考虑级配多样性的颗分试验取样质量理论研究

颗粒分析试验被广泛应用于土木、水利水电和采矿等诸多工程中,以确定材料的颗粒级配。但对于工程中常见的超大粒径填料合理取样质量问题,尚缺少可依据的文献资料。将试样选取视为一种分层抽样过程,结合抽样分析理论,建立了能够确定样本容量的理论公式;考虑到颗粒材料平均粒径与其级配分布的关系,提出了一种为确定材料整体级配所需试样质量的通用方法。对不同级配分布情况开展了针对性试验,验证了所提出方法的适用性。并将该方法应用于确定重庆江北机场和贵州龙洞堡机场填料的颗粒级配,取得了良好效果。所得结果可为相关工程实践及规范的发展和完善提供参考。     

An efficient approach to generating DEM samples having coincident void ratios with actual sand

The ranges of initial void ratios that can be achieved for numerical samples with the same grading as actual sand under gravity are explored using three-dimensional discrete element method (DEM). A corrected compressible accumulation model is proposed to predict the packing density of sand. Compared with the measured results, the errors of the prediction results are small. For three-dimensional DEM samples, when the ratio of sample size to particle size L/R is equal to or larger than 30, the maximum and the minimum void ratios are minimally affected by the sample size L. The maximum void ratios and the minimum void ratios of numerical samples with spherical particles are much smaller than those of actual sands. The generation method for numerical samples with non-spherical particles is proposed based on the theory of CPM. The variations of void ratios of numerical samples with non-spherical particles are wider than actual sands. So it can meet all the need of DEM simulation on the void ratio of actual sand.     

结构面粗糙度统计测量最小样本数确定方法

由于结构面粗糙度具有各质异性、各向异性、非均一性和尺寸效应等特征,结构面粗糙度系数(JRC)取值具有不确定性,工程中广泛采用统计方法来分析结构面粗糙度性质,然而以往研究往往忽略样本数不足对统计结果的影响。针对结构面粗糙度统计测量时无法确定合理样本数的问题,分别提出基于变异系数级比分析及简单随机抽样原理的最小样本数确定方法。以实际工程岩体结构面表面数据为研究对象,对比分析两种方法在系列尺寸下确定的统计测量最小样本数。实例分析表明:小尺寸样本的变异系数(CV)值明显大于大尺寸样本,且CV值随取样尺寸的增大而减小,取样尺寸为10～50cm的CV值基本稳定在0.31～0.47之间,取样尺寸为60～100cm的CV值基本稳定在0.21～0.31之间;最小样本数与取样尺寸基本满足幂函数关系,且最小样本数随取样尺寸的增大而减少;系列尺寸下级比分析方法在允许误差为±2%时确定的最小样本数与简单随机抽样原理在最大允许误差为10%、置信度为95%时计算的最小样本数是一致的,相似度大于0.997。该研究方法可为工程岩体中定量获取结构面粗糙度统计测量最小样本数提供依据,保证了JRC(结构面粗糙度系数)统计测量...     

激光粒度仪测试结果及其与沉降法、筛析法的比较

分析了Cilas 940L激光粒度仪的测试结果,并与沉降法、筛析法进行了比较。激光粒度仪测试结果的重复性较好,测量精度较高。对于玻璃珠样品,激光粒度仪和筛析法测试结果十分接近,对于天然沉积物,激光粒度仪测定的平均粒径偏粗,分选偏差。和沉降法相比,激光粒度仪测定的粘土组份 (<8%)的含量为沉降法的 46.7%～ 70.5 %,平均为 6 0 %,测定的平均粒径较沉降法偏粗,分选偏差。造成激光粒度仪与沉降法、筛析法之间差异的原因主要在于这些测试方法原理的不同和天然沉积物不规则的形状。     

Investigations into the Preparation of Ultra-Fine Particle Size Geochemical Reference Materials

Although over recent years, sensitivity and precision of modern analytical techniques have continuously improved, traditional analytical specification for the particle size of samples has remained at 74 μm (-200 mesh). For this reason, the uncertainty caused by inhomogeneity in test portions of the sample itself has become a more and more significant contribution to the total analytical uncertainty. Therefore, to reduce this total uncertainty, the first step is to improve the homogeneity by reducing the particle size of a sample. For this purpose, we have investigated a method for the preparation of ultra-fine reference materials. Using the modern ultra-fine crushing technique (jet mill), six marine sediment samples MSAn and MSCS-1 to 5 were prepared and the particle distributions of these samples were measured using a laser particle-analyser. The average particle size of these samples was 4–5 (im and the largest particle size was less than 30 (im. MSAn will be used as the sample for a future GeoPT(tm) proficiency testing round and MSCS-1 to 5 will be prepared as reference materials. All geochemical laboratories are welcome to participate in this co-operative research programme. The processing and use of ultra-fine samples (< 30 μm) will have a significant influence on the future development of geoanalytical techniques as a consequence of the potential reduction in the mass of test portion and the development of new geoanalytical systems.     

沉积物中黑碳的提取和测定方法 : 误差分析和回收率实验

介绍了从沉积物中提取黑碳的一种误差较小的改进方法，并对实验误差及引起误差的原因进行了详尽的分析和探讨，同时给出了方法的回收率。经过未均匀处理样品的平行实验，得到实验结果的总体偏差为8．89％，其中个别样品的偏差可达10％－20％；在样品进行了均匀处理后，得到平行实验的总体偏差为3．29％，HCl-HF单步处理的总体偏差为1．96％，而K2Cr2O7氧化处理单步实验的总体偏差为2．50％。其中回收率实验表明，黑碳的回收率可达80％以上。由此可见，所取样品具有代表性，是准确测定沉积物黑碳含量的前提。     

激光法粒度筛析校正研究

激光法和筛析法分析作为两种最常见的用于沉积地质粒度分析的方法,其间的数据转换校正是在数据对比、数据对接时经常遇到且无法回避的问题。为此设计了两个实验,实验一对比了窄粒度范围样品两种分析方法的分析结果,统计分析了筛析法比激光法偏大的幅度,并提出一个校正方法;实验二对不同磨圆程度的样品进行分析,研究了磨圆度与两种分析方法差异程度之间的相关关系,认为实验一提出的校正方法适合一般条件下的天然沉积物粒度分析校正。文章又以实例展示了所提出的校正方法的校正效果并讨论了激光粒度法存在的问题。激光粒度分析法用于天然沉积物粒度分析时,结果常见明显的光滑化、正态化、双峰合并现象,扭曲了真实的粒度分布。文章认为实际样品具体情况远远复杂于米氏理论的设定条件,样品条件参数并未全部带入计算过程,所以激光法粒度求解是不精确的。更好的数据校正方法有待于激光粒度仪的软件、硬件改进。激光法合理的用于天然沉积物粒度分析还有一些问题需要讨论。     

联用筛析法与激光法进行粒度接序分析的界点选择

筛析法、激光法和图像法是三种常用的粒度分析方法,但由于测试原理的不同,三种测试方法有不同的适用性。筛析法和图像法能够精确测量砂质颗粒的粒径,但不适用于泥质细颗粒（<0.063 mm）的粒径测量;相反,激光法无法准确测量中粗砂粒级颗粒（2~0.21 mm）,但能高精度测量较细沉积物粒径。分选较差的天然沉积物粒径分布范围较广,需要综合运用筛析法-激光法进行接序粒度测试。通常选用2 mm为界点开展接序粒度分析,但因激光法在测量中粗砂颗粒时误差较大,易导致接序粒度分析结果准确性不高。建议以0.21 mm为分界点开展接序粒度分析,分别避开筛析法和激光法测量精度不高的粒级区间,可使测试结果的准确性得到有效的提高。     

The Precision and Sensitivity of Thermal Ionisation Mass Spectrometry (TIMS): An Overview of the Present Status

This paper illustrates that sample size cannot be reduced below a theoretical limit and still achieve the highest precision obtainable on modern mass spectrometers. Reproducibility at the few ppm level is achievable and is related essentially to ion counting statistics. The number of atoms necessary to carry out such measurements is related directly to the sensitivity of the instrumentation. As most of the elements of interest are not major constituents of natural silicates, a lower limit to the size of the starting sample is assessed. Even for a number of elements for which very high ion per atom yields are attained by TIMS, minimum sample mass is an important limiting factor for precious or rare samples and may reduce the scientific output of experiments or place a major constraint on the sampling strategy itself. For rare meteorites or individual Martian samples expected to be returned in amounts at the gramme scale for rocks or at the microgramme scale for dust, the high sensitivity of TIMS is a requirement. Nevertheless, a compromise has to be found between sample consumption and the minimal desirable precision for a useful isotopic measurement.     

基于数字图像处理技术的砂土颗粒级配分析研究

砂土颗粒级配是影响砂土工程性质的重要参数之一,传统的颗分试验方法由于试验原理不同而具有不同的适用范 围。为更加方便、准确地获取砂土颗粒级配,提出了一种基于数字图像处理技术来获取SEM照片中的砂颗粒粒径参数及级 配特征的新方法。将准备好的砂土样品打磨成薄片放在扫描电镜下拍照,然后利用Photoshop软件对照片进行拼接,并采用 自主研发的SMAS数字图像分析系统对拼接好的照片进行定量分析处理,获取样品的微观结构参数,将获得的“土颗粒等 效直径”和“土颗粒面积”分别等效为实际土颗粒粒径和土颗粒质量,进而换算得到砂土的颗粒级配曲线;然后将通过数 字图像技术获得的砂土颗粒级配曲线与通过传统筛分法和激光粒度分析法得到的颗粒级配曲线进行对比,验证了提出的数 字图像处理方法的有效性和可靠性,同时分析了两种方法之间存在的差异及其原因,并对数字图像处理方法和传统颗分方 法各自的优缺点进行了讨论。     

基于数字图像处理技术的砂土颗粒级配分析研究

砂土颗粒级配是影响砂土工程性质的重要参数之一，传统的颗分试验方法由于试验原理不同而具有不同的适用范 围。为更加方便、准确地获取砂土颗粒级配，提出了一种基于数字图像处理技术来获取SEM照片中的砂颗粒粒径参数及级 配特征的新方法。将准备好的砂土样品打磨成薄片放在扫描电镜下拍照，然后利用Photoshop软件对照片进行拼接，并采用 自主研发的SMAS数字图像分析系统对拼接好的照片进行定量分析处理，获取样品的微观结构参数，将获得的“土颗粒等 效直径”和“土颗粒面积”分别等效为实际土颗粒粒径和土颗粒质量，进而换算得到砂土的颗粒级配曲线；然后将通过数 字图像技术获得的砂土颗粒级配曲线与通过传统筛分法和激光粒度分析法得到的颗粒级配曲线进行对比，验证了提出的数 字图像处理方法的有效性和可靠性，同时分析了两种方法之间存在的差异及其原因，并对数字图像处理方法和传统颗分方 法各自的优缺点进行了讨论。     

Assessing the microped size distributions of desert soils erodible by wind

The microped size distribution of erodible soils is one of the main factors controlling the emissions of mineral aerosol. To date, the microped size distributions of desert soils in natural field conditions are not well known and thus the existing dust source models cannot be applied to natural sites. Based on dry sieving and elemental analysis of 26 soil samples collected in arid and semiarid regions, it is shown that the microped size distributions of these desert soil samples involve a combination of four major mass size populations. These four size populations correspond to salty soils, fine quartz sand, coarse dune sand and aluminosilicate silt. We show that the microped size distributions of the various desert soils, according to their mineralogical characteristics, can be calculated by a mixture involving two or three of these four populations. The main field of application for this scheme is the characterization of the erodible soil size distributions for modelling the atmospheric dust cycle.     

动态图像法应用于海滩沉积物粒度粒形测试及其与筛析法的比较

筛析法是海滩沉积物粒度分析较经典和常用的方法。随着科学技术的发展,利用动态图像法分析沉积物粒度逐渐得到推广。本文利用动态图形法和筛析法对海南岛5个海滩剖面20组沉积物样品进行粒度粒形测试,并将两种方法所测得的粒度进行比较。测试分析结果显示,该方法的测试结果重复性好,精度高;通过与筛析法的对比显示,动态图像法与筛析法的测试结果非常接近,粒度级配曲线基本一致,各个粒度参数值很接近且相关性非常好（R2>0.94）;由动态图像法得出的粒形参数可以看出,粒径相当的不同海滩沉积物粒形参数有很大差别,同一海滩不同部位的球形度和宽长比变化很大,对称度和凹凸度变化稍小。研究表明,动态图像法与筛析法之间的粒度分析差异主要来自于两者测量原理的不同和天然海滩砂颗粒形状的不规则;动态图像法解决了不规则沉积物粒度的测量。因此,动态图像法可以替代筛析法来测量沉积物粒度,应用前景广阔。     

压裂支撑剂密度测定方法及应用研究

论证了支撑剂体积密度、视密度和绝对密度的概念与内涵,降低概念混用现象的发生。结合SY/T5018-2006和SY/T5018-2014两个标准,重新设计了测定视密度的方法、步骤和计算式。分析得出100 ml规格密度瓶是50 ml规格密度瓶测量值稳定性的7倍以上;用纯水做测试液比煤油的测量值稳定性高出2倍左右;选用100 ml规格的密度瓶,样品质量大于40 g后,会使测量值更趋稳定。支撑剂的密度指标主要用于压裂施工中的产品优选、压裂液携砂能力、地层造缝能力和变密度加砂压裂等方面。建议除非支撑剂为典型的亲油性物质,否则宜选择纯水、100 ml规格密度瓶、40 g左右支撑剂样品组合开展实验为宜。     

浅谈微粒金刚石在找矿中的作用

微粒金刚石是指粒度<0.5mm的金刚石,用作找矿指示矿物可帮助发现不含或少含其他找矿指示矿物的金刚石原生矿。找矿中遇到可疑的风化岩体,筛取<4mm的泥砂,细砾样品40kg,运回室内加工处理,淘洗时水中应加入肥皂水,使泥水表面起一层皂泡,以防微粒金刚石悬浮进入废弃的尾泥中。磁选后对<0.5mm无磁性精矿采用磁液電力分离仪选取微粒金刚石。     

Comparison between analytical and mineralometric methods in regional scheelite exploration

The scheelite dispersion was studied in a drainage system over an area of 150 km² with stratabound mineralization of scheelite in a Pre-Ordovician volcano-sedimentary Series in the Hercynian Iberian Massif (Zamora province, NW Spain). A density of two samples per square kilometer (approximately 500 m sample spacing along streams), a sample volume of 10 l and sieving at 5 mm ensure that an anomaly source is detected. It was found that the dispersion of scheelite is typically less than 1 km. The methods applied to panned concentrates (mineralometric scheelite study, with or without multifractional grain size basis, and X-ray fluorescence tungsten analysis) give similar anomaly patterns and are efficient in exploration for scheelite mineralization.     

Bounding the required sample size for geologic site characterization

The proposed objective of limited sample geologic site characterization is to minimize the chance of unknown and unexpected extremes. This problem proves to be extremely difficult when the data are spatially correlated. A generalization of the classical one-sided nonparametric tolerance interval, based upon the statistical concept of associated random variables, establishes a rigorous, almost distribution-free, tool for computing the minimum required sample size for site characterization. An upper bound on the required number of samples follows from a heuristic measure for the quantity of information in a spatially dependent sample; the measure presented is the equivalent number of uncorrelated samples and is calculated using an estimated variogram. An empirical check of the upper and lower bounds, using more than 2 million simulations and seven real data sets produces a heuristic rule for quantifying the required number of samples.This paper was presented at Emerging Concepts, MGUS-87 Conference, Redwood City, California, 13–15 April 1987.     

封闭酸溶-等离子体质谱法分析超细粒度地质样品中42个元素

采用封闭压力酸溶,电感耦合等离子体质谱法（ICP—MS）测定了超细样品的42个元素,研究了样品的粒度、分解条件、取样量对分析准确度和精密度的影响。结果表明,用超细粉碎样品（〈30μm）,取样量减小至2mg仍能保证取样代表性,总用酸量可减至0．5mL,反应时间也可大大缩短。采用超细样品可更好地发挥ICP—MS技术高灵敏度的效能,从而达到保护环境、降低分析成本、提高分析效率的目的。     

Determination of the distribution of size of irregularly shaped particles from laser diffractometer measurements

The formal stereological transformation equation for particle sieve size distribution from measurements in lower dimensional spaces is applied to laser diffractometer measurements. The transformation function for iron ore particles is measured experimentally, and modeled. The solution is tested against the measured transformation function data as well as synthetic composite distributions of the original sample. The natural size distribution of a sample taken from a grinding circuit stream was measured by a combination of standard sieving and cyclosizer, and the result is compared to the transformed size distribution calculated from laser diffractometer measurements. The stereological transformation technique performed well in all cases.     

Capturing the complete stress–strain behaviour of jointed rock using a numerical approach

This paper presents the results of a series of numerical experiments using the synthetic rock mass (SRM) approach to quantify the behaviour of jointed rock masses. Field data from a massive sulphide rock mass, at the Brunswick mine, were used to develop a discrete fracture network (DFN). The constructed DFN model was subsequently subjected to random sampling whereby 40 cubic samples, of height to width ratio of two, and of varying widths (0.05 to 10 m) were isolated. The discrete fracture samples were linked to 3D bonded particle models to generate representative SRM models for each sample size. This approach simulated the jointed rock mass as an assembly of fractures embedded into the rock matrix. The SRM samples were submitted to uniaxial loading, and the complete stress–strain behaviour of each specimen was recorded. This approach provided a way to determine the complex constitutive behaviour of large‐scale rock mass samples. This is often difficult or not possible to achieve in the laboratory. The numerical experiments suggested that higher post‐peak modulus values were obtained for smaller samples and lower values for larger sample sizes. Furthermore, the observed deviation of the recorded post‐peak modulus values decreased with sample size. The ratio of residual strength of rock mass samples per uniaxial compressive strength intact increases moderately with sample size. Consequently, for the investigated massive sulphide rock mass, the pre‐peak and post‐peak representative elemental volume size was found to be the same (7 × 7 × 14 m). Copyright © 2015 John Wiley & Sons, Ltd.