Microwave-assisted extraction of organochlorine pesticides from sediments and determination by gas chromatograph with electron capture detection

A simple and rapid procedure to extract organochlorine pesticides （OCPs） from sediments by means of microwave energy is proposed. Sediment samples were irradiated with microwaves in a closed vessel system while immersed in hexane-acetone （1 ： 1, v/v）. The sample extracts were cleaned up using solid phase extraction with Florisil as adsorbent. Pesticides were eluted with hexane-ethyl acetate （80 ： 20, v/v） and determined by gas chromatographic separation with electron capture detection. Three oven programs were assayed with two different solvent mixtures in order to achieve adequate experimental conditions for the complete extraction of organochlorine pesticides from the matrix. Different variables such as the composition of extraction solvent,     

基于广义Hough变换的不规则形状目标提取方法

提出了一种基于广义Hough变换的不规则形状目标的提取方法。该方法主要包括目标参数描述和目标提取两部分。实验表明，该方法精度好、效率高。     

Identification of ore extraction and metal working in ancient times: a case study of Sagalassos (SW Turkey)

The extensive territory of the ancient (Hellenistic to Byzantine) city of Sagalassos (SW Turkey) offered a rich variety in natural mineral resources. The frequent occurrence of iron slag in the excavations at the site proved the local working of metal. A geochemical prospection campaign was done in the territory of the ancient city in order to identify or discard the city and its territory as a self-sustaining metallurgical centre. Secondly, the geochemical impact of ancient metallurgy was investigated. Geochemical anomalies identified in stream sediments are explained by the presence of mineralised deposits and ancient metal working. Mg, Cr, Co and Ni anomalies point to chromite and chrysotile-magnetite deposits related to the basic rocks of the Lycian nappes in the area. Fe, V and Ti anomalies indicate the presence of iron mineralisations, which have been worked for iron production in ancient times. Finally, the association of P, Cu, Pb, Mn, As and Ag anomalies are an indicator of human activity at archaeological sites. Within the framework of this geochemical prospection, a metal working site apart from the city of Sagalassos was identified. Here, ore was both extracted and processed to workable iron.     

Transformation of Residuals to Avoid Artifacts in Geostatistical Modelling with a Trend

Trend modelling is an important part of natural resource characterization. A common approach to account for a variable with a trend is to decompose it into a relatively smoothly varying trend and a more variable residual component. Then, the residuals are stochastically modelled independent of the trend. This decomposition can result in values outside the plausible range of variability, such as grades below zero or ratios that exceed 1.0. We transform the residuals conditional to the trend component to explicitly remove these complex features prior to geostatistical modelling. Back transformation of the modelled residual values allows the complex relations to be reproduced. A petroleum-related application shows the robustness of the proposed transformation. Furthermore, a mining application shows that when this conditional transformation is applied to the original variable, instead of the residual, simulated values are assured to be nonnegative.     

Calcified roasting-acid leaching process of vanadium from low-grade vanadium-containing stone coal

The low-grade vanadium-containing stone coal used in this experiment was collected from Wuxi Coun- try, Chongqing City, China. The experiment focused on the vanadium recovery from roasted residue through opti- mizing the process conditions of an effective and environmentally-friendly technology, named calcified roast- ing-sulfuric acid leaching technology. By single-factor experiments and orthogonal experiments, the effects of roast- ing temperature, roasting time, sulfuric acid concentration and leaching time on the leaching ratio of vanadium were analyzed. The results showed that the leaching ratio of vanadium reached 85.5% under the proper technological con- ditions of roasting temperature=950℃, roasting time=4 h, 40% concentration of sulfuric acid and leaching time=6 h.     

小体积萃取-石墨炉原子吸收法测定高纯硝酸钡中纳克级重金属元素

本文研究了石墨炉原子吸收光谱法测定高纯硝酸钡中超痕量重金属元素的分析技术。提出在大量钡基体存在时,采用小体积萃取体系APDC-MIBK同时萃取纳克级的Fe、Cu、Co和Ni。该法具有灵敏度高、无干扰、操作方便和减少沾污等特点。方法检出限为:Fe 7.2ng/g、Cu 12.8ng/g、Co 4.4ng/g和Ni 6.7ng/g。应用于红外光纤原料硝酸钡、硝酸铝中痕量重金属的测定,效果良好。     

Analytical perspective on trace element species of interest in exploration

Analysis of soil and sediment samples, using selective extraction methods to distinguish different phases, is of particular interest in exploration geochemistry to locate deeply buried mineral deposits. There are various mechanisms of binding labile elements in the secondary environment, including physical and chemical sorption, precipitation, chelation and complexation. Phases present in soils and sediments which are likely to scavenge ‘free' elements include amorphous Mn and Fe oxides, the humic and fulvic components of humus, and clays. This paper reviews these forms of trace elements and the methods in current use to quantify them. Examples of precision data, both for control and survey samples, are given with respect to trace elements dissolved from the ‘soluble organic' component of humus, Mn oxides and amorphous Fe oxides. The high sensitivity of inductively coupled plasma mass spectrometry (ICP–MS) is required to measure accurately and precisely a large suite of trace elements, especially where only small fractions of elements are dissolved by such leaches as the commercially available Enzyme and MMI (Mobile Metal Ion) extractions. The relative standard deviations (RSD) obtained for 33 elements (e.g. Ag, Cd, In, I) in the standard reference sample (SRM), TILL-2, are in the range 0.5–8% for the hydroxylamine hydrochloride (NH₂OH·HCl) leach designed to extract hydrous Fe and Mn oxides. The corresponding RSDs for elements in the reactive Mn oxide phase extracted by the Enzyme leach are in the range 3–19% except for some trace elements at levels close to detection limit (e.g. Cd, Bi). The RSDs obtained for field duplicates are inferior to those for analytical replicates (i.e. sample splits), probably a reflection of different concentrations of the host phase. In one soil survey, the Fe extracted by a 0.25 M NH₂OH·HCl leach ranged conservatively from 0.2 to 1.7% whereas the Mn extracted by the Enzyme leach varied extensively, from 0.3 to >999 ppm. In contrast, precision, at 1–7% RSD, for field duplicates was found to be comparable with that for both analytical duplicates and the SRM, LKSD-4, for elements associated with the humic and fulvic component of humus samples sieved to <177 μm.     

我国月降水和气温网格点资料的处理和分析

用逐步搜索逼近法的客观分析技术计算出１９５１－１９９２年中国月降水量和月平均气温的格点资料，并利用图象识别原理对格点值和站点观测值进行了比较。     

Valency Study of Vanadium in Stone Coal Ash of Jiangxi Province

Vanadium-bearing stone coal is a new vanadium resource;recovery ofV_2O_5 from the coal has been investigated.It has been found that a satisfactoryextraction of V_2O_5 depends on both the oxidation of V and its reaction with so-dium salt.V in the coal ash of Yushan mainly exists in two oxidation states:98％V(Ⅲ)and2％V(Ⅳ).The distribution of valency of V shows that organicmatter determines V valency at low temperatures,at about470℃,V(Ⅲ)iscompletely oxidized to V(Ⅳ);above500℃,the temperature is the most impor-tant factor for the oxidation of V .At higher temperatures no more V is oxidizedto V(Ⅴ);an equilibrium is established after92％of V is oxidized to V(Ⅴ).The roles of NaCl in the recovery of V_2O_5 from the coal ash were discussed.The best conditions for roasting are temperature750-800℃for1 h.underthe oxidation-chlorination atmosphere.When the ore:NaCl=100:10 by weight,η_roast reaches85.5％.According to the results,a flowsheet for V_2O_5 extrac-tion from coal ash has been proposed.