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.

한국 남서해 환경보전해역의 표층퇴적물 내 중금속 오염

정희호 ( Hui Ho Jeong ),김동우 ( Dong Wu Kim ),( Nguyen Hoang Lam ),최태봉 ( Tae Bong Choi ),조현서 ( Hyeon Seo Cho ) 한국환경분석학회 2017 환경분석과 독성보건 Vol.20 No.2

Gamak Bay, Deukryang Bay, and Doam Bay were designated as Environmental preservation sea areas for conservation of fishery resources by the Korean government. It is essential to maintain the chemical status of these environments, particularly for heavy metals that pose potential risks to fishery resources. This study was, therefore, carried out to investigate the concentration distribution and potential risk of seven heavy metals, namely Cd, Cr, Cu, Zn, Pb, As, and Hg present in the surface sediments (n = 116) of these sea areas during March and August 2009. The metal concentrations in the sampling sites was found to be highly variable. The dominant metals were Zn (mean = 118.22 mg/kg) for Gamak Bay, Cr (mean = 19.07 mg/kg) for Dyukryang Bay, and Zn (mean = 39.07 mg/kg) for Doam Bay. Overall, the order of the target metals was Zn > Cr > Pb > Cu > As > Hg > Cd. Additionally, the metal concentrations were categorized as less than Igeo Class 2 `Moderately polluted`; except for As determined during March in Gamak Bay. As had concentrations that categorized it under Igeo Class 3 `Moderately/strongly polluted`.

다중 검출 유도결합 플라즈마 질량분석기를 이용한 납 및 카드뮴안정동위원소비 분석의 질량 편향 보정방법 비교

김지영 ( Jee Young Kim ),김명진 ( Myung Jin Kim ),유은진 ( Eun Jin Yoo ),이강현 ( Kang Hyun Lee ),이경석 ( Kyoung Seok Lee ),이원석 ( Won Seok Lee ),최종우 ( Jong Woo Choi ),권오상 ( Oh Sang Kwan ) 한국환경분석학회 2014 환경분석과 독성보건 Vol.17 No.3

To obtain precise and accurate isotope ratios with a multi-collector ICP-MS, three methods such as interelementalinternal calibration, sample-standard bracketing (SSB), and log-log linear regression correction model were applied to isotope ratio measurement of lead (Pb) and cadmium (Cd) for the correction of instrumental mass discrimination. Certified reference materials including NIST SRM 981 (Pb), NIST SRM 3108(Cd), and BAM I012 (Cd) were used as reference materials for the isotope ratios of lead and cadmium to compare the corrected results obtained from the respective correction models. The accuracies of lead isotope ratio measurements were in the range of -0.002 (207/206Pb) to -0.035 (208/204Pb) % when the inter-elemental internal calibration applied. The same range of -0.002 (207/206Pb) to -0.035 (208/204Pb) % was also found with the SSB method. The log-log linear regression correction model, on the other hand, showed a different range of -2.160 (207/206Pb) to 0.219 (208/204Pb) %. The precisions of lead isotope ratios with these three correction methods ranged from 0.027 (206/204Pb) to 0.127 (208/204Pb), 0.025 (206/204Pb) to 0.124 (208/204Pb), and1.265 (207/204Pb) to 1.367 (207/206Pb), respectively. Therefore, both of the inter-elemental internal calibration and the SSB method were selected as good methods for mass bias correction of lead isotope ratios. Theε114/110Cd values obtained from the application of the three different correction models were -14.5±0.7 (Agas an internal standard), -13.0±2.1 (SSB), and -15.2±1.8 (log-log linear regression correction model), respectively. For ε114/110Cd values, the inter-elemental internal calibration showed the best precision among the three correction methods. Isobaric interferences with cadmium were also corrected when correction coefficients were applied to each isotope of cadmium. The difference of correction coefficients between the isotope ratios with natural abundances and the empirical ratios in the isobaric interferences reached up to 11%. The heavier isobaric interferences (106, 108, 110Pd vs. 105Pd) were underestimated in the application of the natural ratios, while the lighter isobaric interferences (112,114,116Sn vs. 118Sn and113In vs. 115In) were overestimated. In conclusion, the inter-elemental internal calibration and the SSB method can properly correct the isotope ratios of interest in the isotope ratio measurement using the MC-ICP-MS. Further research on the isotope ratio analysis of environmental samples should follow to improve precision and accuracy.

LC/MS를 이용한 물 환경내의 잔류의약품 분석

김주형 ( Joo Hyung Kim ),박찬구 ( Chan Koo Park ),김민영 ( Min Young Kim ),안승구 ( Seoung Gu Ahn ) 한국환경분석학회 2008 환경분석과 독성보건 Vol.11 No.2

n-butylsilane의 마이크로파 스펙트럼 분석 및 ab initio 계산을 통한 Conformer 분석

김지현 ( Ji Hyun Kim ),가수현 ( Soo Hyun Ka ),오정진 ( Jung Jin Oh ) 한국환경분석학회 2011 환경분석과 독성보건 Vol.14 No.4

Using microwave spectroscopy, many gas molecules have been determined dipole moments, spectroscopic constants, and structure parameters. Through this study, we find out characteristics of gas molecules and these data can be good information about the atmospheric chemical reaction. The spectrum of n-butylsilane, expected to exist in the atmosphere, was analyzed. n-butylsilane has five conformers aa, ag, ga, gg, gg`. All conformers are prolate asymmetric rotors; the kappa value is between -0.96 and -0.99. To assign rotational spectra, the tentative rotational constants were calculated using Gaussian 03. For aa conformer strong a-type transition with J from 3 to 7 were found and assigned. For ag conformer, a-type transitions and some of c-type transitions were found. For ga conformer, a-type transition and some of b-type transitions constants were found. However, the spectra of the gg, gg` conformer were not found. The three rotational, centrifugal distortion constants were determined and the fit was done using Watson`s S reduced Hamiltonian.

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.

온라인 모니터링 시스템의 의한 대기환경오염물질 자동측정분석

김민영 한국환경분석학회 1999 환경분석과 독성보건 Vol.2 No.2

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.

환경분야 시험 · 검사기관 현장평가 결과 분석

황종연,이혜리,고상호,전수아,김지혜,이진주,이경로,박창희,정현미,최종우 한국환경분석학회 2020 환경분석과 독성보건 Vol.23 No.2

The on-site assessment of environmental testing and inspection laboratories is conducted every three years and consists of an evaluation of the operations and technology sectors and an evaluation of eight environmental media. This study analyzed the results of on-site assessments conducted on the environmental testing and inspection laboratories in 2017. The evaluations of the operations and technology sectors showed that it is necessary to supplement the independence of the internal quality control work, the appropriateness of the ability assessment when changing the personnel power and evaluating of equipment, and the verification of testing methods prompted by changes in facilities and equipments. Finally, four were the common points that emerged from the eight assessment areas, namely records management for sampling and experiment, management of laboratory waste, records management for consumables and standard reference materials.

총질소와 총인 수동 및 자동 분석의 비교평가(1) - 총질소 분석

김기동 ( Kee Dong Kim ),허미경 ( Mi Kyung Heo ),서용찬 ( Yong Chan Seo ) 한국환경분석학회 2006 환경분석과 독성보건 Vol.9 No.3