• Title/Summary/Keyword: microwave digestion method

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A Study on Sample Preparation for the Analysis of Trace Elements in Foods of Animal Origin by Ultra High Pressure Microwave Digestion (초고압초음파분해법을 이용한 축산물내 미량금속 잔류분석을 위한 시료전처리 방법)

  • Lee, Myoung-heon;Lee, Hee-su;Son, Seong-wan;Jung, Gab-soo;Park, Jong-myung;Kim, Sang-keun
    • Korean Journal of Veterinary Research
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    • v.43 no.3
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    • pp.393-398
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    • 2003
  • Simple and rapid sample preparation method for trace elements in foods of animal origin using ultra high pressure microwave digestion system (UHP/MDS) and inductively coupled plasma atomic emission spectrometer (ICP/AES) were developed. 1. For the digestion of sample using UHP-MDS, 20% nitric acid (v/v) was the most suitable solvent for the determination of trace elements in foods of animal origin. 2. The optimal digestion conditions for UHP-MDS were as follows: final temperature $180^{\circ}C$, final pressure 400 PSI, and magnetic power 900 W in the solid sample. For the liquid sample final temperature $170^{\circ}C$, final pressure 300 PSI and magnetic power 700 W were optimal conditions. 3. As result of interlaboratory test, the average recovery rate of the for solid sample were 88.3~99.1% for As, 82.4~93.3% for Cd, 89.2~101.2% for Hg and 86.5~93.8% for Pb, respectively. In liquid sample, it were 87.0~96.8% for As, 80.9~96.6% for Cd, 87.5~91.2% for Hg and 91.4~95.5% for Pb, respectively. 4. The average coefficient variation rate were 3.3~15.9% for solid sample and 2.9~10.8% for liquid sample.

Improvement of Acid Digestion Method by Microwave for Hazardous Heavy Metal Analysis of Solid Refuse Fuel (고형연료제품의 유해중금속 분석을 위한 마이크로파 산 분해법의 개선)

  • Yang, Won-Seok;Park, Ho-Yeun;Kang, Jun-Gu;Lee, Young-Jin;Lee, Young-Kee;Yoon, Young-Wook;Jeon, Tae-Wan
    • Journal of Korea Society of Waste Management
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    • v.35 no.7
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    • pp.616-626
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    • 2018
  • The quality standards of solid refuse fuel (SRF) define the values for 12 physico-chemical properties, including moisture, lower heating value, and metal compounds, according to Article 20 of the Enforcement Rules of the Act on Resource Saving and Recycling Promotion. These parameters are evaluated via various SRF Quality Test Methods, but problems related to the heavy metal content have been observed in the microwave acid digestion method. Therefore, these methods and their applicability need improvement. In this study, the appropriate testing conditions were derived by varying the parameters of microwave acid digestion, such as microwave power and pre-treatment time. The pre-treatment of SRF as a function of the microwave power revealed an incomplete decomposition of the sample at 600 W, and the heavy metal content analysis was difficult to perform under 9 mL of nitric acid and 3 mL of hydrochloric acid. The experiments with the reference materials under nitric acid at 600 W lasted 30 minutes, and 1,000 W for 20 or 30 minutes were considered optimal conditions. The results confirmed that a mixture of SRF and an acid would take about 20 minutes to reach $180^{\circ}C$, requiring at least 30 minutes of pre-treatment. The accuracy was within 30% of the standard deviation, with a precision of 70 ~ 130% of the heavy metal recovery rate. By applying these conditions to SRF, the results for each condition were not significantly different and the heavy metal standards for As, Pb, Cd, and Cr were satisfied.

Multi - elemental Analysis of Hair by Inductively Coupled Plasma/Mass Spectrometry (유도결합 플라스마 질량분석법에 의한 모발의 다원소 분석)

  • Cha, Myung Jin;Kang, Jun Mo;Park, Chang Joon
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.335-340
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    • 2002
  • An analytical method has been developed to determine multi-elements in human hair samples by inductively coupled plasma mass spectrometry (ICP-MS). 0.05 g of hair sample was added to the Teflon digestion bomb together with 1.5 mL of nitric acid and an appropriate amount of In as an internal standard. The sample was then decomposed in the microwave digestion system. The hair certified reference material, GBW 09101, was analyzed for the validation of the analytical method. The determined values were in good agreement with the certified values within the uncertainty range.

Analytic study on arsenic content in plastic materials (플라스틱 소재의 비소 함유량 분석에 관한 연구)

  • Lee, Jae-In;Choi, Zel-Ho;Choi, Ki-In;Ko, Byung-Rae;Choi, In-Suk;Cho, Hun-Sik
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.402-409
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    • 2012
  • Quantitative analytical condition for arsenic in plastic materials by the flow injection-hydride generation-inductively coupled plasma-atomic emission spectrometry was studied. The plastic samples were dissolved by wet-acid digestion method and microwave-acid digestion method. The reproducibility and accuracy in this method was verified using of certified reference materials(CRMs) CRM-EC680k and CRM-EC681k. The analyical results agrees with certified value within the range of uncertainty. The results of CRM-EC680k wer 4.1~4.3 mg/kg (certified value $4.1{\pm}0.5$ mg/kg), and the results of CRM-EC681k were 28.9~30.6 mg/kg (certified value $29.1{\pm}1.8$ mg/kg).

Method and proficiency test for analysis of toxic metals in livestock products by ICP/MS (ICP/MS를 이용한 축산물의 유해중금속 분석방법 및 숙련도 검증)

  • Jang, Jung-Hee;Kim, Dong-Gyu;Kwon, Hyun-Jeong;Lim, Chae-Mi;Son, Seong-Wan;Kim, MeeKyung
    • Korean Journal of Veterinary Research
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    • v.52 no.2
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    • pp.69-74
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    • 2012
  • The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

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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Matrix effect on the Determination of Inorganic Priority Pollutants in Sludges (오니 시료중의 무기 Priority Pollutants의 분석 과정에 미치는 매질의 영향)

  • Lee, Huk-Hee;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.11 no.4
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    • pp.297-304
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    • 1998
  • The three analysis methods, EPA method 3050, the method offered by Ministry of Environment in Korea, and modified method corrected in this laboratory, were studied to investigate the effect of matrix on the analysis of inorganic priority pollutants. 7 inorganic priority pollutants(Ni, Cr, Cu, Zn, Pb, Cd, Hg) were spiked to the plating, leather, paper, electric, and dye sludges. Mean recovery of the elements except Hg was 95.5% when the procedure of EPA method was applied. However, recovery by the two other extraction methods showed 11.1% and 27.7%, respectively. Digestions were done by MDS (microwave digestion system) and $HNO_3+HClO_4$ methods. To study organic and inorganic matrix effect, samples were made by adding triethanol amine as a organic matrix and $FeCl_3{\cdot}6H_2O$+$AlCl_3{\cdot}6H_2O$ as a inorganic matrix, respectively. The extracts were analyzed by AAS and HG-AAS. Mean recovery of the elements by the $HNO_3+HClO_4$ procedure, except Hg, gave better result than that of the MDS method. Mean recovery of elements was decreased when organic and inorganic matrices were added in the sludge samples. The procedure of MDS and $HNO_3+HClO_4$ digestion gave higher recoveries than that of direct analysis. In general, the results of the studies showed a significant matrix effect on the inorganic priority pollutants analysis in sludges.

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Considerations of Acid Decomposition System for the Analysis of Heavy Metals in Packaging-grade Paper (포장용지류에서의 중금속 분석을 위한 산분해 전처리 방법의 탐색)

  • Lee, Tai-Ju;Ko, Seung-Tae;Kim, Hyoung-Jin
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.43 no.1
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    • pp.65-73
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    • 2011
  • The fibrous raw materials in packaging-grade paper production in Korea were mainly obtained from waste paper. The use of recycled paper has both positive and negative impacts in papermaking process. The primary positive impacts are the environmental protection and manufacturing cost reduction, and the negative impacts are the quality reduction in paper quality and the accumulation of heavy metals and other pollutants in wet- and dry-end process. This study was carried out to consider the optimum acid decomposition system with the highest recovery rate for the analysis of heavy metals in packaging-grade paper. The open digestion system using Kjeldahl apparatus and the closed digestion system using microwave oven for decomposing the organic materials in paper were compared. In both open and closed digestion method, the combination of nitric acid, hydrochloric acid and hydrogen peroxide showed higher recovery rate than using only nitric acid alone because the presence of Cl- ions in hydrochloric acid stabilizes ligand formation with metal ions. KOCC was observed to have the highest heavy metal content among the recycled paper samples. The heavy metal contents decomposed with the closed digestion system were relatively higher than with open digestion system.

In Vitro Effects of Cooking Methods on Digestibility of Lipids and Formation of Cholesterol Oxidation Products in Pork

  • Hur, Sun Jin;Lee, Seung Yuan;Moon, Sung Sil;Lee, Seung Jae
    • Food Science of Animal Resources
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    • v.34 no.3
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    • pp.280-286
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    • 2014
  • This study investigated the effects of cooking methods on the digestibility of lipids and formation of cholesterol oxidation products (COPs) in pork, during in vitro human digestion. Pork patties were cooked using four different methods (oven cooking, pan frying, boiling, and microwaving), to an internal temperature of approximately $85^{\circ}C$. The digestibility of pork patties were then evaluated, using the in vitro human digestion model that simulated the composition (pH, minerals, surfaceactive components, and enzymes) of digestive juices in the human mouth, stomach, and small intestine. The total lipid digestibility was higher after microwave cooking, whereas pan-frying resulted in lower in vitro digestibility, compared to the other cooking methods. The microwaving method followed by in vitro digestion also showed significantly higher content of free fatty acids and thiobarbituric acid reactive substances (TBARS), compared to the other cooking methods; whereas, the pan frying and boiling methods showed the lowest. Cholesterol content was not significantly different among the cooked samples before, and after in vitro human digestion. The formation of COPs was significantly higher in the microwave-treated pork samples, compared to those cooked by the other methods, which was consistent with the trend for lipid peroxidation (TBARS). We propose that from the point of view of COPs formation and lipid oxidation, the pan-frying or boiling methods would be useful.