• Title/Summary/Keyword: 내부표준법

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Quantitative X-ray Diffraction Analysis of Synthetic Mineral Mixtures Including Amorphous Silica using the PONKCS Method (PONKCS 방법을 이용한 비정질 실리카 함유 인공광물혼합시료의 정량 X-선회절 분석)

  • Chon, Chul-Min;Lee, Sujeong;Lee, Sung Woo
    • Journal of the Mineralogical Society of Korea
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    • v.26 no.1
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    • pp.27-34
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    • 2013
  • X-ray powder diffraction is one of the most powerful techniques for qualitative and quantitative analysis of crystalline compounds. Thus, there exist a number of different methods for quantifying mineral mixtures using X-ray diffraction pattern. We present here the use of Rietveld and PONKCS (partial or no known crystal structure) methods for quantification of amorphous and crystallized mineral phases in synthetic mixtures of standard minerals (amorphous silica, quartz, mullite and corundum). Pawley phase model of amorphous silica was successfully built from the pattern of 100 wt% amorphous silica and internal standard-spiked samples by PONKCS approach. The average of absolute bias for quantities of amorphous silica was 1.85 wt%. The larger bias observed for lower quantities of amorphous silica is probably explained by low intensities of diffraction pattern. Averages of absolute bias for minerals were 0.53 wt% for quartz, 0.87 wt% for mullite and 0.57 wt% for corundum, respectively. The PONKCS approach achieved improved quantitative results compared with classical Rietveld method by using an internal standard.

An Experimental Study on the Compressive Strength of Reinforcing Bars in Concrete Specimens and Compressive Strength Measurement Methods (콘크리트 압축강도 측정법과 공시체 내 철근이 압축강도 측정에 미치는 실험적 연구)

  • Lee, Won-Hong;Choi, Sang-Gi;Lee, Seuong-Yeol;Ahn, Jin-Hee;Kang, Beom-Ju
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.25 no.6
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    • pp.33-40
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    • 2021
  • Measuring the compressive strength of concrete is a very important factor in the safety review of concrete structures. Concrete compressive strength measurement methods include destructive and non-destructive methods. The destructive method includes the uniaxial compression failure method, and the non-destructive method includes the rebound hardness method and the elastic wave measurement method. In this study, the type of measurement method and the effect of reinforcing bars inside the concrete were tested to examine the relationship between them. Regardless of the type of specimen, the average compressive strength by the elastic wave measurement method among the three experimental methods was greater than the average compressive strength by the other methods. When the specimen type is the same, the standard deviation of the measured values of the elastic wave measurement method is smaller than that of the other measurement methods, so it can be seen that the elastic wave measurement method does not show large variance in the measured values compared to the other two measurement methods. When the average compressive strength according to the test method for each specimen was compared with the average compressive strength of the compressive failure test method, the average compressive strength was measured to be high in the order of the elastic wave measurement method, the compression failure test, and the rebound hardness method. Since the measured values of the compressive strength of concrete are different depending on the method of measuring the compressive strength of concrete and the presence or absence of reinforcing bars inside the concrete, further research is required considering the effect of various concrete covers.

Quantitative Analysis Cholesterol in Each Parts of Korean Squid by the Chromarod TLC-FID System(Iatroscan) (Iatroscan에 의한 한국산 오징어의 부위별 콜레스테롤 함량 측정)

  • 조순영;김옥선;최용석;송진향;야스시엔도;겐시로후지모토
    • Journal of Life Science
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    • v.14 no.2
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    • pp.221-224
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    • 2004
  • Comparisons of enzymatic method, gas chromatographic method, and the Iatroscan method for the determination of cholesterol in each parts of Korean squid were undertaken. The Iatroscan method was the most suitable procedure for the rapid and simple determination of net cholesterol concentration in parts of Korean squid. 5$\alpha$-cholestane is used as a good internal standard. The cholesterol contents in body, leg, viscera, eye, skin, and liver part of Korean squid, Todarodes pacificus STEEN STRUP by Iatroscan method were 178.9, 321.4, 168.9, 159.5, 608.8 and 634.2 mg%, respectively.

Rapid Analysis of Major Putrefactive Metabolites by GC and GC/MSD (GC 및 GC/MSD를 이용한 주요 분변 부패산물 신속분석법)

  • 박규용;김민철;우강융;이나경;백현동
    • KSBB Journal
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    • v.18 no.1
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    • pp.74-77
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    • 2003
  • A simple, reproducible, and rapid gas chromatographic method for putrefactive metabolite determination in feces was developed. The method involves the direct injection of fecal supernatants into the gas chromatograph, without pretreatment. The mass spectra of these metabolites were obtained using an HP 5971 mass selective detector operated in electron impact (EI) ionization mode. This method produced sharp peaks and allowed the simultaneous determination of fecal putrefactive metabolites.

Changes in Volatile Compounds of Green Tea during Growing Season at Different Culture Areas (녹차엽의 채취 시기와 재배지역에 따른 휘발성 향기 성분의 변화)

  • Lee, Joo-Yeon;Wang, Li-Fei;Baik, Joo-Hyun;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.39 no.3
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    • pp.246-254
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    • 2007
  • Fresh tea leaves grown in Jeju Island and Jeonnam Province of South Korea were plucked and processed. Volatile compounds (VCs) were analyzed and identified with SPME-GC/GC-MS/GC-O. The VCs of green teas were classified into two major categories based on their aroma characteristics: the Greenish (Group I), and Floral (Group II) odorants. It was found that the VCs were decreased significantly in fresh tea leaves as they were plucked at the later stages of cultivation. The ratio of VCs responsible for Group I and Group II compounds was well-balanced in tea leaves plucked in May, but the balances were changed when the fresh leaves were processed. The major VCs of fresh tea leaves in Jeju and Jeonnam were n-hexanal, E-2-hexenal, Z-3-hexenal, myrcene, benzyl alcohol, linalool, and phenyl alcohol. Also, Jeju and Jeonnam tea leaves had different aroma composition. n-Heptanol, ${\beta}-pinene$, benzaldehyde, and ethyl salicylate were found in Jeju fresh tea leaves, and Z-3-hexenol, E-2-hexenol, and methyl n-heptanoate were detected in Jeju dry tea leaves. On the other hand, Z-linalool oxide and myrcene were found in Jeonnam dry tea leaves. The SPME-GC method showed high reproducibility (RSD, 7.4%) with no-artifact formation. In this study, optimum plucking period of tea leaves could be determined for production of high quality green tea with a well-balanced aroma and characteristic VCs in green tea according to growing areas.

Development of Enhanced Analytical Method for Perchlorate in Food by IC-MS/MS with an Internal Standard (IC-MS/MS와 내부표준물질을 이용한 식품 중 perchlorate 분석법 개선)

  • Yang, Min-June;Kim, Jong-Sung;Han, Jong-Hun;Her, Nam-Guk
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.532-536
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    • 2011
  • The internal standard method using ion chromatography combined with tandem mass spectrometry (IC-MS/MS) for quantifying perchlorate in different types of food was established. Because the presence of ions and other biomolecules in matrices usually interrupts accurate determination of perchlorate, it is necessary to develop efficient, reproducible method to determine perchlorate concentrations in food. In this study, the internal standard method was compared with the external standard method to determine perchlorate concentrations in standard samples. The obtained method detection limit (MDL) for perchlorate was 0.005 ${\mu}g/L$ for bottled water, 0.12 ${\mu}g/L$ for milk, 0.27 ${\mu}g/kg$ for rice, 0.16 ${\mu}g/kg$ for vegetables, and 0.07 ${\mu}g/kg$ for seaweed, respectively. The limit of quantitation (LOQ) was calculated by multiplying the MDL by 7. The recoveries of perchlorate from food samples spiked with perchlorate ranged from 98 to 105% and their percent relative standard deviation (%RSD) levels were <20%. This method was successfully applied for the quantitative determination of perchlorate in various kinds of food.

Improvement of Field Uniformity in a Reverberation Chamber with Various Numbers of a 2D CRD (2D CRD 수에 따른 전자파 잔향실 내의 필드 균일성 개선)

  • Kim, Jin-Bok;Rhee, Joong-Geun;Kim, Jung-Hoon;Rhee, Eu-Gene
    • Journal of the Institute of Electronics Engineers of Korea TC
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    • v.47 no.4
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    • pp.18-24
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    • 2010
  • This paper presents the improvement of the field uniformity in a reverberation chamber which can be substitute an anechoic chamber for the electromagnetic interference (EMI) and immunity test. Nowadays, there are many EMI issues due to the increasing use of wireless local area network (LAN), digital multimedia broadcasting (DMB), and mobile internet. With this reason, this paper studied the field characteristics in a reverberation chamber for 2.3 GHz band. In this paper, the finite difference time domain (FDTD) method is used to analyze the field characteristics in a reverberation chamber. To improve the field uniformity in the reverberation chamber, this paper adopted a 2D cubical residue diffuser (CRD) with varying the disposition and number of CRD. For each case, the tolerance and standard deviation of the electric field strength are evaluated. In comparison with the reverberation chamber without any CRD, the reverberation chamber with two CRDs showed improved results; 1.98 dB improvement in standard deviation and 3.6 dB improvement in tolerance.

Analytical Methods for Diethylstibestrol and Zeranol in Muscle Foods (근육 식품 중의 diethylstibestrol과 zeranol 분석법)

  • Ha, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.385-389
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    • 2002
  • Analytical method for diethylstibestrol (DES) and zeranol, which are growth promoters, in muscle foods was studied. Through selected ion monitoring analysis by GC-MSD for hormones, $M^+$ 412, 420, 416, and 433 for DES, $D_8DES$, ${\beta}-estradiol$, and zeranol, respectively, were selected for quantitative analysis. Removal of interferences in meat was done by passing the meat through 1 cc of strong anion exchanges resin, Dowex $2{\times}8$, 400 mesh, whereby the recoveries of DES and zeranol were achieved. Recoveries of DES and zeranol were ranged from 85 to 110%, and 75 to 110%, respectively, in meat using $D_8DES$ as an internal standard, while were 82 to 105%, and 65 to 120%, respectively, using ${\beta}-estradiol$ as an internal standard. These results show that both $D_8DES$ and ${\beta}-estradiol$ can be adopted as the internal standard for the analysis of DES and zeranol in muscle foods. Limits of detection of DES and zeranol were 0.05 and 1.0 ng/g, and limits of quantitation were 0.5 and 1.0 ng/g, respectively. The results of this study revealed no DES and zeranol were present in 14 samples of beefs, porks, ducks, chickens, mutiplicated flat fish, and trout.

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

  • Na, Yuncheol;Chang, Yoon-Seok;Kim, Hai-Dong;Hong, Jongki
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.29-36
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    • 2004
  • An analytical method of polybrominated diphenyl ethers in soil samples by isotope dilution method using gas chromatography/mass spectrometry (GC/MS)-selected ion monitoring (SIM) was described. PBDEs in soil were extracted with soxhlet extractor and then silica and florisil solid phase extraction (SPE) methods as purification of extract were compared. After clean-up, the extractions were analyzed by GC/MS with SIM mode. Quantitation was performed isotope dilution method using four $^{13}C$ isotopically labeled PBDEs as internal standards. This developed method was validated for eight congeners of PBDEs in the concentration range 0.04~4 ng/g in soil and the average recovery of the analytes ranged 30.8~110.8% for florisil and 44.4~110.7% for silica, respectively. The method detection limits of PBDEs were 0.04~0.3 ng/g.

Accurate Analysis of Trace Phthalates and Method Validation in Cosmetics using Gas Chromatography with Mass Spectrometric Detection (화장품에 함유된 미량의 프탈레이트 함량을 정확히 분석하기 위한 가스크로마토그래피-질량분석 시험법 및 그 시험법의 유효성)

  • Kim, Min-Kee;Jeong, Hye-Jin;Cho, Jun-Cheol
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.38 no.1
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    • pp.33-41
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    • 2012
  • An effective, environmentally friendly analytic methods using gas chromatography with mass spectrometric detector (GC-MSD) have been developed for the quantitative analysis of trace phthalate levels in cosmetics such as nail lacquer and hair spray. Since such cosmetics are largely comprised of organic solvents, conventional clean-up methods that have been widely used for phthalate analyses are in adequate. In addition, analysis of trace phthalate levels is notorious for its sensitivity to contamination, which causes high analytical values. A direct sample dilution method using an organic solvent was adopted to the sample preparation process to determine the exact amounts of phthalates and simultaneously avoid the high risk of secondary contamination. The method has many advantages including high accuracy, sensitivity, and simplicity in sample preparation. Dibutyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were selected for analysis because they have been frequently detected in cosmetics and consistently reported as endocrine disruptors in humans and animals. Internal standard method using two deuterium substitutes (DBP-$d_4$, DEHP-$d_4$) as the internal standard was also used. The results of 'Method validation' showed the capabilities of this method for the routine analysis of phthalates at the ppm level. The recovery ranges were between 95 % and 106.1 %, and relative standards deviations (RSD) were less than 3.9 % in fortified nail lacquer and hair spray samples at the concentration of $25{\mu}g/g$.