• Title/Summary/Keyword: 시료전처리

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Sample Preparation Method for Perfluorochemicals with LC-Tandem Mass Spectrometry in Agricultural Water (LC-Tandem Mass Spectrometry를 활용한 농업용수 중 Perfluorochemicals 분석시료 전처리법)

  • Kim, Jin Hyo;Jin, Cho-Long;Choi, Geun-Hyoung;Park, Byung-Jun
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.1-4
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    • 2015
  • The current official perfluorochemicals (PFCs) analysis method is established with hydrophilic-lipophilic balance (HLB) solid phase extraction (SPE) clean-up method with LC-tandem mass spectrometry ($MS^n$). Herein the HLB clean-up method from the official method by Korean government was modified with Envi-Carb$^{TM}$ to improve the clean-up efficiency for agricultural water and the unexpected UV disturbance in the water was effectively removed by the adsorbent treatment without a significant disturbance of quantitation. And quadrupole time of flight mass spectrometry (qTOFMS) was suggested to the available $MS^n$ instruments for the residue analysis of PFCs based on the ng/L of quantitation limits in water as well.

Characteristics and Sampling of Dioxins/Furans from Emission Gas and Fly Ash Produced in Municipal Waste Incinerator (도시 소각로 쓰레기 소각후 생성된 폐가스 및 비산재중에 포함된 다이옥신류의 측정 및 특성고찰)

  • Lim, Chae-Hyun;Kim, Hee-Taik;Sohn, Jung-Hyun;Chang, Yoon-Seok
    • Applied Chemistry for Engineering
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    • v.8 no.5
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    • pp.790-795
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    • 1997
  • Polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofuransfurans are the archetype of toxic chemicals. So it has absorbed public attention. The majors primary sources of PCDDS and PCDFs are chemical, thermal and photochemical reactions. Municipal solid waste incinerator facilities has been reported as the major contributors of dioxins to the environment. In this paper, Dioxins and furans were examined emission gas and fly ash produced during combustion in municipal solid waste incinerator. More effective method for sampling, extraction was described. The sample was extracted using a soxhlet method and purified using silicagel, alumina and carbon fibre HPLC to remove interfering compound. The extract was then analyzed by HRGC/HRMS. The result of this study showed recovery standard was good and the data resembled those of thermal processes. Total dioxins and furans were $1076.20pg/Nm^3$ and $1452.34pg/Nm^3$ respectively. The amount of highly chlorinated compound was more than that of lowly chlorinated compound. The 2,3,7,8-substituted TCDD was Just 0.34% of the total dioxins/furans amount.

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Quantitative Analysis and Qualification of Amitrole Using LC/ESI-MS (LC/ESI-MS를 이용한 아미트롤의 정성확인 및 정량분석)

  • Park, Chan-Koo;Eo, Soo-Mi;Kim, Min-Young;Sohn, Jong-Ryeul;Mo, Sae-Young
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.117-129
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    • 2004
  • Amitrole in environment, difficult to be analyzed by GC or GC/MS due to high polarity and low volatility, was analyzed by LC/ESI/MS in the study. Maximum peak intensity of amitrole in LC/MS/ESI mass spectrum is m/z 85 of protonated molecular ion $(M+H)^+$ with 30V of cone voltage at SIR mode. It was confirmed that ratios between main ion of amitrole, 85 of protonated molecular ion, and m/z 58 fragmented ion of amitrole, had increased corresponding with the increment of cone voltage from 20V to 70V. The isotope molecular weight of amitrole was $86([M+H])^+$ at LC/MS analysis and the mass spectrum ratio between 85 mass and 86 mass was not different by the change of concentration but similar to theoretical ratio(less than 10% standard deviation).The linearity of standard calibration curve under same condition with sample treatment method had $y=1.09354e^6X+26947.2$ and $r^2=0.99$. Recovery rates in water and soil samples were 77.64~83.44% and 71.11~79.44%, respectively. Reliability of the analysis was performed with 5 repeated measurements at each level of standard concentration and the result showed that relative standard deviation was less than 10%; therefore, the extraction and analysis method in the study suggested that it would be reliable to measure amitrole in water and soil media.

Effects of Thawing Conditions in Sample Treatment on the Chemical Properties of East Siberian Ice Wedges (동시베리아 얼음쐐기 시료의 해동방법이 시료의 화학적 특성분석에 미치는 영향)

  • Subon Ko;Jinho Ahn;Alexandre Fedorov;Giehyeon Lee
    • Economic and Environmental Geology
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    • v.55 no.6
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    • pp.727-736
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    • 2022
  • Ice wedges are subsurface ice mass structures that formed mainly by freezing precipitation with airborne dust and surrounding soil particles flowed through the active layer into the cracks growing by repeating thermal contractions in the deeper permafrost layer over time. These ice masses characteristically contain high concentrations of solutes and solids. Because of their unique properties and distribution, the possibility of harnessing ice wedges as an alternative archive for reconstructing paleoclimate and paleoenvironment has been recently suggested despite limited studies. It is imperative to preserve the physicochemical properties of the ice wedge (e.g., solute concentration, mineral particles) without any potential alteration to use it as a proxy for reconstructing the paleo-information. Thawing the ice wedge samples is prerequisite for the assessment of their physicochemical properties, during which the paleo-information could be unintentionally altered by any methodological artifact. This study examined the effect of thawing conditions and procedures on the physicochemical properties of solutes and solid particles in ice wedge samples collected from Cyuie, East Siberia. Four different thawing conditions with varying temperatures (4 and 23℃) and oxygen exposures (oxic and anoxic) for the ice wedge sample treatment were examined. Ice wedge samples thawed at 4℃ under anoxic conditions, wherein biological activity and oxidation were kept to a minimum, were set as the standard thawing conditions to which the effects of temperature and oxygen were compared. The results indicate that temperature and oxygen exposure have negligible effects on the physicochemical characteristics of the solid particles. However, the chemical features of the solution (e.g., pH, electric conductivity, alkalinity, and concentration of major cations and trace elements) at 4℃ under oxic conditions were considerably altered, compared to those measured under the standard thawing conditions. This study shows that the thawing condition of ice wedge samples can affect their chemical features and thereby the geochemical information therein for the reconstruction of the paleoclimate and/or paleoenvironment.

Effects of Modified Atmosphere Packaging on the Quality of Chitosan and $CaCl_2$ Coated Mushroom (Agaricus bisporus) (환경가스조절 포장이 키토산 및 $CaCl_2$로 코팅 처리된 양송이 버섯의 품질에 미치는 영향)

  • Lee, Jin-Sil
    • Korean Journal of Food Science and Technology
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    • v.31 no.5
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    • pp.1308-1314
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    • 1999
  • The effects of modified atmosphere(MA) packaging and coating on the quality of mushroom (Agaricus bisporus) were investigated. Whole mushrooms(100 g) were packed with polyvinyl chloride(PVC) film wrap, PD941 and PD961 film bags and were stored in a chamber at $12^{\circ}C$ and 80% RH for 6 days. Gas composition of packages, respiration rate, weight loss, color and maturity index of MA packaged mushrooms were examined. The wrap packaged mushrooms showed different level of internal $CO_2$ concentrations among water washed, chitosan coated and $CaCl_2$ coated subgroups significantly at 5% level. The maximum $CO_2$ concentration of PD941 and PD961 packages for all coated showed $4.1{\sim}4.7%$ and $10.4{\sim}11.7%$, respectively, for the first day. PD961 package showed the lowest $O_2$ concentration compared to other groups. There were no significant respiration rate differences between wrap packed and PD941 packaged. Respiration rate of water washed. chitosan coated and $CaCl_2$ coated in PD961 packaged was 192 mg, 226 mg and 245 mg, respectively. Maturity index of PD961 packaged were not significantly different among the water washed, chitosan and $CaCl_2$ coated packages. Chitosan coating showed a negative effect on color change of mushrooms. The weight loss of 961 packaged was lower $(7.0{\sim}8.0%)$ that those of wrap packaged and PD941 packaged.

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Error factors and uncertainty measurement for determinations of amino acid in beef bone extract (사골농축액 시료 중에 함유된 아미노산 정량분석에 대한 오차 요인 및 측정불확도 추정)

  • Kim, Young-Jun;Kim, Ji-Young;Jung, Min-Yu;Shin, Young-Jae
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.125-134
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    • 2013
  • This study was demonstrated to estimate the measurement uncertainty of 23 multiple-component amino acids from beef bone extract by high performance liquid chromatography (HPLC). The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, standard solution, calibration curve, recovery and repeatability) in associated with the analysis of amino acids were evaluated. The estimation of uncertainty obtained on the GUM (Guide to the expression of uncertainty in measurement) and EURACHEM document with mathematical calculation and statistical analysis. The content of total amino acids from beef bone extract was 36.18 g/100 g and the expanded uncertainty by multiplying coverage factor (k, 2.05~2.36) was 3.81 g/100 g at a 95% confidence level. The major contributors to the measurement uncertainty were identified in the order of recovery and repeatability (25.2%), sample pretreatment (24.5%), calibration-curve (24.0%) and weight of the reference material (10.4%). Therefore, more careful experiments are required in these steps to reduce uncertainties of amino acids analysis with a better personal proficiency improvement.

Study on the Synthesis Method of Simulated CRUD for Chemical Decontamination in NPPs (원전 화학제염을 위한 모의크러드 제조방법 연구)

  • Kang, Duk-Won;Kim, Jin-Kil;Kim, Kyeong-Sook
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.8 no.2
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    • pp.91-97
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    • 2010
  • As nuclear power plants are getting older, interests on a decontaminating process are increasingly attracting more attention. Chemical decontamination is crucial to lower the production of radioactive waste and radiation dose rate. Prior to this, oxidizers and detergents for target material should be chosen so as to decontaminate major systems and components of a nuclear power plant chemically. In order to decontaminate it properly, it is crucial to have information about the chemical composition and crystalline structure of CRUD, analyzing its samples from the target or the decontamination system with components. However, there is no program which enables the extraction of samples directly from the object or the decontamination system with components carrying genuine radioactivity. Therefore, it is limited to samples from corrosion products carrying partial radioactivity as a resource. The composition of CRUD varies considerably depending on refueling cycle because it is closely related to the constituent of basic material. After settling a target, it is crucial to analyze and obtain analytical information about CRUD as a decontamination target. In this paper, various technologies for manufacturing simulated CRUD are introduced as alternatives to unattained samples. A metal oxide or metal hydroxide was used to synthesize simulated cruds having chemical compositions and crystalline stricture similar to the actual one by 12 different methods. CRUD 4(metal oxides in the autoclave vessel) and CRUD 10(metal oxides in a crucible after hydrazing pretreatment)were chosen as the best method for Type 1 and Type 2.respectively. As these CRUD can be synthesized easily without using any specialized equipment or reagents in a short time and in large quantities, they are expected to stimulate the development of decontaminating agents and processes.

Analysis of Minimum Detectable Activity Concentration of Water Samples and Evaluation of Effective Dose (물 시료의 최소검출가능 농도 분석과 유효선량 평가)

  • Jang, Eun-sung;Kim, Yang-su;Lee, Sun-young;Kim, Jung-Soo
    • Journal of the Korean Society of Radiology
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    • v.14 no.7
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    • pp.857-862
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    • 2020
  • In March 2011, a tsunami off Japan caused radioactive material that had seeped into the sea from the Fukushima nuclear accident to flow to the Pacific Ocean, causing pollution to sea life. For a comparative evaluation with the area surrounding the site of a nuclear power plant by the release of radioactive materials, an area 20 to 30 km away from the emergency protection plan area was selected as a comparative point considering weather conditions, population distribution, etc. In addition, the government intends to analyze the minimum detection radiation received by residents around the nuclear power plant and evaluate the effective dose. Analysis of tritium radiation from water samples showed that most of the samples were not detected and that 0.0014 % to 0.777 % of the annual legal standard of 1 mSv for the general public had little effect on the human body. Therefore, the measurement and analysis of water samples around the nuclear power plant site is expected to help relieve anxiety, such as exposure to the general public and neighboring residents due to radiation release.

Comparison of Flavor-related Components of Polygonatum odoratum in Root by Growth Year (둥글레 근경의 연근별 향미관련 성분의 비교)

  • Park, Nan-Young;Jeong, Yong-Jin;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.35 no.1
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    • pp.28-32
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    • 2003
  • As part of studies on the high quality dunggule tea, made of Polygonatum odoratum root with different growth year were analyzed for their flavor compounds. The quality attributes related to flavors were compared between raw and roasted samples which were treated at $130^{\circ}C$ for 15 min. Free sugars in the roots were mainly composed of fructose ($3.59{\sim}4.83%,\;d.b.$), sucrose ($1.78{\sim}2.49%$), and glucose ($1.60{\sim}1.80%$). Threonine ($1,239{\sim}1,444\;mg/100g,\;d.b.$), arginine ($589{\sim}689$), histidine ($289{\sim}370$) were three major free amino acids. The root grown for three years showed the highest content in total free sugar and amino acids (p<0.05). There was negligible difference in proximate composition and Hunter's color parameter depending on the growth year of the roots. However, sensory scores on color, taste and aroma were highest in 3 years' root, which is found most suitable for the preparation of dunggule tea. The roasting of 3 years old root significantly reduced the content of fructose and sucrose (p<0.01). It caused most apparent changes in the decreasing amount of threonine and in the decreasing rate of lysine, showing the significant decrease in total free amino acid content (p<0.01).

The Effects of Cocoon Deguming on the Process of Floss Silk and Hand Spun Silk (견사의 정련조건이 제면 및 수방견사질에 미치는 영향)

  • 이인전
    • Journal of Sericultural and Entomological Science
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    • v.17 no.2
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    • pp.171-173
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    • 1975
  • This experiment was conducted to study the reasonable deguming method of cocoon on the Boss silk making. The results obtained are as follows: 1. Reasonable deguming method of cocoon on the floss silk making was observed to be about 0.75% Na$_2$SiO$_3$, 2% NaCO$_3$ solution during 40 minutes boiling Process. 2. Treatment 6 increased qualities of floss silk and hand spun silk as compared with the other conventional method.

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