• 한국해양학회지:바다
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• 제21권2호
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• pp.78-90
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• 2016

본 보고는 2014년 수행된 해양환경공정시험기준의 제정/개정(안)작성의 전체과정에 대한 안내 보고이다. 제정/개정(안) 작성과정은 수요자 설문조사, 인증표준물질(CRM) 분석을 통한 QA/QC 확인절차, 전문가 자문회의 3단계로 수행되었다. 이번 제정/개정(안) 작성과정에서 다섯 가지 주요 개선방안은 다음과 같다. 첫째, 해양환경 특유의 시료채취, 운반, 보관, 및 전처리에 관한 상세한 내용이 추가되었고, 둘째, 유기물질의 항목별 분석방법에서 되도록 동일한 초자기구와 유기용매를 사용할 수 있도록 편의성을 추구하였으며, 셋째, 인증표준물질(CRM) 분석과정을 통하여 QA/QC 검정을 수행함으로써 신뢰성을 확보하였으며, 넷째, 다양하고 새로운 정량기기에 대한 사용방법을 기술함으로써 편의성을 제고하였고, 다섯째, 분석절차를 쉽게 기술함으로써 사용자의 범위를 넓혔다. 이런 노력을 통해 향후 기대효과는 첫째, 철저한 QA/QC 과정을 거침으로써 국제적인 수준의 신뢰성과 동등성을 확보하고, 둘째, 사용자의 폭을 넓힘으로써 국가표준으로서 신뢰성과 대표성을 갖도록 하였다. 이번 제정/개정(안)에 포함하지 못한 몇 가지 내용은 향후 관련기관과 협조를 통해 조속히 해결될 수 있을 것으로 기대한다.

• 분석과학
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• 제21권4호
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• pp.316-325
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• 2008

연속흐름주입-수소화물생성-유도결합플라스마질량분석장치를 사용하여 바닷물시료중의 비소를 분석하였다. 두 종류의 바닷물표준시료인 CASS-4, NASS-5를 사용하여 측정값과 인증값을 비교함으로써 본 분석법의 정확성을 확인하였다. 분석결과 CASS-4의 경우 $1.17{\pm}0.07{\mu}g/L$ (인증값 $1.11{\pm}0.16{\mu}g/L$), NASS-5의 경우 $1.24{\pm}0.08{\mu}g/L$ (인증값 $1.27{\pm}0.12{\mu}g/L$)의 값을 얻었다. 이는 각각 독립적으로 5회 측정된 결과의 확장불확도로 표시된 결과이며 CASS-4의 경우 6.2%, NASS-5의 경우 6.8%이었으며 모두 인증값의 불확도 범위안에 있었다. 검량선의 기울기와 바탕값의 표준편차로부터 구한 $As^+$ (m/z=74.9216)의 검출한계는 0.01 ug/kg이었다. 검량선의 직선성은 매우 양호하였다. ($R^2=1$). DRC gas로 산소기체를 사용하여 $AsO^+$ (m/z=90.9165)로 검출하는 방법을 사용하여 결과를 비교하였으며 분석감도는 약 25배 정도 감소하였으나, 검량선의 직선성이 매우 잘 나타났으며, 분석결과도 $As^+$(m/z=74.9216)로 검출할 때와 동일한 결과를 얻을 수 있었다.

• Carbon letters
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• 제26권
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• pp.43-50
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• 2018

In this research, a novel and efficient quinoline thioacetamide functionalized magnetic graphene oxide composite ($GO@Fe_3O_4@QTA$) was synthesized and utilized for dispersive magnetic solid phase preconcentration of Cd(II) and Ni(II) ions in urine and various food samples. A number of diverse methods were employed for characterization of the new nanosorbent. The design of experiments approach and response surface methodology were applied to monitor and find the parameters that affect the extraction performance. After sorption and elution steps, the concentrations of target analytes were measured by employing FAAS. The highest extraction performance was achieved under the following experimental conditions: pH, 5.8; sorption time, 6.0 min; $GO@Fe_3O_4@QTA$ amount, 17 mg; 2.4 mL $1.1mol\;L^{-l}$ $HNO_3$ solution as the eluent and elution time, 13.0 min. The detection limit is 0.02 and $0.2ng\;mL^{-1}$ for Cd(II), and Ni(II) ions, respectively. The accuracy of the new method was investigated by analyzing two certified reference materials (sea food mix, Seronorm LOT NO 2525 urine powder). The interfering study revealed that there are no interferences from commonly occurring ions on the extractability of target ions. Finally, the new method was satisfactorily employed for rapid extraction and determination of target ions in urine and various food samples.

• Bulletin of the Korean Chemical Society
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• 제24권3호
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• pp.285-290
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• 2003

An analytical method for the simultaneous determination of trace Ge, As and Se in biological samples by inductively coupled plasma/mass spectrometry has been investigated. The effects of added organic gas into the coolant argon gas on the analyte signal were studied to improve the detection limit, accuracy and precision. The addition of a small amount of methane (10 mL/min.) into the coolant gas channel improved the ionization of Ge, As and Se. The analytical sensitivity of the proposed Ar/CH₄system was superior by at least two-fold to that of the conventional Ar method. In the present method, the detection limits obtained for Ge, As and Se were 0.014, 0.012 and 0.064 ㎍/L, respectively. The analytical reliability of the proposed method was evaluated by analyzing the certified standard reference materials (SRM). Recoveries of 99.9% for Ge, 103% for As, 96.5% for Se were obtained for NIST SRM of freeze dried urine sample. The proposed method was also applied to the biological samples.

• 대한화학회지
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• 제57권5호
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• pp.568-573
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• 2013

A selective and sensitive method for simultaneous determination of copper in blood by adsorptive differential pulse cathodic stripping voltammetry is presented. The procedure involves an adsorptive accumulation of Cu(II)-ETSC (4- ethyl-3-thiosemicarbazide) on a hanging mercury drop electrode, followed by a stripping voltammetry measurement of reduction current of adsorbed complex at about -715 mV. The optimum conditions for the analysis of copper (II) ion are : pH 10.3, concentration of 4-ethyl-3-thiosemicarbazide $3.25{\times}10^{-6}$ M and an accumulation potential of -100 mV. The peak current is proportional to the concentration of copper over the range 0.003-125 ng/mL with a detection limit of 0.001 ng/mL and an accumulation time of 60 s. Moreover, with the use of the proposed method, there is a considerable improvement in the detection limit, the linear dynamic range and the deposition time, compared with the methods of adsorptive stripping voltammetry for the determination of copper. The developed method was validated by analysis of whole blood certified reference materials.

• Nuclear Engineering and Technology
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• 제27권2호
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• pp.234-247
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• 1995

Trace elements in airborne particulates were analyzed by instrumental neutron activation analysis (INAA) under the optimum analytical condition. Neutron irradiation for sample was done at the irradiation hole(neutron flux 1$\times$10$^{13}$ n/$\textrm{cm}^2$.s) of TRIGA MARK-III research reactor in the Korea Atomic Energy Research Institute. For the verification of the analytical method, NIST SRM-1648 and NIES CRM No.8 ore chosen and analyzed. The accuracy and precision of the analysis of 40 and 24 trace elements in the samples were compared with the certified and reported values, respectively. The analytical method was found to be reliable enough when the analytical data of NIES sample were compared with those of different counties. In the analytical result of two or both of standard reference materials, relative standard deviation wes within the 15％ except a few elements and the relative error was within the 10％. We used this method to analyze 30 trace elements in airborne particulates collected with the high volume air sampler(PM-10) at too different locations and also confirmed the possibility to use this method as a routine monitoring tool to find out environmental pollution sources.

• Nuclear Engineering and Technology
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• 제36권5호
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• pp.450-459
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• 2004

For the evaluation of emission sources by air sampling, airborne particulate matter for fine (<2.5 ${\mu}m2$ EAD : $PM_{2.5}$) and coarse partical (2.5-10 ${\mu}m2$ EAD : $PM_{2.5-10}$ fractions were collected using a Gent stacked filter unit low volume sampler and two types of polycarbonate filters. Air samples were collected twice monthly at two regions in and around Daejeon city in the Republic of Korea from January to December 2002. Monthly mass concentration of $PM_{2.5}$ and $PM_{2.5-10}$ were measured and the concentrations of 10 marker elements (Al, Sc, Ti ; Na, Cl ; As, V. Sb, Br, Se) were determined by an instrumental neutron activation analysis. Analytical quality control was corried out using certified reference materials. Enrichment factors were also calculated from the monitoring data to classify the anthropogenic and crustal origins.

• 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.

• 대한화학회지
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• 제38권6호
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• pp.411-417
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• 1994

난용성 신소재 중의 하나인 파인 세라믹의 분석을 위하여, 알칼리 용융법과 고압 산분해법 등의 시료 전처리법을 유도결합원자발광분석기(ICP-AES)를 이용하여 연구하였다. Al2O3 분말을 분석하여 본 결과, 고압 산분해법이 알칼리 용융법보다 재현성 있는 측정치를 얻을 수 있었다. SiC분말의 경우에서는 고압산분해법으로 처리한 후 Si매트릭스를 Si-F형태로 증발시켜서 분석하여 본 결과 분말 중의 ppm 농도 범위의 불순물들이 매트릭스에 의한 간섭없이 분석되었다. 일본 인증기준물인 JCRM022, JCRM023 초미립 분말을 고압 산분해법으로 분석하여 본 결과, 좋은 재현성과 높은 정확성을 나타내었다.

• 분석과학
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• 제20권3호
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• pp.183-192
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• 2007

최근의 전기전자제품 중 유해물질규제지침(RoHS)이나 폐전기전자제품 처리 지침(WEEE) 등의 각종 환경규제는 국제교역에 있어 실질적인 무역장벽으로 작용하고 있다. 한국표준과학연구원(KRISS)에서는 이와 같은 환경규제와 관련하여 국내시험연구기관 및 관련산업체실험실의 측정 신뢰성 확보를 위한 숙련도 시험을 실시하였다. 참여기관은 국내 전기전자 제품 및 자동차 관련 실험실 31개소이다. 숙련도시험용 시료는 pellet type 폴리프로필렌 소재 2 종이며, 측정대상원소는 유럽공동체의 RoHS 지침에서 규정하고 있는 6개 성분 중 카드뮴 (Cd)과 납 (Pb)이다. 시료는 2006년 9월 1일 각 참여실험실에 우편 송부하였으며 10월 10일까지 측정 결과를 접수하였다. 각 실험실의 측정 결과는 KRISS 기준값과의 비교, Robustic Z-score, Youden plot 등에 의해 비교 평가하고 전처리 방법에 따른 측정 결과도 비교 검토하였다. 전반적으로 기준값과의 10% 범위 내에서 일치되는 결과를 보고하였으나 일부 실험실은 심각한 bias를 보이고 있어 측정결과의 신뢰성 향상을 위한 품질보증 시스템을 갖추어야 할 필요가 있다.