• Title/Summary/Keyword: N-R Method

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Selection of Calibration Approaches and Their Impact on the Quantification of Unknown Samples: Case Study on Reduced Sulfur Gases (환원황화합물의 분석과 검량기준의 선택에 따른 오차발생의 특성)

  • Jo, Hyo-Jae;Hong, One-Feel;Kim, Ki-Hyun
    • Journal of Korean Society for Atmospheric Environment
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    • v.27 no.2
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    • pp.133-141
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    • 2011
  • In this study, different calibration approaches for reduced sulfur compounds (RSCs) were investigated by using thermal desorption coupled with gas chromatography (GC) and pulsed flame photometric detection (PFPD). To evaluate the effects of calibration procedures, gaseous standards of 4 RSCs ($H_2S$, $CH_3SH$, DMS, and DMDS) prepared at 10 ppm level were analyzed at 7 loading injection volumes (40, 60, 80, 100, 160, 240, and 320 ${\mu}L$). The results were then compared with calibration curves made with the Z (zero offset) and N (non-zero offset) method. The concentrations of unknown samples were then quantified by using R (ratio) method in which the slope values are compared between standards and samples. Secondly, in A (average) method, results obtained from a multi-point analysis of unknown samples were also averaged to extract representative values for each sample. Results of both experiments showed that analytical error of low molecular weight components (such as $H_2S$ and $CH_3SH$) was greatly expanded with the Z method. In conclusion, the combined application of N-A method was the more realistic approach to reduce biases in the quantification of RSCs.

Quantitative Analysis of Ellagic Acid in Nymphaea tetragona Georgi Root by HPLC-UVD (HPLC-UVD를 이용한 수련(Nymphaea tetragona Georgi)의 Ellagic Acid 정량 분석)

  • Lee, Dong Young;Jeong, Eun Ju;Jeon, Byung Ju;Sung, Sang Hyun
    • Korean Journal of Pharmacognosy
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    • v.45 no.1
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    • pp.84-87
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    • 2014
  • A high performance liquid chromatography (HPLC) method for the quantitation of ellagic acid in Nymphaea tetragona was developed for the quality control of functional cosmetic ingredient, the extract of N. tetragona. Separation and quantitation were successfully achieved with a Kromasil C18 column ($5{\mu}m$, $250mm{\times}4.6mm$, i.d.) by isocratic elution of a mixture of acetonitrile containing 0.1% trifluoroacetic acid and water containing 0.03% phosphoric acid at a flow rate of 1.0 ml/min. The UV detector was used for the detection and the wavelength for quantitation was set at 254 nm. The presence of ellagic acid in the extract was determined by comparison of retention time and spiking with authentic standard. Analytical results showed good linearity ($R^2=0.99996$) in relatively wide concentration ranges. The R.S.D. for precision test was less than 3.0%. Recovery of the compound was 98.55~101.72% with R.S.D values less than 4.0%. In conclusion, this method has been successfully applied to the determination of ellagic acid in N. tetragona.

Use of Near-Infrared Spectroscopy for Estimating Fatty Acid Composition in Intact Seeds of Rapeseed

  • Kim, Kwan-Su;Park, Si-Hyung;Choung, Myoung-Gun;Jang, Young-Seok
    • Journal of Crop Science and Biotechnology
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    • v.10 no.1
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    • pp.13-18
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    • 2007
  • Near-infrared spectroscopy(NIRS) was used as a rapid and nondestructive method to determine the fatty acid composition in intact seed samples of rapeseed(Brassica napus L.). A total of 349 samples(about 2 g of intact seeds) were scanned in the reflectance mode of a scanning monochromator, and the reference values for fatty acid composition were measured by gas-liquid chromatography. Calibration equations for individual fatty acids were developed using the regression method of modified partial least-squares with internal cross validation(n=249). The equations had low SECV(standard errors of cross-validation), and high $R^2$(coefficient of determination in calibration) values(>0.8) except for palmitic and eicosenoic acid. Prediction of an external validation set(n=100) showed significant correlation between reference values and NIRS estimated values based on the SEP(standard error of prediction), $r^2$(coefficient of determination in prediction), and the ratio of standard deviation(SD) of reference data to SEP. The models developed in this study had relatively higher values(> 3.0 and 0.9, respectively) of SD/SEP(C) and $r^2$ for oleic, linoleic, and erucic acid, characterizing those equations as having good quantitative information. The results indicated that NIRS could be used to rapidly determine the fatty acid composition in rapeseed seeds in the breeding programs for high quality rapeseed oil.

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Process of the Selective Production of 1-Butene through Positional Isomerization from 2-Butenes (2-부텐으로부터 위치 이성화 반응을 통한 선택적 1-부텐의 제조 공정)

  • Ko, MinSu;Jeon, Jong-Ki;Cho, Jungho;Lee, Seong Jun;Lee, Jae Ho
    • Korean Chemical Engineering Research
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    • v.46 no.4
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    • pp.692-696
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    • 2008
  • There is not much method of using C4 Raffinate III, despite having high olefin contents. The majority of the C4 Raffinate III have been converted into n-butane through hydrogenation, and sold as LPG. The C4 Raffinate III is rich 2-butenes with very low isobutene and isobutene contents. The 2-butenes are converted into 1-butene in the vicinity of thermodynamic equilibrium yield through positional isomerization with n-almumina catalyst calcinated at $400{\sim}600^{\circ}C$. The overall process is composed of isomerization-reactor, de-1-buteneizer to prepare the reactants and to enrich reactive products, and 1-butene column to product a high purity 1-butene. The production of 1-butene increases by 40~60 wt% with the selective positional isomerization from the existing separation method.

Low Temperature Sintering Process of Sol-gel Derived Ferroelectric Sr0.9Bi2.1Ta1.8Nb0.2O9 Thin films (Sol-gel 법으로 제조된 강유전체 Sr0.9Bi2.1Ta1.8Nb0.2O9 박막의 저온결정화 공정)

  • 김영준;김병호
    • Journal of the Korean Ceramic Society
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    • v.40 no.3
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    • pp.279-285
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    • 2003
  • Ferroelectric S $r_{0.9}$B $i_{2.1}$T $a_{1.8}$N $b_{0.2}$ thin films with 200 nm thicknesses were deposited on Pt/Ti $O_2$/ $SiO_2$/Si Substrates by a sol-gel method. In these experiments, Sr(O $C_2$ $H_{5}$)$_2$, Bi(TMHD)$_3$, Ta(O $C_2$ $H_{5}$)$_{5}$ and Nb(O $C_2$ $H_{5}$)$_{5}$ were used as precursors, which were dissolved in 2-methoxyethanol. After UV-irradiation and RTA processes, the remanent polarization value (2 $P_{r}$) of SBTN thin films with annealed at $650^{\circ}C$ was 8.49 and 11.94 $\mu$C/$\textrm{cm}^2$ at 3 V and 5 V, respectively.

Effects of HA/TiN Coating on the Electrochemical Characteristics of Ti-Ta-Zr Alloys (Ti-Ta-Zr합금의 전기화학적 특성에 미치는 HA/TiN 코팅의 영향)

  • Oh, Mi-Young;Kim, Won-Gi;Choe, Han-Cheol
    • Korean Journal of Metals and Materials
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    • v.46 no.10
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    • pp.691-699
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    • 2008
  • Electrochemical characteristics of Ti-30Ta-xZr alloys coated with HA/TiN by using magnetron sputtering method were studied. The Ti-30Ta containing Zr(3, 7, 10 and 15wt%) were 10 times melted to improve chemical homogeneity by using a vacuum furnace and then homogenized for 24hrs at $1000^{\circ}C$. The specimens were cut and polished for corrosion test and coating, and then coated with HA/TiN, respectively, by using DC and RF-magnetron sputtering method. The analyses of coated surface and coated layer were carried out by using optical microscope(OM), field emission scanning electron microscope(FE-SEM) and X-ray diffractometer(XRD). The electrochemical characteristics were examined using potentiodynamic (-1,500 mV~ + 2,000 mV) and A.C. impedance spectroscopy(100 kHz ~ 10 mHz) in 0.9% NaCl solution at $36.5{\pm}1^{\circ}C$. The microstructure of homogenized Ti-30Ta-xZr alloys showed needle-like structure. In case of homogenized Ti-30Ta-xZr alloys, a-peak was increased with increasing Zr content. The thickness of TiN and HA coated layer showed 400 nm and 100 nm, respectively. The corrosion resistance of HA/TiN-coated Ti-30Ta-xZr alloys were higher than that of the non-coated Ti-30TaxZr alloys, whic hindicate better protective effect. The polarization resistance($R_p$) value of HA/TiN coated Ti-30Ta-xZr alloys showed $8.40{\times}10^5{\Omega}cm^2$ which was higher than that of non-coated Ti-30Ta-xZr alloys.

Finite Element Analysis on the Strength Safety of a Fuel Tank for Highly Compressed Gas Vehicle (수술실 내의 아산화질소($N_2O$) 노출평가)

  • Baek, Jong-Bae;Uhm, Min-Yong
    • Journal of the Korean Institute of Gas
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    • v.13 no.6
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    • pp.34-38
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    • 2009
  • Nitrous oxide, which is used as an anesthetic gas, has been shown to be a chronic health hazard. It is necessary to monitor and control the nitrous oxide exposure of the operating theaters staff. In this study, N2O exposure level of the operating nurses is assessed with a GC-ECD. The nitrous oxide gas is collected on a molecular sieve 5A contained in a glass tube and desorbed for 12 hours at $100^{\circ}C$ in heating block. As a result of the test using GC-ECD, calibration curve's $R^2$ of $N_2O$ is 0.9992, LOD is $0.96{\mu}g$/injection, LOQ is $3.21{\mu}g$/injection, desorption efficiency is 94.78 4.50% in average and break through is within 10% compared with the concentration. The average concentration before operation is 5.12ppm and it is 42.3ppm during operation. There are a significant difference showing that the P value is lower than 0.05. Assessing exposure level to nitrous oxide based on nurses' working positions, the exposure levels do not show significant difference( P>0.005). And $N_2O$ in active sampling method is higher than passive sampling method(P<0.05).

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Quantitative Ga-67 Scintigraphy in patients with Silicosis: Comparison with Chest X-ray and Pulmonary Function (규폐증에서 Gallium-67 신티그라피의 정량적인 분석: 흉부 X-선과 폐기능검사와의 비교)

  • Shin, Kwang-Hyun;Sohn, Hyung-Sun;Chung, Yong-An
    • The Korean Journal of Nuclear Medicine
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    • v.33 no.4
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    • pp.381-387
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    • 1999
  • Purpose: The International Labor Organization (ILO) has established an international standard for chest X-ray diagnosis of pneumoconiosis since 1980. However, there is a need for improved diagnosis and staging in occupational disease. We evaluated Ga-67 citrate scintigraphy quantitatively and correlated the scintigraphic findings with pulmonary function tests and chest X-ray results. Materials and Methods: Twenty-five patients underwent whole body scintigraphy with additional chest and abdomen images 48 hrs after intravenous injection of 185 MBq of Ga-67 citrate. Ten normal controls were also studied. Regions of interest (ROI) were drawn on the posterior image to measure counts from the liver and lungs (Lung/Liver Ratio). Results: L/L ratio according to the stages of chest X-ray classification were as follows; stage 0 (normal, n=10): $0.3948{\pm}0.0692$, stage 1 (n=10): $0.5763{\pm}0.1537$, stage 2 (n=11), $0.6849{\pm}0.1459$, stage 3 (n=4) $0.9913{\pm}0.0712$. There was a significant correlation between the scintigraphic L/L ratio and the X-ray stage (r=0.618, p<0.05). However, no significant correlation between L/L ratio and pulmonary function tests were observed (p>0.05). Conclusion: Quantitative Ga-67 scintigraphy can be a useful method for staging of silicosis. However, it is not a method to assess pulmonary functional impairment.

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Determination of benzophenone in water, soil and sediment by gas chromatography/mass spectrometry (기체크로마토그래피/질량분석기에 의한 수질, 토양 및 저질 시료중의 benzophenone 분석법에 관한 연구)

  • Jeon, Hee Kyung;Choi, Hae Yeon;Ryu, Jae-Chun
    • Analytical Science and Technology
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    • v.18 no.2
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    • pp.147-153
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    • 2005
  • Benzophenone (BP) which is one of endocrine disrupting chemicals is suspected to contaminate waters (river, lake and industrial drainage) and soils (ground soil and sediment). Analytical method for determination of BP in soil and water was developed by gas chromatography/mass spectrometry. Water sample (100 mL) was extracted with n-hexane, and soil (10 g) was extracted with methanol and n-hexane. Recovery for BP was >71.4% in water and 86.5-94.7% in soil with coefficient variation of less than 19.8%. Calibration curves showed a good linearity ($r^2$ >0.998). In water, soil and sediment collected at nation-wide sites, BP was detected at 5 sites among 43 water sites at the concentration range of 30-200 ng/L. No BP was found in the soil and sediment samples. It is suggested that this method will be useful to the determination of BP in the environmental matrices such as waters, soils and sediments in minute quantities.

Determination of Phthalate Esters and Adipate in Water and Sediment Samples (수질 및 저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.616-623
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    • 2000
  • The most common phthalate acid esters (8 compounds) and adipate were determined from water and sediment simultaneously. After liquid-liquid extraction with n-hexane for water and sonication extraction with dichloromethane for sediment, these were determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.993$) on the range of the 0.1-20 ng/ml (water) and 10-500 ng/g (sediment), and the detection limits of method were below 0.1 ng/ml and 10 ng/g for water samples and sediment samples, respectively. The method shows a good precision and accuracy for measurement of phthalates and adipate.

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