• 분석과학
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• 제16권2호
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• pp.110-116
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• 2003

사용 후 핵연료의 화학특성 연구를 위하여 요오드의 분리와 정량에 관한 연구를 수행하였다. 사용 후 핵연료를 용해시키는 과정에서 핵연료 중에 CsI로 존재하는 요오드가 $I_2$로 산화되어 휘발되지 않도록 질산과 염산의 혼합산 (80:20 mol%)을 이용하여 비휘발성 ${IO_3}^-$­로 안정화시켰다. 2.5 M $HNO_3$ 매질에서 $NH_2OH{\cdot}HCl$을 이용하여 $I_2$로 환원시킨 후 사염화탄소로 추출하여 우라늄과 핵분열생성물로부터 분리, 회수하였다. 0.1 M $NaHSO_3$을 사용하여 요오드를 역추출하였으며 수용액층으로 회수된 요오드를 이온 크로마토그래피로 정량하였다. 방사성 물질 분석에 적합한 이온 크로마토그래피/차폐 시스템을 구성하였으며 42,000~44,000 MWd/MtU 의 연소도를 갖는 사용후핵연료를 대상으로 요오드를 분석한 결과 Origin 2 연소도 전산코드에 의한 계산결과인 $324.5{\sim}343.6{\mu}g/g$와는 -8.3~-0.5%의 편차를 나타내었다.

• 한국식품조리과학회지
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• 제24권3호
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• pp.349-357
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• 2008

In an effort to augment extractability of carnosine and anserine at the levels of pro-oxidants such as iron and protein in Tuna boiled extracts(Skipjack, Yellowfin and Bigeye), we assessed the effects of heated and ion exchange chromatography(IEC) and ultrafiltration(UF) using a MW 500 cut-off(500 MWCO). We also evaluated the antioxidant activity of these extracts processed as free radical scavengers and reducing agents. Tuna boiled extracts of dark and ordinary muscle protein and total iron were reduced, whereas carnosine and anserine concentrations and antioxidant activity were increased. The carnosine and anserine concentrations of the ion exchange and permeate UF(IEC-UF) extracts were higher than those observed in the heated and permeate UF(heat-UF), whereas the protein and total iron contents were lower than that observed in the heat-UF. The quantity of carnosine and anserine in ordinary muscle was higher than that detected in dark muscle. HPLC analysis and SDS-PAGE were shown to removes the effect of UF on high molecular weight impurities in the tuna boiled extracts. The major free amino acids(FFAs) from Skipjack, Yellowfin and Bigeye tuna IEC-UF extracts were anserine, histidine and carnosine. These three peptides constituted more than 80～85%. of the detected amino acid. The IEC-UF treated ordinary muscle extracts evidenced the highest levels of DPPH radical scavenging activity and the highest levels of reducing power among the various extracts. The IEC-UF extracts evidenced a DPPH radical scavenging effect equal to that of 1mM ascorbic acid.

• 대한화학회지
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• 제41권11호
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• pp.612-638
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• 1997

모나자이트광 속에 포함되어 있는 회토류 원소들을 이온교환수지를 이용하여 분리 회수 하는 방법에 관해 연구하였다. 이온교환수지로는 양이온교환수지와 음이온교환수지를 사용하고, 용리액으로는 EDTA, DTPA, IMDA, Ln-EDTA 용액을 사용하였으며, 양이온교환수지는 retaining 이온 곧 $H^+, Zn^{2+}, Fe^{3+}, Al^{3+}, Cu^{2+}, NH^+_4$으로 치환된 수지를 사용하였다. 음이온교환수지는 EDTA로 치환된 수지에 Ln-EDTA착물을 흡착시켜 분리하였다. 여러 가지 회토류 원소 중에서 선택적으로 한 원소만 분리하기 위해 용리액으로 Ln-EDTA를 사용하였으며, 수지통의 크기 변화와 여러 가지 용리형태의 메카니즘, 그리고 다량의 회토류 원소를 분리 회수하는 방법 등에 관해 연구하였다.

• 대한화학회지
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• 제38권9호
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• pp.660-666
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• 1994

이웃하는 란탄족 원소의 분리에서 온도와 흐름속도의 영향을 치환크로마토그래피로 연구하였다. 일렬로 연결된 두 컬럼에 Amberlite 120 양이온 교환수지를 채워서 충전용과 분리용으로 나누어 사용하였다. 보유이온은 $H^+$을, 흐름용액은 0.012M과 0.015M의 EDTA 용액을 사용하였다. 실험중에는 관의 온도를 90$^{\circ}C$로 유지하였으며 이온교환수지 관 속에 생기는 기포를 줄이기 위해 일정한 압력을 걸었다. 용출액은 ICP-AES로 직접 분석하였다. 이 실험에서 란탄족 원소쌍 La: Ce, Ce :Pr, Pr: Nd에 대한 분리인자는 각각 4.6, 2.8, 1.9이었으며 이것은 25$^{\circ}C$에서 이론적으로 얻은 것보다 큰 값이다. 흐름속도를 2.5 ml/min에서 1.5 ml/min로 줄이면 이론단해당높이(HETP)도 1.60 cm에서 0.88 cm로 줄었다. 따라서 용리액의 흐름속도를 줄이고 온도를 높이므로써 분리효율을 증가시킬 수 있었다. 이 실험에서 99.9% 이상의 순수 란탄족 원소에 대한 회수율은 49∼77%이었다.

• Bulletin of the Korean Chemical Society
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• 제30권4호
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• pp.783-786
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• 2009

Thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and ion chromatography(IC) were employed to analyze the thermal behavior of $Li_xCoO_2$ cathode material of lithium ion battery. The mass loss peaks appearing between 60 and 125 ${^{\circ}C}$ in TGA and the exothermic peaks with 4.9 and 7.0 J/g in DSC around 75 and 85 ${^{\circ}C}$ for the $Li_xCoO_2$ cathodes of 4.20 and 4.35 V cells are explained based on disruption of solid electrolyte interphase (SEI) film. Low temperature induced HF formation through weak interaction between organic electrolyte and LiF is supposed to cause carbonate film disruption reaction, $Li_2CO_3\;+\;2HF{\rightarrow}\;2LiF\;+\;CO_2\;+\;H_2O$. The different spectral DSC/TGA pattern for the cathode of 4.5 V cell has also been explained. Presence of ionic carbonate in the cathode has been identified by ion chromatography and LiF reported by early researchers has been used for explaining the film SEI disruption process. The absence of mass loss peak for the cathode washed with dimethyl carbonate (DMC) implies ionic nature of the film. The thermal behavior above 150 ${^{\circ}C}$ has also been analyzed and presented.

• 대한화학회지
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• 제39권4호
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• pp.288-293
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• 1995

chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid)를 착화제로 이용한 붕소에 대한 분리 정량을 이온쌍 액체 크로마토그래피로 연구하였다. 이동상$(MeOH\; 61{\%},\;H_2O\;39{\%}$, 인산완충용액 pH=8.5)에 tetrabutylammonium bromide를 첨가하므로서 붕소-chromotropic acid 착물과 chromotropic acid를 poly(styrene-devinylbenzene) 역상컬럼(PRP-1, 15 $cm{\times}4.6$ mm i.d.) 상에서 분리할 수 있었으며, 또한 시료 용액중에 0.1 M의 tetrabutylammonium bromide를 첨가하므로 붕소와 chromotropic acid간의 착물형성을 촉진시켜 감도를 높일수가 있었다. 0.5~1000 ${\mu}g/L$ 농도범위에서 좋은 직선성을 나타내었고 검출 한계는 0.5 ${\mu}g/L$ (S/N=2)이었다. 제안된 방법으로 시판용 시약, $Na_2SO_4,\; NaOH,\; KCl$에 있는 미량의 붕소를 정량하였다.

• 한국환경농학회지
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• 제34권3호
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• pp.230-237
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• 2015

BACKGROUND: To identify the sources of inaccuracy in LC/MS/MS methods used in the routine quantitation of small molecules are described and discussed. METHODS AND RESULTS: Various UPLC coupled to triple quadrupole mass spectrometer and time of flight (TOF) were used to identify the potential sources of inaccuracy and inducing the pitfalls of qualification and quntitation during the veterinary drug residue analysis. Some of stable isotope labelled veterinary drugs, which were used as internal standards, presented "cross-talk", regardless of manufactures of mass spectrometer and types of spectrometer. Group of sulfonamides also presented inaccuracy qualification and quantitation due to the multi-residue analytical method with the same fragment ions at the close retention times. CONCLUSION: The phenomena of "cross-talk" occurring between subsequently monitored transition from stable isotope labelled and isotope non-labelled authentic chemical were identified. To prevent errors and achieve more accurate data during the analysis of small molecules by LC/MS/MS SRM method, Followings should be taken care of and kept checking; purity and concentration of stable isotope as an internal standard, prevention of carry-over during the separation in column, minimizing the ion suppression by matrix effect, identification of retention time, precursor ion and product ion, and full knowledge of data processing including smoothing and peak integration.

• Archives of Pharmacal Research
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• 제22권3호
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• pp.288-293
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• 1999

Postabsorptive serum iron level was determined after oral administration of the compounds to human. In serum and whole blood, $Fe^{3+}$ was measured by ion chromatography (IC) using a pyridine-2,6-dicarboxylic acid (PDCA) as an eluent. The serum sample solutions were pretreated with I N HCI and 50% TCA. The whole blood sample solutions were treated with 3 N HCI for 30 min at $125^{\circ}C$. The limit of detection (LOD) of the IC technique is $0.2 {\mu}M$ for$Fe^{2+}$and 0.1 $\mu$M for $Fe^{3+}$. The area under concentration (AUC) can be obtained by the above analytical condition. In addition, to compare the stability of $Fe^{2+}$ to that of $Fe^{3+}$ in pharamaceutical preparations, accelerated stability test was carried out. After storing the samples under $40^{\circ}C$, 75%RH in light-resistant container for various time intervals, the contents of iron of different valencies were determined separately by the IC technique and the change and/or the interchange of among those iron species in preparations was investigated. Iron raw materials are stable, but $Fe^{2+}$ in$Fe^{3+}$ source materials was slightly converted to $Fe^{3+}$ by oxidation. $Fe^{2+}$ in$Fe^{3+}$ source raw materials and $Fe^{3+}$ in $Fe^{2+}$ raw materials are determined as impurities. Therefore, IC technique is found to be an appropriate method for comparative evaluation of dissimilar bioavailability of $Fe^{2+}$ and $Fe^{3+}$, stability of $Fe^{2+}$ and $Fe^{3+}$ raw materials and preparations.

• Biotechnology and Bioprocess Engineering:BBE
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• 제6권2호
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• pp.144-149
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• 2001

For the production and purification of a single chain human insulin precursor, four types of fusion peptides $\beta$-galactosidase (LacZ), maltose binding protein (MBP), glutathione-S-transferase (GST), and (His)(sub)6-tagged sequence (HTS) were investigated. Recombinant E. coli harboring hybrid genes was cultivated at 37$\^{C}$ for 1h, and gene induction occurred when 0.2mM of isopropyl-D-thiogalactoside (IPTG) was added to the culture broth, except for E. coli BL21 (DE3) pLysS harboring a pET-BA cultivation with 1.0mM IPTG, followed by a longer than 4h batch fermentation respectively. DEAE-Sphacel and Sephadex G-200 gel filtration chromatography, amylose affinity chromatography, glutathione-sepharose 4B affinity chromatography, and a nickel chelating affinity chromatography system as a kind of immobilized metal ion affinity chromatography (IMAC) were all employed for the purification of a single chain human insulin precursor. The recovery yields of the HTS-fused, GST-fused, MBP-fused, and LacZ-fused single chain human insulin precursors resulted in 47%, 20%, 20%, and 18% as the total protein amounts respectively. These results show that a higher recovery yield of the finally purified recombinant peptides was achieved when affinity column chromatography was employed and when the fused peptide had a smaller molecular weight. In addition the pET expression system gave the highest productivity of a fused insulin precursor due to a two-step regulation of the gene expression, and the HTS-fused system provided the highest recovery of a fused insulin precursor based on a simple and specific separation using the IMAC technique.

• 분석과학
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• 제6권5호
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• pp.471-477
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• 1993

새로운 거대고리 리간드인 {(4, 5):(13, 14)-dibenzo-6, 9, 12-trioxa-3, 15, 21, -triazabicyclo [15. 3. 1]heneicosa-(1, 17, 19)(18, 20, 21) triene: HDBPDA}를 합성하여 양성자화 상수를 구하고, 알칼리 및 알칼리 토금속에 대한 안정도상수(pK)를 구하였다. 안정도상수로부터 유도되는 식을 이용하여 분리인자(${\Delta}$)를 구했다. HDBPDA 리간드를 chloromethylated styrene-divinylbenzene(Merrifield resin)에 결합시켜 새로운 이온교환체인 HDBPDA 이온교환체를 만들었다. 그리고 이것을 사용하여 칼람크로마토그래피로 물 속에서 알칼리 금속 및 알칼리 토금속 양이온들을 분리하여 보았으며, 여기서 얻어진 크로마토그램으로부터 알칼리 및 알칼리 토금속 이온들의 선택성(selectivity), ${\alpha}$와 분리도(resolution), Rs를 구하고, HDBPDA 리간드와 알칼리 및 알칼리 토금속 이온과의 안정도상수(pK)를 구한 값으로부터 ${\Delta}$값을 얻어 이들의 관련성을 비교하였다. 이 두 방법으로 구한 분리능(${\Delta}$와 Rs)값이 잘 일치함을 보였다. 알칼리 및 알칼리 토금속 이온들의 이온교환용량을 측정하고, pH의 의존도를 알아보았다.