• 제목/요약/키워드: spectrometry (ICP-MS)

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Trace Element Compositions and Optically Stimulated Luminescence Characteristics of Sedimentary Quartz (퇴적물 내 석영의 광여기 루미네선스 특성과 미량원소 조성)

  • Jeon, Gi-Young;Choi, Jeong-Heon;Kil, Young-Woo
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.4
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    • pp.357-365
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    • 2010
  • Optically stimulated luminescence (OSL) of quartz is commonly applied to the age dating of Quaternary sediments. However, one of the issues is that some of the quartz samples are not suitable to OSL dating. Mineralogical analysis of the quartz samples with diverse OSL signals are required to strengthen the reliability and applicability of the OSL dating. We analysed the OSL signal characteristics of sedimentary quartz samples from diverse geological environments and measured their trace element contents using laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Quartz samples could be grouped into ones suitable to OSL dating and ones unsuitable on the basis of their OSL signal characteristics. The average trace element contents ranged from 73 to 260 ppm (Al), and from 61 to 248 ppm (Ti) with minor Li, Mg, Cr, Mn, and Fe contents below 40 ppm. We did not find any significant variation of trace element contents of quartz samples consistent with their OSL signal characteristics. This indicates unknown mineralogical factors causing diverse OSL characteristics which should be confirmed by further analysis of sufficient set of samples.

Monitoring of some heavy metals in oriental animality medicines (동물성 생약에 함유되어 있는 몇 가지 중금속에 대한 실태 조사)

  • Baek, Sunyoung;Chung, Jaeyoen;Lee, Jihye;Park, Kyungsu;Kang, Inho;Kang, Sinjung;Kim, Yunje
    • Analytical Science and Technology
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    • v.22 no.3
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    • pp.201-209
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    • 2009
  • Four heavy metals (Pb, Cd, As, and Hg) in 38 species (total 325 samples) of oriental animality medicines were monitored by inductively coupled plasma-mass spectrometry (ICP-MS) and automatic mercury analyzer (AMA). The detected concentration range of Pb, Cd, As was presented as $0.02{\mu}gkg^{-1}$ $(D.L){\sim}11.29mgkg^{-1}$, $0.01{\mu}gkg^{-1}$ $(D.L){\sim}2.50 mgkg^{-1}$, $0.12{\mu}gkg^{-1}$ $(D.L){\sim}5.27mgkg^{-1}$, respectively. In case of Hg, it the concentration range was $0.01{\sim}77.11mgkg^{-1}$ except one sample which exceeded detection limit. In all samples of Amydae Carapax and Gallnut, it was not detected over the maximum residue limits of metals. Pb is in charge of the greatest portion of contamination in 22 species of animality medicines, and in case of Hg, 54.46% of total samples were over the maximum residue limits. Therefore, environmental levels of Pb and Hg are needed to continue the researches and the studies for tracking pollution source are required.

Material Characteristics of White Wares from Yeongdong Province, Gangwon-do: Gangneung and Donghae Kiln Sites (강원 영동지역 백자의 재료과학적 특성 연구: 강릉 남양리 백자가마터와 동해 발한동2(사문동) 가마터를 중심으로)

  • Lee, Byeong Hoon;So, Myoung-Gi
    • Journal of Conservation Science
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    • v.31 no.3
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    • pp.181-192
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    • 2015
  • This study aims to examine production technique of twelve white wares from the Gangneung Namyang-ri and Donghae Balhan-dong2(Samun-dong) kiln sites, Kangwon Province and characteristics of the used materials, and to find a correlation among materials of the excavated white wares. X-ray fluorescence sequential spectroscopy(XRF), X-ray diffraction(XRD), Dilatometer and Inductively coupled plasma mass spectrometry(ICP-MS), Inductively coupled plasma automic emission spectrometer(ICP-AES) were applied to determine the chemical composition, crystalline phase of samples, firing temperatures, trace elements and rare earth elements. When analyzing body crystalline phases of the white wares using the XRD method, quartz and mullite were extracted from all the samples. Though firing temperature of each sample was different, they were mostly fired at a temperature below $1200^{\circ}C$. Analyzing the excavated white wares using the Seger formula, compositional properties of white wares in Gangneung Namyang-ri kiln showed diffrently from the Donghae Balhan-dong2(Samun-dong) kiln. The body of white wares from Gangneung Namyang-ri kiln have higher raito of $RO_2$ and $RO+R_2O$ than of white wares from Donghae Balhan-dong2(Samun-dong) kiln site. The white wares from Gangneung Namyang-ri kiln and Donghae Balhan-dong2(Samun-dong) kiln were made of host rocks of the different geological origin, according to the result of rare earth elements analysis.

A Study on Chemical Composition and Firing Temperature of White Wares from the Guyre-2ri Kiln Sites, Wonju (원주 귀래2리 가마터 출토 백자의 화학조성과 소성온도 연구)

  • Lee, Byeong Hoon;So, Myoung-Gi
    • Journal of Conservation Science
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    • v.30 no.3
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    • pp.249-261
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    • 2014
  • This study aims to examine production technique of white wares from the Guyre-2ri 1st and 2nd kiln sites, Wonju, Gangwon Province and characteristics of the used materials, and to find a correlation among materials of the excavated white wares. X-ray fluorescence sequential spectroscopy(XRF), X-ray diffraction(XRD), Dilatometer and Inductively coupled plasma mass spectrometry(ICP-MS), Inductively coupled plasma automic emission spectrometer(ICP-AES) were applied to determine the chemical composition, crystalline phase of samples, firing temperatures, trace elements and rare earth elements. White wares from the Guyre-2ri kiln sites contained high contents of coloring oxides and fluxes. Though firing temperature of each sample was different, they were mostly fired at a temperature below $1200^{\circ}C$ and some of them experienced a low temperature of $1000^{\circ}C{\pm}20^{\circ}C$ and a high temperature above $1200^{\circ}C$. When analyzing body crystalline phases of the white wares using the XRD method, quartz and mullite were extracted from all the samples, and the proportions were similar to each other. When analyzing the excavated white wares using the Seger formula, also, all the samples showed similar clay sources and production techniques. Moreover, the white wares were made of host rocks of the same geological origin, according to the result of rare earth elements analysis.

Quantification of seleno proteins in Korean blood serum using solid phase extraction and affinity chromatography-inductively coupled plasma/mass spectrometry (고체상 추출과 친화 크로마토 그라피-유도결합 플라즈마 질량분석법을 이용한 한국인 혈청에서의 셀레노 단백질 정량)

  • Ahn, Ji-Yun;Kwon, Hyo-Sik;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.27 no.2
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    • pp.92-99
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    • 2014
  • Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

Gemological Characterization of B. C. Jade (비씨 제이드의 보석학적 연구)

  • Kim, Won-Sa;Wight, Willow
    • Journal of the Mineralogical Society of Korea
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    • v.21 no.2
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    • pp.177-182
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    • 2008
  • The Gemological characteristics of B.C. jade from Cassiar Mine, British Colombia, Canada, have been investigated, using polarizing microscopy, Mohs' hardness, refractive index and density measurements, X-ray powder diffraction, X-ray fluorescence spectrometry, ICP-MS, Infrared absorption spectrometry, and DTA/TGA. The B.C. jade is deeply green (spinach peen or olive green) in color and is translucent. It shows a resinous or waxy luster. The principal mineral of the material is tremolite-actinolite solid solution and minor amount of Cr-garnet and unidentified opaque minerals are accompanied. Mohs' hardness value ($5.5{\sim}6$). refractive index (1.62), and specific gravity (3.01) are measured. It is very highly tough and shows hackly fracture. The high Fe content ($Fe_2O_3\;4.14{\sim}4.66\;wt%$) in B.C. jade is attributable to a deepening of green color of the material. The B.C. jade starts to dehydrate at v and dehydration is completed at $1000.8^{\circ}C$, transforming tremolite-actinolite solid solution to enstatite, diopside, quartz, and water in its place. This possible reaction is supported by the weight loss of B.C. jade (1.93 wt%) at $1000.8^{\circ}C$ indicated by TGA curve.

Determination of trace arsenic in seawater by flow injection-hydride generation inductively coupled plasma mass spectrometry (연속흐름주입-수소화물생성-유도결합플라스마 질량분석장치를 이용한 바닷물표준시료중의 극미량 비소분석방법의 확립)

  • Suh, Jung-Ki
    • Analytical Science and Technology
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    • v.21 no.4
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    • pp.316-325
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    • 2008
  • An inductively coupled plasma mass spectrometry (ICP-MS) instrument equipped with flow injection-hydride generation system was used for the determination of trace arsenic in seawater sample. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of seawater (CASS-4, NASS-5). The analytical results agreed with certified value within the range of uncertainty. The expanded uncertainties for CASS-4 and NASS-5 in this experiment were ranged from 6.2% to 6.8% obtained from repeated analyses of the CRMs (n=5). The detection limit of $As^+$ (m/z=74.9216) in this method was confirmed about 0.01 ug/kg. Linearity obtained from calibration curve of arsenic was excellent ($R^2=1$). The detection at $As^+$ (m/z=74.9216) and $AsO^+$ (m/z=90.9165) by using oxygen reaction gas in DRC mode was compared. Sensitivity at $AsO^+$ (m/z=90.9165) was decreased about 25-fold, but the analytical results are the same that at $As^+$ (m/z=74.9216).

Accurate Measurement of Arsenic in Laver by Gravimetric Standard Addition Method Combined with High Resolution Inductively Coupled Plasma Mass Spectrometry

  • Lee, Kyoung-Seok;Kim, Hyeon-Ji;Yim, Yong-Hyeon;Kim, Jeongkwon;Hwang, Euijin
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.57-61
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    • 2014
  • A gravimetric standard addition method combined with internal standard calibration has been successfully developed for the accurate analysis of total arsenic in a laver candidate reference material. A model equation for the gravimetric standard addition approach using an internal standard was derived to determine arsenic content in samples. Handlings of samples, As standard and internal standard were carried out gravimetrically to avoid larger uncertainty and variability involved in the volumetric preparation. Germanium was selected as the internal standard because of its close mass to the arsenic to minimize mass-dependent bias in mass spectrometer. The ion signal ratios of $^{75}As^+$ to $^{72}Ge^+$ (or $^{73}Ge^+$) were measured in high resolution mode ($R{\geq}10,000$) to separate potential isobaric interferences by high resolution ICP/MS. For method validation, the developed method was applied to the analysis of arsenic content in the NMIJ 7402-a codfish certified reference material (CRM) and the result was $37.07mg{\cdot}kg^{-1}{\pm}0.45mg{\cdot}kg^{-1}$ which is in good agreement with the certified value, $36.7mg{\cdot}kg^{-1}{\pm}1.8mg{\cdot}kg^{-1}$. Finally, the certified value of the total arsenic in the candidate laver CRM was determined to be $47.15mg{\cdot}kg^{-1}{\pm}1.32mg{\cdot}kg^{-1}$ (k = 2.8 for 95% confidence level) which is an excellent result for arsenic measurement with only 2.8 % of relative expanded uncertainty.

Analysis of volatile compounds and metals in essential oil and solvent extracts of Amomi Fructus (사인으로부터 추출한 정유와 용매 추출물의 휘발성 물질 및 금속성분 분석)

  • Lee, Sam-Keun;Eum, Chul Hun;Son, Chang-Gue
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.436-445
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    • 2015
  • Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

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.