The effect of operating conditions on the time-dependent X-ray intensity variation is of great importance for the optimal EPMA conditions for accurate determinations of various elements in carbonate minerals. Beam dia...The effect of operating conditions on the time-dependent X-ray intensity variation is of great importance for the optimal EPMA conditions for accurate determinations of various elements in carbonate minerals. Beam diameters of 0, 1, 2, 5, 10, 15, and 20 μm, and beam currents of 3, 5, 10, 20,and 50 nA were tested. Ca, Mg, Zn, and Sr were found to be more sensitive to electron beam irradiation as compared to other elements, and small currents and large beam diameters minimized the timedependent X-ray intensity variations. We determined the optimal EPMA operating conditions for elements in carbonate: 10 μm and 5 nA for calcite;10 μm and 10 nA for dolomite;5 μm and 10 nA or 10 μm and 20 nA for strontianite;and 20 nA and 5 μm for other carbonate. Elements sensitive to electron beam irradiation should be determined first. In addition, silicate minerals are preferred as standards rather than carbonate minerals.展开更多
Red mud is a bauxite residue generated during the process of alumina production. In this research, the occur- rence mode of scandium in the Bayer red mud was investi- gated mainly by electron probe microanalysis （EPM...Red mud is a bauxite residue generated during the process of alumina production. In this research, the occur- rence mode of scandium in the Bayer red mud was investi- gated mainly by electron probe microanalysis （EPMA）. The Bayer red mud used in this work is composed of 21.47 wt% hematite, 12.13 wt% goethite, 8.86 wt% gibbsite, 5.02 wt% perovskite, 9.70 wt% quartz, 3.23 wt% anhydrite, 29.92 wt% Na_2Al_2Si_5O_14 and 9.67 wt% Al_3Fe_5O_12. Besides, the scandium content in the Bayer red mud is 84.32 × 10-6, indicating that this Bayer red mud is an important scandium resource deserving exploitation. The EPMA results show that the scandium within the Bayer red mud is mainly occurring in the iron minerals of hematite and goethite with the isomorphism form, but its distribution is not homogeneous in these iron minerals with the Sc_2O_3 content between 330 × 10-6 and 2040 × 10-6. This study provides a theoretical base for the further experimental work on the scandium extraction from this Bayer red mud.展开更多
Laser-induced breakdown spectroscopy （LIBS） was used to decipher the unique multi-elemental characteristics of Juncus effusus L. The spectral fingerprints of Juncus effusus L. were established based on elemental mic...Laser-induced breakdown spectroscopy （LIBS） was used to decipher the unique multi-elemental characteristics of Juncus effusus L. The spectral fingerprints of Juncus effusus L. were established based on elemental microanalysis via LIBS. Microanalysis and multimode sampling methodologies were designed in this study. The relative standard deviation （RSD） approach was performed to optimize the multi-shot measurements. Taking advantage of the capability with no or minimal sample pre-treatment of LIBS, a thermodynamic chart of four elements （Mg, Ca, Ba, and Na） was created from twelve collection regions. The diagram of elemental distribution on a micro-scale was generated to explore the nature of Juncus effusus L. by LIBS. The results demon- strated that LIBS is a promising technique for rapid elemental microanalysis of heterogeneous samples.展开更多
A rapid, sensitive and reproducible high performance liquid chromatography （HPLC） method with post-column fluorescence derivatization has been developed to determine the amount of low-molecular- weight sulfated poly...A rapid, sensitive and reproducible high performance liquid chromatography （HPLC） method with post-column fluorescence derivatization has been developed to determine the amount of low-molecular- weight sulfated polysaccharide （GFS） in vivo. The metabolism of GFS has been shown to fit a two component model following its administration by intravenous injection, and its pharmacokinetic parameters were determined to be as follows： half-time of distribution phase （t1/2α）=11.2±2.93 min, half-time of elimination phase （tl/2α）=98.20±25.78 min, maximum concentration （Cmax）=110.53 gg/mL and peak time （Tmax）=5 min. The pharmacokinetic behavior of GFS was also investigated following intragastric administration. However, the concentration of GFS found in serum was too low for detection, and GFS could only be detected for up to 2 h after intragastric administration （200 mg/kg body weight）. Thus, the bioavailability of GFS was low following intragastric administration because of the metabolism of GFS. In conclusion, HPLC with post-column derivatization could be used for quantitative microanalysis and pharmacokinetic studies to determine the presence of polysaccharides in the serum following intravenous injection.展开更多
The 50 wt pct TiC-C films were prepared on stainless steel substrates by using a technique of ion beam mixing. These films were irradiated by hydrogen ion beam with a dose of 1×10^18 ions/cm^2 and an energy of 5 ...The 50 wt pct TiC-C films were prepared on stainless steel substrates by using a technique of ion beam mixing. These films were irradiated by hydrogen ion beam with a dose of 1×10^18 ions/cm^2 and an energy of 5 keV. Microanalysis of X-ray photoelectron spectroscopy （XPS） and secondary ion mass spectroscopy （SIMS） were used to analyze the films before and after hydrogen ion irradiation and to study the mechanism of hydrogen resistance.展开更多
Nickel laterites are considerable sources of nickel. To be successfully exploited it is important to know the mineralogical and microstructural characteristics of the ore. Besides, the identification of the mineralogi...Nickel laterites are considerable sources of nickel. To be successfully exploited it is important to know the mineralogical and microstructural characteristics of the ore. Besides, the identification of the mineralogical components as well as the fabric description, can lead to the interpretation of the mechanism of deposit genesis. The aim of the present study is the microscopic and microanalytical investigation of the Fe-Ni ores from Komnina Vermion area (N.W. Greece). The mineralogical composition of the ore is mainly hematite, quartz, chromite and chlorite, while in minor quantities goethite, nickeliferous chlorite, serpentine, talc and calcite are also present. The ore structure is allotriomorphic inequigranular and the texture is oolitic-pisolitic. According to microscopic examination the deposit can be registered as a secondary pseudo-autochthonous.展开更多
OBJECTIVE: To observe the distribution of copper in the subcellular structure for the understanding of primary pathogenesis of hepatolenticular degeneration (HLD). METHODS: Skin fibroblasts taken from HLD patients wer...OBJECTIVE: To observe the distribution of copper in the subcellular structure for the understanding of primary pathogenesis of hepatolenticular degeneration (HLD). METHODS: Skin fibroblasts taken from HLD patients were cultured as an in vitro model of HLD, and the control cells taken from healthy volunteers were clutured in the same way. The distribution of copper inside and outside of lysosomes in fibroblasts was detected by quantitative electron probe X-ray microanalysis. The relationship between the subcellular location of copper and the genotype of the patients, and relationship between the distribution of copper and the course of the disease were analyzed. RESULTS: The content of Cu^(2+) inside lysosomes of HLD cells (14.6±2.1 mmol/kg) and of heterozygote cells (11.6±0.6 mmol/kg) was higher than that of normal cells (4.5±1.2 mmol/kg) (P<0.01). The content of Cu^(2+) outside lysosomes of HLD cells (17.5±4.2 mmol/kg) and of heterozygote cells (12.0±0.9 mmol/kg) was higher than that of normal cells (4.7±1.2 mmol/kg) (P<0.01). The distribution of copper in the subcellular structure was correlated with disease courses of HLD patients. With the progression of the disease, more copper was deposited in lysosomes (r=0.85, P<0.01). The content of copper in the diffused cytoplasmic compartment in HLD cells was correlated with that of sulfur (r=0.86, P<0.05), but not in heterozygote and normal cells. CONCLUSIONS: In the early stage of HLD, copper is accumulated outside lysosome, which is paralleled with increase of metallothionein-like proteins (copper and sulfur-binding proteins). With the development of the disease, more copper is deposited inside lysosome than outside lysosome. We conclude that the up-regulation expression of copper and sulfur-binding proteins and copper accumulation in lysosomes may play an important role in lowering the ATP7B gene mutation-induced toxic effects of free copper on the cell.展开更多
AIM To develop methods of articular cartilage preparation for X-ray-electron probe microanalysis and to study its elements content in experimental osteoarthrosis.METHODS Twenty dogs aged 2-8 years were divided in rese...AIM To develop methods of articular cartilage preparation for X-ray-electron probe microanalysis and to study its elements content in experimental osteoarthrosis.METHODS Twenty dogs aged 2-8 years were divided in research(aged 2 years, induction of osteoarthrosis-IOA) and intact group. Intact group included three subgroups(aged 2, 5 and 8 years). Samples of cartilage after araldite saturation and pouring were partially cut into semithin sections stained with methylene blue and with methylene blue-basic fuchsin. Their smooth surfaces were investigated by X-ray-electron probe microanalysis. Spatial distribution of sulfur, calcium and phosphorus and their concentrations(weight %) were investigated.RESULTS X-ray electron probe microanalysis revealed non-uniformsulfur distribution in cartilage of intact animals: Its content increases from superficial zone to deep one, this regularity was preserved in animals with IOA. Differences of IOA with spontaneous chondropathy were revealed. Spontaneous aging was characterized by calcium and phosphorus storage in deep and calcified zones and compensatory increase of sulfated glycosaminoglycans in intermediate and deep cartilage zones as evidenced by the metachromatic reaction and microanalysis data. Unlike spontaneous chondropathy connected with aging in experimentally stimulated osteoarthrosis more intensive storage of calcium but minor phosphorus in intermediate zone were marked. In IOA the calcified cartilage thinning and osteoclastic resorption are apparent with few changes of elements composition; the only difference from control is minority phosphorus content.CONCLUSION The obtained results demonstrate specific tricks of X-ray electron probe microanalysis and its possibility in the research of mechanisms of articular cartilage alterations in osteoarthrosis.展开更多
Tomatoes are one of the main vegetables in the food industry that are consumed fresh and processed. A multi-element microanalysis was performed with the use of scanning electron microscopy (SEM) in conjunction with en...Tomatoes are one of the main vegetables in the food industry that are consumed fresh and processed. A multi-element microanalysis was performed with the use of scanning electron microscopy (SEM) in conjunction with energy dispersion spectroscopy (EDS), to see changes in nutrient concentration in roots and leaves, as well as fresh and dry biomass in tomato seedlings. Exposed in nutrient solution (NS) with different levels of Ca (control, 25, 50 and 100 mM). The root was put in also<span lang="EN-US" style="font-size:10pt;font-family:;" "=""> </span><span lang="EN-US" style="font-size:10pt;font-family:;" "="">to H<sub>2</sub>O<sub>2</sub> for 8 hours to observe the changes that occurred. It was observed that NS with 100 mM Ca in fresh stem biomass and fresh leaf biomass increased by 25% and 38% compared to the control. It was observed that the NS with 100 and 50 mM of Ca, the content of Ca and Cl in foliar tissue increased by 34.50% and 13.15% compared to the control. Treatment with H<sub>2</sub>O<sub>2</sub> and with 25 and 100 mM of Ca at NS increased the height of the seedling and fresh leaf bio-mass by 19.75% and 60.80% compared to the control. The treatment with H<sub>2</sub>O<sub>2</sub> and with the different levels of Ca in the NS increased the content of C, P, K, Ca and Cl in the leaf tissue. Only S was significant for the control. Treatment with H<sub>2</sub>O<sub>2</sub> and 100 mM Ca in the NS increased Ca and Mg by 83.48% and 40.47% for the root compared to the control. The K and Cl in the root was higher in the control treatment by 47.61% and 55% respect to the highest level of Ca.</span><span lang="EN-US" style="font-size:10pt;font-family:;" "=""> </span><span lang="EN-US" style="font-size:10pt;font-family:;" "="">It is concluded that multielemental microanalysis is a powerful, non-destructive, fast and accurate tool for the determination of plant nutrients. Also, it is applicable for the areas like horticulture, physiology and agronomy.</span>展开更多
Laser-ablation laser-induced breakdown spectroscopy （LA-LIBS） based on single Nd：YAG laser is used to analyze copper impurity in silver jewellery with enhanced sensitivity and minimal sample ablation. 6-30 folds si...Laser-ablation laser-induced breakdown spectroscopy （LA-LIBS） based on single Nd：YAG laser is used to analyze copper impurity in silver jewellery with enhanced sensitivity and minimal sample ablation. 6-30 folds signal enhancement can be achieved under the re-excitation of the breakdown laser and the spatial resolution is only determined by the ablation laser. 50 ppm limit of detection of copper is achieved when the crater diameter is 17.2 μm under current experimental condition. This technique gives higher analysis sensitivity under the same sample ablation in comparison with single pulse （SP） LIBS. It is useful for high sensitive element mieroanalvsis of precious samples.展开更多
基金supported by the Natural Science Foundation of China (No. 41403022)the Fundamental Research Funds for the Central Universities, China University of Geosciences (Wuhan) (No. CUGL150401)
文摘The effect of operating conditions on the time-dependent X-ray intensity variation is of great importance for the optimal EPMA conditions for accurate determinations of various elements in carbonate minerals. Beam diameters of 0, 1, 2, 5, 10, 15, and 20 μm, and beam currents of 3, 5, 10, 20,and 50 nA were tested. Ca, Mg, Zn, and Sr were found to be more sensitive to electron beam irradiation as compared to other elements, and small currents and large beam diameters minimized the timedependent X-ray intensity variations. We determined the optimal EPMA operating conditions for elements in carbonate: 10 μm and 5 nA for calcite;10 μm and 10 nA for dolomite;5 μm and 10 nA or 10 μm and 20 nA for strontianite;and 20 nA and 5 μm for other carbonate. Elements sensitive to electron beam irradiation should be determined first. In addition, silicate minerals are preferred as standards rather than carbonate minerals.
基金supported by the National Natural Science Foundation of China (Nos. 51604026 and 51234008)the China Postdoctoral Science Foundation (Nos. 2016M590046 and 2016T90034)
文摘Red mud is a bauxite residue generated during the process of alumina production. In this research, the occur- rence mode of scandium in the Bayer red mud was investi- gated mainly by electron probe microanalysis （EPMA）. The Bayer red mud used in this work is composed of 21.47 wt% hematite, 12.13 wt% goethite, 8.86 wt% gibbsite, 5.02 wt% perovskite, 9.70 wt% quartz, 3.23 wt% anhydrite, 29.92 wt% Na_2Al_2Si_5O_14 and 9.67 wt% Al_3Fe_5O_12. Besides, the scandium content in the Bayer red mud is 84.32 × 10-6, indicating that this Bayer red mud is an important scandium resource deserving exploitation. The EPMA results show that the scandium within the Bayer red mud is mainly occurring in the iron minerals of hematite and goethite with the isomorphism form, but its distribution is not homogeneous in these iron minerals with the Sc_2O_3 content between 330 × 10-6 and 2040 × 10-6. This study provides a theoretical base for the further experimental work on the scandium extraction from this Bayer red mud.
基金supported by National Natural Science Foundation of China(No.81303218)Beijing Municipal Government for the University Affiliated with the Party Central CommitteeDoctoral Fund of Ministry of Education of China(No.20130013120006)
文摘Laser-induced breakdown spectroscopy （LIBS） was used to decipher the unique multi-elemental characteristics of Juncus effusus L. The spectral fingerprints of Juncus effusus L. were established based on elemental microanalysis via LIBS. Microanalysis and multimode sampling methodologies were designed in this study. The relative standard deviation （RSD） approach was performed to optimize the multi-shot measurements. Taking advantage of the capability with no or minimal sample pre-treatment of LIBS, a thermodynamic chart of four elements （Mg, Ca, Ba, and Na） was created from twelve collection regions. The diagram of elemental distribution on a micro-scale was generated to explore the nature of Juncus effusus L. by LIBS. The results demon- strated that LIBS is a promising technique for rapid elemental microanalysis of heterogeneous samples.
基金Supported by the National Natural Science Foundation of China(No.41376166)the Ocean Public Welfare Scientific Research Project(Nos.201005024,201405040)+1 种基金the Jiangsu Science and Technology Project(No.BE2012687)the Special Fund for Cooperation between Jilin Province and Chinese Academy of Sciences(No.2013SYHZ0023)
文摘A rapid, sensitive and reproducible high performance liquid chromatography （HPLC） method with post-column fluorescence derivatization has been developed to determine the amount of low-molecular- weight sulfated polysaccharide （GFS） in vivo. The metabolism of GFS has been shown to fit a two component model following its administration by intravenous injection, and its pharmacokinetic parameters were determined to be as follows： half-time of distribution phase （t1/2α）=11.2±2.93 min, half-time of elimination phase （tl/2α）=98.20±25.78 min, maximum concentration （Cmax）=110.53 gg/mL and peak time （Tmax）=5 min. The pharmacokinetic behavior of GFS was also investigated following intragastric administration. However, the concentration of GFS found in serum was too low for detection, and GFS could only be detected for up to 2 h after intragastric administration （200 mg/kg body weight）. Thus, the bioavailability of GFS was low following intragastric administration because of the metabolism of GFS. In conclusion, HPLC with post-column derivatization could be used for quantitative microanalysis and pharmacokinetic studies to determine the presence of polysaccharides in the serum following intravenous injection.
文摘The 50 wt pct TiC-C films were prepared on stainless steel substrates by using a technique of ion beam mixing. These films were irradiated by hydrogen ion beam with a dose of 1×10^18 ions/cm^2 and an energy of 5 keV. Microanalysis of X-ray photoelectron spectroscopy （XPS） and secondary ion mass spectroscopy （SIMS） were used to analyze the films before and after hydrogen ion irradiation and to study the mechanism of hydrogen resistance.
文摘Nickel laterites are considerable sources of nickel. To be successfully exploited it is important to know the mineralogical and microstructural characteristics of the ore. Besides, the identification of the mineralogical components as well as the fabric description, can lead to the interpretation of the mechanism of deposit genesis. The aim of the present study is the microscopic and microanalytical investigation of the Fe-Ni ores from Komnina Vermion area (N.W. Greece). The mineralogical composition of the ore is mainly hematite, quartz, chromite and chlorite, while in minor quantities goethite, nickeliferous chlorite, serpentine, talc and calcite are also present. The ore structure is allotriomorphic inequigranular and the texture is oolitic-pisolitic. According to microscopic examination the deposit can be registered as a secondary pseudo-autochthonous.
文摘OBJECTIVE: To observe the distribution of copper in the subcellular structure for the understanding of primary pathogenesis of hepatolenticular degeneration (HLD). METHODS: Skin fibroblasts taken from HLD patients were cultured as an in vitro model of HLD, and the control cells taken from healthy volunteers were clutured in the same way. The distribution of copper inside and outside of lysosomes in fibroblasts was detected by quantitative electron probe X-ray microanalysis. The relationship between the subcellular location of copper and the genotype of the patients, and relationship between the distribution of copper and the course of the disease were analyzed. RESULTS: The content of Cu^(2+) inside lysosomes of HLD cells (14.6±2.1 mmol/kg) and of heterozygote cells (11.6±0.6 mmol/kg) was higher than that of normal cells (4.5±1.2 mmol/kg) (P<0.01). The content of Cu^(2+) outside lysosomes of HLD cells (17.5±4.2 mmol/kg) and of heterozygote cells (12.0±0.9 mmol/kg) was higher than that of normal cells (4.7±1.2 mmol/kg) (P<0.01). The distribution of copper in the subcellular structure was correlated with disease courses of HLD patients. With the progression of the disease, more copper was deposited in lysosomes (r=0.85, P<0.01). The content of copper in the diffused cytoplasmic compartment in HLD cells was correlated with that of sulfur (r=0.86, P<0.05), but not in heterozygote and normal cells. CONCLUSIONS: In the early stage of HLD, copper is accumulated outside lysosome, which is paralleled with increase of metallothionein-like proteins (copper and sulfur-binding proteins). With the development of the disease, more copper is deposited inside lysosome than outside lysosome. We conclude that the up-regulation expression of copper and sulfur-binding proteins and copper accumulation in lysosomes may play an important role in lowering the ATP7B gene mutation-induced toxic effects of free copper on the cell.
基金Supported by The RF Ministry of Health within government-mandated program for FSBI Russian Ilizarov Scientific Center "Restorative Traumatology and Orthopaedics"(RISC"RTO") for Scientific Research,No.01201155770
文摘AIM To develop methods of articular cartilage preparation for X-ray-electron probe microanalysis and to study its elements content in experimental osteoarthrosis.METHODS Twenty dogs aged 2-8 years were divided in research(aged 2 years, induction of osteoarthrosis-IOA) and intact group. Intact group included three subgroups(aged 2, 5 and 8 years). Samples of cartilage after araldite saturation and pouring were partially cut into semithin sections stained with methylene blue and with methylene blue-basic fuchsin. Their smooth surfaces were investigated by X-ray-electron probe microanalysis. Spatial distribution of sulfur, calcium and phosphorus and their concentrations(weight %) were investigated.RESULTS X-ray electron probe microanalysis revealed non-uniformsulfur distribution in cartilage of intact animals: Its content increases from superficial zone to deep one, this regularity was preserved in animals with IOA. Differences of IOA with spontaneous chondropathy were revealed. Spontaneous aging was characterized by calcium and phosphorus storage in deep and calcified zones and compensatory increase of sulfated glycosaminoglycans in intermediate and deep cartilage zones as evidenced by the metachromatic reaction and microanalysis data. Unlike spontaneous chondropathy connected with aging in experimentally stimulated osteoarthrosis more intensive storage of calcium but minor phosphorus in intermediate zone were marked. In IOA the calcified cartilage thinning and osteoclastic resorption are apparent with few changes of elements composition; the only difference from control is minority phosphorus content.CONCLUSION The obtained results demonstrate specific tricks of X-ray electron probe microanalysis and its possibility in the research of mechanisms of articular cartilage alterations in osteoarthrosis.
文摘Tomatoes are one of the main vegetables in the food industry that are consumed fresh and processed. A multi-element microanalysis was performed with the use of scanning electron microscopy (SEM) in conjunction with energy dispersion spectroscopy (EDS), to see changes in nutrient concentration in roots and leaves, as well as fresh and dry biomass in tomato seedlings. Exposed in nutrient solution (NS) with different levels of Ca (control, 25, 50 and 100 mM). The root was put in also<span lang="EN-US" style="font-size:10pt;font-family:;" "=""> </span><span lang="EN-US" style="font-size:10pt;font-family:;" "="">to H<sub>2</sub>O<sub>2</sub> for 8 hours to observe the changes that occurred. It was observed that NS with 100 mM Ca in fresh stem biomass and fresh leaf biomass increased by 25% and 38% compared to the control. It was observed that the NS with 100 and 50 mM of Ca, the content of Ca and Cl in foliar tissue increased by 34.50% and 13.15% compared to the control. Treatment with H<sub>2</sub>O<sub>2</sub> and with 25 and 100 mM of Ca at NS increased the height of the seedling and fresh leaf bio-mass by 19.75% and 60.80% compared to the control. The treatment with H<sub>2</sub>O<sub>2</sub> and with the different levels of Ca in the NS increased the content of C, P, K, Ca and Cl in the leaf tissue. Only S was significant for the control. Treatment with H<sub>2</sub>O<sub>2</sub> and 100 mM Ca in the NS increased Ca and Mg by 83.48% and 40.47% for the root compared to the control. The K and Cl in the root was higher in the control treatment by 47.61% and 55% respect to the highest level of Ca.</span><span lang="EN-US" style="font-size:10pt;font-family:;" "=""> </span><span lang="EN-US" style="font-size:10pt;font-family:;" "="">It is concluded that multielemental microanalysis is a powerful, non-destructive, fast and accurate tool for the determination of plant nutrients. Also, it is applicable for the areas like horticulture, physiology and agronomy.</span>
基金the National"973"Program of China(No.2012CB921900)the National Natural Science Foundation of China(Nos.11274123 and 11304100)the Basic Scientific Research Program of South China University of Technology(No.2014ZZ0066)
文摘Laser-ablation laser-induced breakdown spectroscopy （LA-LIBS） based on single Nd：YAG laser is used to analyze copper impurity in silver jewellery with enhanced sensitivity and minimal sample ablation. 6-30 folds signal enhancement can be achieved under the re-excitation of the breakdown laser and the spatial resolution is only determined by the ablation laser. 50 ppm limit of detection of copper is achieved when the crater diameter is 17.2 μm under current experimental condition. This technique gives higher analysis sensitivity under the same sample ablation in comparison with single pulse （SP） LIBS. It is useful for high sensitive element mieroanalvsis of precious samples.
