• Title/Summary/Keyword: Atomic emission spectrometry

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Analytical method of trace elements in ceramic capacitor materials (세라믹 축전물질들의 미량성분 분석방법)

  • Choi, J.K.;Kim, T.H.;Lim, H.B.
    • 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.

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Metallurgical Study of Bronze Relics Excavated from Sanoesa Temple, Chongju (청주(淸州) 사뇌사지(思惱寺址) 출토 청동유물의 금속학적 조사)

  • Kwon, H.N.;Yu, H.S.;Ahn, B.C.
    • Journal of Conservation Science
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    • v.9 no.1
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    • pp.1-10
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    • 2000
  • In 1993, many bronze artifacts were excavated from the Sanoesa Temple(思惱寺), Chongju, Chungbuk. Twelve items were selected and chemically analyzed with AA Spectrometry and ICP-Atomic Emission Spectrometry. They were also observed under the optical microscopy and SEM. According to the results from chemical analysis, production method and use, these artifacts were classified into four groups: casting, wrought and welding products, and bells. Cast products, probably used for ritual, were alloy of 70% Cu, 10% Sn and 20% Pb. They showed ${\alpha}+{\beta}$ phase as a typical microstructure of casting. The ${\delta}$ phase was rarely observed due to the small amount of Sn. These artifacts included more lead than other alloys. They showed segregation like island-shape on the lead part. Wrought products used for daily too1s. were alloy of 80% Cu and 20% Sn. Since they were consist of ${\alpha}$ phase and martensite ${\beta}$ phase, it could be presumed that they were heat-treated. The production method could be identified from twinned grains in ${\alpha}$ phase. Lead was not included in because it had a bad effect to alloy. The bells were alloyed with 85% Cu, 10% Sn, 5% Pb or 90% Cu and 10% Sn. They show the dendrite structure because they were cast and alloyed with many tin. Weldinged were alloyed with 83% Cu, 12% Sn and 5% Pb. lt showed the fine dendrite structure because of fast cooling in air.

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A Novel Volumetric Method for Quantitation of Titanium Dioxide in Cosmetics (용량분석법을 이용한 화장품 중 티타늄옥사이드의 정량)

  • Kim, Young-So;Kim, Boo-Min;Park, Sang-Chul;Jeong, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.31 no.4 s.54
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    • pp.289-293
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    • 2005
  • Nowadays there are many sun protection cosmetics including organic or inorganic UV filter as an active ingredient. Chemically stable inorganic sunsEreen agents, usually metal oxides, we widely employed in high SPF products. Titanium dioxide is one of the most frequently used inorganic UV filters. It has been used as pigments for a long period of cosmetic history. With the development of micronization techniques, it becomes possible to incorporate titanium dioxide in sunscreen formulations without whitening effect and it becomes an important research topic. However, there are very few works related to quantitations of titanium dioxide in sunscreen products. In this research, we analyzed amounts of titanium dioxide in sunscreen cosmetics by adapting redof titration, reduction of Ti(IV) to Ti(III) and reoxidation to Ti(IV). After calcification of other organic ingredients of cosmetics, titanium dioxide is dissolved by hot sulfuric acid. The dissolved Ti(IV) is reduced to the Ti(III) by adding aluminum metals. The reduced Ti(III) is titrated against a standard oxidizing agent, Fe(III) (ammonium iron(III) sulfate), with potassium thiocyanate as an indicator In order to test accuracy and applicability of the proposed method, we analyzed the amounts of titanium dioxide in four types of sunscreen cosmetics, such as cream, make-up base, foundation and powder, after adding known amounts of titanium dioxide $(1{\sim}25w/w%)$. The percent recoveries of the titanium dioxide in four types of formulations were in the range between 96 and 105%. We also analyzed 7 commercial cosmetic products labeled titanium dioxide as an ingredient and compared the results with those of obtained from ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry), one of the most powerful atomic analysis techniques. The results showed that the titrated amounts were well coincided with the analyzed amounts of titanium dioxide by ICP-AES. Although instrumental analytical methods, ICP-MS (Inductively Coupled Plasma-Mass Spectrometry) and ICP-AES, are the best for the analysis of titanium, it is hard to adopt because of their high prices for small cosmetic companies. It was found that the volumetric method presented here gat e quantitative and reliable results with routine lab-wares and chemicals.

Study for Conductive and Non-conductive Multi-layers Depth Profiling Analysis of Radio Frequency Gas-jet Boosted Glow Discharge Spectrometry (Modified Gas-jet Boosted Radio-frequency Glow Discharge 셀의 개발 및 최적화에 관한 연구)

  • Cho, Won Bo;Borden, Stuart;Jeong, Jong Pil;Kang, Won Kyu;Kim, Kyu Whan;Kim, Hyo Jin
    • Analytical Science and Technology
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    • v.15 no.2
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    • pp.108-114
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    • 2002
  • The new system using a glow discharge atomic emission spectrometer for the direct analysis of solid samples has been developed and characterized. The system was consisted of new glow discharge cell improved previous gas-jet boosted nozzle and radio-frequency power supply. In the case of previous type glow discharge chamber, it had been fitted trace analysis of low alloy steel with low discharge power, because it was to decrease redeposition and increase sample weight loss. But it had a problem that plasma becomes unstale due to increased sample weight loss and redeposition resulting from the high discharge power. Because of being problem of previous glow discharge, it is impossible to analyze using high power. The modified gas-jet boosted glow discharge to solve this problem would improve to be less sample loss rate of modified nozzle than sample loss rate of previous nozzle on the equal discharge condition, and improve to increase stability of plasma. The effect of discharge parameters such as discharge pressure, gas flow rate and power on the sample loss rate, emission intensity has been studied to find optimum discharge conditions. The calibration curves of Fe were obtained with 3 low-alloy samples.

Quantifying Uncertainty of Calcium Determination in Infant Formula by AAS and ICP-AES (AAS 및 ICP-AES에 의한 조제분유 중 칼슘 함량 분석의 측정불확도 산정)

  • Jun, Jang-Young;Kwak, Byung-Man;Ahn, Jang-Hyuk;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.36 no.5
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    • pp.701-710
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    • 2004
  • Uncertainty was quantified to evaluate calcium determination result in infant formula with AAS (Atomic Absorption Spectrometry) and ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). Uncertainty sources in measurand, such as sample weight, final volume of sample, sample dilution and the instrumental result were identified and used as parameters for combined standard uncertainty based on the GUM (Guide to the expression of uncertainty in measurement) and Draft EURACHEM/CITAC Guide. Uncertainty components of each sources in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, standard material molecular weight, standard solution concentration, standard solution dilution factor, sample dilution factor, calibration curve, recovery, instrumental precision, reproducibility, and stability, Each uncertainty components were evaluated by uncertainty types and included to calculate combined uncertainty. The kinds of uncertainty sources and components in the analytical method by AAS and ICP-AES were same except sample dilution factor for AAS. The analytical results and combined standard uncertainties of calcium content were estimated within the certification range $(367{\pm}20\;mg/100g)$ of CRM (Certified Reference Material) and were not significantly different between method by AAS followed by ashing and method by ICP-AES followed by acid digestion as $359.52{\pm}23.61\;mg/100g\;and\;354.75{\pm}16.16\;mg/100g$, respectively. Identifying uncertainty sources related with precision, repeatability, stability, and maintaining proper instrumental conditions as well as personal proficiency was needed to reduce analytical error.

A Study on the Heavy Metal Contamination of paddy Soil in the Vicinity of the Seosung Pb-Zn Mine (서성 연-아연광산 주변 농경지 토양의 중금속 오염 연구)

  • 황은하;위수민;이평구;최상훈
    • Journal of Korea Soil Environment Society
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    • v.5 no.2
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    • pp.67-85
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    • 2000
  • Fifty seven soil samples were collected from the paddy soil filled with tailings in the vicinity of the Seosung Pb-Zn mine. Those samples were analyzed for As, Cd, Co, Cr, Cu, Pb, and Zn in order to investigate heavy metal pollution levels in the paddy soil. Analyses of the soil samples were carried out using Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES) . Paddy soils show pH range from 6.55 to 8.26. X-ray diffraction analyses of the paddy soil indicate that the soils consist predominantly ankerite, siderite, quartz, mica, and clay minerals with minor amounts of amphibole and chlorite. The mineral composition of the waste rocks consists of massive galena, sphalerite, and minor amounts of pyrite, arsenopyrite, chalcopyrite, calcite, siderite, Pb-sulfosalt, and marcasite. The paddy soils were significantly contaminated by heavy metals(average concentrations, As: 334.4 ppm, Cd: 37.6 ppm, Co: 15.7 ppm, Cu: 214.1 ppm, Pb: 4,612 ppm, and Zn: 4,468 ppm).

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Metal Concentrations Analysed in the Inorganic Bulk Pigment Samples by ICP-AES and the Provision Rate of MSDS and Agreement Rate with MSDS (우리 나라에서 제조/사용하는 일부 무기 안료중 ICP-AES를 이용한 주요 중금속 농도와 MSDS 비치율 및 일치율 비교)

  • Kim, Hyoung-Ah;Lee, Kyoung-Joo;Kim, Yong-Woo;Kim, Hyun Wook
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.8 no.2
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    • pp.196-208
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    • 1998
  • To improve the quality of environmental measurements and evaluation of the workplace air in the pigment manufacturing industries, we analyzed metal(chromium, cadmium, lead, iron, cobalt, manganese, antimony, titanium, arsenic, and selenium) concentrations by ICP-AES in sixty seven samples of inorganic bulk pigments which are produced and/or used in Korea. We also collected MSDS which has to be supplied by manufacturer and/or supplier and posted in the workplace according to the Hazard Communication Standards, and compared the number of metals listed in each MSDS with the number of metals determined by ICP-AES. Results were as followed; 1. Among seventeen yellowish-colored samples, chromium(2~19%) and lead(0.1~61%) were the two major metals. In thirteen reddish-colored samples, iron was the major component with 37~81%. Cobalt and manganese were detected in blue-colored samples with less than 1%, while antimony and titanium were the major two metals in white-colored pigments with 178~300 ppm and with 36~65%, respectively. 2. In area samples collected in workplace air(one pigments producing factory and five retailer stores), iron and manganese were detected but the concentrations not exceeded the TLVs(1 and $5mg/m^3$, respectively). In three of fifteen samples, the concentrations of lead exceeded the TLV ($0.05mg/m^3$). 3. Two out of seven companies provided MSDS, and the average provision rate was 22.4%. And the coincidence rate of the number of metals referenced in MSDS and determined by ICP-AES mostly accorded, but in one sample, different metal was detected from MSDS. In summary, metals have to be concerned in evaluation of the workplace air dealing with compounds of inorganic pigments dust are cobalt, chromium, iron, manganese, lead and antimony, and these are simultaneously determined by ICP-AES. Taking this opportunity, it is needed to reinforce that the personnel is to be concerned about prevention of workers' ill health regarding to provision of MSDS.

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Identification and Characterization of Protein Encoded by orf382 as $\small{L}$-Threonine Dehydrogenase

  • Ma, Fei;Wang, Tianwen;Ma, Xingyuan;Wang, Ping
    • Journal of Microbiology and Biotechnology
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    • v.24 no.6
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    • pp.748-755
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    • 2014
  • In the genome annotation of Escherichia coli MG1655, the orf382 (1,149 bp) is designated as a gene encoding an alcohol dehydrogenase that may be Fe-dependent. In this study, the gene was amplified from the genome by PCR and overexpressed in Escherichia coli BL21(DE3). The recombinant $6{\times}$His-tag protein was then purified and characterized. In an enzymatic assay using different hydroxyl-containing substrates (n-butanol, $\small{L}$-threonine, ethanol, isopropanol, glucose, glycerol, $\small{L}$-serine, lactic acid, citric acid, methanol, or $\small{D}$-threonine), the enzyme showed the highest activity on $\small{L}$-threonine. Characterization of the mutant constructed using gene knockout of the orf382 also implied the function of the enzyme in the metabolism of $\small{L}$-threonine into glycine. Considering the presence of tested substrates in living E. coli cel ls and previous literature, we believed that the suitable nomenclature for the enzyme should be an $\small{L}$-threonine dehydrogenase (LTDH). When using $\small{L}$-threonine as the substrate, the enzyme exhibited the best catalytic performance at $39^{\circ}C$ and pH 9.8 with $NAD^+$ as the cofactor. The determination of the Km values towards $\small{L}$-threonine (Km = $11.29{\mu}M$), ethanol ($222.5{\mu}M$), and n-butanol ($8.02{\mu}M$) also confirmed the enzyme as an LTDH. Furthermore, the LTDH was shown to be an ion-containing protein based on inductively coupled plasma-atomic emission spectrometry with an isoelectronic point of pH 5.4. Moreover, a circular dichroism analysis revealed that the metal ion was structurally and enzymatically essential, as its deprivation remarkably changed the ${\alpha}$-helix percentage (from 12.6% to 6.3%).

Determination of Heavy Metal Contents in Medicinal Herb (유통 한약재의 중금속 함량 조사)

  • Lee, Mi-Kyung;Park, Jung-Suk;Lim, Hyun-Cheol;Na, Hwan-Sik
    • Food Science and Preservation
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    • v.15 no.2
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    • pp.253-260
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    • 2008
  • Comparative study was performed on heavy metal contents among domestic herbal medicines and imported one. The heavy metal contents in 89 samples of 65 types of herbal medicines were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES) and mercury analyzer. The mean values of heavy metal contents (mg/kg) for herbal medicines were as follows: Hg, 0.010 (domestic: 0.010, imported: 0.010); Pb, 0.380 (domestic: 0.311, imported: 0.449); Cd, 0.080 (domestic: 0.101, imported: 0.059); As, 2.085 (domestic: 1.845, imported: 2.324); Mn, 31.564 (domestic: 33.844, imported: 29.283); Zn, 15.436 (domestic: 18.703, imported: 12.168); Cu, 3.406 (domestic: 3.374, imported: 3.437); Fe, 134.944 (domestic: 108.327, imported: 161.561). The measured values of Hg, Pb and Cd of domestic and imported herbal medicines showed lower levels than the recommended levels of those in herbal medicines by WHO/PHARM (Pb : not more than 5 mg/kg, Cd : not more than 0.3 mg/kg). This results will he used as a basic data for the future legislation on the regulation and control of heavy metal contents of herbal medicines.

Application of Microwave Digestion Pretreatment Techniques for ICP-AES Analysis of Used Monolithic Automobile Catalysts Having Platinum Group-Metals and Silicates (백금족 금속과 규산염을 포함하는 모노리스형 자동차 폐촉매의 ICP-AES 분석을 위한 극초단파 분해 전처리 기법의 응용)

  • Kim, Choong-Hyon;Woo, Seong Ihl;Jeon, Sung Hwan
    • Applied Chemistry for Engineering
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    • v.10 no.4
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    • pp.568-575
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    • 1999
  • Two different digestion procedures for the simultaneous determination of major and platinum-group element(PGE) in spent automobile catalysts containing PGE and silicates by inductively coupled plasma atomic emission spectrometry(ICP-AES) are compared. Combinations of mixed aids using HF, $HNO_3$, HCl, $HClO_4$, $H_2O_2$, and $H_3BO_3$ are utilized for the hot plate dissolution method and the closed-vessel microwave digestion method, The latter method has been shown to be relatively superior in terms of recovery, analysis time, and amount of aqua regia (3 parts HCl + part $HNO_3$ required to dissolve PGE in comparison with conventional open vessel hot-plate dissolution. The best results were drawn from the following conditions: In closed Teflon PFA vessels under microwave heating with temperature/pressure regulation, a 0.25 g portion of sample was digested in 2 mL of HF, 2 mL of $HNO_3$ and 6mL of HCl under the pressure of 200 psi(13.79 bar) at $180^{\circ}C$ for 1hr, followed by a second digestion stage with 16 mL of 5%(w/v) boric acid under the pressure of 20 psi(1.38 bar) at $100^{\circ}C$ for 10 min. After the microwave heating, the sample was post-treated with 10 mL of aqua regia twice by hot-plate heating. This condition gives the PGE recovery within 85~110% and the relative standard deviations within 2%. The method developed can therefore be regarded as an alternative method for routine analysis of spent automobile catalysts.

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