• 제목/요약/키워드: Method of stationary phase

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HILIC 분석법 개발을 위한 지능형 솔루션 (Hydrophilic Interaction Liquid Chromatography)

  • Matt James;Colin Pipe;Mark Fever;Jen Field;Seungho Chae
    • FOCUS: LIFE SCIENCE
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    • 제1호
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    • pp.6.1-6.9
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    • 2024
  • The document is a white paper on Hydrophilic Interaction Liquid Chromatography (HILIC) analysis method development. HILIC is a type of chromatography that uses an organic/aqueous mobile phase and a polar stationary phase. In HILIC, water is a strong solvent, and unlike in Reversed Phase Liquid Chromatography (RPLC), increasing the proportion of water in the mobile phase reduces the retention time of the analyte. The paper discusses when to consider HILIC analysis methods, the advantages of HILIC, and the challenges often encountered due to the lack of understanding of HILIC mechanisms compared to RPLC. It also provides a systematic flowchart for intelligent solutions for HILIC analysis method development, which includes a three-step approach for chromatography analysis method development. The first step involves gathering as much information as possible about the analyte (e.g., pKa, log P, log D). The second step involves analyzing the sample under different pH conditions using three HILIC columns in either isocratic or gradient mode to identify the suitable column/pH combination for the analyte. The third step involves optimizing the separation by investigating other parameters such as temperature and ionic strength, and assessing the robustness of the method. The paper emphasizes that the selection of the appropriate stationary/mobile phase combination, based on the differences between the HILIC stationary phases and the mobile phase pH, can provide high selectivity in the analysis. This step-by-step approach can help users develop an efficient analysis method.

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Synthesis, Characterization and Enhanced Selectivity in RP-HPLC of Polar Carbonyl Group Embedded Poly (Vinyl Octadecanoate) Grafted Stationary Phase by Simple Heterogeneous "Graft from" Technique

  • Rana, Ashequl A.;Karim, Mohammad Mainul;Takafuji, Makoto
    • Bulletin of the Korean Chemical Society
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    • 제32권1호
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    • pp.77-82
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    • 2011
  • A new high performance liquid chromatograpgy (HPLC) stationary phase that possesses an internal carbonyl functional group is synthesized by heterogeneous "graft from" method. This new stationary phase, poly (vinyl octadecanoate) grafted silica (Sil-2) is then characterized by different physico-chemical methods such as diffuse reflectance infrared fourier transform, suspension state $^1H$ NMR, solid state $^{13}C$ CP/MAS NMR, $^{29}Si$ CP/MAS NMR, elemental analysis and thermogravimetric analysis. Chromatographic properties of Sil-2 were evaluated under reversed phase condition by separating polycyclic aromatic hydrocarbons (PAHs) and comparing the chromatographic results with those on polymeric as well as monomeric octadecylated silica stationary phases.

Alternative chromatographic method for the assay test of terbutaline and salbutamol using ionic liquid assisted aqueous mobile phase

  • Mai, Xuan-Lan;Choi, Yusung;Truong, Quoc-Ky;Nguyen, Thi-Ngoc-Van;Han, Sang Beom;Kim, Kyeong Ho
    • 분석과학
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    • 제33권4호
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    • pp.169-176
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    • 2020
  • Separation of basic compounds using reverse phase chromatography on a silica-based stationary phase represents a major challenge, because of the interaction between the cationic sites of the basic compounds with the anionic silanols of the stationary phase. This study presents a simple, reliable, and organic solvent - free liquid chromatographic method for the determination of terbutaline and salbutamol, in which a room temperature ionic liquid (RTIL) is used as mobile phase additive. We investigated various mobile phase parameters affecting the retention of the two compounds, such as types and concentration of RTILs and, pH of the mobile phase were investigated. The developed method was validated according to International Conference on Harmonization (ICH) guidelines and successfully applied effectively to determine salbutamol sulfate in pharmaceutical preparations.

인지에 중요한 음향신호의 위상에 대해 (On the Perceptually Important Phase Information in Acoustic Signal)

    • 한국음향학회지
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    • 제19권7호
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    • pp.28-33
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    • 2000
  • 음성 신호의 효과적인 양자화를 위해서 인간의 청각 인지 특성을 이용하는 방법이 널리 사용되고 있다. 그러나 아직까지는 음성 스펙트럼의 크기 정보에 대한 인지 특성만을 이용하고 있을 뿐, 음성의 위상 정보는 그 중요성에 비해 간과되어 온 것이 사실이다. 본 논문에서는, 음향 신호로부터 청각 인지 측면에서 관련 없는 위상 성분을 추정하는 PIPE(Perceptually Irrelevant Phase Elimination) 방법을 제안하였다. 제안된 방법은 청각 특성이 critical band 대역 내의 상대적인 위상 관계에 민감하다는 관측 결과에 근거하여, 일반적인 stationary 푸리에(Fourier) 신호와 고조파(harmonic) 신호에 대해 각각 인지 측면에서 관련 없는 위상을 판별하는 방법을 제공한다. 제안된 방법을 음성 분석-합성(analysis / synthesis) 시스템에 적용함으로써 일부 위상 정보만을 이용해 음성을 복원하였으며, 청취 실험 결과 제안된 방법의 효율성을 알 수 있었다.

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Inductance Measurement of Interior Permanent Magnet Synchronous Motor in Stationary Frame of Reference

  • Lee, Geun-Ho;Choi, Woong-chul;Lee, Byeong-Hwa;Jung, Jae-Woo;Hong, Jung-Pyo
    • Journal of Magnetics
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    • 제16권4호
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    • pp.391-397
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    • 2011
  • An inductance measurement method for interior permanent magnet synchronous machine (IPMSM) is proposed in this paper. In this method, the motor is measured at standstill condition, and only a 3-phase voltage source, an oscilloscope and a DC voltage source are required. Depending on the deductive dq-axis voltage equations in the stationary frame of reference, the dq-axis inductances at different current magnitude and vector angle can be calculated by the measured 3-phase voltages and currents. And hence, the saturation and cross-magnetizing effect of the inductances are measurable. This paper introduces the principle equations, experiment setup, data processing, and results comparison on the concentrated-winding and distributed-winding IPMSMs.

Application of Immersed Boundary Method for Flow Over Stationary and Oscillating Cylinders

  • Lee Dae-Sung;Ha Man-Yeong;Kim Sung-Jin;Yoon Hyun-Sik
    • Journal of Mechanical Science and Technology
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    • 제20권6호
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    • pp.849-863
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    • 2006
  • IBM (Immersed Boundary Method) with feedback momentum forcing was applied to stationary and moving bodies. The capability of IBM to treat the obstacle surfaces, especially with moving effect has been tested for two dimensional problems. Stationary and oscillating cylinders were simulated by using IBM based on finite volume method with Cartesian coordinates. For oscillating cylinder, lateral and vertical motions are considered, respectively. Present results such as time histories of drag and lift coefficients for both stationary and oscillating cases are in good agreement with previous numerical and experimental results. Also, the instantaneous wake patterns of oscillating cylinder with different oscillating frequency ratios well represented those of previous researches. More feasibility study for IBM has been carried out to two oscillating cylinders. Drag and lift coefficients are presented for two cylinders oscillating sinusoidally with phase difference of $180^{\circ}$.

Wheeled Blimp: Hybrid Structured Airship with Passive Wheel Mechanism for Tele-guidance Applications

  • Kang, Sung-Chul;Nam, Mi-Hee;Kim, Bong-Seok
    • Journal of Mechanical Science and Technology
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    • 제18권11호
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    • pp.1941-1948
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    • 2004
  • This paper presents a novel design of indoor airship having a passive wheeled mechanism and its stationary position control. This wheeled blimp can work both on the ground using wheeled vehicle part and in the air using the floating capability of the blimp part. The wheeled blimp stands on the floor keeping its balance using a caster-like passive wheel mechanism. In tele-guidance application, stationary position control is required to make the wheeled blimp naturally communicate with people in standing phase since the stationary blimp system responds sensitively to air flow even in indoor environments. To control the desired stationary position, a computed torque control method is adopted. By performing a controller design through dynamic analysis, the control characteristics of the wheeled blimp system have been found and finally the stable control system has been successfully developed. The effectiveness of the controller is verified by experiment for the real wheeled blimp system.

웨이브렛 변환을 이용한 비정상 신호의 순간 주파수 결정 (Non-stationary signal analysis by Continuous Wavelets Transform)

  • 조익현;이인수;윤동한
    • 한국정보전자통신기술학회논문지
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    • 제2권2호
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    • pp.29-36
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    • 2009
  • 비선형적인 위상 변화를 지닌 비정상(non-stationary)신호는 레이더(Radar), 통신(telecommunication), 생체공학, 지질탐사, 음향 등 여러 분야에서 쉽게 접하는 신호이다. 비정상신호는 일반적으로 시간에 따라 신호의 물리적 특성이 변화하는 신호를 의미하며, 순간 주파수는 신호의 특정시간에 해당하는 신호의 주파수를 의미한다. 이 논문에서는 순간 주파수를 결정하기 위한 연속 웨이브렛 변환의 적용에 대하여 논하였다.

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The Influence of Temperature, Ultrasonication and Chiral Mobile Phase Additives on Chiral Separation: Predominant Influence of β-Cyclodextrin Chiral Mobile Phase Additive Under Ultrasonic Irradiation

  • Lee, Jae Hwan;Ryoo, Jae Jeong
    • Bulletin of the Korean Chemical Society
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    • 제33권12호
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    • pp.4141-4144
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    • 2012
  • This paper introduces a technique for resolving amino acids that combines the advantages of the conventional CSP (chiral stationary phase) method with the CMPA (chiral mobile phase additive) method. A commercially available chiral crown ether column, CROWNPAK CR(+), was used as the CSP and three cyclodextrins (${\beta}$-CD, ${\gamma}$-CD, HP-${\beta}$-CD) were used as the mobile phase additives. Chromatographic resolution was performed at $25^{\circ}C$ and $50^{\circ}C$ with or without sonication. A comparison of the chromatographic results under ultrasonic conditions with those under non-ultrasonic conditions showed that ultrasound decreased the elution time and enantioselectivity at all temperatures. In the case of the ${\beta}$-CD mobile phase additive, the elution time and enantioselectivity under ultrasonic condition were significantly higher than under non-sonic condition at all temperatures. Commercially available Chiralpak AD, Whelk-O2 and Pirkle 1-J columns were used as CSPs to examine more meticulously the effects of ultrasonication and temperature on the optical resolution. The optical resolution of some chiral samples analyzed at $25^{\circ}C$ and $50^{\circ}C$ with or without sonication was compared. As in the previous case, the enantioselectivity was lower at $25^{\circ}C$ but similar enantioselectivity was observed at $50^{\circ}C$.