地质样品铜、铁、锌同位素标准物质的研制

合适的标准物质是进行同位素准确分析的基础和关键,本文介绍了基于地质样品的铜、铁、锌同位素分析标准参考物质的研制过程.所研制的标准物质为CAGSR-1,用于该标准物质研制的原始样品为玄武质组分的岩石成分分析国家标准物质GBW07105.按照国家一级标准的要求,对该标准物质进行了严格的均一性、稳定性检验和同位素定值分析.标准物质CAGSR-1的主要特性量值δ65Cu、δ56Fe、δ66Zn的推荐值及95%置信水平的不确定度为:δ65CuSRM976(‰)=0.10±0.02、δ56FeIRMM014(‰)=0.12±0.02、δ66ZnRomil(‰)=7.45±0.01.该标准物质可用于地质与环境样品铜、铁、锌同位素测定中化学流程评价和验证、质谱仪的校正及整个过程的分析质量控制.     

胃肠酸度下中药及补铁制剂中铁活性的影响研究

在人体胃肠液的酸度条件下,采用正辛醇-水分配体系模拟药物在人体肠胃中的分配情况,研究了中药和补铁制剂中铁的形态及其在人体内的吸收情况,并探讨了中药不同比例的配伍、胃肠酸度及还原性物质的存在对水溶态铁和醇溶态铁的影响。结果表明,药物溶液中的铁形态与药物本身特性和配伍情况有关,酸度及配伍对药物中铁的溶出率和溶液中铁的形态有较大影响,人体对铁的吸收与胃肠酸度和还原性物质的存在有关。     

金矿石化学物相分析标准物质的研制

介绍了金矿石化学物相分析标准物质的研制工艺及技术关键，列出了单体金、连生体金、硫化物包裹金、其他矿物包裹金及总金的原始数据和定值数据。经9个实验室共同分析协作，研制的5个标准物质已被国家质量监督检验检疫总局批准为国家一级标准物质。该系列标准物质主要用于金矿石化学物相分析质量监控、分析方法评价等。     

江汉平原东北部地区高铁锰地下水成因与分布规律

肖港地区位于江汉平原东北部,属于大别山连片贫困区和贫水区,地下水资源较贫乏,且地下水水质不佳,水中铁锰离子含量普遍超过了国家饮用水标准。为查明高铁锰地下水成因及空间分布规律,服务区内地下水开发利用及安全供水问题,系统采集区内岩石、土壤和地下水样品,测试岩土与地下水中铁锰的含量,分析地下水中铁锰含量与含水层沉积物的铁锰含量、地下水的氧化还原条件和酸碱度之间的关系。结果表明:江汉平原东北部地区地下水中铁锰超标现象普遍存在,其中锰的超标率大于铁,第四系孔隙潜水超标最严重,铁锰最大浓度分别达到44.88 mg/L和19.21 mg/L。研究区岩土中铁锰氧化物为地下水中铁锰提供了物质来源,弱酸性、强还原环境为沉积物中铁锰的溶解释放提供了有利条件,总体上从研究区东西两侧（补给、径流区）向中部第四系孔隙潜水含水层（排泄区）,沿地下水流向Eh值、pH值逐渐减小,铁锰含量逐渐增大,形成北北东向带状分布的高铁锰地下水区。     

敦煌某地铁矿中磁性铁的化学物相分析

本文选用HAC—H_2O_2和HCl—NaHCO_3作为选择性溶剂,对敦煌某地铁矿中磁性铁的化学物相分析进行了研究,将磁性铁物相从传统1项细化为3项,测定了磁性铁相态中磁黄铁矿、假象赤铁矿、磁铁中铁的含量。使用国家标准物质GBW07272对方法进行了评价,分析结果与标准值或参考值吻合良好(RE为0.28%~4.75%,RSD为0.13%~5.59%)。方法简单、准确。     

应用磁测法快速检测石英砂中铁含量的研究

为了快速检测石英砂中铁含量，通过对安徽省凤阳县灵山工业园区30个湿法石英砂样品磁学参数和代表性样品中磁性离子含量的测量以及石英砂中铁含量与磁学参数相关关系的研究，提出石英砂中铁含量的磁学检测方法。通过在高纯石英砂中掺入不同质量磁选物的合成实验建立石英砂的磁化率(χ)、饱和等温剩磁(SIRM)与铁元素含量之间的标准曲线方程，合成实验结果显示石英砂的磁化率与铁含量在143.3×10^-6～500.0×10^-6范围内呈线性关系，相关系数R²=0.994 5,饱和等温剩磁与铁含量在67.9×10^-6～500.0×10^-6范围内呈线性关系，相关系数R²=0.999 2。实例检测结果显示，应用χ和SIRM测量石英砂中铁含量与应用分光光度法测量相比，相对误差分别在-9.83%～3.03%之间和-4.91%～2.42%之间，说明采用磁测法测量石英砂中铁含量是可行的，测量精度良好，采用SIRM测量精度较χ高，对石英砂进行700℃高温处理后，测量精度会增加。该研究为石英砂中铁含...     

郭山高岭土铁钛赋存状态的分析电子显微术研究

使用分析电子显微术对福建郭山高岭土中铁、钛元素的赋存状态进行了研究。结果表明,高岭土中铁钛的赋存状态分为两类,一类为参加到粘土矿物晶格中的铁和钛,简称为结构铁、结构钛;另一类为游离出现或吸附在高岭矿物(高岭石和埃洛石)颗粒表面的铁、钛矿物。查明了在全铁和全钛中,结构铁和结构钛仅占少数,大部分以铁、钛独立矿物形式出现。从而确定了可将高岭土粘粒级(<2μm)中铁、钛含量降低到的最低限度,这便为提高高岭土品级和经济价值提供了可靠的依据。     

中国与世界铂族元素地球化学标准物质评介

铂族元素分析一直是地质材料分析中最棘手的任务之一,是铂族金属矿产资源勘查、评价和相关研究工作的瓶颈。铂族元素标准物质作为铂族元素分析的计量标准,在分析质量监控、分析仪器校准、分析方法评价和仲裁分析中发挥着重要作用。笔者等评介了我国研制的超基性岩和铬铁矿铂族元素标准物质、铂族元素地球化学标准物质、铂族元素矿石标准物质和海山富钴结壳铂族元素标准物质共4个系列21个标准物质,也给出了其他地球化学标准物质中铂族元素的定值数据;并与南非、加拿大、俄罗斯和岩石矿物分析标准国际工作组(GIT-IWG)研制的13个铂族元素标准物质及其他国际地球化学标准物质中铂族元素的数据进行了对比。这些标准物质的研制与应用将大大提高铂族元素分析数据的可靠性,为我国和世界铂族金属矿产资源勘查、评价及研究提供了有力的技术支撑。     

聚硅氯化铝铁（PSAFC）絮凝剂的形态分析

通过对聚硅氯化铝铁水解共聚物的合成制备及水解共聚过程PH变化的研究，对铝铁共物的化学形态、二氧化硅的加入和碱化度B对铝铁共聚物的影响进行了研究和讨论；并应用Ferron配合逐时比色法对聚合物中铁的形态进行了表征，为深入研究聚硅氯化铝铁铁奠定了理论基础。     

用于多接收器等离子体质谱测定的铁铜锌同位素标准溶液研制

近十来年铁铜锌同位素研究已经成为热门研究领域,铁铜锌同位素分析方法日趋成熟,但是铁铜锌同位素标准物质却十分匮乏。目前欧盟参考物质及测量研究所(IRMM)有1个铁同位素标准物质和1个锌同位素标准物质,前者售罄,后者价格昂贵;美国国家标准局(NIST)有1个铜同位素标准物质。为了适应我国铁铜锌同位素研究的发展,本文使用铁铜锌元素浓度标准溶液作为备选标准溶液研制了铁铜锌三个同位素标准溶液(CAGS-Fe、CAGS-Cu和CAGS-Zn)。三个备选标准溶液经过F检验均匀性良好;在38个月内δ56Fe、δ57Fe、δ65Cu、δ66Zn和δ68Zn值没有显著性变化,具有良好的稳定性;主要特性值的推荐值及95%置信水平的不确定度为:CAGS-Fe,δ56FeIRMM014(‰)=0.80±0.05,δ57FeIRMM014(‰)=1.20±0.10;CAGS-Cu,δ65CuIRMM976(‰)=0.57±0.06;CAGS-Zn,δ66ZnIRMM3702(‰)=-0.77±0.10,δ68ZnIRMM3702(‰)=-1.55±0.13。本文研制的标准溶液可用于多接收器等离子体质谱仪测定铁铜锌同位素时的仪器校正和质谱分析过程监控,对于不同实验室的测试数据对比具有重要意义。     

Composition and Assemblage Characteristics of Magnetic Minerals in Layer S_(5-1) of Xifeng and Duanjiapo Sections

Magneticmineralsintheloess paleosolseriesaccountforabout 1 % -2 %ofthetotal (LiuTungshengandZhangZhonghu ,1 962 ) .Duetotheiraerolianorigin ,themagneticmineralsarecomplicatedincomposition ,largeingrainsizerange ,andsignificantlydifferentincrystallinity .Asaresult,researchonthesemagneticmineralswouldbesetwithalotofdifficulties.Previousre searchersemployedopticalmicroscopic ,X raydiffractionandM ssbauerspectrometrictechniquestostudythemagneticmineralsintheloess paleosolseries,andchieflyontheb…     

The Experimental Study of Iron Sulfide Mineral Evolution Under Thermal Sulfurization Condition

Iron sulfide minerals are widely distributed, of which characteristics had the identification significance of formation environment. Previously, there were more research on iron sulfide minerals under hydrothermal condition, and few studies under volcanism formation condition. To simulate volcanic mineralization, the study of different temperature from 250 to 410℃ , different iron sulfur ratio from Fe:S=2∶1 to 1∶8, and two different sources of iron, reduced iron powder (Fe) and ferrous sulfide (FeS), on iron sulfide mineral evolution was investigated under thermal sulfurization condition. By using scanning electron microscopy (SEM), X-ray diffraction (XRD) and other methods, the morphology, composition and structural characteristics of the products were observed and analyzed.     

In situ iron isotope ratio determination using UV-femtosecond laser ablation with application to hydrothermal ore formation processes

The feasibility of in situ stable Fe isotope ratio measurements using UV-femtosecond laser ablation connected to a multiple-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) has been investigated. Different types of matrices, independently determined by solution MC-ICP-MS after chromatographic separation of Fe, have been analysed by laser ablation using the isotopically certified iron reference material IRMM-014 as the bracketing standard. The samples have been pure iron metal (JM Puratronic), Fe-meteorites (North Chile, Glenormiston and Toluca), the meteorite phases kamacite and taenite in Toluca and Fe-sulphides. Furthermore, Fe isotope ratios from hydrothermal hematite, siderite and goethite from an old mining area in the Schwarzwald, Germany, and of magnetite from the metamorphic Biwabik iron formation have been determined. The results show that a precision of better than 0.1‰ (2 sigma) can be achieved with laser ablation and that all the results obtained agree with those determined by solution ICP to better than 0.1‰. This precision and accuracy is achievable in both raster and spot ablation mode. A matrix-matched bracketing standard is not required , and all these materials can be measured accurately against a metal standard. The hydrothermal minerals show significant Fe isotope zonations. In some samples the range of δ⁵⁶Fe in a single aggregate encompasses the entire spectrum of ratios found by bulk solution analyses in multiple samples distributed over the whole mining district. For example, isotopic zonations found in secondary fibrous hematites show a continuous change in the δ⁵⁶Fe values from −0.5‰ in the core to −1.8‰ in the rim. Primary hydrothermal siderite shows the reverse pattern with lighter values in the core than in the rim. While the siderite is thought to record primary fluid histories, the hematite pattern is interpreted as a reworked isotopic signature generated by oxic dissolution of primary zoned siderite and immediate close range re-precipitation of the oxidized Fe. Abrupt changes are documented for secondary goethite showing a distinct overgrowth that is 0.4‰ lighter than the core of the grain. If indeed Fe isotopes in secondary minerals from hydrothermal ore deposits record the initial isotopic signatures of their precursor minerals, and these in turn record hydrothermal fluid histories, then the tools are in place for a detailed reconstruction of the deposit‘s genesis. We expect similar observations from other Fe-rich deposits formed at intermediate and low-temperatures (e.g. banded iron formations). Laser ablation now provides us with the spatial resolution that adds a further dimension to our interpretation of stable Fe-isotope fractionation.     

铁同位素体系及其在矿床学中的应用

本文报道了世界范围内不同含铁矿物的Fe同位素组成,进一步了解了铁同位素在不同含铁矿物中的基本分布特征;系统总结了铁同位素在不同储库和不同类型矿床中的分布特征,构筑了铁同位素体系的基本框架;结合最新的研究成果,较全面地总结了铁同位素在矿床学领域的应用,得出了铁同位素可以用来示踪流体出溶、流体演化、表生蚀变作用和成矿物质来源的基本认识。在流体出溶过程中,相对于岩体,出溶的流体富集铁的轻同位素;成矿流体体系的演化过程中,矿物的结晶沉淀会导致铁同位素发生分馏,随着Fe(III)矿物的结晶沉淀,流体逐渐富集铁的轻同位素,随着Fe(II)矿物的结晶沉淀,流体逐渐富集铁的重同位素,随着矿物的结晶沉淀,流体的Fe同位素组成随时间发生演化;在成矿后的表生蚀变作用过程,高温蚀变作用形成的产物相对于原矿物富集铁重同位素,低温蚀变作用形成的产物基本保留了原矿物的铁同位素组成;Fe同位素在示踪成矿物质来源具有应用潜力,流体出溶、流体演化等重要成矿作用过程中Fe同位素组成的变化规律是利用Fe同位素示踪Fe来源的关键所在。     

河水入渗过程中近岸带地下水中砷的形成与影响因素研究

沈阳黄家水源地是我国北方地区典型的傍河地下水水源地,近岸带地下水中铁(Fe)、锰(Mn)、砷(As)含量严重超标。为查明地下水中As的来源与影响因素,对研究区河水、地下水以及土壤样品进行采集与测试,分析了水样常规指标与碳硫稳定同位素、土样中典型矿物、砷的含量及赋存形态。结果表明,研究区河水中As含量很低,而地下水中As含量普遍超标。河水入渗初期,氧化性河水使部分含As矿物发生氧化而释放As;随着河水入渗,地下水向还原环境转变,含As的Fe/Mn矿物发生还原性溶解,地下水中As含量逐渐升高。研究区典型矿物有黄铁矿、菱铁矿、软锰矿、赤铁矿、针铁矿、菱锰矿等,通过可交换态砷解吸、有机质结合态砷氧化、铁锰氧化物结合态砷还原性溶解等,介质中的As释放至地下水中。地下水中As含量与酸碱度(pH)、氧化还原电位(Eh)呈一定负相关,与溶解有机碳(DOC)、 {\mathrm{HCO}}_3^{-}、Fe、Mn含量呈正相关。     

Quantitative mineralogical and chemical assessment of the Nkout iron ore deposit,Southern Cameroon

The Nkout deposit is part of an emerging iron ore province in West and Central Africa. The deposit is an oxide facies iron formation comprising fresh magnetite banded iron formation (BIF) at depth, which weathers and oxidises towards the surface forming caps of high grade hematite/martite–goethite ores. The mineral species, compositions, mineral associations, and liberation have been studied using automated mineralogy (QEMSCAN^®) combined with whole rock geochemistry, mineral chemistry and mineralogical techniques. Drill cores (saprolitic, lateritic, BIF), grab and outcrop samples were studied and divided into 4 main groups based on whole rock Fe content and a weathering index. The groups are; enriched material (EM), weathered magnetite itabirite (WMI), transitional magnetite itabirite (TMI) and magnetite itabirite (MI). The main iron minerals are the iron oxides (magnetite, hematite, and goethite) and chamosite. The iron oxides are closely associated in the high grade cap and liberation of them individually is poor. Liberation increases when they are grouped together as iron oxides. Chamosite significantly lowers the liberation of the iron oxides. Automated mineralogy by QEMSCAN^® (or other similar techniques) can distinguish between Fe oxides if set up and calibrated carefully using the backscattered electron signal. Electron beam techniques have the advantage over other quantitative mineralogy techniques of being able to determine mineral chemical variants of ore and gangue minerals, although reflected light optical microscopy remains the most sensitive method of distinguishing closely related iron oxide minerals. Both optical and electron beam automated mineralogical methods have distinct advantages over quantitative XRD in that they can determine mineral associations, liberation, amorphous phases and trace phases.     

Mineralogy,geochemistry and origin of Mn in the high-Mn iron ores,Bahariya Oasis,Egypt

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.     

Iron isotope fractionation during hydrothermal ore deposition and alteration

Iron isotopes fractionate during hydrothermal processes. Therefore, the Fe isotope composition of ore-forming minerals characterizes either iron sources or fluid histories. The former potentially serves to distinguish between sedimentary, magmatic or metamorphic iron sources, and the latter allows the reconstruction of precipitation and redox processes. These processes take place during ore formation or alteration. The aim of this contribution is to investigate the suitability of this new isotope method as a probe of ore-related processes. For this purpose 51 samples of iron ores and iron mineral separates from the Schwarzwald region, southwest Germany, were analyzed for their iron isotope composition using multicollector ICP-MS. Further, the ore-forming and ore-altering processes were quantitatively modeled using reaction path calculations. The Schwarzwald mining district hosts mineralizations that formed discontinuously over almost 300 Ma of hydrothermal activity. Primary hematite, siderite and sulfides formed from mixing of meteoric fluids with deeper crustal brines. Later, these minerals were partly dissolved and oxidized, and secondary hematite, goethite and iron arsenates were precipitated. Two types of alteration products formed: (1) primary and high-temperature secondary Fe minerals formed between 120 and 300 °C, and (2) low-temperature secondary Fe minerals formed under supergene conditions (<100 °C). Measured iron isotope compositions are variable and cover a range in δ⁵⁶Fe between −2.3‰ and +1.3‰. Primary hematite (δ⁵⁶Fe: −0.5‰ to +0.5‰) precipitated by mixing oxidizing surface waters with a hydrothermal fluid that contained moderately light Fe (δ⁵⁶Fe: −0.5‰) leached from the crystalline basement. Occasional input of CO₂-rich waters resulted in precipitation of isotopically light siderite (δ⁵⁶Fe: −1.4 to −0.7‰). The difference between hematite and siderite is compatible with published Fe isotope fractionation factors. The observed range in isotopic compositions can be accounted for by variable fractions of Fe precipitating from the fluid. Therefore, both fluid processes and mass balance can be inferred from Fe isotopes. Supergene weathering of siderite by oxidizing surface waters led to replacement of isotopically light primary siderite by similarly light secondary hematite and goethite, respectively. Because this replacement entails quantitative transfer of iron from precursor mineral to product, no significant isotope fractionation is produced. Hence, Fe isotopes potentially serve to identify precursors in ore alteration products. Goethites from oolitic sedimentary iron ores were also analyzed. Their compositional range appears to indicate oxidative precipitation from relatively uniform Fe dissolved in coastal water. This comprehensive iron isotope study illustrates the potential of the new technique in deciphering ore formation and alteration processes. Isotope ratios are strongly dependent on and highly characteristic of fluid and precipitation histories. Therefore, they are less suitable to provide information on Fe sources. However, it will be possible to unravel the physico-chemical processes leading to the formation, dissolution and redeposition of ores in great detail.     

57Fe M?ssbauer spectroscopy study of organic rich sediments (source rocks) from test well CT-1, Chinnewala structure of Jaisalmer basin, India

~(57)Fe M?ssbauer spectroscopic study was carried out on the organic rich sedimentary samples collected at different depth intervals from newly drilled test well Chinnewala Tibba-1(CT-1) located in Jaisalmer Petroliferous basin India. It is found that iron is mainly distributed in high spin Fe3tand Fe2tstate in clay minerals. The plot of Fe2t/(Fe2tt Fe3t) indicates the presence of poor redox conditions in the samples.Results obtained are also compared with those already reported in the literature. This comparison shows that there may exist a correlation between prospecting of the basin, the redox environment in sediments and the nature of iron bearing minerals distributed in the sedimentary sequence.