• Title/Summary/Keyword: Inductively coupled plasma spectrometry

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Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.233-236
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    • 2004
  • Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.

Extraction Chromatographic Separation of Technetium-99 from Spent Nuclear Fuels for Its Determination by Inductively Coupled Plasma-Mass Spectrometry (유도결합플라스마 질량분석을 위한 사용후핵연료 중 테크네튬-99의 추출크로마토그래피 분리)

  • Suh, Moo-Yul;Lee, Chang-Heon;Han, Sun-Ho;Park, Yeong-Jae;Jee, Kwang-Yong;Kim, Won-Ho
    • Analytical Science and Technology
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    • v.17 no.5
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    • pp.438-442
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    • 2004
  • To determine the contents of $^{99}Tc$ in the spent PWR (pressurized water reactor) nuclear fuels by ICP-MS (inductively coupled plasma-mass spectrometry), a technetium separation method using an extraction chromatographic resin (TEVA Spec resin) has been established. $^{99}Tc$ was separated from a spent PWR nuclear fuel solution by this separation procedure and its concentration was determined by ICP-MS. The result agrees well with the value calculated by the program ORIGEN 2 and also the value measured by AG MP-1 resin/ICP-MS method described in our previous paper. It can be concluded that the present separation procedure is superior to the AG MP-1 resin procedure with respect to the time required for technetium separation as well as the efficiency of decontamination from other radioactive nuclides.

Nanometrology and its perspectives in environmental research

  • Kim, Hyun-A;Seo, Jung-Kwan;Kim, Taksoo;Lee, Byung-Tae
    • Environmental Analysis Health and Toxicology
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    • v.29
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    • pp.16.1-16.9
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    • 2014
  • Objectives Rapid increase in engineered nanoparticles (ENPs) in many goods has raised significant concern about their environmental safety. Proper methodologies are therefore needed to conduct toxicity and exposure assessment of nanoparticles in the environment. This study reviews several analytical techniques for nanoparticles and summarizes their principles, advantages and disadvantages, reviews the state of the art, and offers the perspectives of nanometrology in relation to ENP studies. Methods Nanometrology is divided into five techniques with regard to the instrumental principle: microscopy, light scattering, spectroscopy, separation, and single particle inductively coupled plasma-mass spectrometry. Results Each analytical method has its own drawbacks, such as detection limit, ability to quantify or qualify ENPs, and matrix effects. More than two different analytical methods should be used to better characterize ENPs. Conclusions In characterizing ENPs, the researchers should understand the nanometrology and its demerits, as well as its merits, to properly interpret their experimental results. Challenges lie in the nanometrology and pretreatment of ENPs from various matrices; in the extraction without dissolution or aggregation, and concentration of ENPs to satisfy the instrumental detection limit.

Concentration of Fe, Cu, Zn in 24-hour Food Duplicate Samples: Quantitative Analysis by Inductively Coupled Plasma - Atomic Emission Spectrometry (24시간 복제 음식물 중의 Fe, Cu, Zn 함량: 유도결합플라즈마-원자발광분광법에 의한 정량분석)

  • Paik, Jong-Min;Moon, Chan-Seok
    • Journal of Environmental Health Sciences
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    • v.33 no.5
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    • pp.397-402
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    • 2007
  • The present study was initiated to examine the measures of dietary intake of Fe, Cu and Zn. The food duplicate samples were collected in Busan and its neighboring area, from the 69 middle-aged women (healthy non-smoking, mostly house wives), who provided informed consent. The samples were wet ashed by being heated in the presence of mineral acids, and Fe, Cu, Zn in the wet-ashed samples were analyzed by inductively coupled plasma - atomic emission spectrometry(ICP-AES). Dietary intake of Fe, Cu and Zn were 10.4 mg/day in Fe, 1.2 mg/day in Cu, 7.4 mg/day as arithmetic mean. The values for dietary Fe and Zn were lower, and the values for dietary Cu were higher than the recommended daily intake from Korean Nutrition Society. Further studies of Korean foods are needed to clarify the representative values for daily dietary Fe, Cu and Zn intake in the Korean population.

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.

Determination of Li by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J.;Chung, Bag S.
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.427-434
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    • 1995
  • Inductively coupled plasma mass spectrometry combined with the isotope dilution method is used for the determination of lithium. The isotope dilution method is based on the addition of a known amount of enriched isotope (spike) to a sample. The analyte concentration is obtained by measuring the altered isotope ratio. The spike solution is calibrated through so called reverse isotope dilution with a primary standard. The spike calibration is an important step to minimize error in the determined concentration. It has been found essential to add spike to a sample and the primary standard so that the two isotope ratios should be as dose as possible. Since lithium is neither corrosive nor toxic, lithium is used as a chemical tracer in the nuclear power plants to measure feedwater flow rate. 99.9% $^7Li$ was injected into a feedwater line of an experimental system and sample were taken downstream to be spiked with 95% $^6Li$ for the isotope dilution measurements. Effects of uncertainties in the spike enrichment and isotope ratio measurement error at various spike-to-sample ratios are presented together with the flow rate measurement results in comparison with a vortex flow meter.

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Determination of Trace Elements of Ge and P in a Gold Bonding Wire by Inductively Coupled Plasma Atomic Emission Spectrometry

  • Choi, Sung-Min;Lee, Gae-Ho;Han, Jae-Kil
    • Bulletin of the Korean Chemical Society
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    • v.29 no.2
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    • pp.393-397
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    • 2008
  • Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to determine the presence of germanium and phosphorus in a pure gold bonding wire. The samples were dissolved with hydrobromic acid and nitric acid at room temperature. The quantitation limits were 0.012 mg L-1 at 265.118 nm for Ge and 0.009 mg L-1 at 177.495 nm for P. Using the mixed acid digestion formula of DIW+HBr+HNO3, the recoveries were in the range of 98-100% and the relative standard deviation was within 1.1-2.3%. On the other hand, the amount of Ge decreased by about 16.2% using DIW+HCl+HNO3, due to the formation of a volatile compound. The Ge contents determined using the external method and the standard addition method were 9.45 mg kg-1 and 9.24 mg kg-1, respectively, and the P contents, using the same methods, were 22.49 mg kg-1 and 23.09 mg kg-1, respectively. Both methods were successfully used to determine the trace amounts of P and Ge in the pure gold bonding wire samples.

Determination of Total Arsenic in Drinking Water by Inductively Coupled Plasma-Mass Spectrometry (유도결합 플라스마 질량 분석법(ICP-MS)을 이용한 음용수 중의 전체 비소의 정량)

  • Lim, Yoo-Ree;Park, Kyung-Su;Yoon, Yang-Hee;Kim, Sun-Tae;Chung, Jin-Ho
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.423-427
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    • 2000
  • Total arsenic in drinking water such as spring, small water-supply system and mineral water was determined by inductively coupled plasma mass spectrometry. The contents of total arsenic were analyzed after acidification by nitric acid to become 1% in water samples. According to the results, total concentration of arsenic in drinking water was below 30ppb.

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Determination of osmium using sulfurous acid as reductant by ICP-AES (Sulfurous acid 환원제를 이용한 ICP-AES에 의한 Osmium의 정량 분석)

  • Park, Han-Seok;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.251-254
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    • 2007
  • In this study, a convenient, fast and accurate inductively coupled plasma atomic emission spectrometry (ICP-AES) method has been optimized for the determination of osmium in aqueous solutions. The method makes use of the reaction of sulfurous acid with osmium to quantitative conversion of volatile Os(VIII) to non-volatile Os(IV) in the pH range 2-10. The response was found to be stabilized immediately after sulfurous acid reacted with osmium. The precision was calculated to be 0.5-4.5 % (RSD) under various ICP-AES conditions. The detection limit was 2.5-57.7 ng/g based on $3{\sigma}$ of the blank response (n=3) using a concentric flow nebulization.

Preconcentration of Cd by Continuous Hydroxide Precipitation-Dissolution in Atomic Emission Spectrometry

  • 연평흠;허걸;박용남
    • Bulletin of the Korean Chemical Society
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    • v.19 no.7
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    • pp.766-770
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    • 1998
  • On-line preconcentration by direct precipitation with hydroxide has been developed and applied for the analysis of Cd in Inductively Coupled Plasma Atomic Emission Spectrometry. Cadmium is continuously precipitated with hydroxide and dissolved by nitric acid in on-line mode. Currently, the enrichment factor is more than 90 times for 20.0 mL of sample and could be further increased very easily. For a large sample throughput, 1.0 mL of sample loop is used and the enrichment factor is 4.5 with the sampling speed of 15/hr. The method has been applied to the analysis of NIST reference sample and has yielded good results with the certified value.