• 광물과 암석
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• 제35권4호
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• pp.507-520
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• 2022

지질과학 분야에서 암석의 생성 시기, 지각과 맨틀 진화연구의 기초자료로 활용되는 Sr 동위원소비는 열이온화 질량분석기(thermal ionization mass spectrometry, TIMS) 혹은 다검출기 유도결합 플라즈마 질량분석기(multi-collector plasma ionization mass spectrometry, MC-ICP-MS)와 같은 질량분석기를 이용하여 측정할 수 있다. 이 기술보고에서는, Sr 동위원소비 측정시, 원소의 불완전한 화학적 분리가 Sr 동위원소비의 참값 (true value)에 어떤 영향을 미치는지를 비교하였다. 실험에는 상업용 레진, NBS987(NIST SRM987) Sr 동위 원소 표준물질 그리고 일본지질조사소의 암석표준시료 JG1a, JB3, JA1를 이용하였다. 비교실험 결과, NBS987 Sr 동위원소 표준시료, 일본지질조사소의 암석표준시료 JG1a, JB3, JA1 모두 불완전한 분리에 의해 Rb이 남아있는 경우 ⁸⁷Sr/⁸⁶Sr의 측정값이 변하는 것이 명확하게 관찰된다. 이는 질량분석기 특히 MC-ICP-MS로 동위 원소비를 측정하고자 하는 경우, 동종동위원소의 간섭에 대한 보정에도 불구하고 측정값은 참값에서 벗어나므로 완전한 분리가 중요한 인자임을 지시해준다. 그러므로 MC-ICP-MS를 이용한 Sr 동위원소비 측정결과를 보고할 때는, 동종동위원소에 의한 영향을 판단할 수 있도록 Sr의 동위원소 전체의 측정강도와 더불어 ⁸⁵Rb의 측정강도도 함께 보고돼야 할 것이다.

• 분석과학
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• 제19권6호
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• pp.473-481
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• 2006

• 대한화학회지
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• 제37권9호
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• pp.800-805
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• 1993

정도관리용 생체기준물질 중의 극미량원소에 대한 분석법을 확립하였다. 생체시료를 질산-과산화수소 혼합산화제와 함께 테플론 가압분해용기에 넣어 마이크로파 오븐에서 분해하는 시료전처리법(microwave digestion)을 사용하였다. 시료를 분해시키기 전에 정량할 극미량금속의 안정 동위원소를 첨가하여 동위원소희석 질량분석법을 적용하였다. 혈액과 소나무잎 기준물질에 이러한 분석방법을 적용하여 기준값과 일치되는 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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• 제35권12호
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• pp.3482-3488
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• 2014

Matrix-induced mass bias and its effect on the accuracy of isotope ratio measurements have been examined for a quadrupole-based inductively coupled plasma-mass spectrometer (Q ICP-MS). Matrix-induced mass bias effect was directly proportional to % mass difference, and its magnitude varied for element and nebulizer flow rate. For a given element and conditions in a day, the effect was consistent. The isotope ratio of Cd106/Cd114 under $200{\mu}g\;g^{-1}$ U matrix deviated from the natural value significantly by 3.5%. When Cd 111 and Cd114 were used for the quantification of Cd with isotope dilution (ID) method, the average of differences between the calculated and measured concentrations was -0.034% for samples without matrix ($0.076{\mu}g\;g^{-1}$ to $0.21{\mu}g\;g^{-1}$ for the period of 6 months). However, the error was as large as 1.5% for samples with $200{\mu}g\;g^{-1}$ U. The error in ID caused by matrix could be larger when larger mass difference isotopes are used.

• 분석과학
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• 제26권5호
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• pp.307-314
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• 2013

셀레늄은 다양한 화학종으로 존재하며 그 농도와 형태에 따라 활성도나 생물학적 이용도가 달라지므로 식품에 대한 셀레늄 화학종의 정확한 분리 및 정량이 필요하다. 본 연구에서는 역상 (RP; reversed phase) 고성능 액체 크로마토그래피 (HPLC; high performance liquid chromatography)와 유도결합 플라즈마 (ICP; inductively coupled plasma) 질량분석법 (MS; mass spectrometry)을 사용하여 해산물 시료 중 셀레늄 화학종을 분리 검출 한 뒤에 후 컬럼 동위원소희석법 (post column isotope dilution)으로 정확히 정량 하였다. 시료 중 $^{80}Se$의 간섭요인인 $^{79}Br$을 제거하기 위해 고체상 추출법을 사용하여 대부분의 $^{79}Br$을 제거하였고 남아있는 $^{79}Br$은 수학적 보정식을 이용하여 보정해주었다. CRM (certified reference material) DOLT-4를 사용하여 셀레늄의 총량을 분석한 결과는 인증치와 잘 일치하였지만 각 화학종에 대한 정보는 비교할 수 없었다. 한국인 식탁에 오르는 대표적인 해산물 시료인 갈치, 삼치, 오징어, 등을 분석한 결과, 주된 셀레늄 화학종은 SeCys (selenocysteine)와 SeMet (selenomethionine)이었으며 각각은 0-661.6 mg/kg and 137.3-462.7 mg/kg의 농도로 존재함 을 알 수 있었다.

• Mass Spectrometry Letters
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• 제7권2호
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• pp.50-54
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• 2016

Multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is currently used in our laboratory for isotopic and quantitative analyses of nuclear materials at ultra-trace levels in environmental swipe samples, which is a very useful for monitoring undeclared nuclear activities. In this study, to improve measurement precisions of uranium isotopes at ultratrace levels, we adopted a desolvating nebulizer system (Aridus-II, CETAC., USA), which can improve signal sensitivity and reduce formation of uranium hydride. A peristaltic pump was combined with Aridus-II in the sample introduction system of MC-ICP-MS to reduce long-term signal fluctuations by maintaining a constant flow rate of the sample solution. The signal sensitivity in the presence of Aridus-II was improved more than 10-fold and the formation ratio of UH/U decreased by 16- to 17- fold compared to a normal spray chamber. Long-term signal fluctuations were significantly reduced by using the peristaltic pump. Detailed optimizations and evaluations with uranium standards are also discussed in this paper.

• Journal of Pharmaceutical Investigation
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• 제37권2호
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• pp.79-84
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• 2007

This study was aimed to establish analytical method of Bi to develop a guideline of the bioequivalence test of tripotassium dicitrato bismuthate (TDB). For this purpose, a simple, specific and sensitive inductively coupled plasma-mass spectrometry (ICP/MS) method were developed and validated in human plasma. Various concentrations of bismuth standard solution (0-25ng/mL) were prepared with distilled water and human blank plasma. To 10mL of the volumetric flasks, 2mL of blank plasma was added with 8ml of distilled water. Bi standard solution was added to prepare the calibration samples and injected into ICP-MS. The plasma samples obtained from volunteers given 3 tablets of bismuth (total 900mg as TDB) were analyzed as described above. As a result, the coefficients of variation were <20% in quantitation limit (0.2 ng/mL) and <15% at the rest of concentrations. The stability test by repeated freezing-thawing cycles showed that the samples were stable only for 24hr. The stability tested for samples with a short-term period of storage at room temperature and pre-treatment prior to the analysis showed very stable over 24hr. In 8 healthy Korean subjects received Denol tablets at the dose of 900mg bismuth, AUC, $C_{max},\;T_{max}$ and half-life $(t_{1/2})$ were determined to be $198.33{\pm}173.78 ng{\cdot}hr/mL,\;64.48{\pm}27.06 ng/mL,\;0.52{\pm}0.21 hr,\;and\;5.15{\pm}2.67 hr$, respectively, from the plasma bismuth concentration-time curves. In conclusion, the method was suitable for the determination of bismuth in human plasma samples and could be applied to bioequivalence test of bismuth tablet.

• 한국산업보건학회지
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• 제23권2호
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• pp.65-74
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• 2013

Objectives: This study attempted to develop a method to measure ultra-trace lead concentrations in plasma using Inductively Coupled Plasma Mass Spectrometry(ICP-MS) and to test whether plasma lead can be used as a biomarker for the biological monitoring of exposure to lead. Methods: Lead concentrations in 160 plasma samples of field workers and 42 plasma samples from the control group were measured by ICP-MS. Blood zinc protophorphyrin(ZPP) concentrations and urinary ${\delta}$-aminolevulinic acid${\delta}-ALA$) were measured for correlation analysis with plasma lead. Results: The mean lead level in the plasma of the workers exposed to lead at work were 786.1 ng/L. Plasma lead levels were not correlated with blood ZPP or urinary ${\delta}-ALA$ concentrations. Otherwise, plasma lead levels showed a good correlation coefficient of 0.400 with blood lead levels, and their correlation coefficient had a better value of 0.552 for the non-smoking and drinking group. In the general population group which was not exposed to lead in the workplace and was considered the control group, the mean concentration of plasma lead was 123.1 ng/L. The plasma lead levels for the general population group showed a good correlation coefficient of 0.520 with blood ZPP and urinary ${\delta}-ALA$ concentrations.

• 분석과학
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• 제15권2호
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• pp.120-126
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• 2002

유도결합 플라스마 질량분석기(ICP-MS)와 유도결합 플라스마 원자방출분광기 (ICP-AES)를 이용하여 상업적으로 유통되고 있는 4 종의 분무기(Meinhard, ESI PFA, Cross-flow, Babington)와 한국표준과학연구원(KRISS)에서 직접 제작한 분무기인 KRISS Inert 분무기와 KRISS conespray 분무기의 성능을 평가하였다. 각 분무기의 압력, 시료주입량의 변화에 따른 시료주입 효율을 조사하였으며 ICP-MS와 ICP-AES에 연결하였을 때 시료주입량의 변화에 따른 감도, 안정성, 바탕선 세기, 산화물과 수소화물의 생성 비율을 조사하였다. 시료의 종류, 시료 양의 제한성, 분석기기의 종류, 분석 원소에 따라 가장 적합한 분무기를 선택해야 높은 감도, 낮은 바탕값, 안정한 신호세기 등의 좋은 분석결과를 얻을 수 있음을 알 수 있었다.