Detection of distribution of copper inside and outside of lysosomes in cultured hepatolenticular degeneration fibroblasts by electron probe X-ray microanalysis

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.

Electron probe microanalysis оf experimentally stimulated osteoarthrosis in dogs

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.

Electron probe microanalysis for revealing occurrence mode of scandium in Bayer red mud

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.

Effect of Beam Current and Diameter on Electron Probe Microanalysis of Carbonate Minerals

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.

A double toroidal analyzer for scanning probe electron energy spectrometer

An ultra-high vacuum （UHV） compatible electron spectrometer employing a double toroidal analyzer has been de- veloped. It is designed to be combined with a custom-made scanning tunneling microscope （STM） to study the spatially localized electron energy spectrum on a surface. A tip-sample system composed of a piezo-driven field-emission tungsten tip and a sample of highly ordered pyrolytic graphite （HOPG） is employed to test the performance of the spectrometer. Two-dimensional images of the energy-resolved and angle-dispersed electrons backscattered from the surface of HOPG are obtained, the performance is optimized and the spectrometer is calibrated. A complete electron energy loss spectrum covering the elastic peak to the secondary electron peaks for the HOPG surface, acquired at a tip voltage of -140 V and a sample current of 0.5 pA, is presented, demonstrating the viability of the spectrometer.

东昆仑大格勒富铌碳酸岩矿物学特征

东昆仑大格勒地区新发现一套碱性岩-碳酸岩杂岩体,具有很好的铌等稀有金属成矿潜力。本文在岩相学研究基础上,结合背散射电子图像,应用电子探针能谱半定量分析和波谱定量分析技术,对东昆仑大格勒富铌碳酸岩中的铌矿物进行了原位微区成分分析。岩相学观察表明,铌矿物主要为铌铁矿族、铌钙矿、烧绿石、褐铈铌矿、铌易解石,含铌矿物为含铌钛铁矿、斜锆石。铌矿物嵌布粒度较细,嵌布关系紧密而复杂。其中,铌铁矿族常与磁铁矿、铌钙矿、褐铈铌矿和磷灰石紧密共生,多以细粒状集合体呈浸染状、星散型沿磁铁矿裂纹与边部进行交代。铌钙矿、烧绿石和褐铈铌矿常与铌铁矿、磁铁矿和磷灰石紧密共生,铌钙矿局部与铌铁矿呈不规则状接触分布,烧绿石呈不规则状沿铌铁矿边部分布,褐铈铌矿多以团块状沿铌铁矿边部分布。铌易解石与磁铁矿紧密共生,呈不规则状接触。初步推断铌矿物包括岩浆期形成的烧绿石和铌易解石,热液期形成的铌铁矿、铌钙矿、烧绿石和褐铈铌矿。矿物组合初步显示,大格勒富铌碳酸岩中的铌至少经过了岩浆和热液两个时期的富集。电子探针分析结果表明,主要铌矿物的Nb_(2)O_(5)平均含量分别为:铌铁矿族69.92%,铌钙矿59.55%,烧绿石59.14%,褐铈铌矿43.12%,铌易解石41.55%;含铌矿物的Nb_(2)O_(5)平均含量分别为:含铌钛铁矿1.33%,斜锆石1.22%。其中,铌铁矿族和铌钙矿、烧绿石为可选且具有工业价值的铌矿物。

Frequency dependence of electron temperature in hollow cathode-type discharge as measured by several different floating probe methods

We measured electron temperatures through a hollow cathode-type discharge tube using several different floating probe methods. This method detected a shift in the floating potential when an AC voltage was applied to a probe through an intermediary blocking capacitor. The shift in the floating potential is described as a function of the electron temperature and the applied AC voltage. In this study, the effects of the frequency and waveform on the electron temperatures were systematically investigated. The electron temperature measured when using the floating probe method with applied sinusoidal and triangular voltages was lower than that measured with an applied rectangular voltage.The value in the high frequency range was close to that of the tail electron temperature.

Electron Temperature Measurement by Floating Probe Method Using AC Voltage

This study presents a novel floating probe method to measure electron temperatures using a hollow cathode-type discharge tube. The proposed method detects a shift in the floating potential when an AC voltage is applied to a probe through an intermediary blocking capacitor. The shift in the floating potential is described as a function of the electron temperature and the applied AC voltage. The floating probe method is simpler than the Langmuir probe method because it does not require the measurement of volt-ampere characteristics. As the input AC voltage increases, the electron temperature converges. The electron temperature measured using the floating probe method with an applied sinusoidal voltage shows a value close to the first （tail） electron temperature in the range of the floating potential.

基于耳石微化学的大洋河刀鲚生境履历研究

为探明大洋河刀鲚(Coilia nasus)的“生境履历”,利用电子探针微区分析技术(EPMA)对2020年7月和9月采自大洋河下游水域20尾刀鲚的矢耳石进行了锶(Sr)和钙(Ca)的微化学分析研究。定量线分析结果显示,刀鲚样本均为淡水起源,淡水生境Sr/Ca比值在(1.49±0.61—2.75±0.53),淡水系数(Fc)在(0.08—0.52),淡水区域径长在(150—900μm)。进入第二变化阶段后“生境履历”波动显著,Sr/Ca比值变化可将大洋河刀鲚分为3种模式,第一种是中高值区(半咸水或海水)越冬,繁殖季溯河洄游至低值区(淡水);第二种是长期栖息于中高值区,无溯河洄游现象;第三种是在中高值区和低值区多次转换,DYH 05、19个体最高完成9次转换。Sr面分析结果也与上述Sr/Ca比值结果相同。这三种模式直观地反映出大洋河刀鲚群体“生境履历”的多样性特点。

川西南峨眉山玄武岩中蚀变绿泥石的成分特征及其地质意义

在火山岩和碎屑岩储层中普遍发育大量绿泥石,影响着物性。为查明火山岩中蚀变绿泥石的成因及其对储层物性的影响,本次工作选取川西南峨眉山典型剖面、ZG1井、ZG2井以及YT1井等系列玄武岩样品进行岩相学研究和电子探针微区成分分析。结果显示:玄武岩中绿泥石大致可分为显晶质、隐晶质和微晶3种结晶类型,总体上属于富铁种属的铁斜绿泥石(辉绿泥石)和铁镁绿泥石,形成于富铁的还原环境;隐晶质与微晶和显晶质绿泥石分别受到岩浆期后热液和来自深部的多期次构造热液叠加蚀变的控制,形成主要表现为Fe^(2+)对Mg^(2+)的成分置换,反映流体具有从碱性向弱酸性-中酸性过渡的变化规律。绿泥石的形成过程对火山岩储集空间的影响具有双重作用:岩浆期后热液的充填结晶充填减少了火山岩原生孔隙并降低储层物性,对火山岩储层起到破坏性作用;多期次构造热液的溶蚀迁移沉淀则产生了新的微孔,对火山岩储层起到建设性作用。

松辽盆地砂岩型铀矿铀含量配分比例的半定量分析

钱家店铀矿是位于松辽盆地南部的复成因砂岩型铀矿,受表生淋滤、辉绿岩中低温热液和深部油气等多流体影响,目前铀矿物赋存状态尚有一定争议,铀在矿石内不同矿物中的配分尚不明确。为了进一步明确铀赋存状态和在不同矿物中的配分,计算钱家店矿石中不同矿物中铀的配分比例,本文运用岩矿鉴定、铀化学逐级提取、电子探针和激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)微区原位分析技术开展综合测试分析。明确了钱家店铀矿物的赋存状态,认为钱家店铀矿物以吸附态为主,约占总铀含量的80%,结合态铀矿物或含铀矿物约占比20%。其中吸附态铀矿物主要富集在方解石等碳酸盐矿物中,占总铀含量的47.86%,其次是在黏土矿物中占17.94%,在铁锰氧化物矿物中占12.21%。独立铀矿物是与黄铁矿密切共生的沥青铀矿为主,约占铀总含量的9.07%,另有少量含钛铀矿物和铀石约占5.08%。这种矿石中各碎屑组分中铀的占比量化研究,为矿床地浸开采及资源量计算提供依据。

磁相变材料热膨胀与磁致伸缩效应测试

基于综合物理性能测试系统的低温与磁场环境,采用应变片测试方法开发了磁相变材料热膨胀系数的表征方法,验证了测试结果的可靠性,并开展了磁相变材料LaFe11Co0.8Si1.2负膨胀性能的研究。结果表明:在居里温度处,LaFe11Co0.8Si1.2材料的热膨胀量随温度的升高而减小,这是因为材料发生了铁磁性向顺磁性的磁相变,导致其产生磁致伸缩效应,抵消了原子非简谐振动引起的热胀冷缩,最终导致材料发生负热膨胀现象。

高碳中锰耐磨钢凝固过程溶质微观偏析模型

通过定向凝固、电子探针(EPMA)、Factsage等多种实验与理论计算相结合的手段对中锰耐磨钢凝固过程溶质元素微观偏析行为进行了系统研究.研究表明在定向凝固试验中当拉速为50μm·s-1时,中锰钢的二次枝晶间距平均值为59.77μm;中锰钢凝固过程组织转变为L→L+γ→γ属于奥氏体凝固模式,无包晶反应的发生,也无铁素体相及其他相的出现;中锰钢定向凝固过程中Mn、Cr在枝晶间的含量明显高于枝晶内,表明Mn、Cr元素发生了明显的正偏析行为;通过对各特征参数求解,构建了中锰钢溶质元素微观偏析模型,发现中锰钢定向凝固过程中Mn元素偏析指数与Brody–Flemings模型符合较好,而Cr元素偏析指数与Clyne–Kurz模型分布较为一致.

“雅安绿”图章石的宝石矿物学特征研究

图章石普遍“缺蓝少绿”,“雅安绿”以其明艳的绿色成为近年图章石的重要品种,而迄今为止,关于“雅安绿”图章石相关报道较少,且易与其它绿色图章石相混淆,故本文对“雅安绿”图章石这一品种进行深入研究,为其鉴别提供一定的依据。主要采用X射线粉末衍射、拉曼光谱、扫描电子显微镜、电子探针及紫外-可见光谱对“雅安绿”图章石样品的矿物组成、微形貌特征、化学成分、颜色成因进行测试分析。结果表明,“雅安绿”图章石样品中的绿色基质的矿物组成为白云母,黄色杂质矿物组成主要为白云石和黄铁矿,并含少量的石英、磷灰石和金红石。扫描电子显微镜观察发现,“雅安绿”图章石样品中的白云母呈假六方片状,呈三维空间无序排列;可见自形黄铁矿及完全解理块状的白云石。紫外-可见光光谱分析认为,“雅安绿”图章石样品的翠绿色主要由白云母中微量元素Cr引起。

实验室研究等离子体鞘套测量方法和干预技术

航天飞行器再入大气层时,由于激波加热和热化学防护材料的烧蚀等原因,会在飞行器表面形成致密的等离子体鞘套,从而造成无线电通信信号中断。因此,减轻和消除黑障对飞行器测控安全至关重要。为了解决该难题,本文针对性地发展了适用于等离子体鞘套测量的探针设备和主动干预的技术,并利用实验室等离子体进行了验证。首先,提出了一种静电-微波复合探针,基于探针和飞行器表面曲面共形的优势,可以实时、有效地探测黑障高温流场中的电子密度;进一步,发展了亲电子物质释放实验主动干预方法,地面模拟实验表明该方法可以有效地降低流场等离子体中的电子密度。

地外样品研究中电子探针元素面扫描分析技术的应用

由于月壤等地外样品十分珍贵,在实验室研究中优先使用原位、微区、无损的元素分析方法。电子探针元素面扫描是地外样品研究中常用的分析方法之一,它可获取样品整体或者感兴趣区域的多种元素分布数据,应用于矿物相识别与含量估算,锆石等定年矿物的快速定位,矿物环带、出溶、反应边结构等特殊岩相和矿物接触关系等分析和研究。以嫦娥五号月壤、月球陨石、火星陨石研究为例,介绍目前元素面扫描的应用方法,对比、分析了电子探针面扫描技术与其他面扫描技术的优缺点和适用范围。未来十年,我国将实施一系列月球、火星、小行星等天体采样返回任务。电子探针元素面扫描分析未来将在这些地外样品研究中广泛使用。同时,建议行星科学家围绕所关心的科学问题,合理搭配多种分析方法以实现各种技术优势互补和样品科学价值最大化,服务我国月球与深空探测任务科学产出和行星科学发展。

下庄新桥西铀矿床硫化物地球化学特征及其地质意义

新桥西铀矿床为下庄矿田内的铀矿床之一,位于贵东岩体东部。文章利用电子探针分析技术(EPMA)测定了新桥西铀矿床中黄铁矿、闪锌矿的微量元素组成。数据显示,该矿床中黄铁矿、闪锌矿具富Fe、Zn亏S的特征,其中黄铁矿主要富集Mo、Mn、Cu、Zn、As、Co、Ni、Pb、U;闪锌矿富集Mo、Mn、Fe、Cu、Cd。Cu、Fe、As、Co、Ni、Zn、Pb、Mo及Mn等微量元素可能以矿物包体或类质同象的形式存在于黄铁矿和闪锌矿中;黄铁矿中Co、Ni、Mo、As与U在流体中具相似的地球化学行为,可能具有相似的物质来源。硫化物微量元素特征指示其主要形成于中-浅部、中温成矿环境。结合下庄矿田的成矿地质背景,认为新桥西铀矿床属于典型的岩浆热液型矿床。

球形敏感单元微瞄准形成金属/空气/金属微观界面中的电子输运机理研究

针对惯性陀螺和航空、航天发动机等高端/尖端仪器装备中,深孔、沟槽等内腔体结构的高精度测量对非接触传感方法提出的挑战性需求,展开球形敏感单元瞄准被测件形成金属/空气/金属微观界面中的敏感机理研究。从绝缘介质薄层电子输运机理和绝缘介质性质改变而产生电子输运两个角度,对包括电子隧穿在内的电子输运机理进行形成条件和电流密度特性的分析,揭示球形敏感单元微瞄准形成的金属/空气/金属微观界面中,产生传感电流的电子输运主要机理为福勒-诺德海姆隧穿效应,为探索新原理的三维非接触式纳米传感方法奠定了基础。

45Mn2钢圆管开裂原因

将某45Mn2钢圆坯加工成圆管后,发现其表面存在裂纹。采用宏观观察、化学成分分析、微观分析、电子探针显微分析等方法对钢管表面开裂的原因进行分析。结果表明:异常金属与基体未融合,在对钢管进行磨削处理时,异常金属发生了脱落现象;异常金属与基体的组织、化学成分不同,异常金属压入钢管表面,导致钢管表面发生开裂。

福建梅仙铅锌矿田磁铁矿成因类型与指示意义

梅仙铅锌矿田为闽中地区的大型铅锌矿集区,矿床成矿年代与成因类型尚有争议。梅仙铅锌矿石中普遍发育磁铁矿,通过电子探针分析磁铁矿成分特征,判别其成因类型,对矿床成矿过程进行约束。研究表明,铅锌矿石中磁铁矿成矿可分为3个阶段,不同阶段磁铁矿主量与微量元素含量差异明显;微量元素地球化学特征指示第一阶段磁铁矿属于喷流沉积成因,第二、三阶段磁铁矿为矽卡岩型;不同阶段磁铁矿的成因类型反映了梅仙矿田多期次岩浆活动与成矿作用的特征。