scholarly journals Fourier Transformation Infrared Spectroscopic Studies of Acidity of NaH-13 X Zeolites

2018 ◽  
Vol 21 (3) ◽  
pp. 428-435
Author(s):  
Shatha Abd-Alhameed Al. Sofy

Fourier transformation Infrared spectroscopy (FTIR) has been used to characterize and measure the concentration of acid sites (Si-OH-Al groups) in NaH-13 X Zeolites. Ion exchange was followed by dealumination to get (28, 40, 65, 85.8 and 97.5 Wt. %) of NaH-13 X Zeolites samples. The conclusion of homogeneity of OH groups was obtained by analysis of Fourier transformation infrared spectroscopy absorption bands of OH groups after adsorption and desorption of Ammonia. It found that there were different acid sites on a broader absorption (3,800-3,000 cm-1) corresponds to hydroxyl groups of the less acidic Brønsted acid sites approximately at 3464cm-1 and the more acidic at 3441cm-1 and Lewis acid sites was found at 1636 cm-1 which is few and weak acid sites . It can be conclusion that concentrations of OH groups increased with increasing the exchange degree and delamination. The concentration of acid sites in samples were calculated from stretching frequencies and extinction coefficients of OH bands, also the frequency shift  ΔνOH = 23 cm-1 which was due to the hydrogen bonding of OH groups with ammonia in 97.5 % NaH-13 X Zeolites. Knowing the acidity of catalyst is important for the reactions which required acidic surface.

Clay Minerals ◽  
1967 ◽  
Vol 7 (1) ◽  
pp. 51-61 ◽  
Author(s):  
Koji Wada

AbstractThe OH-OD exchange of kaolin minerals through contact with D2O introduced into interlayer space via intersalation resulted in a partial shift of the OH absorption bands. The total decrease in OH absorbance upon deuteralion was 52, 56, and 47% for the kaolinite, dickite-nacrite, and halloysite respectively, but the percentage decrease differed for the different absorption maxima of any one mineral. A secondary OH—OD exchange in the deuterated specimens was also observed upon heating to 350 and 400° C. These data together with the lack of deuteration in montmorillonite, and available orientation data on the kaolin OH groups by infrared spectroscopy, suggest that only two-thirds of the inner-surface OH groups form the interlayer OH—O bonds.


Clay Minerals ◽  
1979 ◽  
Vol 14 (2) ◽  
pp. 109-114 ◽  
Author(s):  
J. D. Russell

AbstractIR spectroscopy has shown that adsorbed water is almost completely removed from ferrihydrite by evacuation at room temperature. Absorption bands at 3615 and 3430 cm−1 appearing thereafter are interpreted as arising from OH groups located respectively at the surface and deeper in the structure. These groups are readily converted to OD on treatment with D2O vapour and this has allowed the OH deformation vibration to be identified at 800 cm−1. It is proposed that OH groups in ferrihydrite are about half as numerous as those in akaganéite (β-FeOOH) and that they may occur in environments similar to those in this mineral. The formula for ferrihydrite proposed by earlier workers, 5 Fe2O3.9H2O, should thus be amended to Fe2O3. 2 FeOOH.2·6H2O in order to indicate the presence of structural OH groups. A re-appraisal of the ferrihydrite structure appears desirable.


Author(s):  
Kuralla Hari ◽  
Saripilli Rajeswari ◽  
Kolapalli Venkata Ramanamurthy

Objective: To formulate orally disintegrating taste masked tablets of drotaverine hydrochloride (HCl) by sublimation technique.Methods: Initially superdisintegrant was selected and its concentration was optimized by pre-compression and post-compression parametric evaluation. Camphor and menthol were used as sublimating agents alone and in combination to mask the taste of drotaverine hydrochloride. Prepared tablets were evaluated for physicochemical evaluation, in vitro dissolution studies and fourier transformation-infrared spectroscopy, differential scanning calorimetry and X-ray diffractometry studies.Results: The optimised formulation DCM2 prepared with a mixture of camphor and menthol was characterised by fourier transformation-infrared spectroscopy, differential scanning calorimetry and X-ray diffractometry studies and found no incompatibility and no major shifts were noticed.Conclusion: The results demonstrated that the prepared drotaverine HCl orally disintegrating tablets showed better taste masking. The present sublimation technique can be effectively used for taste masking and also for orally disintegrating tablets.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Ashraf Yehia El-Naggar

The prepared, modified, and coated alumina surfaces were characterized by infrared spectroscopy (FTIR) to investigate the surface properties of the individual and double modified samples. FTIR helps in reporting the changes occurred in hydroxyl groups as well as the structure changes as a result of thermal treating, hydrothermal treating, silylation treating, alkali metal treating, coating, and bonding with polymer. FTIR spectroscopy represents the strength and abundance of surface acidic OH which determine the adsorption properties of polar and nonpolar sorbents. Generally, all treated samples exhibit decrease of OH groups compared with those of parent ones producing alumina surfaces of different adsorptive powers.


1964 ◽  
Vol 42 (4) ◽  
pp. 802-809 ◽  
Author(s):  
N. W. Cant ◽  
L. H. Little

The infrared spectrum of ammonia adsorbed on porous glass at 20 °C and 150 °C has been studied in the region 1450–4000 cm−1. No absorption band due to the asymmetric bending mode of ammonia was observed but in the NH stretching region, bands occurred at 3280 cm−1, 3320 cm−1, 3365 cm−1, and 3400 cm−1. The bands at 3320 cm−1 and 3400 cm−1 were easily removed by evacuation and are due to ammonia molecules hydrogen bonded through the nitrogen atom to surface hydroxyl groups. The bands at 3280 cm−1 and 3365 cm−1 were not removed by evacuation even at 150 °C and are due to ammonia molecules held to surface Lewis acid sites by the nitrogen lone-pair electrons. The site for this adsorption is not a surface hydroxyl group. These results are further evidence for the existence of the two adsorption sites proposed by Folman and Yates. Deuteration of the surface OH groups was easily accomplished with D2O vapor at 300 °C and the rate of hydrogen exchange between adsorbed ammonia molecules and surface OD groups was found to be rapid.


Author(s):  
В.И. Иванов-Омский ◽  
С.М. Герасюта ◽  
Е.И. Иванова

Исследованы ИК-спектры древесины ели обыкновенной в области поглощения валентными колебаниями гидроксильных групп. Изучались как образцы естественной влажности, так и подвергнутые отжигу при 105 °С. Образцы для исследований отбирались из взрослого дерева ели обыкновенной (Picea abies) на высоте 2,5–3 м (возраст в районе спилов 25–30 лет). Из безcучковой зоны вырезались образцы в виде кубиков размером 3×3×3 см3, из которых непосредственно перед записью спектра изготовлялось пять тангенциальных микротомных срезов толщиной 80–100 мкм. Спектральный анализ проводился с помощью ИК-Фурье спектрометра ФСМ-1201 с разрешением 4 см–1. Показано, что реальная микроструктура ели не препятствует разделению рассеянного и поглощаемого излучений. Для характеристики длин и энергий водородных связей использованы известные корреляционные соотношения частот поглощения гидроксильными группами, охваченными водородными связями, с их длиной и энергией. C этой целью экспериментальный спектр в области поглощения ОН-группами аппроксимируется гауссовыми контурами, каждый из которых ассоциируется с определенной разновидностью Н-связи. Сдвиги частот подгоночных контуров относительно частоты ОН-группы, не охваченной Н-связью, использованы для оценки энергий и длин связей, а соотношение их площадей – для оценки их концентраций. Показано, что при термическом отжиге происходит выжигание низкочастотного крыла полосы поглощения ОН-групп. Приводится диаграмма распределения Н-связей по концентрациям до отжига и после. Показано, что при отжиге число наиболее сильных связей незначительно уменьшается, но их энергия уменьшается заметно. Судя по величине частоты эти полосы поглощения относятся к межмолекулярным связям, и уменьшение их энергии означает, что отжиг затрагивает в первую очередь именно эти связи. Самые слабые исчезают совсем. Детальное исследование этого явления позволит обосновать выбор предельных температур тепловой обработки древесины, не нарушающих ее механических свойств. Отмечается более высокая температурная стабильность внутримолекулярных связей с энергией ≈10 кДж/моль. Investigated the IR spectra of spruce wood in the area of absorption of the stretching vibrations of hydroxyl groups. Been studied, as samples with natural moisture, and subjected to annealing at S. Samples for research were collected from adult trees of Norway spruce (Picea abies) at a height of 2.5–3.0 m (age in the area of cut 25–30 years). From cleared areas were cut samples in the form of cubes of size 3×3×3 cm3, of which just before recording the spectrum produced 5 tangential microtome sections with a thickness of 80–100 nm. Spectral analysis was performed using IR-Fourier spectrometer FSM-1201 with a resolution of 4 cm–1. Shows that the real microstructure of spruce does not prevent the separation of scattered and absorbed radiation. For the characteristic lengths and energies of hydrogen bonds used are known from the literature correlation of the ratio between the frequency of absorption of hydroxyl groups covered by hydrogen bonds with their length and energy. To this end, the experimental spectrum in the region of absorption of OH-groups approximated by a Gaussian contours, each of which is associated with a certain kind of H-bonds. The frequency shifts fitting contours of the relative frequency of OH-groups not covered by the H-bond, is used to evaluate energies and bond lengths, and the ratio of their squares to estimate their concentrations. It is shown that under thermal annealing is burning low frequency wing of the absorption bands of OH-groups. A diagram of the distribution of H-bonds energy on concentrations presented before and after annealing. It is shown that annealing the strongest bonds is slightly decreasing, but their energy decreases significantly. The weakest disappear altogether. A detailed study of this phenomenon will allow us to justify the choice of limiting the temperature of the heat treatment of wood that do not violate its mechanical properties. Noteworthy higher temperature stability of intramolecular bonds with energies of ≈10 kJ/mol.


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