• Title/Summary/Keyword: X-ray fluorescence analysis

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Study on the screening method for determination of heavy metals in cellular phone for the restrictions on the use of certain hazardous substances (RoHS) (유해물질 규제법(RoHS)에 따른 휴대폰 내의 중금속 함유량 측정을 위한 스크리닝법 연구)

  • Kim, Y.H.;Lee, J.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.1-14
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    • 2010
  • It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.

Purification, and Biochemical and Biophysical Characterization of Cellobiohydrolase I from Trichoderma harzianum IOC 3844

  • Colussi, Francieli;Serpa, Viviane;Da Silva Delabona, Priscila;Manzine, Livia Regina;Voltatodio, Maria Luiza;Alves, Renata;Mello, Bruno Luan;Nei, Pereira Jr.;Farinas, Cristiane Sanches;Golubev, Alexander M.;Santos, Maria Auxiliadora Morim;Polikarpov, Igor
    • Journal of Microbiology and Biotechnology
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    • v.21 no.8
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    • pp.808-817
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    • 2011
  • Because of its elevated cellulolytic activity, the filamentous fungus Trichoderma harzianum has a considerable potential in biomass hydrolysis applications. Trichoderma harzianum cellobiohydrolase I (ThCBHI), an exoglucanase, is an important enzyme in the process of cellulose degradation. Here, we report an easy single-step ion-exchange chromatographic method for purification of ThCBHI and its initial biophysical and biochemical characterization. The ThCBHI produced by induction with microcrystalline cellulose under submerged fermentation was purified on DEAE-Sephadex A-50 media and its identity was confirmed by mass spectrometry. The ThCBHI biochemical characterization showed that the protein has a molecular mass of 66 kDa and pI of 5.23. As confirmed by smallangle X-ray scattering (SAXS), both full-length ThCBHI and its catalytic core domain (CCD) obtained by digestion with papain are monomeric in solution. Secondary structure analysis of ThCBHI by circular dichroism revealed ${\alpha}$- helices and ${\beta}$-strands contents in the 28% and 38% range, respectively. The intrinsic fluorescence emission maximum of 337 nm was accounted for as different degrees of exposure of ThCBHI tryptophan residues to water. Moreover, ThCBHI displayed maximum activity at pH 5.0 and temperature of $50^{\circ}C$ with specific activities against Avicel and p-nitrophenyl-${\beta}$-D-cellobioside of 1.25 U/mg and 1.53 U/mg, respectively.

A Study on the Luminescence Properties of LiGd9(SiO4)6O2:Ce3+ (LiGd9(SiO4)6O2:Ce3+ 형광 특성 연구)

  • Jin, Seongjin
    • Journal of the Korean Society of Radiology
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    • v.9 no.3
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    • pp.169-174
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    • 2015
  • $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ phosphors were synthesized by solid-state reaction method. The structural characteristic was investigated by X-ray powder diffraction analysis. The emission and excitation spectra of the $Ce^{3+}$ ions doped $LiGd_9(SiO_4)_6O_2$ phosphors were obtained under the UV excitation. The emission spectra of $LiGd_9(SiO_4)_6O_2:Ce^{3+}$ shows the band at 410 nm corresponding to the $^2F_{5/2}$ and $^2F_{7/2}$ states of $Ce^{3+}$. The red shift of $Ce^{3+}$ emission is found as the $Ce^{3+}$ concentration increases, which could be explained by the change in crystal-field symmetry and strength with increasing $Ce^{3+}$ concentration. Fluorescence decay time of $Ce^{3+}$ was about 20 ns. When the concentration of $Ce^{3+}$ increases life time was slightly reduced.

Size-resolved Source Apportionment of Ambient Particles by Positive Matrix Factorization at Gosan, Jeju Island during ACE-Asia (PMF 분석을 이용한 ACE-Asia 측정기간 중 제주 고산지역 입자상 물질의 입경별 발생원 추정)

  • Moon K.J.;Han, J.S.;Kong, B.J.;Jung, I.R.;Cliff Steven S.;Cahill Thomas A.;Perry Kelvin D.
    • Journal of Korean Society for Atmospheric Environment
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    • v.22 no.5
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    • pp.590-603
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    • 2006
  • Size-and time-resolved aerosol samples were collected using an eight-stage Davis rotating unit for monitoring (DRUM) sampler from 23 March to 29 April 2001 at Gosan, Jeju Island, Korea, which is one of the super sites of Asia-Pacific Regional Aerosol Characterization Experiment(ACE-Asia). These samples were analyzed using synchrotron X-ray fluorescence for 3-hr average concentrations of 19 elements including Al, Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Br, Rb, and Pb. The size-resolved data sets were then analyzed using the positive matrix factorization(PMF) technique to identify possible sources and estimate their contributions to particulate matter mass. PMF analysis uses the uncertainty of the measured data to provide an optimal weighting. Twelve sources were resolved in eight size ranges($0.09{\sim}12{\mu}m$) and included continental soil, local soil, sea salt, biomass/biofuel burning, coal combustion, oil combustion, municipal incineration, nonferrous metal source, ferrous metal source, gasoline vehicle, diesel vehicle, and volcanic emission. The PMF result of size-resolved source contributions showed that natural sources represented by local soil, sea salt, continental soil, and volcanic emission contributed about 79% to the predicted primary particulate matter(PM) mass in the coarse size range ($1.15{\sim}12{\mu}m$) while anthropogenic sources such as coal combustion and biomass/biofuel burning contributed about 58% in the fine size range($0.56{\sim}2.5{\mu}m$). The diesel vehicle source contributed mostly in ultra-fine size range($0.09{\sim}0.56{\mu}m$) and was responsible for about 56% of the primary PM mass.

Rapid Screening of Naturally Occurring Radioactive Nuclides (238U, 232Th) in Raw Materials and By-Products Samples Using XRF

  • Park, Ji-Young;Lim, Jong-Myoung;Ji, Young-Yong;Lim, Chung-Sup;Jang, Byung-Uck;Chung, Kun Ho;Lee, Wanno;Kang, Mun-Ja
    • Journal of Radiation Protection and Research
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    • v.41 no.4
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    • pp.359-367
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    • 2016
  • Background: As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of $^{238}U$ and $^{232}Th$ using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. Materials and Methods: A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of $^{238}U$ and $^{232}Th$ based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results and Discussion: Results of the XRF measurement for $^{238}U$ and $^{232}Th$ showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of $^{238}U$ and $^{232}Th$ in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS ($R^2{\geq}0.95$) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Conclusion: Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ($^{238}U$ and $^{232}Th$) in NORM samples.

A Study on the Modification of NH4+Y-zeolite for Improving Adsorption/Desorption Performance of Benzene (NH4+Y-zeolite의 개질을 통한 벤젠 흡·탈착 성능 증진 연구)

  • Jang, Young Hee;Noh, Young Il;Lee, Sang Moon;Kim, Sung Su
    • Clean Technology
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    • v.25 no.1
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    • pp.33-39
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    • 2019
  • A.C (activated carbon) is mainly used to remove VOCs (volatile organic compounds), however, it has many problems such as fire risk due to increasing of adsorbent surface temperature during VOCs ad/desorption, increased cost by frequent replacement cycles requirement and performance degradation when containing moisture. In order to solve these problems, many researches, hydrophobic zeolite adsorbents, have been reported. In this study, $NH_4{^+}Y$-zeolite was synthesized with Y-zeolite through steam treatment and acid treatment, which is one of the hydrophobic modification methods, to secure high surface area, thermal stability and humidity resistance. The Y, Y-550-HN, Y-600-HN and Y-650-HN had adsorption capacities of $23mg\;g^{-1}$, $38mg\;g^{-1}$, $77mg\;g^{-1}$, $61mg\;g^{-1}$. The change of Si/Al ratio, which is an index to confirm the degree of modification, was confirmed by XRF (X-ray fluorescence spectrometer) analysis. As a result, the adsorbtion performance was improved when Y-zeolite modified, and the Si/Al ratio of Y, Y-550-HN, Y-600-HN, Y-650-HN were increased to 3.1765, 6.6706, 7.3079, and 7.4635, respectively. Whereas it was confirmed that structural crystallization due to high heat treatment temperature affected performance degradation. Therefore, there is an optimal heat treatment temperature of Y-zeolite, optimum modification condition study could be a substitute for activated carbon as a condition for producing an adsorbent having high durability and stability.

Material Analysis of Bosu of the Royal Seals of the Joseon Dynasty and the Korean Empire (조선 왕실과 대한제국 황실 어보 보수(寶綬)의 재료학적 분석)

  • Lee, Hyeyoun;Kim, Jooyoung;Cho, Mungyeong;Kim, Minji;Park, Daewoo;Lee, Jungmin
    • Journal of Conservation Science
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    • v.37 no.2
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    • pp.154-166
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    • 2021
  • The royal seal, in either gold or jade, is used to symbolize Joseon's royal family, and it is made up of a Bonu (a handle), Bosin (a body), Bomun (a letter inscribed on the seal), and Bosu (a string attached to the seal). The Bosu was designed to enhance the seal's dignity and facilitate convenient handling. Bosu consists of Kkeun-mog and Bangwool-sul (decorated with gilt paper), which are made of Bangwool, Bangwool-mog, and Sul. In this study, the form survey, color, material, and composition of 318 Bosu pieces from the Joseon Dynasty and Korean Empire produced from 1441 to 1928 were analyzed. As time passed, the strings on the seals became longer and thinner. Bangwool-mog disappeared from the mid-1800s, and a ring appeared at the end of the Sul. Most of the colors used were scarlet, but orange and purple were also identified. Although most of the Bosu are silk, five Bosu from the 1900s and one Bosu from the 1740s (likely replaced in the 1900s) are estimated to be rayon. The gilt paper's main chemical components used to decorate the Bangwool-sul vary according to age. Until the mid-1800s, gold (Au) was used for the Sul and Bangwool, but since the mid-1800s, gold (Au) and brass (Cu-Zn) were used for Sul and Bangwool, respectively, and then brass (Cu-Zn) was used for Sul and Bangwool. While the Bosu was a seal accessory, it can be used to identify changes in the manufacturing techniques and materials of the period.

Development of Mineral Admixture for Concrete Using Spent Coffee Grounds (커피찌꺼기를 활용한 콘크리트 혼화재의 개발)

  • Kim, Sung-Bae;Lee, Jae-Won;Choi, Yoon-Suk
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.10 no.3
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    • pp.185-194
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    • 2022
  • Coffee is one of the most consumed beverages in the world and is the second largest traded commodity after petroleum. Due to the great demand of this product, large amounts of waste is generated in the coffee industry, which are toxic and represent serious environmental problems. This study aims to study the possibility of recycling spent coffee grounds (SCG) as a mineral admixture by replacing the cement in the manufacturing of concrete. To recycle the coffee g rounds, the SCG was dried to remove moisture and fired in a kiln at 850 ℃ for 8 hours. Carbonized coffee grounds are produced as coffee grounds ash (CGA) through ball mill grinding. The chemical composition of the prepared coffee grounds ash was investigated using X-ray fluorescence (XFR). According to the chemical composition analysis, the major elements of coffee grounds ash are K2O(51.74 %), CaO(15.92 %), P2O5(14.39 %), MgO(7.74 %) and SO3(6.89 %), with small amounts of F2O3(0.66 %), SiO2(0.59 %) and Al2O3(0.31 %) content. To evaluate quality and mechanical properties, substitutions of 5, 10, and 15 wt.% of coffee grounds ash (CGA) were tested. From the quality test results, the 28-day activity index of CGA5 reached 80 %, and the flow value ratio reached 96 %, which is comparable to the minimum requirement for second-grade FA. From the test results of the mortar, the optimal results have been found in specimens with 5 wt-% coffee grounds ash, showing good mechanical and physical properties.

Surface Coating Treatment of Phosphor Powder Using Atmospheric Pressure Dielectric Barrier Discharge Plasma (대기압 유전체배리어방전 플라즈마를 이용한 형광체 분말 코팅)

  • Jang, Doo Il;Ihm, Tae Heon;Trinh, Quang Hung;Jo, Jin Oh;Mok, Young Sun;Lee, Sang Baek;Ramos, Henry J.
    • Applied Chemistry for Engineering
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    • v.25 no.5
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    • pp.455-462
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    • 2014
  • This work investigated the hydrophobic coating of silicate yellow phosphor powder in the form of divalent europium-activated strontium orthosilicate ($Sr_2SiO_4:Eu^{2+}$) by using an atmospheric pressure dielectric barrier discharge (DBD) plasma with argon as a carrier and hexamethyldisiloxane (HMDSO), toluene and n-hexane as precursors. After the plasma treatment of the phosphor powder, the lattice structure of orthosilicate was not altered, as confirmed by an X-ray diffractometer. The coated phosphor powder was characterized by scanning electron microscopy, fluorescence spectrophotometry and contact angle analysis (CAA). The CAA of the phosphor powder coated with the HMDSO precursor revealed that the water contact angle increased from $21.3^{\circ}$ to $139.5^{\circ}$ (max. $148.7^{\circ}$) and the glycerol contact angle from $55^{\circ}$ to $143.5^{\circ}$ (max. $145.3^{\circ}$) as a result of the hydrophobic coating, which indicated that hydrophobic layers were successfully formed on the phosphor powder surfaces. Further surface characterizations were performed by Fourier transform infrared spectroscopy and X-ray photoelectron spectrometry, which also evidenced the formation of hydrophobic coating layers. The phosphor coated with HMDSO exhibited a photoluminescence (PL) enhancement, but the use of toluene or n-hexane somewhat decreased the PL intensity. The results of this work suggest that the DBD plasma may be a viable method for the preparation of hydrophobic coating layer on phosphor powder.

A Study on Cation Extraction and Impurity Separation in Slag (슬래그 내 양이온 추출 및 불순물 분리 연구)

  • Lee, Ye Hwan;Kang, Hyerin;Jang, Younghee;Lee, Si-Jin;Kim, Sung Su
    • Clean Technology
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    • v.25 no.4
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    • pp.311-315
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    • 2019
  • The cation extraction and impurity separation were studied in order to investigate the recyclability of a slag produced from the steel refinery industry. Two types of slag (Slag-A, B) were collected and characterized in this study. The initial characterization by X-ray diffraction (XRD) and X-ray fluorescence (XRF) confirmed the existence of various kinds of ions in the slag such as Ca2+ (30 ~ 40%), Fe3+ (20 ~ 30%), Si4+ (15%), Al3+ (10%), Mn2+ (7%), and Mg2+ (3 ~ 5%). Inductively coupled plasma atomic emission spectroscopy (ICP-AES) analysis on the extracted slag using 2 M HCl as a solvent indicated that a higher concentration of Ca2+ was extracted as the S/L ratio was increased. The Ca2+ extraction concentration were found to be 8,940 mg L-1 (Slag-A) and 10,690 (Slag-B) mg L-1 when the S/L ratio for Ca2+ extraction was 0.1. However, the extract was strongly acidic ( < pH 1) at 0.1 S/L. Also the other ions (impurities) were extracted simultaneously in addition to Ca2+. To increase the purity of Ca2+ in order to transform the slag to a high value resource, a pH-swing was conducted. The impurities tended to precipitate at higher rate as the pH was increased. Notably, the Ca2+ rapidly precipitated above a certain pH and at a pH of 10.5, while the selectivity of Ca2+ was over 99%. It is expected that the aqueous solution in which high contents of Ca2+ was selectively dissolved in this study would be suitable for the carbonation process for reducing CO2 and for the production of calcium carbonate.