• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.203-210
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• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Analytical Science and Technology
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• v.21 no.5
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• pp.412-423
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• 2008

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

• Korean Journal of Environmental Agriculture
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• v.33 no.3
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• pp.169-177
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• 2014

BACKGROUND: The ferronickel and rapid cooling slags used in present study are industrial wastes derived from a steel factory in Korea. These slags are used as almost road construction materials after magnetic separation. However, the use of slag to remove phosphorus from wastewater is still a relatively less explored. The objective of this work was to evaluate the feasibility of ferronickel slag (FNS) and rapid cooling slag (RCS) as sorbents for phosphorus removal in wastewater. METHODS AND RESULTS: Adsorption experiments were conducted to determine the adsorption characteristics of the FNS and RCS for the phosphorus. Adsorption behaviour of the phosphorus by the FNS and RCS was evaluated using both the Freundlich and Langmuir adsorption isotherm equations. FNS and RCS were divided into two sizes as effective sizes. Effective sizes of FNS and RCS were 0.5 and 2.5 mm, respectively. The adsorption capacities (K) of the phosphorus by the FNS and RCS were in the order of RCS 0.5 (0.5105) > RCS 2.5 (0.3572) ${\gg}$ FNS 2.5 (0.0545) ${\fallingdotseq}$ FNS 0.5 (0.0400) based on Freundlich adsorption isotherm. The maximum adsorption capacities (a; mg/kg) of the phosphorus determined by the Langmuir isotherms were in the order of RCS 0.5 (3,582 mg/kg) > RCS 2.5 (2,983 mg/kg) > FNS 0.5 (320 mg/kg) ${\fallingdotseq}$ FNS 2.5 (187 mg/kg). RCS 0.5 represented the best sorbent for the adsorption of phosphorus. In the experiment, the Langmuir model showed better fit with our data than the Freundlich model. CONCLUSION: This study indicate that the use of RCS in constructed wetlands or filter beds is a promising solution for phosphorus removal via adsorption and precipitation mechanisms.

• Journal of Soil and Groundwater Environment
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• v.7 no.4
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• pp.68-76
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• 2002

In this study, we have investigated the geochemical behavior and fate of heavy metals in acid rock drainage (ARD). The ARD was collected from the area of the former Dongrae pyrophyllite mine. The Dongrae Creek waters were strongly acidic (pH : 2.3~4.2) and contained high concentrations of $SO_4$, Al, Fe, Mn, Pb, Cu, Zn, and Cd, due to the influence of ARD generated from weathering of pyrite-rich pyrophyllite ores. However, the water quality gradually improved as the water flows downstream. In view of the change of mole fractions of dissolved Fe, Al and Mn, the generated ARD was initially both Fe- and AA-ich but progressively evolved to more Al-rich toward the confluence with the uncontaminated Suyoung River. As the AR3 (pH 2.3) mixed with the uncontaminated waters (pH 6.5), the pH increased up to 4.2, which caused precipitation of $SO_4$-rich Fe hydroxysulfate as a red-colored, massive ferricrete precipitate throughout the Dongrae Creek. Accompanying the precipitation of ferricrete, the Dongrae Creek water progressively changed to more Al-rich toward downstream sites. At the mouth of the Dongrae Creek, it (pH 3.4) mixed with the Suyoung River (pH 6.9), where pH increased to 5.7, causing precipitation of Al hydroxysulfate (white precipitates). Neutralization of the ARD-contaminated waters in the laboratory caused the successive formation of Fe precipitates at pH<3.5 and Al precipitates at higher pH (4~6). Manganese compounds were precipitated at pH>6. The removal of trace metals was dependent on the precipitation of these compounds, which acted as sorbents. The pHs for 50% sorption ($pH_{50}$) in Fe-rich and Al-rich waters were respectively 3.2 and 4.5 for Pb, 4.5 and 5.8 for Cu, 5.2 and 7.4 for Cd, and 5.8 and 7.0 for Zn. This indicates that the trace metals were sorbed preferentially with increasing pH in the general order of Pb, Cu, Cd, and Zn and that the sorption of trace metals in Al-rich water occurred at higher pH than those in Fe-rich water. The results of this study demonstrated that the partitioning of trace metals in ARD is not only a function of pH, but also depends on the chemical composition of the water.

• Journal of the Mineralogical Society of Korea
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• v.22 no.3
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• pp.177-189
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• 2009

Iron (oxyhydr)oxides commonly form as secondary minerals of high reactivity and large surface area resulting from alteration and weathering of primary minerals, and they are efficient sorbents for inorganic and organic contaminants. Accordingly, they have a great potential in industrial applications and are also of substantial interest in environmental sciences. Goethite (${\alpha}$-FeOOH) is one of the most ubiquitous and stable forms of iron (oxyhydr)oxides in terrestrial soils, sediments, and ore deposits, as well as a common weathering product in rocks of all types. This study focused on adsorption reaction as a main mechanism in scavenging arsenic using goethite. Goethite was synthesized in the laboratory to get high purity, and a variety of mineralogical and physicochemical features of goethite were measured and related to adsorption characteristics of arsenic. To compare differences in adsorption reactions between arsenic species, in addition, a variety of experiments to acquire adsorption isotherm, adsorption edges, and adsorption kinetics were accomplished. The point of zero charge (PZC) of the laboratory-synthesized goethite was measured to be 7.6, which value seems to be relatively higher, compared to those of other iron (oxyhydr)oxides. Its specific surface area appeared to be $29.2\;m^2/g$ and it is relatively smaller than those of other (oxyhydr)oxides. As a result, it was speculated that goethite shows a smaller adsorption capacity. It is likely that the affinity of goethite is much more larger for As(III) (arsenite) than for As(V) (arsenate), because As(III) was observed to be much more adsorbed on goethite than As(V) in equivalent pH conditions. When the adsorption of each arsenic species onto goethite was characterized in various of pH, the adsorption of As(III) was largest in neutral pH range (7.0~9.0) and decreased in both acidic and alkaline pH conditions. In the case of As(V), the adsorption appeared to be highest in the lowest pH condition, and then decreased with an increase of pH. This peculiarity of arsenic adsorption onto goethite might be caused by macroscopic electrostatic interactions due to variation in chemical speciation of arsenic and surface charge of goethite, and also it is significantly affected by change in pH. Parabolic diffusion model was adequate to effectively evaluate arsenic adsorption on goethite, and the regression results show that the kinetic constant of As(V) is larger than that of As(III).

• Korean Chemical Engineering Research
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• v.50 no.3
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• pp.492-498
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• 2012

In this study, hydrodynamics such as solid circulation rate and voidage in the desulfurizer and the reaction characteristics of Zn-based solid sorbents were investigated using lab-scale high pressure and high temperature desulfurization process. The continuous HGD (Hot Gas Desulfurization) process consist of a fast fluidized bed type desulfurizer (6.2 m tall pipe of 0.015 m i.d), a bubbling fluidized bed type regenerator (1.6 m tall bed of 0.053 m i.d), a loop-seal and the pressure control valves. The solid circulation rate was measured by varying the slide-gate opening positions, the gas velocities and temperatures of the desulfurizer and the voidage in the desulfurizer was derived by the same way. At the same gas velocities and the same opening positions of the slide gate, the solid circulation rate, which was similar at the temperature of $300^{\circ}C$ and $550^{\circ}C$, was low at those temperatures compared with a room temperature. The voidage in the desulfurizer showed a fast fluidized bed type when the opening positions of the slide gate were 10~20% while that showed a turbulent fluidized bed type when those of slide gate were 30~40%. The reaction characteristics of Zn-based solid sorbent were investigated by different desulfurization temperatures at 20 atm in the continuous operation. The $H_2S$ removal efficiency tended to decrease below the desulfurization temperature of $450^{\circ}C$. Thus, the 10 hour continuous operation has been performed at the desulfurization temperature of $500^{\circ}C$ in order to maintain the high $H_2S$ removal efficiency. During 10 hour continuous operation, the $H_2S$ removal efficiency was above 99.99% because the $H_2S$ concentration after desulfurization was not detected at the inlet $H_2S$ concentration of 5,000 ppmv condition using UV analyzers (Radas2) and the detector tube (GASTEC) which lower detection limit is 1 ppmv.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• KSCE Journal of Civil and Environmental Engineering Research
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• v.29 no.3B
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• pp.303-310
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• 2009

Natural zeolite is widely used as sorbents and bio-media materials because it is cheap as well as it has efficient porous structures and large cation exchange. In this study, the effect of metal cations $(Na^+,\;Ca^{2+},\;Mg^{2+},\;Al^{3+})$ adsorbed to natural zeolite on the microorganism attachment was investigated. Metal-modified zeolites (MMZ) were prepared with 0.01 M, 0.02 M and 0.1 M NaCl, $CaCl_2$, $MgCl_2$ and $AlCl_3$ solutions respectively, which concentrations were equivalent to 10%, 20% and 100% of cation exchange capacity (CEC) of natural zeolite. Pseudomonas putida was used as microorganism which was cultivated in Beef Extract Medium at $26^{\circ}C$. The microorganism attachment to MMZ was increased more than natural zeolite. The amount of bacterial adhesion to MMZ and natural zeolite were $Mg^{2+}>natural>Na^+>Al^{3+}>Ca^{2+}$ under 10% of CEC, $Mg^{2+}>Ca^{2+}>Al^{3+}>natural>Na^+$ under 20% of CEC and $Ca^{2+}>Mg^{2+}>natural>Al^{3+}>Na^+$ under 100% of CEC. Especially, Mg-modified zeolite (Mg-MZ) showed the highest amount of bacterial adhesion, which increased the microorganism attachment 60% higher than natural zeolite under 10% of CEC. However, the amount of bacterial adhesion was decreased as the concentration of metal cations modified to zeolite were increased, showing that the increased amounts were 60% under 10% of CEC, 50% under 20% of CEC and 10% under 100% of CEC in Mg-MZ. Additionally, the effect of $Mg^{2+}$ in solution on the bacterial adhesion was investigated in order to compare it with the effect of $Mg^{2+}$ adsorbed to zeolite. The maximum quantity of bacterial adhesion to Mg-MZ was not different from the amount of microorganism attachment to the natural zeolite when $Mg^{2+}$ solution was added.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.124-134
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• 2019

An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

• Economic and Environmental Geology
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• v.56 no.2
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• pp.125-138
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• 2023

Most of previous cesium (Cs) sorbents have limitations on the treatment in the large-scale water system having low Cs concentration and high ion strength. In this study, the new Cs sorbent that is eco-friendly and has a high Cs removal efficiency was developed by improving the coal mine drainage treated sludge (hereafter 'CMDS') with the addition of Na and S. The sludge produced through the treatment process for the mine drainage originating from the abandoned coal mine was used as the primary material for developing the new Cs sorbent because of its high Ca and Fe contents. The CMDS was improved by adding Na and S during the heat treatment process (hereafter 'Na-S-CMDS' for the developed sorbent in this study). Laboratory experiments and the sorption model studies were performed to evaluate the Cs sorption capacity and to understand the Cs sorption mechanisms of the Na-S-CMDS. The physicochemical and mineralogical properties of the Na-S-CMDS were also investigated through various analyses, such as XRF, XRD, SEM/EDS, XPS, etc. From results of batch sorption experiments, the Na-S-CMDS showed the fast sorption rate (in equilibrium within few hours) and the very high Cs removal efficiency (> 90.0%) even at the low Cs concentration in solution (< 0.5 mg/L). The experimental results were well fitted to the Langmuir isotherm model, suggesting the mostly monolayer coverage sorption of the Cs on the Na-S-CMDS. The Cs sorption kinetic model studies supported that the Cs sorption tendency of the Na-S-CMDS was similar to the pseudo-second-order model curve and more complicated chemical sorption process could occur rather than the simple physical adsorption. Results of XRF and XRD analyses for the Na-S-CMDS after the Cs sorption showed that the Na content clearly decreased in the Na-S-CMDS and the erdite (NaFeS₂·2(H₂O)) was disappeared, suggesting that the active ion exchange between Na⁺ and Cs⁺ occurred on the Na-S-CMDS during the Cs sorption process. From results of the XPS analysis, the strong interaction between Cs and S in Na-S-CMDS was investigated and the high Cs sorption capacity was resulted from the binding between Cs and S (or S-complex). Results from this study supported that the Na-S-CMDS has an outstanding potential to remove the Cs from radioactive contaminated water systems such as seawater and groundwater, which have high ion strength but low Cs concentration.