• Title/Summary/Keyword: Organic silica

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Dual Capillary Column System for the Qualitative Gas Chromatography: 2. Comparison between Splitless and On-Column Injection Modes

  • Kim, Kyoung-Rae;Kim, Jung-Han;Park, Hyoung-Kook;Oh, Chang-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.14 no.2
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    • pp.250-255
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    • 1993
  • A dual capillary column system is described for the simultaneous analysis of a given sample and measurement of retention index (RI) and area ratio (AR) values of each peak on two capillary columns of different polarity, DB-5 & DB-1701 from a single injection. Both capillary columns were connected to either a splitless injector or an on-column injector via a deactivated fused-silica capillary tubing of 1 m length and a 'Y' splitter. Both injection modes allowed to measure RI and AR values with high reproducibility (<0.01% RSD) and high accuracy (<10% RE), respectively with the exception that the trace and high boiling solutes required the on-column mode for the accurate quantification and AR comparison. When the dual capillary column system in on-column injection mode was applied to the blind samples containing organic acids, each acid was positively indentified by the combined computer RI library search-AR comparison.

Problem-solving approach for salbutamol analysis by HPLC during pharmaceutical assay

  • Gholizadeh-Hashjin, Aiesheh;Hamishehkar, Hamed;Monajjemzadeh, Farnaz
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.189-196
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    • 2022
  • When cationic basic compounds are chromatographed using hydro-organic mobile phase, the presence of anionic free silanols in the silica-based stationary phases results in broad and asymmetrical peaks. The addition of an ionic reagent to the mobile phase prevents analytes from accessing free silanols, improving peak shape. In this study, the chromatographic behavior of salbutamol sulfate as a basic compound was investigated under various conditions, including the use of different columns, mobile phases, and ion-pair reagents such as triethanolamine (TEA) and sodium heptane sulfonate (SHS). The retention and peak shape of chromatograms were both evaluated. The results show that pre-conditioning the column with TEA and including it in the mobile phase can prevent cationic analytes from accessing anionic silanols, resulting in improved peak shape. Furthermore, buffering the mobile phase is an important factor in keeping the pH constant throughout the process. The chosen method was validated in part. This study could be helpful for researchers and analyst to solve such problems with cationic basic components.

The Application of NIRS for Soil Analysis on Organic Matter Fractions, Ash and Mechanical Texture

  • Hsu, Hua;Tsai, Chii-Guary;Recinos-Diaz, Guillermo;Brown, John
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1263-1263
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    • 2001
  • The amounts of organic matter present in soil and the rate of soil organic matter (SOM) turnover are influenced by agricultural management practice, such as rotation, tillage, forage plow down direct seeding and manure application. The amount of nutrients released from SOM is highly dependent upon the state of the organic matter. If it contains a large proportion of light fractions (low-density) more nutrients will be available to the glowing crops. However, if it contains mostly heavy fractions (high-density) that are difficult to breakdown, then lesser amounts of nutrients will be available. The state of the SOM and subsequent release of nutrients into the soil can be predicted by NIRS as long as a robust regression equation is developed. The NIRS method is known for its rapidity, convenience, simplicity, accuracy and ability to analyze many constituents at the same time. Our hypothesis is that the NIRS technique allows researchers to investigate fully and in more detail each field for the status of SOM, available moisture and other soil properties in Alberta soils for precision farming in the near future. One hundred thirty one (131) Alberta soils with various levels (low 2-6%, medium 6-10%, and high >10%) of organic matter content and most of dry land soils, including some irrigated soils from Southern Alberta, under various management practices were collected throughout Northern, Central and Southern Alberta. Two depths (0- 15 cm and 15-30 cm) of soils from Northern Alberta were also collected. These air-dried soil samples were ground through 2 mm sieve and scanned using Foss NIR System 6500 with transport module and natural product cell. With particle size above 150 microns only, the “Ludox” method (Meijboom, Hassink and van Noorwijk, Soil Biol. Biochem.27: 1109-1111, 1995) which uses stable silica, was used to fractionate SOM into light, medium and heavy fractions with densities of <1.13, 1.13-1.37 and >1.37 respectively, The SOM fraction with the particle size below 150 microns was discarded because practically, this fraction with very fine particles can't be further separated by wet sieving based on density. Total organic matter content, mechanical texture, ash after 375$^{\circ}C$, and dry matter (DM) were also determined by “standard” soil analysis methods. The NIRS regression equations were developed using Infra-Soft-International (ISI) software, version 3.11.

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Study on Characteristics and Preparation of Binderless ZSM-5 Granules for Adsorption of Xylene Isomers (Binderless ZSM-5 성형체의 합성 및 자일렌 이성체의 흡착 특성에 관한 연구)

  • Yun, Hyo-Sang;Hong, Ji-Sook;Suh, Jeong-Kwon;Shin, Chae-Ho
    • Applied Chemistry for Engineering
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    • v.21 no.4
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    • pp.417-423
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    • 2010
  • In this study, an effective method to prepare granular binderless ZSM-5 which is as efficient p-xylene separatory adsorbent was explored. Colloidal silica sol 30 wt% solution as an inorganic binder and microcrystalline cellulose as an organic additive were added to ZSM-5 powder ($SiO_2/Al_2O_3$ = 50). Adsorbent with enough strength (0.721 kgf), high crystallinity (94.6%) and high BET specific surface area ($379.2m^2$/g) was obtained by calcination, binderless treatment, ${NH_4}^+$ ion exchange, and activation after spherical granulation process. A batch type adsorption experiment was proceeded with solutions comprising 3 xylene isomers by 1 : 1 : 1 weight ratio to evaluate adsorption characteristics of prepared absorbent. As a result, the obtained binderless ZSM-5 granule showed a higher selective adsorption performance for para-xylene than that of commercial adsorbent.

Performance Evaluation of a Fiber-Optic Cerenkov Radiation Sensor System Using a Simulated Spent Fuel Assembly (사용후핵연료 집합체 모사장치를 이용한 광섬유 체렌코프 방사선 센서 시스템의 성능평가)

  • Shin, Sang Hun;Yoo, Wook Jae;Jang, Kyoung Won;Cho, Seunghyun;Park, Byung Gi;Lee, Bongsoo
    • Journal of Sensor Science and Technology
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    • v.23 no.4
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    • pp.245-250
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    • 2014
  • When the charged particle travels in transparent medium with a velocity greater than that of light in the same medium, the electromagnetic field close to the particle polarizes the medium along its path, and then the electrons in the atoms follow the waveform of the pulse which is called as Cerenkov light or radiation. This type of radiation can be easily observed in a spent fuel storage pit. In optical fibers, the Cerenkov light also can be generated due to their dielectric components. Accordingly, the radiation-induced light signals can be obtained using optical fibers without any scintillating material. In this study, to measure the intensities of Cerenkov radiation induced by gamma-rays, we have fabricated the fiber-optic Cerenkov radiation sensor system using silica optical fibers, plastic optical fibers, multi-anode photomultiplier tubes, simulated spent fuel assembly and a scanning system. To characterize the Cerenkov radiation generated in optical fibers, the intensities of Cerenkov radiation generated in the silica and plastic optical fibers were measured. Also, we measured the longitudinal distribution of gamma rays emitted from the Ir-192 isotope by using the fiber-optic Cerenkov radiation sensor system and simulated spent fuel assembly.

Structure and Isolation of Antioxidative Substance Derived from Phaeodactylum tricornutum (Phaeodactylum tricornutum으로부터 항산화성 물질의 분리 및 구조)

  • KIM Se-Kwon;BYUN Hee-Guk;BAEK Ho-Chul;PARK Pyo-Jam;KANG Ok-Ju;KIM Jong-Bae
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.34 no.5
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    • pp.556-562
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    • 2001
  • The antioxidative activity of marine microalgae, Phaeodactylum tricornutum (P. tricornutum) of Bacillariophyceae, was determined by measuring radical scavenging effect on 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical. The chloroform fraction of P. tricornutum showed strong antioxidative activity, The potential antioxidative activity of factions extracted with mixture solution of organic solvents was detected in dichloromethane : methanol (2 : 1) fraction, This fraction was further purified by preparative thin layer chromatography (PTLC) and repeated reverse-phase HPLC. On the basis of chemical and spectoscopic evidence from results obtained by UV, FT-IR, EIMS and NMR, the compound purified from P. tricornutum was identified as zeaxanthin.

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Analytical Determination of Alkylphenols, Chlorophenols and Bisphenol A in Biota Samples using Gas Chromatography/Mass Spectrometry (기체 크로마토그래피/질량분석기를 이용한 생물시료 중 알킬 페놀류, 클로로페놀류 및 비스페놀 A의 분석법)

  • Hong, Jongki;Kim, Hyup;Baek, In-Girl;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Chung, Bong-Chul;Pyo, Hee-Soo;Kim, Kyung-Rae;Kim, Yong-Hwa
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.484-493
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    • 2000
  • The simultaneous analysis of alkylphenols, chlorophenols and bisphenol A in biota samples was performed by gas chromatography-mass spectrometry-selected ion monitoring mode. The phenols were extracted from sample with organic solvent and Forisil and Silica columns for clean-up procedure were compared. Recovery studies were performed at 1-ppm level of phenols added to each biota sample. Their recoveries ranged between 83 and 116% with coefficient of variations of 2.4-11.9%. To improve the detection limits of phenols, trimethylsilyl (TMS) derivatization was applied. The gas chromatographic properties of free phenols and TMS derivatized phenols were also investigated.

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Purification and Structure of Antioxidative Substance Derived from Tetraselmis suecica (Tetraselmis suecica유래의 항산화성 물질의 정제 및 구조)

  • Kim Se Kwon;Byun Hee Guk;Park Pyo Jam;Adachi Kyoko
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.35 no.2
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    • pp.155-161
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    • 2002
  • Tetraselmis suecica (T. suecica) of Prasinophyta was selected because the growth rate is comparatively higher and the culturing is also easy. In order to investigate antioxidative activity, the soluble elements of T. suecica were fractionated using water and organic solvents such as methanol, hexane, chloroform, ethylacetate and butanol. The chloroform fraction of T. suecica showed strong antioxidative activity. The potential antioxidative activity was detected in hexane: ethylacetate (1:5) once used the fractions by different mixtures of organic solvents. This fraction was further purified by preparative thin layer chromatography (PTLC) and repeated reverse-phase HPLC. On the basis of chemical and spectroscopic evidences obtained by UV, FT-IR, FAB-MS and NMR, the compound purified from T. suecica was identified as pheophorbide-a. The antioxidative activity of the compound was comparable to that of $\alpha$-tocopherol and could be act as an antioxidant in foods.

Aphicidal Activity of Different Fraction Extracts of Culture Filtrate of Beauveria bassiana Isolate against Aphids (Beauveria bassiana 배양여액 분획추출물의 진딧물 살충활성)

  • Jeong, Ga-Young;Han, Ji-Hee;Kim, Jeong-Jun;Lee, Sang-Yeob
    • Korean Journal of Organic Agriculture
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    • v.25 no.1
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    • pp.113-124
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    • 2017
  • Cotton aphid (Aphis gossypii) and green peach aphid (Myzus persicae) are serious pests damaging various crops including vegetables such as pepper, cucumber, and Chinese cabbage. We conducted a study to control two aphids with secondary metabolite of entomopathogenic fungus Beauveria bassiana. A B. bassiana was already selected as a high virulence isolate against cotton aphid and green peach aphid. The culture filtrate of the isolate showed high pathogenicity against both aphids as 100% mortality against cotton aphid 3 days after treatment and 99% against green peach aphid 5 days after treatment. A different fraction extracts with $CHCl_3$ : MeOH of B. bassiana culture filtrate (30:1, 50:1, 70:1, 90:1, 100:1; v/v) through silica gel column chromatography showed different control effect to aphids. Among them, 50:1 ($CHCl_3$ : MeOH) fraction had highest mortality as 77.3% and 75.4% against A. gossypii and M. persicae, respectively. A mixture of each fraction (1:1) had no synergistic effects because control effect of every mixture was lower than only 50:1 extract; for example, mortality of 50:1 + 70:1 showed $2^{nd}$ highest as 72% of cotton aphid and 70.2% of green peach aphid and other mixtures were lower than these values. In future we will study the identification and mass production of aphicidal compound isolated from 50:1 fraction to develop stable aphid control agent.

Preparation of blocking ultraviolet mica composites using Nano-TiO2 (Nano-TiO2를 이용한 자외선차단 마이카 복합체 제조)

  • Yun, Ki Hoon;Lee, Jaebok;Moon, Young-Jin;Go, Hee Kyoung;Lee, Yi;Lee, Dong-Kyu
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.1197-1205
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    • 2018
  • UV protection cosmetics belong to functional cosmetics and contain organic or inorganic UV blocking pigments. The inorganic UV blocking pigments are mainly zinc oxide and titanium dioxide. It is known that inorganic UV blocking pigment has a diameter of 60 to 100 nm and has good blocking ability of UVA and UVB. Also, it has high inactivity against sunlight including UV and is excellent in safety. In addition, it is not absorbed or accumulated on the skin like organic pigments and does not cause skin irritation or allergy. In this study, mica, a plate-shaped inorganic pigment, nanosized titanium dioxide, an UV blocking material, and hydrophobic silica were surface-treated with surfactants. And then, titanium dioxide nanoparticles and silica were physically adsorbed on the mica by non-chemical mutual attraction due to differences in charge. Thereafter, the mica complex was surface-treated with silane to prepare a hydrophobic UV blocking pigment complex. The plate-shaped UV blocking composite improves the cohesiveness of a general nanoparticle material titanium dioxide, enhances UV blocking effect due to uniform dispersion, and can greatly improve dispersion stability in cosmetic formulations by surface treatment with hydrophobic property. The surface charge of the pigment was evaluated by zeta potential. The properties of the UV blocking pigment complex were evaluated by FE-SEM, XRD, FT-IR and UV-VIS.