• 대한환경공학회지
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• 제32권4호
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• pp.349-356
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• 2010

과염소산이온의 분석을 위해 전기전도도 검출기(CD; conductivity detector)를 연결한 이온크로마토그래피(IC; ion chromatography) 방법이 지금까지 가장 널리 사용되어 왔다. 그러나 이 방법은 시료의 조성에 영향을 받을 수 있고, 정량한계를 낮추는데 한계가 있다. 따라서, 본 연구에서는 미량의 과염소산이온 분석을 위해 이온크로마토그래피 질량분석법(IC-MS/MS; ion chromatography mass spectrometry)을 제시하였다. IC-MS/MS를 이용한 과염소산이온의 분석방법을 적용한 결과 평균회수율 104.4 ${\pm}$ 5.7%, 상대표준편차 1.9 ${\pm}$ 1.3%를 얻었으며, 검출한계(MDL; method detection limit)는 0.0207 ${\pm}$ 0.0099 ${\mu}g/L$를 얻을 수 있었다. IC-MS/MS를 한강수계 지류천과 본류에 적용시킨 결과, 최소 <0.1 ${\mu}g/L$에서 최고 18.30 ${\mu}g/L$ 범위로 나타났다. 서울시 6개 아리수정수센터의 취수원수와 정수에서는 과염소산이온이 0.18~0.34 ${\mu}g/L$의 농도로 존재하는 것으로 나타났다.

• Preventive Nutrition and Food Science
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• 제1권1호
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• pp.1-5
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• 1996

Rapid analytical method was investigated to determine precursors of N-nitrosamine such an nitrite and nitrate in squid(Illex illecebrosus and Sepiell maindroni), codfish(Gadus marcrocephalus)and flatfish(Paralichthys olivaceus) by ion chromatography(IC) and colorimetric methods. Recoveries of nitrite and nitrate in fish tissues were 89~98.7% and 94.1~99.8% for IC, and 98.4~103.7% and 67.7~102.2% for colori-metric method, respectively. Using IC, nitrite was not detected and nitrate was 0.89~1.23mg/kg, while using colorimetric method, nitrite and nitrate were NO~0.08mg/kg and 0.3~0.42mg/kg, respectively. Therefore, the IC method showed better recoveries, and was applicable to extract nitrite and nitrate simultaneously, and is simpler compared with colorimetric method in analyzing nitrite and nitrate from fish tissues.

• 분석과학
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• 제21권4호
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• pp.284-295
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• 2008

플라스틱 시료 중 각종 유해물질 유무 확인을 위한 여러 가지 시험항목을 저비용으로 빠르게 분석할 수 있는 방법으로 Combustion ion chromatography(연소IC)를 사용한 방법을 채택하였다. F, Cl 및 Br의 3개 항목에 대하여 연소IC로 시험법 유효화 검증을 실시한 결과, 검량선은 0.5~4.0 mg/kg 농도범위에서 $r^2$ = 0.999~1.000의 상관관계 계수를 갖는 좋은 직선성을 나타내었으며, 검출한계는 0.005~0.024 mg/kg, 정량한계는 0.014~0.073 mg/kg 이였다. 인증표준물질(CRM)을 사용한 연소IC의 회수율은 95.5~104.9%이었다. 본 결과를 토대로 국내외 시험기관간 비교 숙련도 시험을 실시하였으며, 그 결과 연소IC 방법이 전기전자제품 중에 halogen-free 및 기타 유해물질 규제 대응을 위한 효율적인 분석방법임을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제24권12호
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• pp.1805-1808
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• 2003

The simultaneous determination of As(III), As(V), and DMA has been performed by ion chromatography (IC) coupled with inductively coupled plasma-mass spectrometry (ICP-MS). The separation of the three arsenic species was achieved by an anionic separator column (AS 7) with an isocratic elution system. The separated species were directly detected by ICP-MS as an element-selective detection method. The IC-ICP-MS technique was applied for the determination of arsenic species in a NIST SRM 1643d water sample. An As(III) only was detected in the sample. The detection limits of As(III), As(V) and DMA were 0.31, 0.45, and 2.09 ng/mL, respectively. It was also applied for the determination of arsenic species in a human urine obtained by a volunteer, and three arsenic species were identified. The determination of total As in human urines that were obtained from 25 volunteers at the different age was also carried out by ICP-MS.

• 분석과학
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• 제14권1호
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• pp.28-33
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• 2001

자연수에 존재할 가능성이 있는 $Pu^{3+}$, $Pu^{4+}$, $PuO_2{^+}$, $PuO_2{^{2+}}$ 상태의 플루토늄을 이온크로마토그래피로 분리하는 방법을 연구하였다. 각각 $SiO^-$, SiO-$SO_3{^-}$작용기를 가진 이온교환체를 충전한 두 컬럼을 이용하는 방법과, Dionex사 AG11컬럼에 oxalate/$HNO_3$ 용리액을 사용하여 IC로 분리하는 두 가지 방법을 시도하였다. 예비실험으로서 플루토늄과 화학적 성질이 유사하며 산화수가 안정한 $Eu^{3+}$, $Th^{4+}$, $NpO_2{^+}$, $UO_2{^{2+}}$을 사용하여 분리조건을 얻었다. 이 분리조건을 플루토늄에 적용시켰을 때, $SiO^-$, SiO-$SO_3{^-}$ 이온교환체를 이용한 방법은 산화수별 플루토늄을 성공적으로 분리할 수 있었다. 그러나 IC를 사용한 방법은 oxalate 용액에서 $Pu^{3+}$가 쉽게 $Pu^{4+}$로 산화되며, $PuO_2{^{2+}}$도 $PuO_2{^+}$로 환원되어 분리가 곤란하였다.

• Bulletin of the Korean Chemical Society
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• 제33권6호
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• pp.1967-1971
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• 2012

A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg.

• Bulletin of the Korean Chemical Society
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• 제15권9호
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• pp.786-791
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• 1994

A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

• 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.

• 한국산업보건학회지
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• 제7권2호
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• pp.223-232
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• 1997

The accuracy and precision of a modified method of NIOSH Method 7600 and EPA method 218.6 was determined for analyzing hexavalent chromium, Cr(VI), collected on PVC filter from workplace air. The method was designed to extract from Cr(VI) on PVC filter with a alkali solution, 2% NaOH/3% $Na_2CO_3$, and to analyze it using ion chromatography/visible absorbance detection(IC/VAD). The results and conclusion are as the following. 1. The peak of Cr(VI) was separated sharply on chromatogram and was linearly related with Cr(VI) concentration in sloution. The correlation coefficient was 0.9999 in a calibration curve. The limit of detection was 0.25 $0.25{\mu}g/sample$. 2. The accuracy(% recovery) was 93.3% in a set of sample($9-50{\mu}g$) stored for a day, and 100.1%($10-60{\mu}g$) in another set of samples stored for 2 hours. It is assumed that the difference in recovery by storage time was due to reduction of Cr(VI) to Cr(III). 3. The precision(coefficient of variation, CV) of the method was 0.015 in spiked samples with Cr(VI) standard solution, and 0.010 in spiked samples with plating solution from a chrome electroplating factory. The overall CV in all types of samples was 0.0013. 4. The Cr(VI) was stable in 2% NaOH/3% $Na_2CO_3$ at least for 10 hours. In conclusion, the IC/VAD method is appropriate for determining low-level Cr(VI) in workplace air containing various interferences.

• Bulletin of the Korean Chemical Society
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• 제25권4호
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• pp.447-451
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• 2004

Low and high resolution inductively coupled plasma mass spectrometry (ICP-MS) coupled with ion chromatography (IC) has been investigated for speciation of Cr(III) and Cr(VI). In particular, the interference of ArC^+formed by the carbon in a sample on the simultaneous determination of Cr(III) and Cr(VI) has been studied. In chemical speciation, this study shows that quadrupole type ICP-MS with low resolution has a limitation of simultaneous determination fo chromium species if the sample contains the carbon elements. The interference problems can be solved by high resolution ICP-MS.