• 제목/요약/키워드: Limit of determination

검색결과 1,160건 처리시간 0.022초

HPLC-PDA를 이용한 Amitraz의 분석법 확립 및 검증 (Determination of amitraz by high-performance Liquid chromatography with photodiode array detection and method validation)

  • 윤형준;윤소미;이명헌;손성완
    • 대한수의학회지
    • /
    • 제48권1호
    • /
    • pp.33-38
    • /
    • 2008
  • In veterinary medicine amitraz has been used as an insecticide to eliminates mites, lice, and ticks in dogs, cats, goats, swine and cattle. The objective of present study was to developed an analytical method using one-step extraction and determination of the amitraz in veterinary drugs by liquid chromatography (LC). The amitraz was analyzed by LC equipped with Waters XTerra RP18 ($4.8{\times}250mm;\;5{\mu}m;\;Waters,\;USA$) analytical column, using 75% acetonitrile (acetonitrile/D.W; 75/25) at 1.0 ml/ min. The UV-VIS detection of amitraz was made at 290 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $80{\sim}120{\mu}g/ml$. The limit of detection was $0.09{\mu}g/ml $ and limit of quantification was $0.27{\mu}g/ml $. The method showed good intra-day precision (CV 0.05~0.09%) and inter-day precision (CV 0.06~0.18%).

Determination of Ag(Ⅰ) Ion at a Modified Carbon Paste Electrode Containing N,N'-Diphenyl Oxamide

  • Won, Mi-Sook;Yeom, Jeong-Sik;Yoon, Jang-Hee;Jeong, Euh-Duck;Shim, Yoon-Bo
    • Bulletin of the Korean Chemical Society
    • /
    • 제24권7호
    • /
    • pp.948-952
    • /
    • 2003
  • New approach for the determination of Ag(I) ion was performed by using a carbon paste electrode (CPE) containing N,N'-Diphenyl oxamide (DPO) with anodic stripping voltammetry. The CMEs have been prepared by making carbon paste mixtures containing an appropriate amount of DPO salt coated onto graphite particles to analyze trace metal ions via complexation followed by stripping voltammetry. Various experimental parameters affecting the response, such as pH, deposition time, temperature, and electrode composition, were carefully optimized. Using differential pulse anodic stripping voltammetry, the logarithmic linear response range for the Ag(I) ion was 1.0 × $10^{-7}$ - 5.0 × $10^{-9}$ M at the deposition time of 10 min, with the detection limit was 7.0 × $10^{-10}$ M. The detection limit adopted from anodic stripping differential pulse voltammetry was 7.0 × $10^{-10}$ M for silver and the relative standard deviation was ± 3.2% at a 5.0 × $10^{-8}$ M of Ag(I) ion (n = 7). The proposed electrode shows a very good selectivity for Ag(I) in a standard solution containing several metals at optimized conditions.

한계상태설계법 지반정수 산정을 위한 풍화대 강도특성 측정장치의 개발 및 현장적용에 관한 연구 (Development and Field Application of Apparatus for Determination of Limit State Design Strength Characteristics in Weathered Ground)

  • 김기석;김종훈;최성웅
    • 터널과지하공간
    • /
    • 제30권2호
    • /
    • pp.164-179
    • /
    • 2020
  • 지반구조물에 대한 한계상태설계법의 적용에 있어서 단위중량, 포아송비, 변형계수, 점착력 및 내부마찰각 등은 설계의 정확성 및 신뢰도 향상에 매우 큰 영향을 미치는 지반특성값이다. 특히 풍화토 및 풍화암 등 풍화대에 지반구조물이 위치하게 될 경우 이들 지반특성값 중에서도 점착력과 내부마찰각이 구조물과 지반의 하중 및 저항계수를 판정하는데 매우 높은 연관성이 있으며 따라서 공내전단시험과 같은 현장시험으로부터 구해지는 이들 지반정수의 정확한 산정은 지반구조물의 최적설계를 좌우하는 중요한 요소이다. 본 연구에서는 국내 38개 시공사례 분석을 통해 이들 지반정수들의 설계적용 사례를 검토, 현장시험의 중요성을 확인하였으며 이를 토대로 ASTM에서 규정하는 모든 표준절차를 반영하는 새로운 풍화대 강도특성 측정장치를 개발하였다. 또한 본 장비의 현장적용을 통해 시험장비 및 시험자의 주관적 오류에 의한 오차발생 가능성을 최소화한 장비의 개선성능을 확인하였으며, 이를 토대로 한계상태설계법의 적용 시 핵심 지반특성값의 정량적 산정을 위한 기틀을 마련하였다.

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
    • /
    • 제24권2호
    • /
    • pp.173-177
    • /
    • 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.

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
    • /
    • 제27권6호
    • /
    • pp.875-880
    • /
    • 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.

Application of Organized Media for Rapid Spectrofluorimetric Determination of Trace Amounts of Cr(VI) in the Presence of Cr(III)

  • Madrakian, Tayyebeh;Afkhami, Abbas;Mohammadnejad, Masoumeh
    • Bulletin of the Korean Chemical Society
    • /
    • 제30권6호
    • /
    • pp.1252-1256
    • /
    • 2009
  • A simple, selective and sensitive fluorescence quenching method was developed to the determination Cr(VI). The method is based on the oxidation of $I^-\;to\;{{I_3}^-}$ by Cr(VI) in sulfuric acid solution followed by immediate formation of ion association compound between I3 − and rhodamine 6G in Tween-80 micellar media at room temperature. The influence of several surfactants on rhodamine 6G fluorescence signal was studied; particular attention was paid in the aggregation behavior of rhodamine 6G–Tween-80 system. The experimental parameters (e.g., type of surfactant, reagent concentration) were studied and the optimal conditions were established. The linear calibration graph was obtained in the range 2.0 - 100.0 ng m$L^{-1}$ Cr(VI). The detection limit of the method was 0.37 ng m$L^{-1}$. The relative standard deviation (R.S.D.) is less than 5% (n = 5). The efficiency of the method for the determination of Cr(VI) in the presence of Cr(III) in the sample was investigated. The method was applied successfully to the determination of Cr(VI) and total Cr in water, and liver tissue samples.

탄소나노튜브 소재의 정밀 수동소자 적용을 위한 한계 정격전력 용량에 관한 연구 (A Study on the Limited Rate Power Capacity for Applications for Precision Passive Devices Based on Carbon Nanotube Materials)

  • 이선우
    • 한국전기전자재료학회논문지
    • /
    • 제35권3호
    • /
    • pp.269-274
    • /
    • 2022
  • We prepared carbon nanotube (CNT) paper by a vacuum filtration method for the use of a chip-typed resistor as a precision passive device with a constant resistance. Hybrid resistor composed of the CNT resistor with a negative temperature coefficient of resistance (T.C.R) and a metal alloy resistor with a positive T.C.R could lead to a constant resistance, because the resistance increase owing to the temperature increase at the metal alloy and decrease at the CNT could counterbalance each other. The constant resistance for the precision passive devices should be maintained even when a heat was generated by a current flow resulting in resistance change. Performance reliabilities of the CNT resistor for the precision passive device applications such as electrical load limit, environmental load limit, and life limit specified in IEC 60115-1 must be ensured. In this study, therefore, the rated power determination and T.C.R tests of the CNT paper were conducted. -900~-700 ppm/℃ of TCR, 0.1~0.2 A of the carrying current capacity, and 0.0625~0.125 W of the rated power limit were obtained from the CNT paper. Consequently, we confirmed that the application of CNT materials for the precision hybrid passive devices with a metal alloy could result in a better performance reliability with a zero tolerance.

Simultaneous Determination of Phenobarbital, Pentobarbital, Amobarbital and Secobarbital in Raw Milk via Liquid Chromatography with Electron Spray Ionization Tandem Mass Spectrometry

  • Tian, Huaixiang;Zhou, Xingxin;Chen, Chen;He, Yabin;Yu, Haiyan;Zheng, Xiaoping
    • 한국축산식품학회지
    • /
    • 제37권6호
    • /
    • pp.847-854
    • /
    • 2017
  • A rapid, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of four barbiturates (phenobarbital, pentobarbital, amobarbital and secobarbital) in raw milk. The barbiturates were extracted using liquid-liquid extraction, ultrasonication and centrifugation, and purified on an SPE column. Analytes were separated by HPLC on a CSH C18 column eluted using an acetonitrile-water system with a linear gradient dilution programme, and detected by MS/MS. The recoveries of the barbiturates were 85.0-113.5%, and the intra- and inter-assay RSDs were less than 9.8% and 7.3%, respectively. The limit of detection was 5 ng/mL for all four of the barbiturates. The analytical method exhibited good linearity from 10 to 1000 ng/mL; the correlation coefficient ($r^2$) was greater than 0.9950 for each barbiturate. This method was also applied to the determination of barbiturates in real milk samples and was found to be suitable for the determination of veterinary drug residues in raw milk.

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
    • /
    • 제25권1호
    • /
    • pp.79-84
    • /
    • 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.

Highly Selective Derivative Spectrophotometry for Determination of Nickel Using 1-(2-Pyridylazo)-2-naphthol in Tween 80 Micellar Solutions

  • Eskandari, Habibollah
    • Bulletin of the Korean Chemical Society
    • /
    • 제25권8호
    • /
    • pp.1137-1142
    • /
    • 2004
  • A spectrophotometric and first derivative spectrophotometric method was developed in aquatic Tween 80 micellar solutions for selective determination of nickel without using any pre-separation step. 1-(2-Pyridylazo)-2-naphthol (PAN), as a sensitive chromogenic complexing agent formed a red-colored Ni(II)-PAN complex in Tween 80 media with satisfactory solubility and stability. Conditions such as pH, PAN concentration, type and concentration of micellizing agent were optimized. Molar absorptivity of Ni-PAN complex was found $4.62\;{\times}\;10^4L\;cm^{?1}\;mol^{?1}$ at 569 nm, under the optimum condition. Calibration graphs were derived by zero, first and second derivative spectrophotometry at maximum wavelengths of 569, 578 and 571 nm with linear ranges of 30-1800, 20-2500 and 30-2000 ng $mL^{?1}$ , respectively. Precision as standard deviation as well as accuracy as recovery percent were in the range of 1-20 ng $mL^{?1}$, and 93.3-103.3%, respectively, for the entire of the linear ranges. Spectrophotometric detection limit was 3 ng $mL^{?1}$ and effects of diverse ions on the first derivative determination of nickel were studied to investigate selectivity of the method. Interferences of cobalt and copper on the nickel determination were prevented using o-phenanthroline as masking agent. The recommended procedures were applied to the various synthetic and stainless steel alloys, tea leaves and human hair, with satisfactory results.