• Analytical Science and Technology
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• v.36 no.6
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• pp.259-266
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• 2023

The demand for rare-earth elements (REEs) is increasing owing to their significance as prominent materials in electronics, high-tech industries, geological research, nuclear forensics, and environmental monitoring. In general, the utilization of REEs in various applications requires the use of chromatographic techniques to separate individual elements. However, REEs have similar physicochemical properties, which makes them difficult to separate. Recently, several studies have examined the separation of REEs using LN resin as the stationary phase and aqueous nitric acid and hydrochloric acid solutions as eluents. Using this method, light REEs have been separated using dilute acid solutions as the eluent, whereas heavy REEs are separated using solutions with high acid concentrations. To increase the separation resolution between different REEs, either the column length or resin size is changed. In addition, the suggested methods are implemented to decrease the analysis time. This review presents technical information on the chromatographic separation of REEs using the LN resin and discusses the optimal experimental conditions.

• Resources Recycling
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• v.25 no.4
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• pp.60-67
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• 2016

This study was conducted to establish the adsorption-desorption mechanism and the optimum condition of chromatographic operation for separations of heavy rare earth elements (Gd, Tb, Dy) using a p507-containing resin. By employing Langmuir and Freundlich isotherm together with pseudo first and second order kinetics, absorption-desorption reaction mechanism was investigated. Langmuir and Freundlich isotherm was applied under assumption that adsorption reaction occurs in form of monolayer, and because the result was identical to the assumption, now we know adsorption of heavy rare earth elements occurs in form of monolayer. Concerning the pseudo first and second order kinetic, the pseudo second order seemed to be more suitable to represent heavy rare earth element adsorption mechanism. By using the extraction chromatography to separate heavy rare earth elements, ${\alpha}^{Tb}_{Gd}=1.24$, and ${\alpha}^{Dy}_{Tb}=1.03$ were confirmed in eluent HCl 0.25 M which indicates almost perfect separations of three elements. Furthermore, as concentrations of eluent became higher, the resolution value decreased and the elution area got shortened.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.135-139
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• 1999

A new effective and economic method was developed, removing interferences such as chlorophyll and lipid from leaves with small amounts of reagents and solvents in order to analyse PAHs(Polycyclic Aromatic Hydrocarbons). The extract from a soxhlet containing $4{\sim}5g$ of leaves and 100ml of dichlormethane and refluxed for 20 hrs was concentrated and eluted with 60ml of a hexane:dichloromethane (1:1) mixture through a column of 9mm wide inner diameter and 130mm long, packed from the bottom with 2.5g of $Al_2O_3$, 1.5g of $SiO_2$and 2g of anhydrous $Na_2SO_4$. The eluent was concentrated and loaded on a GPC column of 20mm wide inner diameter and 280mm long, packed with 12g of Bio-beads. The column was washed with 37ml of the hexane:dichloromethane(1:1) mixture. Another 43ml of the mixture was eluted as a PAH fraction and collected. This eluent was concentrated under gentle nitrogen to $50{\mu}l$ and analysed using GC-MS. The recoveries, obtained by comparing with the amounts of the internal standards of deuterated PAHs were $43.3{\sim}107.5%$(RSD $2.2{\sim}9.5%$).

• Analytical Science and Technology
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• v.15 no.4
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• pp.329-334
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• 2002

Tributyl phosphate(TBP) is used in solvent extraction process for radioactive waste. This compound may be degraded to dibutyl phosphate($DBP^-$), monobutyl phosphate($MBP^{2-}$) and ${PO_4}^{3-}$ by radioactive material. Amount of $DBP^-$ and $MBP^{2-}$ in TBP must be monitored because they production of these compounds means degradation of which leads to a decrease in the extraction yield. Retention behavior for $DBP^-$, $MBP^{2-}$, $F^-$, $Cl^-$, ${NO_2}^-$, ${NO_3}^-$, ${SO_4}^{2-}$ and ${PO_4}^{3-}$ are studied with AS4A-SC(Dionex) analytical column and $Na_2CO_3$/NaOH eluent by Ion chromatography. Optimum condition for these anions is 2 mM $Na_2CO_3$/1 mM NaOH eluent. All anions by this condition is well separated within 15min. Dynamic range is $10{\mu}g/mL$ - $100{\mu}g/mL$ for DBP and $5{\mu}g/mL$ - $50{\mu}g/mL$ for $MBP^{2-}$, respectively. The Detection limit for AS4A-SC are $1{\mu}g/mL$ for $DBP^-$ and $0.5{\mu}g/mL$ for $MBP^{2-}$ in this system with a $25{\mu}L$ sample loop.

• Korean Journal of Food Science and Technology
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• v.39 no.4
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• pp.360-365
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• 2007

The studies for the derivatization of 3-monochloropropane-1,2-diol (3-MCPD) were performed mainly as acylation with HFBI (heptafluorobutyrylimidazole), alkylation with PBA (phenylboric acid) and silylation with BSTFA (N,O-bis[trimethylsilyl]trifluoroacetamide). Also silylation with MTBSTFA(N-methyl-N-[tert.-butyldimethylsilyl] trifluoroacetamide) and acylation with MBTFA (N-Methyl-bis[trifluoro-acetamide]) were also considered. Except the TBDMS derivative of 3-MCPD, all the derivatives were detected well. The derivatives of 3-MCPD with HFBI, PBA and BSTFA showed below 10 ${\mu}g/kg$ which was sensitive enough to satisfy Korea maximum residue limit 0.3 mg/kg. Among the tested adsorbents, Extrelut20 and Florisil were evaluated as the proper adsorbents to eliminate the soy sauce matrix for 3-MCPD. Ethyl acetate was the most efficient eluent with good recovery rate. The desired surrogate compound and internal standard were 1,2-butanediol and 1,2-dibromo-3-chloropropane, respectively. The limit of detection for PB-MCPD and TMS-MCPD were 10.16 and 7.06 ${\mu}g/kg$ on GC/MSD, respectively. HFB-MCPD derivative showed the lowest detection limits 2.98 and 5.32 ${\mu}g/kg$ by GC/ECD and GC/MSD, respectively.

• Analytical Science and Technology
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• v.13 no.5
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• pp.601-607
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• 2000

Lanthanum has been used as one of the burnup monitor in spent nuclear fuel. $U_3Si/Al$ spent nuclear fuel contains small amount of La in high concentration of U and Al. Therefore, chemical separation of La is required to remove matrix elements. At first, ion chromatography (IC) and inductively coupled plasma systems were installed in radiation shielded glove box to handle the radioactive samples. Retention behavior of uranium, aluminum, lanthanum and some interesting fission products (Sr, Zr, Y, Mo, Ru, Pd, Rh, Cs, Ba, Ce, Pr, Nd, Sm, Eu and Cd) was investigated using the CG10 column and ${\alpha}$-HiBA eluent. As all elements were eluted earlier than lanthanum in 0.2 M ${\alpha}$-HiBA eluent, a portion of U and Al was directly passed to waste using a three way valve between the column and the nebulizer. Thus it was possible to determine the lanthanum in a high concentration of U and Al matrix. Retention time of La was about 12 minutes in this separation condition. Optimum range for the determination of La in $U_3Si/Al$ spent nuclear fuel was $1-10{\mu}g/L$ (ppb) with this system and detection limit was $0.25{\mu}g/L$ in case of $200{\mu}L$ of sample volume.

• Analytical Science and Technology
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• v.13 no.5
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• pp.584-591
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• 2000

The separation of Nd from the simulated $U_3Si/Al$ spent fuel solution with sequential two-step anion exchange separation has been studied. To prepare the simulated $U_3Si/Al$ spent nuclear fuel, unirradiated $U_3Si/Al$ whose composition consists of small $U_3Si$ particle dispersed in an Al matrix with Al cladding was dissolved with a mixture of 4 M HCl and 10 M $HNO_3$ and 8 or 15 fission product elements were added to the dissolved solution. The trace amount of silica in the solutions was removed by evaporating to dryness with HF and the U was adsorbed on the first anion exchange resin. Neodymium can be purely isolated from the fission product elements with a methanol-nitric acid eluent using the second anion exchange resin. A large excess of Al didn't influence on the elution velocity of Nd, but reduced the eluted contents of Nd, Al, Eu, Gd, Sm and Sr, A large amount of Al was removed first from the column with 3 mL of loading solution (0.8 M $HNO_3$/99.8% MeOH) before Nd elution by the eluent [0.04 M $HNO_3$-99.8% MeOH(1:9)]. The recovery of Nd was more than 94%, regardless of Al contents. Taking the 9 to 13 mL fraction of eluate was effective to purely isolate Nd.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.17 no.5
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• pp.368-372
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• 1984

This paper deals with a rapid method for determination of ATP and its related compounds in fish and shellfish products using high performance liquid chromatography(HPLC). The HPLC used is a HPLC/ALC-224 equiped with UV-spectrophotometer (254 nm) as detector and integrator (Yanagimoto system-1000). The column used is a stainless steel tubing ($30.0\;cm{\times}3.9\;mm\;i.d.$) packed with ${\mu}-Bon-dapak\;C_{18}$. A mixture of $1\%$ triethylamine-phosphoric acid(pH6.5) was used as an eluent and the flow rate of the eluent was controlled at 2 ml/min. For the separation of ATP and its related compounds, a standard mixture of ATP, ADP, AMP, IMP, inosine and hypoxanthine was subjected to HPLC under the above mentioned conditions. Six peaks were obtained with retention times within 20 min, and elution order were hypoxanthine, IMP, inosine, AMP, ADP and ATP. But 5'-IMP and 5'-GMP fractions were not separated by this method. In generally, IMP content in boiled-dried fish and shellfish products purchased from the market was comparatively higher than that of other nucleotides. Especially, boiled-dried big eye herring marked higher value in IMP content than other boiled-dried ones. Hypoxanthine and inosine were major components of ATP-related compounds in dried products and seasoned-dried ones. And IMP content in seasoned-dried products was higher than that of dried ones. This fact is suggested that a part of IMP in seasoned-dried ones was derived from flavoring matter (MSG, 5'-IMP and 5'-GMP) which is added during the seasoning treatment.

• Journal of Korean Society of Forest Science
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• v.96 no.4
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• pp.408-413
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• 2007

The dried bark of Platycarya strobilacea were ground, extracted with 95% EtOH, concentrated, and one of EtOH extracts was fractionated with a series of n-hexane, dichloromethane and another was fractionated with a series of petroleumether, $Et_2O$, ethyl acetate on a separatory funnel. A portion of dichloromethane soluble was chromatographed on a Sephadex LH-20 column ($72.0{\times}5.0cm$) using EtOH-$CHCl_3$ (7:3, v/v) as eluent and A portion of $Et_2O$ soluble was chromatographed on a silica gel column ($42.0{\times}3.5cm$) using $CHCl_3$-MeOH (9:3, v/v) as eluent. The isolated compounds were identified by TLC, $^1H$-, $^{13}C$-NMR, HMBC and EI-MS. Two flavonoids and three flavonoid glycosides were isolated from the bark of P strobilacea. The structures were determined to quercetin (compound 1), myricetin (compound 2) as flavonol compounds and afzelin (compound 3), quercitrin (compound 4), myricitrin (compound 5) as flavonol glycosides, respectively, on the basis of spectrosopic data.

• KSBB Journal
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• v.11 no.6
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• pp.663-668
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• 1996

In the production of recombinant protein using E. coli, phage lysogen system can be usefully applied for simultaneously achieving protein production at high cell concentration and recovery by cell disruption in the same bioreactor. A major drawback of this system is that the intracellular product and complex broth components are mixed together in culture broth and hence purification efficiency is reduced. With the E. coli double-lysogen system, the expanded bed adsorption is very useful because the pretreatment processes in a routine bioseparation process can be done in a single column operation, and therefore may contribute towards lowering the operating cost of overall recovery/purification process. In the operation of EBA, it has been observed that the change in broth feed volume does not influence much the protein recovery in a tested range. The amount of protein adsorption per mL of resin was increased from $3.44{\times}106unit to 5.28{\times}106unit$ by doubling the column length. By two-fold increase of the column diameter, the ratio of protein concentration in eluent to that in feed was increased from 0.8 to 2.1. It is concluded from the present investigation that the increase of column length and diameter is necessary to enhance the protein adsorption amount per volume of resin and protein concentration in the eluent. The development of resins with various physical properties will be necessary for more extensive application of EBA.