• 제목/요약/키워드: Z-M method

검색결과 629건 처리시간 0.024초

Development of an Isotope-Dilution Flow-Injection Electrospray/ Mass Spectrometric Method for the Accurate Determination of Glucosamine in Pharmaceutical Formulation

  • Kim, Gui-Nam;Kim, Byung-Joo;Ahn, Seong-Hee;Hwang, Eui-Jin;Kim, Yong-Seong
    • Bulletin of the Korean Chemical Society
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    • 제30권2호
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    • pp.363-367
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    • 2009
  • An isotope-dilution flow-injection electrospray/mass spectrometric method was developed for the accurate determination of glucosamine contents in pharmaceutical formulations. Samples were extracted by methanol. After spiking glucosamine-1-$^{13}C_1$ as an internal standard, the extracts were then analyzed by flow-injection ESI/MS in a selected ion monitoring (SIM) mode to detect [M+H]$^+$ ions of the analyte and its isotope analogue at m/z 180 and m/z 181, respectively. Confirmatory measurements were made by selectively monitoring the collisionally induced dissociation channels of m/z 180 $\rightarrow$ m/z 72 and m/z 181 $\rightarrow$73, respectively, to test the possibility of bias in the SIM method due to matrix interferences, but any significant bias in the SIM mode was not observed. Repeatability and reproducibility studies showed that the flow-injection ESI/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0 %. Other results for the method validation are reported.

밀도지수와 어획량으로서 수산자원의 가입량을 근사적으로 추정하는 방법 (APPROXIMATE ESTIMATION OF RECRUITMENT IN FISH POPULATION UTILIZING STOCK DENSITY AND CATCH)

  • 김기주
    • 한국수산과학회지
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    • 제8권2호
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    • pp.47-60
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    • 1975
  • 자원해석은 일반적으로 시계열적 견지에 입각하고 있으나, 본 연구에서는 단면적인 견지에서, 2년간의 자원변동을 극수적인 관계에서 파악하여 자원해석을 하였으며, 이것으로 각년의 가입량을 추정하는 방법 시도하였다. 이를 요약하면 다음과 같다. 1. 단일 population에 있어서 t 시기(년 또는 어기)와 t+1 시기와의 초기자원량(미수)의 관계는 $N_{0,\;t+1}=N_{0,\;t}(1-m_t)-C_t+R_{t+1}$ 단, $N_0$ : 초기자원량 (미수), C : 어획미수, R : 가입미수, m : 자연사망률 이다. 위의 식에서 다음의 관계가 성립된다. $\phi_{t+1}=\frac{(1-\varrho^{-z}{t+1})Z_t}{(1-\varrho^{-z}t)Z_{t+1}}-\frac{1-\varrho^{-z}t+1}{Z_{t+1}}\phi_t-a'\frac{1-\varrho^{-z}t+1}{Z_{t+1}}C_t+a'\frac{1-\varrho^{-z}t+1}{Z_{t+1}}R_{t+1}$ 단, $\phi$ : 밀도지수, M : 자연사망계수, Z : 감소계수, a' : 평균자원량에 대한 밀도지수 이 식에서 $\phi$$C_t$를 독립변수, $\phi_{t+1}$를 종속변수라해서 중회귀분석하여 $\phi_t$$C_t$ 의 각 계수를 구하고, 이 각 계수로서 저연사망계수 M, 단위노력당 어획계수 a'을 구하여 t+1연의 가입량추정치 $\hat{R}_{t+1}$를 구할 수 있다. 중회귀분석하는 데 있어서는 $R_{t+1}$이 거의, 같으며 $X_{t+1}$에 심한 차이가 없는 시기를 선정하여 취급할 수 있다. 2. 각 시기의 추정된 가입량은 가입량의 상대치로서 인정하는 것이 안전하다. 3. 밀도지수 대신으로 자원량지수를 사용하여도 같은 추정방법으로 가입량이 추정된다. 단, 어장면적을 고려해야 한다. 4. 변동관계를 미수로서 취급할 때는 이론적으로 가입량의 절대치를 구할 수 있으나, 중량으로 취급할 때는 이론적으로 가입량의 상대치를 구하게 된다. 그러나 어느 경우나 같은 추정방법이 적용된다. 5. 인도양의 bigeye tuna에 대하여 수전(1970)의 자료를 이용하여 본 추정방법에 적용시켜 보았다. 수전(1970)가 구한 M,q(단위노력당 어획계수)로서 계산된 각년의 가입량의 변화와 본연구에서 구한 각년의 가입량의 변화와는 극히 비례적이었다(Table 2, Fig.2). 6. 한국동안의 꽁치에 있어서 해황어황 주간예보 ($1964.3\~1974.8$ : 국립수산진흥원 포항지원)의 자료를 이용하여 어느 해의 춘하기의 밀도지수와 그해의 추동기의 밀도지수와의 관계에서 각년의 추기의 가입량을 추정하고 어느 해의 추동기의 밀도지수와 다음해의 춘하기의 밀도지수와의 관계에서 각년의 춘하기의 가입량을 추정하였다(Table4, Fig.5, Fig.7). 그 결과, 년금의 폭이 좁은 이 꽁치 군단에 있어서 각년의 밀도지수와 가입량이 상당히 비례적이었다.

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Co2Z-type Barium Hexaferrite의 합성방법에 따른 결정구조 및 자기적 특성 (Structure and Magnetic Properties on Synthesis Route of Co2Z-type Barium Hexaferrite)

  • 백인승;남인탁
    • 한국자기학회지
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    • 제24권1호
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    • pp.1-10
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    • 2014
  • $Co_2Z$-type hexaferrite 시편을 다양한 합성법을 이용하여 제조하였다. 수열합성법을 이용하여 M-type, $Co_2Y$-type, $Co_2Z$-type을 제조하였으며, 제조된 M-type과 $Co_2Y$-type을 출발물질로 하여 고상반응법(ball milling)과 수열합성법(hydrothermal)으로 $Co_2Z$-type을 제조하였다. 제조된 시편의 결정구조와 미세구조 자기적 성질은 XRD, FESEM, VSM, impedance analyzer를 이용하여 조사하였다. M-type과 $Co_2Y$-type은 단일상의 결정구조를 얻을 수 있었다. 여러 합성법 중에 M+Y ball milling, M+Y hydrothermal에서 제조한 시편이 $Co_2Z$-type hexaferrite의 단일상과 대체로 일치하는 것을 알 수 있었으며, $Co_2Z$-type의 모든 시편들은 이론적인 포화 자화값(50 emu/g)과 비슷한 값을 나타내었다. 소결한 시편들의 투자율은 시약을 precusor로 하여 제조한 $Co_2Z$-type의 투자율이 가장 높았으며, 열처리 온도가 증가함에 따라 투자율은 낮아졌다. 다른 합성법에서는 열처리 온도에 따른 변화가 거의 나타나지 않는 것을 확인할 수 있었다.

Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Folic Acid in Infant Milk Formula

  • Jung, Min-Young;Kim, Byung-Joo;Boo, Doo-Wan;So, Hun-Young
    • Bulletin of the Korean Chemical Society
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    • 제28권5호
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    • pp.745-750
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    • 2007
  • An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of folic acid in infant milk formula. Sample was spiked with 13C5-folic acid and then extracted with phosphate buffer (pH 6) solution. The extract was further cleaned up by deproteinization followed by a C18 solid-phase extraction cartridge. The extract was analyzed by using LC/ ESI/MS/MS with selectively monitoring the collisionally induced dissociation channels of m/z 442 → m/z 295 and m/z 447 → m/z 295, which are the neutral glutamyl loss from the [M+H]+ ions of folic acid and 13C5-folic acid, respectively. LC/MS/MS chromatograms showed substantially reduced background from chemical noises compared to LC/MS chromatograms. Repeatability and reproducibility studies showed that the LC/MS/ MS method is a reliable and reproducible method which can provide less than 1.5 relative percentage of method precision.

지글러-니콜스 제어파라미터 조정법(1),(2)의 상호 연관성에 대한 해석적 연구 (An Analytic Study On the Mutual Relation between Method(1) and (2) of ZIEGLER-NICHOLS Control Parameter Tuning)

  • 강인철;최순만;최재성
    • 한국마린엔지니어링학회:학술대회논문집
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    • 한국마린엔지니어링학회 2001년도 추계학술대회 논문집(Proceeding of the KOSME 2001 Autumn Annual Meeting)
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    • pp.112-119
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    • 2001
  • Parameter tuning methods by Ziegler-Nickels for control systems are generally classified into Z-N(1) and Z-N(2). The purpose of this paper is to describe what relations exist between methods of Z-N(1) and Z-N(2), or how Z-N(1) method can be originated from Z-N(2) method by analyzing one loop control system of P or PI controller and time delay process. The formulas of Z-N(1) consist of process parameters, L(time delay), $K_m$(gain) and $T_m$(time constant), but Z-N(2) method is based only on the ultimate gain $K_u$ and the ultimate period $T_u$ acquired normally by practical trial without any parameters of Z-N(1). In this paper, for the first step to seek mutual relations, the simple formulas of Z-N(2) are transformed into the formulas composed of the same parameters as Z-N(1) which is derived from the analysis of frequency characteristics. Then, the approximation of the actual ultimate frequency is proposed as important premise in the translation between Z-N(1) and (2). Such equalization and approximation brings a simple approximated formula which can explain how Z-N(1) is originated from the Z-N(2) in the form of formula. And a model system is adopted to compare the approximated formula to Z-N(1) and Z-N(2) methods, the results of which show the effectiveness of the proposals.

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Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Acrylamide in Potato Chips

  • Park, Sun-Young;Kim, Byung-Joo;So, Hun-Young;Kim, Yeong-Joon;Kim, Jeong-Kwon
    • Bulletin of the Korean Chemical Society
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    • 제28권5호
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    • pp.737-744
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    • 2007
  • An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

고체표면에 도포한 도료 박막의 열전도율과 열확산율의 측정법 (The Measurement Method of Thermal Conductivity and Diffusivity of Thin Paint Layer Sprayed on Solid Surface)

  • 김은영;박수천;김병문;이덕복
    • 대한기계학회논문집B
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    • 제23권3호
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    • pp.311-319
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    • 1999
  • The thermal conductivity ${\lambda}_b$, thermal diffusivity ${\alpha}_b$ of the thin black paint layer sprayed on solid surface and absorptivity a for laser beam are measured by applying a non-contact measurement method of the thermophysical properties of solids. The values of a=0.67, ${\lambda}_b=1.45W/mK$ and ${\alpha}_b=1.24{\times}10^{-6}m^2/s$ are obtained for the sprayed lay~ thickness $z_b{\fallingdotseq}40\;{\mu}m$. Furthermore, for the $z_b{\fallingdotseq}24\;{\mu}m$ thick layers which arc formed by rubbing with a glass rod after spraying, the values of a=0.73, ${\lambda}_b=1.85W/mK$. and ${\alpha}_b=1.09{\times}10^{-6}m^2/s$ are obtained. It is also shown that the present thermal diffusivity ${\alpha}_b$ for $z_b{\fallingdotseq}40\;{\mu}m$ Is about 30~80% larger than those obtained by Araki et al. for the thicker layer $z_b{\fallingdotseq}150{\sim}248\;{\mu}m$. This method could be applied to the measurement of thermophysical properties of thin layer on solids.

디지탈 영역에서의 다항식 행렬의 분해와 MIMO LBR 구현에의 응용 (Polynomial matrix decomposition in the digital domain and its application to MIMO LBR realizations)

  • 맹승주;임일택;이병기
    • 전자공학회논문지S
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    • 제34S권1호
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    • pp.115-123
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    • 1997
  • In this paper we present a polynomial matrix decomposition algorithm that determines a polynomial matix M(z) which satisfies the relation V(z)=M(z) for a given polynomial matrix V(z) which is paraconjugate hermitian matrix with normal rank r and is positive semidenfinite on the unit circle of z-plane. All the decomposition procedures in this proposed method are performed in the digitral domain. We also discuss how to apply the polynomial matirx decomposition in realizing MIMO LBR two-pairs.

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A Direct Method to Derive All Generators of Solutions era Matrix Equation in a Petri Net - Extended Fourier-Motzkin Method -

  • Takata, Maki;Matsumoto, Tadashi;Moro, Seiichiro
    • 대한전자공학회:학술대회논문집
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    • 대한전자공학회 2002년도 ITC-CSCC -1
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    • pp.490-493
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    • 2002
  • In this paper, the old Fourier-Motzkin method (abbreviated as the old FH method from now on) is first modified to the form which can derive all minimal vectors as well as all minimal support vectors of nonnegative integer homogeneous solutions (i.e., T-invariants) for a matrix equation $Ax=b=0^{m{\times}1}$, $A\epsilonZ^{m{\times}n}$ and $b\epsilonZ^{m{\times}1}$, of a given Petri net, where the old FM method is a well-known and direct method that can obtain at least all minimal support solutions for $Ax=0^{m{\times}1}$ from the incidence matrix . $A\epsilonZ^{m{\times}n}$, Secondly, for $Ax=b\ne0^{m{\times}n}$ a new extended FM method is given; i.e., all nonnegative integer minimal vectors which contain all minimal support vectors of not only homogeneous but also inhomogeneous solutions are systematically obtained by applying the above modified FH method to the augmented incidence matrix $\tilde{A}$ =〔A,-b〕$\epsilon$ $Z^{m{\times}(n+1)}$ s.t. $\tilde{A}\tilde{x}$ = 0^{m{\times}1}$ However, note that for this extended FM method we need some criteria to obtain a minimal vector as well as a minimal support vector from both of nonnegative integer homogeneous and inhomogeneous solutions for Ax=b. Then those criteria are also discussed and given in this paper.

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고용량 양극재료 개발을 위한 $LiNi_{1-y-z}(M_1)_y(M_2)_zO_2$의 합성과 전기화학적 특성 (Synthesis and Electrochemical Properties of $LiNi_{1-y-z}(M_1)_y(M_2)_zO_2$ for the Development of Cathode Materials with Large Capacity)

  • 송명엽
    • 한국수소및신에너지학회논문집
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    • 제18권3호
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    • pp.325-333
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    • 2007
  • [ $LiNi_{0.995}Al_{0.005}O_2$ ], $LiNi_{0.990}Ti_{0.010}O_2$ and $LiNi_{0.0990}Al_{0.005}Ti_{0.005}O_2$ were synthesized with a combustion method by calcining in an $O_2$ stream at $750^{\circ}C$ for 36 h. The X-ray diffraction patterns of these synthesized samples showed $-NaFeO_2$ structure of rhombohedral system(space group; $R{\bar{3}}\;m$) with no evidence of impurities. Among these samples, $LiNi_{0.995}Al_{0.005}O_2$ exhibited comparatively high first discharge capacity and discharge capacity, and the best cycling performance. $LiNi_{0.995}Al_{0.005}O_2$ had the first discharge capacity of 165.2 mA h/g and a discharge capacity of 116.7 mA h/g at the 50th cycle at 0.1C rate. It showed the first discharge capacity of 141.0 mA h/g and a discharge capacity of 93.5 mA h/g at the 50th cycle at 0.5C rate.