• Bulletin of the Korean Chemical Society
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• 제25권2호
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• pp.233-236
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• 2004

Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

• 분석과학
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• 제17권5호
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• pp.438-442
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• 2004

To determine the contents of $^{99}Tc$ in the spent PWR (pressurized water reactor) nuclear fuels by ICP-MS (inductively coupled plasma-mass spectrometry), a technetium separation method using an extraction chromatographic resin (TEVA Spec resin) has been established. $^{99}Tc$ was separated from a spent PWR nuclear fuel solution by this separation procedure and its concentration was determined by ICP-MS. The result agrees well with the value calculated by the program ORIGEN 2 and also the value measured by AG MP-1 resin/ICP-MS method described in our previous paper. It can be concluded that the present separation procedure is superior to the AG MP-1 resin procedure with respect to the time required for technetium separation as well as the efficiency of decontamination from other radioactive nuclides.

• Environmental Analysis Health and Toxicology
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• 제29권
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• pp.16.1-16.9
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• 2014

Objectives Rapid increase in engineered nanoparticles (ENPs) in many goods has raised significant concern about their environmental safety. Proper methodologies are therefore needed to conduct toxicity and exposure assessment of nanoparticles in the environment. This study reviews several analytical techniques for nanoparticles and summarizes their principles, advantages and disadvantages, reviews the state of the art, and offers the perspectives of nanometrology in relation to ENP studies. Methods Nanometrology is divided into five techniques with regard to the instrumental principle: microscopy, light scattering, spectroscopy, separation, and single particle inductively coupled plasma-mass spectrometry. Results Each analytical method has its own drawbacks, such as detection limit, ability to quantify or qualify ENPs, and matrix effects. More than two different analytical methods should be used to better characterize ENPs. Conclusions In characterizing ENPs, the researchers should understand the nanometrology and its demerits, as well as its merits, to properly interpret their experimental results. Challenges lie in the nanometrology and pretreatment of ENPs from various matrices; in the extraction without dissolution or aggregation, and concentration of ENPs to satisfy the instrumental detection limit.

• 한국환경보건학회지
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• 제33권5호
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• pp.397-402
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• 2007

The present study was initiated to examine the measures of dietary intake of Fe, Cu and Zn. The food duplicate samples were collected in Busan and its neighboring area, from the 69 middle-aged women (healthy non-smoking, mostly house wives), who provided informed consent. The samples were wet ashed by being heated in the presence of mineral acids, and Fe, Cu, Zn in the wet-ashed samples were analyzed by inductively coupled plasma - atomic emission spectrometry(ICP-AES). Dietary intake of Fe, Cu and Zn were 10.4 mg/day in Fe, 1.2 mg/day in Cu, 7.4 mg/day as arithmetic mean. The values for dietary Fe and Zn were lower, and the values for dietary Cu were higher than the recommended daily intake from Korean Nutrition Society. Further studies of Korean foods are needed to clarify the representative values for daily dietary Fe, Cu and Zn intake in the Korean population.

• 분석과학
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• 제15권4호
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• pp.335-340
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• 2002

유도결합 플라스마 질량분석법 (ICP-MS)을 이용하여 모발 중 다원소 동시 정량법을 확립하였다. 0.05 g의 모발 시료에 내부표준물질인 In을 가하고 질산 1.5 mL와 함께 테플론 가압분해 용기에 넣어 마이크로파를 이용하여 분해하는 시료전처리법을 사용하였다. 측정값의 정확도 및 신뢰도를 확인하기 위하여 모발 인증표준물질인 GBW 09101을 반복 분석하였는데 측정값은 인증값과 불확도 범위 내에서 잘 일치하는 결과를 얻었다.

• 분석과학
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• 제8권4호
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• pp.427-434
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• 1995

Inductively coupled plasma mass spectrometry combined with the isotope dilution method is used for the determination of lithium. The isotope dilution method is based on the addition of a known amount of enriched isotope (spike) to a sample. The analyte concentration is obtained by measuring the altered isotope ratio. The spike solution is calibrated through so called reverse isotope dilution with a primary standard. The spike calibration is an important step to minimize error in the determined concentration. It has been found essential to add spike to a sample and the primary standard so that the two isotope ratios should be as dose as possible. Since lithium is neither corrosive nor toxic, lithium is used as a chemical tracer in the nuclear power plants to measure feedwater flow rate. 99.9% $^7Li$ was injected into a feedwater line of an experimental system and sample were taken downstream to be spiked with 95% $^6Li$ for the isotope dilution measurements. Effects of uncertainties in the spike enrichment and isotope ratio measurement error at various spike-to-sample ratios are presented together with the flow rate measurement results in comparison with a vortex flow meter.

• Bulletin of the Korean Chemical Society
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• 제29권2호
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• pp.393-397
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• 2008

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to determine the presence of germanium and phosphorus in a pure gold bonding wire. The samples were dissolved with hydrobromic acid and nitric acid at room temperature. The quantitation limits were 0.012 mg L-1 at 265.118 nm for Ge and 0.009 mg L-1 at 177.495 nm for P. Using the mixed acid digestion formula of DIW+HBr+HNO3, the recoveries were in the range of 98-100% and the relative standard deviation was within 1.1-2.3%. On the other hand, the amount of Ge decreased by about 16.2% using DIW+HCl+HNO3, due to the formation of a volatile compound. The Ge contents determined using the external method and the standard addition method were 9.45 mg kg-1 and 9.24 mg kg-1, respectively, and the P contents, using the same methods, were 22.49 mg kg-1 and 23.09 mg kg-1, respectively. Both methods were successfully used to determine the trace amounts of P and Ge in the pure gold bonding wire samples.

• 분석과학
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• 제13권4호
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• pp.423-427
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• 2000

유도결합 플라스마 질량 분석법(ICP-MS)을 이용하여 음용수 중의 전체비소를 정량하였다. 지하수 및 간이 상수도와 시판되는 먹는 물에 질산을 첨가하여 1%로 산성화한 후에 ICP-MS로 전제비소의 함량을 분석하였다. 그 결과 음용수 중의 전체 비소는 $30{\mu}g/L$ 이하로서 수질 기준치인 $50{\mu}g/L$ 이하의 값을 나타내었다.

• 분석과학
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• 제20권3호
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• pp.251-254
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• 2007

수용액 내에서 환원제인 sulfurous acid와 휘발성이 강한 Os(III)을 반응시킨 후 생성된 비휘발성 Os(IV)을 inductively coupled plasma atomic emission spectrometry (ICP-AES)로 분석하였다. pH 2-10의 수용액에서 sulfurous acid와 Os(VIII)의 정량적 반응에 의하여 생성된 Os(VI)을 ICP-AES로 분석하였다. 동축형 분무기(concentric type nebulizer)에 의한 시료 도입 방법에서 sulfurous acid와 osmium은 반응 직후부터 안정한 신호를 나타내었으며 다양한 ICP-AES 조건에서 3회 반복 측정했을 때 재현성은 0.5-4.5%였으며, 검출 한계는 2.5-57.7 ng/g이었다.

• Bulletin of the Korean Chemical Society
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• 제19권7호
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• pp.766-770
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• 1998

On-line preconcentration by direct precipitation with hydroxide has been developed and applied for the analysis of Cd in Inductively Coupled Plasma Atomic Emission Spectrometry. Cadmium is continuously precipitated with hydroxide and dissolved by nitric acid in on-line mode. Currently, the enrichment factor is more than 90 times for 20.0 mL of sample and could be further increased very easily. For a large sample throughput, 1.0 mL of sample loop is used and the enrichment factor is 4.5 with the sampling speed of 15/hr. The method has been applied to the analysis of NIST reference sample and has yielded good results with the certified value.