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K-Ar稀释法中~(40)Ar含量的测量需经过样品熔融释气、气体纯化富集、质谱测量等步骤,随着新型设计的双真空加热炉和气体纯化系统的应用,实验流程逐渐由人工操作向自动化程序控制转变。为建立完整的K-Ar稀释法中~(40)Ar含量测量方法,相关参数还需多次条件实验得以确定。本文以空气标准为对象,通过活性炭冷指释放和吸附空气标准,确定活性炭冷指最佳加热释气时间为500s,液氮条件下最佳吸附时间为200s,在此条件下,加热炉熔融产生的~(40)Ar气体可以完全转移和释放,避免发生同位素分馏;根据不同熔融温度下相同质量样品释放~(40)Ar强度,确定黏土矿物、黑云母、白云母等类型样品加热炉熔融温度设置为1400℃,角闪石熔融温度为1500℃,基性岩熔融温度为1550℃,钾长石熔融温度为1600℃,不同类型样品采用对应熔融温度,保证样品完全熔融释气。对10组SK01透长石标准进行测量,得到K-Ar年龄结果与~(40)Ar-~(39)Ar定年标准值相一致,结果表明所得条件参数可满足K-Ar稀释法中~(40)Ar含量的准确测量。 相似文献
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多金属结核富含多种关键战略金属,是重要的深海沉积矿产。多金属结核疏松多孔,具有从海水/孔隙水中吸附痕量金属进而富集成矿的关键材料学特性,其比表面积是成矿作用研究的一个关键参数。目前比表面积测试技术方法成熟,但很少应用于多金属结核的比表面积分析,且由于研究目的不同,样品预处理条件也不同。本文探究了多金属结核BET比表面积测试的预处理条件,为多金属结核富集痕量金属研究提供必要参数。对取自西太平洋、印度洋和大西洋的多金属结核样品,基于低温氮吸附法与静态容量法,采用程序升温、累积加热和粒度对比三种实验技术路线,对多金属结核比表面积分析的预处理温度、时间和试样粒度条件进行了研究。结果表明,程序升温测试在加热到210℃时比表面积测试结果进入平台期,一直持续到350℃;在210℃条件下,以1h为梯度累积加热测试比表面积,样品在累计加热3h后测试结果基本稳定。毫米级的块状试样相较微米级的粉末状试样,其比表面积测试值偏高1.027～28.535m~2/g。研究认为,选取毫米级精度的块状样品在真空状态下210℃加热3h,比表面积测试所得数据能够代表多金属结核的稳定测试结果。该成果为多金属结核成矿作用研究提供了比表面积分析的预处理条件。 相似文献
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1方法的选择对天然水的红同位素分析，最初有浮沉子法，比重法、落滴法等方法，1953年费里德曼采用水与加热的锌反应的方法。1961年克雷格等改用金属铀代替金属锌来制备氢气。目前国内外主要采用锌法和铀法。本实验室在原有锌法的基础上进行了一些改进，由原来的纯锌改为加入微量铅。Zn的熔点为419．4℃，而Ph的熔点较低，为327.3℃。当反应器加热到400℃左右时，Ph已全部熔化，附着在Zn粒的表面。经实验此方法能达到与纯锌法等同的效果，故采用了这种方法。2氢同位素分析样品的制备2．1天然水中的氢同位素分析样品的制备（1）实验装置装… 相似文献
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以云南重楼为实验材料采用正交实验设计方法,对从重楼中提取薯蓣皂甙元的方法--直接提取法、改进酸水解法、加酶水解法、微波加热水解法的工艺条件进行了优化,对比了选定最佳条件下不同提取方法的提取效果.实验结果表明:在实验室务件下.直接提取法中采用无水甲醇为溶剂,最优实验条件为:样品粒度20-40 目、温度80 ℃、提取时间6 h时提取率最高,微波其次.通过对比各种提取方法,对制定从重棱中提取薯蓣皂甙元的工艺具有参考价值. 相似文献
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为了验证现代常用的古玉白沁作伪方法的可行性,对市场上常见的作伪方法进行了验证实验,得到了作伪效果最佳的实验方法,为鉴定古玉白沁提供一定的理论依据,并初步探讨了古玉白沁的成因。实验以闪石玉和蛇纹石玉为原料,采用酸处理、碱处理和热处理等方法分别对样品进行了实验研究。结果表明,采用氢氟酸溅洒法和蜡封斑沁法可达到白色斑沁的效果,采用碱处理法伪作沁色的效果不明显,采用高温热处理方法的效果较理想。对比伪作玉器样品与真品古玉的白沁特征发现,酸处理样品的表面可见均匀分布的蚀坑;碱处理样品有似霜状白沁浮于其表面;热处理样品的表面局部存在火烧裂痕,加热至1000℃时稳定物相为辉石类矿物。 相似文献
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李培忠 《矿物岩石地球化学通报》1992,(4)
80年代末以来,稳定同位素地球化学在实验技术和理论研究方面取得了长足的发展,主要表现在用激光技术加热分解样品供同位素分析测量和同位素分子配分函数比与分馏实验相结合推导新的同位素计温方程两方面。现将其简单介绍如下。 1.稳定同位素实验方法的革新传统的稳定同位素实验方法基本上都是采用对真空系统外加热方法(H同位素例外)使样品直接分解或与化学试剂作用产生气体供质谱分析的。这些方法有两大缺点,一是所需样品量大,特别是对于某些难于分选的试样,人们只好以全岩代替单矿物测定它们的同位素组成;二是样品分析时间长,例如用BrF_5法释放硅酸盐中氧的流程长达24小时(其中高温反应时间在10小时以上),磷酸分解碳酸盐法需在25℃下恒温24小时。这些条件不仅对水、电等环境因素提出了较高的要求,而且不利于快速分析样品。激 相似文献
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分析岩石矿物中的气体化学组成,可为岩石圈地幔的不同地球化学过程、地球内部氧化还原环境以及水在深部地球中的循环等研究提供重要的信息与约束条件。对岩矿样品加热使气体脱出是一种常用的实验手段,使用单石英玻璃管作为样品管,石英玻璃结构中不规则的空隙使得气体在高温下易发生扩散与渗透;由钼、钽坩埚组成的双真空炉管一般用于稀有气体同位素组成分析,较少用于气体化学组成分析,且该装置结构复杂,不易组装拆解,也易被损坏。针对以上问题,本文研制了石英玻璃与金属零件组成的双真空盛样炉管,该炉管具有体积小、易于组装、拆解和移动等特点。在相同的实验条件下与单石英玻璃管进行对照实验。根据实验结果,尤其是H_2浓度的测量结果表明:不论哪种类型的样品在500℃和950℃加热脱气时,应用本文研制的双真空盛样炉管,测量的H_2浓度均高于同等实验条件下应用单石英玻璃管测量的H_2浓度,该双真空炉管的气密性优于单石英玻璃管,有利于获得样品中更加真实的气体化学组成。 相似文献
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对采自我国南方燕山期五里亭花岗岩体中的褐帘石,经偏光显徽镜、电子探针仪、差热仪、X射线等方法进行分析得出,该矿物为变生褐帘石。加热800℃,850℃,950℃,970℃,1100℃退火系列样品的X射线粉晶数据分析得出:1.变生褐帘石X射线粉晶分析的最宜加热温度为800-850℃;2.加热至970℃的退火样品,褐帘石已分解为方铈石、赤铁矿、钙长石,加热到1100℃,褐帘石已渐消失,方铈石、钙长石和赤铁矿成为主要矿物相。 相似文献
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锰结核矿物及其原位复合材料吸氢性能的初步研究 总被引：4，自引：1，他引：4
采自东太平洋中国开辟区的锰结核，主矿物相为钡镁锰矿、钠水锰矿，以及属XRD隐晶质的针铁矿与四方纤铁矿，部分矿物相结构特征与人工合成的纲伙碳管十分相似。在室温中压下采用等容压差法测量了锰结核的气态贮氢能力，测得锰结核样品的吸氢量为0.31%。以乙炔为碳源，在750℃下采用气相沉积法直接在锰结核上成功地催化制备出多壁纳米碳管和纳米碳纤维，同样条件测试这种矿物碳管原位复合材料的吸氢性能，其吸氢能力达到1％左右。保持锰结核矿物结晶结构在加热脱水过程中的稳定性，对提高其贮氢能力至关重要。 相似文献
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Reduction roasting of limonite ores: effect of dehydroxylation 总被引：2，自引：0，他引：2
The effect of pre-calcination in the reducibility of tropical limonite ore, obtained from New Caledonia, was investigated in this study. A series of reduction tests were carried out with pre-calcined and raw limonite ores. The extent of metallisation was determined from nickel and iron which dissolved in ammoniacal solution. Mineralogical transformations that occurred during reduction were analysed using thermal gravimetric, differential thermal analysis (TGA/DTA) and in situ high temperature synchrotron based X-ray diffraction. Bulk mineral analysis of the raw ore was also obtained using neutron diffraction. This study suggests that there is benefit in the pre-calcination of limonite ores. Pre-calcination of the ores which opens the main gangue mineral structure, goethite, allows a rapid interaction between the reductant gases and the nickel species during reduction. The greater nickel metallisation achieved in reduction of pre-calcined ores resulted in higher dissolved nickel whilst reduced raw limonite showed poorer nickel recovery. Reduction of metal minerals was also accompanied by diffusion of nickel into the reduced iron matrix that resulted in the formation of ferro-nickel alloy (Ni3Fe). The formation of this solid solution was monitored by in situ synchrotron based X-ray diffraction and was also reflected by the lower nickel leachability in ammoniacal solution. It was found that incorporation of nickel into the reduced iron oxide resulting from pre-calcination is significantly less in comparison to the diffusion occurring in reduced raw or uncalcined limonite ores. This effect is prevalent in prolonged reduction periods (greater than 20 min), at higher temperatures (>500 °C) and highly reducing conditions (H2/CO2=1:1). This study showed that optimal nickel recovery can be achieved by controlling the incorporation of nickel into the reduced iron structure by pre-calcination of the limonite ore. 相似文献
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微波消解-化学蒸气发生-原子荧光光谱法同时测定铁矿石中的痕量砷和汞 总被引：1，自引：0，他引：1
采用HCl-HNO3混合酸(体积比1∶1)微波消解铁矿样品,在消解后的样品母液中直接加入硫脲-抗坏血酸,预还原五价砷为三价砷,消除铁和其他共存离子对砷、汞测定的干扰,采用化学蒸气发生-双道原子荧光光谱法同时测定铁矿石中的痕量砷和汞。结果表明5%的HCl-HNO3混合酸(体积比1∶1)、20 g/L硼氢化钾溶液能有效保证砷、汞双元素的同时测定,制备的砷、汞标准使用溶液在2～5℃下密闭保存,在245 d内具有稳定性。砷的检出限为0.085μg/L,汞的检出限为0.008μg/L。通过分析5个铁矿石有证标准物质,测定As的相对标准偏差为0.9%～5.5%,回收率为77.7%～105.4%,检测值与标准值吻合;测定Hg的相对标准偏差为1.1%～3.7%,回收率为86.2%～113.2%。本方法是以牺牲汞元素的检出限来实现砷、汞两元素的同时测定,是建立在砷、汞单独测定基础上的一种快速检测方法,经全国不同地区9家实验室采用5个标准样品进行协同实验验证,能够满足日常分析要求。 相似文献
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采用熔融片制样,加入钴元素(Co Kα)作铁的内标,用X射线荧光光谱法测定铁等多种元素。用多种类型铁矿标准样品作为校准,理论α系数内标法及康普敦散射作内标校正基体效应。方法的最大绝对误差AE(TFe)≤0.23%,满足了ISO 9507对TFe分析结果准确度的要求[AE(TFe)≤0.3%]。 相似文献
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Although Mn is one of the major impurities in the economic iron ores from the Bahariya Oasis, information on its modes of occurrence and origin is lacking in previous studies. High-Mn iron ores from El Gedida and Ghorabi–Nasser iron mines were subjected to detailed mineralogical, geochemical, and petrographic investigations using X-ray diffraction (XRD), infrared absorption spectrometry (IR), Raman spectroscopy, X-ray fluorescence (XRF), scanning electron microscopy (SEM), and electron probe microanalyzer (EPMA) to clarify the modes of occurrence of Mn in these deposits and its origin. The results showed that the MnO2 contents range between 0.03 and 13.9 wt.%. Three mineralogical types have been identified for the Mn in the high-Mn iron ores, including: (1) inclusions within the hematite and goethite and/or Mn accumulated on their active surfaces, (2) coarse-grained and crystalline pyrolusite, and (3) fine-grained cement-like Mn oxide and hydroxide minerals (bixbyite, cryptomelane, aurorite, romanechite, manjiroite, and pyrochroite) between the Fe-bearing minerals. The Mn carbonate mineral (rhodochrosite) was detected only in the Ghorabi–Nasser high-Mn iron ores. Since IR patterns of low-Mn and high-Mn samples are almost the same, a combination of XRD analysis using non-filtered Fe-Kα radiations and Raman spectroscopy could be the best way to identify and distinguish between different Mn minerals.Assuming that both Fe and Mn were derived from the same source, the occurrence of high-Mn iron ores at the base of the stratigraphic section of the deposits overlain by the low-Mn iron ores indicated a supergene origin of the studied ores by descending solutions. The predominance of Mn oxide and hydroxide minerals in botryoidal shapes supports this interpretation. The small grain size of Mn-bearing minerals as well as the features of microbial fossils such as spherical, elliptical, and filamentous shapes of the Fe-bearing minerals suggested a microbial origin of studied iron ores.Variations in the distribution and mineralogy types of Mn in the iron ores of the Bahariya Oasis demanded detailed mineralogical and petrographic characterizations of the deposits before the beneficiation of high-Mn iron ores from the Bahariya Oasis as feedstock for the ironmaking industries in Egypt by magnetizing reduction. High Mn contents, especially in the Ghorabi–Nasser iron ore and occurrence of Mn as inclusions and/or accumulated on the surface of the Fe-bearing minerals would suggest a possible utilization of the high-Mn iron ores to produce ferromanganese alloys. 相似文献
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采用X射线荧光光谱、X射线衍射等测试手段,对大冶李德贵冶炼遗址矿冶遗物进行了物理测试、成分分析和物相分析。物理测试结果表明,遗址炼渣的熔融温度高于1280℃;成分分析结果表明,李德贵炼渣中铜含量很低,远低于炼铜渣的铜含量;而其铁含量很高,与欧洲早期铁器时代和罗马时代的块炼铁渣相近;物相分析结果表明,李德贵炼渣的主要物相与炼铜渣没有区别,但炼铜渣中发现一些铜氧化矿和硫化矿。结合对其他冶炼遗物的分析,可以初步判断该冶炼遗址是一处炼铁遗址。工作台面上发现的炼渣与铁矿石的混合物,表明古人很可能已将炼渣回收利用,与铁矿石原料一起回炉冶炼。 相似文献
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微波消解-电感耦合等离子体质谱法测定铁矿石中15个稀土元素 总被引：6，自引：5，他引：1
分析地质样品中稀土元素的含量,现有的方法都受到基体干扰和共存元素干扰,电感耦合等离子体质谱(ICP-MS)已在痕量元素分析中得到广泛应用,通过条件优化可准确测定稀土元素。本文建立了ICP-MS同时测定铁矿石中钇镧铈镨钕钐铕钆铽镝钬铒铥镱镥15个稀土元素的方法,样品用盐酸、硝酸和氢氟酸高温密闭消解,消解完全后转移定容,在线加入103Rh、115In、185Re内标液进行测定,方法回收率为95%~104%,精密度(RSD)≤3.5%。对12个国家24个代表性主产区进口的铁矿石样品进行检测,分析其稀土元素的配分模式特征为右倾型轻稀土富集,现阶段的进口铁矿粉多为多产区复合配矿。本方法较其他传统方法大幅降低能耗,提高了分析效率,初步探讨的稀土元素丰度特征可为研究主产区铁矿石的矿床成因、提高我国烧结球团矿的加工工艺提供依据。 相似文献
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磁异常小波多尺度分解及危机矿山的深部找矿: 以大冶铁矿为例 总被引：22，自引：2，他引：20
大冶铁矿是多年开采老矿山, 浅部的铁矿已开采殆尽, 为了进一步挖潜, 利用小波多尺度分析方法, 将磁异常分解到不同尺度空间, 结合谱分析方法解释深部盲矿体.理论模型和19-1勘探线的实际资料的小波分解结果表明, 该方法比常规的空间延拓、高次导数、匹配滤波等方法要好.通过处理与解释指出了西段(尖林山、龙洞、铁门坎) 五阶小波细节已无剩余异常存在, 推测在1000m以下已没有大型的铁矿体存在.但在东段(尖山、犁头山) 五阶小波细节还有剩余异常, 推测1000m深部可能还有铁矿体.根据小波多尺度分析方法结合人机交互反演推断15~12线有铁矿体, 2005年9月布钻验证, 在15~1线打到30多米厚磁铁矿体. 相似文献
19.
Rare earth elements in apatite and magnetite in Kiruna-type iron ores and some other iron ore types 总被引：6，自引：0，他引：6
An investigation of the content and distribution of REE in apatite and magnetite in the iron ores of Kiruna type and some other iron ores is presented. REE in apatite and magnetite in different ore types show characteristic patterns which are related to different modes of formation of the ores.The magnetite-apatite iron ores of the world can be divided into two types: (a) Kiruna iron ores proper which occur in volcanic rocks, and (b) iron ores connected with deuteric processes and/or related to intrusive rocks. Apatite of the Kiruna ores proper in Fennoscandia (e.g. Kiirunavaara, Malmberget and Grängesberg) shows a common pattern with 2000–7000 ppm REE, a weak to moderate LREE/HREE fractionation and negative Eu anomalies. In the Kiruna area, apatite of the main, P-poor ores and of the later, hydrothermal-exhalative P-rich ores, have the same REE distribution which indicates a common source. There is a similar REE distribution in magnetite-apatite trachytic-rhyodacitic host rock which confirms a close magmatic relationship. Apatite in phosphorites (such as the Paleoproterozoic Påläng deposit in northern Sweden) has a different composition (< 1000 ppm REE with Ce depletion) which excludes a sedimentary origin of the Kiruna apatite.Apatite in other volcanogenic magnetite-apatite ores outside Fennoscandia differ by a stronger LREE/HREE fractionation and by a medium to large Eu depletion, partly indicating a relationship to alkaline intrusions. The Avnik apatite, Turkey, shows a weak differentiation in combination with a pronounced negative Eu anomaly, indicating provenance from silicic magmatic sources.The REE pattern of apatite in the deuteric-hydrothermal apatite-bearing iron ores is in general similar to that of apatite in the Kiruna iron ores proper. The similarity indicates a common process of formation for both ore types.The apatite-iron ores of the Kiruna type proper were formed by a late-magmatic differentiation. The ores of the Kiruna area are, in similarity with some other magnetite-apatite ores, emplaced along regional fracture-fault lines and close to an older basement. In general the REE pattern of apatite in the different deposits shows an affinity to alkaline or sub-alkaline magmas, indicating a rifting environment. The alkaline, trachytic volcanics hosting the Kiruna ores in northern Sweden are clearly related to an extensional setting where rifting was important. A probable source for this large-scale ore-forming process was partial melting of deep-seated rocks. The ores evolved in an intracontinental setting with magma generation caused by underplating of older crust.The process giving rise to magnetite-apatite ores of the Kiruna type has occurred during the time span from Paleoproterozoic to Tertiary. The Proterozoic ores occur mainly in cratonized areas, whereas the younger ones occur in fold belts. The amount of ore formed in post-Proterozoic time is as large as that formed in Proterozoic time. 相似文献
20.
Chemical analysis for major and trace elements have been performed on 30 Swedish Precambrian iron ores and on some from Iran and Chile. The Swedish ores consist of apatite iron ores, quartz-banded iron ores, skarn and limestone iron ores from the two main ore districts of Sweden, the Bergslagen and the Norrbotten province. Some Swedish titaniferous iron ores were also included in the investigation. The trace element data show that the Swedish ores can be subdivided into two major groups: 1. orthomagmatic and exhalative, 2. sedimentary. Within group 1 the titaniferous iron ores are distinguished by their high Ti-contents. From the ferride contents of the Kiruna apatite iron ores, the ores are considered to be mobilization products of skarn iron ores from the Norbotten province. 相似文献