실시간 모드의 유도결합플라즈마 질량분석기술을 이용한 금속나노입자의 분석

김현아 ( Hyun A Kim ),나소영 ( So Young Na ),이병태 ( Byung Tae Lee ),김경웅 ( Kyoung Woong Kim ),이우춘 ( Woo Chun Lee ),김순오 ( Soon Oh Kim ),이병천 ( Byoung Chun Lee ) 한국환경분석학회 2013 환경분석과 독성보건 Vol.16 No.4

나노입자의 환경 유출에 따른 인체 및 생태계에 미치는 독성 문제가 제기됨에 따라 나노입자의 환경 안정성에 대한 우려가 증대되고 있다. 다양한 나노 연구분야중에서도 환경 시료 내 나노입자의 검출 및 분석에 대한 연구가 최우선과제로 인식되고 있다. 유도결합플라즈마 질량분석기(ICP-MS)는 무기물질에 대한 정확하고 정밀한 분석기술로서, 환경 시료 내에 존재하는 금속나노입자의 검출을 위한 유망한 분석기술이다. 이에, 본 연구에서는 실시간 모드의 유도결합플라즈마 질량분석기술(RTSP-ICP-MS)의 원리 및 분석절차를 소개하였으며, 구연산(citrate)으로 코팅된 은나노입자를 대상으로 분석기술의 적용 가능성을 평가하였다. RTSP-ICP-MS 분석 결과, 60 nm와 100 nm 은나노입자의 입자수 기준(number-weighted) 평균 크기는 53.0±7.4 nm와 103.6±13.8 nm였다. RTSP-ICP-MS 분석결과를 검증하기 위해 전자투과현미경(TEM) 분석을 실시한 결과 입자의 평균크기는 각각 60.1±3.7 nm와 96.8±9.5 nm였고, 동적산란기(DLS) 분석을 통한 z-average 값은 59.1±0.2 nm와 95.3±0.8 nm로 나타났다. 다양한 기술을 적용한 은나노입자의 크기분석 결과를 통해 RTSP-ICP-MS 기술을 이용한 금속나노입자의 분석가능성을 검증하였다. 향후, 다양한 환경 매질(담수, 폐수, 슬러지, 퇴적물 및 토양 등)내에 존재하는 금속나노입자의 검출 및 분석을 위한 향후 연구가 필요하다. Significant concern has been laid on the environmental safety of nanoparticles due to their exposure and toxicity to human and ecosystems. Among the research topics, detection and analysis of nanoparticles in the environmental matrix is regarded as the most important and pressing work. Owing to its precise and accurate analytical power to inorganics, inductively coupled plasma mass spectrometry (ICP-MS) is a very promising tool to detect metal nanoparticles in the environmental samples. Here, we introduced the principles and procedures of on Realtime Single Particle mode ICP-MS (RTSP-ICP-MS) technique and evaluated its applicability to citrate-coated silver nanoparticles (AgNPs). RTSP-ICP-MS determined AgNPs of 60 nm and 100 nm to 53.0 ±7.4 nm and 103.6±13.8 nm, respectively, which were the number-weighted average sizes. Comparative measurements suggested that sizes by Transmission Electron Microscopy (TEM) were 60.1±3.7 nm and 96.8±9.5 nm and z-averages by Dynamic Light Scattering (DLS) were 59.1±0.2 nm and 95.3±0.8 nm, respectively. The results prove the feasibility of RTSP-ICP-MS for metal-nanoparticles. We have many challenges to be overcome for detection and measurement of metal nanoparticles in environmental samples such as fresh water, wastewater, sludges, sediments and soils.

주거환경 중 다환방향족탄화수소(PAHs) 분석방법 제시를 위한 연구

고상호,임태숙 한국환경분석학회 2019 환경분석과 독성보건 Vol.22 No.4

In this study, methods of extraction, purification, and instrumental analysis are validated for 16 types of polycyclic aromatic hydrocarbons (PAHs) defined by the United States Environmental Protection Agency (US EPA), to analyze their occurrence during cooking in residential environments. Accelerated solvent extraction (ASE), which is more efficient than other extraction methods, are used and the recovery rate of gaseous samples (excluding NaP) and particulate samples was 80-110% with a relative standard deviation (RSD) of 0.6-19.8%. The purification method was compared with the column and the cartridge purification, with recovery rates of 80-110% and 60-100%, respectively. Through this process, a high recovery rate of the 16 substances was confirmed by the column purification method after ASE. The rate was 78-102% (RSD: 0.3-10%) for the gas samples and 73.7-101.7% (RSD: 0.7-20%) for particulate samples, respectively. The recovery rate of the analytical method used in this study was 66.6-80.2% (RSD: 4.7-8.3%) in the gas phase samples and 72.5-97% (RSD: 5.1-10.1%) in the particulate samples. As a result, it seems reasonable to apply the analytical method proposed in this study to real sample analyses.

용매추출에 의한 매질제거와 동위원소희석 유도결합플라스마 질량분석법에 의한 침적토양표준물질중의 Cu, Zn 및 Ni의 분석

서정기 ( Jung Ki Suh ) 한국환경분석학회 2005 환경분석과 독성보건 Vol.8 No.2

환경 중 의약품 분석방법에 관한 고찰

장태수 ( Tae Soo Jang ),홍영민 ( Young Min Hong ),권오성 ( Oh Sung Kwon ),김현욱 ( Hyun Ook Kim ) 한국환경분석학회 2009 환경분석과 독성보건 Vol.12 No.2

국내 SRF 사용시설의 배출가스 내 바이오매스 함량 분석방법 연구- 용해선별법과 탄소동위원소 질량분석법 비교

권준화,권영현,유하녕,고영재,전태완,신선경,강준구 한국환경분석학회 2019 환경분석과 독성보건 Vol.22 No.4

Carbon dioxide produced from biomass is biogenic. It is considered to be neutral carbon, and is therefore excluded from calculations of greenhouse gas emissions. In Korea, methods for calculating greenhouse gas emissions are categorized into Tiers 1 to 4, according to emission activities. Emissions measured by the methods in Tiers 1 to 3 are partially excluded from total CO2 emissions according to the proportion of biomass contained in the waste. The Tier 4 method measures CO2 emissions by measuring the amount and composition of the exhaust gas. However, this method does not consider the biomass content. In Tier 4, as in Tiers 1 to 3, it is necessary to partially exclude CO2 emissions from the greenhouse gas emissions in the flue gas according to the biomass ratio. In this study, the biomass content of SRF used in domestic facilities was analyzed using SDM. In addition, the biomass content of the exhaust gas from these facilities was analyzed using AMS. It was found that SRF contains 43.6% biomass on average. Furthermore, it was confirmed that the biomass content of the SRF used in facilities measured by SDM and the biomass content of the exhaust gases measured by AMS were similar.

흡착-열탈착 가스크로마토그래피 질량분석 방법을 이용한 숲속 대기 중 자연적 휘발성 유기화합물 분석에 관한연구

이효정,이경민,김현영,최성민,박범진 한국환경분석학회 2022 환경분석과 독성보건 Vol.25 No.4

Phytoncide, a forest healing indicator, is known to help suppress depression, anxiety, and stress of human. Furthermore, it has positive effects on blood pressures, pulses, and mood fluctuations. Previous studies mostly focused on phytoncide emission trends and its concentration prediction in forest. Moreover, a direct comparison of phytoncide concentrations between existing studies is often challenging owing to the use of differingunits, target analytes, analysis conditions, as well as unreported concentrations per type of the compound. Therefore, this study evaluated the overall performance of adsorption sampling and thermal desorption coupled with gas chromatography to evaluatethe phytoncide concentration in a forest atmosphere. To this end, the analysis quality management and analysis accuracy were evaluated for on-site samples in two different laboratories. The phytoncide analysis results obtained from each laboratory can serve as reference data for the adsorption capture-thermal desorption method applied to biogenic volatile organic compounds.

HPLC/ESI-MS/MS를 이용한 환경 시료중 Estrogens의 분석

서천규 ( Cheon Kyu Seo ),명승운 ( Seung Woon Myung ) 한국환경분석학회 2010 환경분석과 독성보건 Vol.13 No.3

Trace concentrations of estrogens such as 17β-estradiol (E2), 17α-estradiol (αE2), estrone (E1), estriol (E3), and 17α-ethinylestradiol (EE2) may have adverse effects on humans and the aquatic ecosystem. The environmental analysis of estrogens at physiologically active concentrations (low ng/L) requires the use of very sensitive and selective method. An analytical procedure for the simultaneous determination of five steroid estrogens in an aqueous environmental sample is described. The procedure includes solid phase extraction/clean-up with C18 cartridge, and analysis by liquid chromatography/tan dem mass spectrometry of five estrogens. After 500 mL of sample loading on C18 cartridge, sample was eluted with acetonitrile and dryness. The reconstituted analytes were separated on HPLC system with 0.1% formic acid and acetonitrile followed by analyzed using (-) electrospray ionization-mass spectrometer with multiple reaction monitoring mode. In the range of 0.05-1 ng/mL, the calibration curves were showed the good linearities (above r2=0.99). The limits of detection and limits of quatitation estimated for the estrogens in blank surface water were the concentration range of 0.055~0.154 ng/mL and 0.184~0.514 ng/mL, respectively. The absolute recovery, precision (intra-day) and accuracy in the low, medium and high (0.005~1.0 ng/mL) were in the range of 69.5~95.1%, 0.4~7.9% (RSD) and -9.1~9.3% (bias), respectively.

다검출기 유도결합 플라즈마 질량분석기를 이용한 스트론튬 동위원소비 분석법 개선

이신우,박재선,박현우,황종연,김금희,정현미,최종우 한국환경분석학회 2018 환경분석과 독성보건 Vol.21 No.4

Strontium (Sr) commonly exists in rock, groundwater, soil, plants, and animals. The Sr isotope ratio offers important information as a tracer on nature because the Sr isotopic composition is not fractionated by any biological process in these ecosystems. Hence, Sr isotope ratio has been used in several studies on tracing the Sr source for contaminated sites and human migration. In this study, we developed a separation method for Sr content, and then improved Sr isotope analysis using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). A powdered rock standard (NIST 2710a) was used to determine the removal of interference elements (Rb and Ca) and the recovery rate of Sr content. The results ranged from 98% to 106%. Additionally, three standard samples (NBS 987, IAPSO and NIST 1486) were analyzed to evaluate the precision and accuracy of the results. The measured 87Sr/86Sr ratio for all the samples were consistent with the reported values, within an error. These results indicate that our established Sr separation and Sr isotope measurement methods are reliable and can hence be useful in the fields of environmental and forensic sciences.

환경규제 대응을 위한 페인트 중의 중금속 분석용 인증 표준물질 개발

유병규,선일식 한국환경분석학회 2018 환경분석과 독성보건 Vol.21 No.4

In the areas of RoHS, WEEE, ELV and REACH, reinforcement of environmental regulations against harmful substances is a global trend not only in EC but also in all over the world. In the fields of Korea's major export products such as material parts, electrical and electronic products and automobile parts, we are responding to these regulations consistently. To develop reference material for analyzing lead and cadmium in paints, the candidate materials were produced through the screening process which separated shapes and sizes. To secure the traceability of the candidate materials produced, the characteristics and uncertainties are estimated by ICP-AES analysis using the primary reference material. The short-term and long-term stabilities also are evaluated in parallel. In order to calculate the final certification value of the candidate material, the verification were carried out by the performance evaluation through the comparison among the KOLAS (Korea Laboratory Accreditation Scheme) laboratories, and the CRM was produced in accordance with ISO Guide 35. The certified values and uncertainties of Pb and Cd of the final paint standard, determined according to the joint analysis among laboratories, are Pb [(191.4±3.1) mg/kg, (944.1±5.6) mg/kg] and Cd [(45.0±2.6) mg/kg, (225.5± 3.5) mg/kg]. These standard materials were developed to enhance the reliability of measurement analysis, including the validity and traceability of measurement results. Also it is expected that the CRM will be used as QCM (quality control material) for the product design and the process monitoring, so that regulation and management of hazardous heavy metals can be systematically implemented.

고분해능 질량분석장치를 이용한 동시분석법 1. 수계의 유기인계 농약-1

최재원 ( Jae Won Choi ),김윤석 ( Yun Seok Kim ) 한국환경분석학회 2010 환경분석과 독성보건 Vol.13 No.4

A gas chromatography-high resolution mass spectrometry (GC-HRMS) method with solid-phase extraction has been developed for the quantitation of organophosphorous pesticides in surface water. Target compounds in this study were bromacil, cyanazine, dichlorovos (DDVP), metribuzin, phorate, propazine, trifluralin, edifenphos, molinate, iprobenfos (kitazine), diazinon, parathion ethyl, fenitrothion, parathion methyl, simazine and chlorpyrifos. Prior to sample analysis, solid-phase extraction was optimized using RP-1, FL-PR, C18, PESTICIDE, ENVI18 and LRC-SI. The result of the recovery test showed there was no ideal SPE cartridge to produce over 80% recovery. The order of recoveries was RP-1>PESTICIDE>C18>ENVI18>FL-PR>LRCSI. The use of a 5% acetone in dichloromethane helped to increase the recovery rates for some pesticides. Method detection limits of HRMS using RP-1 ranged from 2.2 to 11 ng/L for all of target compounds. The method was applied to the measurement of organophosphorus pesticide residues in surface water (n=56) from Han River. Major pesticides detected in the samples were iprobenfos (nd~160 ng/L), chlorpyrifos (nd~10 ng/L) and others with the low ranges of ng/L. Higher concentrations for these compounds were observed in sites close to highly populated or agricultural area. The use of HRMS with optimized SPE provides increasing sensitivity of detection for target compounds.