• Title/Summary/Keyword: Analytical mode

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A case study on the fire victim in the vehicle by GC/MS through derivatization of cyanide with pentafluorobenzyl bromide (PFBBr) (시안화이온의 pentafluorobenzyl bromide (PFBBr)에 의한 유도체화 후 GC/MS 분석에 의한 차량화재 변사체 사인규명에 관한 사례연구)

  • Lee, Joon-Bae;Shon, Sung Kun;Woo, Sang Hee;Park, Se Yeon;Hwang, Jung Ho;Kwon, O-Seong;Kim, Nam Yi;Paeng, Ki Jung
    • Analytical Science and Technology
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    • v.29 no.2
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    • pp.73-78
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    • 2016
  • Hydrogen cyanide (HCN) is an extremely toxic gas frequently produced during the incineration of plastics, such as acrylonitrile-butadiene-styrene (ABS). A victim of a fire who has inhaled smoke could have cyanide in the blood. Therefore, cyanide could be a good marker for a post-mortem examination of a fire as well as carboxyhemoglobine (COHb) test of blood samples. For a particular fire case, a burned body with a suicide note was found inside a burned vehicle. Even though the COHb value is conclusive evidence, measuring the COHb for denatured blood might be difficult due to severe thermal denaturation or the formation of methemoglobin (MetHb). To overcome this difficulty, cyanide could be used as an indicator when investigating the death of a fire victim. In this study, gas chromatography/mass spectrometry (GC/MS) was adopted to measure the levels of cyanide in the blood through derivatization with pentafluorobenzyl bromide (PFBBr) under cation surfactant by scan and SIM mode. The concentration of cyanide in the blood of heart blood and brain of the victim was found to be 0.36 µg/mL and 1.20 µg/mL respectively, which was higher than the average value (0.041 µg/mL) found in the blood of 14 people who smoked.

Analysis of sorbic acid in tea-drink using isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) (동위원소희석 액체 크로마토그래피-질량분석법을 이용한 차음료 중의 소르빈산의 분석)

  • Ahn, Seong-Hee;Lee, In-Sun;Kim, Byung-Joo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.25-32
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    • 2012
  • Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

Uncertainty evaluation for the determination of creatinine in urine by LC-MS/MS (LC-MS/MS를 이용한 소변 중 크레아티닌 분석의 측정불확도 평가)

  • Kim, Jin-Young;Kwon, Woon-Yong;Suh, Sung-Ill;In, Moon-Kyo
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.83-90
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    • 2012
  • The objective of the study was to estimate the measurement uncertainty associated with determination of creatinine (Cr) in urine samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Centrifuged urine samples (10 ${\mu}L$) were diluted with 390 ${\mu}L$ of distilled water. To 20 ${\mu}L$ aliquots of diluted urine samples, 30 ${\mu}L$ of internal standard solution (Cr-$d_3$, 5 ${\mu}g/mL$) and 10 ${\mu}L$ of acetonitrile were added and filtered. The samples (1 ${\mu}L$) were introduced into LC-MS/MS with no further pretreatment. Cr was separated on a multi-mode ODS column (Scherzo SM-C18, 75 ${\times}$ 2.0 mm I.D., 3 ${\mu}m$) and quantified by LC-MS/MS operating in MRM mode (Cr, m/z 114.0${\rightarrow}$ 86.0; Cr-$d_3$, m/z 117.0${\rightarrow}$ 89.1). The four factors that contribute uncertainty to the final result were extracted and evaluated. The principal factors of contribution to combined standard uncertainty were sample dilution, calibration curve and repeatability, while the preparation of standard solution was only a minor factor. Relative extended uncertainty of the measured concentration was 14.2% in a real urine sample.

An Analysis of the Causes of the Welfare Gain Achieved by Congestion Pricing and Transit Subsidies (혼잡통행료와 대중교통 보조금의 효용개선 원인 분석)

  • Rhee, Hyok-Joo;Yu, Sang-Gyun
    • Journal of Korean Society of Transportation
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    • v.31 no.3
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    • pp.74-85
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    • 2013
  • We analyze the efficiency of congestion pricings and transit subsidies in the spatial micro-economic model based on a general equilibrium environment. In this setting, we decompose the total welfare change into component factors and identify the reason of the change in the efficiency caused by policy instruments; these component factors are divided into indirect factors and direct factors including of origin-destination and mode choices. We set up the model as adding mode choice to the standard format in the fashion of Anas and Kim (1996) and extend the methodology proposed by Yu and Rhee (2011) and Rhee (2012) for deriving theoretical and analytical solution. Most of welfare gain comes from the modal shift from car to bus. The relative efficiency of subsidies in relation to the first-best pricing is lower than it of congestion pricings although the change in bus share by subsidies is similar to it by congestion pricing. Subsidies give rise to more modal shift from a car to a bus for long-distance commuting than it caused by congestion pricings. As the increase of bus share for long-distance commuting leads to the increase of cross-commuters passing through CBD, the welfare gain by subsidies is lower than it by congestion pricings.

Analysis of clenbuterol in bovine muscle and milk by LC-ESI/MS/MS (LC-ESI/MS/MS를 이용한 소고기와 우유에서의 클렌부테롤 분석)

  • Hong, Selyung;Jeong, Jiyoon;Park, Hyejin;Lee, Soonho;Lee, Jongok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.535-542
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    • 2008
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

Qunatitative analysis of liquiritin and glycyrrhizin in glycyrrhizae radix by HPLC-MS/MS (HPLC-MS/MS에 의한 감초의 liquiritin과 glycyrrhizin의 분석)

  • Yu, Young-Beob;Kim, Mi-Jung;Huang, Dae Sun;Ha, Hye-Kyeong;Ma, Jin-Yeul;Shin, Hyeun-Kyoo
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.331-338
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    • 2007
  • Licorice, Glycyrrhizae Radix is widely used as a herbal medicines and a dietary supplements in East Asia. We employed high performance liquid chromatography electrospray ionization tandem mass spectrometry to determine liquiritin and glycyrrhizin in the Glycyrrhizae Radix. Liquiritin and glycyrrhizin in Glycyrrhizae Radix were ionized by positive ion pneumatically assisted electrospray and detected by HPLC-MS/MS in the multiple-reaction monitoring (MRM) mode using precursor ${\rightarrow}$ product ion combinations at m/z $436.2{\rightarrow}257.0$ and $823.4{\rightarrow}453.4$, respectively. The assay had a calibration range from 10 to 3,000 ng/mL. The limits of detection (LOD) of the liquiritin and glycyrrhizin were 0.4 ng/mL and 0.01 ng/mL, respectively. The reproducibility and repeatability (relative standard deviation) at different analyte concentrations varied from 103 to 113 % and 0.95 to 1.8 %, respectively. According to the above results, HPLC-MS/MS method permits assignment of tentative structures such as liquiritin and glycyrrhizin in the Glycyrrhizae Radix.

Mapped relationships between pier settlement and rail deformation of bridges with CRTS III SBT

  • Jiang, Lizhong;Liu, Lili;Zhou, Wangbao;Liu, Xiang;Liu, Chao;Xiang, Ping
    • Steel and Composite Structures
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    • v.36 no.4
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    • pp.481-492
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    • 2020
  • To study the rail mapped deformation caused by the pier settlement of simply - supported bridges with China Railway Track System III (CRTS III) slab ballastless track (SBT) system under the mode of non-longitudinal connection ballastless track slab, this study derived an analytical solution to the mapped relationships between pier settlement and rail deformation based on the interlayer interaction mechanism of rail-pier and principle of stationary potential energy. The analytical calculation results were compared with the numerical results obtained by ANSYS finite element calculation, thus verifying the accuracy of analytical method. A parameter analysis was conducted on the key factors in rail mapped deformation such as pier settlement, fastener stiffness, and self-compacting concrete (SCC) stiffness of filling layer. The results indicate that rail deformation is approximately proportional to pier settlement. The smaller the fastener stiffness, the smoother the rail deformation curve and the longer the rail deformation area is. With the increase in the stiffness of SCC filling layer, the maximum positive deformation of rail gradually decreases, and the maximum negative deformation gradually increases. The deformation of rail caused by the pier settlement of common-span bridge structures will generate low-frequency excitation on high-speed trains.

Nonlinear Analysis of RC Members Using Truss Model (트러스 모델을 이용한 철근콘크리트 부재의 비선형해석)

  • Eom, Tae-Sung;Park, Hong-Gun
    • Journal of the Korea Concrete Institute
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    • v.18 no.2 s.92
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    • pp.177-188
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    • 2006
  • Conventional nonlinear finite element analysis requires complicated modeling and analytical technique. Furthermore, it is difficult to interpret the analytical results presented as the stress-strain relationship. In the present study, a design-oriented analytical method using the truss model was developed. A reinforced concrete member to be analyzed was idealized by longitudinal, transverse, and diagonal line elements. Basically, each element was modeled as a composite element of concrete and re-bars. Simplified cyclic models for the concrete and re-bar elements were developed. RC beams and walls with various reinforcement details were analyzed by the proposed method. The inelastic strength, energy dissipation capacity, deformability, and failure mode predicted by the proposed method were compared with those of existing experiments. The results showed that the proposed model accurately predicted the strength and energy dissipation capacities, and to predict deformability of the members, the compression-softening model used for the concrete strut element must be improved.

ESTIMATION OF SUGAR AND REDUCING SUGAR IN MOLASSES USING NEAR INFRARED REFLECTANCE SPECTROSCOPY

  • Mehrotra, Ranjana;Gupta, Alka;Tewari, Jagdish;Varma, S.P.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1258-1258
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    • 2001
  • Estimation of sugar and reducing sugar content in molasses is very important task in sugar refineries. Conventional methods of determination of sugar content in molasses samples are highly time consuming and employ hazardous chemicals. Due to the physical properties of molasses, probability of error in conventional analytical techniques is high. These methods have proven to be inefficient for a process control in any sugar industry. Hence development of a rapid, inexpensive, physical and also accurate method for sugar determination in molasses will be highly useful. Near Infrared spectroscopy is being widely used worldwide as an analytical technique in food industry. The technique offers the advantage of being non-destructive and rapid. The present paper highlights the potential of near infrared reflectance spectroscopy as a rapid and automated analytical technique for determination of sugar and reducing sugar content in molasses. A number of molasses samples were collected during and after the sugar season from Havana Sugar Industry, Havana. The samples were chosen so as to obtain a wide range of concentration of sugar and reducing sugars. This was done in order to achieve a good calibration curve with widely spread data points. These samples were scanned in the region of 1100 - 2500 nm in diffuse reflectance mode. An indigenous ELICO NIR spectrophotometer, modified according to the requirements of sugar industry was used for this purpose. Each sample was also analyzed simultaneously by standard chemical methods. Chemical values were taken as reference for near infrared analysis. In order to obtain the most accurate calibration for the set of samples, various mathematical treatments were employed. Partial Least Square method was found to be most suitable for the analysis. A comparison is made between the actual values (chemical values) and the predicted values (NIR values). The actual values agree very well with the predicted values showing the accuracy of the technique. The validity of the technique is checked by predicting the concentration of sugar in unknown molasses samples using the calibration curve. The present investigation assesses the feasibility of the technique for on-line monitoring of sugars present in molasses in sugar industries.

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Effects of Geometric Configuration on the Vibro-acoustic Characteristics of Radial Vibration of an Annular Disc (환형 디스크 형상이 래디얼 진동에 의한 음향방사 특성에 미치는 영향)

  • Lee, Hyeong-Ill
    • Transactions of the Korean Society for Noise and Vibration Engineering
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    • v.17 no.7 s.124
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    • pp.596-604
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    • 2007
  • This article investigates the effects of geometric configuration on the vibro-acoustic characteristics of in-plane vibration of a thick annular disc. Disc thickness and outer radius for a given inner radius are selected as independent variables having reasonable ranges. Variations in structural eigensolutions for radial modes are investigated using pre-developed analytical method. Based on these data, far-field sound pressure distributions due to the modal vibrations for a given geometry are also calculated using an analytical solution. Modal sound powers and radiation efficiencies are calculated from the far-field sound pressure distributions and vibratory velocity distributions on the radial surfaces. Based on the results explained above, the geometric configuration that minimizes modal sound radiations in a given frequency range is determined. Finally sound power and radiation efficiency spectra for a unit harmonic force from the selected geometric configuration are obtained from structural and acoustic modal data using the modal expansion technique. Multi-modal sound radiations of the optimized disc that are obtained using proposed analytical methods are confirmed with numerical results. Using the procedure introduced in this article, sound radiation due to in-plane modes within a specific frequency range can be minimized by the disc geometry modifications in a comprehensive and convenient manner.