• 제목/요약/키워드: Materials Metrology

검색결과 140건 처리시간 0.022초

회귀식 사용에 따른 화학 분석 과정의 불확도 처리 연구 (A Study on the Treatment of Uncertainty in Linear Regression Method for Chemical Analysis)

  • 우진춘;서정기;임명철;박민수
    • 분석과학
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    • 제16권3호
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    • pp.185-190
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    • 2003
  • 회귀식 사용에 따른 불확도 계산의 정확성을 조사하기 위하여, 수정된 방법의 최소제곱법(Modified Least Square Method, MLS)과 회귀식에서 일반적으로 적용되는 불확도 처리 과정을 각각 1차 식에 적용하고 비교하였다. 회귀식에서 일반적으로 적용되는 불확도 처리 과정에서, 대부분의 경우 불확도 값이 크게 계산되고 있어 확률적으로 안전한 범위를 표기할 수 있는 것으로 평가되었다. 그러나, 표준시료 농도의 상대 표준불확도가 클 때 (교정점이 우발적으로 흩어지는 정도의 표준 편차가 5% 수준, 표준시료 농도의 상대 표준불확도가 7% 수준) 회귀식에서 일반적으로 적용되는 불확도 계산 방법으로 얻은 값이 고 농도 측정에서 매우 작게 평가되고 있어 확률적으로 매우 위험한 것으로 평가되었다. 이 경우, 통계학적으로 불확도를 정확히 계산하기 위하여, 수정된 방법의 최소제곱법이 유리하다고 판단하였다.

A New Analytical Method to Determine the Purity of Synthetic Fluorophores using Single Molecule Detection Technique

  • Song, Nam-Yoong;Kim, Hyong-Ha;Park, Tae-Sook;Yoon, Min-Joong
    • Journal of Photoscience
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    • 제12권2호
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    • pp.87-93
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    • 2005
  • A new assay technique to distinguish between pure compounds and the isomeric mixtures has been suggested using single molecule (SM) fluorescence detection technique. Since the number of emission spots in a fluorophorespread film prepared from a genuine dye solution was determined by experimental condition, the deviation of spot numbers from the expected values could be considered to be an indication of lower purity of the sample solution. The lower limit of sample concentration for this assay was determined to be $5{\times}10^{-10}$ M to show uniform number of expected spots within 10% uncertainties in our experimental condition. An individual fluorescence intensity distribution for a mixture of isomers having doubly different emissivities was simulated by adding distributions obtained from Cy3 and nile red (NR) independently. The result indicated that the mixture could be identified from the pure compounds through the difference in the number of Gaussian functions to fit the distribution. This new assay technique can be applied to the purity test for synthetic biofluorophores which are usually prepared in small quantities not enough for classical ensemble assays.

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Evanohm R 합금 히터를 사용한 크로멜-콘스탄탄 다중접합 열전변환기의 제작 및 특성 (Fabrication and Characteristics of Chromel-Constantan Multijunction Thermal Converter with Evanohm R Alloy Heater)

  • 이영화;권성원;김국진;박세일;임영언
    • 센서학회지
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    • 제13권1호
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    • pp.35-40
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    • 2004
  • A thin-film multijunction thermal converter was fabricated through the process using 6 inch silicon wafer semiconductor process and bulk micromachining. Evanohm R alloy and chromel-constantan were used as a heater and thermocouple materials, respectively. The temperature coefficient of resistance of Evanohm R heater was about 75.12 ppm/$^{\circ}C$ and the voltage sensitivity of the thermal converter indicated about 5.75 mV/mW in air. The transfer differences, measured by FRDC-DC method in the frequency range from 20 Hz to 10 kHz, showed the value under about 1.36 ppm, 0.83 ppm for the film thickness of 500, 200 nm, respectively. And in case of a 200 nm-thick thermal converter, the AC-DC transfer differences seems to be stabilized below the value of 1 ppm in the frequency range from 1 kHz to 500 kHz.

High Resolution Transmission Electron Microscopy Observations on Sintering Processes in KNbO3 Ceramics

  • Lee, Hwack Joo;Kim, Young Heon;Ryu, Hyun;Cho, Yang-Koo;Nahm, Sahn
    • Applied Microscopy
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    • 제47권3호
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    • pp.203-207
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    • 2017
  • A homogeneous $KNbO_3$ (KN) phase was formed by sintering at $1,040^{\circ}C$ for 1 hour, without formation of the $K_2O$-deficient secondary phase even though suffering the minor loss of $K_2O$. KN liquid phase was formed during sintering and abnormal grain growth occurred in this specimen. The detailed microstructural observations on KN during sintering were carried out using high resolution transmission electron microscopy. The ledged structures were found at the KN grain boundary and the abnormal grain growth was performed by the lateral migration of these ledges in the presence of the liquid phase. The liquid pockets were found in the KN grains. They have various external shapes mainly due to the kinetic factors. They have atomically flat interfaces with some ledges with one atomic height. The slight deficient $K_2O$ by evaporation might somewhat reduce the melting point of KN from the reported at $1,058^{\circ}C$. The liquid pockets play an important role in supplying the liquid phase during the abnormal grain growth in the sintering process of KN ceramics.

실리콘 미세 가공을 이용한 열전형 미소유량센서 제작 및 특성 (Fabrication and characteristics of micro-machined thermoelectric flow sensor)

  • 이영화;노성철;나필선;김국진;이광철;최용문;박세일;임영언
    • 센서학회지
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    • 제14권1호
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    • pp.22-27
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    • 2005
  • A thermoelectric flow sensor for small quantity of gas flow rate was fabricated using silicon wafer semiconductor process and bulk micromachining technology. Evanohm R alloy heater and chromel-constantan thermocouples were used as a generation heat unit and sensing parts, respectively. The heater and thermocouples are thermally isolated on the $Si_{3}N_{4}/SiO_{2}/Si_{3}N_{4}$ laminated membrane. The characteristics of this sensor were observed in the flow rate range from 0.2 slm to 1.0 slm and the heater power from 0.72 mW to 5.63 mW. The results showed that the sensitivities $(({\partial}({\Delta}V)/{\partial}(\dot{q}));{\;}{\Delta}V$ : voltage difference, $\dot{q}$ : flow rate) were increased in accordance with heater power rise and decreasing of flow rate.

동위원소희석 질량분석법에 의한 저니토 중의 카드뮴, 구리, 납, 니켈, 아연의 정량 (Determination of Cadmium, Copper, Lead, Nickel, and Zinc in Sediments by ID-ICP/MS)

  • 조경행;박창준;서정기;한명섭
    • 분석과학
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    • 제13권3호
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    • pp.297-303
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    • 2000
  • 저니토 시료 중의 미량 Cd, Cu, Pb, Ni, Zn 등의 분석을 위해 동위원소희석 질량분석법을 이용하였다. 시료는 마이크로파 혼합산(질산, 불산, 과염소산) 분해법을 이용하여 용해하였다. Ammonium pyrrolidenedithiocarbamate(APDC) 용매 추출법을 이용하여 알칼리 및 알칼리 토금속을 분리한 다음 Pb를 측정하고, 나머지 원소들은 이 용액에 $NH_4OH$ 첨가 후 원심 분리하여 Fe, Sn, Ti 등을 제거한 다음 측정하였다. 측정원소의 회수율은 다소 떨어지나 동중원소 방해를 일으키는 매질원소를 효율적으로 제거할 수 있었다. 2종의 저니토 인증표준물질 중의 미량원소 분석에 이 방법을 적용한 결과 인증값과 잘 일치하는 측정 결과를 얻을 수 있었다.

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Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • 제35권11호
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

폴리프로필렌 수지 중 카드뮴과 납 측정 숙련도시험 (Proficiency testing of cadmium and lead in polypropylene resin)

  • 조경행;임명철;민형식;한명섭;송현주;박창준
    • 분석과학
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    • 제20권3호
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    • pp.183-192
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    • 2007
  • 최근의 전기전자제품 중 유해물질규제지침(RoHS)이나 폐전기전자제품 처리 지침(WEEE) 등의 각종 환경규제는 국제교역에 있어 실질적인 무역장벽으로 작용하고 있다. 한국표준과학연구원(KRISS)에서는 이와 같은 환경규제와 관련하여 국내시험연구기관 및 관련산업체실험실의 측정 신뢰성 확보를 위한 숙련도 시험을 실시하였다. 참여기관은 국내 전기전자 제품 및 자동차 관련 실험실 31개소이다. 숙련도시험용 시료는 pellet type 폴리프로필렌 소재 2 종이며, 측정대상원소는 유럽공동체의 RoHS 지침에서 규정하고 있는 6개 성분 중 카드뮴 (Cd)과 납 (Pb)이다. 시료는 2006년 9월 1일 각 참여실험실에 우편 송부하였으며 10월 10일까지 측정 결과를 접수하였다. 각 실험실의 측정 결과는 KRISS 기준값과의 비교, Robustic Z-score, Youden plot 등에 의해 비교 평가하고 전처리 방법에 따른 측정 결과도 비교 검토하였다. 전반적으로 기준값과의 10% 범위 내에서 일치되는 결과를 보고하였으나 일부 실험실은 심각한 bias를 보이고 있어 측정결과의 신뢰성 향상을 위한 품질보증 시스템을 갖추어야 할 필요가 있다.