• Title/Summary/Keyword: certified soil

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표준시료를 이용한 토양중 중금속 분석방법 비교

  • Yun Jeong-Gi;Kim Tae-Seung;Kim Dong-Ho;Jeon Seong-Hwan;Jeong Il-Rok;Kim Hyeok
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.242-246
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    • 2005
  • The heavy metal analysis (Cd, Pb, Cu, Cr, Zn, Ni) with various extraction methods was performed using the certified sample and real soil sample. In case of the certified samples, $10.5{\sim}118%$ of recovery was showed with various ranges depend on the metal kinds and extraction methods. Also, the alkali-digestion method was showed the proper results by applying in hexavalent chromium. In case of real sample, compared to amounts of heavy metals extracted using 0.1N-HCl, those extracted using acid digestion are higher by $3{\sim}24$ times in Cu, $1.1{\sim}1.5$ times in Cd, $2{\sim}23$ times in Pb, $3{\sim}104$ times in Zn, $12{\sim}101$ times in Ni, $30{\sim}202$ times in Cr. There is no considerable difference between four acid digestion methods.

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Development of soil certified reference material for determination of the hazardous elements (유해원소 측정용 토양 인증표준물질 개발)

  • Kim, In-Jung;Min, Hyung-Sik;Suh, Jung-Ki;Han, Myung-Sub;Lim, Myung-Chul;Kim, Young-Hee;Shin, Sun-Kyoung;Cho, Kyung-Haeng
    • Analytical Science and Technology
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    • v.23 no.5
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    • pp.485-491
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    • 2010
  • A certified reference material (CRM) of KRISS 109-03-SSD was developed for the analysis of hazardous elements in soil. The target elements were As, Cd, Cr, Cu, Hg, Ni, Pb, Zn being regulated by the Soil Environment Conservation Act. Starting material was collected from tailing dump of an unworked tungsten mine at Sangdong (Gangwon-do, Korea). The starting material under-went through a series of fabricating process steps of screening, drying, grinding, sieving, blending, bottling, sterilization and was certified according to the ISO Guide 35. Isotope dilution-inductively coupled mass spectrometry (ID-ICP/MS) and instrumental neutron activation analysis (INAA) were used for the measurement. Homogeneity was tested according to ISO 13528 annex B. The certified values were determined using the results from two different methods or from two independent measurements using a method. Finally, certified values of seven elements of arsenic, cadmium, chromium, copper, lead, nickel and zinc were determined. Mercury did not satisfied the criteria of homogeneity and the result would be provided for information only, together with iron and tungsten. It was also studied, the extractable fraction of elements by aqua regia according to the ISO 11466 protocol being frequently studied for the purpose of environmental monitoring. It was performed as a inter-laboratory study by 6 laboratories of a public institute and universities. Standard deviation among the laboratories was much bigger than the uncertainty of the certified value. The result of inter-laboratory study on the extractable fraction will be provided for information, only.

Comparison of the Heavy Metal Analysis in Soil Samples by Bench-Top ED-XRF and Field-Portable XRF (Bench-Top ED-XRF 및 휴대용 XRF를 이용한 토양 시료 중의 중금속 비교 분석)

  • Choi, Soo-Jung;Kim, Chong-Hyeak;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.293-301
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    • 2009
  • As a basic research for development of the domestic field-portable XRF spectrometer, we discussed the analytical results of bench-top ED-XRF and field-portable XRF method for polluted heavy metals such as Cr, As, Se, Hg, Pb, Cd in soil samples. To obtain the best performance of the XRF spectrometer, the instrumental parameters of X-ray tube-voltage and measurement time were optimized for 6 heavy-metal elements in soil using certified reference material. The quantitative analysis of Cr, As, Se, Hg, Pb, Cd concentration in certified reference materials and soil samples were compared by empirical method and fundamental parameter method.

Comparison of analytical methods for quantifying total chromium in soil using Atomic Absorption Spectrometer (AAS) and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) (토양 시료 중 Atomic Absorption Spectrometry (AAS) 및 Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES)를 이용한 총 크롬 분석방법 비교)

  • Lee, Hong-gil;Kim, Ji-in;Byun, Yoonjoo;Kim, Hyunkoo;Yoon, Jeong Ki
    • Journal of Soil and Groundwater Environment
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    • v.22 no.6
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    • pp.22-28
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    • 2017
  • The accuracy of analytical results in response to the use of different additives ($NH_4Cl$, KCl, $LaCl_3$) and oxidant gases was evaluated and compared by using Atomic Absorption Spectrometry (AAS). Identification of spectroscopic interferences and possible improvements in Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) analysis were also discussed. The average accuracies of total chromium using Certified Reference Materials (CRMs) were found to be 72.1~94.2% in air/acetylene flame condition by AAS, and they were improved to 100.5~110.5% when the oxidants was changed to nitrous oxide rather than adding the additives. The field samples showed similar trends to CRMs, but chromium concentrations were highly variable depending on analytical conditions. The average accuracies using CRMs were estimated to be 89.3~166.1% by ICP-AES, and improved to below 121.7% after eliminating iron interference. Field samples with low chromium and high iron concentration were measured to be > 30% lower in total chromium concentrations by ICP-AES than AAS in nitrous oxide/acetylene flame. Total chromium concentrations in soil could be analyzed with better accuracy under nitrous oxide/acetylene flame by AAS because it was more effective to increase the temperature of the flame than to eliminate the chemical interference for maximizing atomization of chromium. When using ICP-AES, interference substances, total chromium levels, and analytical conditions should be also considered.

Yielding Behavior of Compacted Decomposed Granitic Soil under Anisotropic Compression Previous Loading (비등방 압축의 선행재하를 받은 다짐풍화화강토의 항복거동)

  • Jeong, Sang-Guk;Kang, Kwon-Soo;Yang, Jae-Hyouk
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.5 no.3
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    • pp.233-244
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    • 2001
  • Stress-strain behaviour of soil varies based on stress path and stress history. There has been few study on the characteristics of yielding curve which has anisotropic compression stress history in decomposed granite soil. During this study, various stress path tests in previous anisotropic compression stress history are performed on compacted decomposed granite soil sampled at Iksan, Chonbuk. Yielding points are determined from various stress-strain curves (${\eta}-{\varepsilon}$, ${\eta}$-v, and ${\eta}$-k, ${\eta}$-W curves). Stress-strain curve is certified which shows yielding point very clearly. The shape and characteristics of anisotropic compression yielding curves are examined. The main results are summarized as follows : 1) p' constant and compressive direction in stress paths, which has experienced previous anisotropic compression stress history, shows relatively dear yielding points. 2) Yielding curves defined from ${\eta}$-k and ${\eta}$-W curve show almost perfect ellipse. 3) Directions of plastic strain incremental vector($dv^p/d{\varepsilon}^p$) are not perpendicular to yielding curve.

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Measurement of heavy metals in antarctic soil at the king sejong station: application of isotope dilution inductively coupled plasma mass spectrometry (동위원소희석 ICP-MS분석법에 의한 남극 세종기지 주변 토양의 중금속 측정)

  • Suh, Jung-Ki;Hwang, Euijin;Min, Hyung Sik
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.364-374
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    • 2008
  • Antarctic Environmental Monitoring Handbook' was published by COMNAP/SCAR in 2000. The standardized method described in this handbook is recommended for monitoring of antarctic environment. High pressure bomb technique in this guide was used to decompose soil samples. In compliance with this guide book, high pressure bomb technique was applied to decompose the antarctic soil sampled at the King Sejong Station. An Isotope Dilution-Inductively Coupled Plasma-Mass Spectrometry (ID-ICP-MS) was applied to determine mass concentrations of Pb, Cu and Zn in the soil. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of NIST 2702 (marine sediment). The analytical results agreed with certified value within the range from 99.5~100.8%. Matrix separation was necessitated for the determination of Cu and Zn by Chelex 100 ion exchange resin. As a result, the average mass concentrations of Pb, Cu and Zn which are suspected to be caused by anthropogenic pollution were 332.9 mg/kg, 95.6 mg/kg and 115.3 mg/kg, respectively. Those for the metals sampled in the soils of the remote regions from the station were 28.1 mg/kg, 101.8 mg/kg and 115.6 mg/kg, respectively.

A Study on the Development of Soil-based PTMs for Analysis of BTEX (BTEX 분석용 토양 숙련도 표준시료(PTMs) 개발에 관한 연구)

  • Lee, Minhyo;Lee, Guntaek;Lee, Bupyoel;Lee, Wonseok;Kim, Gumhee;Hong, Sukyoung
    • Journal of Soil and Groundwater Environment
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    • v.18 no.5
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    • pp.15-25
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    • 2013
  • In this study, two kinds of soil-based proficiency testing materials (PTMs), NICE-012L and NICE-012R were prepared and certified for Benzen, Toluene, Etylbenzene and Xylene with evaluation of uncertainties. In order to analyse BTEX (Benzen Toluene Etylbenzene Xylene) for the candidate materials, GC/MS was used after pretreatment according to methods of soil analysis by Ministry of Environment. For the homogeneity test among bottles in terms of candidate materials, ISO 13528 and IUPAC Protocol were used and according to the result, both candidate materials showed sufficient homogeneity. Also, the stability test over the candidate materials was accessed according to the ISO Guide 35 by classifying short-term and long-term stability and the result showed that both candidate materials showed decent stability. The reference values of the two candidate materials depending on BTEX components were derived from the average of the 11 samples that were used for verification of the samples' homogeneity. Uncertainty of measurement was combined by uchar that was caused by a characteristic value, $u_{bb}$ that was caused by between-bottle homogeneity, and $u_{stab}$ that was caused by stability, and then combined uncertainty ($u_{PTM}$) was multiplied to the coverage factor (k) derived from the effective degree of freedom from each factor that leads to expanded uncertainty (U) in about 95% of confidence level. The proficiency testing materials developed through this study were supplied to National Institute of Environmental Research (NIER) and utilized as an external proficiency testing materials for evaluating analysis capacity of soil agencies with specialty in terms of soil analysis approved by Minister of Environment.

A Study of Interference Factor of Analysis Method of Hexavalent Chromium in Soil using UV/VIS Spectrometry and Application of Ion Chromatography (자외선/가시선 분광법을 이용한 토양 중 6가 크롬 분석방법의 방해요인 분석 및 이온크로마토그래피 적용에 관한 연구)

  • Noh, Hoe-Jung;Lee, Myung-Gyu;Lee, Hyeon Seok;Kim, Mira;Kim, Dongho;Kim, Tae Seung
    • Journal of Soil and Groundwater Environment
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    • v.17 no.6
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    • pp.33-42
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    • 2012
  • This study was performed to find the problems according to interference factors (organic matter, pH, Cr, Mn, Fe, clay, and etc.) when we analyzed the hexavalent chromium [Cr(VI)] in soils using UV/VIS spectrometer (US EPA 7196A), attempted to evaluate the domestic applicability of analytical method (US EPA 7199) using IC-UV/VIS spectrometer as alternative method. The recovery rate of certified reference materials was 75.0% (US EPA 7196A) and 101.4% (US EPA 7199) by the analytical methods. As the results of performing QA/QC about US EPA 7199, method detection limit (MDL) and limit of quantification (LOQ) were 0.062 mg/kg, 0.196 mg/kg, respectively. The LOQ of US EPA 7199 was lower than that of the current soil official testing method in Korea (0.5 mg/kg). Cr(VI) contents in 23 soil samples were compared by the analytical methods of EPA 7196A and 7199. Cr(VI) was detected in 13 of 23 soil samples by EPA 7196A, while EPA 7199 was not detected in any soil samples. The Cr(VI) content in 23 soil samples by EPA 7196A was not clearly correlated with Cr, Fe, Mn and clay content in the soil samples. However, the contents of Cr(VI) and organic matter of the soil samples had the highest coefficient of determination ($R^2$) of 0.80. In order to evaluate the correlation between the recovery rates of Cr(VI) and organic matter contents in the soil samples, the recovery rates of 5 soil samples added Cr(VI) standard solution were analyzed by the analytical methods. According to the results, the higher the organic matter contents in soil samples, the lower the recovery rates of Cr(VI) by US EPA 7196, while in case of US EPA 7199, the recovery rates were stable regardless of the organic matter contents.

Thermal Property of the Roof Green Unit System Using Artificial Lightweight Soil Recycled with Bottom Ash (바텀애시 재활용 인공토양 적용 옥상녹화 유니트 시스템의 열특성)

  • Yoo, Jong-Su;Lee, Jong-Chan;Oh, Chang-Won
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.8 no.1
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    • pp.49-55
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    • 2020
  • In this study, the surface temperature of the roof green system using ALSRBA(Artificial Lightweight Soil Recycled with Bottom Ash) was measured in each season and the thermal property of the ALSRBA was investigated. As a result, it was certified that ALSBRA has superior thermal property than the usual artificial soil. In addition, The daily temperature range in each season was measured to investigate the thermal isolation property of EUS(Existing Unit System) and DUS(Developed Unit System). The result showed that the thermal isolation effect of EUS was lower than that of SPSS(Site-Place-Soil System), but thermal isolation effect of DUS was similar to that of SPSS because DUS has continuous ALSBRA layer by removing unit barrier.

Sequential Extraction of Soil Heavy Metals Aided by Ultrasound Sonication (토양 중금속의 초음파 연속추출)

  • Suh, Jj-Won;Yoon, Hye-On
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.1
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    • pp.85-91
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    • 2010
  • The various forms of heavy metals in soil environments have been studied by sequential extraction method. We tested conventional Tessier sequential extraction and new ultrasound-sonication extraction methods, and compared their extraction efficiency. Total As, Cd, Cu, Pb, and Zn contents of the target soil (NIST SRM 2710 Montana Soil), by three methods (USEPA Method 3050B, KBSI Method, and ultrasound-sonication method) were all consistent with the certified values. Sequential extraction efficiency along with step-wise extraction values was similar in both Tessier method and ultrasound-sonication method. The ultrasound-sonication method took about 3 hours to complete whole procedure while the Tessier sequential extraction method took around 12 hours. Ultrasound-sonication method was estimated as one of the best methods with a relatively short application time and no requirement of high temperature treatment.