• Journal of the Korean Chemical Society
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• v.48 no.2
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• pp.203-206
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• 2004

• Analytical Science and Technology
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• v.14 no.4
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• pp.324-330
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• 2001

For the analysis of S, P and Zn in lubricating oil, microwave digestion method was studied by using inductively coupled plasma-atomic emission spectrometry(ICP-AES). Lubricating oil was completely decomposed with nitric acid or a mixture of nitric acid and hydrogen peroxide using and closed microwave digestion system. Digestions are completed within 50 min, a factor of at least 3~4 times faster than for the conventional digestion. A gradual heating program operated by the pulsed mode was found suitable for decomposing the lubricating oil matrix safely. The proposed method of digestion gave relative standard deviations(RSD) less than 3% for the elements determined.

• Analytical Science and Technology
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• v.14 no.1
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• pp.21-27
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• 2001

In this work, analytical performance of a laboratory built double membrane desolvator (DMD) was studies using perfluoroalkoxy (PFA) nebulizer and microconcentirc nebulizer (MCN) in inductively coupled plasma atomic emission spectrometry. Compared with MCN, PFA nebulizer coupled to DMD showed similar analytical sensitivity for aqueous solution and better sensitivity for isopropyl alcohol. Since PFA resisted various acids, HCI, $H_2SO_4$ and HF solution were analyzed with less than 2% RSD. Rinse-out time for the signal reduction to 1% was obtained to be 35 s for PFA but about 45 s for MCN.

• Analytical Science and Technology
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• v.13 no.6
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• pp.781-788
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• 2000

Tellurium in simulated nuclear spent fuels (SIMFUEL) has been determined by hydride generation-inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Parameters such as concentrations of HCl and $NaBH_4$, flow rate of HCl and $NaBH_4$ were optimized and then the effects of U, Mo, Pd, Rh and Ru on the Te intensity were investigated. A thiourea as a masking agent was used to eliminate or minimize such interferences specially caused by palladium. Tellurium was measured by HG-ICP-AES and ICP-MS after separation of tellurium from SIMFUEL with cation exchange chromatography. The relative deviation between direct measurement and separation method was less than 6% based on the data by ICP-MS.

• Journal of the Korean Chemical Society
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• v.41 no.8
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• pp.399-405
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• 1997

We examined the determination of trace amount of germanium in rocks and sediments by hydride vapor generation-ICP-AES. Germanium is formed volatile compounds with various types of acid reagents, but volatilizing of germanium was decreased in the presence of $H_3PO_4$. Sediments and rocks can be dissolved by mixed acids of $HF-HNO_3-H_3PO_4$ without volatilizing loss of germanium in open digestion system and it was possible to determine germanium by hydride generation-ICP-AES without further sample treatment. Detection limit of Ge is reached to 0.08 ppb under the condition of 5M $H_3PO_4$ and 1% $NaBH_4$ as a supporting acid and a reducing reagent, respectively. The measured values by hydride generation-ICP-AES agreed well with the reference values of SRMs as well as the values determined by solution nebulization-ICP-MS.

• Analytical Science and Technology
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• v.13 no.2
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• pp.189-193
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• 2000

Arsenic (III) and arsenic (V) in disused mine tailing samples have been determined simutaneuously by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Total arsenic was determined using 2% $NaBH_4$ and 6 M HCl after prereduction of As(V) to As(III) with) 1M KI. Arsenic (III) was determined selectively using citrate/citric acid buffer with range of pH 5-6, it was determined by HG-ICP-AES. Arsenic (V) can be evaluated by the differences. According to the results, arsenic (V) was over 90% among the total arsenic extracted from disused mine tailing samples.

• Analytical Science and Technology
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• v.20 no.2
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• pp.131-137
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• 2007

The urania-gadolinia fuels were dissolved with nitric acid. The analytical conditions of ICP-AES for the direct determinations of gadolinium in the uranium matrices without separation process were investigated. Based on the effect of uranium on gadolinium intensity, the best wavelength for gadolinium was 336.223 nm. The relative deviation of two methods, direct and indirect measurements with anion exchange chromatography, was less than 5 %. Therefore it was possible for this procedure directly to measure 5~10 wt.% of gadolinium in urania-gadolinia fuels without separation by ICP-AES.

• Journal of the Korean Chemical Society
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• v.43 no.2
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• pp.182-192
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• 1999

The new GD/ICP-AES quick change over system has been developed and characterized. Within less than 15 minutes, ICP-AES could be switched to GD-AES and vise a versa. As a result, both solid and liquid samples could be analyzed in a very short period of time by the ICP/GD-AES quick change over system developed in our laboratory. The influences of the experimental variables, such as flow rate of coolant gas, flow rate of auxiliary gas, flow rate of sample carrier gas, sampling depth, orifice size of sampling cone, and rf (radio frequency) power on emission intensity have been presented. The detection limits of Cd(I) 228.8 nm, Mn (II) 257.61 nm, and Fe(II) 259.95 nm were found to be 3.86, 1.49, and 5.79 ppb, respectively. And linealities of the calibration curves were measured to be unity.

• Analytical Science and Technology
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• v.6 no.1
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• pp.131-139
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• 1993

The separation of gallium and indium from the matrix elements such as zinc and other ions, especially form Fe(III) ion was studied for the determination of trace level of them in zinc ores and zinc blendes by inductively coupled plasma atomic emission spectrometry(ICP-AES). Gallium and indium were extracted from the sample solution with a solvent of tributyl phosphate(TBP). The type and concentration of acid, interferences of other ions, the ratio of aqueous phase to organic phase, TBP concentration, sripping efficiency were optimized for the effective extraction. Gallium and indium were separated from other ions in the 5N hydrochloric acid solution of the samples by the extraction with 100% TBP. In this time, Fe(III) was reduced to Fe(II) with hydroxylamine hydrochloride to prevent its coextraction prior to the main extraxtion. After stripped from organic phase by the back-extraction with 0.02N HCl, they were determined in the aqueous phase by ICP-AES. This method was known to be quantitative from the overall extraction of more than 95%.

• Analytical Science and Technology
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• v.13 no.4
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• pp.446-452
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• 2000

The simulated nuclear spent fuel (SIMFUEL) containing the platinum group elements which will not be dissolved in a nitric acid was completely dissolved with a acid digestion bomb. The metallic elements separated in the SIMFUEL were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). Because the peaks of metallic elements were spectrally interfered by uranium spectrum, uranium and metallic elements were separated by cation exchange resin for Mo, Pd, Rh and Ru and by anion exchange resin for Ba, Ce, La, Nd, Rh, Sr, Y and Zr, respectively. The recovery of Mo, Pd, Rh and Ru after separation by cation exchange chromatography found to be 99-103% and anion exchange separation showed 96.5-107% of recovery except Y with the simulated solution whose concentration was similar to the spent nuclear fuel. The relative standard deviation of this method showed 1.3-6.7% in the SIMFUEL whose concentrations of metallic elements were between several $10^2-10^3$ppm.