• The Journal of the Petrological Society of Korea
• /
• v.10 no.3
• /
• pp.179-189
• /
• 2001

The determination of trace concentration of U, Th and Pb was carried out for chemical dating of zircon and monazite by electron microprobe. Detection limit and error range should be considered to measure characteristic X-rays of M-line from those minerals, which are low in the ionization of atom and low peak intensity in the spectrum. The element of U, Th and Pb were simultaneously measured with 3 spectrometers equipped with PET crystal to reduce a total counting time and error due to drift of instrumental operating condition. Detection limit could be improved from increase of the peak/background ratio through adjusting pulse height analyzer about 1000 mv baseline. Under permissible maximum analytical conditions, theoretical detection limit of U, Th and Pb is down to 30 ppm (99% confidence level). The analytical result was maintained at a relative error $\pm$10% ($2{\sigma}$) in 800 ppm Pb, $\pm$5% ($2{\sigma}$) in 2330 ppm U and $\pm$10% ($2{\sigma}$) in dating from a single measurement of zircon at 15 keV and 100 nA. However, for the precise dating of zircon and monazite, if it is considered a 3 $\mu\textrm{m}$ spatial resolution, <100 ppm ($3{\sigma}$) detection limit and <$\pm$10% ($2{\sigma}$) relative error, optimum analytical conditions are given as 15~20 keV accelerating voltage, 100~200 nA beam current and 300~1200 sec total counting time. To reduce material damage by high current, there is need to be up to 3~5 $\mu\textrm{m}$ of electron beam diameter, or to use arithmetic average of multiple measuring at a shorter counting time. A younger or relatively low concentration rocks can be dated chemically by lower detection limit and improved precision resulted from increase of current and measuring time.

• Journal of the Mineralogical Society of Korea
• /
• v.16 no.1
• /
• pp.1-17
• /
• 2003

The chemical composition of the arsenopyrite Ib adjoining“triple mutual contact”arsenopyrite + pyrite + hexagonal pyrrhotite may serve as a useful geothermometer in Stage II. In this study it corresponds to temperature T=33$0^{\circ}C$ and f( $S_2$)=10$^{-9.5}$ atm. And the pyrite-hexagonal pyrrhotite buffer curve indicates the probable range of the two variables; T= 315∼345$^{\circ}C$, and f( $S_2$)=10$^{-1}$0.5/∼10$^{-9}$ atm. The present antimony-bearing arsenopyrite (arsenopyrite Ic) is characterized by relatively high content of antimony, ranging from 4.95 to 8.91 percent Sb by weight and excess of iron and deficiency of anions are evident. Such a high antimonian arsenopyrite has never been known within single grain. But being the high content of antimony as in the arsenopyrite Ic, it does not serve as a geothermometer. The results of microprobe analyses for four pairs of asenopyrite and sphalerite in Stage III indicate the temperature range from 310 to 34$0^{\circ}C$, and sulphur fugacity range from 10$^{-10}$ ∼10$^{-9}$ atm. These values seem to correspond with those inferred from the Fe-As-S system.m..

• Journal of the Mineralogical Society of Korea
• /
• v.18 no.4 s.46
• /
• pp.259-266
• /
• 2005

X-ray diffraction (XRD), Electron microprobe analyses (EPMA) and heating experiments were used for mineralogical characterization of natural buserites collected from the Janggun and Dongnam mines. They are closely associated with $7-{\AA}$ phase (usually rancieite) in manganese oxide ores of the supergene oxidation zones of manganese carbonate deposits. Electron microprobe analyses give the average formula $(Ca_{0.78}Mg_{0.64}Mn^{2+}\;_{0.45})Mn^{4+}\;_{8.03}O_{18}\cdot13.2H_{2}O\;and\;(Zn_{0.81}Ca_{0.77}Mg_{0.26})Mn^{4+}\;_{8.00}O_{18}\cdot10.9H_{2}O$ for buserite from the Janggun and the Dongnam mine, respectively. The basal reflection of buserite from the Janggun mine shifts continuously from $9.86\;{\AA}\;at\;40^{\circ}C\;to\;7.60\;{\AA}\;at\;90^{\circ}C$, but the buserite from the Dongnam mine shows tendency of decreasing intensity in the $9.67^{\circ}C$ peak and of increasing intensity in the $7.53\;{\AA}$ peak in the range of $40\∼90^{\circ}C$, showing no gradual shifting of peaks.

• Journal of the Mineralogical Society of Korea
• /
• v.26 no.4
• /
• pp.299-312
• /
• 2013

Magnetite, a major constituent mineral of the Hongcheon carbonatite-phoscorite complex, was produced over three stages in each rock type and decreased in quantity toward the late stage. Electron microprobe analyses for magnetite revealed that Ti and V were detected in traces, but showed increasing tendency from early to late stage. On the contrary, Mg and Mn decreased distinctly, and it is the general differentiation trend of carbonatitic magma. Al also showed decreasing tendency in carbonatite and phoscorite, and Cr was mostly below detection limit except late phoscorite. In early stage, $Fe^{2+}$ was largely replaced by $Mg{2+}$ and $Mn^{2+}$, and $Fe^{3+}$ by $Al^{3+}$ in magnetite, but it has nearly pure composition in late stage. Tendency of increase in V and decrease in Mn toward late stage represents that magma differentiation progressed under the condition of decreasing oxygen fugacity. Low concentrations of Mg, Al, Cr and Ti, as well as the absence of olivine and phlogopite, suggest that the Hongcheon carbonatite-phoscorite complex was generated from depleted magma. Especially, lower concentrations of Mg in magnetite compared to other typical carbonatite-phoscorite complex, and abundant occurrence of Fe-carbonate minerals and quartz in late stage, suggest that magma differentiation of the Hongcheon carbonatite-phoscorite proceeded to the latest stage.

• Economic and Environmental Geology
• /
• v.26 no.2
• /
• pp.167-174
• /
• 1993

Limited geochemical components have been detected in fluid inclusions from ore deposits in south Korea by non-destructive and destructive analytical methods. Review of fluid inclusion studies display that the homogenization temperatures and salinities are in direct proportion. W and Cu ore deposits tend to show higher homogenization temperatures and salinities than Au ore deposits. Abundant halite-bearing fluid inclusions from the Eonyang Granite producing precious amethyst crystals may indicate that the initial fluid originated from magma is highly saline as shown by the quartz from the granite. Raman Laser microprobe detected $CO_2$, $N_2$ and $CH_4$ in a gold deposit, while these components are hardly detected from other deposits, even though destrucive analysis has dectected $CO_2$, $N_2$, $CH_4$, $H_2S$, and $SO_2$ from most of ore deposits. Individual fluid inclusion shows quite different components. These results suggest that large numbers of fluid inclusions should be analysed by Raman Laser microprobe to gain reliable data. Halite-bearing inclusion is hardly found in fluid inclusions from epithermal gold deposits in south Korea. Geochemistry, homogeinzation temperature and salinity of fluid inclusions may be useful to apply for exploration to find a concealed orebody.

• Korean Journal of Mineralogy and Petrology
• /
• v.35 no.4
• /
• pp.457-467
• /
• 2022

Electron bombardment to silicate glass during electron probe microanalysis (EPMA) causes outward migration of Na from the excitation volume and subsequent decrease in the measured X-ray count rates of Na. To acquire precise Na₂O content of silicate glass, one should use proper analytical technique to avoid or minimize Na migration effect or should correct for decreases in the measured Na X-ray counts. In this study, we analyzed 8 silicate glass standard samples using automated Time Dependent Intensity (TDI) correction method of Probe for EPMA software that can calculate zero-time intercept by extrapolating X-ray count changes over analysis time. We evaluated an accuracy of TDI correction for Na measurements of silicate glasses with EPMA at 15 kV acceleration voltage and 20 nA probe current electron beam, which is commonly utilized analytical condition for geological samples. Results show that Na loss can be avoided with 20 ㎛-sized large beam (<0.1 nA/㎛²), thus silicate glasses can be analyzed without TDI correction. When the beam size is smaller than 10 ㎛, Na loss results in large relative errors up to -55% of Na₂O values without correction. By applying TDI corrections, we can acquire Na₂O values close to the reference values with relative errors of ~ ±10%. Use of weighted linear-fit can reduce relative errors down to ±6%. Thus, quantitative analysis of silicate glasses with EPMA is required for TDI correction for alkali elements such as Na and K.

• Economic and Environmental Geology
• /
• v.22 no.2
• /
• pp.117-127
• /
• 1989

Devonian Geochang foliated granite and Jurassic plutonic rocks intrude Precambrian metamorphic Complex at Geochang area, southern part of the Korean Peninsular. Among them hornblendes from four Jurassic plutonic bodies which have had no trace of metamorphism or deformation since their intrusion were dated by K-Ar method. Hornblende gabbro dike which intruded Anorthosite of unknown age revealed $204{\pm}10Ma$, and hornblende granite and hornblende-biotite granodiorite were $178{\pm}9Ma$ and $181{\pm}9Ma$, repectively. Also, hornblende diorite which partly showing primary foliations were $178{\pm}9Ma$, so igneous activity of Geochang area, northern part of Jirisan, were active about 180 Ma before. Microprobe data of dated hornblends and other major constituent minerals such as plagioclases and biotites were also reported, and their chemical composition showed systematic changes in terms of lithologic types.

• Journal of the Mineralogical Society of Korea
• /
• v.6 no.2
• /
• pp.145-155
• /
• 1993

Mineralogical, textural, and chemical changes of chlorite by weathering in anorthosite in the Sancheong district were stucdied using X-ray diffraction, scanning electron microscopy, and electron microprobe analysis. Chlorite in anorthosite corresponds to ferroan clinochlore with IIb structural type. It weatheres firstly to regularly mixed-layered chlorite/vermiculite(C/V) and then, to halloysite without the intermediate stage of vermiculite. Clinochlore packet cleaves and transforms to several thin packets of C/V, which subsequently change to halloysite developint fan-sharped structures by large volume increase. Direct halloysitization of C/V is attributed to the rapid weathering of anorthosite.

• Journal of the Korean Ceramic Society
• /
• v.13 no.3
• /
• pp.55-62
• /
• 1976

순수한 닉켈과 금 박막을 (III)규소 단 결정위에 진공 증착시켰다. Ni/Au/Si나 Au/Ni/Si시료를 진공중에서 약 55$0^{\circ}C$로 가열하였을 때 육방정 혹은 변형된 육방정의 미소 결정들이 규소 기질위에 형성되었다. 이들 미소 결정들의 형성과정 및 조성은 X-선 회절법, scanning electron microscopy 및 scanning Auger microprobe 법을 사용하여 결정하였다. 이들 미소 결정은 NiSi2임이 확인되었다. Ni/Au/Si 시료에서는 Au-Si 공융점(37$0^{\circ}C$) 이상으로 온도가 증가됨에 따라 닉켈과 규소가 Au-Si 공융체 속으로 이동한 후 반응하여 NiSi2를 형성하였다. Au/Ni/Si 시료에 있어서의 Au-Si 공융체 형성은 닉켈 박막에 있는 바늘구멍형의 표면 결함과 관련 지을 수 있겠다. 금이 닉켈 박막의 grain boundary를 통하여 Ni/Si 계면으로 확산되어 그 계면을 습윤시킨 다음 Au-Si 공융체를 형성하였다. 이런 Au-Si 공용체는 닉켈과 규소 원자에 대한 높은 확산 매질로서 작용하여 NiSi2 형성을 촉진시켰다. 표면에 평행한 (III)규소면 위의 NiSi2 미소 결정은 유사한 육방정으로 나타났으며, 경사진 미소결정은 부등변 사변형과 유사하였다. Auger 스펙트럼 및 Ni, Au 및 Si에 대한 내층조성(indepth Composition Profiles)은 NiSi2 미소 결정이 Au-Si 공융체의 matrix에 미소 부분으로 나타났음을 보여주었다.

• Economic and Environmental Geology
• /
• v.28 no.1
• /
• pp.33-41
• /
• 1995

Tin mineralizations in South Korea have been found only in the Ulchin and the Sangdong areas. The Wangpiri and the Yuchang Sn pegmatites appear to be in close spatial and genetical relation to the Wangpiri granitoid in the Ulchin area, and the Soonkyeong Sn pegmatite be in close association with the Nonggeori granites in the Sangdong area from geochemical viewpoint. The electron-microprobe analysis of muscovite, biotite, tourmaline and cassiterite from the granitoids and pegmatites in the Ulchin and the Sangdong areas has revealed a distinct differences of geochemical compositions. The Wangpiri and the Yuchang Sn pegmatites show an enrichment of MnO and a depletion of $TiO_2$, FeO and MgO in comparison with the Soonkyeong Sn pegmatite. This result coincides with the geochemical compositions of granitoid rocks in these areas. Enrichment of MnO and depletion of $TiO_2$ FeO and MgO are characteristic in muscovite, biotite and tourmaline of pegmatites compared with those of granitoids. These geochemical differences of muscovite, biotite and tourmaline between granitoids and pegmatites in these areas implies that pegmatites are more fractionated than granitoids.