• Title/Summary/Keyword: ICPMS

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Producing of Bronze Artifacts Excavated from Gulsansa Temple Site in Gangneung: Technology and Provenance (강릉 굴산사지에서 출토된 청동기의 제작: 제작기술 및 원료산지)

  • Han, Woo Rim;Kim, So Jin;Lee, Eun Woo;Hwang, Jin Ju
    • Journal of Conservation Science
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    • v.35 no.3
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    • pp.187-196
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    • 2019
  • Bronzes excavated from a Gulsansa temple site in Gangneung were investigated in order to study the production of technology and provenance in this area. The bronze artifacts were discovered to consist of copper-tin or copper-tin-lead alloys using chemical analysis(EDS and EPMA). The excavated bronzes were manufactured using a casting or hammering process, and a bronze belt was gilded with gold foil. The provenance of 25 bronzes was studied using lead isotope analysis(TIMS and LA-MC-ICPMS). The results reveal the use of raw materials found near the excavated site. The object of this study was to investigate the manufacturing techniques and provenance in Gangneung without the need for a lot of data. Our results will contribute to the study of Gulsansa and bronze artifacts in Goryo(12-13th century).

Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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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.

Errors in Isotope Dilution Caused by Matrix-induced Mass Bias Effect in Quadrupole Inductively Coupled Plasma-Mass Spectrometry

  • Pak, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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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.

Preliminary Results of Extraction, Separation and Quantitation of Arsenic Species in Food and Dietary Supplements by HPLC-ICP-MS

  • Nam, Sang-Ho;Cheng, John;Mindak, William R.;Capar, Stephen G.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.903-908
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    • 2006
  • Various extraction procedures were investigated using reference materials and samples to evaluate extraction efficiency and effectiveness. Inductively coupled plasma mass spectrometry (ICP-MS) was used to measure total arsenic and to quantitate arsenic species when coupled to an HPLC (high pressure liquid chromatography). Arsenic species were extracted from rice flour (NIST SRM 1568a) with water/methanol mixtures using accelerated solvent extraction (ASE). Total arsenic extraction efficiency ranged from 42 to 64%, for water and various methanol concentrations. From spinach (NIST SRM 1570), freeze-dried apple, and rice flour (NIST SRM 1568a), arsenic species were extracted with trifluoroacetic acid (TFA) at 100 ${^{\circ}C}$. Total arsenic extraction efficiency was 90% for spinach, 75% for freeze-dried apple, and 83% for rice flour. Enzymatic extraction with alpha-amylase and sonication resulted in extraction efficiency of 104% for rice flour, 98% for freeze-dried apple, and 7% for spinach. Chromatograms of arsenic species extracted by the optimum extraction methods were obtained, and the species were quantified. Arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were found in the apple sample, and DMA and As(V) in the rice flour sample. As(V) and MMA were found in three herbal dietary supplement samples.

The simultaneous determination of germanium and selenium in plant by hydride vapour generator inductively coupled plasma mass spectrometry (HVG-ICPMS을 이용한 식물체 중 게르마늄과 셀레늄의 동시분석 연구)

  • Ham, Yong-Gyu;Kim, Bo-Kyong;Kwon, Young-Uk;Baek, Hyo-Hyu;Lee, Seok-Ki
    • Analytical Science and Technology
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    • v.24 no.3
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    • pp.159-167
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    • 2011
  • In this study, the hydride vapour generator inductively coupled plasma mass spectrometry (HVGICPMS) was applied as the new analytical method to show the high accurate and reproductive data analysing the amounts of selenium and germanium being existed inside a system of plant. In order to decrease the interference effects, such as ion and molecular interference. Mini torch was used into the ICPMS instead of the conventional torch. At conditions of the different kinds and concentrations of acid solution, the different reductive conditions for composing hydride, and the different methods for making ash, the contents of selenium and germanium in lettuce were analysed. The inspection of yields and data comparison from SRM-1574 and -1570a were used for increasing the accuracy of this analysis.

Geology and U-Pb Age in the Eastern Part of Yeongdeok-gun, Gyeongsangbuk-do, Korea (경북 영덕군 동부 일원의 지질과 U-Pb 연령)

  • Kang, Hee-Cheol;Cheon, Youngbeom;Ha, Sangmin;Seo, Kyunghan;Kim, Jong-Sun;Shin, Hyeon Cho;Son, Moon
    • The Journal of the Petrological Society of Korea
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    • v.27 no.3
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    • pp.153-171
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    • 2018
  • This study focuses on the investigation of geologic distribution and stratigraphy in the eastern part of Yeongdeok-gun, based on Lidar imaging, detailed field survey, microscopic observations, SHRIMP and LA-MC-ICPMS U-Pb age dating, and a new geological map has been created. The stratigraphy of the study area is composed of the Paleoproterozoic metamorphic rocks consisting of banded gneisses of sedimentary origin and schists ($1841.5{\pm}9.6Ma$) of volcanic origin, Triassic Yeongdeok plutonic rocks ($249.1{\pm}2.3Ma$) and Pinkish granites ($242.4{\pm}2.4Ma$), Jurassic Changpo plutonic rocks ($193.2{\pm}1.9Ma{\sim}188.8{\pm}2.0Ma$) and Fine-grained granites ($192.9{\pm}1.7Ma$), Formations [Gyeongjeongdong Fm, Ullyeonsan Fm. (~108 Ma), Donghwachi Fm.] of the Early Cretaceous Gyeongsang Supergroup and acidic volcanic rocks and dykes erupted and intruded in the Late Cretaceous, Miocene intrusive rhyolitic tuffs ($23.1{\pm}0.2Ma{\sim}22.97{\pm}0.13Ma$) and sedimentary rocks of the Yeonghae basin, and the Quaternary sediments. The Triassic Pinkish granites, Jurassic Changpo plutonic rocks and Fine-grained granites are newly defined plutonic rocks in this study. Miocene intrusive rhyolitic tuffs bounded by the Yangsan Fault, which was first discovered in the north of Pohang city, are believed to play an important role in the understanding of the Miocene volcanic activity and the crustal deformation history on the Korean Peninsula. It is confirmed that The NNE-SSW-striking Yangsan Fault penetrating the central part of the study area and branch faults are predominant in the dextral movement and cutting all strata except the Quaternary sediments.

Determination of selenium in grains by hydride generation-ICP/MS (수소화물발생-유도결합플라즈마 질량분석법(HG-ICP/MS)을 이용한 곡류 중 셀레늄의 정량분석)

  • Kim, Minkyung;Jung, Jinok;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.135-141
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    • 2013
  • The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.

The Late Cretaceous Emplacement Age of Masan Hornblende-Biotite Granite (마산 각섬석-흑운모 화강암의 연령: 후기 백악기 정치연령)

  • Lee, Tae-Ho;Park, Kye-Hun;Kim, Jeongmin;Kim, Myoung Jung
    • The Journal of the Petrological Society of Korea
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    • v.26 no.1
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    • pp.1-11
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    • 2017
  • We have dated the K-Ar, Ar-Ar and U-Pb ages of the Masan hornblende-biotite granite in the southern Cretaceous Gyeongsang basin to constrain its emplacement age. The ~108 Ma hornblende K-Ar age obtained in the study is similar to the previously reported Rb-Sr age. However, the single grain total fusion $^{40}Ar/^{39}Ar$ dating on hornblende failed to yield statistically meaningful ages because the isotopic system was open during its alteration. Thus the hornblende K-Ar age in the study is also unlikely to be reliable. The single grain total fusion $^{40}Ar/^{39}Ar$ dating on biotite yielded an average age of $75.8{\pm}3.0Ma$. Apart from scattered data in the range of ~45-75 Ma, the average age increased to ~80 Ma. The SHRIMP and LA-MC-ICPMS U-Pb isotopic compositions of zircon from the Masan hornblende-biotite granite yielded its emplacement age as $87.6{\pm}2.7Ma$ and $86.8{\pm}0.4Ma$, respectively. It is thus likely that the ~80 Ma $^{40}Ar/^{39}Ar$ age of biotite might reflect the cooling age of Masan hornblende-biotite granite or the thermal influences from later intense igneous activities in the Gyeongsang basin.

Determination of bromine in 1000 ㎍/g Cl standard solution by ID-ICPMS (동위원소희석 질량분석법에 의한 1000 ㎍/g 염소 표준용액 중 브롬 불순물 분석)

  • Park, Chang Joon;Suh, Jung Kee;Song, Hyun Joo;Lee, Dong Soo
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.1-8
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    • 2006
  • The isotope dilution method was used for the determination of Br impurity in $1000{\mu}g/g$ Cl standard solution. Since relatively pure KCl salt was used for the preparation of the Cl standard solution, the Br impurity determination suffers from both spectral and non-spectral interferences due to the presence of a large amount of K and Cl matrices. AG2-X8 anion-exchange resin was employed to separate the Br analyte from the matrices, and RF power was raised to 1500 W and nebulizer gas flow rate was lowered to 0.77 L/min to reduce background from the $ArArH^+$ molecular ions. The Br impurity in the $1000{\mu}g/g$ Cl standard solution was determined to be 43.7 ng/g with the standard addition method. The analytical result was in good agreement with 41.2 ng/g (RSD 1.6%) determined by the isotope dilution method to lower uncertainty from poor reproducibility of the anion-exchange process.

Study on the Behavior of Colloidal Hematite: Effects of Ionic Composition and Strength and Natural Organic Matter in Aqueous Environments (교질상 적철석의 거동 특성: 수환경 내 이온 조성 및 세기, 자연 유기물이 미치는 영향)

  • Lee, Woo-Chun;Lee, Sang-Woo;Kim, Soon-Oh
    • Economic and Environmental Geology
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    • v.53 no.4
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    • pp.347-362
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    • 2020
  • Iron (hydro)oxides in aqueous environments are primarily formed due to mining activities, and they are known to be typical colloidal particles disturbing surrounding environments. Among them, hematites are widespread in surface environments, and their behavior is controlled by diverse factors in aqueous environments. This study was conducted to elucidate the effect of environmental factors, such as ionic composition and strength, pH, and natural organic matter (NOM) on the behavior of colloidal hematite particles. In particular, two analytical methods, such as dynamic light scattering (DLS) and single-particle ICP-MS (spICP-MS), were compared to quantify and characterize the behavior of colloidal hematites. According to the variation of ionic composition and strength, the aggregation/dispersion characteristics of the hematite particles were affected as a result of the change in the thickness of the diffuse double layer as well as the total force of electrostatic repulsion and van der Walls attraction. Besides, the more dispersed the particles were, the farther away the aqueous pH was from their point of zero charge (PZC). The results indicate that the electrostatic and steric (structural) stabilization of the particles was enhanced by the functional groups of the natural organic matter, such as carboxyl and phenolic, as the NOM coated the surface of colloidal hematite particles in aqueous environments. Furthermore, such coating effects seemed to increase with decreasing molar mass of NOM. On the contrary, these stabilization (dispersion) effects of NOM were much more diminished by divalent cations such as Ca2+ than monovalent ones (Na+), and it could be attributed to the fact that the former acted as bridges much more strongly between the NOM-coated hematite particles than the latter because of the relatively larger ionic potential of the former. Consequently, it was quantitatively confirmed that the behavior of colloidal hematites in aqueous environments was significantly affected by diverse factors, such as ionic composition and strength, pH, and NOM. Among them, the NOM seemed to be the primary and dominant one controlling the behavior of hematite colloids. Meanwhile, the results of the comparative study on DLS and spICPMS suggest that the analyses combining both methods are likely to improve the effectiveness on the quantitative characterization of colloidal behavior in aqueous environments because they showed different strengths: the main advantage of the DLS method is the speed and ease of the operation, while the outstanding merit of the spICP-MS are to consider the shape of particles and the type of aggregation.