• Title/Summary/Keyword: EDTA determination

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A Simple Method for Determining Residual p-arsanilic Acid in Aquatic Products using EDTA-Assisted Solvent Extraction and LC-MRM

  • Min Kyeong Kwon;Ye Bin Shin;Young Min Kim;Jin Hwan Kim;Ji Seong Kim;Yong Seok Choi
    • Mass Spectrometry Letters
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    • v.14 no.2
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    • pp.36-41
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    • 2023
  • A simple method was developed to determine residual p-arsanilic acid (ASA), an organo-arsenic compound used as a feed additive, in aquatic products (eel, halibut, and shrimp) using EDTA-assisted solvent extraction and LC-MRM. The method was successfully validated in terms of specificity, linearity (coefficient of determination ≥ 0.995), accuracy (recovery or R, 72.72-78.73%), precision (the relative standard deviation of R, 2.08-6.98%), and sensitivity (the lower limit of quantitation, 5 ppb) according to CODEX guidelines (CAC-GL 71-2009). The use of EDTA in the extraction solvent and water with a suitable pH modifier as the reconstitution solvent may be the key factors for successful results. This is the first method that can be used for monitoring residual ASA in aquatic products using LC-MRM and could contribute to establishing a better aquatic product safety management system.

Detection and Determination of the Peroxyl Radical in the Photolysis with TiO2 (TiO2와의 광반응하에서 생성되는 페록시라디칼(HO2・/O2-)의 검출 및 정량화)

  • Kwon, Bumgeun;Kim, Jongoh
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.7
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    • pp.45-49
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    • 2010
  • We have developed and demonstrated the use of a new kinetic method as an analytical tool for the measurement of $HO_2{\cdot}/O_2{\cdot}^-$. This new method is based on the reduction of $Fe^{3+}$-Ethylene Diamine Tetra Acetate, EDTA) into $Fe^{2+}$-EDTA by $HO_2{\cdot}/O_2{\cdot}^-$ and the well-known Fenton-like reaction of $H_2O_2$ and $Fe^{2+}$-EDTA to yield the hydroxyl radicals ($OH{\cdot}$). Since this method for $HO_2{\cdot}/O_2{\cdot}^-$ shows high sensitivity and allows a simple calibration system, it can contribute significantly to understanding the basic functions of $HO_2{\cdot}/O_2{\cdot}^-$ in advanced oxidation processes for water treatment. Moreover, the present technique has the advantage of using inexpensive and easily available nonenzymatic reagents and of being insensitive to the moderate concentration of possible interferences often found in aqueous phase.

Quantitative Analysis of Prussic Acid by "Micro-Diffusion Analsis." II Determination of Prussic Acid in Human Blood (미량확산분석법에 의한 청산의 정량법 (제2보) 혈액중(CN-Met Hb)청산의 정량)

  • 심상혁;서정현
    • YAKHAK HOEJI
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    • v.4 no.1
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    • pp.47-49
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    • 1959
  • Another application of the new quantitative analytical method of prussic acid by "Microdiffusion analysis" for the determination of prussic acid in human blood was studied. The blood containing potassium cyanide was dropped in outer room of unit, and then N-sulfuric acid was added. The liberated HCN gas was absorbed into nickel sulfate solution of inner room, afterward, absorbed prussic acid was determined with EDTA by residual titration. The result was coincided with the result of Liebig Denigs' method at ordinary temperature.

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Differential Titrimetric Determination of Bismuth$^1$

  • Choi, Q.-Won;Lim, H. S.
    • Bulletin of the Korean Chemical Society
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    • v.4 no.5
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    • pp.217-219
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    • 1983
  • A precise EDTA titrimetric method involving a weight titration of major portion with solid reagent followed by titration of the remainder with a very dilute standard solution has been developed for the determination of bismuth. When the end point is determined by means of amperometry with a rotating mercury electrode, the error in bismuth analysis is less than 0.01 % even when $Pb^{2+}$, $Zn^{2+}$, or $Cd^{2+}$ is present. However, copper interferes appreciably and masking with thiourea gives too low results.

Construction and Use of an Optical Semi-Automatic Titrator Employing the Technique of Reflectance Photometry (반사분광분석기법을 채용한 광학적 반자동적정장치의 제작과 응용)

  • Hwang, Hoon
    • Journal of the Korean Chemical Society
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    • v.45 no.6
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    • pp.513-519
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    • 2001
  • An optical semi-automatic titrator was constructed employing the technique of the reflectance spectrometry and was tested for the determination of the end points of the acid-base, precipitation, and EDTA titrations. And since the current optical semi-automatic titrator built on the principle of the reflectance spectrometry could be successfully used even for the determination of the end point in the precipitation titration where the solid particles are formed during the titration process, it was found to be feasible that a completely automated optical titrator would be designed and built based on the current findings.

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Spectrophotometric Determination of Co (Ⅱ) with 7-Nitroso-8-Hydroxyquinoline-5-Sulfon (7-Nitroso-8-Hydroxyquinoline-5-Sulfonate 에 依한 Co (Ⅱ) 의 吸光光度定量)

  • Lee, Dong-Hyung
    • Journal of the Korean Chemical Society
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    • v.9 no.2
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    • pp.101-105
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    • 1965
  • Spectrophotometric method for the determination of Co(Ⅱ) is developed based on the fact that Co(Ⅱ) forms a stable red complex with 7-nitroso-8-hydroxyquinoline-5-sulfonate at pH 4. 5. The absorbance is measured at 528$m{\mu}$, $25^{\circ}C$. Beer's law is followed in the concentration range of 0. 3 to 6. 0 p.p.m. of Co(Ⅱ) and molar extinction coefficient of the complex was $1.1{\times}10^4$. Of the diverse ions checked, Fe(Ⅱ), Fe(Ⅲ), Cu(Ⅱ), Mn(Ⅱ), Hg(Ⅰ), CN-, EDTA interfere. The composition of the complex is found to be 3:1 ligand to metal species by mole ratio and continuous variation methods.

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Development of Photo-Fenton Method for Gaseous Peroxides Determination and Field Observations in Gwangju, South Korea

  • Chang, Won-Il;Shim, Jae-Bum;Hong, Sang-Bum;Lee, Jai H.
    • Journal of Korean Society for Atmospheric Environment
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    • v.23 no.E1
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    • pp.16-28
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    • 2007
  • An improved method was developed to determine gas-phase hydrogen peroxide($H_2O_2$) and organic hydro-peroxides (ROOH) in real-time, The analytical system for $H_2O_2$ is based on formation of hydroxybenzoic acid (OHBA), a strong fluorescent compound. OHBA is formed by a sequence of reactions, photoreduction of Fe(III)-EDTA to Fe(II)-EDTA, the Fenton reaction of Fe(II)-EDTA with $H_2O_2$, and hydroxylation of benzoic acid. By use of this analytical method rather than a previous similar method, Fenton reaction time was reduced from 2 min. to 30s. Air samples were collected by a surfaceless inlet to prevent inlet line losses. With a special arrangement of the sampling apparatus, sample delivery time was drastically reduced from ${\sim}5\;min\;to\;{\sim}20\;s$. The automated system was found to be sensitive, capable of continuous monitoring, and affordable to operate. A comparison of this method with a well-established one showed an excellent linear correlation, validating applicability of this technique to $H_2O_2$ determination. The system was applied to field measurements conducted during summertime of 2004 in Gwangju, South Korea. $H_2O_2$ was found to be a predominant species of peroxides. The diurnal variation of $H_2O_2$ displayed the maximum in early afternoon and the broad minimum throughout night. $H_2O_2$ was correlated positively with ozone, photochemical age, and temperature, however, negatively with $NO_x$ and relative humidity.

Determination of Hydroperoxyl/superoxide Anion Radical (HO2·/O2·-) Concentration in the Decomposition of Ozone Using a Kinetic Method

  • Kwon, Bum-Gun;Lee, Jai H.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1785-1790
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    • 2006
  • A novel kinetic method for determination of $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ in ozone decomposition in water is described. In this study, potential interferences of $O_3$ and the hydroxyl radicals, $^{\cdot}OH_{(O3)}$, are suppressed by $HSO_3{^-}/SO_3{^{2-}}$. $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ formed in ozone decomposition reduces $Fe^{3+}$-EDTA into $Fe^{2+}$-EDTA and subsequently the well-known Fenton-like (FL) reaction of $H_2O_2$ and $Fe^{2+}$-EDTA produces the hydroxyl radicals, $^{\cdot}OH_{(FL)}$. Benzoic acid (BA) scavenges $^{\cdot}OH_{(FL)}$ to produce OHBA, which are analyzed by fluorescence detection (${\lambda}_{ex}=320nm$ and ${\lambda}_{ex}=400nm$). The concentration of $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ in ozone decomposition has been determined by the novel kinetic method using the experimentally determined half-life ($t_{1/2}$). The steady-state concentration of $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ is proportional to the $O_3$ concentration at a given pH. However, the steady-state concentration of $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ in ozone decomposition is inversely proportional to pH values. This pH dependence is due to significant loss of $O_2{^{{\cdot}-}}$ by $O_3$ at higher pH conditions. The steady-state concentrations of $HO_2{^{\cdot}}/O_2{^{{\cdot}-}}$ are in the range of $2.49({\pm}0.10){\times}10^{-9}M(pH=4.17){\sim}3.01({\pm}0.07){\times}10^{-10}M(pH=7.59)$ at $[O_3]_o=60{\mu}M$.

Determination of Emamectin Benzoate in Eel, Halibut, and Shrimp Using QuEChERS-EDTA and LC-MRM

  • Cho, Ha Ra;Kim, Dong Yoon;Lee, Hyo Chun;Han, Sang Beom;Shin, Ho-Chul;Choi, Yong Seok
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.100-104
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    • 2018
  • As a part of efforts to establish the positive list system (PLS) in South Korea, a method to determine residual emamectin benzoate (EB) in various aquatic products using QuEChERS-EDTA and LC-MRM was developed. The developed method was validated in the aspects of specificity, linearity (correlation coefficient of at least 0.996), sensitivity (the limit of detection and the lower limit of quantitation ${\leq}5ng/g$), recovery (the recovery range of 87.4 and 96.2), and precision (the relative standard deviation of recovery between 0.9 and 13.5). Additionally, the validated method was successfully applied for monitoring EB contamination in eel, halibut, and shrimp collected from local food markets. To our knowledge, the present method is the first one to determine residual EB in various aquatic products at the level satisfying the PLS and could contribute to the establishment of the PLS in South Korea.

Pulsed Amperometric Detection of Metal Ions Complexing with EDTA in a Flow Injection System

  • 이준우;여인형;편종홍
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.316-318
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    • 1997
  • A general and universal detection method, which can be used in high performance liquid chromatography (HPLC) and flow injection analysis (FIA) system for the determination of any metal ions complexing with ethylenediaminetetraacetic acid (EDTA), is demonstrated. Pulsed amperometric detection scheme is applied in a flow-through thin layer electrochemical cell at an Au working electrode. Fluctuation of peak current level at the same flow rate of carrier solution is minimized at this solid working electrode, whereas not at a dropping mercury electrode. Removal of dissolved oxygen can be omitted with this detection method, which is a required step for cathodic detection methods. Also, a group of metal ions can be determined selectively and indirectly with this detection scheme.