雾化进样石墨炉原子吸收光谱法的研究 Ⅰ.直接雾化进样装置及其性能

介绍一种自行设计和加工的直接雾化石墨炉进样装置的结构、工作原理和操作方法。该装置由微机控制与石墨炉加热程序同步工作,可以实现自动控制和自动测量。对雾化进样石墨炉分析的仪器参数和实验条件进行了研究和选择。结果表明,该装置与石墨炉结合具有自动化程度高、重现性好、样品利用率高和分析速度快等特点。     

塞曼石墨炉原子吸收法直接测定海水中的铬

海水基体对Cr有增感作用。本文研究了抗坏血酸、柠檬酸三铵、酒石酸、乙酸铵等有机基体改进剂对消除基体干扰效果。前二者均有效地消除基体干扰,但1％抗坏血酸 1％柠檬酸三铵混合试剂的效果更好,它不仅可以消除基体干扰,还可降低背景及噪声,Cr的吸收峰也较平滑。本法准确,相对偏差在0.7—4.4％范围内。回收率在92—109％范围内。若海水Cr含量低于定量下限时,可采用多次进样法。     

成像光谱矿物填图精度兼与矿物丰度关系初探

成像光谱遥感技术在岩石矿物识别和矿物填图方面发挥着越来越大作用,而成像光谱矿物填图的精度问题一直是研究的焦点。文章利用高光谱数据HyMap对新疆东天山地区的矿物填图结果,通过引入矿物填绘分布强度的概念,探索性的分析了成像光谱矿物填图与填绘矿物丰度的关系。     

激光剥蚀等离子体质谱分析中激光剥蚀参数对信号响应的影响

探讨了激光剥蚀等离子体质谱固体微区分析中激光剥蚀参数对元素分析信号灵敏度及稳定性的影响。这些参数包括激光功率、脉冲频率、剥蚀孔经、散焦距离、剥蚀方式等。讨论了优化的激光剥蚀等离子体质谱信号采集及数据处理方式。在全质量范围内选用具有代表性的元素作为研究对象,建立了激光剥蚀的一般性特征规律和266nm紫外激光系统的最佳操作条件。在选定的激光剥蚀参数下,大多数被测元素的检出限为22.8~457ng/g,能够满足固体微区分析的要求。     

Surface chemical analysis in coal preparation research: complementary information from XPS and ToF-SIMS

The application of X-ray photoelectron spectroscopy (XPS) to coal surface characterisation for preparation research is described. Progress towards the acquisition of complementary surface chemical information by time-of-flight secondary ion mass spectrometry (ToF-SIMS) is also discussed. Surface-based beneficiation techniques such as flotation are assuming greater importance as the proportion of fines in raw coal increases due to the proliferation of high capacity mining methods. A necessary condition for the floatability of a coal particle is adequate hydrophobicity, and the degree of hydrophobicity of the flotation concentrate is one factor influencing the ease with which its dewatering can be affected. The hydrophobicity of a coal is very difficult to measure directly because of microporosity, and it is often necessary to deduce the degree of hydrophobicity from a knowledge of the surface chemistry. XPS is able to provide sufficient analytical data to allow relative levels of hydrophobicity to be estimated. In principle, ToF-SIMS should be able to supply additional information enabling refinement of such estimates; however, there are insufficient data at present to allow the ionic fragments detected to be related to specific functional groups at the coal surface.     

广西第三代1∶50万数字地质图特点及其意义

文章扼要介绍了广西第三代 1∶5 0万数字地质图的主要内容、特点及编图新理论和新技术 ,并指出该项成果所具有的科学意义和实用价值。     

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。     

高温密闭溶样电感耦合等离子体质谱准确测定辉钼矿铼-锇地质年龄

采用Carius管高温密闭溶样,电感耦合等离子体质谱(ICP MS)法对采自两个不同金属矿床的辉钼矿样品的Re Os同位素地质年龄进行了准确测定。所得出的Re Os年龄的平均值分别为14.26±0.19Ma和34.39±0.81Ma,相对标准偏差分别为1.3%(以2s计算,n=6)和2.4%(以2s计算,n=7)。采用国际通用的ISOPLOT软件按Model1模式对这两组样品分别进行处理,所得Re Os等时线年龄分别为14.32±0.46Ma和34.52±0.38Ma(均为95%置信水平)。同批次样品中所带的内部管理样JDC的Re Os年龄与国际先进实验室采用负离子热表面电离质谱测量所得的结果吻合也较好。说明在严格的质量体系保证及有效地降低实验室空白水平的前提下,ICP MS完全可以准确地测定辉钼矿的Re Os年龄。     

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.     

二连盆地与地沥青密切相关的砂岩型铀矿床微观矿物特征及成因分析

内蒙古二连盆地产在下白垩统碎屑岩系中的砂岩型铀矿床,其矿化与地沥青密切相关,有铀矿物存在之处必有地沥青;岩石中也普遍含地沥青。笔者通过蚀刻α径迹示踪,对铀含量在(200~1770)×10~(-6)的碎屑岩进行扫描电镜分析,采用分子量计算方法确定了该地区含铀碎屑岩中的铀是以多种超显微铀矿物形式存在。其中,以赛汉高毕铀矿床为代表,铀主要形成复成分磷钙铀矿。其它铀矿床也普遍有复成分磷钙铀矿产出:巴彦乌拉矿床样品因钙含量低、硅含量高,则铀石多于复成分磷钙铀矿;道尔苏矿床以铀石和磷铀矿为主,有少量沥青铀矿及复成分磷钙铀矿;哈达图矿床主要是沥青铀矿,未见复成分磷钙铀矿。除了地沥青之外,各矿床中与铀矿物共生的主要矿物还有草莓状、鲕粒状黄铁矿。由此推断,铀矿床的可能成因是:来自盆地深部的UH_3、PH_3、CaH_2、SiH_4、FeH_2、H_2S等在伴随油气向上运移过程中,由于温度、压力降低和氧化作用而发生分解及凝聚,形成草莓状、鲕粒状黄铁矿;同时派生出含U、P、Si、Ca等的氧化物的低温热水溶液,并最终结晶析出铀矿物,形成有大量黄铁矿共生的铀矿体;而油气经过长期挥发,最终演变成地沥青,成为铀矿物的载体。