FTIR STUDY ON MOLECULAR CONTAMINATION ON SURFACE OF OPTICAL MATERIALS

2006 ◽  
Vol 20 (25n27) ◽  
pp. 3860-3865 ◽  
Author(s):  
MASAHIRO KATOH ◽  
NOBUAKI OKANO ◽  
TOSHIHIDE HORIKAWA ◽  
TAHEI TOMIDA ◽  
NOBUNARI ITOH

The IR spectra of the molecular contaminants on surface of optical materials were measured. The optical disks used were SiO 2, BK7 ( SiO 2 70%, B 2 O 3 10%, K 2 O 8%, N 2 O 8%), CaF 2, ZnSe and Al 2 O 3. N 2, O 2, H 2 O , and CO 2 were adopted as contamination gases. IR spectra of H 2 O (2.7kPa) on BK7 at 373K showed two absorption bands ( OH stretching vibration: around 4000cm-1-3500cm-1 and OH bending vibration: around 2000cm-1-1500cm-1). The absorption intensity decreased with a decrease in temperature and a new band (around 3250cm-1) appeared at 173K. The new band was attributed to phase transition of H 2 O . These phenomena were also observed on the other three discs, except for SiO 2. IR spectra of SiO 2 showed OH stretching band (3676cm-1). The absorption intensity decreased with a decrease in temperature. But two new bands (3720cm-1 and 3620cm-1) appeared under an atmosphere of N 2 (66.5kPa), O 2 (66.5kPa), H 2 O (2.7kPa) or CO 2 (0.7 or 13.3kPa). A similar phenomenon was also observed for BK7, which has OH group. These results suggested the functional group of SiOH interacted with contamination molecules.

2005 ◽  
Vol 60 (8-9) ◽  
pp. 633-636 ◽  
Author(s):  
Nuri Öztürk ◽  
Çağrı Çırak ◽  
Semiha Bahçeli

The adsorption of 1,5-pentanedithiol (1,5-PDT) and 1,6-hexanedithiol (1,6-HDT) in liquid phases on NaA (or 4A-type), CaA (or 5A-type) and NaY zeolites has been studied by using infrared spectroscopy. From the IR spectra it is found that the peak positions of the symmetric as well as the antisymmetric modes of the methylene (CH2) groups are observed at almost the same band values for the title dithiolates adsorbed on the A-type and NaY zeolites. On the other hand, the weak SH stretching vibration, observed for all samples, can be attributed to the sulphure atoms of 1,5-PDT and 1,6-HDT coordinatively adsorbed on cationic sites of the zeolites.


1972 ◽  
Vol 27 (1) ◽  
pp. 110-128 ◽  
Author(s):  
H. Seydewitz ◽  
E.D. Schmid

Abstract On the basis of a simple MO-approach a model to interprete the IR-absorption intensity of the aromatic CH-stretching vibration is developed. Accordingly the gradient of the CH-bond moment is a linear function of the ionicity of the CH-bond.Eight azulenes, which were deuterated at various specified positions, were synthetisized and out of their IR-spectra the gradients of the CH-bond moment at all positions of azulene could be determined. From these experimental data it is concluded, that in relation to benzene the electrons of the CH-bonds in azulene are displaced towards the C-atom at positions with high and towards the H-atom at positions with low π-electron density.Such a polarisation of the CH-bonds in azulene is confirmed, although only qualitatively, by the ionicities of the CH-bonds calculated by the CNDO/2-method and is also in accordance with other experimental observations such as bond lengths and angles, C13H-coupling constants, and the frequencies of the CH-stretching vibrations.It is demonstrated that experiment and calculation fail to correlate quantitatively due to in-adequacies inherent in the CNDO/2-method.


2007 ◽  
Vol 40 (2) ◽  
pp. 984
Author(s):  
E. Theodosoglou ◽  
A. Koroneos ◽  
K. M. Paraskevopoulos ◽  
G. Christofides ◽  
L. Papadopoulou ◽  
...  

Powder IR spectra of natural Ca-amphiboles were studied in the spectral range 4000 to 400 cm'1. The examined samples are: actinolite, tremolite, Mg-hornblende and pargasite. According to their spectra all the minerals of the four species present common features at 3658-3660, 919, 683-687, 661-668, 505-513, 457-464 and 419 cm . Additionally to these bands, the spectra of the actinolites, tremolites and Mghornblendes present common characteristics at 3673, 1094-1098, 989-998, 951, 752-758 and 441-449 cm'1. Moreover, six absorption bands are shown in the spectra of the pargasites at 3690, 981-984, 931, 805-811, 734 and 696-698 cm'1, in addition to the common bands appeared in all Ca-amphiboles, which do not appear in the spectra of the actinolites, tremolites and Mg-hornblendes. The spectra of pargasites are remarkably different from the spectra of the other three mineral species. These discrepancies could be attributed to differences in the structure of pargasites relative to the other three species as well as to the occupancy of the A site especially with Na+.


1981 ◽  
Vol 54 (1) ◽  
pp. 1-14 ◽  
Author(s):  
Shoichiro Yano

Abstract On irradiation with uv light, changes in uv and ir spectra were observed. In the uv spectrum, a minimum at 290 nm due to sulfur, dibenzothiazyl disulfide, and double bonds in the main chains disappeared initially by the consumption of them; but the minimum reappeared on further irradiation reflecting the formation of carbonyl groups. On the other hand, in the ir spectrum two absorption bands appeared at 1720 cm−1 (due to carbonyl groups) and 3450 cm−1 (due to hydroxyl groups). The latter band faded out suggesting the decomposition of hydroperoxides when the vulcanizate was kept in the dark after irradiation. From the findings of the wavelength dependence of photo-oxidation on uv and ir spectra, it was found that the degradation occurred below about 430 nm. However, investigation of the wavelength dependence of photo-oxidation by the measurement of the crosslink density gave the results that crosslinking reactions occurred below about 340 nm, scissions of C-C and polysulfide crosslinks between 340 and about 400 nm, and scissions of polysulfide crosslinks between 400 and 600 nm. These were confirmed by measurements of the dynamic modulus during irradiation. The relative modulus E′(t)/E′(0) increased on irradiation with light at 253.7 nm in a longer time region reflecting a crosslinking reaction. On the other hand, on irradiation with light above 330 nm, E′(t)/E′(0) decreased with time. Change in E′(t)/E′(0) could be represented by the equation of the first order reaction containing an exponential term and the rate constant was determined. The activation energy was calculated as 18.6 kcal/mole from the temperature dependence of the rate constant and agreed with that for scission of polysulfide crosslinks. The photodegradation of the IR vulcanizate occurred also on irradiation with visible light (> 430 nm), and the modulus decreased.


The red absorption bands of CH 2 , previously shown to correspond to a transition between singlet states, have been analysed in detail. In the lower electronic state a 1 A 1 the molecule is a strongly asymmetric top with rotational constants A 000 = 20.14, B 000 = 11.16 and C 000 = 7.06 cm -1 . From these constants a CH distance of 1.11 A and an HCH angle of 102.4° is obtained. In the upper state b 1 B 1 the molecule is nearly linear, having an HCH angle of about 140° and a CH distance of 1.05 A. Most of the observed absorption bands correspond to excitation of the bending vibration v 2 in the upper state (v 2 = 6, 8, ..., 18). In some of them in addition the symmetric stretching vibration v 2 is singly excited. The levels 1, v 2 -4, 0 cause strong perturbations in the levels 0, v 2 , 0 for v 2 = 8, 10, 12, 14. In the lower state only one excited vibrational level 0, 1, 0 has been established which yields v 2 = 1352.6 cm -1. Fragments of some other singlet absorptions in the near ultraviolet and in the vacuum ultraviolet have been observed and are briefly described. The upper state of the near ultraviolet system is probably the predicted 1 A 1 state corresponding to 1 E + in the linear conformation.


KOVALEN ◽  
2021 ◽  
Vol 7 (1) ◽  
pp. 51-58
Author(s):  
Pratiwi Listyana Sareu ◽  
Nurhaeni ◽  
Ahmad Ridhay ◽  
Moh. Mirzan ◽  
Syamsuddin

Gembili bulbs (Dioscorea esculenta L.) have a fairly high carbohydrate content, so they can potentially be a new source of glucomannan compounds. This study aims to determine the yield and glucomannan characteristics of Gembili bulbs at different extraction times and temperatures. Glucomannan was obtained by extraction with water at temperatures of 45, 60, 75, 90, and 105oC for 45, 60, 75, 90, and 105 minutes, and precipitated with isopropyl alcohol. The results showed that the highest yield was obtained at the extraction time of 90 minutes and a temperature of 105oC of 53.09%. The glucomannan of Gembili bulb has a molecular weight of 1,865 x 104 g/mol with ash and water content values of 0.866% and 10.45%, respectively. The results of identification of functional groups with an FTIR spectrophotometer showed that there was a functional group stretching vibration of glucomannan compounds, including the –OH group at a wavenumber of 3431 cm-1 and -C-O-C (glycosidic bond) at a wavenumber of 1020.34 cm-1 and bending vibration of -CH functional groups on wavenumber of 850.61 cm-1.


2003 ◽  
Vol 56 (9) ◽  
pp. 903 ◽  
Author(s):  
Gavin E. Collis ◽  
Dieter Wege

Addition of 2-diazopropane to 1,4-naphthoquinone at low temperature, followed by in situ enolization and acetylation or silylation gave 3,3-dimethyl-1H-benz[f]indazol-4,9-diyl diacetate and 3,3-dimethyl-9-(t-butyl-dimethylsilyloxy)-1H-benz[f]indazol-4-ol, respectively. Functional group manipulation of the latter compound provided a number of other 4,9-disubstituted 3,3-dimethyl-3H-benz[f]indazoles. Irradiation of the diacetate led to clean extrusion of nitrogen to give the naphtho[b]cycloproparene and an alkene. Attempts to elaborate the cycloproparene into the derived cyclopropanaphthoquinone were unsuccessful. Of the other 4,9-disubstituted 3,3-dimethyl-3H-benz[f]indazoles examined, only the compound possessing an acetoxy group at C9 was photoactive, and afforded the expected cycloproparene and alkene. Compounds bearing a hydroxy or alkoxy group at C9 were photochemically inert.


1883 ◽  
Vol 36 (228-231) ◽  
pp. 285-286

After the reading of the note on chlorophyll at the meeting of the society on December 13th, I was reminded by Professor Stokes that e and others had succeeded in separating the complex to which the erm chlorophyll had previously been applied into two substances, or ather groups of substances, one characterised by its green colour and ed fluorescence, the other showing a more distinctly yellow colour without fluorescence, and he suggested to me that it would be advisable to ascertain whether the property of yielding glucose by decomposition with acids might not belong to one of these substances or groups of substances only. Professor Stokes at the same time kindly communicated to me the details of the process whereby he succeeded n effecting the separation referred to, a process depending on the action of carbon disulphide in' removing some of the bodies contained n an alcoholic solution of crude chlorophyll in preference to others. The process employed for the same purpose by Mr. Sorby is essentially the same. Before applying disulphide of carbon to an alcoholic extract of green leaves according to the process of Professor Stokes, it was necessary first to remove the ready-formed glucose, tannin, and other matters soluble in water, which almost always exist in such extracts, and which would by their presence have rendered the result of the experiment quite uncertain. This was done in the way I have already described. An ethereal solution of chlorophyll prepared by my method was evaporated, and the residue having been dissolved in alcohol, the solution was mixed with a quantity of carbon disulphide larger than the alcohol would dissolve, and the mixture well shaken. The carbon disulphide acquired a dark green colour, while the supernatant alcoholic liquid, containing principally the xanthophyll of Professor Stokes and Mr. Sorby, was yellow with a tinge of green. The two liquids having been separated, the lower dark green one was washed several times with alcohol to remove any of the xanthophyll that might still be present, and having then been mixed with a large quantity of alcohol, a current of air was passed through it to remove the excess of carbon disulphide as directed by Professor Stokes. In this way I obtained two liquids, one intensely green, the other deep yellow with only a tinge of green. The two liquids were found to contain substances essentially different so far as regards their products of decomposition with acids. The yellow liquid having been mixed with dilute sulphuric acid was evaporated in the waterbath, water being added during evaporation, until the liquid had lost nearly all its colour. A quantity of yellow fatty matter separated during evaporation, and this having been filtered off the liquid was found to contain an abundance of glucose. The yellow fatty matter insoluble in water, dissolved easily in alcohol, but the yellow solutio showed none of the characteristic absorption bands of “acid chloro phyll.” The dark green liquid, treated in exactly the same way yielded a dark green product insoluble in water. The filtrate Iron this gave a slight reaction with Fehling’s solution, but so trifling comparatively that I am inclined to attribute it to the presence o some substance not completely removed from the disulphide of carboi solution by washing with alcohol. The dark green product of tin action of acid insoluble in water was soluble, though with difficultyin boiling alcohol, the solution being dull green and showing the absorption bands due to “acid chlorophyll.” If, therefore, chloro phyll be defined as the constituent of the green parts of plants, which gives a spectrum showing the well-known bands at the red end, and yields by decomposition with acids the product or products going by the name of “acid chlorophyll,” of which Fremy’s phyllocyanin is the most important and most characteristic, then chlorophyll is not a glucoside. The glucoside which accompanies it and resembles it as regards solubility in various menstrua may have to be sought among the group of bodies to which the generic name of xanthophyll has been applied.


2021 ◽  
Vol 43 (3) ◽  
pp. 198-203
Author(s):  
S.M. KUZMENKO ◽  
◽  
E.O. SPORYAGIN ◽  
O.M. KUZMENKO ◽  
A.YA. PUZENKO ◽  
...  

The paper describes the synthesis, the reaction of a mixture of isomers (2,4–2,6) of toluilendiisocyanate with a double molar excess of aliphatic individual or oligomeric diols, a number of previously unknown oligodiuretanediols and their physicochemical constants. It is shown that with an increase in the synthesis temperature from 50 to 70 °C, the reaction time to complete depletion in the mixture of free NCO-groups decreases from 8–9 hours to 3–4 hours. The reaction temperature of 70–2 °С should be considered optimal, because at higher temperatures side reactions of free NCO-groups with already formed urethane ones are possible. Because the presence of even a small amount of moisture in the diols can provoke side effects during the urethane formation reaction, all of the above diols were dried from the adsorbed moisture by azeotropic distillation with toluene before use in the reaction. Since the final products are even at the synthesis temperature (68–70 °C) viscous liquids, and there are difficulties with the homogenization of the reaction mass during synthesis, and when unloading the finished product from the reaction plant, in all cases, the synthesis was performed in solution cyclohexanone by 50 % by weight of the final product. Control of the reaction was performed by changing the % wt. free NCO-groups in time. The reaction was considered complete if the measured % wt. free NCO-groups in the reaction mixture for at least one hour twice showed zero. The isolated oligodiuretanediols range from solid at room temperature to very viscous products, which significantly depends on the molecular weight of the diol used in the reaction (ie the concentration of urethane groups formed). They are homogeneous, transparent compounds that are readily soluble in esters, ethers, aromatic and halide-containing, aprotic solvents, ketones, poorly or completely insoluble in aliphatic saturated hydrocarbons. The structure of the synthesized oligomeric products is confirmed by functional analysis, IR–spectra. In the IR-spectra of each of the synthesized oligodiuretanediols there are no absorption bands in the region of 2270 cm-1, which confirms the complete completion of the reaction of urethane formation according to the scheme. At the same time, the absorption bands in the region of 3450 cm-1, 1720 cm-1, 1540 cm-1 are fixed, which are characteristic of the presence of urethane groups in the structure of the target products. As the chain length of the diol component –R– increases in the target product (which synchronously leads to an increase in molecular weight), the intensity of these absorption bands decreases, which is associated with a decrease in the concentration of formed urethane groups in the structure of oligodiuretanediols. The refractive index also decreases synchronously. Synthesized series of oligodiuretanediols can be used for synthesis on its basis of other classes of oligomers with the simultaneous presence in the structure of urethane groups. The ability of such compounds to be soluble in solvents of different nature has been studied, which provides information for the directions of their further use (varnishes, enamels, primers).


2005 ◽  
Vol 8 (1) ◽  
Author(s):  
Masanori Shinohara ◽  
Teruaki Katagiri ◽  
Keitaro Iwatsuji ◽  
Yoshinobu Matsuda ◽  
Yasuo Kimura ◽  
...  

AbstractPlasma oxidation processes of hydrogen-terminated Si(100), (110), and (111) surfaces are investigated by infrared absorption spectroscopy (IRAS) in multiple internal reflection (MIR) geometry. We measured IRAS spectra of hydrogen-terminated Si surfaces exposed to oxygen-plasma in the Si-H stretching vibration region. IRAS data demonstrated that oxygen-plasma affects two influences on the Si surfaces; one is that oxygen-plasma removes surface hydrogen to oxidize the Si surfaces. The other is that it forces the hydrogen into the subsurface regions where oxygen species cannot reach. The former effect does not depend on the crystal graphic orientations, but the latter depends on it. Therefore, in order to oxidize perfectly the H-terminated Si surfaces using oxygen-plasma, the sample surfaces need to be heated so that oxygen atoms can diffuse into the subsurface regions.


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