• 제목/요약/키워드: Volume determination

검색결과 531건 처리시간 0.024초

MSPD 전처리법과 HPLC를 이용한 Furazolidone의 계란내 잔류분석 (Matrix Solid-Phase Dispersion (MSPD) Isolation and Liquid Chromatographic Determination of Residual Furazolidone in Eggs)

  • 서계원;이재일;이채용;이정치
    • 한국식품위생안전성학회지
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    • 제18권2호
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    • pp.43-50
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    • 2003
  • A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

식이보충제로 사용되는 히알루론산의 분석법에 대한 불확도 산정 (Measurement Uncertainty for Analytical Method of Hyaluronic Acid Used as a Dietary Supplement)

  • 박상욱;김형범;김광준;이원재
    • KSBB Journal
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    • 제32권1호
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    • pp.54-62
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    • 2017
  • This study aimed to estimate the measurement uncertainty related to determination of hyaluronic acid used as a dietary supplement by high-performance liquid chromatography. According to the guidelines of the Association of Official Analytical Chemists, the analytical processes for determination of hyaluronic acid were performed. And the measurement uncertainty obtained during the analytical processes were expressed in accordance with mathematical/ statistical guidances of GUM (Guide to the Expression of Uncertainty in Measurement) & EURACHEM (Focus for Analytical Chemistry in Europe) for the analytical operations. For the uncertainty in measurement produced based on this analytical method, the expanded uncertainty was calculated by using the relative standard uncertainty between analytical results and sources of uncertainty in measurement (sample weight, final volume, extraction volume, standard solution, matrix and instrument etc). In the results of 95% confidence interval, it was calculated that the uncertainty in measurement was $57.75{\pm}8.76{\mu}g/kg$ (k=2.0). Therefore, it showed that the measurement uncertainty obtained by this analytical method influences on 15.2% of the contents of hyaluronic acid as the analytical results.

Determination of antibiotics by SPE-LC-MS/MS in wastewater and risk assessment

  • Aydin, Senar;Aydin, Mehmet E.;Ulvi, Arzu;Kilic, Havva
    • Advances in environmental research
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    • 제7권3호
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    • pp.201-212
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    • 2018
  • In this study, conditions of solid phase extraction (SPE) for determination of some antibiotics such as trimethoprim, oxytetracycline, erythromycin, clarithromycin, azythromycin, doxycycline, sulfamethazine, ciprofloxacin, chlortetracycline, sulfamethoxazole in wastewaters were optimized. After the optimum volume and pH of the sample were determined, the effect of the concentration of the compounds and matrix were investigated. The highest recovery rates for antibiotic compounds were determined between 82% and 105% in 200 mL sample volume and pH 2.5. Then, antibiotic compounds were investigated in influent and effluent samples taken from Konya Urban Wastewater Treatment Plant. The concentration of the antibiotics was detected range of 0.11-101 ng/L in influent waters and

양성자치료에서의 종양의 위치 및 깊이 검출 자동화 시스템에 관한 연구 (Automated Determination of Prostate Depth for Planning in Proton Beam Treatment)

  • 정민호;윤명근;김진성;신동호;박성용;이세병
    • 한국의학물리학회지:의학물리
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    • 제20권3호
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    • pp.180-190
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    • 2009
  • 전립선암의 위치는 방사선 치료도중 변하는 경우가 많으며 이는 종양선량을 낮추고 정상조직선량이 높아질 수 있다. 이 논문의 목적은 방사선 치료중에 전립선암의 위치 및 깊이 변화를 자동적으로 감지하는 시스템을 개발하고 이를 적용해 환자의 국부에 조사되는 방사선량의 변화를 최소화 하는 데 있다. 이 연구에서는 10명의 환자로부터 38장의 영상자료를 통해 수행되었으며 전립선암에 부착된 금-표지자를 이용해 종양의 질량중심을 구하고 이를 기반으로 종양의 위치변화를 감지하였다. 전립선암의 평균적인 위치변화는 좌우와 위아래로 각각 0.9 mm와 2.3 mm이었으며 최고 위치변화는 각 각 3.3 mm와 7.2 mm였다. 일상적으로 전립선암의 양성자치료에 많이 사용되는 마주보는 두 개의 양성자빔(bilateral beam configuration) 조건에서 좌우의 위치변화는 깊이 변화를 의미하며 이는 약 0.7 mm에서 3.3 mm까지 변화하고 있음을 알 수 있었다. 실험결과 종양의 깊이 변화가 1 mm, 2 mm 그리고 3 mm 보다 많이 차이 나는 경우가 각각 42.1%, 26.3% 그리고 2.6%로 나타났다. 이러한 결과를 토대로 봤을 때 양성자치료에서 자동적으로 종양의 깊이 변화를 분석하는 것이 가능하다는 것을 알 수 있었으며 이를 이용한다면 종양선량을 높이고 정상조직선량을 낮추어 치료효과를 높일 수 있다.

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Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • 제27권6호
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

Sorption Preconcentration and Determination of Nickel in Wastes of Heat Power Industry by Diffuse Reflection Spectroscopy

  • Kalyakina, O.P.;Kononova, O.N.;Kachin, S.V.;Kholmogorov, A.G.
    • Bulletin of the Korean Chemical Society
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    • 제24권2호
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    • pp.173-177
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    • 2003
  • The present work is focused on the preconcentration of nickel and its determination by means of diffuse reflection spectroscopy. The preconcentration of nickel was carried out by sorption on macroporous aminocarboxylic amphoteric resin ANKB-35. Based on this collector, a method to determine nickel in wastes of heat power industry was worked out using solid-phase spectroscopy. The colored surface compound to be determined was obtained by a preceding nickel sorption on the resin and by subsequent treatment of the concentrate obtained with definite amounts of 1-(2-pyridilazo)-2-naphtol (PAN). The Ni calibration curve is linear in the concentration range of 0.5-20.0 mg/L (sample volume is 200.0 mL) and the detection limit is 0.05 mg/L. The presence of $Cu^{2+},\;Fe^{3+},\;Co^{2+}$ ions as well as macrocomponents of natural water $(Na^+,\;K^+,\;Ca^{2+},\;Mg^{2+})$ do not hinder the solid-phase spectroscopy determination of nickel. The nickel determination by diffuse reflection spectroscopy was carried out in model solutions as well as in solutions obtained after the dissolution of wastes of heat power industry.

모래 치환법을 이용한 흙의 밀도 시험에 관한 고찰 (Evaluation of Sand-Cone Method for Determination of Density of Soil)

  • 박성식;최현석
    • 한국지반공학회:학술대회논문집
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    • 한국지반공학회 2009년도 춘계 학술발표회
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    • pp.23-29
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    • 2009
  • A sand-cone method is commonly used to determine the density of the compacted soils. This method uses a calibration container to determine the bulk-density of the sand for use in the test. The density of the test or compacted soil is computed on the assumption that the calibration container has approximately the same size or volume and allows the sand to fall approximately the same height as a test hole in the field. However, in most cases the size or shape of test hole is not exactly the same as the calibration container. There is certain discrepancy between sand particle settlement or arrangement in the laboratory calibration and in the field testing, which may cause an erroneous determination of in-situ density. The sand filling process is simulated in the laboratory and its effect on the determination of density is investigated. Artificially-made holes with different heights and bottom shapes are prepared to simulate various shapes of the test hole in the field. The sands with different gradations are used in the testing to examine how sand grain size influences the determination of density in the field.

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Ion Exchange Recovery of Rhenium and Its Determination in Aqueous Solutions by Diffuse Reflection Spectroscopy

  • Kalyakina, O.P.;Kononova, O.N.;Kachin, S.V.;Kholmogorov, A.G.
    • Bulletin of the Korean Chemical Society
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    • 제25권1호
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    • pp.79-84
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    • 2004
  • The existing technological schemes for processing rhenium-containing raw materials involve the recovery of Re from solutions, which can be effectively achieved by anion exchange method. The application of anion exchange also allows to study rhenium state in aqueous solutions and to develop analytical control methods. The present work is focused on investigation of ion exchange equilibrium in the analytical system Re(VII)-HCl-$SnCl_2$-KSCN-anion exchanger by means of sorption-desorption method as well as by electron, IR- and diffuse reflection spectroscopy. It was shown that rhenium can be quantitatively recovered from this system. It is proposed to use the sorption-spectroscopic method for Re(VII) determination in aqueous solutions. The calibration curve is linear in the concentration range of 0.5-20.0 mg/L (sample volume is 25.0 mL) and the detection limit is 0.05 mg/L. The presence of Mo(VI), Cu(II), Fe(II, III), Ni(II), Zn(II) as well as $K^+,\;Na^+$ do not hinder the solid-phase determination of rhenium. Rhenium (VII) determination by diffuse reflection spectroscopy was carried out in model solutions as well as in samples of river-derived water and in solutions obtained after the dissolution of spent catalysts.

소유역 오염예측모형 AGNPS 의 특성과 실험적 적용 (The Characteristics and Experimental Application of AGNPS Model for Pollution Predicting in Small Watershed)

  • 최진규;이명우;손재권
    • 환경영향평가
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    • 제3권2호
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    • pp.47-56
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    • 1994
  • AGNPS model is an event-based model to analyze nonpoint-source and to examine potential water quality problems from agricultural watershed. This model uses a square grid-cell system to represent the spatial variability of watershed conditions, and simulates runoff, sediment, and nutrient transport for each cell. AGNPS model was applied on Yeonwha watershed, and the test results were compared with the measured data for runoff volume, peak runoff rate, suspended solids, and phosphorus concentration. The watershed of 278.8 ha was divided into 278 cells, each of which was 1 ha in size. The coefficients of determination for runoff volume and peak flow were (0.893 and 0.801 respectively from regression of the estimated values on the measured values. The concentration of suspendid solid was increased but decreased that of phosphate with runoff volume.

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3차원 납 접합부 형상을 이용한 표면실장기술의 적정 납량 결정 (Determination of Adequate Solder Volume using 3D Solder Joint Configuration in SMT)

  • 최동필;김성관;유중돈
    • Journal of Welding and Joining
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    • 제14권2호
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    • pp.71-78
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    • 1996
  • In order to rpovide proper SMT design criteria in a systematic way, a mathematical formulation has been developed to predict the configuration of the solder fillet formed between the gullwing type lead and rectangular pad. Effects of SMT design parameters such as the solder volume and pad dimension on the solder profile are investigated using the FEM that calculates the 3D configuration by minimizing the energy due to surface tension and gravity in the equilibrium state. Design criteria of QFP and SOP are illustrated by plotting the acceptable range of the solder volume with respect to the length and width ratios of the pad and lead. The results show that the acceptable design range increases with increase in the pad length and width. The pad length has more significant effects on design criteria compared with the pad width, and Bond number can be utilized to predict the joint quality.

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