• 제목/요약/키워드: Room temperature solid-phase

검색결과 120건 처리시간 0.026초

타액 중 ${\Delta}^9$-Tetrahydrocannabinol 및 11-Nor-9-carboxy-${\Delta}^9$-Tetrahydrocannabinol의 분석법 확립 및 안정성 검토 (Development of Quantification Method and Stability of ${\Delta}^9$-Tetrahydrocannabinol and 11-Nor-9-carboxy-${\Delta}^9$-Tetrahydrocannabinol in Oral Fluid)

  • 최혜영;백승경;장문희;최화경;정희선
    • 약학회지
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    • 제54권4호
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    • pp.226-231
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    • 2010
  • Oral fluid has become increasingly popular as an alternative specimen in the field of driving under the influence of drugs (DUID) and work place drug testing. In this study, an analytical method for the detection and quantification of ${\Delta}^9$-tetrahydrocannabinol (THC) and its metabolite, 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH) in oral fluid by SPE and GC-MS was established and fully validated. The stability of THC and THC-COOH in oral fluid during storage was also determined by examining the THC and THC-COOH concentration changes depending on time and container materials. Oral fluid samples were kept over 21 days at room temperature, $-4^{\circ}C$ and $-20^{\circ}C$ in two different specimen collection tubes; glass and polypropylene tubes. Three replicates for each condition with different temperature and types of a container were analyzed at five different time points over 21 days. When oral fluid samples were stored in glass tubes, the loss of both THC and THC-COOH was less than 10% at all room temperature, $-4^{\circ}C$ and $-20^{\circ}C$. However, in polypropylene tubes, the loss of both THC and THC-COOH increased significantly over the study period. In particular, the concentration of THC decreased more rapidly than that of THC-COOH at room temperature and the maximal percentage of THC lost was 90.3% after 21 days. The result indicates that it would be necessary to collect oral fluid samples in glass containers and cool the samples until analysis in order to prevent the degradation of analytes.

쑥 추출물 함유 음료와 미세캡슐의 제조 및 저장 중 휘발성분 변화 (Volatile Changes in Beverages and Encapsulated Powders Containing an Artemisia Extract during Production and Storage)

  • 박민희;김미자;조완일;장판식;이재환
    • 한국식품과학회지
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    • 제43권3호
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    • pp.271-276
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    • 2011
  • 저장온도 및 기간에 따른 참쑥(Artemisia princeps Pampan) 추출물을 함유한 음료 및 미세캡슐의 휘발성 성분변화를 SPMEGC/MS로 분석하였다. 쑥 추출물을 0.32, 0.64% 함유한 음료 S1, S2는 상온에서 8주간, $60^{\circ}C$에서 8일간 저장하고 쑥 추출물 함유미세캡슐은 상온과 $60^{\circ}C$에서 각각 8일간 저장하였으며 휘발성성분을 측정하였다. 저장 기간이 증가할수록 쑥 추출물 함유 음료의 총 휘발성 성분 함량은 유의적으로 감소하였다(p<0.05). Cymene, thujone, ${\beta}$-myrcene 등을 포함한 terpenoid류는 쑥 추출 물 함유 음료의 주요 휘발성 성분으로 동정되었으며, $60^{\circ}C$에서 저장한 쑥 추출물 함유 음료에서는 추가적으로 ethylfuran, vinylfuran, 2-fufural의 furan류 성분이 증가하였다. 쑥 추출물 함유 미세캡슐을 8일간 저장한 후, 총 휘발성 성분함량을 측정한 결과 상온에서 저장한 경우는 유의적인 변화가 없었으나 $60^{\circ}C$에서 저장한 경우는 유의적으로 16.5배 증가하였다(p<0.05). 쑥 추출물 함유 미세캡슐의 주요 휘발성 성분으로는 limonene이 가장 높았으며, $60^{\circ}C$에서 저장한 쑥 추출물 함유 미세캡슐에서만 유지산화에 의한 hexanal, pentanal, octanal, heptanal, nonanal 등의 aldehyde류와 2-butylfuran, 2-pentylfuran과 같은 furan류가 추가로 검출되었다. 이는 미세캡슐제조 시 사용된 피복물질의 산화에서 유래한 된 것으로 예측된다.

상안정화된 Leucite의 미세분말 합성과 열적 팽창 특성 연구 (Fabrication of Stabilized Fine Leucite Powder and Its Thermal Expansion Properties)

  • 홍성진;김득중;유영성
    • 한국세라믹학회지
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    • 제46권5호
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    • pp.493-496
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    • 2009
  • Phase stabilized leucite, which has high coefficient of thermal expansion, was synthesized, and its thermal expansion behavior was investigated. The homogeneous leucite phase was synthesized by solid state reaction from the mixture of $K_2CO_3-Al_2O_3-SiO_2$. and its stabilization from tetragonal to cubic phase was attempted by adding $Cs_2CO_3$ into starting materials. And fine powder with an average particle size of a few hundreds ${\mu}m$ were fabricated by planetary milling. During milling, amorphization of leucite was observed and recrystallized after heat treatment. The thermal expansion behavior of tetragonal and cubic leucite has measured and discussed. The average coefficient of thermal expansion of tetragonal and cubic phase leucite from room temperature to $750^{\circ}C$ was $21.4{\times}10^{-6}/^{\circ}C$ and $14.5{\times}10^{-6}/^{\circ}C$, respectively.

게터용 Zr57V36Fe7 합금의 수소 흡수특성에 미치는 비정질화의 영향 (The Effects of Amorphization on Hydrogen Absorption Properties of Zr57V36Fe7 Getter alloy)

  • 박제신;서창열;김원백
    • 한국재료학회지
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    • 제15권12호
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    • pp.802-808
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    • 2005
  • The hydrogen sorption speeds of $Zr_{57}V_{36}Fe_7$ amorphous alloy and its crystallized alloys were evaluated at room temperature $Zr_{57}V_{36}Fe_7$ amorphous alloy was prepared by ball milling. The amorphous alloy was crystallized through two stages. Initially, $\alpha-Zr$ solid solution was appeared from the amorphous phase. Two cubic Laves compounds were precipitated afterwards from the remained amorphous and from excessively saturated solid solution at higher temperature. The hydrogen sorption speed of the partially crystallized alloy was higher than that of amorphous. The enhanced sorption speed of partially crystallized alloy was explained in terms of surface oxygen stability which has been known to retard the activation of amorphous alloys. The retardation could be reduce by crystallization process resulting in the observed increase in sorption property.

솔-젤법에 의한 $Li_2O-ZrO_2-P_2O_5-SiO_2$계 유리 고체전해질의 제조와 그의 이온전도성 (Preparation of $Li_2O-ZrO_2-P_2O_5-SiO_2$ based Glassy Solid Electrolytes by Sol-Gel Process and Their Ionic Conduction)

  • 박강석;김기원;강은태
    • 한국세라믹학회지
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    • 제31권6호
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    • pp.660-670
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    • 1994
  • Transparent, crack-free dried gel monoliths with a composition of LiZr1.5Si2P2O12.5 have been synthesized by the low temperature polymerization of the Sol-Gel technique using metal alkoxides as starting materials. After initial reaction (20~40 min), each metal alkoxide closely paralleled each other during the hydrolysis reactions. The safe drying conditions of gels with no creaks the control of the shrinkage rate. The gels converted into the glass by heat treatment at 75$0^{\circ}C$. FTIR data indicated that the gels were phase separated into silicarich and phosphate-rich regions with the lithium. XRD results showed the formation of crystalline LiH2PO4. The gels dried at 15$0^{\circ}C$ or fired at 75$0^{\circ}C$ contained the residual water. The high ionic conductivity at room temperature for these gels was attributed to the motion of protons.

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중·저온 영역 SOFC용 고체 전해질로의 응용을 위한 Bi가 첨가된 아파타이트형 란타늄 실리케이트의 전기적 특성 (Electrical Properties of Bi-doped Apatite-type Lanthanum Silicates Materials for SOFCs)

  • 김대영;정광호;이성갑
    • 한국전기전자재료학회논문지
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    • 제25권6호
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    • pp.486-490
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    • 2012
  • $La_{7.33}Bi_2(SiO_4)_6O_2$ specimens were fabricated by standard solid-state synthesis route for solid oxide electrolytes. The calcined powders exhibited uniform particles with a mean particle size of about $28{\mu}m$. The room-temperature structure of $La_{7.33}Bi_2(SiO_4)_6O_2$ specimens was analyzed as hexagonal, space group P63 or P63/m, and the unit cell volume increased with increase a sintering temperature. The specimens sintered at $1,175^{\circ}C$ showed X-ray patterns of homogeneous apatite single phase without the second phase such as $La_2Si_2O_7$ and $La_2SiO_5$. The specimen sintered at $1,175^{\circ}C$ showed the maximum sintered density of 5.49 $g/cm^3$. Increasing the sintering temperature, total conductivities increased, activation energy decreased and the values were $1.98{\times}10^{-5}Scm-1$ and 1.23 eV, respectively.

$WS_2$ 고체윤활제의 마찰.마모 거동 (Tribological Behaviour of $WS_2$Solid Lubricant)

  • 신동우;김인섭;윤대현;김경도;김성진;정진수
    • Tribology and Lubricants
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    • 제14권2호
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    • pp.35-41
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    • 1998
  • The $WS_2$ solid lubricant synthesized through the vapour phase transport method was coated on the commercial bearing steel (SUJ 2) substrate, and the tribological behaviour of the lubricant was investigated using a ball-on-disk type tester. The $WS_2$ powder was spray-coated at room temperature using compressed air, and the change of friction coefficient was examined in various conditions, i.e., specimen configuration, atmosphere (air and nitrogen), applied load and rotating speed. $WS_2$ coated ball and disk showed the optimum friction coefficient of 0.07 and wear life of 45,000 cycles in the nitrogen atmosphere under 0.3 kgf and 100 rpm, whereas relatively high coefficient of 0.13 and reduced wear life of 4,000 cycles were observed in air atmosphere. The effect of rotating speed on the friction coefficient was not observed both in nitrogen and in air atmospheres. This confirmed that the spray-coated $WS_2$ solid lubricant was effective in reducing the friction coefficient and improving wear life in nitrogen atmosphere, and the oxygen and moisture existing in air could seriously deteriorate the lubrication effect of $WS_2$ coating layer.

초음파 분무 열분해법을 이용한 고체전해질용 Lithium Lanthanum Titanium Oxide 제조 (The Synthesis of Lithium Lanthanum Titanium Oxide for Solid Electrolyte via Ultrasonic Spray Pyrolysis)

  • 노재석;양민호;이근재
    • 한국분말재료학회지
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    • 제29권6호
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    • pp.485-491
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    • 2022
  • Lithium lanthanum titanium oxide (LLTO) is a promising ceramic electrolyte because of its high ionic conductivity at room temperature, low electrical conductivity, and outstanding physical properties. Several routes for the synthesis of bulk LLTO are known, in particular, solid-state synthesis and sol-gel method. However, the extremely low ionic conductivity of LLTO at grain boundaries is one of the major problems for practical applications. To diminish the grain boundary effect, the structure of LLTO is tuned to nanoscale morphology with structures of different dimensionalities (0D spheres, and 1D tubes and wires); this strategy has great potential to enhance the ion conduction by intensifying Li diffusion and minimizing the grain boundary resistance. Therefore, in this work, 0D spherical LLTO is synthesized using ultrasonic spray pyrolysis (USP). The USP method primarily yields spherical particles from the droplets generated by ultrasonic waves passed through several heating zones. LLTO is synthesized using USP, and the effects of each precursor and their mechanisms as well as synthesis parameters are analyzed and discussed to optimize the synthesis. The phase structure of the obtained materials is analyzed using X-ray diffraction, and their morphology and particle size are analyzed using field-emission scanning electron microscopy.

광열변위의 최소위상을 이용한 열확산계열수 측정 (Measurement of Thermal Diffusivity Using Minimum Phase Based on the Photothermal Displacement)

  • 이은호;이광재;전필수;유재석;김기현
    • 대한기계학회논문집B
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    • 제25권3호
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    • pp.296-304
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    • 2001
  • A new method of measuring the thermal diffusivity of solid material at room temperature using photothermal displacement is proposed. The influence of the parameters, such as radius and modulation frequency of the pump beam and the sample thickness, was studied. From the minimum position of phase of measured deflection with respect to the pump beam, the thermal diffusivity of the materials can be obtained. The position where phase has the minimum value is determined using multiparameter least-square regression fitting. The experimental values for different samples obtained by applying the new method are in good agreement with the literature values.

EPR SPECTRA OF Mn ION WITH TWO PHASES IN THE Y-Ba-Cu-Mn-O HIGH Tc SUPERCONDUCTOR

  • Kim, Seon-Ok;Rudowicz, Czeslaw;Lee, Soo-Hyung;Yu, Seong-Cho
    • 한국자기학회지
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    • 제5권5호
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    • pp.782-785
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    • 1995
  • In this paper, $Mn^{2+}$ ion was doped in Y-Ba-Cu-O as an EPR probe. The following samples were prepared by conventional solid-state reaction method : $YBa_{2}Cu_{2.96}Mn_{0.04}O_{7-\delta}$ (MN-I), annealed $YBa_{2}Cu_{2.96}Mn_{0.04}O_{7-\delta}$ (AMN) and $YBa_{2}Cu_{2.94}Mn_{0.06}O_{7-\delta}$ (MN-II). AMN sample was obtained from MN-I by annealing for 1 hr under the Ar gas atmosphere at $600^{\circ}C$. X-band (~9.05 GHz) EPR spectra were measured from 103 K to room temperature by employing a JES-RE3X spectroscopy with a $TE_{0.11}$ cylindrical cavity and 100 kHz modulation frequency. In MN-I we have observed only the $Cu^{2+}$ signal. The fact that no $Mn^{2+}$ signal was observed, in spite of $Mn^{2+}$ being a very sensitive EPR probe, indicates that most likely isolated $Mn^{2+}$ ions don't exist in the MN-I sample. Most probably $Mn^{2+}$ ions in the MN-I sample interact antiferromagnetically and hence are EPR silent. The AMN spectra of at room temperature and 103 K indicate not only the $Cu^{2+}$ signal but also an extra signal, which increases with decreasing temperature. It is suggested that the extra signal originates from Mn ions that were antiferromagnetically coupled before the annealing process. In MN-II, from 103 K to room temperature, also, the extra signal was observed together with the $Cu^{2+}$ signal. The extra signal in MN-II, however, decreases with decreasing temperature and nearly disappears at 103 K. The signal originates from Mn ions in impurity phases that include $Mn^{2+}$ ions. We suppose that there exist at least two $Mn^{2+}$ doped phases in Y-Ba-Cu-O. The $Mn^{2+}$ signal of one phase is undectable at all temperature and that of another phase decreases with decreasing temperature and disappears around 103 K.

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