• Journal of the Korean Chemical Society
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• v.33 no.1
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• pp.70-81
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• 1989

Reverse phase liquid chromatographic elution behaviors of salicylic acid and its derivatives were studied with classical and modern high-performance liquid chromatography(HPLC) using Amberlite XAD-4 and XAD-7 resin packed columns. Capacity factors(k') were determined in the comparatively high concentration(from 0. 010F to 0. 150F) of ferric nitrate-50% methanol solution to elucidate the elution behaviors with classical method. On the other hand, k's were measured in the various concentrations of methanol and ferric nitrate(from $2.5{\times}10^{-4}F\;to\;1.0{\times}10^{-3}F$) solution of pH 2. 25 and 293K with HPLC to explain the elution mechanism of them, and to find their optimum separation condition. As a result, it was found that log k's of salicylic acid and its derivatives were decreased with increasing the concentration of ferric ion, and the decreasing slopes of the compounds on the increasing ferric ion concentrations were related with each stability constant of ferric salicylates. Some isomers of derivatives of salicylic acid could be separated in the optimum condition.

• Analytical Science and Technology
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• v.13 no.3
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• pp.323-331
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• 2000

Two chelating resins, XAD-16-TAC and XAD-16-TAO were synthesized by Amberlite XAD-16 macroreticular resin with 2-(2-thiazolylazo)-p-cresol (TAC) and 4-(2-thiazolylazo)-orcinol (TAO) as functional groups. The sorption behaviour of Zr(IV), Th(IV) and U(VI) with two chelating resins were examined with respect to the effect of pH and masking agent by batch methods. It was obtained that the optimum pH was in the range of 5-6, and two chelating resins showed good separation efficiency of Zr(IV) or Th(IV) by using $NH_4F$ as a masking agent. Characteristics of desorption were investigated with 0.1-2 M $HNO_3$ as desorption agent. It was found that 2 M $HNO_3$ showed high desorption efficiency to most of metal ions except Zr(IV). XAD-16-TAC resin is applied to separation and preconcentration of trace Zr(IV) from mixed metal ions. Also, Th(IV) ion can be successfully separated from U(VI) and Zr(IV) ion by using XAD-16- TAO resin.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1293-1296
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• 2006

In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

• Analytical Science and Technology
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• v.6 no.5
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• pp.489-499
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• 1993

Some sorption behaviors of U(VI) ion on Arsenazo I-XAD-2 chelating resin were investigated. This chelating resin was synthesized by the diazonium coupling of Amberlite XAD-2 resin with Arsenzo I chelating reagent and characterized by elementary analysis method and IR spectrometry. The optimum conditions for the sorption of U(VI) ion were examined with respect to pH, U(VI) ion concentration and shaking time. Total sorption capacity of this chelating resin on U(VI) ion was 0.39mmol U(VI)/g resin in the pH range of 4.0~4.5. This chelating resin was showed increased sorption capacity on the increased pH value. It was confirmed that sorption mechanism of U(VI) ion on the Arsenazo I-XAD-2 chelating resin was competition reacting between U(VI) ion and $H^+$ ion. Breakthrough volume and overall capacity of U(VI) ion measured by column were was 600 ml and 0.38 mmol U(VI)/g resin, respectively. The desorption of U(VI) ion was showed recovery of 90~96% using 3M $HNO_3$ and 3M $Na_2CO_3$ as a desorption solution. The separation and concentration of U(VI) ion from natural water and sea water was performed successfully by Arsenazo I-XAD-2 chelating resin.

• Bulletin of the Korean Chemical Society
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• v.23 no.5
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• pp.693-698
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• 2002

A method has been described for the determination of Cu(Ⅱ), Pb(Ⅱ), Ni(Ⅱ), Cd(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ) by flame atomic absorption spectrometry (FAAS) after preconcentration on Amberlite XAD-16 resin, using hexamethyleneammonium-hexamethylenedithiocarbamate (HMA-HMDTC) as a chelating agent, and NH3/NH4Cl buffer solution (pH 9). Influences of various analytical parameters such as pH, concentration of nitric acid, amount of analytes, diverse ions and sample volume were investigated. The relative standard deviation (RSD) and the detection limit (LOD) were found in the range of 0.8-2.9% and 0.006-0.277 ㎍/mL,respectively. Recoveries obtained by the column method were quantitative ( >95%) at optimum conditions.The method was applied to the determination of some metal ions in seawater and wastewater samples. A high preconcentration factor (about 150 for seawater and 75 for wastewater samples) and simplicity are the main advantages of this suggested method.

• Journal of the Korean Chemical Society
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• v.31 no.1
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• pp.45-54
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• 1987

Dowex 1-X8 resin ion exchanged with calcon carboxylic acid (CCA-Dowex 1-X8) and 2-methyl-8-hydroxyquinoline(MHQ) impregnated-Amberlite XAD-4 resin (MHQ-XAD-4) were examined for the separation and preconcentration of ferric ion from the various matrices. The stabilities of these resins were investigated, and their capacities on ferric ion were also measured. The effect of pH on the adsorption of ferric ion and matrix ions, such as Al(Ⅲ) and Ca(Ⅱ), was investigated to determine the optimun pH ranges. Separation and preconcentration of iron in aluminium foil and mineral water samples were studied by elution method with these resin columns. The recovered ions by 10ml of 2F nitric acid was determined by flame atomic spectrophotometry. SP-Sephadex C-25 column was used to separate ferrous and ferric ion in mineral water by stepwise elution with ferrozine and 1 % ascorbic acid-ferrozine solution. The concentrated and separated each ion could be determined spectrophotometrically at the analytical wavelenth of Fe(Ⅱ)-ferrozine complex (562nm).

• Bulletin of the Korean Chemical Society
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• v.27 no.1
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• pp.77-81
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• 2006

The commercially available Amberlite XAD-2 and XAD-4 resins were modified with macrocyclic protoporphyrin IX (PPIX) or tetrakis(p-carboxyphenyl) porphyrin (TCPP) to enhance the adsorption capacity for phenol and chlorophenols. The chemically modified polymeric adsorbents (XAD-2+PPIX, XAD-2+TCPP, XAD-4+PPIX, and XAD-4+TCPP) were applied to the solid phase extraction as an adsorbent material for the preconcentration of phenol and chlorophenols in environmental waters. Generally, the synthesized adsorbents showed higher recoveries than underivatized adsorbents, XAD-2 and XAD-4, without matrix interferences. Especially, XAD-4+PPIX showed more than 90% recoveries for all compounds used in this study including hydrophilic phenol. The major factor for the increase of the adsorption capacity was the increase of $\pi$-$\pi$ interaction between adsorbents and samples due to the introduction of the porphyrin molecule. However, the breakthrough volumes and recovery values of the XADs+TCPP columns were slightly decreased for the bulky chlorophenols such as TCP and PCP. Using molecular mechanics methods, the structures of TCPP and PPIX were compared with that of porphine, the parent molecule of porphyrin. Four bulky p-carboxyphenyl groups of TCPP were torsional each other, thus the molecular plane of TCPP were not on the same level. In conclusion, the decrease of breakthrough volumes and recovery values of XADs+TCPP columns for bulky phenols can be explained by the steric hindrance of the $\pi$-$\pi$ interaction between porphyrin plane and the phenols.

• Advances in environmental research
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• v.6 no.4
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• pp.301-315
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• 2017

An Amberlite XAD-4 resin impregnated with di(2-ethylhexyl)phosphoric acid was prepared and its adsorption-desorption behaviors with Sr(II) ions under various conditions was examined. The resin was characterized by fourier transform infrared and thermal analysis techniques. The effects contact time, temperature, pH, interfering ions and eluants were studied. Results showed that adsorption of Sr (II) well fitted with pseudo-second-order kinetic model. The equilibrium adsorption data of Sr (II) on the impregnated resin were analyzed by Jossens, Weber-van Vliet, Redlich-Peterson and Fritz-Schlunder models to find out desirable equilibrium condition. Among them, the Fritz-Schlunder model best fitted to the experimental data. The maximum sorption capacity of impregnated resin amounted to 0.45 mg/ g at pH 8.0 and $20^{\circ}C$.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.461-468
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• 2018

A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

• YAKHAK HOEJI
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• v.45 no.5
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• pp.455-459
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• 2001

Melandrii Herba has been used for tympanitis, sore throat, dysentery and dehumidifying diuretic. From the BuOH fraction of methanol extracts, three ecdysteroids (ecdysterone, ecdysterone 22-acetate and inokosterone) were isolated by column chromatography using Amberlite XAD-4, ODS and Sephadex LH-20 gel and by HPLC method. The structures of these compounds were identified on the basis of spectroscopic methods.