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Comparison of Blood Lead Concentration Using Graphite Furnace Atomic Absorption Spectrometry (GF-AAs) and Inductively Coupled Plasma-mass Spectrometry (ICP-MS) (흑연로 원자 흡광 광도법과 유도 결합 플라즈마 질량 분석법을 이용한 혈중 납 농도 비교)

  • Kang, Min-Kyung;Kwon, Jung-Yeon;Kim, Byoung-Gwon;Lim, Hyoun-Ju;Seo, Jeong-Wook;Kim, Yu-Mi;Hong, Young-Seoub
    • Journal of Environmental Health Sciences
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    • v.45 no.3
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    • pp.258-266
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    • 2019
  • Objectives: In this study, blood lead was analyzed using graphite furnace atomic absorption spectrometry (GF-AAs) and inductively coupled plasma mass spectrometry (ICP-MS). We tried to examine the difference and consistency of the analytical values and the applicability of the analytical method. Methods: We selected 57 people who agreed to participate in this study. After confirming the linearity of the calibration standard curves in GF-AAs and ICP-MS, the concentrations of lead in quality control material and samples were measured, and the degree of agreement was compared. Results: The detection limit of the ICP-MS was lower than that of GF-AAs. The coefficient of variation of reference materials was shown to be stable in the ICP-MS and GF-AAs. When the correspondence between the two equipments was verified by bias of the analysis values, a concordance was shown, and approximately 98% of the ideal reference lines were present within ${\pm}40%$ of the deflection. Conclusion: GF-AAs showed high sensitivity to single heavy metal analysis, but it took much time and showed higher detection limit than ICP-MS. Therefore, it would be considered necessary to switch to ICP-MS analysis method, considering that the level of lead exposure is gradually decreasing.

Comparison of Human Blood Cadmium Concentrations using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS) and Inductively Coupled Plasma-mass Spectrometry (ICP-MS) (흑연로 원자 흡광 광도기와 유도 결합 플라즈마 질량 분석기를 이용한 인체 혈중 카드뮴 농도 비교)

  • Kwon, Jung-Yeon;Kim, Byoung-Gwon;Lim, Hyoun-Ju;Seo, Jeong-Wook;Kang, Min-Kyung;Kim, Yu-Mi;Hong, Young-Seoub
    • Journal of Environmental Health Sciences
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    • v.44 no.5
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    • pp.491-501
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    • 2018
  • Objectives: The aims of this study were to compare concentrations and the correspondence of human blood cadmium by using graphite furnace atomic absorption spectrometry (GF-AAS) and inductively coupled plasma-mass spectrometry (ICP-MS), which are representative methods of heavy metal analysis. Methods: We randomly selected 79 people who agreed to participate in the research project. After confirming the linearity of the calibration curves for GF-AAS and ICP-MS, the concentrations of cadmium in a quality control standard material and blood samples were measured, and the correlation and the degree of agreement were compared. Results: The detection limit of ICP-MS (IDL: $0.000{\mu}g/L$, MDL: $0.06{\mu}g/L$) was lower than that of GF-AAS (IDL: $0.085{\mu}g/L$, MDL: $0.327{\mu}g/L$). The coefficient of variation of the quality control standard material showed stable values for both ICP-MS (clinchek-1: 5.35%, clinchek-2: 6.22%) and GF-AAS (clinchek-1: 7.92%, clinchek-2: 5.22%). Recovery was relatively high for both ICP-MS (clinchek-1: 95.1%, clinchek-2: 92.8%) and GF-AAS (clinchek-1: 91.4%, clinchek-2: 98.8%), with more than 90%. The geometric mean, median, and percentile of blood samples were all similar. The agreement of the two instruments compared with the bias of the analytical values found that about 81% of the analytical values were within ${\pm}30%$ of the deviation from the ideal reference line (y=0). As a result of the agreement limit, the value included in the confidence interval was about 94%, which shows high agreement. Conclusion: In this study, we confirmed there was no significant difference in concentrations of a quality control standard material and blood samples. Since ICP-MS showed lower concentrations than GF-AAS at concentrations below the method detection limit of GF-AAS, it is expected that more precise results will be obtained by analyzing blood cadmium with ICP-MS.

Comparisons of sample preparation (acid digestion and microwave digestion) and measurement (inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry) in the determination of bone lead (골중납 측정의 시료 전처리 (산분해법과 마이크로웨이브 분해법)와 측정 방법 (유도결합 플라즈마 질량분석법과 흑연로 원자 흡수 분광 광도법)의 비교)

  • Yoon, Chungsik;Choi, Inja;Park, Sungkyun;Kim, Rokho
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.152-158
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    • 2003
  • This study was conducted to evaluate two sample digestion procedures and instrumental determination parameters for analysis of lead in bone. Amputated human legs were treated by acid digestion or microwave dissolution prior to spectrometric analysis. Inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS) were used for determining bone lead levels. Recovery efficiencies using standard reference material from acid digestion measured by ICP-MS were in good agreement with those of the certified value, but in cases of acid digestion by GF-AAS and microwave digestion by both two methods, recovery underestimated and overestimated, respectively. For the bone samples, the lead concentrations obtained by ICP-MS after acid digestionwere in good agreement with those by GF-AAS (correlation coefficient = 0.983), but GF-AAS gave systematically higher values than ICP-MS. While a good agreement between two analytical methods after microwave digestion was also obtained (correlation coefficient = 0.950), bone lead concentrations from microwave were relatively higher than those from acid digestion. In conclusion, the use of the simple nitric acid digestion procedure at an ambient temperature coupled to ICP-MS seems to be efficient for the determination of lead in bone in consideration for both the convenience and validity.

The role of matrix modifier and for the determination of cadmium in blood by graphite furnace atomic absorption spectrometry (흑연로 원자흡수분광법에 의한 혈중 카드뮴 분석시 매트릭스 개선제(matrix modifier)의 역할)

  • Yoo, Kwang-Sik;Kim, Chang-Bok;Kwon, Jin-Kee
    • Analytical Science and Technology
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    • v.8 no.1
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    • pp.9-16
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    • 1995
  • The low concentration of cadmium in the whole-blood was determined by graphite furnace atomic absorption spectrometry(GFAAS) after the sample was diluted five-fold by 1% Triton X-100, 2% $(NH_4)_2HPO_4$ as matrix modifier and pyrocoated graphite tube with L'vov platform was tried remove the interferences of blood matrix and reduce the loss of volatility of cadmium at higher ashing temperature($600^{\circ}C$). The criteria for evaluating the accuracy and precision of this analysis was confirmed by analysis of interlaboratory comparison(Japan) and NIST SRM No. 909(Cd in Serum). The limit of the determination for cadium was 0.1ng/ml and the relative standard deviation(RSD) at 1.0ng/ml level was about 10% for the GFAAS.

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Analysis of Lead in Blood using SR(self-reversal) and $D_2$ Arc Background Correction Methods (SR 바탕보정법과 $D_2$ 바탕보정법에 의한 혈액 중 Pb 분석)

  • Lee, Seokki;Kim, Poongzag
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.427-434
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    • 1994
  • For the analysis of the relatively volatile lead in blood by GFAAS(graphite furnace atomic absorption spectrophotometer), one can not raise the ashing temperature beyond certain degree due to the elevation of the baseline. Previous investigations showed that background is stabilized when the ashing temperature is raised to $700^{\circ}C$ using a matrix modifier. In this study, same result was obtained at the ashing temperature of around $550^{\circ}C$ even when the matrix modifier is not used and only Triton X-100 is used as a diluent, on an instrument which is equipped with both temperature and current controller(Shimadzu, AA-6501S) and thus the temperature control is fast and accurate. Background correction methods of $D_2$ arc and SR(self reversal) were reviewed. The results show that the absorbance is higher for the $D_2$ arc method, but the background correction is higher for the SR method.

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The role of matrix modifier for the determination of Lead (Pb) in blood by graphite furnace atomic absorption spectrometry (흑연로 원자흡수분광법에 의한 혈중 납분석시 매트릭스 변형제의 역할)

  • Yoo, Kwang-Sik;Kwon, Jin-Kee
    • Analytical Science and Technology
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    • v.5 no.4
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    • pp.349-358
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    • 1992
  • The direct determination of lead in the whole-blood by graphite furnace atomic absorption spectrometric analysis was carried out by using the sample which was diluted five-fold with 1% Triton X-100. Matrix modification was tried to remove the interferences of blood matrix and also to get the optimum analytical condition. Good agreement with certificated values in reference materials(bovine blood) supplied by comparison program in Japan was obstained when 1% $(NH_4)_2HPO_4$ as matrix modifier and ashing temperature, $700^{\circ}C$ were used or 1% $(NH_4)_2HPO_4$ and 0.1% $PdCl_2$ as matrix modifier and ashed at $700^{\circ}C$. Standard deviations were appeared as 2.2~6.3% for 1% $(NH_4)_2HPO_4$ and 3.1~9.1% for 1% $(NH_4)_2HPO_4$ and 0.1% $PdCl_2$ in the range of $31{\sim}624{\mu}gPb/l$.

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A Study on the Developement of Soil Geochemical Exploration Method for Metal Ore Deposits Affected by Agricultural Activity (농경작업 영향지역의 금속광상에 대한 토양 지구화학 탐사법 개발 연구)

  • Kim, Oak-Bae;Lee, Moo-Sung
    • Economic and Environmental Geology
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    • v.25 no.2
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    • pp.145-151
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    • 1992
  • In order to study the optimum depth for the soil geochemical exploration in the area which is affected by agricultural activities and waste disposal of metal mine, the soil samples were sampled from the B layer of residual soil and vertical 7 layers up to 250 cm in the rice field and 3 layers up to 90 cm in the ordinary field. They were analyzed for Au, As, Cu, Pb and Zn by AAS, AAS-graphite furnace and ICP. To investigate the proper depth for the soil sampling in the contaminated area, the data were treated statistically by applying correlation coefficient, factor analysis and trend analysis. It is conclude that soil geochemical exploration method could be applied in the farm-land and a little contaminated area. The optimum depth of soil sampling is 60 cm in the ordinary field, and 150~200 cm in the rice field. Soil sampling in the area of a huge mine waste disposal is not recommendable. Plotting of geochemical map with factor scores as a input data shows a clear pattern compared with the map of indicater element such as As or Au. The second or third degree trend surface analysis is effective in inferring the continuity of vein in the area where the outcrop is invisible.

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Organic Precipitate Flotation of Trace Metallic Elements with Ammonium Pyrrolidinedithiocarbamate (II). Application of Solvent Sublation for Determination of Trace Cd, Co, Cu and Ni in Water Samples

  • 김영상;정용준;최희선
    • Bulletin of the Korean Chemical Society
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    • v.19 no.1
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    • pp.50-56
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    • 1998
  • A solvent sublation was studied for the determination of trace Cd, Co, Cu and Ni in water samples. Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. Experimental conditions such as pH of solution, amounts of APDC, the type and amount of surfactant, the type of solvent, etc. were optimized for the effective sublation of analytes. After metal-PDC complexes were formed in sample solutions of pH 2.5, the precipitate-type complexes were floated in a flotation cell with an aid of sodium lauryl sulfate as a surfactant and by bubbling with nitrogen gas. The precipitates were dissolved and separated into the surface layer of methyl iso-butyl ketone (MIBK). The analytes preconcentrated were determined by a graphite furnace atomic absorption spectrophotometry (GF-AAS). Extractability of each element was 88% for Cd(Ⅱ), 86% for Co(Ⅱ), 95% for Cu(Ⅱ) and 76% for Ni(Ⅱ), respectively. And this procedure was applied to the analysis of real samples. From the recoveries of more than 92%, it was concluded that this method could be simple and applicable for the determination of trace elements in various water samples of a large volume.

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Development and Validation of Reference Material for Proficiency Testing of Blood Heavy Metals in Environmental Biomonitoring (환경 바이오모니터링에서의 혈중 중금속 분석 숙련도 시험을 위한 표준물질 제조 및 적용성 평가)

  • Im, Hosub;Yang, Minho;Oh, Selim;Kim, Soyoung;Jung, Hojun;Cho, Yong Min;Lee, Jung Sub;Kim, Hyun Jeong;Lee, Chae Kwan;Moon, Chan-Seok;Lee, Jong-Wha
    • Journal of Environmental Health Sciences
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    • v.42 no.6
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    • pp.450-464
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    • 2016
  • Objectives: This study developed and validated reference materials (RMs) to analyze metal compounds in blood. Methods: We referred to KoNEHS (Korea National Environmental Health Survey) to estimate concentrations of blood metals (cadmium, Cd; lead, Pb; mercury, Hg) and applied analytical methods (inductively coupled plasma - mass spectroscopy, ICP-MS, for Cd and Pb; graphite furnace - atomic absorption spectrometry, GF-AAS, for Cd and Pb; and direct mercury analyzer, DMA, for Hg). Homogeneity and stability tests were carried out. In addition, certified values and uncertainties of RMs were calculated through internal and external experiments. All RMs were developed and assessed in various forms according to element, analytical method, and two types of concentration levels high concentration for occupational exposure and low concentration for environmental exposure. Results: All samples showed acceptable homogeneity, except for low concentration of Cd in the GF-AAS method. Short- and long-term stabilities were satisfied by ANOVA testing. In the inter-laboratory comparison, robust medians were lower than the certified values of all RMs (robust median/reference value; $1.301/1.327{\mu}g/L$ for Cd, ICP-MS, low concentration; $3.152/3.388{\mu}g/L$ for Cd, ICP-MS, high concentration; $1.219/1.301{\mu}g/L$ for Cd, GF-AAS, low concentration; $3.074/3.321{\mu}g/L$ for Cd, GF-AAS, high concentration; $14.473/14.516{\mu}g/L$ for Pb, ICP-MS, low concentration; $50.069/50.114{\mu}g/L$ for Pb, ICP-MS, high concentration; $12.881/14.147{\mu}g/L$ for Pb, GF-AAS, low concentration; $47.015/47.591{\mu}g/L$ for Pb, GF-AAS, high concentration; $4.059/4.218{\mu}g/L$ for Hg, DMA, low concentration; $11.474/11.181{\mu}g/L$ for Hg, DMA, high concentration). Conclusion: This study demonstrates procedures for developing and validating RMs for biomonitoring in the field of the environmental health.

X-Ray Diffractometric Study on Modification Mechanism of Matrixes for Electrothermal AAS Determination of Volatile Lead and Bismuth

  • Kim, Yeong Sang;Choe, Jong Mun
    • Bulletin of the Korean Chemical Society
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    • v.21 no.1
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    • pp.56-60
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    • 2000
  • The mechanism of a matrix modification for the trace determination of volatile lead and bismuth by an electro-thermal atomic absorption spectrophotometry was studied by a X-ray diffractometry (XRD). For the investigation of structures, the ash products of the elements were produced by using a palladium as a matrix modifier with or without aluminum or nickel as an auxiliary modifier. The same charring conditions as in the analysis of samples were applied together with much concentrated solution of analytical elements and modifiers in a graphite furnace to get a large amount of the product for XRD. The XRD patterns showed PbPd3 for lead and BiPd3 for bismuth. These mean that the reaction procedures through the charring and atomization were changed from $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}$$Pb^0$ to $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}PbPd_3$ ${\rightarrow}$ Pb o for lead and from $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ Bi o to $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ $BiPd_3$ ${\rightarrow}$ $Bi^0$ for bismuth by the addition of modifiers. The volatile elements were stabilized by the formation of palladium alloys through a charring process. Charring temperatures were raised about 500 $^{\circ}C$ by the alloying and the atomization was also stabilized for the enhancement of sensitivities.

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