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1.
邻二氮菲分光光度法测定碳酸盐相中微量亚铁 总被引：2，自引：2，他引：2
建立了在超声波作用下，HAc—NaAc缓冲溶液和邻二氮菲选择性溶解分光光度法直接测定碳酸盐相中微量亚铁的方法。结果表明，在适宜条件下，含2g／L邻二氮菲的HAc—NaAc缓冲溶液（pH3）可选择性溶解并络合碳酸盐相中的Fe（Ⅱ），通过加入EDTA溶液有效地抑制了Fe（Ⅲ）的光还原作用。常见含铁矿物如赤铁矿、磁铁矿及硅酸盐等均对碳酸盐中Fe（Ⅱ）的测定无干扰。样品经30％的H2O2浸泡、过滤、晾干预处理，能有效地消除黄铁矿和有机物的干扰。方法用于石灰岩国家一级标准物质的测定，结果与标准值相符。 相似文献
2.
石煤是一种可综合利用的矿产资源,提取石煤中钒、钼、镍等金属是其综合利用之一.石煤在发电燃烧过程中钒的物相发生显著变化,而钒物相的变化对钒的可浸出性产生较大的影响.笔者采用选择性连续提取方法对四川某地石煤原矿和石煤飞灰进行分析研究,发现石煤原矿中钒主要存在于硅铝酸盐相和有机质相中,部分存在于铁锰氧化物相及吸附态中,极少部分存在于碳酸盐相中.而石煤发电飞灰中钒主要存在于有机质相、硅铝酸盐相和铁锰氧化物相中,少量的钒以吸附态形式赋存.燃烧过程中石煤的各种含钒矿物发生离解,其中的钒得到释放并被氧化成高价态.高价钒一部分与Na、Cl等结合生成可溶性化合物,形成吸附态的钒;另一部分与Fe、Na、Ca等发生反应生成难溶性化合物,并以一定形式富集在飞灰的有机质相、硅铝酸盐相和铁锰氧化物相中. 相似文献
3.
电感耦合等离子体质谱法测定砂岩型铀矿样品中分步提取的铀 总被引：1，自引：0，他引：1
本文研究地质样品中铀形态的分析方法及应用技术,以进一步说明铀形态分析在地球化学找矿中的重要作用。该方法参考Tessier流程,将样品中的铀分为可交换离子态、碳酸盐结合态、铁锰氧化物结合态、硫化物及有机物结合态和结晶态,分别提取,提取溶液用高分辨率电感耦合等离子体质谱仪进行测量。设计的形态提取配方具有良好的可选择性和可重复性,经过国家标准物质、国际形态标准物质和人工模拟样品验证,证明形态提取试剂配方适合所定义的形态分析。通过对实际样品(总量铀为635μg/g)验证表明,碳酸盐结合态铀提取结果的可重复性最好(RSD为2.6%),其次为硫化物及有机物结合态铀(RSD为4.0%)、结晶态铀(RSD为6.0%)和铁锰氧化物结合态铀(RSD为6.1%),可交换离子态铀提取结果的可重复性最差(RSD为26%)。碳酸盐结合态铀与结晶态铀之比,可以用于反映地下铀矿的存在概率。 相似文献
4.
在乙醇存在下,以偶氮胂Ⅲ为指示剂,乙二胺、磺基水杨酸为掩蔽剂,EDTA容量法直接测定稀土萃取分离工艺负载有机相中稀土浓度。省去了有机相的反萃取分离过程,提高了测定的准确度。对不同浓度的稀土有机相样品进行测定,其相对标准偏差(n=5)在1.00—0.29％范围。方法适合于环烷酸体系萃取分离稀土元素工艺各级水相、有机相中稀土浓度的直接测定。 相似文献
5.
6.
遵义黄家湾下寒武统底部Mo-Ni-PGE矿中铂族元素赋存形态分析及成因意义 总被引：5，自引：1，他引：5
本项目采用6级不同化学物相形态系统,用化学试剂选择性提取和对比提取相结合的方法,研究了PGE元素及Au的物相分布特点.得出了Ru、Rh、Pd、Os、Ir、Pt及Au在各物相中的含量及相对比率,参照电子探针等对Mo、Ni硫化矿物分析成果,表明PGE在镍的硫化物相中丰度较高外,在可交换态、黄铁矿态及残渣态等中亦有一定分布,显示PGE元素以超微细粒分散赋存特点.表明矿体在沉积时未发生PGE元素的显著成矿分异,成岩期也未出现明显的再次富集作用.此矿床系我国黑色岩系中确凿伴生有PGE矿的典型代表,铂族元素赋存状态研究对其成因、寻找和开发有关键意义. 相似文献
7.
建立了用单道扫描电感耦合等离子体发射光谱法测定珊瑚礁中主量和微量元素的方法。珊瑚礁样品经酸溶解后,直接进行Ca、Mg、K、Na、V、Sr、Ba、Co、Ni、Pb、Li、Rb的测定,方法检出限为0.0004～0.1mg/L,精密度RSD<5%(n=6),样品的加标回收率为97%～105%。测定w(CaO)为50%的样品,结果与传统的EDTA容量法相符。方法经碳酸盐岩石国家一级标准物质验证可行,已用于大批量的珊瑚礁样品的测定。 相似文献
8.
提出了超声波提取-火焰原子吸收光谱法测定灰岩中Fe(Ⅱ)的方法,通过对总铁含量进行测定,采用差减法计算Fe(Ⅲ)的含量,从而实现了灰岩中铁的价态分析。探讨了Al2(SO4)3溶液选择性提取岩石样品中微量Fe(Ⅱ)的化学条件及其他仪器参数。结果表明,20~30℃下,0.025 mol/L Al2(SO4)3在土液比1∶300、提取时间1 h条件下可有效提取碳酸盐相中Fe(Ⅱ)离子。该方法用于国家一级标准物质中Fe(Ⅱ)和Fe(Ⅲ)的测定,测定结果与推荐值吻合。运用本法对实际地质样品中的总铁和Fe(Ⅱ)进行分析测定,加标回收率分别为96.07%~103.23%,95.79%~102.11%。 相似文献
9.
海底沉积物中碳酸钙分析方法的研究 总被引：4，自引：0，他引：4
探讨了海底沉积物中ＣａＣＯ３的测定方法。用１ｍｏｌ／ＬＮａＡｃ＋ＨＡｃ做碳酸盐相＋离子交换相的浸取剂,１ｍｏｌ／ＬＮａＡｃ做离子交换相的浸取液,在沸水浴中３０ｍｉｎ分解样品,然后用ＡＡＳ或ＩＣＰＡＥＳ分别测定离子交换相＋碳酸盐相及离子交换相中的Ｃａ,差减法计算样品中ＣａＣＯ３含量。方法经深海沉积物、水系沉积物等国家标准物质验证,结果与标准值相符。对同一样品进行１２次测定,相对标准偏差小于５％。 相似文献
10.
大气颗粒物中铅的序列提取与分析表征 总被引：2，自引：0，他引：2
用石英纤维滤膜采集大气颗粒物样品,采用序列提取的方法把铅的总量分成环境可迁移态、碳酸盐和氧化物态、有机质和残渣态3个分量,用石墨炉原子吸收分光光度法测定铅的浓度,仪器检出限为1μg/L。对实际大气颗粒物样品进行序列提取,5份平行的序列提取3个分量测定及加和值的RSD分别为7.1%、3.3%、7.3%、5.0%。该样品三级序列提取的加和值(756μg/g)约为总量测定(738μg/g)的102%,两组数据一致性良好,且环境可迁移态、碳酸盐和氧化物态、有机质和残渣态的铅分别为加和值的64%、17%和20%。对几种典型的铅污染源排放样品进行序列提取和分析测定,不同源排放样品的形态特征各有特点,说明该序列提取的方案是可行的,达到了将不同形态的铅化合物分开的目的。 相似文献
11.
Distribution of trace elements in the coastal sea sediments of Maslinica Bay, Croatia 总被引：1，自引：0，他引：1
Nenad Mikulic Visnja Orescanin Loris Elez Ljiljana Pavicic Durdica Pezelj Ivanka Lovrencic Stipe Lulic 《Environmental Geology》2008,53(7):1413-1419
Spatial distributions of trace elements in the coastal sea sediments and water of Maslinica Bay (Southern Adriatic), Croatia
and possible changes in marine flora and foraminifera communities due to pollution were investigated. Macro, micro and trace
elements’ distributions in five granulometric fractions were determined for each sediment sample. Bulk sediment samples were
also subjected to leaching tests. Elemental concentrations in sediments, sediment extracts and seawater were measured by source
excited energy dispersive X-ray fluorescence (EDXRF). Concentrations of the elements Cr, Cu, Zn, and Pb in bulk sediment samples
taken in the Maslinica Bay were from 2.1 to over six times enriched when compared with the background level determined for
coarse grained carbonate sediments. A low degree of trace elements leaching determined for bulk sediments pointed to strong
bonding of trace elements to sediment mineral phases. The analyses of marine flora pointed to higher eutrophication, which
disturbs the balance between communities and natural habitats. 相似文献
12.
锶钡比是常用的海陆相沉积环境判别手段之一,黄河三角洲钻孔沉积物的传统全量锶钡比介于0.45±0.5之间,无法判别其海陆相沉积环境。黄河三角洲钻孔样品的选择性提取结果表明,全样的总量钡和锶中的75%以上的钡和50%以上的锶赋存于与沉积时的海陆相地球化学环境无关的陆源碎屑矿物中,在判别海陆相沉积环境时是应该剔除的。不同选择性提取方法的分析结果表明,黄河三角洲沉积物中的锶除碎屑硅酸盐矿物态外,主要呈现可交换态和碳酸态,赋存形态比较单一;而钡除了碎屑硅酸盐矿物态外其赋存形态复杂。以提取可交换态为主的醋酸钠法和醋酸铵法、以提取可交换态和碳酸盐态为主的柠檬酸法和稀盐酸法及络合剂+稀盐酸法所提取的锶钡比,均能较好地区分黄河三角洲的海陆相沉积环境。来自黄土的黄河三角洲物源的高碳酸钙和醋酸不能提取重晶石中钡的双重特殊性,导致黄河三角洲沉积物稀醋酸法提取的结果具有高锶低钡的特征并造成锶钡比偏高,尽管其锶钡比都大于1.0,但其对沉积时盐度环境的响应灵敏度大于其他选择性提取方法。选择性提取方法是解决目前传统的全样总量锶钡比海陆相沉积环境判别效果不佳问题的唯一有效手段。 相似文献
13.
Backfills of dredged sediments onto a former sand and gravel mine site in Charles City County, VA may have the potential to
contaminate local groundwater. To evaluate the mobility of trace elements and to identify the potential contaminants from
the dredged sediments, a sequential extraction scheme was used to partition trace elements associated with the sediments from
the local aquifer and the dredged sediments into five fractions: exchangeable, acidic, reducible, oxidizable, and residual
phases. Sequential extractions indicate that, for most of the trace elements examined, the residual phases account for the
largest proportion of the total concentrations, and their total extractable fractions are mainly from reducible and oxidizable
phases. Only Cd, Pb, and Zn have an appreciable extractable proportion from the acidic phase in the filled dredged sediments.
Our groundwater monitoring data suggest that the dredged sediments are mainly subject to a decrease in pH and a series of oxidation reactions, when exposed to the atmosphere. Because the trace elements released by carbonate dissolution
and the oxidation (e.g., organic matter degradation, iron sulfide and, ammonia oxidation) are subsequently immobilized by
sorption to iron, manganese, and aluminum oxides, no potential contaminants to local groundwater are expected by addition
of the dredged sediments to this site. 相似文献
14.
M.N. ag&#x;atay 《Journal of Geochemical Exploration》1984,21(1-3)
Selective extraction techniques employing 0.05 M EDTA, 1 M hydroxylamine hydrochloride (Hxl) in acetic acid and 0.157 M ammonium oxalate in oxalic acid were used to assess the mode of occurrence of the trace elements in the various geochemical sample media and to increase the anomaly contrast over the concealed massive ore bodies in the the Eastern Black Sea region of Turkey.In hematitized pumice tuffs, an exhalate horizon overlying the Madenköy massive sulphide ore body, the trace elements such as As, Cu, Zn, Pb and Mo are partly associated with sulphides and partly occur in clays, and Fe- and Mn-oxides.The extraction data on stream sediments suggest that a hot nitric acid attack is the best digestion procedure for detecting mechanical dispersion trains in regional geochemical programmes. Comparison of the extractabilities of metals in soils from mineralized areas with those from the background Sirtköy soils by the different extraction procedures demonstrates that EDTA, and to lesser extent Hxl are the best extraction procedures for increasing the anomaly/background ratio. These two extraction procedures were found to also enhance Zn and Pb anomalies over the cover rocks of the Madenköy massive ore body relative to the largely exposed stockwork-impregnation zones.Among the EDTA, Hxl and ammonium oxalate extractions, only the last procedure extracted considerable amounts of As from the soil samples. Vapor-phase analysis suggests that mercury occurs mainly in sulphide form which is leachable only by ammonium oxalate solution that also leaches adsorbed mercury. The EDTA and the Hxl solutions only extracted adsorbed mercury. These three extractants have no effect on either mercuric oxide or mercuric sulphate. Arsenic, a very useful pathfinder in this region, can only be partly extracted from the pumice tuff and soil samples by ammonium oxalate solution. 相似文献
15.
M. E. Essington 《Environmental Geology》1989,13(1):59-66
A laboratory study was conducted to evaluate the influence of hydration and recarbonation on the solidphase distribution of trace elements in retorted oil shale. The oil shale samples were retorted by the Paraho direct heating process and equilibrated with deionized—distilled water under controlled carbon dioxide conditions. A sequential extraction technique was then used to fractionate trace elements into soluble, KNO3-extractable (easily exchangeable), H2O-extractable (easily adsorbed), NaOh-extractable (organic), EDTA-extractable (carbonate), HNO3-extractable (sulfide), and residual (nonextractable silicate) phases. The chemical fractions present in retorted oil shale and hydrated and recarbonated retorted oil shale were compared to identify trace element mineralogical changes that may occur in retorted oil shale disposal environments.Trace elements examined in this study were found to reside predominantly in the HNO3-extractable and residual fractions. Hydration of retorted oil shale resulted in a shift in the majority of trace elements from residual to extractable forms. Cobalt, nickel, and zinc extractabilities were not significantly influenced by hydration, whereas antimony increased in the residual fraction. Subjecting retorted oil shale to atmospheric (0.033%) and 10% CO2(g) levels over a nine-month equilibration period resulted in partial and full recarbonation, respectively. As the influence of recarbonation increased, trace elements reverted to residual forms. Vanadium, choromium, copper, zinc, antimony, and molybdenum in the 10% CO2(g) recarbonated material were more resistant to sequential extraction than in retorted oil shale, whereas strontium, barium, and manganese were less resistant to sequential extraction. The extractabilities of cobalt, nickel, and lead were not affected by recarbonation. Recarbonation did not result in a predicted increase in EDTA-extractable trace elements. In general, the amounts of trace elements extracted by EDTA (and correlated to carbonate forms) were invariant with respect to equilibrium CO2(g) levels.A significant result of this study was that the mineralogical residencies of trace elements in retorted oil shale were altered in response to conditions that may be present in a disposal environment. Thus, the long-term release of trace elements in retorted oil shale disposal environments may not be adequately predicted by applying the toxicity characteristic leaching procedure (TCLP). 相似文献
16.
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. 相似文献
17.
A sequential extraction procedure, using acid digestion in a CEM MDS-81D® microwave system, is reported for the investigation of trace and minor element associations in coal in (1) mineral phases other than pyrite, (2) pyrite and (3) the organic matrix. The concentrations of sulphate, pyrite and organic sulphur can also be determined by this method. The extract solutions from each stage are rapidly analysed by ICP-AES. The association of major, minor and trace elements with mineral and organic phases is suggested for a suite of certified reference coal samples. In stage 1, a significant percentage of the total Ba, Co, Cr, Cu, Mn, Ni, Pb and Sr was extracted suggesting an association with silicate, carbonate, sulphate and phosphate minerals for these elements. In stage 2, a proportion of the Cu, Mn, Ni, Pb and Zn was dissolved implying the occurrence of these elements in pyrite. An association with the organic matrix is suggested for Cr and also for Ba and Sr in lower rank coals. 相似文献
18.
Adeline CharriauLudovic Lesven Yue GaoMartine Leermakers Willy BaeyensBaghdad Ouddane Gabriel Billon 《Applied Geochemistry》2011,26(1):80-90
Three sediment cores were collected in the Scheldt, Lys and Spiere canals, which drain a highly populated and industrialized area in Western Europe. The speciation and the distribution of trace metals in pore waters and sediment particles were assessed through a combination of computational and experimental techniques. The concentrations of dissolved major and trace elements (anions, cations, sulfides, dissolved organic C, Cd, Co, Fe, Mn, Ni, Pb and Zn) were used to calculate the thermodynamic equilibrium speciation in pore waters and to evaluate the saturation of minerals (Visual Minteq software). A sequential extraction procedure was applied on anoxic sediment particles in order to assess the main host phases of trace elements. Manganese was the most labile metal in pore waters and was mainly associated with carbonates in particles. In contrast, a weak affinity of Cd, Co, Ni, Pb and Zn with carbonates was established because: (1) a systematic under-saturation was noticed in pore waters and (2) less than 10% of these elements were extracted in the exchangeable and carbonate sedimentary fraction. In the studied anoxic sediments, the mobility and the lability of trace metals, apart from Mn, seemed to be controlled through the competition between sulfidic and organic ligands. In particular, the necessity of taking into account organic matter in the modelling of thermodynamic equilibrium was demonstrated for Cd, Ni, Zn and Pb, the latter element exhibiting the strongest affinity with humic substances. Consequently, dissolved organic matter could favour the stabilization of trace metals in the liquid phase. Conversely, sulfide minerals played a key role in the scavenging of trace metals in sediment particles. Finally, similar trace metal lability rankings were obtained for the liquid and solid phases. 相似文献
19.
青岛胶州湾沉积物痕量元素黄铁矿化程度及其剖面类型 总被引：4，自引：0，他引：4
为了探索青岛近海不同沉积环境下不同痕量元素的黄铁矿化规律, 2003年5月潜水员潜入海底采集了4个不同沉积环境的未扰动柱样, 并利用Huerta-Diaz and Morse (1990) 连续提取技术测试分析了沉积物痕量金属的不同存在形式(活性态和黄铁矿结合态) 在垂直剖面上的分布规律.结果表明: 除了在涨潮三角洲上部沉积和潮下带沉积物柱子的Cd和Cr外, 痕量元素的黄铁矿化度的增高取决于其相应剖面上的DOP的增高; 并且不同痕量元素向黄铁矿中转移的规模存在着较大的差别, 即元素As、Hg和Mo转移的规模最大, Cu、Zn、Cd、Cr、Co和Ni中等, Pb和Mn最小; 此外, 还进一步揭示了河流三角洲沉积物的下部各元素的黄铁矿化程度高, 而潮下带沉积物以及涨潮三角洲沉积物低.最后指出在河口水下三角洲进行的清淤工作应注意黄铁矿结合态痕量元素的活化而产生生物有效的毒性元素. 相似文献
20.
对银额盆地石板泉西石炭系白山组碳酸盐岩进行详细的地球化学分析,探讨各特征元素对古环境、古气候的指示意义。地球化学测试结果显示：除样品CH3外,其余样品主量元素中的Al及微量元素中的Ti、Zr、Th等典型陆源特征元素的含量较低,Y/Ho平均值为45.58,反映研究区白山组碳酸盐岩较少受陆源物质输入的影响;δCe与δEu、w（ΣREE）、（La/Sm）N未见良好的相关性,也不具备Eu正异常,说明研究区白山组碳酸盐岩受成岩作用和热液作用的影响也较为有限。碳酸盐岩中所含微量元素主要为海水自生成因,能够反映原始沉积环境。根据特征元素对古水深、古盐度、古气候、古氧相和古水温进行研究,显示研究区白山组碳酸盐岩段虽然岩性较为单一,但其地球化学特征可以反映早晚的沉积古环境差异。研究区白山组碳酸盐岩总体经历了1个大的海侵海退旋回,沉积于正常海水,气候潮湿,弱氧化—弱还原环境,古水温为8.51~27.10℃,早期水温低,晚期水温升高。 相似文献