X射线衍射全谱拟合法分析蓝晶石的矿物含量

蓝晶石矿物定量分析通常采用的化学物相法分析流程繁琐,易受同质异象矿物和难熔矿物的干扰;采用X射线衍射内标法需要提纯矿物绘制标准曲线,但矿物包体的存在使得获取纯净单矿物成为难题;由于不同矿区蓝晶石矿物成分之间存在着差异性,以上两种方法都仅仅适用于同一矿区样品的矿物定量分析。为简化分析流程,提高测试效率,本文采用X射线衍射(XRD)全谱拟合法对蓝晶石国家二级标准物质和野外样品进行分析,并与RIR法、绝热法和K值法等衍射定量方法及化学分析结果进行了比较验证方法的可靠性。结果表明:全谱拟合法无需采用标准物质,也不用引入内标物,一次扫谱分析能获得样品中所有成分的信息,操作简单,能有效降低择优取向对衍射定量结果的影响;对于含量大于5%的矿物,组分分析结果的绝对误差小于1%,显著低于绝对误差允许限;采用Highscore和Jade两种衍射数据处理软件获得的定量结果吻合度高,目标矿物蓝晶石分析结果的双差均小于0.8%,相对偏差小于2.5%;蓝晶石的加标回收率在95.3%～101.0%之间,能实现不同矿区蓝晶石矿的快速定量分析。     

土壤中高岭石的X射线衍射全谱拟合定量分析方法研究

本文通过提纯高纯度石英、方解石、高岭石,配置了三种已知矿物成分含量的土壤模拟样品（高岭石、石英二相模拟土壤样品,高岭石、石英、方解石三相模拟土壤样品,高岭石、自然土壤混合样品）,利用X射线衍射TOPAS全谱拟合定量分析方法对配制的9组高岭石、石英二相模拟土壤样品,9组高岭石、石英、方解石三相模拟土壤样品,9组高岭石、自然土壤混合样品三种系列覆盖4个矿物梯度的模拟土壤实验样品进行矿物定量分析,成功对比了其矿物理论含量与测试含量。通过对不含高岭石系土壤和含高岭石系土壤加标高岭石的方法,验证了X射线衍射全谱拟合定量分析法可以应用于土壤高岭石定量分析的稳定性与准确性。     

X射线粉晶衍射仪在千枚岩鉴定与分类中的应用

以往千枚岩是依据显微镜下观察岩石结构构造及矿物成分进行分类定名.实际上千枚岩中鳞片状绿泥石和黑云母以及微粒石英、钾长石和斜长石在岩石薄片中区分十分困难.为了准确鉴定千枚岩中鳞片状和微粒状造岩矿物种类及其相对含量,利用X射线粉晶衍射半定量技术对19件千枚岩岩石进行分析测试.研究结果显示：利用云母、绿泥石、石英、钾长石和斜长石等造岩矿物X射线衍射峰的明显差异,结合X射线衍射全谱拟合半定量分析测试技术,能快速检测云母、绿泥石、石英、钾长石和斜长石等造岩矿物种类与含量.实践证明,将千枚岩岩石野外观察、岩石薄片鉴定和X射线粉晶衍射技术紧密结合起来,才能准确定出千枚岩岩石的名称.     

花岗岩类主要造岩矿物的X射线衍射定量分析方法的研究

本文介绍了X射线衍射无标样解联立方程测定多元物相含量的方法和原理。用X射线衍射、求积仪、化学分析三种方法同时对十三个花岗岩样中的主要造岩矿物的含量进行了测定,结果比较一致。这证明用X射线衍射无标样的解联立方程法测定多元物相的含量是可行的。 由于以往的X射线定量分析需提取纯样作标样,但有些样品提纯相当困难,从而使X射线定量分析工作受到一定限制。本文采用无标样解联立方程的方法,仅在被测样品中加入合适的参考物质,测出各物相的参考常数K,便可测定各物相的重量百分数。正确测定花岗岩类的主要造岩矿物的含量,不仅能为花岗岩类的正确命名提供依据,而且对花岗岩的演化和成因的探讨也很有意义。以前这项繁杂的工作,主要用求积仪和化学分析的方法来进行,既费工又费时,其结果往往不理想。尤其是对斑状和细粒花岗岩,求积仪法难以测定,只能靠目估。为此,作者开展了用X射线衍射法测定花岗岩中主要造岩矿物含量的研究。通过对十三个花岗岩样的测试证明,用无标样解联立方程法,测定花岗岩中多种物相的含量是行之有效的。     

蛇纹石物相X射线衍射定量分析精密度评估方法的探讨

蛇纹石是一种重要的矿物材料和化工原料,广泛应用于化工、农业、建材、冶金及环保等领域,中国由于对蛇纹石矿开采品位要求较高,形成了较多的弃尾矿,造成了大量的浪费和环境污染。根据弃尾矿中蛇纹石的不同含量,进而生产不同的工业产品,可改善生态环境,为蛇纹石企业寻求到新的发展出路。这些工作的基础是能够对蛇纹石进行快速和精确的测定。目前蛇纹石矿石的测定方法采用行业标准《蛇纹石矿石分析方法》(HG/T 3575—2006)进行,其分析步骤繁琐,分析时间过长,现有的检测方法已不能满足市场和企业的急需,而长期以来利用X射线衍射进行的蛇纹石定量分析,其分析方法的精密度一直没有得到规范的量化控制,实验室之间的精密度比对也缺乏相应的依据。为进一步提高X射线衍射法检测蛇纹石矿物含量的水平,本文根据GB/T 6379.2—2004标准中的要求,首先通过挑选加配制共10个不同含量的样品,进行均匀性检验,当检测结果F实测值均小于F临界值,表明试验样品是均匀的,然后选择8家实验室使用检验后合格的样品进行精密度协作试验,对得到的测试结果进行格拉布斯检验和柯克伦检验,通过检验的数据才能参与精密度参数的计算,最终获得X射线衍射标准曲线法和K值法的精密度与含量之间的数学函数关系。实验结果表明：本次协作试验的数据,全部通过格拉布斯检验和柯克伦检验,均可参与精密度参数的计算,结果也侧面证明了不同实验室不同仪器测试的结果一致性较高。精密度参数的计算结果显示：在X射线衍射标准曲线法和K值法重复性限和再现性限数据中,含量最低的样品,其重复性限和再现性限也最小,验证了X射线衍射对物相定量分析的误差主要源自于样品的均匀性误差这一特征。证实了在所有影响X射线衍射定量分析结果的因素中,样品的均匀性是最关键的因素,而其他因素产生的影响可用改变测试条件等相应方法来克服。只要样品足够均匀,就能将定量分析的误差限定在可控范围内。本文针对蛇纹石物相定量分析方法精密度的研究,可为蛇纹石物相定量分析标准方法的建立和分析方法的评价及分析质量的监控等提供依据。     

Rietveld定量方法在蒸发岩矿物组分分析中的精确度评价和误差来源

Rietveld物相定量分析(RQPA)方法在地质学中已有大量应用,在蒸发岩定量分析中,对精确度的评价和误差控制是提高分析质量的重要因素。本文对人工配制和野外采集的样品(石膏和钾盐)进行RQPA分析,并与化学分析结果对比,评价其精确度并分析其主要的误差来源。结果表明:人工配制的氯化钠-氯化钾二元物相的绝对误差为0.4%~0.9%;氯化钠-氯化钾-碳酸钙三元物相的绝对误差为0.1%~1.2%;二元物相样品10次分析的标准偏差为0.702%,相对标准偏差为1.74%(氯化钾)和1.17%(氯化钠);野外采集的石膏和钾盐样品的RQPA分析结果与化学分析结果具有很好的一致性。表明RQPA方法在蒸发岩矿物组分定量分析中具有较高的精确度,其误差主要来源于样品性质、样品制备、测试条件和精修过程等。RQPA方法具有减弱择优取向效应、无需纯样以及提高数据利用率等优点,与化学分析技术联用在蒸发岩矿产勘探、储量评价以及工业应用中具有广泛的前景。     

X射线粉晶衍射法在变粒岩鉴定与分类中的应用

变粒岩的鉴定通常以显微镜鉴定技术为主,但在显微镜下区分颗粒细小的长石、石英及绿泥石、蒙脱石、云母等层状硅酸盐矿物十分困难,仅通过显微鉴定技术对变粒岩进行定名可能产生较大误差,这对地质填图和原岩恢复工作会造成一些偏差,导致得出错误的地质结论。随着X射线衍射分析技术的发展,该技术已广泛应用于矿物学和岩石学的研究,本研究将结合X射线粉晶衍射技术,对显微镜下难以区分的细小矿物进行鉴定。共选用23件变粒岩样品,利用X射线粉晶衍射分析和显微镜岩石薄片鉴定技术,对变粒岩矿物组分进行检测,用X射线粉晶衍射矿物半定量分析结果验证岩石薄片鉴定结果准确性。显微镜岩石薄片鉴定结果与X射线粉晶衍射物相分析结果对比显示,10件样品定名一致,其余13件样品详细定名有差异。通过分析产生差异的原因,可以认为显微镜岩石薄片鉴定优势在于能确定岩石结构和构造,以及常见矿物组分;X射线粉晶衍射法的优势在于能检测出显微镜下较难区分的细小石英和长石颗粒的相对含量,并能检测出颗粒较小的绿泥石、蒙脱石及云母等层状硅酸盐矿物,该方法对含量较少、颗粒较细的矿物检测效果较好。实验证明将显微岩石薄片鉴定技术和X射线粉晶衍射技术相结合,才能更准确对变粒岩进行定名,为地学研究提供更符合客观实际的技术数据和分析结论。     

X射线衍射增量法在三水铝石定量分析中的应用--以桂西堆积型铝土矿中的红土为例

简述了X射线衍射增量法进行定量分析的原理、实验过程和实验条件,并用该方法对桂西堆积型铝土矿中的红土三水铝石进行了定量分析.实验表明,在红土样品中加入一定量的标准样品后,利用X射线衍射增量法测定红土样品中三水铝石的含量,与原有的利用化学物相分析方法相比,具有不受红土样品中物相数量和矿物组合限制的优点;同时,X射线射线衍射增量法具有简便、快速、准确、经济的特点,是测定桂西堆积型铝土矿中的红土中三水铝石最为理想的定量分析方法.     

X射线粉晶衍射法在片麻岩鉴定与分类中的应用

利用偏光显微镜岩石薄片鉴定和X射线粉晶衍射物相分析技术,对34件片麻岩样品矿物组分进行检测.两种方法分析结果比对显示,有18件岩石样品定名一致,其余16件岩石样品详细定名有差异.偏光显微镜鉴定技术的优势在于能准确定出岩石构造和结构,能鉴定出更多的金属矿物、电气石、榍石、磷灰石、绿帘石,有效区分白云母和黑云母;X射线粉晶衍射法优势在于更准确区分出岩石中层状硅酸盐矿物绿泥石、蒙脱石和云母,确定钾长石、钠长石和石英矿物种类与含量.研究表明：片麻岩鉴定应该把偏光显微镜岩石薄片法与X射线粉晶衍射矿物半定量技术结合起来,才能更好地确定片麻岩的矿物组分,为地学研究提供更符合客观实际的技术数据和分析结论.     

红外光谱法定量测定石灰岩中游离二氧化硅

采用红外光谱定量测定石灰岩中游离SiO_2可以克服化学分析中硅酸盐(高岭石族矿物例外)中SiO_2的干扰以及X衍射法不能测定非晶质SiO_2相的不足。在样品不含高岭石族矿物时分析的绝对误差小于0.5％。方法具有快速、准确、样品用量少、消耗低等优点。     

The terrestrial fauna of the Late Triassic Pant-y-ffynnon Quarry fissures,South Wales,UK and a new species of Clevosaurus (Lepidosauria: Rhynchocephalia)

Pant-y-ffynnon Quarry in South Wales yielded a rich cache of fossils in the early 1950s, including articulated specimens of new species (the small sauropodomorph dinosaur Pantydraco caducus and the crocodylomorph Terrestrisuchus gracilis), but no substantial study of the wider fauna of the Pant-y-ffynnon fissure systems has been published. Here, our overview of existing specimens, a few described but mostly undescribed, as well as freshly processed material, provides a comprehensive picture of the Pant-y-ffynnon palaeo-island of the Late Triassic. This was an island with a relatively impoverished fauna dominated by small clevosaurs (rhynchocephalians), including a new species, Clevosaurus cambrica, described here from a partially articulated specimen and isolated bones. The new species has a dental morphology that is intermediate between the Late Triassic Clevosaurus hudsoni, from Cromhall Quarry to the east, and the younger C. convallis from Pant Quarry to the west, suggesting adaptive radiation of clevosaurs in the palaeo-archipelago. The larger reptiles on the palaeo-island do not exceed 1.5?m in length, including a small carnivorous crocodylomorph, Terrestrisuchus, and a possible example of insular dwarfism in the basal dinosaur Pantydraco.     

The effect of water on accessory phase solubility in subaluminous and peralkaline granitic melts

The solubilities of columbite, tantalite, wolframite, rutile, zircon and hafnon were determined as a function of the water contents in peralkaline and subaluminous granite melts. All experiments were conducted at 1035 °C and 2 kbar and the water contents of the melts ranged from nominally dry to approximately 6 wt.% H₂O. Accessory phase solubilities are not affected by the water content of the peralkaline melt. By contrast, solubilities are affected by the water content of the subaluminous melt, where the solubilities of all the accessory phases examined increase with the water content of the melt, up to 2 wt.% H₂O. At higher water contents, solubilities are nearly constant. It can be concluded that water is not an important control of accessory phase solubility, although the water content will affect diffusivities of components in the melt, thus whether or not accessory phases will be present as restite material. The solubility behaviour in the subaluminous and peralkaline melts supports previous spectroscopic studies, which have observed differences in the coordination of high field strength elements in dry vs. wet subaluminous granitic glasses, but not for peralkaline granitic glasses. Lastly, the fact that wolframite solubility increases with increasing water content in the subaluminous melt suggests that tungsten dissolved as a hexavalent species.     

Quaternary stresses revealed by calcite twinning inversion: insights from observations in the Savonnières underground quarry (eastern France)

Calcite samples were extracted both from the rock matrix and the superficial coating of a karstified fault plane of an underground quarry, located in the eastern border of the Paris basin. The karstification is dated as Quaternary. Analysis of mechanical calcite twinning reveals that only the calcite matrix has also undergone a compression trending WNW that can be attributed to the Mio-Pliocene alpine collision. Both coating and matrix have undergone a strike-slip regime with σ₁ roughly trending north–south, that could correspond to the regional present-day state of stress, a strike-slip compression rather trending NNW, modified by local phenomena. To cite this article: M. Rocher et al., C. R. Geoscience 335 (2003).     

HYDROGEOLOGY

正20141756 Chen Ruige(Mathematical College,China University of Geosciences,Beijing100083,China);Zhou Xun Numerical Simulation of Groundwater Level Fluctuation in a Coastal Confined Aquifer with Sloping Initial Groundwater Level Induced by the Tide(Geological Bulletin of China,ISSN1671-2552,CN11-4648/P,32(7),2013,p.1099-1104,6 illus.,16 refs.) Key words:confined water,groundwater level     

METAMORPHIC PETROLOGY

正20141408 Cai Jia(Institute of Geology,Chinese Academy of Geological Sciences,Beijing100037,China);Liu Fulai Petrogenesis and Metamorphic P-T Conditions of Garnet-Spinel-Biotitebearing Paragneiss in Danangou Area,Daqingshan-Wulashan Metamorphic Complex Belt(Acta Petrologica Sinica,ISSN1000-0569,CN11-1922/P,29(7),     

SERIALS

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GEOPHYSICAL EXPLORATION

正20142386An Guoying(China Aero Geophysical Survey and Remote Sensing Center for Land and Resources,Beijing 100083,China)Application of Satellite Remote Sensing in Regional Hydrogeological Investigation:Taking Cenozoic Strata in Wenquan Sheet(1∶250 000)of Karakoram Range as an Example(Geosci-     

QUATERNARY GEOLOGY & GEOMORPHOLOGY

正20141016An Chengbang(Key Laboratory of Western China’s Environmental Systems,Ministry of Education,Lanzhou University,Lanzhou 730000,China);Zhao Yongtao Lake Records during the Last Glacial Maximum from Xinjiang,NW China and Their Climatic Impli-     

PETROLEUM GEOLOGY

正20141538 Cao Qing(School of Earth Sciences and Engineering,Xi’an Petroleum University,Xi’an 710065,China);Zhao Jingzhou Characteristics and Significance of Fluid Inclusions from Majiagou Formation,Yichuan Huangling Area,Ordos Basin(Advances in Earth Science,ISSN1001-8166,CN62-1091/P,28(7),2013,p.819-828,7 illus.,3 tables,43 refs.)     

GEOCHEMISTRY

正20142002 Wei Hualing(Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang065000,China);Zhou Guohua Element Content and Mineral Compositions in Different Sizes of Soil in Tongling Area,Anhui Province(Geological Bulletin of China,ISSN1671-2552,CN11-4648/P,32(11),2013,p.1861