• Title/Summary/Keyword: isotope dilution

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Separation and Purification for the Determination of Samarium and its Isotopes in PWR Spent Nuclear Fuels (PWR 사용후핵연료 중 Sm 동위원소 정량을 위한 분리 및 정제)

  • Kim, Jung Suk;Jeon, Young Shin;Choi, Kwang Soon;Park, Soon Dal;Lee, Chang Heon;Kim, Won Ho
    • Analytical Science and Technology
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    • v.14 no.4
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    • pp.291-299
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    • 2001
  • A method of separation and purification of Sm for quantitation of Sm isotopes from various fission products in PWR spent nuclear fuels has been studied. Simulated solution containing inactive metal ions(Cs, Ba, Gd, Eu, Sm and Nd) in place of radioactive fission products was prepared. Sm was separated with 0.5 M $HNO_3$/80% MeOH after washing with 1 M $HNO_3$/90% MeOH on AG $1{\times}8$, anion exchange resin. Sm was purified on cation exchange resin, AG $50W{\times}8$, pretreated with 0.2 M alpha-hydroxisobutyric acid(pH 4.5-4.6) to remove Ba causing isobaric effect Sm from PWR spent fuel. As a result of mass spectrometric measurement, eluted Sm portion did not include isobars form other elements such as Gd, Eu, Pm, Nd and BaO. The contents of Sm and its isotopes($^{147}Sm$, $^{148}Sm$, $^{149}Sm$, $^{150}Sm$, $^{151}Sm$, $^{152}Sm$ and $^{154}Sm$) in spent fuel were determined by isotope dilution mass spectrometric method spiking $^{154}Sm$.

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The Characteristics of Organic Matter in the Quaternary Sediments from ODP Leg 127 Site 794A, East Sea (동해 ODP Leg 127 Site 794A에서 채취한 제4기 퇴적물의 유기지화학적 특성 연구)

  • Lee Sang Il;Lee Young-Joo;Kim Ji Hoon;Oh Jae Ho;Yun HyeSu
    • Economic and Environmental Geology
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    • v.38 no.6 s.175
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    • pp.707-716
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    • 2005
  • Organic geochemical analyses including Rock-Eval pyrolysis, elemental analysis and stable carbon isotope analysis were performed to evaluate the characteristics of organic matter in the ODP Leg 127 Site 794A sediments and to understand paleoceanographic changes. Based on the TOC contents, C/N ratio, HI vs. OI, $\delta^{13}C_{org}$ and C/S ratio, results imply that dark layers containing a large amount of terrigenous organic matter were deposited under the suboxic/anoxic conditions, whereas the light layers containing largely marine organic matter were deposited under the oxic conditions. These results indicate that increasing surface-productivity by the input of a large amount of terrigenous organic matter from adjacent continent led to the deposition of dark layers during the interglacial highstands, whereas marine primary production and dilution caused by Kosa from the China desert area led to the deposition of light layers with the decreased to terrigenous organic matter during the glacial lowstands.

A Study on Renin-Angiotensin System and Total Exchangeable Sodium in Hypertension (고혈압(高血壓)에 있어서 Renin-Angiotensin계(系) 및 총교환(總交換) 나트륨에 관(關)한 연구(硏究))

  • Choe, Kang-Won;Park, Jung-Sik;Lee, Jung-Sang;Koh, Chang-Soon
    • The Korean Journal of Nuclear Medicine
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    • v.10 no.1
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    • pp.1-14
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    • 1976
  • The etiologic role of renin-angiotensin system and sodium-volume status in the pathophysiology of various forms of hypertension was investigated. Plasma renin activity (PRA) was measured by radioimmunoassay, while sodium-volume status was evaluated by the determination of total exchangeable sodium(NaE) using isotope dilution method. The subjects consisted of 25 controls, 24 patients with essential hypertension, with chronic renal failure (13 with hypertension, 9 without hypertension) and with malignant hypertension. The results were as follows: 1. An inverse correlation between NaE and PRA was noted in control subjects (r=-0.598, p<0.001) and normal renin essential hypertension(r=-0.551, p<0.05) and the chronic renal failure with hypertension. (r=-0.790, p<0.001) 2. NaE increased markedly the in chronic renal failure with hypertension ($66.9{\pm}8.69mEq/kg$ of LBM, p<0.001) and the chronic renal failure without hypertension ($54.9{\pm}9.28mEq/kg$ of LBM, p<0.05), while mild increase was noted in malignant hypertension ($51.7{\pm}6.24mEq/kg$ of LBM, 0.05$50.1{\pm}7.24mEq$) as well as in its renin subgroups.(p>0.1) 3. Absolute value of PRA was not deviated significantly from control group ($2.53{\pm}1.416ng/ml/hr$) except in malignant hypertension ($6.09{\pm}2.042$, p<0.001). But PRA was inappropriately high in relation to prevailing NaE in the chronic renal failure with hypertension (eleven of thirteen patients) and malignant hypertension (ten of fourteen patients), while PRA variatiation was within physiologic range in the chronic renal failure without hypertension. 4. The NaE-PRA product was markedly increased in the chronic renal failure with hypertension ($514.4{\pm}42.10$, p<0.001) and in malignant hypertension ($442.7{\pm}55.03$, p<0.001), while moderately increased NaE-PRA product was noted in the chronic renal failure without hypertension ($402.6{\pm}59.67$, p<0.001). No significant difference in NaE-PRA product was noted in essential hypertension ($354.4{\pm}62.38$, p>0.1). It is suggested that renin-angiotensin system plays a predominant role in the pathogenesis of malignant hypertension and in hypertension of chronic renal failure, though sodium retention is also contributing factor. PRA variation in essential hypertension does not appear to be associated with any consistent change in Na-volume status, suggesting the existence of another mechanism in the genesis of hypertension and PRA variation.

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Speciation Analysis of Seleno-Compounds in Hair and Finger Nails (손톱과 모발에서의 셀레노 화합물의 화학종 분석)

  • Ji, Young;Keum, Daeseop;Pak, Yong N.
    • Journal of the Korean Chemical Society
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    • v.64 no.4
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    • pp.203-209
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    • 2020
  • Selenium species in hair and nails were extracted, separated and analyzed with HPLC-ICP/MS. The result showed that Se species was mostly SeCys and the information related to the change of selenium concentration in a body could be obtained. The Se fortification study was performed for 5 participants during 12 months. The average of Se concentration was 858.6 ± 201.2 ng g-1, which did not change much during the research period nor the difference between the individuals was striking. In the case of hair, the average concentration was 205.3 ng g-1 which was lower than nails. Se supplement of 22 ㎍ day-1 was taken for 3 months by the volunteers and the difference between before and after (3 months period for each) the taking of supplement was not striking. However, when the dose was increased to 300 ㎍ day-1 for 2 months, the concentration was increased noticeably to 1,230 ng g-1. It can be thought that the analysis of finger nail for Se can provide valuable information for the long period (several months) of exposure or intake of Se for a human body.

A study on the development of phthalate plasticizers CRM in ABS resin (ABS 중 phthalates 가소제 CRM 개발에 대한 연구)

  • Jung, Jung-Sul;Park, Jung-Woo;Yoo, Seok;Kweon, Seong-Il;Hong, Sung-Taeg;Sun, Yle-Shik;Park, Cheon-Min;Choi, Chang-Hyoo
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.273-283
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    • 2012
  • Phthalate plasticizers are regulated by RoHS, REACH and CPSC as hazardous substances. Responding to these international environmental restrictions, we developed ABS certified reference material (CRM) for determination of phthalate plasticizers such as DMP, DEP, DBP, BBP, DEHP and DnOP. The candidate material has been made with ABS resin widely used in electric and electronic products and 6 kinds of phthalate plasticizers. The making of the material involved a series of processes like extruding, cooling, pelletizing, and drying using twin screw extruder. Then it has been certified according to ISO Guide 35. Using isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS), homogeneity, short-term stability, and long-term stability were evaluated. The certified values were determined by using primary reference material (PRM) of KRISS for traceability. From now on, we will provide ABS CRM to national and international companies and research institutes after certification as certified reference material and registering on COMAR (code of reference material).

Determination of Cholesterol, Fatty Acids and Polyaromatic Hydrocarbons in PM10 Particles Collected from Meat Charbroiling (고기구이 스모크에서 채취한 PM10입자에서 콜레스테롤, 지방산과 PAH의 분포)

  • Seo, Young-Hwa;Ko, Kwang-Youn;Jang, Young-Kee
    • Journal of Korean Society of Environmental Engineers
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    • v.32 no.2
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    • pp.155-164
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    • 2010
  • Emission from biomass combustion such as meat charbroiling is an important source of organic aerosol. Since source profiles are necessary input profiles for source apportionment of aerosol by a chemical mass balance model, meat cooking organic source profiles are developed by measuring organic marker compounds, including palmitic acid, stearic acid, oleic acid and cholesterol as well as PAH compounds. Emissions from meat and pork charbroiling are collected on quartz filters with a PM10-high volume sampler, extracted with organic solvents, derivatized with diazomethane/TMS and analyzed by GC/MS isotope dilution method. Organic and elemental carbon are also analyzed by an OCEC analyzer. Wt.% of cholesterol to the organic carbon(OC) content from beef and pork charbroiling is only 0.056 and 0.062, but wt. % of all saturated fatty acids to the OC content from beef and pork charbroiling is 2.727 and 2.022, and the wt% of all unsaturated fatty acids to the OC content is 0.278 and 0.438, respectively. Content of total PAH compounds to the OC content from beef charbroiling is higher than that from pork charbroiling, and those are 0.116 wt% and 0.044 wt%. Among PAH compounds benzo(a)pyrene as a single compound is account for 0.0071 wt% and 0.0023 wt% of OC content from beef and pork charbroiling. Ratios of marker compound to cholesterol are calculated, and those values are in good agreement with the values already reported at the food cooking emission, indicating that they can be used as organic source profiles for the apportionment of organic aerosol.

The Relationship among the Indicator PCBs in Breast Milk and Dietary Habits and Demographic Factors in Women Living in Urban Areas (대도시에 거주하는 여성의 모유 중 Indicator PCBs와 식이습성 및 인구통계학적 인자간의 관계)

  • We, Sung-Ug;Kim, Ki-Ho;Cho, Bong-Hui;Cho, Yu-Jin;Yoon, Cho-Hee;Min, Byung-Yoon
    • Journal of Environmental Health Sciences
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    • v.36 no.3
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    • pp.199-207
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    • 2010
  • In this study, breast milk levels of indicator polychlorinated biphenyls (PCBs) were estimated, and statistics drawn, for 22 Koreans in the general population, aged 26-38, who had resided in metropolitan areas for more than 5 years without occupational exposure to organochlorine pollutants. Concentrations of indicator PCBs were measured using the isotope dilution method with a high resolution gas chromatograph/high resolution mass detector, which provided accurate and precise data for investigation of trends, and international comparisons. The geometric mean of total indicator PCB levels was 22.3 ng/g lipid, which is significantly lower than the level in individuals from European countries. Overall, the geometric mean and 95th percentile of the most abundant congener PCB 153 were 8.04 ng/g lipid and 16.4 ng/g lipid, respectively. PCB congeners 138, 153 and 180 together accounted for about 75% of the indicator congeners analyzed. Breast milk total indicator PCB concentrations were significantly associated with age and parity, but not with body mass index (BMI), rate of body weight increase, or smoking habits. The geometric mean level of PCB 153 in breast milk from mothers with a pre-pregnant BMI < $21\;kg/m^2$ was significantly higher than in pre-pregnant women with a BMI of ${\geqslant}\;21\;kg/m^2$ (p<0.05). Women who ate more fish, meat, and milk products did not have significantly higher total indicator PCB levels than those who ate less of these products, but a significant difference in PCB 153 levels was demonstrated between the subjects consuming higher (11.45 ng/g lipid) and lower (6.79 ng/g lipid) amounts of fish (p<0.05), after adjusting for confounders. These results suggest that age, parity and fish intake are the important factors affecting the concentrations of indicator PCBs in these subjects.

Estimation of Indicator PCBs Exposure in Infants via Breast-Feeding Period (수유기간에 따른 모유 중 Indicator PCBs 분석을 통한 영유아의 인체노출평가)

  • We, Sung-Ug;Yoon, Cho-Hee;Min, Byung-Yun
    • Journal of Korean Society of Environmental Engineers
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    • v.34 no.1
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    • pp.7-15
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    • 2012
  • The levels of indicator PCBs were determined in 132 human milk samples (Colostrum, 30th days after delivery, 60th days after delivery) collected in 2006 according to World Health Organization's (WHO) protocol. In addition, concentrations of indicator polychlorinated biphenyls (PCBs) were measured by the isotope dilution method with high resolution gas chromatograph/high resolution mass detector (HRGC/HRMS), which gave accurate and precise data for estimations of international trend and comparisons. Average daily intakes (ADIs) of all analytes were calculated. The median level of total indicator PCBs was 14 ng/g lipid, which is significantly lower than the level found in individuals from other countries. PCB congeners 138, 153 and 180 accounted for about 65% of the sum of the indicator congeners analyzed. The concentration of the most abundant PCB 153 is positively correlated with the concentration of the sum indicator PCBs (p<0.001). In this study, concentrations of total indicator PCBs significantly decreased with increasing number of children for a mother, indicating that parity and breast-feeding period an important role in the accumulation and elimination of these compounds in lactating women. The ADI for the median of total indicator PCBs for an infant was evaluated at $0.077{\mu}g/kg{\cdot}bw/day$ from birth to 6 months of age. The present study shows that concentrations of PCB 118 primipara breast milk have decreased 25~35 since 1998, and that this trend is continuing.

A sensitive analytical method for determination of 3-monochloropropane-1,2-diol and 1,3-dichloropropan-2-ol in various foods by gas chromatography with mass spectrometer (가스크로마토그래피/질량분석기를 이용한 식품 중 클로로프로판올 화합물 분석)

  • Kim, Eunju;Park, Sungkug;Choi, Dongmi
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.543-552
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    • 2008
  • This paper described the relatively sensitive and simultaneous analytical method for 3-monochloropropane-1,2-diol (3-MCDP, $C_3H_7ClO_2$, MW. 110) as well as 1,3-dichloropropan-2-ol (1,3-DCP, $C_3H_6Cl_2O$, MW. 128) in various foods. Food samples were homogenized in 5M NaCl solution, mixed with aluminum oxide and eluted with dichloromethane. The extracted chloropropanols were concentrated by rotary evaporator and $N_2$ blow serially were derivatized with HFBA (Heptafluorobutyric anhydride, $C_8F_{14}O_3$, MW. 410) and were determined by GC/MS using isotope dilution method. The characteristic molecular ions at m/z 253, 275, 289, 291, and 453 for HFBA derivatives of 3-MCPD (MW. 502) and 110, 275, and 277 for HFBA derivatives of 1,3-DCP (MW. 325) were chosen in selected ion mode. The method validation data showed sufficiently good properties of LOD (0.003 mg/kg), LOQ (0.010 mg/kg), linearity ($R^2{\geq}0.999$ at 0.010~1.000 mg/kg), and recovery rate (${\approx}97%$). The levels of chloropropanols in soy sauce, sauces, processed meat products, fishery products, and seasonings (n=56/157) determined by the presented method were 0.0~0.3 mg/kg.

Background effect on the measurement of trace amount of uranium by thermal ionization mass spectrometry (열이온화 질량분석에 의한 극미량 우라늄 정량에 미치는 바탕값 영향)

  • Jeon, Young-Shin;Park, Yong-Joon;Joe, Kih-Soo;Han, Sun-Ho;Song, Kyu-Seok
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.487-494
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    • 2008
  • An experiment was performed for zone refined Re-filament and normal (nonzone refined) Re-filament to reduce the background effect on the measurement of low level uranium samples. From both filaments, the signals which seemed to come from a cluster of light alkali elements, $(^{39}K_6)^+$, $(^{39}K_5+^{41}K)^+$ and $PbO_2$ were identified as the isobaric effect of the uranium isotopes. The isobaric effect signal was completely disappeared by heating the filament about $2000^{\circ}C$ at < $10^{-7}$ torr of vacuum for more than 1.5 hour in zone refined Refilaments, while that from the normal Re-filaments was not disappeared completely and was still remained as 3 pg. of uranium as the impurities after the degassing treatment was performed for more than 5 hours at the same condition of zone refined filaments. A threshold condition eliminating impurities were proved to be at 5 A and 30 minutes of degassing time. The uranium content as an impurity in rhenium filament was checked with a filament degassing treatment using the U-233 spike by isotope dilution mass spectrometry. A 0.31 ng of U was detected in rhenium filament without degassing, while only 3 pg of U was detected with baking treatment at a current of 5.5 A for 1 hr. Using normal Re-filaments for the ultra trace of uranium sample analysis had something problem because uranium remains to be 3 pg on the filament even though degassed for long hours. If the 1 ng uranium were measured, 0.3% error occurred basically. It was also conformed that ionization filament current was recommended not to be increased over 5.5 A to reduce the background. Finally, the contents of uranium isotopes in uranium standard materials (KRISS standard material and NIST standard materials, U-005 and U-030) were measured and compared with certified values. The differences between them showed 0.04% for U-235, 2% for U-234 and 2% for U-236, respectively.