• Proceedings of the KSEEG Conference
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• 2003.04a
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• pp.76-79
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• 2003

국내의 토양오염 공정시험방법에서는 Zn, Ni 추출시 산분해법에 가까운 방법을 사용하는 반면, Cd, Cu, Pb, $Cr^{6+}$ 추출시 0.1N HCl용액으로 산처리하여 1시간을 진탕한 후 이를 필터로 여과하여 분석용액을 추출하는 용출법을 사용하고 있다(환경부, 2001). 시료내에는 완충 물질이 존재하기 때문에 용출법 사용시 초기 pH 인 1(0.1N HCl)이 유지되지 않아 완충능력이 높은 토양의 경우 현재 국내 공정법상의 용출법이 중금속 오염정도를 추정하는데 적절치 않을 수 있다. (중략)

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.5 no.4
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• pp.267-272
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• 2007

Various kinds of RI wastes are discharged from licensed organizations of radioisotopes les such as hospitals and clinic organizations, educational organizations, research institutions, and public organizations. Radioiodines such as $^{125}I\;and\;^{131}I$ are radioisotopes mainly used in nuclear medicine and industry. A method for the determination of radioiodines in RI wastes has been applied to measure low level activity using acid decomposition method and HPGe gamma ray spectrometer. Prior to analysis of real samples, $^{131}I$ reference solution and 10 g of yellow tissue paper was added to flask in mantle and was heated in 100 mL of 0.4 N $K_2Cr_2O_7$ and 100 mL of 9 M $H_2SO_4$, and then distilled after adding 10 mL of 30% $H_2PO_3$ and 1 mL of 30% $H_2O_2$. The condensed iodine by circulator was extracted into $CCl_4$, then back-extracted into the aqueous phase with 10 mL of 5% $K_2SO_2$ solution. Finally, $^{131}I$ was measured at 364.48 keV using HPGe gamma ray spectrometer after precipitation and filtration. Chemical yield of three steps such as acid decomposition process, chemical separation process, and precipitation and filtration process was more han 94% respectively, MDA(Minimum Detectable Activity) of $^{131}I$ at this analytical condition was 0.6 Bq/g.

• Analytical Science and Technology
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• v.26 no.2
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• pp.135-141
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• 2013

The purpose of this study is to determine the quantity of selenium in grains by hydride generation-inductively coupled plasma mass spectrometry. Two sample preparation methods, beaker and microwave digestions, are compared and the former shows better result. The optimum condition for hydride generation is 4.0 M for HCl, 3% for $NaBH_4$ with the sample flow of 0.6 mL/min. The detection limit is 0.02 ${\mu}g/kg$($3{\sigma}$) and improved by 10 times. Isobaric interferences on Se is removed by Octopole Reactoin Cell and $H_2$ (3.8 mL/min) shows better performance over He. However, in case Br exists in a matrix, $H_2$ could induce interferences on m/z 80 and 82 ($^{80}[BrH]^+$ and $^{82}[BrH]^+$). The accuracy of this experiment is examined successfully by analyzing several reference materials. The results for several domestic grain analysis show that the concentrations are between 12.7 ${\mu}g/kg$ and 29.6 ${\mu}g/kg$.

• The Journal of the Petrological Society of Korea
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• v.23 no.4
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• pp.337-349
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• 2014

We measured rare earth element and Zr concentrations of USGS granite standard material GSP-2 and GSJ granite standard material JG-1a to clarify the effect of zircon during rare earth element analysis using ICP-MS. We also measured rare-earth element and zirconium (Zr) contents of zircon from granite by acid-digestion methods using conventional teflon vial and pressure-bomb. The results show that acid-digestion using teflon vial dissolved ca. 50% of zircon compared to pressure-bomb method. The Zr contents of JG-1a and GSP-2 gave ca 50% of reference value. However, rare-earth element abundance of JG-1a and GSP-2 were similar to those of reference values. This suggests that the decomposition degree of zircon might give a negligible effect on a petrological and geochemical interpretation using chondritenormalized REE pattern.

• Analytical Science and Technology
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• v.16 no.5
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• pp.399-406
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• 2003

This study was conducted to find out the analysis condition of selenium(Se) in oil refinery wastewater with a high concentration of Se using the atomic absorption spectrometry with hydride generation system (HG-AAS). From various experiments that reduced Se(VI) to Se(IV), the optimum pretreatment condition was determined to be a sample volume of 10 mL, HCl 10 mL, with a 30 min heating time in a water bath. In oil refinery wastewater, as the concentration of organics and constitution became higher, the recovery rates of Se decreased. Therefore, three acid digestion methods ($HNO_3/HClO_4$ digestion, $KMnO_4$ digestion, and microwave acid digestion) were tested on the recovery rates of Se in reference to the digestion of organics, petroleum and oxidation from organic Se(org.), Se(IV) to Se(VI). The experiment results showed that the average recovery rate of Se was the highest in microwave acid digestion, although all of the digestions were more than 90%. In consequence, the pretreatment procedure of microwave digestion followed by HCl addition was the most suitable for selenium analysis in oil refinery wastewater by using HG-AAS.

• Analytical Science and Technology
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• v.15 no.1
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• pp.15-19
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• 2002

The pretreatment of tungsten added $BaTiO_x$ ceramics was performed to improve the recovery of Ba, Ti and W. $BaTiO_x$ ceramics were digested with HF : HCl ( 1 : 2 ) mixture in an acid digestion bomb at $220^{\circ}C$ for 3 hrs. The concentration of Ba, Ti and W were determined by ICP-AES. Recoveries of Ba, Ti and W were 99.6%, 99.8% and 99.2%, respectively. And their C.V. values were 1.02%, 0.73% and 1.79%. Using this method, the analytical results of Ba, Ti and W for a real sample were obainted to be 25.9% (w/w), 38.8% (w/w) and 3.31% (w/w), respectively.

• Journal of the Korean Chemical Society
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• v.44 no.6
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• pp.547-555
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• 2000

The surface water in the upstream and midstream of Nakdong river, which is being used as tap water and industrial water supply in Daegu city and Kyungpook province, was analyzed in its water quality. In addition, the sediments of which was analyzed in terms of heavy metal and organic substance contents. All the sampling was done in the drought season for 2 days of June 22-23 and carried out in 10 sampling sites. The sites cover the whole Kyungpook provincial region, starting from Yangsam Bridge in Chyeong Ryang Provincial Park as the upper end, to the Ko Ryung Bridge as the lower end sampling site of Nakdong river that flows through Kyungpook province. The 22 items including $NH^{+}_{4}$, $NO^{-}_{2}$ and COD were analyzed for surface water and 11 items including organic constituents(trichloroethylene, etc) and heavy metals were analyzed for sediments. The sediments samples were analyzed by elution testing method and acid dissolution method and then the results were compared with each other. All heavy metals in samples were determined by Inductively Coupled Plasma-Atomic Emission Spectroscopy(ICP-AES) and other constituents were analyzed by standard testing methods of the Korean Ministry of Environment.

• Analytical Science and Technology
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• v.10 no.1
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• pp.35-42
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• 1997

The sample pretreatment technique using a high pressure acid digestion bomb for the analysis of ceramic capacitor materials, such as barium titanate and PZT, was studied. When the concentrations of hydrochloric acid were varied with the addition of nitric acid or distilled water, quantitative measurements for those samples were carried out using inductively coupled plasma atomic emission spectrometry. From this experiment the results indicate that most of elements, such as Ba, Mn, Zn, Si, etc., aren't affected by the concentration of hydrochloric acid but Nb and Zr are very susceptable to it. It however turns out that the digestion time relatively gave little effects on the analytical result. In case of Nb the ratio of hydrochloric acid to water should be greater than 3:1(v / v) for the best analytical result. For the Pb determination use of diluted hydrochloric acid compared to the mixture of nitric acid and hydrochloric acid showed a better analytical result.

• The Journal of the Petrological Society of Korea
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• v.3 no.1
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• pp.41-48
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• 1994

Three USGS rock standards (G-2, W-2, and BHVO-1) are decomposed by three different methods, such as open beaker, microwave oven, and alkali fusion method, to compare the effect of decomposition methods for trace elememt analysis in the rock samples. Solubilized trace elements are measured with inductively coupled plasma mass spectrometer (ICP-MS). Generally the analytical results of trace elements between open beaker and microwave digestion method are not different. In case of alkali fusion method, some volatile elements such as Pb, Cu, and Rb are considerably lost. Using acid digestion method, Zr and Hf concentrations are lowered in case that these elements are concentrated in refractory minerals. The concentrations of rare earth elements are generally consistent with the recommended values, but due to large dilution factor, there are some analytical problems in alkali fusion method.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.109-115
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• 1999

Lead and cadmium were analyzed with different pretreatemnt methods. Paddy soil and wastewater sludge samples were used and the result was compared each other. Pretreatment method affected the concentration obtained from samples significantly. Large difference was illustrated between the results. The concentration by 0.1N HCl extraction method, an official analytical method for soil and solid wastes, was far lower than those by the EPA3050B and mixed-acid digestion methods. The reason might be that metals associated with organics and silicates are not easily extracted by 0.1N HCl, while digestion methods using strong acids and high temperature dissolved all the elements in the samples. It implies that pretreatment method should be specified in addition to concentration on the report of metal analysis for environmental samples. Acid digestion methods are not necessarily good because the concentration obtained does not represent the natural condition which is our concern in many cases. The 0.1N HCl extraction method does not fully represent the natural condition either. The metals associated with organics will be extracted eventually as organics decompose with time. Therefore, proper pretreatment and analytical methods should be developed for specific purpose, and their standardization is recommended.