• Title/Summary/Keyword: NIST SRM

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A Study on Mineral Distribution in Korean Foodstuffs by Neutron Activation Analysis (중성자방사화분석법에 의한 국내 식품원재료의 무기질 분포 연구)

  • Cho, Seung-Yeon;Hong, Woo-Jung;Lee, Jung-Yeon;Kang, Sang-Hoon;Chung, Young-Sam
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.390-395
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    • 2002
  • Concentrations of minerals (Ca, K, Mg, Na, Se, Zn, Fe, and Mn) in 50 different Korean foodstuffs were determined through neutron activation analysis. To check the accuracy of this method, the U.S. NIST standard reference materials were analyzed. Anchovy, sesame, perilla, and laver were found to contain relatively higher concentrations of Ca, Mg, Fe, and Zn than the other foodstuffs.

Evaluation of a Method for the Measurement of PAHs in the Ambient Atmosphere - Focusing on High Volume Sampling and GC/MS Analysis (대기 중 다환방향족탄화수소 측정방법의 성능평가 - 하이볼륨 샘플링 및 GC/MS 분석방법을 대상으로)

  • Seo, Young-Kyo;Park, Dae-Kwon;Baek, Sung-Ok
    • Journal of Environmental Health Sciences
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    • v.35 no.4
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    • pp.322-333
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    • 2009
  • In this study, a measurement method was evaluated for the determination of polycyclic aromatic hydrocarbons (PAHs) in the ambient atmosphere. PAHs were sampled by high-volume samplers, and were then analysed with a GC/MS system. Particulate PAHs were collected on $8"{\times}10"$ quartz fiber filter, while vapor phase PAHs were adsorbed on polyurethane foam (PUF). Target compounds included a total of 36 PAHs, which are known to be frequently detected in the urban atmosphere. It was not necessary to clean-up samples before samples were analyzed using GC/MS, and the overall performance of the method was tested by a variety of quality control and quality assurance schemes. It is generally known that the clean-up procedure can negatively affect the recovery of samples. Precision and accuracy was evaluated using SRM provided by US NIST, and the results were generally satisfactory and reliable. However, the GC/MS method appeared not to be adequate for 6-rings PAHs, such as coronene, due to its lower sensitivity. In addition, collection efficiencies for low molecular compounds, such as 2-rings PAHs, were poor because of the lower retention volume of the PUF adsorbent. As a result, it was concluded that the method based on high-volume sampling and GC/MS analysis can give very reliable data by simultaneous sampling of both particulate and vapor phases for 3-rings to 5-rings PAHs of environmental concern.

Intercomparison and Determination of Trace Elements in Urban Dust by Neutron Activation Analysis (중성자방사화분석법을 이용한 대기분진중의 미량원소 비교분석)

  • Chung, Yong-Sam;Moon, Jong-Hwa;Kim, Sun-Ha;Park, Kwang-Won;Kang, Sang-Hun
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.179-188
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    • 2000
  • Trace elements in air samples artificially loaded on filters with urban dust and the bulk material of urban dust as an environmental sample were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Dust, SRM 1648) of the National Institute of Standard and Technology was used for the analytical quality control. The relative error for 37 elements was less than 15% and the standard deviation was less than 10%. 29 elements in the urban dust and 21 elements in the loaded filter sample were determined respectively. To evaluate the proficiency and reliability of the measurement, data intercomparison was performed and 39 analytical laboratories participated in the analysis using different analytical methods; neutron activation analysis, particle induced X-ray emission analysis, X-ray fluorescence analysis and atomic absorption spectrometry. Z-scores were calculated using the standard deviation of the laboratorie's mean as target standard deviation, and a good result was obtained that the values fall between -1 and +1 except some elements.

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Quality Control on Neutron Activation Analysis for Urban Dust by the Proficiency Test (비교숙련도 시험을 통한 도시대기분진에 대한 중성자방사화분석법의 품질관리)

  • Moon, Jong-Hwa;Kim, Sun-Ha;Chung, Yong-Sam
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.433-438
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    • 2002
  • Trace elements in two air filters (V-50, P-50) artificially loaded with urban dust provided from IAEA were determined non-destructively using instrumental neutron activation analysis. Standard reference material (Urban Particulate Matter, SRM 1648) of National Institute of Standard and Technology was used for analytical quality control. About 20 elements in both of loaded filter samples were determined. To evaluate inter-laboratory comparison and proficiency test, analytical data were statistically treated with the results which collected from 49 laboratories, 40 countries participated in this study using neutron activation analysis, particle induced X-ray emission, inductively coupled plasma mass spectroscopy, etc,. From the results of statistical treatment, Z-scores are within ${\pm}2$. Furthermore, accuracy and precision of obtained analytical values are passed according to the criteria of the proficiency test. Consequently, it was proved that analytical quality for air dust samples being performed has been controlled properly.

Analysis of $\triangle^9$-Tetrahydrocannabinol and 11-nor-9-carboxytetrahydrocannabinol in Hair by Gas Chromatography/Mass Spectrometry (가스크로마토그라피/질량분석기에 의한 모발중 대마성분 분석)

  • 양원경;한은영;박용훈;임미애;정희선
    • YAKHAK HOEJI
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    • v.48 no.3
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    • pp.207-212
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    • 2004
  • An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane:ethyl acetate (90:10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$>0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91%. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.

Development of Appropriate Acid Digestion Method used for the Determination of Total Uranium in Soil by Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) (유도결합플라즈마-질량분석기(ICP-MS)를 이용한 토양의 총 우라늄 정량에 요구되는 적정 산분해 전처리 방법 개발)

  • Shin, Gunhwan;Lee, Goontaek;Kang, Jiyoung;Yoon, Jungki;Kim, Hyunkoo;Noh, Hoejung;Kim, Jiin;Kim, Kyehoon
    • Journal of Soil and Groundwater Environment
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    • v.23 no.6
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    • pp.73-81
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    • 2018
  • Inductively coupled plasma-mass spectrometry (ICP-MS), one of the most commonly used instruments for metal analysis, was used to determine total uranium in soil. The method was named as "Modified ASTM C1345-96". When comparing with ASTM C1345-96, digestion time (2~3 days) was shorten to 7 hours and the treatment in furnace was eliminated. In analyses of 26 field soil samples, there was a significant difference in the average concentration of total uranium between modified ASTM C1345-96 and ASTM C1345-96 (F : 6.22 > Fc : 4.03, significance level : 0.05, n=26). The average concentration of modified ASTM C1345-96 was 1.8 times larger than that of ASTM C1345-96. In addition, modified ASTM C1345-96 was compared with other acid digestion methods for soil including ISO 11466, Modified ISO 11466, US EPA-3051, US EPA-3051A and US EPA-3052 using a certificated reference material (SRM 2711a, NIST) and field soil samples with different level of organic matter content (1.6%, 5.8%, 10.6%). Modified ASTM C1345-96 showed the best accuracy of 93.01% for SRM 2711a. Also, modified ASTM C1345-96 showed the higher extraction rates than other digestion methods by 11~45%.

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.

Multielement Analysis in Airborne Particulate Matter $(PM_{10})$ by INAA, ICP and AAS (INAA.ICP.AAS를 이용한 대기먼지 $(PM_{10})$의 다원소분석)

  • 정용삼;문종화;정영주;박광원;이길용;윤윤열;심상권;조경행;한명섭
    • Journal of Korean Society for Atmospheric Environment
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    • v.15 no.4
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    • pp.495-503
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    • 1999
  • Airborne particulate matter $(PM_{10})$ collected using high volume air sampler and silica fiber filter were analyzed by Instrumental Neutron Activation Analysis(INAA), Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES) and Atomic Absorption Spectrometry(AAS), and the results were compared with each other. 30~40 trace elements in environmental standard reference materials(NIST SRM 1648 and NIES CRM No.8) were analyzed for the analytical quality control. The relative error for two-third of elements detected was less than 10%, and the standard deviation was less than 15%. During the sampling period for 24 hours, the mass concentration of total suspended particulate was 36.1$\mu\textrm{g}$/㎥ and the value is lower than the critical level in Korea. In the results of NAA, the elements of Al, As, Ba, Fe, La, Mg, Na, Sb, Zn were well agreed with those of other methods. In statistical estimation between different methods, the deviation of Al, Ba, Cr, Fe was less than 10% and quite reliable.

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The Effect of Chelators and Reductants on the Mobilization of Metals from Ambient Particulate Matter: More Transition Metals are Mobilized with PM2.5 than with PM10

  • Song, H-S;Chang, W-C;Bang, W-G;Kim, Y-S;Chung, N
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2002.10a
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    • pp.155-155
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    • 2002
  • Ambient urban particulate matters contain various transition metals. When the particulate matters are inhaled into the lung, not all but some part of metals from the particles might be mobilized to participate in a reaction that can damage various biomolecules, such as DNA and proteins. The dust particle size as well as organic acids may influence the metal mobilization. Thus, the mobilization of the metal from SRM1648 (NIST, USA) and urban particulate matters (PM2.5 and PM10) was measured in the presence of artificial or biological chelator with or without reductant. The degree of the mobilization was higher with the artificial or biological chelator than the control with saline. In some cases, a reductant increased the mobilization as much as about 5 times the control without the reductant. Especially, the mobilization of Fe was greatly influenced by the presence of reductants. In general, the degree of the mobilization of the transition metal was higher with PM2.5 than with PM10. Therefore, it is expected that, considering the previously known toxicities of the transition metals, the PM2.5 is more damaging to various biomolecules than PM10. The results also suggest that not the total amount but the mobilizable fraction of the metal in the dust particles should be considered with regard to the toxicity of the urban particulate matters.

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Continuous Preconcentration of Sn2+/Sn4+ by the On-line Sulfide Precipitation-Dissolution

  • Yeon, Pyung-Heum;Yoon, Young-Suk;Oh, Se-Woung;Nam, Sang-Ho;Par, Yong-Nam
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1156-1160
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    • 2004
  • The technique of an on-line preconcentration by the direct sulfide precipitation has been developed. Sn was homogeneously precipitated by sulfide, which was generated in situ from the hydrolysis of thioaceteamide. Precipitate was collected on a filter in the line and dissolved out instantaneously by KOH to be sent to an ICP. The enrichment factor was 4 with the sampling speed of 15/hr for 1.0 mL of sample. It was increased to more than 40 times when the sampling volume was increased to 10 mL with the sampling speed of 5/hr. $Sn^{2+}/Sn^{4+}$ could be separately determined with the on-line precipitation technique. The method was applied to the analysis of NIST SRM 1566 Oyster sample and yielded good agreement with the certified value.