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1.
采用蒸汽平衡法测定了4种温度(T=5、25、40、60℃)条件下Whatman No.42滤纸的率定曲线,建立了考虑温度影响的双线性率定曲线方程,发现滤纸的持水性能随温度升高而降低,且温度对率定曲线高吸力段滤纸持水性能的影响要弱于低吸力段。在此基础上,以南宁膨胀土为研究对象,使用滤纸法测定了不同温度作用下膨胀土试样的土-水特征曲线。试验结果表明,随着温度的升高,膨胀土持水性能下降,但温度的影响幅度会随着吸力的增大而减弱,当基质吸力达到40MPa时,不同温度下试样的体积含水率并没有明显变化,即此时温度对膨胀土的持水性能变化几乎无影响。为解释上述宏观现象,选取部分试样进行了压汞试验和吸附结合水试验,并根据试验结果从土体中各相及各相界面相互耦合作用的物理机制角度阐述了南宁膨胀土持水性能的温度效应及微观机制。 相似文献
2.
Bence Paul Jon D. Woodhead Chad Paton Janet M. Hergt John Hellstrom C. Ashley Norris 《Geostandards and Geoanalytical Research》2014,38(3):253-263
Here, we present an approach to laser ablation ICP‐MS mapping of multi‐phase assemblages that permits the use of different internal standard elements, concentration values and reference materials for each mineral. In this way, we obtain not only broad pictures of elemental distributions within samples but can also extract high accuracy concentration data for any user‐selected region. This is accomplished by assigning regions of an image to corresponding mineral phases on a pixel‐by‐pixel basis. In this way, accurate trace element concentrations can be determined for each mineral phase, despite potential variations in their ablation characteristics. We present an example where elemental maps are constructed from ablation of a gabbroic sample that includes the phases apatite, amphibole and plagioclase. This work represents an important first step towards development of a method to produce highly accurate LA‐ICP‐MS elemental maps of multi‐phase samples. 相似文献
3.
Determining Biogenic Silica in Marine Samples by Tracking Silicate and Aluminium Concentrations in Alkaline Leaching Solutions 总被引：5，自引：0，他引：5
This study introduces an alkaline leaching technique for the simultaneous analysis of biogenic silica and aluminium in sediments. Measuring aluminium facilitates the discrimination between silica from the biogenic (BSiO2) and the non-biogenic fraction, because it originates almost solely from the lithogenic phase. The method was tested using fine-grained silicagel, standard clay minerals, artificial sediments, and natural samples ranging from fresh diatoms to aged sediment from different depositional settings. To determine the BSiO2 content, four different models each describing the dissolution curves, but of increasing complexity, were applied and for each different type of sample the optimum model was selected on the basis of F-test statistics. For mixtures of silicagel and clay minerals, the contribution of Si from the dissolution of clay was negligible compared to Si originating from silicagel. For natural samples with high clay content, complex dissolution curves were observed and single-phase first order dissolution was the exception. This deviation from `ideal' behavior could only be recognized because of high-resolution sampling, especially in the first 20 minutes of the experiment. For most of the samples, the distinction between the biogenic silica fraction and the silica originating from dissolution of clays could be made on the basis of the Si/Al ratios and reactivity constants of the dissolving phases calculated with the models. Clay minerals typically dissolve slowly at a Si/Al ratio close to 1–2, depending on the type of clay mineral. In contrast, biogenic silica displays a wide range of reactivities and Si/Al ratios. Fresh biogenic silica from the water column usually has a high reactivity and a low Al content. Aged biogenic silica from the sediments has a lower reactivity, but Si/Al ratios as low as 5 were found. The method as described here therefore presents an accurate method to analyze biogenic silica in marine sediments with a relatively high clay mineral content. 相似文献
4.
研究了物质粉末衍射强度与样品堆积密度的关系,将粉末样品紧密度导入衍射强度公式。在此基础上推导出直接法测定多组分混合物质量吸收系数及各相浓度的数学公式,并通过实验证明了方法的实用性。还研究了缺乏纯样品以及样品中存在非晶质相、结晶度变化大的柑、择优取向严重的相等特殊情况的实验方法。 该方法不需要向待测样品中加入任何参考物质,不称样,不混样,不损耗纯样品,制样简便,特别适合大批量样品的定量相分析。 相似文献
5.
锑矿石化学物相分析方法选择性分离条件验证及准确度评估 总被引：1，自引：1，他引：0
目前我国矿石化学物相分析方法,除少数方法具有较广泛的适应性外,多数方法均是针对某一具体矿区的样品而制定,在实际应用中无法确认分析结果的准确性和选择性分离流程的适应范围。验证化学物相分析方法的选择性分离流程及方法准确度是该领域必须解决的问题。本文以我国具有代表性的锑矿类型——单锑硫化矿为研究对象,通过岩矿鉴定确定锑的主要矿物相,从试验样品中挑选验证选择分离条件所需的单矿物,在无法获得锑华单矿物的情况下,通过价态分析确定了锑华与锑酸盐混合物中锑华的比例,并通过系列单矿物选择分离对比条件试验和X射线衍射分析,确定了锑华、辉锑矿和锑酸盐等锑物相的选择性分离条件。结果表明:对于硫化锑含量大于35%的样品,锑硫化相的选择浸出时间从传统的30 min调整为40 min,硫化锑的浸出率提高了4%~6%,硫化锑相对于锑酸盐的串相率降低了45%~70%,硫化锑相浸出完全,提高了硫化锑和黄锑矿相分析的准确度。该方法适用于不同地区、不同类型(氧化矿、硫化矿)锑矿石样品的锑化学物相分析。 相似文献
6.
Byron S. Gottfried 《International Journal of Mineral Processing》1981,8(1):89-91
An earlier paper by this writer presented a method for combining distribution data for float-sink coal-cleaning devices into a single, generalized distribution curve which is independent of the specific gravity of separation. A nonlinear exponential-type equation was used to represent each of the curves and to determine the corresponding generalized probable error. Performance data for five common coal-cleaning devices were analyzed using this method.In this paper the method is applied to another common coal-cleaning device — the sand cone. Numerical values are presented for the constants in the exponential-type generalized distribution equation and for the corresponding generalized probable error. Several different feed size-fractions are considered. 相似文献
7.
钕同位素比值~(143)Nd/~(144)Nd标准溶液研制 总被引：3，自引：2，他引：1
钕同位素比值(~(143)Nd/~(144)Nd)是Sm-Nd同位素方法的关键量值,由于被测样品的~(143)Nd/~(144)Nd比值变化范围很小,所以对~(143)Nd/~(144)Nd比值测试的精准度要求很高(精度优于0.005%)。为了获得高精度和高准确度的测试数据,分析过程中所用Nd同位素标准物质起着重要作用。以往的Nd同位素标准物质都是氧化钕,经过近三十年有的已消耗殆尽。本文阐述了钕同位素比值~(143)Nd/~(144)Nd标准溶液的研制,经检验标准溶液的均匀性和稳定性良好,由11家实验室协同定值,采用MC-TIMS和MC-ICP-MS方法测定~(143)Nd/~(144)Nd,确定了Nd同位素标准溶液的特性值~(143)Nd/~(144)Nd=0.512438,不确定度为5×10-6。此标准溶液于2015年5月获得国家标准样品证书(批号为GSB 04-3258—2015),可被用于地质、资源、海洋、环境、考古等多种样品~(143)Nd/~(144)Nd比值测定时的仪器校准和分析过程的质量监控。 相似文献
8.
A simple method based on high-performance size-exclusion chromatography (HPSEC) has been developed for rapid quantification of humic and fulvic acids (HA and FA) in stream waters. A Tsk-gel column was used to separate natural dissolved organic matter (DOM) into two components: peak A and B. In terms of HPSEC chromatograms and fluorescence patterns, peak A and B were similar to the corresponding XAD-extracted HA and FA, respectively. It is suggested that peak A fraction mainly consisted of HA, and peak B fraction FA. The similar separation of HA and FA using HPSEC and a conventional XAD method suggests the consistency of molecular size distribution and physical–chemical properties of DOM. HPSEC offers a simple and rapid method for the quantification of HA and FA instead of tedious extractions of humic substances. Analyses of natural water samples show that the calculation of HA/FA based on UV absorbance was under- or over-estimated, the calibration using the extracted HS allows a more accurate quantification. The fast screening of HA and FA provides useful quantitative and qualitative information that can be used in environmental or monitoring studies. 相似文献
9.
X射线荧光光谱法测定高锶高钡的硅酸盐样品中主量元素 总被引：6，自引：5，他引：1
用百分总和检查硅酸盐岩石全分析数据的质量是分析工作者的传统做法,但对于微量元素含量较高的样品,采用X射线荧光光谱法(XRF)进行测定,如果不考虑微量元素的含量及其对主量元素基体效应的影响,往往会使主量元素含量更加偏离真实值。本文针对Sr、Ba含量较高的硅酸盐样品,通过人工配制标准样品,扩大了Sr、Ba校准曲线的定量范围,主量元素校准中加入Sr、Ba的基体校正系数,达到了主量元素定量更加准确可靠的实际效果。采用此方法分析国家标准物质,各主量元素的精密度(RSD)均小于2%;分析不参加回归的标准物质和人工配制的标准样品,主量元素的测量值与标准值(或参考值)基本一致。该方法可以满足硅酸盐的测定要求,主量元素各项结果的加和能够达到《地质矿产实验室测试质量管理规范》的一级标准(99.3%～100.7%)。 相似文献
10.
土壤中单环芳烃定量分析的基质效应研究 总被引：1，自引：0，他引：1
来源于燃料油泄露的单环芳烃对土壤的污染已经成为一个很普遍的现象,因此,准确、高效地检测土壤中的挥发性单环芳烃是一个很关键的问题。文章通过在标准系列中加入石英砂和土壤两种基质,比较水、水-石英砂、水-土壤3个定量库中得到的标准曲线的斜率,研究基质效应对土壤样品定量的影响。结果表明,芳香烃类物质在土壤基质中的斜率总体小于在石英砂基质中的斜率,在石英砂基质中的斜率比在水基质中的斜率小1%(苯)～9%(正丁苯),在水基质中得到的斜率最大;只有苯在土壤基质和水基质中的斜率相当,其余组分在土壤基质中的斜率比在水基质中的斜率小9%(丙苯)～24%(1,2,4-三氯苯)。单环芳烃在土壤基质中相对斜率的大小与化合物本身的沸点以及辛醇-水分配系数呈负相关。研究表明,在对土壤样品进行校准的过程中,选择合适的基质建立定量库是一个非常关键的因素。 相似文献
11.
Zusammenfassung Es wird eine einfache Methode zur quantitativen Bestimmung kristalliner Phasen in Gemischen angegeben, die allgemein anwendbar ist. Zu jeder kristallinen Phase muß eine Konstante K experimentell bestimmt werden; das geschieht an künstlichen Gemischen der reinen kristallinen Phasen. Es wurden Gemische mit 2 bis 8 Komponenten analysiert; die Abweichung von der Einwaage beträgt im Mittel 1,2% abs.Es wird vorgeschlagen, eine umfassende Röntgenkartei zum Zweck der quantitativen Phasenanalyse zu schaffen.Die Bestimmung von kristallinen und amorphen Phasen nebeneinander wurde auch angegriffen.
Herrn Professor Dr.F. Machatschki zum 70. Geburtstag gewidmet. 相似文献
Summary A simple method is given for the quantitative determination of crystalline phases in mixtures, which can be applied universally. A constant K must be determined experimentally for each crystalline phase; this is done on artificial mixtures of the pure crystalline phases. Mixtures of 2 to 8 components have been analyzed; the mean deviation from the weighed in quantities is 1,2% abs.The compilation of a comprehensive X-ray file for the quantitative phase analysis is proposed.The determination of crystalline and amorphous phases in a given mixture is also tackled.
Herrn Professor Dr.F. Machatschki zum 70. Geburtstag gewidmet. 相似文献
12.
The understanding of the evolution of microstructures in a metamorphic rock requires insights into the nucleation and growth history of individual grains, as well as the coarsening processes of the entire aggregate. These two processes are compared in impure carbonates from the contact metamorphic aureole of the Adamello pluton (N‐Italy). As a function of increasing distance from the pluton contact, the investigated samples have peak metamorphic temperatures ranging from the stability field of diopside/tremolite down to diagenetic conditions. All samples consist of calcite as the dominant matrix phase, but additionally contain variable amounts of other minerals, the so‐called second phases. These second phases are mostly silicate minerals and can be described in a KCMASHC system (K2O, CaO, MgO, Al2O3, SiO2, H2O, CO2), but with variable K/Mg ratios. The modelled and observed metamorphic evolution of these samples are combined with the quantification of the microstructures, i.e. mean grain sizes and crystal size distributions. Growth of the matrix phase and second phases strongly depends on each other owing to coupled grain coarsening. The matrix phase is controlled by the interparticle distances between the second phases, while the second phases need the matrix grain boundary network for mass transfer processes during both grain coarsening and mineral reactions. Interestingly, similar final mean grain sizes of primary second phase and second phases newly formed by nucleation are observed, although the latter formed later but at higher temperatures. Moreover, different kinetic processes, attributed to different driving forces for growth of the newly nucleated grains in comparison with coarsening processes of the pre‐existing phases, must have been involved. Chemically induced driving forces of grain growth during reactions are orders of magnitudes larger compared to surface energy, allowing new reaction products subjected to fast growth rates to attain similar grain sizes as phases which underwent long‐term grain coarsening. In contrast, observed variations in grain size of the same mineral in samples with a similar T–t history indicate that transport properties depend not only on the growth and coarsening kinetics of the second phases but also on the microstructure of the dominant matrix phase during coupled grain coarsening. Resulting microstructural phenomena such as overgrowth and therefore preservation of former stable minerals by the matrix phase may provide new constraints on the temporal variation of microstructures and provide a unique source for the interpretation of the evolution of metamorphic microstructures. 相似文献
13.
Trace Element Analysis of Natural Gold by Laser Ablation ICP-MS: A Combined External/Internal Standardisation Approach 总被引：1，自引：0，他引：1
Tom E. McCandless Mark E. Baker Joaquin Ruiz 《Geostandards and Geoanalytical Research》1997,21(2):271-278
For the trace element analysis of gold by laser ablation ICP-MS, external calibration samples of differing matrix composition have been used in previous studies. Data presented here suggest that even for calibration samples and unknowns with closely-matched matrices, discrepancies arise due to variations in the coupling behaviour of the laser with the sample at different power deliveries, and can lead to erroneous trace element determinations. Internal standardisation for gold is complicated because Au and Ag, the most common major elements, do not have minor isotopes that can be used as internal standards. This problem was overcome for natural gold samples by using an external calibration sample only for the major elements Au and Ag, then defocussing the ion path and using 107 Ag in each sample as an internal standard against which μg g-1 levels of Te, Sb, Hg, Bi, and Cu were determined. The results suggest that trace elements can occupy lattice sites in gold rather than occurring only as micro-inclusions of other phases. The analytical approach taken here may be used in trace element analysis where adequate external calibration samples are not readily available. 相似文献
14.
广西靖西县新圩铝土矿Ⅶ号矿体矿石热分析 总被引：1，自引：0，他引：1
广西靖西新圩堆积型铝土矿为我国典型的一水铝型铝土矿。以新圩堆积型铝土矿的典型样品为研究对象,通过X衍射分析确定其矿物组成,进一步借助差热(DTA)与热重(TG/DTG)分析,探索铝土矿石加热过程。X衍射分析显示5个铝土矿样品矿物组成主要为硬水铝石、赤铁矿、绿泥石、三水铝石、锐钛矿、金红石、针铁矿以及少量的高岭石。差热(DTA)分析显示铝土矿样品有2个明显的吸热峰,分别为三水铝石和硬水铝石吸热峰;热重(TG/DTG)曲线显示样品分解分为4个阶段,分别为吸附水失去阶段和三水铝石、针铁矿、硬水铝石脱羟基作用阶段。利用热重(TG/DTG)数据分别计算了硬水铝石、三水铝石、针铁矿矿物相对百分含量,与国内外同类型铝土矿矿石热分析特征对比显示具有大体一致的热分析特征。 相似文献
15.
《矿物学报》2013,(Z1)
The glass-ceramics was prepared from coal fly ash, limestone and Na2CO3 by sintering processes. Effects of the crystallization temperature (850–1100 ℃) on crystallization behavior, microstructure, sintering character and chemical stability of the glass-ceramics samples were analyzed by means of DTA, XRD, SEM and other analytical methods. The results show that the main crystalline phase of as-prepared glass-ceramics after crystallization treatment is gehlenite (Ca2Al2SiO7). The species of crystalline phases keep the same, however, the main crystalline intensity, line shrinkage rate and bulk density increase first then decrease with the increasing of heat treatment temperature. Water absorption of the samples was reduced as the heat treatment temperature rising. The glass-ceramics display high performance crystallization properties and chemical stability. The optimized glass-ceramics with desired sintering character and chemical stability was obtained by crystallized at 1050 ℃. 相似文献
16.
Amilcar Soares 《Mathematical Geology》1992,24(2):149-160
A method is proposed for the characterization of the disjoint shapes of a multi-phase set. The method uses a global structural function and provides estimates of the complete mosaic of phases, honoring the individual volume proportions inferred from the experimental samples. The estimates of shapes can be improved by local conditioning to the covariance of each phase and to geometrical characteristics such as spatial orientation of the different strata. The mapping of uncertainty zones for individual phases is one advantage of using a geostatistical approach to characterize the morphology of qualitative (non-numerical) variables. 相似文献
17.
四川冕宁稀土矿床黑色风化物中的稀土元素赋存状态研究 总被引：2，自引：0，他引：2
本文用现代的固体表面分析方法和连续选择性提取法对冕宁黑色风化物中稀土元素的赋存状态进行研究因。在可交换离子相,易还原相,水成相和矿物结晶相四种稀土存在的形式中,易还原相和水成相是自然界矿物中新的稀 存状态。特性吸附是产生这两种新相的内在原因。 相似文献
18.
The uptake of Nd(III) by the crystalline C–S–H phases 11 Å tobermorite and xonotlite has been investigated by the combined use of wet chemistry techniques, extended X-ray absorption fine structure (EXAFS) spectroscopy, and X-ray diffraction (XRD) in combination with Rietveld refinement. The results from XRD and EXAFS allowed the different modes of Nd–Ca substitution in tobermorite and xonotlite to be distinguished from each other. Wet chemistry and EXAFS data showed that the formation of any Nd solid phase with fixed stoichiometry could be ruled out. XRD studies on the samples with high Nd loading (350 μmol Nd/g solid phase) further showed that Nd was bound in the structure of C–S–H phases. The EXAFS data suggested that Nd could form several species on xonotlite and tobermorite at low loadings (7–35 μmol Nd/g solid phase). Neodymium was predominantly bound on the external surface of both crystalline C–S–H phases after 1 day of reaction time and predominantly incorporated in the Ca layers of the crystalline C–S–H phases in the long run (?60 days reaction time). The latter process was faster at low Nd loadings and was apparently controlled by re-crystallization of the C–S–H phases. Neodymium incorporation was accompanied by the release of “zeolitic” water (water molecules in the interlayer of C–S–H) and bridging Si tetrahedra, reflected by the formation of more disordered structures in both C–S–H phases. The Nd retention model proposed in this study helps to improve understanding of the immobilization of trivalent lanthanides and actinides in cementitious materials. This knowledge is essential for long-term predictions of radionuclide retention in conjunction with a more detailed assessment of the safe disposal of actinides in the cementitious near field of a repository for radioactive waste. 相似文献
19.
为研究黄土的孔隙分布(PSD)和土 -水特征曲线(SWCC)与黄土沉积环境的关系,在甘肃榆中县和平镇和正宁县及陕西泾阳县等黄土台塬上部采取原状马兰黄土样,先测定其基本物理指标,再用压汞法测得各土样的PSD曲线,同时用滤纸法测得其SWCC。结果表明:和平镇马兰黄土的PSD曲线为单峰形态,泾阳县马兰黄土的PSD曲线为双峰形态,正宁马兰黄土的PSD曲线具有三峰特点。各土样的SWCC具有与PSD曲线相对应的阶梯状形态。SWCC与PSD曲线之间的对应关系,说明黄土的土水特征受孔隙分布的控制。获取3个原状样扫描电镜图像,微结构显示出这种地域性分异现象。对各采样点的气候环境分析表明,黄土PSD曲线之间的差异主要是由成土作用强弱决定的。将降水量与蒸发量的比值定义为蒸渗系数 (CEI),作为刻画成土作用强弱的指标。发现当CEI≤0.3时,PSD曲线为单峰模式;0.3＜CEI≤0.4时,PSD曲线为双峰模式;0.4＜CEI≤0.5时,PSD曲线为三峰模式,相应的SWCC分别为单拐点、双拐点和三拐点模式。 相似文献
20.
以山西大同新生代玄武岩样品为例, 利用Quanta 200扫描电镜、GENESIS能谱仪对能谱仪PPA分析方法进行了实验研究, 该方法为粒度和物相自动分析方法.笔者首次把能谱仪PPA分析方法应用到地质学领域的岩石光薄片研究中, 快速得出了一系列不同物相的形态学数据及化学成分分析结果: 物相种类、每一种物相的颗粒数、每一个颗粒的平均直径、面积、周长、圆度、长宽比及化学成分等, 并得出了不同物相在该视域所占的面积百分比及每种物相颗粒的平均直径, 克服了传统光薄片粒度分析方法的所有缺点, 为矿物学、岩石学及矿床学研究提供了一套非常有意义的数据. 相似文献