• Journal of Preventive Medicine and Public Health
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• 제28권4호
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• pp.863-873
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• 1995

This report describes a preperation and characterization of canine blood lead(Pb) standard reference material(SRM). Three adult beagle dogs(A, B, and C)were orally dosed with gelatin capsules containing $Pb(NO_3)_2$, equivalent to $10\sim80mg$ Pb/kg body weight. Blood was drawn 24 hours after the dose from the cephalic vein into lead free 500ml Pyrex beaker in which EDTA.K was contained as an anticoagulant. The amount of lead given to individual dog was varied arbitrarily. Three month later, 3 canine animals were orally dosed with lead secondarily to make mixed SRM(D1) which was mixed different concentrations of lead in bloods with A1, B1, and C1 in vitro. The SRMs for A, B, C, A1, B1, C1, and D1 were distributed 2ml each into more than 300 lead free bottles, and were stored in refregerator at $4^{\circ}C$. The amount of lead in canine whole blood samples were determined using a Varian 30A atomic absorption spectrophotometer(AAS) with a model GTA-96 graphite tube atomizer with D2 background correction and a Hitachi Z-8100 AAS with Zeeman background correction. The sensitivity and detection limits for lead determination of Varian 30A were $0.46{\mu}g/L,\;0.34{\mu}g/L,\;and\;0.56{\mu}g/L,\;0.14{\mu}g/L$ of Hitachi Z-8100, respectively. Day to day variations in determination of blood lead concentration in a certain sample were $31.11{\pm}1.36{\mu}g/100ml$ by Varian 30A, and $33.08{\pm}0.82{\mu}g/100ml$ by Hitachi Z-8100, showing the difference of 3% between the two results. At the blood lead concentrations of $56.31{\pm}1.98{\mu}g/100ml(A),\;40.89{\pm}0.80{\mu}g/100ml(B),\;59.01{\pm}1.38{\mu}g/100ml(C)$, the precisions of replicated measurements by AAS were 3.52%, 1.96%, and 2.34%, respectively. Coefficient variation(CV) of SRMs(A, B, and C) within a standard sample were ranged from 0.92% to 7.50%, and those between 5 standard samples were 1.21%, 2.64%, and 1.11%, respectively, showing inter-vial variation of $1{\mu}g/100ml$. Lead levels in SRMs during one month storage were unchanged. The overall recoveries were $89.6\sim100.4%,\;91.6\sim101.9%,\;90.3\sim100.0%$ for A, B, and C SRMs, means were $56.46{\pm}2.69{\mu}g/100ml,\;39.35{\pm}1.89{\mu}g/100ml,\;57.40{\pm}2.31{\mu}g/100ml$, and measurement ranges were$52.88{\pm}59.26{\mu}g/100ml,\;37.47{\pm}41.68{\mu}g/100ml,\;54.80{\pm}60.69{\mu}g/100ml$, respectively. Those results were laid within confidence limits values. The lead concentrations in the mixed sample(D1) stored over one month period were ranged from $32.76{\mu}g/100ml\;to\;33.54{\mu}g/100ml$, with CV ranging from 1.2% to 2.7%. The results were similiar to each of single samples(A1, B1, and C1) in respect of homogeneity and stability. Results of the mixed blood sample analysed after 1 month storage at $4^{\circ}C$ by four other laboratories(L1, L2, L3, L4) were similar with those of our laboratory($L5;31.18{\pm}0.24{\mu}g/100ml$, acceptable range by $CDC;25.18\sim37.18{\mu}g/100ml$), showing the concentrations of $25.91{\pm}1.19{\mu}g/100ml(L1),\;34.16{\pm}0.22{\mu}g/100ml(L2),\;35.68{\pm}0.85{\mu}g/100ml(L3),\;30.95{\pm}0.46{\mu}g/100ml(L4)$ in a each samples.

• 자원환경지질
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• 제49권2호
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• pp.89-95
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• 2016

산화 환원 환경에 민감하게 분별되는 몰리브덴(Mo) 안정동위원소는 지구화학적 과정을 유추할 수 있는 지시자로 사용될 수 있다. 최근 분석기기의 발달로 Mo 동위원소를 활용한 지질물질 연구가 많이 보고되고 있지만, 국내에서는 Mo 동위원소에 관한 연구가 없었다. 이번 연구에서는 컬럼관(BioRad PolyPrep(R) column, 10 ml)과 음이온 교환수지(BioRad Resin AG(R) 1-X8, 200-400 mesh)를 이용한 두 번에 걸친 컬럼 작업을 통해 Mo을 분리 및 회수하였다. 이 분리법을 이용하여 고체(BHVO-2, SDO-1, PACS-2) 및 액체(IAPSO) 표준시료의 Mo 동위원소 분석을 다검출기 유도결합 플라즈마 질량분석기(Multi-collector Inductively Coupled Plasma Mass Spectrometer; MC-ICP-MS)로 측정한 결과, 측정된 표준물질의 Mo 동위원소 분석값은 참값과 오차 범위 내에서 잘 일치하였다.

• Bulletin of the Korean Chemical Society
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• 제31권7호
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• pp.1976-1980
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• 2010

A simple and reliable method has been developed to selectively separate and concentrate trace amounts of Fe(III) ions from water and food samples by using flame atomic absorption spectrometry. A new reagent, 5-hydroxy-4-ethyl-5,6-di-pyridin-2-yl-4,5-dihydro-2H-[1,2,4] triazine-3-thione, was synthesized and characterized by using FT-IR spectroscopy and elemental analysis. Effects of pH, concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of Fe(III) were investigated. The optimum pH was found to be 5. Eluent for quantitative elution was 10 mL of 2 M HCl. The preconcentration factor of the method, detection limit (3s/b, ${\mu}gL^{-1}$) and relative standard deviation values were found to be 25, 4.59 and 1%, respectively. In order to verify the accuracy of the method, two certified reference materials (TMDA 54.4 lake water and SRM 1568a rice flour) were analyzed. The results obtained were in good agreement with the certified values. The method was successfully applied to the determination of Fe(III) ions in water and food samples.

• 자원환경지질
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• 제27권5호
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• pp.469-477
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• 1994

Many researchers have investigated most representative sequential extraction method using various reagents for determining the chemical forms of metals in soils and sediments. In this paper, a newly modified method for sequential extraction scheme based on Tessier's method by Environmental Geochemistry Research, Centre for Environmental Technology, Imperial College, was introduced and examined. In comparison with Tessier's method, originally designed for sediment analysis by Atomic Absorption Spectrophotometry (AAS), the sequential extraction scheme has been developed for the multi-element analysis by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The partitioning of particulate trace elements was classified into five fractions: (i) exchangeable, (ii) bound to carbonates or specially adsorbed, (iii) bound to Fe and Mn oxides, (iv) bound to organic matter and sulphides and (v) residuals. The experimental results of the pilot study for in-house reference material (HRM2) and certified international standard reference material (SRM2711) using the modified method showed not only reasonable precision and accuracy but also acceptable overall recovery rates. In addition, mine dump soils sampled in the Dalsung Cu-W mine, Korea were prepared and sequentially extracted using the method. Most of Cu was bound to organic matter/sulphides and residual fractions. The dominant fraction of soil Pb and Zn in the study area was found in the residuals. The fraction of Cd showed a wide variation between samples and could be found bound to the carbonates or specially adsorbed, oxides, organic fraction and residuals. The recovery rates of Cd, however, were poor due to relatively low Cd concentrations in soils. The heavy metals in these mine dumps appear to be in the more inert forms and should not be readily bioavailable. The soils, however, had very low pH values (average 4.1) and had sandy textures; consequently, rapid infiltration of rainfall may increase leaching of Zn and Cd which were found to be around 5 to 10% of the exchangeable fraction. As a result of the investigation of this study, it has been strongly recommended that these mine waste materials should still be considered a significant contaminant source and will need environmental remediation to prevent pollutants from being released into the environment.

• 한국대기환경학회지
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• 제16권5호
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• pp.453-467
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• 2000

The aim of this research is to collect and characterize fine particles (FPM:$\leq$2.5${\mu}{\textrm}{m}$) and coarse particles (CPM: 2.5~10${\mu}{\textrm}{m}$) using a low volume air sampler provided by the IAEA, at urban (Taejon) and rural area(Wonju) for a period of about two years(April 1996 to May 1998) and to promote a use of nuclear analytical techniques for air pollution studies. For the collection of airborne particulate matter (PM(sub)10), the Gent stacked filter unit sampler and polycarbonate membrane filters were employed. The concentration of trace elements in collected APM samples were determined byu instrumental Neutron Activation Analysis. For validation of the analytical data, internal quality control were implemented by using both the comparison of the analytical results of standard reference materials(NIST SRM 1648) and interlaboratory comparison for proficiency test (NAT-3). The standard uncertainty was less than 15% and Z-score of two samples were within $\pm$1. The monitoring of (PM(sub)10) mass concentration and elemental concentrations were carried out weekly. The average mass concentration of (PM(sub)10) in urban and rural areas were 59.2$\pm$36.5$\mu\textrm{g}$/㎥ and 41.4$\pm$23.7$\mu\textrm{g}$/㎥, respectively. To investigate the emission source, the enrichment factors were calculated for the fine and coarse particle fractions at two sites, respectively and these values were classified for anthropogenic and soil origin elements.

• 대한지하수환경학회지
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• 제5권2호
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• pp.116-121
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• 1998

환경의 오염 및 보존에 대한 연구에 적용하기 위한 원소의 조성이 다른 퇴적물 시료중의 33종의 원소농도를 중성자방사화분석을 이용하여 정량하였다. 분석법의 검증과 평가를 위해 3종의 표준물질(NIST SRM 2종과 NRCC CRM 1종)을 선정하여 분석의 정밀도 및 정확도를 측정하고 보증값과 비교함으로서 분석절차를 평가하였고, 최적의 분석조건을 조사하므로서 실제 시료에 적용하기 위한 분석절차를 확립하였다. 시료의 중성자 조사는 한국원자력연구소의 연구용원자로(TRIGA MARKIII & HANARO, neutron flux, 1-3$\times$$10^{13}$n/$\textrm{cm}^2$.s)를 이용하였다. 추가로, 앞에서 정해진 분석절차에 따른 퇴적물 분석의 정확성 및 신뢰도를 확인하기 위해 두 가지 IAEA의 퇴적물 시료를 분석하여 Al, As, Co, Cr, Fe, Sb, Zn 등의 함량값을 XRF, ICP-MS, AAS에 의한 분석결과와 상호비교하였으며, 비교적 잘 일치하였다.

• Nuclear Engineering and Technology
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• 제32권5호
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• pp.477-484
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• 2000

To estimate the degree of intake of $^{238}$ U and $^{232}$ Th through daily diet, a Korean mixed diet sample was prepared after the investigation of the amount of consumption of the daily diet which corresponds to the age of 20 to 60 years. For the analysis of U and Th, the RNAA method was applied. Two standard reference materials were used for quality control and assurance and the analytical results were compared with a certified value. The determination of U and Th in the Korean mixed diet sample was carried out under the same analytical conditions and procedures with SRM. It is found that the concentration of U and Th in a Korean mixed diet was about 35.4 ppb and 3.4 ppb. From these results, the daily intake of $^{238}$ U and $^{232}$ Th by diet is evaluated to be 6.98 and 0.67 $\mu\textrm{g}$ per day, respectively. Radioactivities related to the intake of $^{238}$ U and $^{232}$ Th were estimated to be about 86 mBq and 27 mBq per person per day and the annual dose equivalents from $^{238}$ U and $^{232}$ Th revealed as 3.18 $\mu$Sv and 0.29 $\mu$Sv per person, respectively.

• 한국식생활문화학회지
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• 제37권6호
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• pp.540-546
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• 2022

This study aimed to determine the changes in the vitamin B₅ content of raw and cooked vegetables. The nineteen vegetables were subjected to different cooking methods, viz. blanching, boiling, pan-broiling, and steaming. Vitamin B₅ was quantified by reversed-phase high-performance liquid chromatography (HPLC) using photodiode-array (PDA) detection (200 nm). The standard reference materials (SRM) were used to validate the accuracy of vitamin B₅ measurement method used in this study. The cooking yields ranged from 82.63 to 107.62% and decreased in most of the vegetables except bitter melon, curled mallow, and eggplant. The raw kabocha squash, Danhobak, had the highest vitamin B₅ content (0.671 mg/100 g) among the samples. All cooked vegetables showed lower vitamin B₅ content compared to the raw samples. The true retention ranged from 0% (crown daisy, blanching) to 84.49% (kabocha squash, steaming). These results indicate that vitamin B₅ is degraded after cooking. Pan-broiling and steaming are better cooking methods than the others for retaining vitamin B₅. The true retention of vitamin B₅ in the samples markedly depends on the cooking method and food matrix. These results can be used as important basic data for nutritional evaluation of meals.

• 분석과학
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• 제16권5호
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• pp.391-398
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• 2003

하나로의 즉발감마선 방사화분석 장치를 이용하여 생물시료중의 붕소의 정량을 위한 기초연구를 수행하였다. 측정조건에 대한 특성조사를 위해 시료에 대한 중성자 조사 위치에서 중성자속 및 균질도를 측정하였다. 시료위치에서 열중성자 빔의 크기가 $2{\times}2cm^2$ 되도록 집속하였으며, 측정된 선속은 $1.0{\sim}6.5{\times}10^7n{\cdot}cm^{-2}{\cdot}s^{-1}$ 범위를 나타냈으며, 중심부로부터 반경 4.5 mm 이내 및 9 mm 이내에서 각각 $5.77{\pm}0.71{\times}10^7n{\cdot}cm^{-2}{\cdot}s^{-1}$, $4.68{\pm}1.64{\times}10^7n{\cdot}cm^{-2}{\cdot}s^{-1}$이었다. 따라서 양질의 균일한 조사를 위해서 시료의 크기를 10 mm 이내로 조정하였다. 검출 시스템은 컴프턴 산란에 의한 백그라운드 요인을 억제하고 분석감도를 높이기 위해 설계되었으며, 감마선 계측 시스템의 에너지 교정과 컴프턴 억제율을 조사하기 위해 NaCl 표준체를 이용하여 단일 및 컴프턴 모드로 백그라운드를 측정하였다. 또한 정확한 붕소의 측정을 위해 시료의 매질효과로서 발생하는 분광학적 Na의 472 keV 피이크에 대한 간섭효과를 결정하였으며, 세 가지 인증표준물질 (NIST SRM 1570a, 1547, 1573a)을 이용한 붕소농도 측정시험을 두 가지 모드로 실시한 후 결과를 비교하였다.

• 분석과학
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• 제25권1호
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• pp.25-32
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• 2012

동위원소희석 액체크로마토그래피-탄뎀질량분석법을 이용하여 차음료 중의 소르빈산을 정밀하게 측정하는 방법을 개발하였다. 소르빈산의 동위원소, $^{13}C_2$-소르빈산은 주문합성하여 구입하였다. 질량 분석기는 음이온 모드로 선택반응분석법 (Selected Reaction Monitoring mode)에서 수행하여, $[M-H]^-$ 이온이 $[M-CO_2H]^-$ 조각이온으로 가는 m/z 111 ${\rightarrow}$ 67와 $^{13}C_2$-소르빈산 m/z 113 ${\rightarrow}$ 68 채널을 선택하여 분석하였다. 분리는 C18 컬럼으로 수행되었으며, 암모니움 아세테이트용액(pH 4.5) 55%와 메탄올 45%로 이동상을 구성하였다. 반복성과 재현성을 포함한 방법의 유효성 검토를 위하여 본 연구원에서 차음료에 소르빈산을 강화하여 균질성있는 기준물질을 제조하였다. 반복성과 재현성 결과는 동위원소희석 액체크로마토그래피-탄뎀질량분석법에 의한 소르빈산의 분석이 신뢰할만 하며 재현성 있는 방법임을 보여주었고, 기준물질들의 소르빈산의 농도는 3.8%의 표준편차를 보여주었다.