• Analytical Science and Technology
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• v.23 no.3
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• pp.240-246
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• 2010

A technique for the determination of trace Cu(II) in various real samples by FAAS after the column preconcentration onto p-dichlorobenzene-SA adsorbent, which is microcrystalline p-dichlorobenzene loaded with salicylaldoxime (SA) has been developed. Several experimental conditions such as pH of the sample solution, the amount of chelating agent salicylaldoxime, the amount of adsorbent p-dichlorobenzene-SA, and flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. $CN^-$ interfered more seriously than any other ions. However, the interference by $1\;{\mu}g\;mL^{-1}\;CN^-$ could be overcome completely by controlling the concentration of Ni(II) to $20\;{\mu}g\;mL^{-1}$. The linear range, correlation coefficient ($R^2$) and detection limit obtained by this technique were $3.0\sim100\;ng\;mL^{-1}$, 0.9901, and $3.1\;ng\;mL^{-1}$, respectively. For validating this technique, the aqueous samples (wastewater, reservoir water and stream water) and the food samples (orange juice, fresh egg and skim milk) were used. Recovery yields of 93~104% were obtained. These measured mean values were not differents from ICP-MS data at 95% confidence level. The good results were obtained from the experiments using the rice flour certified reference material (CRM) sample. Based on the experimental results, it was found that this technique could be applied to the preconcentration and determination of Cu(II) for various real samples.

• Journal of the Korean Chemical Society
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• v.50 no.1
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• pp.23-31
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• 2006

carbon modified methods were used for the preconcentration and determination of copper in some real samples using the flame atomic absorption spectrometry. The copper ions was adsorbed quantitatively on the activated carbon due to their complexation with 4- amino-2, 3-dimethyl-1-phenyl-3-pyrazoline (ADMPP) or 4-(4- methoxybenzylidenimin) thiophenole (MBITP). The adsorbed copper on solid phase was eluted quantitatively using small amount of nitric acid. The influence of important parameters including pH, amount of carrier, flow rate, amount of activated carbon and type and concentration of eluting agent for obtaining maximum recovery were investigated. The methods based on ADMPP and MBITP at optimum conditions is linear over concentration range of 0.05-1.5 g mL-1 and 0.05-1.2 g mL-1 of copper with correlation coefficient of 0.9997 and 0.9994 and both detection limit of 1.4 ng mL-1, respectively. The preconcentration leads to enrichment factor of 310 and break through volume of 1550 mL for both ligands. The method has a good tolerance limit of interfering ion and a selectivity that has been successfully applied for the determination of copper content in real sample such as tap, spring, river and waste water.

• Journal of the Korean Chemical Society
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• v.41 no.7
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• pp.337-342
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• 1997

Acryloylmethylbenzo-15-crown-5 was prepared from the reaction of 4'-hydroxymethylbenzo-15-crown-5 with acryloyl chloride. And, poly(acryloylmethylbenzo-15-crown-5) [poly(AMB15C5)] was synthesized by radical polymerization using AIBN as initiator in benzene. Coated wire lead(II) ion-selective electrodes ($Pb^{2+}$-CWISEs) using either poly(AMB15C5) or B15C5 as neutral carrier were prepared, respectively. $Pb^{2+}$-CWISEs gave linear responses with slopes of 28$\pm$ 1mV per decade within the concentration range of $10^{-5} M{\sim}10^{-1}$ M, respectively. Also, the detection limits were $10^{-6}$ M and response times were either 3 or 5 min. for B15C5 and poly(AMB15C5), respectively. $Pb^{2+}$-CWISE base on B15C5 was rather unstable than poly(AMB15C5)'s due to solubility of the B15C5 in water. The selectivity coefficients of a variety of interfering ions such as $Mg^{2+},\; Ca^{2+},\; Co^{2+},\; Ni^{2+},\; Cu^{2+},\; Zn^{2+}$ and $Cd^{2+}$ were small ($10^{-4}{\sim}10^{-5}$), while those of $Na^+$ and $K^+$ were large (0.1∼0.01). In addition, the electrode responses depended upon the pH of test solution and the composition of the membrane. In the range pH 3∼6 of test solution, potentials of Pb2+-CWISEs were hardly changed. The optimal contents of B15C5 and poly(AMB15C5) were 7.7 wt% and 13.1 wt%, respectively.

• Analytical Science and Technology
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• v.8 no.1
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• pp.63-68
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• 1995

For the preparation of pH-selectrode, tribenzylamine, polyvinylchloride, dioctylphthalate, sodium tetraphenylborate and tetrahydrofuran were mixed with 0.02, 0.62, 1.34, 0.02g and 10ml respectively, and added 1g of acetylene black, graphite, silicon carbide or tungsten carbide respectively to improve electric conductivity. The selectrodes of seven kinds were shown linear to hydrogen ion in the range of pH 2 and 9. The best electric conductor for preparation of pH-selectrode based on tribenzylamine as neutral carrier was acetylene black and responded potential of the selectrode to hydrogen ion was shown the values near to theoretical Nernstian slope at $20^{\circ}C$. The interfering effects of the selectrode on hydrogen ion in the presence of alkali and alkaline earth metal ions were shown the better results with less error than glass electrode. The reproducibility and stability were good for use as a selectrode, especially in the presence of fluoride ion.

• Analytical Science and Technology
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• v.13 no.4
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• pp.466-473
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• 2000

The complex formation constants (${\beta}_{MLn}$) of potassium and various sodium-selective neutral carriers in solvent polymeric membranes have been determined using solvent polymeric membrane-based optodes and ion-selective electrodes (ISEs). Two different types of PVC-based membranes containing the H^+selective chromoionophore (ETH 5294) with and without a sodium ionophore (4-tert-bntylcalix[4]arenetetraacetic acid tetraethyl ester, ETH 2120, bis[(12-crown-4)methyl] dodecylmethylmalonate or monensin methyl ester) were prepared and their optical responses to either the changes in alkali metal cation (e.g., sodium and potassium) concentrations at a fixed pH (0.05 M Tris-HCl, pH 7.2) or varying pH at a fixed alkali metal cation concentration (0.1 M) were measured. The same type of membranes were also mounted in conventional electrode body and their potentiometric responses to varying pH at a fixed alkali metal cation concentration (0.1 M) were measured. The complex formation constants of the ligand could be calculated from the calibration plots of the relative absorbance vs. the activity ratios of cation and proton ($a_{M^+}/a_{H^+}$) and of the emf vs. pH. It was confirmed that the ratio values of the complex formation constants for the primary and interfering ions are closely related to the experimental selectivity coefficients of ISEs.

• Membrane Journal
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• v.31 no.2
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• pp.87-100
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• 2021

With a striking increase in the level of contamination and subsequent degradations in the environment, detection and monitoring of contaminants in various sites has become a crucial mission in current society. In this review, we have summarized the current research areas in membrane-based colorimetric sensors for trace detection of various molecules. The researches covered in this summary utilize membranes composed of cellulose fibers as sensing platforms and metal nanoparticles or fluorophores as optical reagents. Displaying decent or excellent sensitivity, most of the developed sensors achieve a significant selectivity in the presence of interfering ions. The physical and chemical properties of cellulose membrane platforms can be customized by changing the synthesis method or type of optical reagent used, allowing a wide range of applications possible. Membrane-based sensors are also portable and have great mechanical properties, which enable on-site detection of contaminants. With such superior qualities, membrane-based sensors examined in the researches were used for versatile purposes including quantification of heavy metals in drinking water, trace detection of toxic antibiotics and heavy metals in environmental water samples. Some of the sensors exhibited additional features like antimicrobial ability and recyclability. Lastly, while most of the sensors aimed for a detection enabled by naked eyes through rapid colour change, many of them investigated further detection methods like fluorescence, UV-vis spectroscopy, and RGB colour intensity.

• Analytical Science and Technology
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• v.15 no.5
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• pp.417-426
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• 2002

Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry (ICP-DRC-QMS) was characterized for the detection of the six naturally occurring calcium isotopes. The effect of the operating conditions of the DRC system was studied to get the best signal-to-noise ratio. This experiment shows that the potentially interfering ions such as $Ar^+$, ${CO_2}^+$, ${NO_2}^+$, $CNO^+$ at the calcium masses m/z 40, 42, 43, 44 and 48 were removed by flowing $NH_3$ gas at the rate of 0.7 mL/min $NH_3$ as reactive cell gas in the DRC with a RPq value (rejection parameter) of 0.6. The limits of detection for $^{40}Ca$, $^{42}Ca$, $^{43}Ca$, $^{44}Ca$, and $^{48}Ca$ were 1, 29, 169, 34, and 15 pg/mL, respectively. This method was applied to the determination of calcium in synthetic food digest samples (CCQM-P13) provided by LGC for international comparison. The isotope dilution method was used for the determination of calcium in the samples. The uncertainty evaluation was performed according to the ISO/GUM and EURACHEM guidelines. The determined mean concentration and its expanded uncertainty of calcium was ($66.4{\pm}1.2$) mg/kg. In order to assess our method, two reference samples, Riverine Water reference sample (NRCC SLRS-3) and Trace Elements in Water reference sample (NIST SRM 1643d), were analyzed.

• Journal of the Korean Chemical Society
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• v.44 no.5
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• pp.422-428
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• 2000

Optimum analytical conditions of the aluminium ion were established by flow injection analysis. Eriochrome Cyanine R(ECR) dye reacts with the aluminium ion at pH 6.0 to form a complex that exhibits maximum absorption at 535 nm. Reaction conditions including the mixing and the reaction coil length, the concentration and the pH of the buffer solutio, temperature, and injection loop volume were optimized to intro-duce this reaction into flow injection analysis. The results were as follows. A mixing coil length of 0.5 m and a reaction coil length of 4.0 m, the pH 6.0 and 1M of acetate buffer solution, the ECR concentration of 0.56 mM, the reaction temperature of 40$^{\circ}C$, the injection loop volume of 300${\mu}L$ were chosen as optimum conditions. Under these conditions the detection limit of the aluminiumion was less than 0.05 mg/L and the repeatability was better than 1%. A sampling frequency of 24 times for an hour was achieved. Interfering ions such as $F^-$, HP$O_4^{2-}$, $Fe^{2+}$, $Fe^{3+}$, $Mn^{2+}$, and other anions were tested, interference did not occur up to 1,000mg/L of ion concentration and up to 2,CO0mg/L of sulfate ion con-centration. This method was applied for the determination of aluminium ion in tap water and ground water of Jeonju and the Gochang area. The results showed that the aluminium residual in tap water of the Jeonju area was at a mean of 0.478mg/L and that in tap water of the Gochang area was at a mean of 0.278mg/L. Aluminium ion residual of the tap waters in the Jeonju area was higher level than that in the Gochang area. Aluminium residual in the ground water of the Jeonju area was 0.386 mg/L and was lower compared to 0.564 mg/L for the Gochang area.