• Title/Summary/Keyword: Atomic Absorption Spectrometry

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Simultaneous Preconcentration and Determination of Trace Elements in Water Samples by Coprecipitation-Flotation with Lanthanum Hydroxide $[La(OH)_3]$

  • 김영상;김기찬
    • Bulletin of the Korean Chemical Society
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    • v.16 no.7
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    • pp.582-588
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    • 1995
  • The preconcentration and determination of trace Cd(Ⅱ), Cu(Ⅱ), Pb(Ⅱ), Mn(Ⅱ) and Zn(Ⅱ) in water samples were studied by the precipitate flotation using La(OH)3 as a coprecipitant. The analytes were quantitatively coprecipitated by adding 3.0 mL of 0.1 M La(Ⅲ) solution in a 1,000 mL water sample and adjusting the pH to 9.5 with NaOH solution. After the addition of the 1:8 mixed surfactant solution of each 0.1% sodium oleate and sodium lauryl sulfate, the solution was stirred with a magnetic stirrer for 10 minutes. The precipitates were floated to the surface by bubbling with nitrogen gas and collected in a small sampling bottle. The precipitates were dissolved in nitric acid and then the solutions were diluted to 25.00 mL with a deionized water. The analytes were determined by flame atomic absorption spectrometry. This procedure was applied to the waste water analysis. This technique was simple, convenient and especially rapid for the analysis of a large volume of sample. And also, from the recoveries of better than 92% which were obtained from real samples, this method could be judged to be applicable to the preconcentration and quantitative determination of trace elements in water samples.

Fundamental Studies on the Development of On-line Monitoring of Trace Mercury in Drinking Water (음용수 중 수은 연속자동측정시스템의 개발에 관한 연구)

  • Chang, Soo-Hyun;Kim, Hyo-Jin;Kim, Sun-Tae;Kim, Young-Man
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.299-305
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    • 1999
  • The electrolyte cathode atomic glow discharge (ELCAD) is a new plasma source for direct determination of trace heavy metals in drinking and waste water. ELCAD has been successfully developed for on-line monitoring of heavy metals, however, shows difficulty to measure mercury. In this study, ELCAD has been modified to apply the atomic absorption spectrometry (AAS) for the direct determination of trace elements of mercury in flowing water.The fundamental characteristics of this new types of plasma source have been investigated and found that the pH of the solution, discharge voltage, and current are most important factors.The absorbance of 1.0 ppm Hg standard solution increases as pH of the solution increases from pH 1.0 to 3.0.However, % RSD of the absorbance also increases as the pH of solution increasesdue to plasma unstability.The detection limits of the standard solution of pH 1.5 and pH 3.0 are about 40 ppb and 10 ppb level, respectively.

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EXPERIMENTAL STUDY ON THE DISSOLUTION COMPONENTS AND CORROSION PRODUCTS OF SEVERAL AMALGAMS IN ARTIFICIAL SALIVA (인공타액에서 수종 아말감의 부식시 용해성분 및 표면 부식 생성물에 관한 실험적 연구)

  • Cho, Seung-Joo;Lee, Myung-Jong
    • Restorative Dentistry and Endodontics
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    • v.19 no.1
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    • pp.1-26
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    • 1994
  • The purpose of this study was to investigate the dissolution components during corrosion of amalgams and to identify surface corrosion products in the modified Fusayama artificial saliva. Four type of amalgam alloys were used: low copper lathe cut amalgam alloy (Cavex 68), low copper spherical amalgam alloy (Caulk Spherical Alloy), high copper admixed amalgam alloy (Dispersalloy) and high copper single composition amalgam alloy (Tytin). Each amalgam alloy and Hg were triturated according to the manufacturer's direction by means of mechanical amalgamator (Capmaster, S.S.White), and then the triturated mass was inserted into the cylindrical metal mold which was 10mm in diameter and 2.0mm in height and condensed with compression of 150kg/$cm^2$ using oil pressor. The specimens were removed from the mold and stored at room temperature for 7 days and cleansed with distiled water for 30 minutes in an ultrasonic cleaner. The specimens were immersed in the modified Fusayama artificial saliva for the periods of 1 month, 3 months and 6 months. The amounts of Hg, Cu, Sn and Zn dissolved from each amalgam specimen immersed in the artificial saliva for the periods of 1 month, 3 months and 6 months were measured using Inductivity Coupled Plasma Atomic Emission Spectrometry (ICPQ-1000, Shimadzu, Japan) and amount of Ag dissolved from amalgam specimen was measured using Atomic Absorption Spectrophotometry (Atomic Absorption/Flame emission spectrophotometer M-670, Shimadzu, Japan). A surface corrosion products of specimens were analysed using Electron Spectroscopy Chemical Analyser (ESCA PHI-558, PERKIN ELMER, U.S.A.). The secondary image and back scattered image of corroded surface of specimens was observed under the SEM, and the corroded surface of specimens was analysed with the EDX. The following results were obtained. 1. The dissolution amount of Cu was the most in high copper admixed amalgam(Dispersalloy) and the least in high copper single composition amalgam(Tytin). 2. Sn and Zn were dissolved during all the experiment periods, and dissolution amounts were decreased as the time elapsed. 3. Initial surface corrosion products were ZnO and SnO. 4. Corrosion of ${\gamma}$ and ${\gamma}_2$ phase in low copper amalgams was observed and Ag-Cu eutectic alloy phase was corroded in low copper spherical amalgam(Caulk Sperical Alloy). 5. Corrosion of ${\gamma}$ and $\eta$' phase in high copper amalgams was observed and Ag-Cu eutectic alloy phase was corroded in high copper admixed amalgam(Dispersalloy). 6. Sn-Cl was produced in the subsurface of low copper amalgams and high copper admixed amalgam.

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Sequential Extraction of Heavy Metals in Soils and A Case Study (토양중의 중금속 연속추출방법과 사례연구)

  • Jung, Myung Chae
    • Economic and Environmental Geology
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    • v.27 no.5
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    • pp.469-477
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    • 1994
  • Many researchers have investigated most representative sequential extraction method using various reagents for determining the chemical forms of metals in soils and sediments. In this paper, a newly modified method for sequential extraction scheme based on Tessier's method by Environmental Geochemistry Research, Centre for Environmental Technology, Imperial College, was introduced and examined. In comparison with Tessier's method, originally designed for sediment analysis by Atomic Absorption Spectrophotometry (AAS), the sequential extraction scheme has been developed for the multi-element analysis by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The partitioning of particulate trace elements was classified into five fractions: (i) exchangeable, (ii) bound to carbonates or specially adsorbed, (iii) bound to Fe and Mn oxides, (iv) bound to organic matter and sulphides and (v) residuals. The experimental results of the pilot study for in-house reference material (HRM2) and certified international standard reference material (SRM2711) using the modified method showed not only reasonable precision and accuracy but also acceptable overall recovery rates. In addition, mine dump soils sampled in the Dalsung Cu-W mine, Korea were prepared and sequentially extracted using the method. Most of Cu was bound to organic matter/sulphides and residual fractions. The dominant fraction of soil Pb and Zn in the study area was found in the residuals. The fraction of Cd showed a wide variation between samples and could be found bound to the carbonates or specially adsorbed, oxides, organic fraction and residuals. The recovery rates of Cd, however, were poor due to relatively low Cd concentrations in soils. The heavy metals in these mine dumps appear to be in the more inert forms and should not be readily bioavailable. The soils, however, had very low pH values (average 4.1) and had sandy textures; consequently, rapid infiltration of rainfall may increase leaching of Zn and Cd which were found to be around 5 to 10% of the exchangeable fraction. As a result of the investigation of this study, it has been strongly recommended that these mine waste materials should still be considered a significant contaminant source and will need environmental remediation to prevent pollutants from being released into the environment.

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Identification of Irradiated Crabs by ESR Spectrometry

  • Nam, Hye-Seon;Ly, Sun-Yung;Yang, Jae-Seung
    • Journal of Food Hygiene and Safety
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    • v.15 no.1
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    • pp.1-4
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    • 2000
  • Electron spin resonance (ESR) spectroscopy was used to investigate the effect of irradiation dose on the ESR signal intensity of irradiated crabs and the stability of these radicals under 9 weeks of storage. Swimming and small crabs were irradiated with doses of 0, 1, 3, 5 and 7 kGy using a Co-60 irradiator at ambient temperature. A claw, a walking leg and a cars- pace of the crab pieced and dried were placed in a resonant quart tube within an EPR X-band spectrometer. The irradiated crabs presented an asymmetric absorption in shape at g$_1$=2.002 $\pm$ 0.003 and g$_2$=1.998$\pm$0.005, and were different from the non-irradiated ones. The intensity of the ESR signals was greatest in the claw, intermediate in the carapace and lowest in the walking leg. Samples given low and high doses of irradiation could also be distinguished. The ESR signal after irradiation was stable, even after a 9-week storage.

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Comparative Analysis of the Physical and Biochemical Properties of Light-cure Resin-modified Pulp Capping Materials

  • Tae Gyeom Kim;Jongsoo Kim;Joonhaeng Lee;Jisun Shin;Mi Ran Han;Jongbin Kim;Yujin Kim;Jae Hee Park
    • Journal of the korean academy of Pediatric Dentistry
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    • v.51 no.2
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    • pp.149-164
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    • 2024
  • This study compared the solubility, water absorption, dimensional stability, release of various ions (hydroxyl, calcium, sulfur, strontium, and silicon), and cytotoxicity of light-cured resin-modified pulp-capping materials. Resin-modified calcium hydroxide (Ultra-blendTM plus, UBP), light-cured resin-modified calcium silicate (TheraCal LCTM, TLC), and dual-cure resin-modified calcium silicate (TheraCal PTTM, TPT) were used. Each material was polymerized; solubility, 24-hour water absorption, and 30- day dimensional stability experiments were conducted to test its physical properties. Solubility was assessed according to the ISO 6876 standard, and 24 hours of water absorption, 30 days of dimensional stability were assessed by referring to the previous protocol respectively. Eluates at 3 and 24 hours and on 7, 14, and 28 days were analyzed according to the ISO 10993-12 standard. And the pH, Ion-releasing ability, cell proliferation rate, and cell viability were assessed using the eluates to evaluate biochemical characteristics. pH was measured with a pH meter and Ion-releasing ability was assessed using inductively coupled plasma atomic emission spectrometry (ICP-AES). Cell proliferation rate and cell viability were assessed using human dental pulp cells (hDPCs). The former was assessed by an absorbance assay using the CCK-8 solution, and the latter was assessed by Live and Dead staining. TPT exhibited lower solubility and water absorption than TLC. UBP and TPT demonstrated higher stability than TLC. The release of sulfur, strontium, calcium, and hydroxyl ions was higher for TLC and TPT than for UBP. The 28-day release of hydroxyl and silicon ions was similar for TLC and TPT. TLC alone exhibited a lower cell proliferation rate compared to the control group at a dilution ratio of 1 : 2 in cell proliferation and dead cells from Live and Dead assay evaluation. Thus, when using light-cure resin-modified pulp-capping materials, calcium silicate-based materials can be considered alternatives to calcium hydroxide-based materials. Moreover, when comparing physical and biochemical properties, TPT could be prioritized over TLC as the first choice.

Determination of boron in steel by HNO3-NH4HF2 digestion and ICP-MS (질산-이플루오린화암모늄 분해 및 ICP-MS에 의한 철강 중 붕소 정량에 관한 연구)

  • Choi, Won Myung;Eum, Chul Hun;Park, Ilyong
    • Analytical Science and Technology
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    • v.27 no.6
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    • pp.352-356
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    • 2014
  • Various studies have been done to improve the properties of the steel by adding boron to the steel. Some studies have reported on the analysis of the boron in steel by AAS (atomic absorption spectrometry), ICP-OES(inductively coupled plasma-optical emission spectrometry), ICP-MS (inductively coupled plasma/mass spectrometry). The volatile loss of boron of steel in sample digestion and the separation procedure for avoiding matrix effect by high concentration of iron are difficulties for determination of boron in steel. The method to determine boron in steel by ICP-MS was developed without volatilization of boron in sample digestion step with $HNO_3-NH_4HF_2$ digestion method, and the additional separation process for avoiding matrix effect. Complete decomposition of steel with $HNO_3-NH_4HF_2$ digestion method, and boron determination by ICP-MS in the matrix of high concentration of iron were possible. Quantitative recoveries of boron in certified standard steel by new method in this study were 103 to 111%, and the relative standard deviation is less than 5%. The method detection limit was $1.17{\mu}g/g$.

A Comparative Analysis of Whole Blood Cadmium by Atomic Absorption Spectrophotometry with a Graphite Furnace (흑연로 원자흡수분광법에 의한 혈액중 카드뮴 정량분석)

  • Park, Jong An;Oh, Hye Jeong;Lee, Jong Hwa
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.6 no.2
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    • pp.301-312
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    • 1996
  • This study was performed to search a optimal analyzing method of cadmium in whole-blood. Cadmium was determined by graphite furnace atomic absorption spectrometry(GFAAS). We investigated the effect of ashing temperature on the absorbance of cadmium in a simple dilution(ten-fold) method with triton X-100 and matrix modifier methods treated with $NH_4H_2PO_4$(1 and 3%) and $Pd(NO_3)_2$(0.00l and 0.005%) as matrix modifier. We also compared the reported reference values of standard blood with values resulted from optimal analyzing conditions of this study. In case of a simple dilution method, when ashing temperature was set at $450^{\circ}C$, the absorbance of sample and background were $0.334{\pm}0.012$ and $1.382{\pm}0.245$, respectively. Background level was higher than the value(0.8) that can be corrected by $D_2$ background correction method. As ashing temperature was rised to $500^{\circ}C$, the absorbance of sample and background were $0.178{\pm}0.008$ and $0.711{\pm}0.223$ respectively. The higher ashing temperature($450^{\circ}C-650^{\circ}C$) was, the lower the absorbance of sample was. In case of a matrix modifier method with $NH_4H_2PO_4$(1 and 3%), when ashing temperature was rised from $500^{\circ}C$ to $650^{\circ}C$, the absorbance of sample slightly changed. The absorbances of sample at $600^{\circ}C$ were $0.230{\pm}0.017$ and $0.137{\pm}0.012$, respectively. These values were larger than that of simple dilution method. But the absorbance of background was higher than the level that can be corrected by $D_2$ method. In case of a matrix modifier method with $Pd(NO_3)_2$(0.001 and 0.005%), the absorbance of sample and background were higher than those of other methods and were stable and reproducible. When ashing temperature was over $550^{\circ}C$, the absorbance of sample was significantly decreased. In case of 0.005% $Pd(NO_3)_2$ carbon residue remained in graphite tube affected the absorbance of sample and background. From these results, We propose that in case of a simple dilution(ten-fold) method with triton X-100 ashing temperature must be maintained below $400^{\circ}C$. In order to diminish the absorbance of background, the alternative method is attenuation of injection volume or multiplication of dilution ratio. We recommend $Pd(NO_3)_2$ than $NH_4H_2PO_4$ as a matrix modifier. In case of a matrix modifier method with $Pd(NO_3)_2$ ashing temperature might be maintained below $550^{\circ}C$.

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A Study of the Relationships Between Proximity to an Industrial Complex and Blood Lead Levels and Urinary Cadmium Levels (거주지와 산업단지간의 거리와 혈 중 납 농도 및 요 중 카드뮴 농도의 상관관계에 관한 연구)

  • Heo, Jin-A;Kim, Hyo-Mi;Lee, Jong-Tae
    • Journal of Environmental Health Sciences
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    • v.38 no.2
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    • pp.95-104
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    • 2012
  • Objectives: The goal of this study was to investigate the relationships between proximity to an industrial complex and blood lead levels and urinary cadmium levels. Methods: We conducted a questionnaire survey and analyzed blood lead and urinary cadmium levels using Atomic Absorption Spectrometry (AAs). Data was analyzed using logistic regression analysis. All statistical analyses were conducted with SAS software version 9.2. The distance between the residence and an industrial complex was calculated through a Geographical Information System (GIS). Results: A total of 967 residents living near a large petrochemical complex in Ulsan participated. The geometric mean levels of blood lead and urinary cadmium were $1.70{\mu}g/dl$ (male: $1.77{\mu}g/dl$, female: $1.67{\mu}g/dl$), and $0.72{\mu}g/g$ creatinine (male: $0.49{\mu}g/g$ cr. female: $0.89{\mu}g/g$ cr.), respectively. Blood lead and urinary cadmium levels both increased with age and were higher among smokers compared to never smokers. Both significantly showed a decreasing trend with rising income. Results from multiple logistic regression analysis showed that urinary cadmium levels for subjects aged less than 20 years old were negatively associated with distance from the industrial area to the residence. The results, however, indicated that the blood lead levels were positively associated with the distance. Conclusions: The results of this study support that proximity to an industrial complex is related to urinary cadmium values for children. A positive finding with blood lead can be explained by the ambiguity of lead exposure sources in the general environment.

The impact of municipal waste disposal of heavy metals on environmental pollution: A case study for Tonekabon, Iran

  • Azizpour, Aziz;Azarafza, Mohammad;Akgun, Haluk
    • Advances in environmental research
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    • v.9 no.3
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    • pp.175-189
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    • 2020
  • Municipal solid waste disposal is considered as one of the most important risks for environmental contamination which necessitates the development of strategies to reduce destructive consequences on the ecosystem as related especially to heavy metal accumulation. This study investigates heavy metal (i.e., As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Zn) accumulation in the Tonekabon region, NW of Iran that is related to city waste disposal and evaluates the environmental impact in the Caspian Sea coastal region. For this purpose, after performing field studies and collecting 50 soil specimens from 5 sites of the study area, geochemical tests (i.e., inductively coupled plasma mass spectrometry, atomic absorption spectroscopy and x-ray fluorescence) were conducted on the soil specimens collected from the 5 sites (named as Sites A1, A2, A3, A4 and A5) and the results were used to estimate the pollution indices (i.e., geo-accumulation index, normalized enrichment factor, contamination factor, and pollution load index). The obtained indices were utilized to assess the eco-toxicological risk level in the landfill site which indicated that the city has been severely contaminated by Cu, Mn, Ni, Pb and Zn. These levels have been developed along the stream towards the nearshore areas indicating uptake of soil degradation. The heavy metal contamination was classified to range from unpolluted to highly polluted, which indicated serious heavy metal pollution in the study area as related to municipal solid waste disposal in Tonekabon.