• 제목/요약/키워드: Mass standards

검색결과 467건 처리시간 0.02초

수소화물 발생-유도결합플라스마 질량분석법에 의한 철강 중의 납의 정량 (Determination of Lead in Steels by Hydride generation-Inductively Coupled Plama/Mass Spectrometry)

  • 박창준;송선진;이동수
    • 분석과학
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    • 제14권5호
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    • pp.410-415
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    • 2001
  • 철강 시료 중의 납 분석을 위하여 수소화물 발생법을 플라스마에 납을 선택적으로 주입하고 유도결합플라스마 질량분석법으로 측정하는 분석법을 개발하였다. 납 수소화물 $PbH_4$의 생성을 위해서는 $NaBH_4$와 반응 전에 먼저 준안정 상태의 Pb(IV)로 만들어주기 위하여 산화제가 필요하다. $1000{\mu}g/mL$ 이상의 철 매질을 함유하는 시료용액으로 납 수소화물을 발생시키기 위한 최적조건을 찾는 연구를 수행하였다. 철 매질이 $10{\mu}g/mL$ 이상 존재할 때는 $K_2Cr_2O_7$이 효과적인 산화제로 작용하였으며 젖산을 가하여 감도를 향상시켰다. 시료용액의 산농도 그리고 산화제와 젖산 농도의 최적값은 철 매질의 농도에 따라 달랐다. 동위원소 희석법을 사용하여 납을 정량하였으며 철강 표준물질 NIST SRM 361, 362 분석결과는 불확도 범위안에서 검정값과 잘 일치하였다.

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Characterization of Forest Fire Emissions and Their Possible Toxicological Impacts on Human Health

  • Kibet, Joshua;Bosire, Josephate;Kinyanjui, Thomas;Lang'at, Moses;Rono, Nicholas
    • Journal of Forest and Environmental Science
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    • 제33권2호
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    • pp.113-121
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    • 2017
  • In flight particulate matter particularly emissions generated by incomplete combustion processes has become a subject of global concern due to the health problems and environmental impacts associated with them. This has compelled most countries to set standards for coarse and fine particles due to their conspicuous impacts on environment and public health. This contribution therefore explores forest fire emissions and how its particulates affects air quality, damage to vegetation, water bodies and biological functions as architects for lung diseases and other degenerative illnesses such as oxidative stress and aging. Soot was collected from simulated forest fire using a clean glass surface and carefully transferred into amber vials for analysis. Volatile components of soot were collected over 10 mL dichloromethane and analyzed using a QTOF Premier-Water Corp Liquid Chromatography hyphenated to a mass selective detector (MSD), and Gas Chromatograph coupled to a mass spectrometer (GC-MS). To characterize the size and surface morphology of soot, a scanning electron microscope (SEM) was used. The characterization of molecular volatiles from simulated forest fire emissions revealed long chain compounds including octadec-9-enoic acid, octadec-6-enoic acid, cyclotetracosane, cyclotetradecane, and a few aromatic hydrocarbons (benzene and naphthalene). Special classes of organics (dibenzo-p-dioxin and 2H-benzopyran) were also detected as minor products. Dibenzo-p-dioxin for instance in chlorinated form is one of the deadliest environmental organic toxins. The average particulate size of emissions using SEM was found to be $11.51{\pm}4.91{\mu}m$. This study has shown that most of the emissions from simulated forest fire fall within $PM_{10}$ particulate size. The molecular by-products of forest fire and particulate emissions may be toxic to both human and natural ecosystems, and are possible precursors for various respiratory ailments and cancers. The burning of a forest by natural disasters or man-made fires results in the destruction of natural habitats and serious air pollution.

Determination of isoquinoline alkaloids by UPLC-ESI-Q-TOF MS: Application to Chelidonium majus L.

  • Jeong, Won Tae;Lim, Heung Bin
    • 분석과학
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    • 제30권6호
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    • pp.379-389
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    • 2017
  • In this study, we set up an analytical method that can be used for rapid and accurate determination of representative isoquinoline alkaloids in medicinal plants using UPLC-ESI-Q-TOF MS (ultra pressure liquid chromatography-electrospray ionization-quadrupole-time-of-flight mass spectrometry). The compounds were eluted on a C18 column with 0.1 % formic acid and acetonitrile, and separated with good resolution within 13 min. Each of the separated components was characterized by precursor ions (generated by ESI-Q-TOF) and fragment ions (produced by collision-induced dissociation, CID), which were used as a reliable database. We also performed method validation: analytes showed excellent linearity ($R^2$, 0.9971-0.9996), LOD (5-25 ng/mL), LOQ (17-82 ng/mL), accuracy (91.6-97.4 %) as well as intra- and inter-day precisions (RSD, 1.8-3.2 %). In the analysis of Chelidonium majus L., magnoflorine, coptisine, sanguinarine, berberine and palmatine were detected by matching retention times and characteristic fragment ion patterns of reference standards. We also confirmed that, among the quantified components, coptisine was present in the highest quantity. Furthermore, alkaloid profiling was carried out by analyzing the fragment ion patterns corresponding to peaks of unknown components. In this manner, protopine, chelidonine, stylopine, dihydroberberine, canadine, and nitidine were tentatively identified. We also proposed the molecular structure of the fragment ions that appear in the mass spectrum. Therefore, we concluded that our suggested method for the determination of major isoquinoline alkaloids by UPLC-Q-TOF can be useful not only for quality control, but also for rapid and accurate investigation of phytochemical constituents of medicinal plants.

High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Won-Woong;Lee, Sun-Young;Yu, Se Mi;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제33권11호
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    • pp.3727-3734
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    • 2012
  • An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.

기체크로마토그래피/동위원소 희석 질량분석법을 이용한 토양 중 폴리브롬화 디페닐에테르의 분석법 (Determination of Polybrominated Diphenyl Ethers(PBDEs) in Soil using Gas Chromatography/Isotope Dilution Mass Spectrometry)

  • 나윤철;장윤석;김해동;홍종기
    • 분석과학
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    • 제17권1호
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    • pp.29-36
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    • 2004
  • 본 연구에서는 토양중에 존재하는 폴리브롬화 디페닐에테르 (polybrominated diphenyl ethers, PBDEs)를 동위원소희석법을 이용한 기체크로마토그래피/질량분석기-선택이온검색법에 의해 검출하는 분석방법을 소개하였다. 토양 중 PBDEs는 속실렛 장치로 추출하고 실리카와 플로리실 흡착제를 이용한 고체상 추출법을 비교하였다. 정제 후 추출물은 기체크로마토그래피/질량분석기-선택이온검색방법으로 분석하였으며, 동위원소로 치환된 4종의 PBDEs를 내부표준물질로 이용한 동위원소 희석법으로 8종의 PBDEs를 정량하였다. 속실렛추출 후 플로리실과 실리카 카트리지를 통한 회수율은 각각 30.8~110.8%, 44.4~110.7%이었다. 이 분석법의 검출한계는 0.04~0.3 ng/g로 나타났다.

LC-MS/MS를 이용한 조피볼락 근육에서 구충제 febantel 및 그 대사체들의 정량분석을 위한 시료 전처리 방법의 비교 분석 (Comparison of sample preparation methods for quantification of febantel, an anthelmintic agent, and its metabolites in rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry)

  • 임재웅;권인영;김태호;김위식;강소영
    • 한국어병학회지
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    • 제34권2호
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    • pp.261-269
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    • 2021
  • This study presents the evaluation of sample extraction and purification procedure for the determination of residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfone in rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different sample preparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service (FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each method was compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities (coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveries from FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higher recoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition, FSIS-Q showed a good linearity over the range of 2.5~200 ㎍/kg, and excellent sensitivities with limit of detection of 0.46~0.71 ㎍/kg and limit of quantification of 1.08~2.15 ㎍/kg. Although all the sample preparation methods turned out to be able to meet CODEX guideline for all the compounds, FSIS method and FSIS-Q validated in this study could be applied to screening and quantification for residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

자율운항선박 육상원격제어사 교육과정 개발에 관한 연구 (A Study on the Development of a Curriculum for Shore Remote Control Officer in Maritime Autonomous Surface Ship (MASS))

  • 박한규;김상희;하민재
    • 해양환경안전학회지
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    • 제28권6호
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    • pp.1002-1012
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    • 2022
  • 4차 산업이 발전함에 따라 해상운송 분야에서도 자율운항선박의 연구가 진행되고 있다. 현재 2, 3단계의 자율운항선박이 운항을 하고 있으며 육상에서 원격조종의 장비로 감시하며 상황에 따라 운항에 개입하는 육상원격제어사가 이미 활용되고 있다. 하지만 이들의 교육과정이 국제적으로 정립되지 않아 부적격한 육상원격제어사에 의한 사고 위험성이 높아지고 있다. 본 논문에서는 육상원격제어사에 필요한 교육을 기존의 해기사 교육 중 육상원격제어사에게 필요한 교육과 원격제어환경에서 필요한 교육으로 구성하였고 효과적인 교육의 활용을 위해 비기술적 역량교육을 포함하였다. 이러한 교육과정은 신속하게 활용될 수 있으며 역량평가를 통한 해사안전에 부합하는 신규 육상원격제어사를 배출할 수 있다. 그리고 기존의 선원들도 육상원격제어사로 전직할 수 있는 교육을 제공할 수 있다.

In vitro anti-Trypanosoma cruzi activity of methanolic extract of Bidens pilosa and identification of active compounds by gas chromatography-mass spectrometry analysis

  • Gabriel Enrique Cazares-Jaramillo;Zinnia Judith Molina-Garza;Itza Eloisa Luna-Cruz;Luisa Yolanda Solis-Soto;Jose Luis Rosales-Encina;Lucio Galaviz-Silva
    • Parasites, Hosts and Diseases
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    • 제61권4호
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    • pp.405-417
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    • 2023
  • Chagas disease, caused by Trypanosoma cruzi parasite, is a significant but neglected tropical public health issue in Latin America due to the diversity of its genotypes and pathogenic profiles. This complexity is compounded by the adverse effects of current treatments, underscoring the need for new therapeutic options that employ medicinal plant extracts without negative side effects. Our research aimed to evaluate the trypanocidal activity of Bidens pilosa fractions against epimastigote and trypomastigote stages of T. cruzi, specifically targeting the Brener and Nuevo León strains-the latter isolated from Triatoma gerstaeckeri in General Terán, Nuevo León, México. We processed the plant's aerial parts (stems, leaves, and flowers) to obtain a methanolic extract (Bp-mOH) and fractions with varying solvent polarities. These preparations inhibited more than 90% of growth at concentrations as low as 800 ㎍/ml for both parasite stages. The median lethal concentration (LC50) values for the Bp-mOH extract and its fractions were below 500 ㎍/ml. Tests for cytotoxicity using Artemia salina and Vero cells and hemolytic activity assays for the extract and its fractions yielded negative results. The methanol fraction (BPFC3MOH1) exhibited superior inhibitory activity. Its functional groups, identified as phenols, enols, alkaloids, carbohydrates, and proteins, include compounds such as 2-hydroxy-3-methylbenzaldehyde (50.9%), pentadecyl prop-2-enoate (22.1%), and linalool (15.4%). Eight compounds were identified, with a match confirmed by the National Institute of Standards and Technology (NIST-MS) software through mass spectrometry analysis.

표현매체로서 SNS(Social Network Service)에 대한 내용규제의 문제점 분석: 법률적.행정적 규제를 중심으로 (The Analysis of Content Regulation on Social Network Service(SNS): Focusing on the Problem of Legal and Administrative Regulation)

  • 황용석
    • 한국언론정보학보
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    • 제58권
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    • pp.106-129
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    • 2012
  • 이 글은 SNS의 보편적 이용이 늘어나고 그것에 대한 규제논의가 증가하는 것을 배경으로 해서, SNS 표현물에 대한 현행 국내 규제체계의 문제점을 분석하고자 한다. 이를 위해 규제대상으로서 SNS표현물의 성격을 살펴보고, SNS 표현물에 대한 국내 내용규제체계의 문제점을 법률적 측면과 규제기관적 차원에서 검토했다. SNS 표현물에 대한 규제체계를 살펴보면, 법률과 행정기구 중심의 국가주의적 규제경향이 강하다는 것을 알 수 있다. 5가지 측면의 규제법률이 SNS 표현물 규제와 연계되어 있으며, 규제의 주체로서 행정기구가 내용심의를 하고 있음을 알 수 있었다. 그로 인해 민간영역의 자율기능은 상대적 약한 것으로 판단된다. SNS와 같은 인터넷공간에는 최소규제의 원칙이 적용되어야 하며, 규제에 적용되는 불법의 정의도 명확히 하고 그것의 판단주체 및 규제대상을 최소화해야 한다. 현재의 행정기구로서 방송통신심의 위원회 구조에 대한 본질적인 고민이 필요하다.

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Practical Application of Lead-free Solder in Electronic Products

  • Cho Il-Je;Chae Kyu-Sang;Min Jae-Sang;Kim Ik-Joo
    • 한국마이크로전자및패키징학회:학술대회논문집
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    • 한국마이크로전자및패키징학회 2004년도 ISMP Pb-free solders and the PCB technologies related to Pb-free solders
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    • pp.93-99
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    • 2004
  • At present, LG Electronics pushes ahead to eliminate the Pb(Lead) -a hazardous material- from all products. Especially, we have performed to select the optimum standard composition of lead free alloy for the application to products for about 3 years from 2000. These days, we have the chance for applying to the mass-production. This project constructed the system for applying the lead free solders on consumer electronic products, which is one of the major products of the LG Electronics. To select the lead free solders with corresponding to the product features, we have passed through the test and applied with Sn-3.0Ag-0.5Cu alloy system to our products, and for the application to the high melting temperature composition, we secured the thermal resistance of the many parts and substrate and optimized the processing conditions. We have operated the temperature cycling test and the high temperature storage test under the standards to confirm the reliability of the products. On these samples, we considered the consequence of our decision by the operating test. For the long life time of the product, we have operated the temperature cycling test at $-45^{\circ}C-+125^{\circ}C$, 1 cycle/hour, 1000 cycles. Also we have tested the tin whisker growth about lead free plating on lead finish. We have analyzed with the SEM, EDS and any other equipment for confirming the failure mode at the joint and the tin whisker growth on lead free finish.

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