• Title/Summary/Keyword: microwave digestion

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Chemical leaching of radioactive cement and paraffin waste form generated from NPPs (원전 발생 고화체 폐기물 핵종분석을 위한 침출 조건)

  • Lee Jeong-Jin;Ahn Hong-Joo;Pyo Hyung-Yeal;;;Jee Kwang-Young
    • Proceedings of the Korean Radioactive Waste Society Conference
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    • 2005.06a
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    • pp.278-283
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    • 2005
  • Cement and paraffin waste form were prepared with a acid extraction method for the analysis of radionuclides generated from nuclear power plants. The acid extraction method was carried out with $HNO_3-HCl$ acid. At first, we compared the method with the microwave acid digestion method using SRM. The solutions of decomposed SRM were then analyzed by AAS and ICP-AES. The acid extraction method had shown good results as microwave acid digestion method. This method provided recovery values greater than $80\%$ for metallic elements.

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Simultaneous Determination of Tin, Nickel, Lead, Cadmium and Mercury in Cigarette Material by Solid Phase Extraction and HPLC

  • Hu, Qun;Yang, Guangyu;Ma, Jing;Liu, Jikai
    • Bulletin of the Korean Chemical Society
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    • v.24 no.10
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    • pp.1433-1436
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    • 2003
  • A new method for the simultaneous determination of heavy metal ions in cigarette material by microwave digestion and reversed-phase high-performance liquid chromatography (RP-HPLC) has been developed. The cigarette material was digested by microwave digestion. Lead, cadmium, mercury, nickel and tin ions in the digested samples were pre-column derivatized with tetra-(2-chlorophenyl)-porphyrin ($T_2$-CPP) to form color chelates, which were then enriched by solid phase extraction with a $C_{18}$ cartridge. The chelates were separated on a Waters Xterra$^{TM}RP_{18}$ column by gradient elution with methanol (containing 0.05 mol/L pyrrolidine-aceticacid buffer salt, pH = 10.0) and acetone (containin0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0)as mobile phase at a flow rate of 0.5mL/min and analyzed with a photodiode array detector from 350-600 nm. The detection limits of lead, cadmium, mercury, nickel and tin were 4,3,3,8 and 5 ng/L, respectively, in the original samples. This method was afforded good results.

Comparison of Heavy Metals Analysis in Sediment (호소내 퇴적물의 중금속 분석 비교)

  • Park, Sun-Ku;Song, Ki-Bong;Cho, Ki-Hwan
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.173-179
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    • 2001
  • The study was carried out to analyze the pollutant Fe, Cu, Cr, Zn, Cd for sediments collected from lake in K river basin. Three analytical methods currently used in Korea, Japan, U.S.A, were compared. Pretreatment using microwave digestion showed higher analytical results for Fe, Cu, Cr, Zn, Cd than Korean Official Method(KOM) and American Toxicity Characteristic Leaching Procedure(TCLP) Method. Also, analytical results using microwave digestion, TCLP and KOM were as follows: 38.1-48.0 mgFe/kg, 10.2-15.9 mgFe/kg AND 3.5-12.6 mgFe/kg, 37.0-50.1 mgCu/kg, 0.06-0.24 mgCu/kg and 0.01-0.03 mgCu/kg, 137.0-152.0 mgZn/kg, 0.67-0.82 mgZn/kg and 0.3-0.5 mgZn/kg, respectively. From this result, a new analytical method for the determination of heavy metal in sediment should be developed for the accurate estimation of pollution degree in sediment.

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Determination of heavy metals in mainstream smoke by ORS-ICP-MS (ORS-ICP-MS를 이용한 담배 연기의 중금속 성분 분석)

  • Cho, Sung-Eel;Ji, Sang-Un;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.1
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    • pp.25-32
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    • 2008
  • In this study, we compared three different pretreatment methods, such as block digestion, microwave digestion and solvent injection, coupled with Octopole Reaction System(ORS)-ICP-MS was used for the quantification of heavy metals in mainstream smoke of 2R4F reference cigarette, and then evaluated those efficiencies in the recovery, repeatability and reproducibility. In all methods, volatile heavy metals, As, showed the highest CV value, and Cd showed the lowest one. However, the solvent injection method showed the most stable recovery rate and CV value of 2.36 %. This method showed also advantages in time-consuming and compatibility with ICP-MS system. This results demonstrate that solvent injection method can be recommended as a superior pretreatment procedure to be able to reduce contaminants and spectral interference as well as loss of the elements interested.

Detection of Heavy Metal Contents in Sesame Oil Samples Grown in Korea Using Microwave-Assisted Acid Digestion

  • Park, Min-Kyoung;Yoo, Ji-Hyock;Lee, Je-Bong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Won-Il
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.45-49
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    • 2013
  • This study aimed to determine heavy metal contents in sesame oil samples produced in Korea through microwave-assisted acid digestion without using an emulsifier. Three heavy metal, cadmium (Cd), lead (Pb) and arsenic (As) in twelve sesame oil samples were determined by ICP-MS. The validation of analysis method was checked by standard addition method (10 and $100{\mu}g/kg$). As a result, linearity ($R^2$) was above 0.999 and RSDs were lower than 4%. The recovery of Cd, Pb and As ranged between 98.5-101.6%, 100.3-101.3%, and 102.1-111.2%, respectively. The detected ranges in sesame oil samples were as follows; N.D. to $0.109{\mu}g/g$ for Cd, 0.014 to $0.200{\mu}g/g$ for Pb and 0.014 to $0.125{\mu}g/g$ for As, respectively. Therefore, sesame seeds and products grown in heavy metal-polluted regions which are used as food should be given priority attention and consideration.

Effect of Temperature-increase Rate and Terminal Temperature on the Solubilization of Sewage Sludge using Microwave Irradiation

  • Park, Woon-Ji;Ahn, Johng-Hwa;Lee, Chan-Ki
    • Environmental Engineering Research
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    • v.14 no.1
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    • pp.48-52
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    • 2009
  • Solubilization of sewage sludge creates favorable conditions for anaerobic microorganisms to produce biogas. In this paper, we quantify the effect of heating pretreatment on the degree of solubilization of sewage sludge. The pretreatment process was carried out using a lab-scale industrial microwave unit (2450 MHz frequency). Response surface analysis was applied to determine the combination of temperature-increase rate (ramp rate) (2.9 to 17.1 ${^{\circ}C}$/min) and terminal temperature (52 to 108${^{\circ}C}$). Both ramp rate and temperature significantly affected the solubilization degree of sludge. Within the design boundaries, the conditions predicted to maximize the solubilization degree of 15.8% were determined to be 2.9 ${^{\circ}C}$/min and 104${^{\circ}C}$.

Changes in Nutritive Value and Digestion Kinetics of Canola Seed Due to Microwave Irradiation

  • Ebrahimi, S.R.;Nikkhah, A.;Sadeghi, A.A.
    • Asian-Australasian Journal of Animal Sciences
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    • v.23 no.3
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    • pp.347-354
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    • 2010
  • This study aimed to evaluate effects of 800 W microwave irradiation for 2, 4 and 6 min on chemical composition, antinutritional factors, ruminal dry matter (DM) and crude protein (CP) degradability, and in vitro CP digestibility of canola seed (CS). Nylon bags of untreated or irradiated CS were suspended in the rumen of three bulls from 0 to 48 h. Protein subfractions of untreated and microwave irradiated CS before and after incubation in the rumen were monitored by sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). Microwave irradiation had no effect on chemical composition of CS (p>0.05). There was a linear decrease (p<0.001) in the phytic acid and glucosinolate contents of CS as irradiation time increased. Microwave irradiation for 2, 4 and 6 min decreased the phytic acid content of CS by 8.2, 27.6 and 48.6%, respectively. The total glucosinolate contents of CS microwave irradiated for 2, 4 and 6 min decreased by 41.5, 54.7 and 59.0% respectively, compared to untreated samples. The washout fractions of DM and CP and degradation rate of the b fraction of CP decreased linearly (p<0.001) as irradiation time increased. Microwave irradiation for 2, 4 and 6 min decreased effective degradability (ED) of CP at a ruminal outflow rate of 0.05 $h^{-1}$ by 4.7, 12.3 and 21.0%, respectively. Microwave irradiation increased linearly (p<0.001) in vitro CP digestibility of ruminally undegraded CS collected after 16 h incubation. Electrophoresis results showed that napin subunits of untreated CS disappeared completely within the zero incubation period, whereas cruciferin subunits were degraded in the middle of the incubation period (16 h incubation period). In 4 and 6 min microwave irradiated CS, napin subunits were degraded after 4 and 16 h incubation periods, respectively, and cruciferin subunits were not degraded untile 24 h of incubation. In conclusion, it seems that microwave irradiation not only protected CP of CS from ruminal degradation, but also increased in vitro digestibility of CP. Moreover, microwave irradiation was effective in reducing glucosinolate and phytic acid contents of CS.

Sludge Solubilization using Microwave Irradiation in the Presence of Fe Powder

  • Yi, Min-Joo;Choi, Hyun-Kyung;Han, Ihn-Sup
    • Journal of Soil and Groundwater Environment
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    • v.15 no.2
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    • pp.40-46
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    • 2010
  • In this study, microwave irradiation, which is reflected by metals, was used to reduce the amount of sewage sludge, and the results were used to verify solubilization efficiency and determine optimum operation conditions. Biogas production and methane content of the gas under optimized conditions were measured with the biochemical methane potential (BMP) test. The sludge was taken from a thickened sludge tank at J sewage treatment plant (JSTP) in Seoul, Korea. For the experiments, 50 mL of sludge was filled in vessels and the vessels were irradiated with the power of 500, 600, 700, and 800W for 2~5 min. In addition, Fe powder was added by 0.01, 0.05, and 0.1 g to compare the efficiency with and without Fe powder. The results confirmed that solubilization efficiency was higher in the presence of Fe powder. The optimum conditions of 0.01 g addition of Fe powder with 800W irradiation for 5 min, yielded nearly 22.95% higher solubilization efficiency than without Fe powder. The BMP tests were carried out using sludge obtained from the experiments carried out under the optimum conditions. As a result, sludge subjected by 800W with 0.01 g of Fe powder for 5 min displayed the highest level of gas production and methane content. Through this study, it could be confirmed that solubilization efficiency increased by addition of Fe powder.

Study on the Pre-treatment for Quantitative Analysis of Mercury in Paper Packaging Materials (지류포장재에서의 수은 정량분석을 위한 전처리 방법 연구)

  • Ko, Seung-Tae;Lee, Tai-Ju;Park, Ji-Hyun;Kim, Hyoung-Jin
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.42 no.5
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    • pp.67-73
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    • 2010
  • Paper packaging materials are essential in protection and transportation of commercial or industrial products. Raw materials for packaging paper production are mainly obtained from various grades of waste paper. For this reason, the recycled fibers from waste paper would probably have possibility of containing heavy metals. This study was focused on the development of optimum pre-treatment method for the quantitative analysis of mercury. The optimum pre-treatment for open digestion system were obtained at the treatment conditions of acid combination with $HNO_3/HCl/H_2O_2$ or $HNO_3/H_2SO_4$ at $80^{\circ}C$. The optimum pre-treatment conditions in closed digestion system were determinated by the acid combination with $HNO_3/HCl/H_2O_2/HF$ in microwave at 320 W for 20 min. The recovery rate in open digestion system was 85~94% and in closed digestion system was indicated as about 100%. Therefore, the closed system is superior than the open system in pre-treatment method for the quantitative analysis of mercury, and the detected mercury contents in the sample of KOCC, AOCC and kraft sack paper were measured below 1 ppm.

A Study of Analytical Method for Trace Metal Ions in Whole Blood and Urine by Inductively Coupled Plasma-Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 혈액 및 소변중 미량금속의 분석에 관한 연구)

  • Lee, Won;Hur, Young-Hoe;Park, Kyung-Su
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.281-291
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    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in blood and urine has been investigated by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Microwave oven was used for the pretreatment of blood samples using nitric acid and hydrogen peroxide in a closedvessel digestion system with 1 mL whole blood for 8 minutes. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Detection limits for Cu, Sn, and Bi by this method were 0.000375 ng/mL, 0.000297 ng/mL, and 0.000174 ng/mL, respectively. Recoveries of 99.1% for Cu, 102.5% for Sn, and 98.4% for Bi were obtained for the standard spiked NIST SRM 955a blood sample. The developed method was applied for whole real blood and urine samples.

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