scholarly journals INVESTIGATION OF THE POSSIBILITY OF USING THE METHOD OF DIFFERENTIAL SPECTROPHOTOMETRY FOR THE ANALYSIS OF OVERLAPPING ABSORPTION BANDS OF TRITERPENE SAPONINS CHROMOPHORES AND THEIR QUANTITATIVE DETERMINATION IN AQUEOUS SOLUTIONS

2021 ◽  
pp. 267-276
Author(s):  
Natal'ya Vladimirovna Mironenko ◽  
Irina Viktorovna Shkutina ◽  
Anastasiya Sergeyevna Kalmykova ◽  
Vladimir Fedorovich Selemenev
Keyword(s):  
Quantitative Determination ◽  
Bathochromic Shift ◽  
Aldehyde Group ◽  
Carboxyl Groups ◽  
Uv Spectrum ◽  
Absorption Bands ◽  
Quillaja Saponaria ◽  
Differential Spectrophotometry ◽  
Calibration Models ◽  
High Concentrations

A detailed analysis of the absorption spectra of mono- and bidesmoside triterpene glycosides was performed. It is suggested that the maximum in the region of 198–208 nm is attributed to the absorption of the double bond in the cyclohexene ring of the aglycone. The second less seen maximum at a wavelength of 280 nm is observed in the spectrum of saponin Quillaja Saponaria and is almost completely absent in the spectrum of saponin Mukorossi Sapindus. Identification of this maximum is extremely difficult, since its presence can be due to both the aldehyde group in the aglycone and the hydroxyl and carboxyl groups in the carbohydrate molecules. Using the method of differential spectrophotometry, a method for decomposing the UV spectrum of saponins into its constituent components is proposed and justified. A spectral analysis was performed, including the assignment of the absorption bands to the functional groups of the studied compounds. The possibility of estimating changes in the spectral properties of glycoside solutions with changes in the acidity of the medium is considered. The possibility of a bathochromic shift of the maximum absorption of the aglyconic part of saponin depending on the microenvironment (the structure of the carbohydrate part) and changes in the pH of the solution is established. It is shown that the bands at 274, 280.5 nm correspond to n-π* transitions of carbonyl and carboxyl groups and are determined only in the regions of high concentrations in Quillaja Saponaria saponin solutions. Based on the results obtained, calibration models for the quantitative determination of saponins in solutions are proposed. The regression analysis of the calibration equations is carried out, the main statistical indicators are calculated.

scholarly journals Oligomeric silsesquioxanes containing dye Rhodamine B in an organic shell

2019 ◽  
Vol 85 (1) ◽  
pp. 47-57
Author(s):  
Mariana Gumenna ◽  
Nina Klimenko ◽  
Alexandr Stryutsky ◽  
Alexandr Shevchuk ◽  
Viktor Kravchenko
Keyword(s):  
Fluorescence Spectrum ◽  
Rhodamine B ◽  
Bathochromic Shift ◽  
Hydroxyl Groups ◽  
Uv Spectrum ◽  
Absorption Bands ◽  
Lactone Form ◽  
Organic Shell ◽  
Langmuir Blodgett Films ◽  
Fluorescence Peak

A method for the synthesis of amphiphilic reactive oligomeric silsesquioxanes (OSS) with fragments of Rhodamine B fluorescent dye and hydroxyl groups in organic shell (OSS-Rh) by the reaction between carboxyl groups of the dye and epoxy groups of the mixture of oligomeric silsesquioxanes (OSS-Ep) was developed. The structure of the synthesized substance was characterized by the methods of IR and 1H NMR spectroscopy. The UV-spectrum of the OSS-Rh compound in dimethylformamide (DMF) solution was characterized by absorption bands of both the colored zwitterion (562 nm and 350 nm) and the colorless lactone (318 nm) forms of Rhodamine B. The absorption band at 562 nm in the spectrum of OSS-Rh in DMF solution was more intense than the analogous band in the spectrum of the original Rhodamine B. Therefore, the attachment of Rhodamine B to the silsesquioxane core of an oligomeric silsesquioxanes mixture does not have a significant effect on the position of the absorption maxima in UV-spectrum and prevents dye’s fragments from converting to the colorless lactone form. In the fluorescence spectra of both Rhodamine B and OSS-Rh, obtained using ethyl alcohol as a solvent, a peak is observed at λmax = 570 nm (λex = 500 nm). In the fluorescence spectrum of OSS-Rh obtained in DMF, a fluorescence peak is observed at λmax = 586 nm (λex = 520 nm). Consequently, the replacement of ethanol by DMF is accompanied by a bathochromic shift of the fluorescence peak of OSS-Rh. In the fluorescence spectrum of Rhodamine B at the same conditions, the peak of fluorescence is absent because of transition of the dye to the lactone form. The compounds obtained can be used in formation of functional Langmuir-Blodgett films as well as in obtaining polymer nanocomposites by covalent bonding.

scholarly journals OLIGOMERIC SILSESQUIOXANES COMBINING AZO- AND FLUORESCENT DYES IN ORGANIC SHELL

2019 ◽  
Vol 85 (4) ◽  
pp. 71-80
Author(s):  
Mariana Gumenna ◽  
Nina Klimenko ◽  
Alexandr Stryutsky ◽  
Alexandr Shevchuk ◽  
Viktor Kravchenko ◽  
...  
Keyword(s):  
Absorption Band ◽  
Rhodamine B ◽  
Fluorescent Dyes ◽  
Hydroxyl Groups ◽  
Uv Spectrum ◽  
Absorption Bands ◽  
Organic Shell ◽  
Similar Band ◽  
Inorganic Nanocomposites ◽  
Epoxy Groups

A method for the synthesis of reactive oligomeric silsesquioxanes, combining fragments of azo dye 4-(phenylazo)phenol and fluorescent dye Rhodamine B in various proportions in an organic shell was developed. These compounds were obtained by the reaction between the oligosilsesquioxane nanoparticles consisting of a mixture of linear, branched, ladder and polyhedral structures with epoxy groups in an organic frame (OSS–Ep) and the dyes. The structure of the synthesized substances was characterized by the methods of IR and 1H NMR spectroscopy. The UV-Vis spectra of OSS–Pp–Rh in DMF solution contain absorption bands characteristic of both acidic (560 and 350 nm) and lactone (in the range of 318–326 nm) forms of Rhodamine B. The absorption band of 4-(phenylazo) phenol fragments corresponding to π−π* transition is observed at 348 nm and overlaps the absorption band of Rhodamine B at 350 nm.The intensity of the absorption bands of fragments of various dyes depends on their content in organic frame of the silsesquioxane core. The intensity of the absorption bands at 348 nm and at 560 nm increases with an increase in the content of 4-(phenylazo)phenol and Rhodamine B correspondingly.It should be noted that when using DMF as a solvent the absorption band corresponding to acidic form of Rhodamine B at 560 nm in the UV-Vis spectra of the compounds obtained is more intense than similar band in the spectrum of the original Rhodamine B. Therefore, the attachment of Rhodamine B to the silsesquioxane core of oligomeric silsesquioxanes mixture does not have a significant effect on the position of absorption maxima in the UV-spectrum and prevents dye’s fragments from converting to the colorless lactone form. In the fluorescence spectra of OSS–Pp–Rh obtained using DMF as a solvent a peak at λ max = 592 nm (λex= 520 nm) is observed. The position of the fluorescence peak and its intensity in the spectra at the same optical density of the medium practically do not depend on the ratio of fragments of 4-(phenylazo)phenol and Rhodamine B in organic frame of OSS–Pp–Rh.  The combination of two different chromophores in organic shell of the silsesquioxane core broadens the range of absorbed light and the change of their ratio allows to adjust the absorption intensity in a certain area. The presence of hydroxyl groups makes it possible to introduce the obtained compounds into the composition of polymeric organic-inorganic nanocomposites by covalent bonding.

scholarly journals SYNTHESIS AND SPECTRAL CHARACTERISTICS OF PERSPECTIVE NANOSIZED CARBON QUANTUM DOTS FOR ADSORPTION AND CATALYTIC PROCESSES

2020 ◽  
Vol 86 (1) ◽  
pp. 3-11
Author(s):  
Volodymyr Ogenko ◽  
Svitlana Orysyk ◽  
Ljudmila Kharkova ◽  
Oleg Yanko
Keyword(s):  
Quantum Dots ◽  
Bathochromic Shift ◽  
Spectral Characteristics ◽  
Carbon Quantum Dots ◽  
Hypsochromic Shift ◽  
Absorption Bands ◽  
Rhodium Chloride ◽  
Electron Transitions ◽  
Trivalent State ◽  
Adsorption Processes

Processes of interaction between carbon quantum dots (CQDs) and solutions of rhodium, ruthenium and palladium chlorides in the surface layer have been investigated by electron and IR spectroscopy. When rhodium chloride is added to a solution of CQDS, a bathochromic shift of the β- and p-absorption bands (ABs) at 48725 and 41711 cm-1 as well as hypsochromic shift of the α-AB at 28935 cm-1 indicate that rhodium adsorption occurs on the surface of CQDs. The bathochromic shift of the absorption bands at 22400 сm1 together with the hypsochromic shift of ABs corresponding to d-d electron transitions in the metal ions indicates the formation of rhodium with CQDs. When ruthenium and palladium chlorides are added to an aqueous solution of CQDs, the intensive of ABs characterizing the complex anions [RuCl6]3-, [RuCl6]2- or [PdCl4]2- are absent in the UV-Vis spectra. This indicates the passage of adsorption processes of metals on the surface of CQDs.  The present of ABs (at 27055 and 25125 сm-1) indicate the trivalent state of ruthenium ion; the p-ABs bathochromic shift as well as α-ABs hypsochromic shift indicates the probable complex formation of CQDs with Ru3+ ions. The change in the position of the absorption bands of d-d electron transitions (at 25448 сm1) together with the bathochromic shift of p-ABs and hypsochromic shift of α-ABs indicates a change in coordination environment in the palladium ion with the possible formation of Pd → N bond. The IR-spectra data of CQDs showed the presence of a number of characteristic ABs for functionalized CQDs: ν(N–H) at 3260 сm1, (C=O) at 1830, 1840 and 1850 сm1, –С=O(NH) at 1770 сm1, ν(C=N) at 1680 and δ(N–H) at 1640 сm1, which confirms the coordination of metals on the surface of CQDs.

DEVELOPMENT OF A METHOD FOR QUANTITATIVE DETERMINATION OF THE AMOUNT OF FLAVONOIDS IN TRIPLEUROSPERMUM INODORUM’S FLOWERS

2021 ◽  
pp. 157-166
Author(s):  
Blinova O.L. ◽  
Gileva A.A. ◽  
Hlebnikov A.V. ◽  
Belonogova V.D. ◽  
Turyshev A.Y.
Keyword(s):  
Quantitative Determination ◽  
Aluminum Chloride ◽  
Chloride Solution ◽  
Uv Spectra ◽  
Raw Material ◽  
Spectral Studies ◽  
Scientific Medicine ◽  
Differential Spectrophotometry ◽  
The Stability

Chamomilla recutita is used in scientific medicine. Tripleurospermum inodorum (L.) Sch. Bip. is widely spread among possible impurities of Chamomilla recutita (L.) Rauschert. This plant is perspective for establishment into scientific medicine but it can’t change Chamomilla recutita (L.) Rauschert. Purpose of research: development of a method for the quantitative determination of the amount of flavonoids in terms of rutin in Tripleurospermum inodorum’s flowers using differential spectrophotometry. Materials and methods. The samples prepared in different parts of Russia were used as objects of research. (2017 – 2020). Spectral studies were carried out in the wavelength range of 350-430 nm with a step of 1 nm using a spectrophotometer SF-2000. Results. To determine the analytical wavelength, the UV spectra of alcohol extraction of Tripleurospermum inodorum’s flowers were studied. Maximum of absorption was noticed at wavelength 370 nm. The differential spectrum of the same extraction with an aluminum chloride solution of 2% in 96% alcohol has a maximum at a length of 410±2 nm, which coincides with the maximum of the Standard Sample (SS) of rutin. The largest number of flavonoids is extracted by 70% alcohol. The maximum optical density and the highest output of the number of flavonoids from the raw material is observed at a degree of grinding of 2 mm with a single extraction for 60 minutes. In the conditions of complexation, the optimal ratio of the volume of the test solution and aluminum chloride with a solution of 2% in 96% alcohol is the ratio of 1:1. The stability of the complex with an aluminum chloride solution of 2% in 96% alcohol is observed in 40 minutes after the start of the reaction and retains it for 30 minutes. Findings. The method is developed and the parameters of the quantitative determination of the amount of flavonoids in Tripleurospermum inodorum flores are determined in terms of rutin using differential spectrophotometry.

scholarly journals Analysis of functional groups in atmospheric aerosols by infrared spectroscopy: sparse methods for statistical selection of relevant absorption bands

2016 ◽  
Vol 9 (7) ◽  
pp. 3429-3454 ◽  
Author(s):  
Satoshi Takahama ◽  
Giulia Ruggeri ◽  
Ann M. Dillner
Keyword(s):  
Infrared Spectra ◽  
Atmospheric Aerosols ◽  
Quantitative Prediction ◽  
Calibration Model ◽  
Vibrational Modes ◽  
Aerosol Composition ◽  
Absorption Bands ◽  
Calibration Models ◽  
Ft Ir ◽  
Selection Of

Abstract. Various vibrational modes present in molecular mixtures of laboratory and atmospheric aerosols give rise to complex Fourier transform infrared (FT-IR) absorption spectra. Such spectra can be chemically informative, but they often require sophisticated algorithms for quantitative characterization of aerosol composition. Naïve statistical calibration models developed for quantification employ the full suite of wavenumbers available from a set of spectra, leading to loss of mechanistic interpretation between chemical composition and the resulting changes in absorption patterns that underpin their predictive capability. Using sparse representations of the same set of spectra, alternative calibration models can be built in which only a select group of absorption bands are used to make quantitative prediction of various aerosol properties. Such models are desirable as they allow us to relate predicted properties to their underlying molecular structure. In this work, we present an evaluation of four algorithms for achieving sparsity in FT-IR spectroscopy calibration models. Sparse calibration models exclude unnecessary wavenumbers from infrared spectra during the model building process, permitting identification and evaluation of the most relevant vibrational modes of molecules in complex aerosol mixtures required to make quantitative predictions of various measures of aerosol composition. We study two types of models: one which predicts alcohol COH, carboxylic COH, alkane CH, and carbonyl CO functional group (FG) abundances in ambient samples based on laboratory calibration standards and another which predicts thermal optical reflectance (TOR) organic carbon (OC) and elemental carbon (EC) mass in new ambient samples by direct calibration of infrared spectra to a set of ambient samples reserved for calibration. We describe the development and selection of each calibration model and evaluate the effect of sparsity on prediction performance. Finally, we ascribe interpretation to absorption bands used in quantitative prediction of FGs and TOR OC and EC concentrations.

scholarly journals Six-fold C–H borylation of hexa-peri-hexabenzocoronene

2020 ◽  
Vol 16 ◽  
pp. 391-397 ◽  
Author(s):  
Mai Nagase ◽  
Kenta Kato ◽  
Akiko Yagi ◽  
Yasutomo Segawa ◽  
Kenichiro Itami
Keyword(s):  
Density Functional ◽  
Bathochromic Shift ◽  
Density Functional Theory Calculations ◽  
Absorption Bands ◽  
Functional Theory ◽  
X Ray ◽  
X Ray Crystallography ◽  
Polycyclic Aromatic ◽  
Direct Functionalization ◽  
Poorly Soluble

Hexa-peri-hexabenzocoronene (HBC) is known to be a poorly soluble polycyclic aromatic hydrocarbon for which direct functionalization methods have been very limited. Herein, the synthesis of hexaborylated HBC from unsubstituted HBC is described. Iridium-catalyzed six-fold C–H borylation of HBC was successfully achieved by screening solvents. The crystal structure of hexaborylated HBC was confirmed via X-ray crystallography. Optoelectronic properties of the thus-obtained hexaborylated HBC were analyzed with the support of density functional theory calculations. The spectra revealed a bathochromic shift of absorption bands compared with unsubstituted HBC under the effect of the σ-donation of boryl groups.

Quantitative determination of carboxyl groups when contained in low proportions in polymers

1980 ◽  
Vol 22 (8) ◽  
pp. 2091-2095 ◽  
Author(s):  
V.B. Lushchik ◽  
M.G. Krakovyak ◽  
S.S. Skorokhodov
Keyword(s):  
Quantitative Determination ◽  
Carboxyl Groups
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