原子荧光法测定高纯石墨粉中的砷、锑

提出以硫脲-抗坏血酸-硼氢化钾反应体系,利用氢化物发生原子荧光法测定高纯石墨粉中的砷、锑含量。讨论了试剂纯度的影响、硫脲一抗坏血酸预还原时间的选择、干扰试验、硼氢化钾溶液的用量等影响。实验结果表明,该方法对高纯石墨粉中的砷、锑含量分析准确、快速、简便,在试验条件下,砷的检出限为0．02mg／kg、锑的检出限为0．007mg／kg;砷的回收率为94％～108％、锑的回收率为96％～108％。采用该方法能满足电池行业用石墨规定的指标。     

信阳上天梯膨润土矿工艺矿物学特征研究

为了使信阳上天梯膨润土矿得到高效合理的开发应用,从应用性基础研究出发,首先开展了上天膨润土矿工艺矿物学特征研究。分析了矿石的矿物组成、结构构造及理化工艺性能,研究了蒙脱石的成分组成、晶体化学特点、层间电荷及其对开发应用的影响。在此基础上,对该矿石进行了高纯钠基膨润土的制备、柱撑蒙脱石试验和高效活性白土的制取。     

某石英砂矿提纯制取高纯石英初探

针对某地石英砂矿石性质特点,经探索性试验研究证明,该石英砂矿采用破碎分级→碱液擦洗→搅拌酸浸→强酸处理→细磨筛分→强酸再处理的提纯工艺流程,可获得二氧化硅含量大于99.99%的高纯石英产品。     

我国高纯石英加工技术现状与发展建议

高纯石英是晶硅、石英玻璃和集成电路基板材料等生产的重要原料,在新能源和新材料等战略性新兴产业具有重要的地位和作用.为了促进我国高纯石英技术发展,介绍了高纯石英的一般概念及其主要品种,并在评述我国高纯石英加工技术现状基础上,针对存在的主要问题,提出加强我国高纯石英矿物资源地质勘查工作、矿物学应用基础研究、提纯加工技术与装备研究、产品质量标准和检测技术研究等具体建议.     

微波在高纯石英提纯实验中的应用

随着水晶资源的日益枯竭,利用脉石英制备高纯石英以代替水晶已经成为一项需要迫切解决的技术问题。高纯石英中,铁杂质是最主要同时也是对产品质量影响最大的有害杂质之一,如何有效地除去脉石英中的铁杂质一直就是高纯石英生产中的难点和重点。当前主要是用酸浸的方法降低铁杂质的含量,主要存在的问题是处理时间较长,同时铁杂质含量也不容易降得更低。通过对微波在高纯石英提纯实验中应用的研究,表明微波可以有效地“打开”石英矿物中含铁的包裹体,不仅能促进含铁杂质矿物的酸浸去除,还可以极大地加快酸浸的速度,促进高纯石英的生产,同时为微波技术在高纯石英生产中的应用奠定了坚实的基础。     

ICP-OES测定锗物料中Ge-As-Cu-Pb-Sb-Sn-Zn的方法研究

锗物料的选冶是高纯锗提纯前必经的重要阶段,详细分析锗物料的主要成分可以对锗物料的进一步选冶提纯起到事半功倍的作用。试验采用ICP-OES法对锗物料中Ge等主要元素进行测定,研究了锗物料试样制备和分解方法的选择和优化,讨论了溶液中硫酸酸度对被测元素谱线强度的影响。方法的检出限为0.0014⁰.0407μg/mL,相对标准偏差小于3%,回收率介于95.22%0.0407μg/mL,相对标准偏差小于3%,回收率介于95.22%¹02.4%。方法得到的Ge结果和现行国家标准方法得到的结果相吻合。结果表明,该方法快速准确、回收率高,是目前较理想的锗物料中Ge-As-Cu-Pb-Sb-Sn-Zn等多元素准确测定方法。     

高纯石英原料特征和矿床成因研究现状综述

高纯石英具有重要的战略地位,是高新技术产业的基础原材料。本文对高纯石英原料的特征和矿床成因研究方法进行了系统的归纳。通过观察石英岩相学特征,分析矿物包裹体及流体包裹体的数量、大小、化学成分、存在形式和分布状态,以及SiO2和微量杂质元素的含量和赋存状态,可以研究高纯石英原料的矿物学特征;通过Ar Ar同位素定年可以计算高纯石英原料矿床的成矿年龄;通过H—O同位素测试,Ti、Al、Ge、Li等微量元素含量分析,可以研究高纯石英原料矿床的成矿物质来源;通过分析流体包裹体的均一温度、盐度、化学组成等特征以及SEM CL微结构观察,可以研究高纯石英原料矿床的成矿作用过程。在此基础上,本论文对我国高纯石英行业的发展提出相关的建议。     

高纯石英原料特征和矿床成因研究现状综述

高纯石英具有重要的战略地位,是高新技术产业的基础原材料。本文对高纯石英原料的特征和矿床成因研究方法进行了系统的归纳。通过观察石英岩相学特征,分析矿物包裹体及流体包裹体的数量、大小、化学成分、存在形式和分布状态,以及SiO2和微量杂质元素的含量和赋存状态,可以研究高纯石英原料的矿物学特征;通过Ar Ar同位素定年可以计算高纯石英原料矿床的成矿年龄;通过H—O同位素测试,Ti、Al、Ge、Li等微量元素含量分析,可以研究高纯石英原料矿床的成矿物质来源;通过分析流体包裹体的均一温度、盐度、化学组成等特征以及SEM CL微结构观察,可以研究高纯石英原料矿床的成矿作用过程。在此基础上,本论文对我国高纯石英行业的发展提出相关的建议。     

高纯石英砂粒度分析与粒度评价体系研究

以中国国家标准(GB/T 6005-2008-R40/3)和国际标准(ISO 565-1990)筛孔尺寸为依据划分高纯石英砂粒级,用筛孔直径d微米单位对数换算值Φ=-log2d进行粒度分组和统计分析,用平均值、标准差和偏度对粒度分布特性予以精确表征,用粒度分布直方图和频率百分图形象地显示粒度分布特征,用累积正态概率图检验分布性质,以此弥补高纯石英砂粒度分布研究和评价体系空白,为高纯石英矿石研究、高纯石英砂制备、高技术石英玻璃熔制工艺以及贸易往来提供统一而精细的粒度评价依据。高纯石英砂最佳粒度特征是平均值应趋近熔制工艺最佳值,σ<0.35,SK→0,正态或近正态分布;不良的粒度分布包括双峰、平顶、细偏和粗偏等。     

玻璃熔片制样X射线荧光光谱法测定矾土中主次量组分

建立了玻璃熔片-X射线荧光光谱测定进出口矾土中主、次量组分的分析方法,用可变α系数校正元素基体效应,同时进行谱线重叠校正。利用高纯化学试剂配制合成标准参考物质,球磨机混匀,熔融玻璃片法制备系列校准样片,用X射线荧光光谱法对样品中的二氧化硅、三氧化二铁、三氧化二铝、氧化钙、氧化镁、氧化钾、五氧化二磷、二氧化钛进行测定。方法回收率为98.1%~111.0%,经国家铝矾土标准物质GBW 07178、GBW 07179验证,结果与标准值基本一致。建立的方法解决了测试过程中标准样品种类和数量不足的难题。     

浙江缙云壶镇盆地一带沸石矿石矿物特征及物化性能分析

运用X射线衍射、扫描电镜形貌研究及微区化学成分分析等手段,对浙江省缙云县壶镇盆地及其外围沸石矿床沸石进行系统研究,确定其矿物组成主要为斜发沸石和丝光沸石,二者可单独产出,也可形成混合型矿石。研究区矿石在成分上属高硅型沸石,SiO2/Al2O3比值接近于8,有害元素Fe,Mn,Ti等质量分数很低。物化性能测试表明,浙江省缙云县壶镇盆地及其外围沸石矿为高品级沸石矿,矿石NH4＋交换容量为163 mmol/100 g～212 mmol/100 g,K＋交换容量为15.73×10-3～19.30×10-3,氮气吸附能力为13.1 ml/g～21.0 ml/g,比表面积测试值为157.17 m^2/g～191.50 m^2/g,具有良好的开发应用前景。     

贵州遵义二叠纪锰矿地球化学特征与沉积环境分析：以遵义谢家坝富锰矿床为例

为分析贵州遵义二叠纪锰矿的沉积环境,对谢家坝锰矿床进行常量元素、微量和稀土元素地球化学研究。研究认为：谢家坝锰矿赋存于茅口组顶部含锰岩系中,可分为下矿层豆状、角砾状菱锰矿、似层状菱锰矿,以及上矿层碎屑状、块状菱锰矿的二元结构矿石类型组合,可广泛代表遵义锰矿的矿石特征。谢家坝锰矿上下矿层之间主量元素和稀土元素含量差异较大,常量元素SiO2、TiO2、S、Fe2O3含量上矿层均大于下矿层,MnO、MgO与 Al2O3之间均呈负相关关系;上矿层Fe/Mn值较高,属高Fe低P型锰矿,而下矿层Fe/Mn值较低,属中低Fe低P型锰矿。上矿层稀土元素PAAS标准化配分后呈现较明显的重稀土亏损、弱的轻稀土富集、右倾配分的特征,具有弱的Ce正异常,类似海底铁锰结核稀土元素特征;下矿层呈现弱的中稀土富集,轻、重稀土亏损,弱的帽式分配特征,具明显的Ce负异常,类似典型深部海水沉积稀土元素特征。微量元素Th/U、Ni/Co、V/Cr、V/（V+Ni）、AU等沉积环境古氧相分析指标和稀土元素PAAS标准化配分模式指示,谢家坝锰矿下矿层是在贫氧-厌氧条件下Mn2+与CO32-直接形成菱锰矿,上矿层在常氧-贫氧环境下Mn3+、Mn4+以氧化物或氢氧化物形式沉淀。     

Investigation on the role of microorganisms in manganese mineralization from Abadeh-Tashk area,Fars Province,southwestern Iran by using petrographic and geochemical data

Hydrothermal manganese and ferromanganese deposits associated with Neyriz ophiolite colored mélange occurred as small ore deposits in the Abadeh-Tashk area, SE of Fars Province, SW Iran. The deposits are found in three types: a) banded syngenetic ores, b) massive boudin and lens shaped diagenetic ores and c) vein and veinlet epigenetic ores. Microtextural, geochemical and mineralogical data associated with petrographic Raman, FTIR and SEM studies indicated that the primary Fe compounds formed series of microbially mediated biomats and Mn compounds were precipitated as an amorphous oxide on an active oxide surface accompanying silica gels. Field relationships between ore and host rock, high Mn/Fe ratio (17.43 to 40.79), ΣLREE, positive Eu and negative Ce anomalies in syngenetic ore types reveal that the ores were formed by hydrothermal fluid in an oceanic floor environment. Manganese was fractionated from iron due to physicochemical changes as well as microbial activities in the sedimentary environment. Microbial remains as filamentous beads with regular circular shapes, vermiform structures, series of Fe-rich biomats, traces of embedded organic material besides trace metals and REE concentrations in Mn ores emphasize the role of microorganisms in Fe and Mn precipitation. Syngenetic mineralization took place under suboxic neutrophilic conditions, while diagenetic processes resulted in variably reduced Fe- and Mn-oxides via organic matter decomposition, forming rhodochrosite as the end product. Braunite formation occurred most probably as a biogeochemically mediated early diagenetic product. Diagenetic and epigenetic Mn ores were formed when primary Mn deposits underwent subsequent diagenetic and remobilization–redeposition events respectively.     

X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素

以钴(钴玻璃粉形式)作内标元素,准确测定全铁含量;加入保护剂硝酸铵和稳定剂碳酸锂,使硫转化为硫酸盐,有效地防止硫的挥发损失。通过条件实验,确立了样品熔融温度和钴玻璃粉的用量。选择经筛选的仪器测定条件,用X射线荧光光谱法同时测定铁矿石中TFe、SiO2、CaO、MgO、Al2O3、TiO2、P、S、Mn、V2O5、As、K2O、Na2O、Cu、Ni等15种主次量元素。采用干扰曲线法对几乎完全重叠的TiΚβ谱线与VΚα谱线进行谱线重叠校正,用理论α系数法校正基体效应。建立的方法可以准确测定全铁和质量分数高达5.29%的S。采用多种标准物质和人工配制标准物质制作工作曲线,可以测定质量分数为5.00%的V2O5及0.1%的As,测定值与标准值符合较好,除低含量钠外方法精密度(RSD)<3.5%,分析误差符合实验质量要求。本法可以快速、准确地测定含砷的钒钛铁矿及含硫高的铁矿石中的主次量元素,满足了日常生产对铁矿石中硫和钒的测定要求。     

鄂尔多斯盆地煤成烃潜力与成气热模拟实验

鄂尔多斯盆地煤的Ｒｏｃｋ Ｅｖａｌ分析结果表明，在肥煤—焦煤阶段，Ｓ１＋Ｓ２达最大值，随后生烃潜力减弱。煤的Ｐｙ ＧＣ分析及热模拟成气实验结果证实煤成气具有３个生气高峰，分别相应于Ｒｏ，ｍ０５％～０７％、１０％～１４％及２５％，表明煤成气具多阶段性的特点。这一规律性的认识有助于煤成气的勘探和开发。同时，随煤级增高，煤成烃特征亦发生有规律的变化：异构烃减少，正构烃增加；类异戊二烯烷烃分布亦存在多变性或多阶段的演化特点；苯系化合物具波动性变化特征。     

Geochemical Characteristics and Genetic Significance of Datangpo‐Type Manganese Ore Deposits during the Cryogenian Period

The Datangpo‐type manganese ore deposits, which formed during the Nanhuan (Cryogenian) period and are located in northeastern Guizhou and adjacent areas, are one of the most important manganese resources in China, showing good prospecting potential. Many middle‐to‐large deposits, and even super‐large mineral deposits, have been discovered. However, the genesis of manganese ore deposits is still controversial and remains a long‐standing source of debate; there are several viewpoints including biogenesis, hydrothermal sedimentation, gravity flows, cold‐spring carbonates, etc. Geochemical data from several manganese ore deposits show that there are positive correlations between Al₂O₃ and TiO₂, SiO₂, K₂O, and Na₂O, and strong negative correlations between Al₂O₃ and CaO, MgO, and MnO in black shales and manganese ores. U, Mo, and V show distinct enrichment in black shales and inconspicuous enrichment in Mn ores. Ba and Rb show strong positive correlations with K₂O in manganese ores. Cu, Ni, and Zn show clear correlations with total iron in both manganese ores and black shales. ∑REE of manganese ores has a large range with evident positive Ce anomalies and positive Eu anomalies. The Post Archean Australian Shale (PAAS) normalized rare earth element (REE) distribution patterns of manganese ores present pronounced middle rare earth element (MREE) enrichment, producing “hat‐shaped” REE plots. ∑REE of black shales is more variable compared with PAAS, and the PAAS‐normalized REE distribution patterns appear as “flat‐shaped” REE plots, lacking evident anomaly characteristics. δ¹³C values of carbonate in both manganese ores and the black shales show observable negative excursions. The comprehensive analysis suggests that the black shales formed in a reducing and quiet water column, while the manganese ores formed in oxic muddy seawater, which resulted from periodic transgressions. There was an oxidation–reduction cycle of manganese between the top water body and the bottom water body caused by the transgressions during the early Datangpo, which resulted in the dissolution of manganese. Through the exchange of the euphotic zone water and the bottom water, and episodic inflow of oxygenated water, the manganese in the bottom water was oxidized to Mn‐oxyhydroxides and rapidly buried along with algae. In the early diagenetic stage, Mn‐oxyhydroxides were reduced and dissolved in the anoxic pore water and then transformed into Mn‐carbonates by reacting with HCO₃^? from the degradation of organic matter or from seawater. In the intervals between transgressions, continuous supplies of terrigenous clastics and the high productive rates of organic matter in the euphotic zone resulted in the deposition of the black shales enriched in organic matter.     

能量色散X射线荧光光谱仪现场快速测定多金属矿中17种组分

直接使用粉末样品,用Minipal 4便携式能量色散X射线荧光光谱仪测定多金属矿样品中的三氧化二铝、氧化镁、二氧化硅、氧化钾、氧化钙、三氧化二铁、硫、铜、锰、锌、铋、锑、铅、镓、银、砷、锡等17种组分,方法简便、快速,用多金属矿石国家一级标准物质验证,分析结果与标准值基本符合;精密度试验表明,各组分的相对标准偏差(RSD,n=12)均小于12%,能够满足矿山和野外现场快速测定的要求。     

Geochemical Behavior of Manganese in Weathering Environments and Its Significance in Exploration

Under and climate conditions the chemical weathering of manganese ores is govermed by the fugacities of O2,CO2 and S2 in the atmosphere and soils.Manganese minerals exhibit solid phase transformations without migration of Fe and Mn.Under tropical and subtropical humid climate condi-tions low-valent Mn is instable and apt to be oxidized into high valency state.High-valent Mn miner-als are stable and easy to form secondary high-grade Mn ores.Secondary concentration is possible for Mn ores in carbonate formations,while those in clastic rocks tend to migrate and may be washed away.Such differences are the main obstacles in prospecting Mn ore deposits.     

Geological and Geochemical Investigation of Three Ophiolite‐Hosted Manganese Prospects,Southeast of Birjand,South Khorasan,East of Iran

The studied ophiolite‐hosted manganese prospects are located in southeast of Birjand, South Khorasan, in the east of Iran. The manganese ores within the ophiolitic sequence in this region occur as small discrete patches, associated with radiolarian chert and shale. Manganese ores in the host rocks are recognizable as three distinct syngenetic, diagenetic, and epigenetic features. The syngenetic manganese ores occurred as bands associated with light‐red radiolarian chert. The diagenetic Mn ores occurred as lenses accompanied by dark‐red to brown radiolarian chert. The epigenetic Mn ores occurred as veins/veinlets within the green radiolarian shale. The major manganese ore minerals are pyrolusite, braunite, bixbyite, ramsdellite, and romanechite showing replacement, colloidal, and brecciated textures. The high mean values of Mn/Fe (15.32) and Si/Al (15.65), and the low mean concentration values of trace elements, such as Cu (85.9 ppm), Ni (249.9 ppm), and Zn (149 ppm), as well as the high concentration values of Si, Fe, Mn, Ba, Zn, Sr, and As in the studied manganese ores furnished sufficient evidence to postulate that the sea‐floor Mn‐rich hydrothermal exhalatives were chiefly responsible for the ore formation, and the hydrogenous processes had negligible role in generation of the ores. The further geological and geochemical evidence also revealed that the ores deposited on the upper parts of the ophiolitic sequence by submarine exhalatives. The intense hydrothermal activities caused leaching of elements such as Mn, Fe, Si, Ba, As and Sr from the basaltic lavas (spilites). After debouching of the sea‐floor exhalatives, these elements entered the sedimentary basin. The redox conditions were responsible for separation of Fe from Mn.     

Mineralogical Characteristics of Unusual Black Talc Ores in Guangfeng County,Jiangxi Province,China

Talc is a hydroxyled, magnesium-rich, layered silicate that has the ideal chemical formula Mg3Si4O10(OH)2. Due to its unique properties, such as softness, chemical inertness, high thermal stability, low electrical conductivity, lamellar habit, adsorption properties, and occurrence of a wide range of particle sizes that can be easily reduced by milling and high specific surface area, talc is widely used in many industries. A stratified deposit of unusual black talc, an occurrence of talc estimated to be more than half a billion tons, was found exposed in the late Neoproterozoic Dengying Formation, located in Guangfeng County, Jiangxi Province, southeastern China. The ores occur primarily as oolitic structures (Fig. 1). The mineralogical and geochemical characteristics of the ores were investigated by using multiple techniques. The ores were found to mainly consist of talc (30%–70%), dolomite, quartz, and magnesite. Most of talc crystals are ultrafine (with an average crystallite size of smaller than 5 μm) and appear as irregular broken or distorted lamellar flakes. The total organic carbon (TOC) content of the black talc ore samples is generally lower than 1.0%. Electron-microprobe analysis (EPMA) revealed low contents of Na, K, Ca and Mn, Fe, Ni, Al in the talc oolitic particles. The talc ores have low contents of toxic elements and relatively high contents of Li and Zn. The infrared spectrum of the black talc is similar to that of white talc from Trimouns (Pyrenees, France), and their Brunauer–Emmett-Teller (BET) specific surface areas, ranging from 15.7 to 23.2 m2/g, is much higher than those of white talc (normally lower than 5.0 m2/g), which may be due to the small size of the talc crystals.