• Bulletin of the Korean Chemical Society
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• 제18권11호
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• pp.1172-1175
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• 1997

Calcium isotopic ratios are precisely measured by removing isobaric interferences originated from water in the plasma. Liquid Ar cryogenic trap combined with membrane desolvator could eliminate backgrounds at m/z 42 and 44. Slow drift of ICP-MS is corrected by the frequent running of the standards. It is found necessary to separate Ca from the sample matrix using Ca oxalate precipitation technique. Currently, the RSD is 0.5-1.0% for 2 minutes of measurement but is expected to be improved if the measurement time is increased. The technique was applied to 42Ca enriched baby fecal samples and successfully determined 42Ca/44Ca ratio changes.

• Mass Spectrometry Letters
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• 제3권2호
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• pp.54-57
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• 2012

Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.

• Mass Spectrometry Letters
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• 제4권4호
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• pp.87-90
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• 2013

Isotope amount ratios of lead in a bronze sample have been successfully determined using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Matrix separation conditions were tested and optimized using ion exchange chromatography with anion-exchange resin, AG1-X8, and sequential elution of the 0.5 M HBr and 7 M $HNO_3$ to separate lead from very high contents of copper and tin in bronze matrix. Mercury was also removed efficiently in the optimized separation condition. The instrumental isotope fractionation of lead in the MC-ICP-MS measurement was corrected by the external standard sample bracketing method using an external standard, NIST SRM 981 lead common isotope ratio standard followed by correction of procedure blank to obtain reliable isotope ratios of lead. The isotope ratios, $^{206}Pb/^{204}Pb$, $^{207}Pb/^{204}Pb$, $^{208}Pb/^{204}Pb$, and $^{208}Pb/^{206}Pb$, of lead were determined as $18.0802{\pm}0.0114$, $15.5799{\pm}0.0099$, $38.0853{\pm}0.0241$, and $2.1065{\pm}0.0004$, respectively, and the determined isotope ratios showed good agreement with the reference values of an international comparison for the same sample within the stated uncertainties

• 한국환경보건학회지
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• 제45권3호
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• pp.258-266
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• 2019

Objectives: In this study, blood lead was analyzed using graphite furnace atomic absorption spectrometry (GF-AAs) and inductively coupled plasma mass spectrometry (ICP-MS). We tried to examine the difference and consistency of the analytical values and the applicability of the analytical method. Methods: We selected 57 people who agreed to participate in this study. After confirming the linearity of the calibration standard curves in GF-AAs and ICP-MS, the concentrations of lead in quality control material and samples were measured, and the degree of agreement was compared. Results: The detection limit of the ICP-MS was lower than that of GF-AAs. The coefficient of variation of reference materials was shown to be stable in the ICP-MS and GF-AAs. When the correspondence between the two equipments was verified by bias of the analysis values, a concordance was shown, and approximately 98% of the ideal reference lines were present within ${\pm}40%$ of the deflection. Conclusion: GF-AAs showed high sensitivity to single heavy metal analysis, but it took much time and showed higher detection limit than ICP-MS. Therefore, it would be considered necessary to switch to ICP-MS analysis method, considering that the level of lead exposure is gradually decreasing.

• 분석과학
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• 제15권2호
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• pp.127-134
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• 2002

추출한 유기상 속의 희토류 원소를 유도결합 플라스마 질량분석법(inductively coupled plasma mass spectrometry, ICP-MS)으로 정량하는 방법에 대하여 연구하였다. 희토류 원소를 추출한 유기상의 과다한 도입을 방지하기 위하여 탈용매화장치를 장착한 초음파 분무기를 이용하여 ICP-MS에 주입하였다. 에탄올(EtOH)에 MIBK(methyl isobutyl ketone)를 섞은 용매를 도입하였을때, 계수율(count rate)이 증가하였고, 여기에 0.03 M의 추출제 HEH(2-ethylhexyl-2-ethylhexyl phosphonic acid, P507, PC88A)를 섞었을 때는 감소하였다. 탈용매화장치의 냉각장치(condenser)의 최적온도는 -10 $^{\circ}C$이었고, 가열관(heating tube)의 최적온도는 150 $^{\circ}C$이었다. 계수율이 최대이고, 반사파(reflect power)가 최소인 최적 운반기체의 흐름속도는 0.7 L/min이었다. MIBK에 추출제 HEH가 0.03 M이 섞여있는 추출용매로 추출을 행하였을 때, 최적 pH는 4.3이었고, 추출시간은 10 분이었다. 최적조건에서 0.2 ${\sim}$ 20 ng/mL의 표준용액으로 얻은 검정곡선으로부터 구한 검출 한계는 0.02 ${\sim}$ 0.05 ng/mL 이었다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2004년도 춘계학술대회 논문집 반도체 재료 센서 박막재료 전자세라믹스
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• pp.22-25
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• 2004

In this study, BST thin films were etched with inductively coupled $CF_4/(Cl_2+Ar)$ plasmas. The etch characteristics of BST thin films as a function of $CF_4/(Cl_2+Ar)$ gas mixtures were analyzed using quadrupole mass spectrometry (QMS) and optical emission spectroscopy (OES). The maximum etch rate of the BST thin films was 53.6 nm/min because small addition of $CF_4$ to the $Cl_2/Ar$ mixture increased chemical effect. The optimum condition appears to be under a 10 % $CF_4/(Cl_2+Ar)$ gas mixture in the present work.

• 암석학회지
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• 제10권3호
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• pp.148-156
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• 2001

경북 경주시 인근의 제4기 추정단층 중 입실단층과 장항리단층의 파쇄대를 충진하고 있는 탄산염암맥을 대상으로 다검출기 유도결합 플라즈마 질량분석기를 이용한 $^{230}$ $Th^{234}$ U 비평형 연대를 측정하였다. 완전히 녹인 시료로부터 공침과 이온교환화학을 통해 간편하게 U, Th을 단체분리하였는데 회수율은 Th 80%, U 70% 정도였다. 이 부분으로부터 기기 조건이 최적화된 다검출기 유도결합 플라즈마 질량분석기를 이용하여 $^{234}$ $U^{238}$ $U^{230}$ $Th^{232}$ Th비를 분석하였고 U/Th비는 처리하지 않은 시료로부터 직접 분석하였다. 분석 결과 입실 단층의 탄산염암 맥은 $^{234}$ U-$^{230}$ Th 시차평형에 도달하여 기존의 ESR 연대측정 결과를 지지하였으며 쇄설성 부분이 보정된 장항리단층 탄산염암 맥의 $^{230}$$Th^{234}$ /U 비평형 연대는$ 48\pm$41 ka로서 파쇄대의 최소 형성시기를 지시한다.

• 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.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3206-3210
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• 2013

This study focused on the matrix interference for the qualitative and quantitative analysis of inorganic arsenic species in seaweed by ion chromatography (IC) combined with inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The matrix of seaweed has a significant effect on the determination of inorganic arsenic species. In particular, the retention times of inorganic arsenic species in the in the standard solution were different from those in seaweed because of the matrix interference. Thus, it was not suitable to use the chromatographic method for the determination of the arsenic species in seaweed. We investigated an alternative method for the determination of inorganic arsenic species in seaweed. The method was applied for the seaweed samples such as laver, green laver, sea tangle and sea mustard. The sample extraction methods of the arsenic species were also investigated in this study.

• 대한화학회지
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• 제48권2호
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• pp.203-206
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• 2004