• Title/Summary/Keyword: elemental analysis

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Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part III); Synthesis and Characterization of Cr(III)-Isothiocyanato, -Azido and -Chloroacetato Macrocyclic Complexes

  • Byun, Jong-Chul;Han, Chung-Hun;Park, Yu-Chul
    • Bulletin of the Korean Chemical Society
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    • v.26 no.7
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    • pp.1044-1050
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    • 2005
  • The reaction of cis-[Cr([14]-decane)($OH_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = isothiocyanate ($NCS^-$), azide ($N3^-$) or chloroacetate(caa)} leads to a new cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ (1), cis-[Cr([14]-decane)($N_3)_2]ClO_4$ (2) or cis-[Cr([14]-decane)($caa)_2]ClO_4$ (3). These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)($NCS)_2]ClO_4{\cdot}H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two $NCS^-$anions are bonded to the chromium(III) ion via the Ndonor atom in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by 13$^{\circ}$ from the ideal value of 180$^{\circ}$ for a perfect octahedron. The bond angle N-Cr-N between the Cr(III) ion and the two nitrogen atoms of the isothiocyanate ligands is close to 90$^{\circ}$. The bond lengths of Cr-N between the chromium and $NCS^-$groups are 1.964(5) and 2.000(5) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 2073, 1344 and 1684 $cm^{-1}$ attributed to the $NCS^-$, ${N_3}^-$ and caa groups stretching vibrations, respectively.

Template Synthesis and Characterization of Host (Nanocavity of Zeolite Y)-Guest ([Cu([18]aneN4S2)]2+, [Cu([20]aneN4S2)]2+, [Cu(Bzo2[18]aneN4S2)]2+, [Cu(Bzo2[20]aneN4S2)]2+) Nanocomposite Materials

  • Salavati-Niasari, Masoud;Mirsattari, Seyed Nezamodin;Saberyan, Kamal
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.348-354
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    • 2009
  • Copper(II) complexes with tetraoxo dithia tetraaza macrocyclic ligands; [18]ane$N_4S_2$: 1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, [20]ane$N_4S_2$: 1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane,Bzo2[18]ane$N_4S_2$: dibenzo-1,4,10,13-tetraaza-5,9,14,18-tetraoxo-7,16-dithia-cyclooctadecane, Bzo2[20]ane$N_4S_2$: dibenzo-1,5,11,15-tetraaza-6,10,16,20-tetraoxo-8,18-dithia-cyclocosane; were entrapped in the nanopores of zeolite-Y by a two-step process in the liquid phase: (i) adsorption of [bis(diamine)copper(II)] (diamine = 1,2-diaminoethane, 1,3-diaminopropane, 1,2-diaminobenzene, 1,3-diaminobenzene); $[Cu(N-N)_2]^{2+}$-NaY; in the nanopores of the zeolite, and (ii) in situ template condensation of the copper(II) precursor complex with thiodiglycolic acid. The obtained complexes and new host-guest nanocomposite materials; $[Cu([18]aneN_4S_2)]^{2+}-NaY,\;[Cu([20]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[18]aneN_4S_2)]^{2+}-NaY,\;[Cu(Bzo_2[20]aneN_4S_2)]^{2+}$-NaY; have been characterized by elemental analysis FT-IR, DRS and UV-Vis spectroscopic techniques, molar conductance and magnetic moment data, XRD and, as well as nitrogen adsorption. Analysis of data indicates all of the complexes have been encapsulated within nanopore of zeolite Y without affecting the zeolite framework structure.

Synthesis of New Spiro[benzo[c]fluorene-7,9'-fluorene] Dimers and Their Optical Properties

  • Seo, Jeong-A;Lee, Chil-Won;Gong, Myoung-Seon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1414-1420
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    • 2013
  • Five novel spiro[benzo[c]fluorene-7,9'-fluorene] based dyes, including 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-5-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (7), 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-9-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (8), 5-[spiro[benzo[c]fluorene-7,9'-fluoren]-2'-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (9), 9-[spiro[benzo[c]fluorene-7,9'-fluoren]-9-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (10), and 2'-[spiro[benzo[c]-fluorene-7,9'-fluoren]-2'-yl] spiro[benzo[c]fluorene-7,9'-fluorene] (11) were successfully prepared from the corresponding halogen and boronic acid derivatives through the Suzuki coupling reaction, respectively. Chemical structures were confirmed by $^1H$ nuclear magnetic resonance (NMR), $^{13}C$ NMR, Fourier transforminfrared spectrscopy, mass spectroscopy, and elemental analysis. The thermal properties were determined by differential scanning calorimetry and thermal gravimetric analysis. The relationships between the optical and electrochemical properties and the combined positions between these dimers were systematically investigated using UV-vis, photoluminescence (PL), and photoelectron spectroscopy. These five dimers exhibited high fluorescent quantum yields and good morphological stability with high glass transition states > $174^{\circ}C$. Dimer 7 showed a UV absorbance peak at 353 nm, emission PL peak at 424 nm, and quantum efficiency of 0.62 in a cyclohexane solution.

The Structure of Phenolic Compounds and Their Antibiotic Activities in Umbilicaria vellea (Umbilicaria vellea 중 페놀성 화합물의 구조 및 항균활성)

  • Min, Tae Jin;Bae, Kang Gyu
    • Journal of the Korean Chemical Society
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    • v.40 no.9
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    • pp.623-629
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    • 1996
  • In order to identify antibiotic substances in the extract of a lichen, Umbilicaria vellea, the extract was chromatographed and two compounds were isolated. Compound I which showed antifungal and antibacterial activities, melted around 129∼132$^{\circ}C$ and showed UV absorption at 217, 265 and 300 nm. It showed a molecular ion at m/z 196. Its molecular formular was confirmed to be $C_{10}H_{12}O_4$ from elemental analysis. From its IR and NMR data it was identified to be ethyl 2,4-dihydroxy-6-methyl benzoate. Compound II melted around 58∼59$^{\circ}C$ and showed UV absorption at 212, 276 and 282 nm. It showed a molecular ion at m/z 124 and molecular formular was confirmed to be $C_7H_8O_2.$ From the analysis of its IR and NMR spectra it was identified to be 5-methyl-1,3-benzenediol.

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Synthesis, Structural Characterization and Thermal Behaviour of Block Copolymers of Aminopropyl-Terminated Polydimethylsiloxane and Polyamide Having Trichlorogermyl Pendant Group (Aminopropyl-Terminated Polydimethylsiloxane과 Trichlorogermyl 곁가지 그룹을 갖는 Polyamide 블록공중합체의 합성, 구조분석 및 열적거동)

  • Gill, Rohama;Mazhar, M.;Mahboob, Sumera;Siddiq, Muhammad
    • Polymer(Korea)
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    • v.32 no.3
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    • pp.239-245
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    • 2008
  • Block copolymers of the general formula $[(-CO-R'-CO-HN-Ar-NH-CO-R'-CO)_xNH(CH_2)_3-(Me_2SiO)_y(CH_2)_3NH_2]_n$, [n=18.00 to 1175.0] where $R'=CH_2CH(CH_2GeCl_3)$;$CH_2CHGeCl_3CH_2$; and $Ar=-C_6H_4$;$-(o.CH_3C_6H_4)_2$;$-o.CH_3OC_6H_4)_2$;$-(o.CH_3C_6H_4)$ were prepared by a polycondensation reaction of polyamide containing a pendant trichlorogermyl group and terminal acid chloride $Cl(-CO-R'-CO-NH-Ar-NH-CO-R'-CO-)_xCl$ with aminopropyl-terminated polydimethylsiloxane $H_2N(CH_2)_3(Me_2SiO)_y-(CH_2)_3NH_2]$, (PDMS). These polymers were characterized by elemental analysis, $T_g$, FT-IR, $^1H$-NMR, solid state $^{13}C$-NMR, and molecular weight determination. The thermal stability of these copolymers was examined using thermal analysis techniques, such as TGA and DSC. Their molecular weights as determined by laser light scattering technique ranged $5.13{\times}10^5$ to $331{\times}10^5\;g/mol$. These polymers display their $T_g$ in the range of 337 to $393^{\circ}C$ with an average decomposition temperature at $582^{\circ}C$.

Evaluation for Contents of Contaminants and Leaching Characteristics of Bottom Ash (바텀애쉬의 유해물질 함량 측정 및 용출특성 평가연구)

  • Koh, Taehoon;Lee, Sungjin;Shin, Minho;Kim, Byongsuk;Lee, Jeakeun;Lee, Taeyoon
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.6
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    • pp.77-83
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    • 2010
  • In this study, we tried to determine any detrimental effects on water quality when bottom ash obtained from a coal-fired power plant intended to be used as a fill material in construction sites. Physical-chemical properties of bottom ash were determined using proximate analysis, elemental analysis, XRD, and XRF. Classification of bottom ash as a waste material and soil contamination due to the use of bottom ash were performed by Korea waste standard leaching test and soil toxicity test, respectively. Results of leaching tests were compared to the regulations for water quality and groundwater quality and no harmful effects on water quality were found. Most of heavy metals in leachate were below detection limits but trace amount of $Cr^{6+}$ was found. However, concentration of $Cr^{6+}$ was below the regulation criteria. Column leaching tests indicated that concentrations of Pb and Zn were slightly higher than regulations but below regulations within 1 PVE, but concentrations of sulfate were 10 times higher than regulation and thus, the required time to reach regulation was almost 8 PVE.

White mineral trioxide aggregate mixed with calcium chloride dihydrate: chemical analysis and biological properties

  • Ahmed, Hany Mohamed Aly;Luddin, Norhayati;Kannan, Thirumulu Ponnuraj;Mokhtar, Khairani Idah;Ahmad, Azlina
    • Restorative Dentistry and Endodontics
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    • v.42 no.3
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    • pp.176-187
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    • 2017
  • Objectives: This study aimed to evaluate the chemical and biological properties of fast-set white mineral trioxide aggregate (FS WMTA), which was WMTA combined with calcium chloride dihydrate ($CaCl_2{\cdot}2H_2O$), compared to that of WMTA. Materials and Methods: Surface morphology, elemental, and phase analysis were examined using scanning electron microscope (SEM), energy dispersive X-ray microanalysis (EDX), and X-ray diffraction (XRD), respectively. The cytotoxicity and cell attachment properties were evaluated on human periodontal ligament fibroblasts (HPLFs) using methyl-thiazoldiphenyltetrazolium (MTT) assay and under SEM after 24 and 72 hours, respectively. Results: Results showed that the addition of $CaCl_2{\cdot}2H_2O$ to WMTA affected the surface morphology and chemical composition. Although FS WMTA exhibited a non-cytotoxic profile, the cell viability values of this combination were lesser than WMTA, and the difference was significant in 7 out of 10 concentrations at the 2 time intervals (p < 0.05). HPLFs adhered over the surface of WMTA and at the interface, after 24 hours of incubation. After 72 hours, there were increased numbers of HPLFs with prominent cytoplasmic processes. Similar findings were observed with FS WMTA, but the cells were not as confluent as with WMTA. Conclusions: The addition of $CaCl_2{\cdot}2H_2O$ to WMTA affected its chemical properties. The favorable biological profile of FS WMTA towards HPLFs may have a potential impact on its clinical application for repair of perforation defects.

Effect of Ca Ion on the SCR Reaction over VOx/TiO2 (Ca 이온이 VOx/TiO2 SCR 반응에 미치는 영향 연구)

  • Kim, Geo Jong;Hong, Sung Chang
    • Applied Chemistry for Engineering
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    • v.27 no.2
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    • pp.165-170
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    • 2016
  • In this study, we investigated the cause of the decrease in activities of $VO_x/TiO_2$ SCR catalyst used for the burner reactor at a scale of $150000Nm^3/hr$ using X-ray diffraction (XRD), brunauer-emmett-teller (BET), atomic emission spectroscopy inductively coupled plasma (AES ICP), $H_2$ temperature programmed reduction ($H_2$-TPR), and $NH_3$ temperature programmed desorption ($NH_3$-TPD) analysis. Since the crystallization of the $VO_x$ and phase transition of $TiO_2$ did not occur, it was concluded that the catalyst was not deactivated by the thermal effect. In addition, from the elemental analysis showing that a large quantity of calcium was detected but not sulfur, the deactivation process of the $VO_x/TiO_2$ SCR catalyst was mainly caused by Ca but not by $SO_2$. The calcium was also found to decrease the catalytic activity by means of reducing $NH_3$ adsorption.

Qualitative Analysis and Plasma Characteristics of Soil from a Desert Area using LIBS Technique

  • Farooq, W. Aslam;Tawfik, Walid;Al-Mutairi, Fahad N.;Alahmed, Zeyad A.
    • Journal of the Optical Society of Korea
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    • v.17 no.6
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    • pp.548-558
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    • 2013
  • In this work, laser induced breakdown spectroscopy (LIBS) is used to investigate soil samples collected from different desert areas of Riyadh city in Saudi Arabia. Both qualitative analysis and plasma parameters are studied via the observed LIBS spectra. These experiments have been done using a Spectrolaser-7000 system with 50 mJ fundamental wavelength of Nd:YAG laser and detection delay time of 1 microsecond. Many spectral lines are highly resolved for many elements like Al, Fe, Mg, Si, Mn, Na, Ca and K. The electron temperatures Te and electron densities Ne, for the constituent of generated LIBS plasma, are determined for all the collected samples. It is found that both Te and Ne vary from one desert area to other. This variation is due to the change of the elemental concentration in different desert areas that affects the sample's matrices. Time dependent measurements have also been performed on the soil samples. While the signal-to-base ratio (SBR) reached its optimal value at 1 microsecond, the plasma parameters Ne and Te reach values of $4{\times}10^{17}cm^{-3}$ and 9235 K, respectively, at 2.5 microsecond. The later indicate that the plasma cooling processes are slow in comparison to the previously observed results for metallic samples. The observed results show also that in the future it is possible to enhance the exploitation of LIBS in the remote on-line environmental monitoring application, by following up only the values of Ne and Te for one element of the soil desert sample using an optical fiber probe.

Kinetics, Isotherm and Adsorption Mechanism Studies of Letrozole Loaded Modified and Biosynthesized Silver Nanoparticles as a Drug Delivery System: Comparison of Nonlinear and Linear Analysis

  • PourShaban, Mahsa;Moniri, Elham;Safaeijavan, Raheleh;Panahi, Homayon Ahmad
    • Korean Chemical Engineering Research
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    • v.59 no.4
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    • pp.493-502
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    • 2021
  • We prepared and investigated a biosynthesized nanoparticulate system with high adsorption and release capacity of letrozole. Silver nanoparticles (AgNPs) were biosynthesized using olive leaf extract. Cysteine was capped AgNPs to increase the adsorption capacity and suitable interaction between nanoparticles and drug. Morphology and size of nanoparticles were confirmed using transmission electron microscopy (TEM). Nanoparticles were spherical with an average diameter of less than 100 nm. Cysteine capping was successfully confirmed by Fourier transform infrared resonance (FTIR) spectroscopy and elemental analysis (CHN). Also, the factors of letrozole adsorption were optimized and the linear and non-linear forms of isotherms and kinetics were studied. Confirmation of the adsorption data of letrozole by cysteine capped nanoparticles in the Langmuir isotherm model indicated the homogeneous binding site of modified nanoparticles surface. Furthermore, the adsorption rate was kinetically adjusted to the pseudo-second-order model, and a high adsorption rate was observed, indicating that cysteine coated nanoparticles are a promising adsorbent for letrozole delivery. Finally, the kinetic release profile of letrozole loaded modified nanoparticles in simulated gastric and intestinal buffers was studied. Nearly 40% of letrozole was released in simulated gastric fluid with pH 1.2, in 30 min and the rest of it (60%) was released in simulated intestinal fluid with pH 7.4 in 10 h. These results indicate the efficiency of the cysteine capped AgNPs for adsorption and release of drug letrozole for breast cancer therapy.