a dead time of 3 ms and a mixing volume of 0.1 mL. The device was tested using myoglobin, where the formation reaction of a high-valent heme species, ferryl-oxo heme, was monitored by time-resolved resonance Raman spectroscopy after mixing a ferric myoglobin solution with a hydrogen peroxide solution. The present device is generally applicable to enzyme–substrate reactions with a significantly higher time resolution than previously reported.

    5. Identification of new spectral signatures associated with dengue virus infected sera

      Ayyaz Amin, Nimrah Ghouri, Safdar Ali, M. Ahmed, M. Saleem and Javaria Qazi

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5110

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      Raman spectroscopy showed an impetus potential for the diagnosis of dengue virus infection based on the unique spectral signatures in human blood sera. It provides a detailed insight about the molecular changes that arise in blood with the onset of dengue virus infection. It may be used as an excellent monitoring tool for studying time-to-time variation in the blood chemistry of patients.

    6. Sample self-absorption in surface-enhanced Raman spectroscopy (SERS): influence of the resonance, dilution and depth of the measurements

      Cyril Muehlethaler, John R. Lombardi and Marco Leona

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5097

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      Sample self-absorption can strongly attenuate the surface-enhanced Raman spectroscopy (SERS) signal when resonant conditions are used. Below a monolayer coverage of the SERS substrate, the signal is weakly attenuated, and a linear relationship to the concentration is maintained. For concentrations of analytes superior to a monolayer coverage, the intensity reaches a maximal plateau value. The increasing amount of molecules in solution act as filters and strongly attenuates the intensity of the SERS scattered main peaks and of the incident excitation light.

    7. Degradation of poly(L-lactic acid) coating on permanent coronary metal stent investigated ex vivo by micro Raman spectroscopy

      Kelim Vano-Herrera and Carla Vogt

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5111

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      Poly(lactic acid) is a biodegradable polymer used as functional coating on implants, e.g. on coronary artery metal stents. Micro Raman spectroscopy was applied for the investigation of the degradation of the poly(L-lactic acid) coating using relative band area ratios from samples of an ex vivo porcine model study. The complete absorption of the coating required more than 24 months for the layer thickness applied in this study, and the degradation was carried out by a hydrolytic degradation through the bulk erosion mode.

    8. Polymorph formation in fenofibrate in the absence and presence of polymer stabilizers: a low wavenumber Raman and differential scanning calorimetry study

      Ye Ying, Christian Beck, Aide Wu, Rajesh Dave and Zafar Iqbal

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5090

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      Low wavenumber Raman (LWR) spectroscopy enables the detection of crystalline features in the early stages of formation from amorphous or molten phases, and identification of emerging polymorphs. The effect of two non-ionic polymers, PF/127 and HPMC/E3, as stabilizers for the polymorphic forms of the drug fenofibrate (FNB) was investigated using LWR spectroscopy and DSC to determine the non-bonded interaction energies between the polymers and FNB.

    9. Investigation of tattoo pigments by Raman spectroscopy

      Betsy Jean Yakes, Tara Jade Michael, Marianita Perez-Gonzalez and Bhakti Petigara Harp

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5095

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      Raman spectroscopy using 532, 633, and 780-nm lasers was used to evaluate approximately 30 inorganic, organometallic, and organic pigments. By using these multiple wavelengths, all pigments could be identified, and searchable spectral libraries based on laser wavelength were created. This work provides a general overview for choosing the best laser wavelength for the identification of pigments used in tattoo inks. The method is poised to be an effective, noninvasive means for qualitatively identifying tattoo pigments.

    10. Titanium doping of BiFeO3 ceramics and identification of minor phases by Raman spectroscopy

      M. S. Bernardo, D. G. Calatayud, T. Jardiel, D. Makovec, M. Peiteado and A. C. Caballero

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5116

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      Raman spectroscopy is for the first time employed to detect almost imperceptible secondary phases in the BiFeO3 system. The comparison of the Raman spectra of undoped and Ti-doped BiFeO3 indicates that the dopant incorporation into the perovskite structure is partial: a certain amount of titanium interacts with the secondary phases shifting the corresponding Raman bands. Our results also demonstrate that Raman spectroscopy is a powerful tool to obtain additional information related with the interaction between dopants and parasitic phases.

    11. Raman spectroscopy of various phosphate minerals and occurrence of tuite in the Elga IIE iron meteorite

      Konstantin D. Litasov and Nikolay M. Podgornykh

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5119

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      The Raman spectra of phosphate minerals: apatite, merrillite, panethite, brianite, czochralskiite, maricite, new phosphate Na2Fe(Mg,Ca)(PO4)2 and high-pressure phase tuite from the Elga IIE iron meteorite are characterized. Panethite, brianite, czochralskiite and new Na-Fe phosphate were described for the first time. Tuite has similar composition and was formed after merrillite. This is the first finding of tuite in iron meteorites and the only second finding of high-pressure mineral in them.

    12. Micro-Raman spectroscopy and complementary techniques (hXRF, VP-SEM-EDS, μ-FTIR and Py-GC/MS) applied to the study of beads from the Kongo Kingdom (Democratic Republic of the Congo)

      Alessia Coccato, Mafalda Costa, Anastasia Rousaki, Bernard-Olivier Clist, Karlis Karklins, Koen Bostoen, Ana Manhita, Ana Cardoso, Cristina Barrocas Dias, António Candeias, Luc Moens, José Mirão and Peter Vandenabeele

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5106

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      This work focuses on the analysis of beads recovered between 2013 and 2015 from eight sites along the Inkisi River valley and one on the southern part of the Bangu range, in the current Democratic Republic of the Congo. Micro-Raman spectroscopy was selected as a first-choice technique for the material characterization of the glass, in terms of matrix (formers, stabilizers, flux, etc.) and colour/opacity, in combination with auxiliary techniques such as hXRF, VP-SEM-EDS, μ-FTIR, and Py-GC/MS, in order to fully characterize glass and non-glass beads from a chemical point of view.

    13. The first use of portable Raman instrumentation for the in situ study of prehistoric rock paintings in Patagonian sites

      Anastasia Rousaki, Cristina Vázquez, Verónica Aldazábal, Cristina Bellelli, Mariana Carballido Calatayud, Adam Hajduk, Emmanuel Vargas, Oscar Palacios, Peter Vandenabeele and Luc Moens

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5107

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      Portable Raman spectroscopy is applied for the first time on rock art paintings from hunter-gatherers in three different provinces in Patagonia, Argentina (Neuquén, Río Negro, and Chubut). During a single research campaign, 17 sites were investigated, which makes this study as one of the most condensed expeditions on measuring rock art paintings. The purpose of this paper is to describe possible difficulties that are encountered during in situ Raman measurement of Patagonian prehistoric rock art, and some possible improvements are suggested.

    14. Obtaining Raman spectra of minerals and carbonaceous matter using a portable sequentially shifted excitation Raman spectrometer – a few examples

      Jan Jehlička, Adam Culka and Filip Košek

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5105

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      A new portable sequentially shifted excitation Raman spectrometer allows obtaining excellent quality, fluorescence-free Raman spectra of minerals in the range of 300–3200 cm−1. First tests on specimens of amorphous carbons from metamorphic rocks, crystalline organic minerals, sulfates, and carbonates are given here. Comparison of performances with other portable Raman spectrometers is made, and future field use for geoscience and exobiology is suggested.

    15. Raman-spectroscopy-based differentiation between cow and buffalo milk

      Rahat Ullah, Saranjam Khan, Hina Ali, Muhammad Bilal, Muhammad Saleem, Arshad Mahmood and Mushtaq Ahmed

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/jrs.5103

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      In this study, Raman spectroscopy together with chemometric technique has been demonstrated to differentiate between cow and buffalo milk. The outcome of results indicate that Raman spectroscopy successfully differentiate between cow and buffalo milk based on the presence and absence of β-carotene, respectively. Principal component analysis further highlighted the spectral differences and shows clear separation on the basis of features obtained from their Raman spectra. Raman spectra of β-carotene in milk make it a very good biomarker to differentiate between these two species.

    16. Raman study of HoFe3(BO3)4 at simultaneously high pressure and high temperature: pT phase diagram

      A. S. Krylov, I. A. Gudim, I. Nemtsev, S. N. Krylova, A. V. Shabanov and A. A. Krylov

      Version of Record online: 8 FEB 2017 | DOI: 10.1002/jrs.5078

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      On the basis of Raman spectra of a HoFe3(BO3)4 crystal, the assignment to one of the two possible crystal phases at high temperature and high pressure has been made. The experimental pT phase diagram of HoFe3(BO3)4 was established. The phase boundary equation was obtained. Neither triple points nor a phase with new symmetry was revealed in the phase diagram. A critical point with the temperature T = 560 K and the pressure p = 2.53 GPa was found. The nanocrystals with different shape began to grow on crystal surface after reaching that point. The composition of new nanocrystals is identical to the composition of initial crystal.

    17. First-order Raman scattering in three-layered Mo-based ternaries: MoAlB, Mo2Ga2C and Mo2GaC

      O. Chaix-Pluchery, A. Thore, S. Kota, J. Halim, C. Hu, J. Rosen, T. Ouisse and M. W. Barsoum

      Version of Record online: 6 FEB 2017 | DOI: 10.1002/jrs.5087

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      The first-order Raman spectra of three-layered Mo-based ternaries, MoAlB, Mo2Ga2C and Mo2GaC, were reported for the first time. The compounds present similarities in their crystal structure consisting of Mo boride or carbide sublattices interleaved by monolayers or bilayers of pure Al or Ga. The experimental peak positions were compared with those predicted from density functional theory; good agreement was obtained, indirectly validating both. All modes in the three compounds were symmetry assigned.

    18. Raman spectroscopy and imaging of Bernal-stacked bilayer graphene synthesized on copper foil by chemical vapour deposition: growth dependence on temperature

      M. Fabiane, M. J. Madito, A. Bello and N. Manyala

      Version of Record online: 27 JAN 2017 | DOI: 10.1002/jrs.5094

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      The Bernal-stacked bilayer graphene synthesized by atmospheric pressure chemical vapour deposition on copper foil exhibits uniform films at low growth temperatures (~780 °C) with a high disorder and becomes non-uniform at high growth temperatures (~867–973 °C) with low disorder. Competition between carbon adatoms supply through dehydrogenation of the CHx species, mobility and desorption rate of the carbon-adatom species for nucleation of the bilayer graphene as a function of temperature is considered the reason for the different growths.

    19. Raman microspectroscopic studies of unirradiated homogeneous (U0.76Pu0.24)O2+x: the effects of Pu content, non-stoichiometry, self-radiation damage and secondary phases

      Zeynep Talip, Sylvain Peuget, Magali Magnin, Lydie Berardo, Christophe Valot, Romain Vauchy and Christophe Jégou

      Version of Record online: 27 JAN 2017 | DOI: 10.1002/jrs.5092

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      Characterization of the radioactive materials by Raman spectroscopy needs special attention. The present study aims at giving a general guidance for the characterization of U-Pu mixed oxides with Raman spectroscopy by comparing the Raman spectrum of annealed (U0.76Pu0.24)O2 and 30-year-old (U0.76Pu0.24)O2+x samples. It has been pointed out that before analysing Raman spectra, Pu content, concentration of decay products, level of radiation damage, storage conditions, non-stoichiometry and formation of secondary phases should be taken into consideration.

    20. Laser alteration on iron sulfides under various environmental conditions

      I. Weber, U. Böttger, S. G. Pavlov, H.-W. Hübers, H. Hiesinger and E. K. Jessberger

      Version of Record online: 13 JAN 2017 | DOI: 10.1002/jrs.5083

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      In preparation for space missions, we investigate iron sulfides to measure the influence of various environmental conditions and the effect of laser irradiation itself on the obtained Raman spectra, relevant for measurements on Mars, the Moon, and asteroids. We found that Raman spectra of different iron di-sulfides are stable under different environmental conditions and with increasing laser power. In contrast, iron sulfides are very sensitive to increasing laser power in ambient air and convert into hematite and magnetite.

    21. Tyrian purple in archaeological textiles: DMF extraction and recrystallization for the Raman identification of precursors and derivatives

      Brenda Doherty, Witold Nowik, Costanza Miliani and Catia Clementi

      Version of Record online: 13 JAN 2017 | DOI: 10.1002/jrs.5096

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      In this work, a micro-Raman sample pre-treatment is proposed for the characterization brominated and unsubstituted isatins and indirubins, the minor components of Tyrian purple. Highlights include the hypothesized presence of carotenoids, porphyrin-type copper and iron complex biomarkers. The method has been validated for a series of reference textiles and archaeological samples in accordance with HPLC photodiode array.

    22. Raman study of structural transformations in self-assembled diphenylalanine nanotubes at elevated temperatures

      Pavel S. Zelenovskiy, Anton O. Davydov, Alexander S. Krylov and Andrei L. Kholkin

      Version of Record online: 13 JAN 2017 | DOI: 10.1002/jrs.5084

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      Structural transformations in diphenylalanine nanotubes at elevated temperatures are studied by Raman spectroscopy. For the first time, these transformations are considered in the context of effective frequency of nanotubes' lattice vibrations and reconstruction of the water subsystem in the nanotubes, demonstrating that many effects in nanotubes are induced by the variation of the water subsystem. The microscopic details of diphenylalanine cyclization are revealed.

    23. Resonance Raman and UV–VIS spectroscopic investigation of the reaction of tetracyanoethylene and N-methyldiphenylamine

      Natália M. Monezi and Rômulo A. Ando

      Version of Record online: 11 JAN 2017 | DOI: 10.1002/jrs.5091

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      In this work, it is showed for the first time the characterization of the intermediate species of the reaction between tetracyanoethylene and N-methyldiphenylamine in solution. Adjusting the reaction conditions such as solvent polarity and the amine concentration, it was possible to stabilize the intermediate species. The comparison of the reactions in dichloromethane and acetonitrile shows that the neutral adduct and zwitterionic intermediate species are stabilized in nonpolar medium, revealing the role played by the solvent in defining the mechanistic pathways of this model charge transfer initiated reaction. These intermediate species as final product were characterized by electronic ultraviolet–visible (UV–VIS) and vibrational (resonance Raman) spectroscopies and combined with density functional theory and time-dependent density functional theory calculations.

    24. Resonance Raman optical activity of zeaxanthin aggregates

      M. Dudek, G. Zajac, A. Kaczor and M. Baranska

      Version of Record online: 11 JAN 2017 | DOI: 10.1002/jrs.5089

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      The goal of this work was an experimental observation of a new phenomenon of enhancement in Raman scattering: aggregation-induced resonance Raman optical activity (AIRROA). Aggregates of zeaxanthin show a strong ECD spectra, but only J1 exhibits RROA. There are two principal conditions to record the RROA spectrum: (1) the polyene chains of zeaxanthin molecules have to be arranged in supramolecular chiral structures and (2) the helical aggregates also have to absorb at the wavelength of ROA excitation (532 nm).

    25. Raman spectroscopic study of cracking and hydrolysis of propane in fused silica capillary capsules between 300 and 400 °C

      Xiaochun Xu and I-Ming Chou

      Version of Record online: 11 JAN 2017 | DOI: 10.1002/jrs.5093

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      Raman spectra of the aqueous phase of two samples containing propane and water (nos. Pr-W-5 and Pr-W-6) collected after heating, showing the production of methanol (peaks near 2847 and 2956 cm−1) and ethanol (peaks near 2885, 2936, and 2983 cm−1) during hydrolysis of propane. The peak at 2992.52 cm−1 is a calibration line from Ne–He emission.

    26. Raman scattering and alternative current conduction mechanism of the high-temperature phase transition in [(C4H9)4N]3Bi2Cl9

      W. Trigui, A. Oueslati, F. Hlel and A. Bulou

      Version of Record online: 29 DEC 2016 | DOI: 10.1002/jrs.5074

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      The evolution of Raman wavenumber versus temperature shows a remarquable shifting of the bands associated to alkyl chains, suggesting that the phase transition is governed by the reorientational motion of the organic part [(C4H9)4N]+.

    27. High-resolution stimulated Raman spectroscopy from collisionally populated states after optical pumping (II): 13C2H2, 13C12CH2, 13C12CD2 and 13C2D2

      Raúl Z. Martínez, Dionisio Bermejo, Gianfranco Di Lonardo and Luciano Fusina

      Version of Record online: 18 NOV 2016 | DOI: 10.1002/jrs.5066

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      A combination of a pump-probe double resonance Raman technique and the naturally occurring process of vibration-to-vibration collisional relaxation is used to populate and obtain high-resolution Raman spectra of vibrationally excited states.

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