• Title/Summary/Keyword: X-ray fluorescence(XRF)

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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.

De-NOX evaluation of SCR catalysts adding vanadium-graphene nanocomposite (바나듐 담지된 그래핀 나노복합체를 첨가한 SCR 촉매의 제조 및 활성 평가)

  • Jeong, Bora;Lee, Heesoo;Kim, Eok-Soo;Kim, HongDae
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.6
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    • pp.252-256
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    • 2015
  • Nitrogen oxides ($NO_X$) was emitted from flue gas of stationary sources and exhaust gas of mobile sources, can leads to various environments problems. Selective Catalysts Reduction (SCR) is the most effective $NO_X$ removal system. Commercial $V_2O_5-WO_3/TiO_2$ catalysts, usually containing $V_2O_5$ 0.5~3 wt%, $WO_3$ 5~10 wt%, and $V_2O_5$ is active in the reduction of $NO_X$ but also in the desired oxidation of $SO_2$ to $SO_3$. To reduce the amount of vanadium, using graphene matrix supported vanadium to synthesize nanocomposite. Then, we fabricated to 1 inch honeycomb type of SCR catalysts adding graphene-vanadium nanocomposite. The chemical-physical characteristics and the catalytic activity were performed by XRD, XRF, BET and Micro-Reactor (MR). As a result, the De-NOX performance was showed, similar to the commercial catalyst activity as 77.8 % and using nanocomposite catalyst as 77.1 % at $350^{\circ}C$.

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 Quantitative Analysis of Portable XRF for the Components Analysis of Metal Cultural Heritage (금속문화재 성분분석을 위한 휴대용 XRF 정량분석법 연구)

  • Lim, So-Mang;Kwon, Young-Suk;Cho, Young-Rae;Chung, Won-Sub
    • Journal of Conservation Science
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    • v.37 no.5
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    • pp.451-463
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    • 2021
  • In this study we conducted component analyses of portable XRF detectors using four Au-Cu alloy standard samples to improve their accuracy by drawing up a calibration curve based on ICP-OES standard values. The portable XRF analysis found absolute errors of 0.3 to 3.7 wt% for Au and 0.2 to 8.2 wt% for Cu, confirming that the error range and standard deviation differed from one detector to another. Furthermore, the calibration curve improved their accuracy, such that the relative error rates of Au and Cu decreased from 9.8% and 14% to 3.5% and 3.7%, respectively. Accordingly, an experiment to confirm the calibration curve was conducted using unknown samples, finding that the measured values of the unknown samples fell on the calibration curve. Therefore, to accurately analyze the components of metal cultural heritage items, it is necessary to prepare a calibration curve for each element after checking whether the detector is suitable for the artifact.

Scientific Analysis of Gilt-Bronze Plaquettes with Buddhist Images(Panbul) from Anapji Pond, Gyeongju (안압지 금동판불의 과학적 분석)

  • Yu, Heisun;Park, Haksoo;Shin, Yongbi
    • Conservation Science in Museum
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    • v.8
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    • pp.49-69
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    • 2007
  • This is about the scientific analysis of the 10 items of the gilt-bronze Panbul excavated from Anapji, Gyeongju. First, the composition of the Panbul was confirmed, using X-ray fluorescence spectrometer (XRF), and the patinas covering the surface of the Panbul were analyzed, using X-ray diffractometer (XRD). And the micro structures and gilt layer of the Panbul were investigated, using microscope and scanning electron microscope with energy dispersive spectrometer (SEM/EDS), and in order to investigate the internal conditions of the Panbul, X-radiography was conducted. As the result, it is found out that the material of the Panbul excavated from Anapji was the bronze of copper (86~95%) and tin (4~12%), and coated with gold. And cuprite (Cu2O) was detected from red patina of the gilt-bronze Panbul, and chalcocite(Cu2S) also was detected from the black patina. As the result of the observation of the micro structure through microscope, it is estimated that it was manufactured, using the wax molding method, and, judging from the fact that the thickness of gilt layer was not even, and that the groove had been filled, it was presumed that the amalgam coating method had been used, but some questions still remain, because mercury was not detected. Lastly, through the X-radiography, it was observed that the tiny round spots existed, which was presumed to have been generated during the casting.

Mineralogical Studies for the Standadization of the Kaolinitum (백석지(白石脂)의 품질표준(品質標準) 설정(設定)을 위한 약용광물학적(藥用鑛物學的) 연구(硏究))

  • Park, Maeng-Eon;Sung, Kyu-Youl;Kim, Pil-Geun;Kim, Chang-Min;Lee, Boo-Kyun;Choi, Yong-Sun;Jung, Yong-Soo;Lee, Jang-Cheon
    • The Korea Journal of Herbology
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    • v.21 no.4
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    • pp.149-158
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    • 2006
  • Objectives : This study was carried out to characterize the 'Kaolinitum' used as mineral medicine before and after physical and chemical manipulation. Methods : The mineralogy of the original raw kaolinitumes with different localities was identified by X-ray diffraction analysis. The concentrations of major, minor and trace elements of samples, furthermore, measured by the X-ray fluorescence spectrometer (XRF) and inductively coupled plasma-mass spectrometer (ICP-MS). In order to understand the variety of kaolinitum after thermal treatment, the differential thermal analysis (DTA) and the thermo-gravimetric analysis (TGA) were carried out. Results : According to the result of X-ray diffraction analysis, the kaolinitumes are composed ofcalcite, alunite and quartz. Si and Al are the major ions and heavy metals such as Cd, Cr, Pb, Zn, As, Ni and Cu are included in the kaolinitumes as trace ions. The concentration of these metals in the samples decreased after physical and chemical manipulation. The weight of kaolinitum was also decreased at $500^{\circ}C$ and about $700^{\circ}C$during experiment of TGA. Conclusion : The results of this study can be used to provide the scientific basis of the medical usage of kaolinitum.

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Characteristics of the Black Surface Layer on Carbonate Stone Pagoda in Urban Area and Its Origin (도심지역에 위치한 탄산염암 석탑 표면에 형성된 흑색층의 특성과 그 기원)

  • Do, Jin-Young;Kim, Jeong-Jin;Cho, Hyen-Goo
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.4 s.50
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    • pp.383-392
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    • 2006
  • Calcium carbonate stone deterioration has been intensified in urban area, mainly due to the action of atmospheric pollutant. Samples from the black surface layer were examined under petrographic and scanning electron microscope, coupled with energy dispersive X-ray analyser X-ray fluorescence and X-ray diffraction analysis was also carried out for chemical composition and mineral phase analysis, respectively. Moreover, sulphur isotope ratio was measured, in order to identify the origin of sulphate compounds in the black surface layer. Optical and electronic petrographic analysis indicated that gypsum and Quartz were contained in the black surface layer and led to microcracks. Microstructure and chemical composition analysis showed that the interface between black layer and original stone is not black but its characteristic is similar to black layer The results indicated that during deterioration process the black layer can be expanded gradually into the interface by adsorption of atmospheric pollutants. The sulphur isotope analysis demonstrates that there are different origins of the sulphur component in black surface layer.

Ingredients and cytotoxicity of MTA and 3 kinds of Portland cements (MTA와 포틀랜드 시멘트의 구성성분분석과 세포독성에 관한 연구)

  • Chang, Seok-Woo;Yoo, Hyun-Mi;Park, Dong-Sung;Oh, Tae-Seok;Bae, Kwang-Shik
    • Restorative Dentistry and Endodontics
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    • v.33 no.4
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    • pp.369-376
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    • 2008
  • The aim of this study was to compare the compositions and cytotoxicity of white ProRoot MTA (white mineral trioxide aggregate) and 3 kinds of Portland cements. The elements, simple oxides and phase compositions of white MTA (WMTA), gray Portland cement (GPC), white Portland cement (WPC) and fast setting cement (FSC) were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray fluorescence spectrometry (XRF) and X-ray diffractometry (XRD). Agar diffusion test was carried out to evaluate the cytotoxicity of WMTA and 3 kinds of Portland cements. The results showed that WMTA and WPC contained far less magnesium (Mg), iron (Fe), manganese (Mn), and zinc (Zn) than GPC and FSC. FSC contained far more aluminum oxide ($Al_2O_3$) than WMTA, GPC, and WPC. WMTA, GPC, WPC and FSC were composed of main phases. such as tricalcicium silicate ($3CaO{\cdot}SiO_2$), dicalcium silicate ($2CaO{\cdot}SiO_2$), tricalcium aluminate ($3CaO{\cdot}Al_2O_3$), and tetracalcium aluminoferrite ($4CaO{\cdot}Al_2O_3{\cdot}Fe_2O_3$). The significance of the differences in cellular response between WMTA, GPC, WPC and FSC was statistically analyzed by Kruskal-Wallis Exact test with Bonferroni' s correction. The result showed no statistically significant difference (p > 0.05). WMTA, GPC, WPC and FSC showed similar compositions. However there were notable differences in the content of minor elements. such as aluminum (Al), magnesium, iron, manganese, and zinc. These differences might influence the physical properties of cements.

Comparison of flux and natural sapphire after heat-treatment (열처리 후 플럭스 사파이어와 천연 사파이어의 비교 분석)

  • Kim, Ki-In;Ahn, Yong-Kil;Seo, Jin-Gyo;Park, Jong-Wan
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.19 no.3
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    • pp.152-158
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    • 2009
  • Various fabrication methods have been used to synthesize sapphire which has qualities of jewelry well beyond the industrial class. Among them, the flux sapphire of Chatham Company which has as high value as jewelry was selected in order to compare natural and synthetic sapphire. First, the WD-XRF (Wavelength dispersive x-ray fluorescence spectrometer) was used to analyze the chemical composition of natural and synthetic sapphire. Although natural sapphire had very diverse chemical compositions, flux sapphire had small quantities of Mo, Pt and Pb elements in addition to the similar chemical ingredients to natural one. Pt is decisive proof of flux sapphire. Next, by investigating spectroscopic characteristics using UV-VIS Spectrophotometer after heat treatment at high temperatures of $1300^{\circ}C$ and $1500^{\circ}C$, the variation of 690 nm absorbance related to $Cr^{3+}$ was detected in the natural sapphire while those of the 690 nm absorbance (related to $Cr^{3+}$) as well as absorbance of 376 nm and 388 nm ($Fe^{3+}$) were seen in the flux sapphire. It was found that the difference in the absorbance variation of flux sapphire is greater than that of natural sapphire after heat treatment. The chemical composition and spectrum analysis were utilized to compare the natural sapphire and the flux synthetic sapphire.

Compositional and microstructural analyses of grayish-blue-powdered celadon in Yeongseo Region in Gangwon-do:by Wonju Beopcheon-temple site (강원도 영서지역 출토 분청사기의 조성 및 미세구조 분석: 원주(原州) 법천사지(法泉寺址)를 중심으로)

  • Lee, Byoung-Hoon;So, Myoung-Gi
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.211-221
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    • 2013
  • This research aims to examine compositional and microstructural properties of grayish-blue-powdered celadon in Wonju Beopcheon-temple site. X-ray fluorescence sequential spectroscopy (XRF) with micro-point analysis, scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) were applied to determine the chemical composition, microstructure and crystallinity of samples, respectively. As a result, the average compositions of bodies were low silica ($RO_2$) and high flux (RO+$R_2O$). Owing to the high content of calcium oxide the glaze is considered lime type between limealkali type. The body of celdon sheard was found quarts, mullite, microcline, albite. Especially, the body's chemical compositions were compared to the results of previous studies by using a Seger formula. The compositional properties of Grayish-blue-powdered celadon in Wonju Beopcheon-temple site showed diffrently from the the other grayish-blue-powdered celadon.