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电解二氧化锰废渣中的重金属元素在雨水淋滤下,通过地表径流对下游水生态系统及农业生态系统造成不同程度的环境污染和安全隐患,因此,准确测定电解二氧化锰废渣浸出液中的重金属元素含量具有重要的现实意义。电解二氧化锰废渣浸出液中的重金属元素含量通常很低,采用原子吸收光谱法、电感耦合等离子体发射光谱法测定,检出限通常难以满足测定要求。采用电感耦合等离子体质谱法(ICP-MS)测定,消除复杂质谱干扰面临挑战。本文采用电感耦合等离子体串联质谱(ICP-MS/MS)测定电解二氧化锰废渣浸出液中的重金属元素含量。电解二氧化锰废渣中6种重金属元素Cr、Ni、As、Cd、Hg、Pb经硫酸和硝酸混合酸浸出后直接采用ICP-MS/MS进行测定,利用串联质谱的O_2反应模式消除分析过程中Cr、Ni、As、Cd受到的质谱干扰,通过考察不同分析模式下~(52)Cr、~(60)Ni、~(75)As、~(111)Cd的背景等效浓度(BEC),评价质谱干扰对分析结果的影响。结果表明:在MS/MS模式下选择O_2为反应气,采用质量转移法和原位质量法可以消除~(52)Cr、~(60)Ni、~(75)As、~(111)Cd的所有质谱干扰。Cr、Ni、As、Cd、Hg、Pb检出限分别为3.06、9.31、3.50、2.72、2.03、1.89ng/L,加标回收率在95.6%～106.2%之间,相对标准偏差(RSD)≤3.9%。所建立的方法已应用于电解二氧化锰废渣浸出液中重金属元素的测定。 相似文献
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碰撞反应电感耦合等离子体质谱法直接测定卤水中的溴碘 总被引：2，自引：2，他引：0
目前使用电感耦合等离子体质谱法(ICP-MS)测定环境水样中的溴和碘,方法较为成熟,但应用于高盐卤水中溴碘的检测研究很少见报道.本文针对柴达木盆地盐湖卤水矿化度高、钾含量高的特点,建立了ICP-MS直接测定卤水中溴和碘的方法.采用碰撞反应接口(CRI)模式,以H2为碰撞气体,降低了检测过程中的多原子离子质谱干扰(例如39K40 Ar+对79Br+的干扰);选用Rh作内标元素,校正高盐样品引起的基体效应、仪器漂移等非质谱干扰;通过延长快泵冲洗时间消除测定过程中的记忆效应.在优化的实验条件下,盐湖卤水样品稀释200倍后用ICP-MS测定,方法检出限溴为0.036μg/mL,碘为0.027 μg/mL;方法精密度(RSD,n=12)溴为2.77％,碘为2.19％;加标回收率溴为91.6％ ～ 106.1％,碘为94.4％ ～ 107.7％.本方法也可应用于钾含量高的岩盐样品中溴和碘的测定. 相似文献
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超纯水(Ultrapure Water,UPW)在痕量元素分析中通常被用来稀释样品、清洗仪器和实验器皿等。对于超纯水中痕量元素的准确分析则取决于仪器是否有足够低的检出限和较高的分析通量。电感耦合等离子体质谱法(ICP-MS)可多元素同时检测,分析速度快,特别是对测超痕量级元素(ng/L或g/L)具备优越的检测性能,因而成为化学品质量控制中一种必不可少的分析手段[1]。在常规等离子体条件下,氩与样品基体之间会形成大量的多元素干扰,例如38Ar1H对39K的干扰,40Ar对40Ca的干扰,40Ar16O对56Fe的干扰等。冷等离子体技术已经被证明对基于氩基体的干扰是有效的。相对于常规等离子体,冷等 相似文献
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微波消解电感耦合等离子体质谱法测定地球化学样品中钒铬镍锗砷 总被引：6，自引：0，他引：6
地质样品中多种元素的分析,通常采用高压密封消解电感耦合等离子体质谱法(ICP-MS),而应用于测定地球化学样品中的V、Cr、Ni、Ge、As等元素,影响分析准确度的主要原因有:样品前处理方面,高压密封罐会释放Cr和Ni污染样品,同时Ge和As属于易挥发元素容易造成损失;质谱测定方面,多原子分子离子会产生干扰。本文针对两方面的干扰因素,对比了微波消解硝酸提取、微波消解王水提取、高压密封硝酸复溶、高压密封王水复溶四种前处理方法中待测元素的溶出效果以及污染或损失情况。结果表明,采用微波消解替代高压密封罐消解可消除引入的Cr、Ni污染,避免了Ge、As挥发损失,同时微波消解的时间短。而采用硝酸提取,由于避免了氯的引入,分析效果优于王水提取。且使用八极杆ICP-MS氦气碰撞模式消除了样品基体中的氯多原子分子离子干扰(如37Cl14N对51V干扰,35Cl16OH对52Cr干扰,35Cl37Cl对72Ge干扰以及40Ar35Cl对75As干扰等)。应用微波消解硝酸提取、ICP-MS测定岩石、水系沉积物和土壤国家标准物质,V、Cr、Ni、Ge、As的检出限分别为1.09、0.19、0.55、0.02、0.50μg/g,精密度(RSD)4%,而采用高压密封消解、ICPMS测定V、Cr、Ni的检出限为3.48、13.09、21.67μg/g(Ge和As由于挥发无法用此法检测)。运用微波消解硝酸提取-ICP-MS氦气碰撞模式测定地球化学样品中V、Cr、Ni、Ge、As,简化了分析流程,样品消解时间仅2 h,相比于高压密封方法(消解时间48 h)具有消解快速、多元素同时测定、检出限低的特点。 相似文献
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微波消解-电感耦合等离子体质谱法测定煤中的硼 总被引：3，自引：3，他引：0
煤中硼的准确测定对于研究成煤的沉积环境具有重要意义。微波消解-电感耦合等离子体质谱(ICP-MS)可以有效地测定煤中的大部分微量元素,但由于硼易挥发等特殊的物理化学性质,致使硼的测定过程较为繁琐,测试结果不够准确。本文对微波消解ICP-MS测定煤中硼含量的分析方法进行了改进。样品中加入磷酸、硝酸和氢氟酸,用微波消解仪消解完全,置于电热板加热赶酸完毕后用硝酸提取。硼的卤化物易挥发,磷酸的加入使硼与磷酸结合生成难挥发的稳定络合物,起到了固硼的作用。ICP-MS测定中采用铍作为内标,通过在线加入的方式有效地补偿了基体效应产生的影响;用稀氨水冲洗进样系统,很好地降低了硼的记忆效应;选择高分辨率模式来测定,避免了12C和40Ar4+等质谱峰的干扰。方法的仪器检出限(0.22ng/mL)和方法检出限(0.34 ng/mL)较低,方法精密度(RSD)小于0.6%,灵敏度高,且测定标准样品的准确度良好。该方法简单快速,适用于批量分析煤样中硼的含量。 相似文献
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电感耦合等离子体质谱法测定土壤重金属普查样品中铬铜镉铅的关键环节研究 总被引：10，自引：8，他引：2
土壤重金属普查样品的基质复杂、数量大、待测元素性质各异,现有土壤中重金属的电感耦合等离子体质谱法(ICP-MS)存在样品分解方式不适宜、上机测定参数需优化等问题。本文采用电热板-酸分解样品,研究了ICP-MS测定土壤中Cr、Cu、Cd、Pb四种主要重金属在分解和上机测定中的关键环节。结果表明采用"硝酸+盐酸+氢氟酸+50%硫酸"体系,样品分解完全且待测元素无损失,并使用工作曲线校准仪器可降低基体效应;优选质谱测定同位素和采用碰撞反应池或数学校正可减少质谱干扰;质谱积分驻留时间和重复次数对痕量元素Cd的精密度有较大影响,宜设为0.4 s和3次。本方法对Cr、Cu、Cd、Pb的检出限分别为1.74、0.89、0.015、0.08μg/g,为普查工作提供了一种可借鉴的分析手段。 相似文献
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研究了微波消解-电感耦合等离子体质谱（ICP-MS）测定玉米中重金属元素的方法。详细讨论了微波样品溶液制备、质谱仪干扰扣除及校准等,在优化的试验条件下,根据国家标准参考物质（GBW10012）的分析结果评价方法的准确性。方法检出限为：Cd：0.003μg/g,Cr：0.04μg/g,Pb：0.1μg/g,相对标准偏差在2.5%-6.0%之间,加标回收率在90.9%-104.9%之间。 相似文献
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琼北火山岩激光40Ar/39Ar定年研究 总被引：1，自引：1，他引：0
新生代以来,雷琼地区多次、大量地喷发了一系列火山岩。前人主要基于K-Ar法对此划分了期次。本文采用激光40Ar/39Ar年代学方法,对琼北火山岩区进行了精细定年研究。低本底激光40Ar/39Ar法能够对低钾含量,极少量样品(毫克级)进行精细测定,非常适合极年轻火山岩的定年工作。结果显示的火山岩激光40Ar/39Ar法高质量数据表明琼北火山喷发活动时限跨越1.3～0.052Ma。在比较了表观年龄与等时线年龄差异之后,本文给出了年龄推荐值。正如测试数据所显示,本地区新生代火山岩普遍存在40Ar和36Ar过剩的问题,此时只有等时线年龄才代表喷发的真实年龄。 相似文献
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Cosmogenic nuclide concentrations measured on abandoned fan surfaces along the Mojave section of the San Andreas Fault suggest that sediment is generated, transported, and removed from the fans on the order of 30-40 kyr. We measured in situ produced cosmogenic 10Be, and in some cases 26Al, in boulders (n = 15), surface sediment (n = 15), and one depth profile (n = 9). Nuclide concentrations in surface sediments and boulders underestimate fan ages, suggesting that 10Be accumulation is largely controlled by the geomorphic processes that operate on the surfaces of the fans and not by their ages.Field observations, grain-size distribution, and cosmogenic nuclide data suggest that over time, boulders weather into grus and the bar sediments diffuse into the adjacent swales. As fans grow older the relief between bars and swales decreases, the sediment transport rate from bars to swales decreases, and the surface processes that erode the fan become uniform over the entire fan surface. The nuclide data therefore suggest that, over time, the difference in 10Be concentration between bars and swales increases to a maximum until the topographic relief between bars and swales is minimized, resulting in a common surface lowering rate and common 10Be concentrations across the fan. During this phase, the entire fan is lowered homogeneously at a rate of 10-15 mm kyr−1. 相似文献
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Constraints from strontium and neodymium isotopic ratios and trace elements on the sources of the sediments in Lake Huguang Maar 总被引：4，自引：0，他引：4
Houyun Zhou Bo-Shian Wang Huazheng Guan Yi-Jen Lai Chen-Feng You Jinlian Wang Huai-Jen Yang 《Quaternary Research》2009,72(2):289-300
The sediments in Lake Huguang Maar in coastal South China were previously thought to originate mainly from wind-blown dust transported from North China, such that the lake sediments recorded the varying strength of the Asian winter monsoon. An alternative explanation was that the local pyroclastic rocks supplied the lake sediments, but the actual contributions from the different sources remained unclear. Geochemical analyses including 87Sr/86Sr and 143Nd/144Nd and trace elements support the local pyroclastic rock as the dominant source: < 22% of the total Sr in the lake sediments and 17% of the Nd arises from the distant source. Nb/Ta and Zr/Hf for the lake sediments are identical to those for the local rock but differ from the ratios for the wind-blown dust, and chondrite-normalized rare earth element patterns for the lake sediments are similar to those for the local rock and soil, but differ from those for the distant source. The sediments in Lake Huguang Maar are probably input into the lake through runoff and thus controlled by the hydrology of the lake. Wind-blown dust transported by the Asian winter monsoon from arid North China is only a minor contribution to the sediments. 相似文献
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对具有不同地质历史背景的3类40Ar/39Ar法样品中的40Ar和39Ar释出特征进行对比,研究结果表明,40Ar/39Ar法样品中的40Ar、39Ar释气曲线主要表现为以下3种形式:完全重合型、过剩氩型和不规则型。当40Ar与39Ar释气曲线呈完全重合型时,40Ar/39Ar法全熔年龄代表了岩体的形成年龄;当40Ar、39Ar释气曲线是过剩氩型时,40Ar/39Ar法全熔年龄则大于岩体的形成年龄;当40Ar与39Ar释气曲线呈不规则型时,表明样品中的放射成固氩(40Ar*)发生了丢失,其全熔年龄一般较岩体的形成年龄小。对于40Ar、39Ar释气曲线呈过剩氩型的样品,40Ar/39Ar法年龄谱通常呈马鞍形,且马鞍形年龄谱的底部年龄一般都具有地质意义,代表了岩体的形成年龄。对于40Ar、39Ar释气曲线呈不规则型的样品,对其年龄谱的解释应持谨慎态度。 相似文献
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H. Knicker G. Almendros F. J. Gonzlez-Vila H. -D. Lüdemann F. Martin 《Organic Geochemistry》1995,23(11-12)
A variety of fungal melanins with natural 15N abundance are characterized by solid-state 13C and 15N NMR spectroscopy and are compared to solid-state 13C and 15N NMR spectra of organic matter from representative soils. In all solid-state 15N NMR spectra the peptide/amide region (−220 to −285 ppm) dominates with more than 70% of the total intensity. The region between −285 and −375 ppm, assigned to amino and ammonium groups, always contains more than half of the remaining intensity. The area in the region from −30 to −220 ppm, where aromatic heterocycles would show signals, makes up less than 10% of the total intensity. These findings call into question common structural models for melanins. The solid-state 13C NMR spectra, on the other hand, reveal large differences when the melanins are compared to each other, and to composts and soils. The concentration of the aromatic carbon varies from 5 to 40% in the melanin series. The ratio Caro/Ntot and Cali/Ntot were calculated, and confirm that nitrogen in these samples is bound in Ca-groups rather than in aromatic heterocyclic structures. 相似文献
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The ^190Pt-^186Os system should be a unique tracer for mantle processes be-cause both Pt and Os are concentrated in the mantle.The ^190Pt-^186Os system will also be a good supplement to the ^187Re-^187Os system for dating and tracing mantle pro-cesses because the ^190Pt-^186Os system is not so easily contaminated by crustal materials as the ^187Re-^187Os system.In turn,the application of the ^187Re-^187Os system to Pt-enriched materials uncontaminated by crustal materials will indirectly refine the half life of ^190Pt.The ^190Pt is refined.In the coupled ^187Re-^187Os and ^190Pt-^186Os sys-tematics,an ^186Os*/^190Pt-^187Os*/^187Re Concordia diagram similar to the ^206Pb*/^238U-^208Pb*/^232Th Concordia can be constructed.In such a Concordia diagram,a date will be obtained so long as the ^190Pt-^186Os system remains closed even if the ^187Re-^187Os sys -tem is contaminated by crustal materials.In addition ,for the coupled ^190Pt-^186Os and ^187Re-^187Os systematics,the mantle processes and the interactions between the mantle and the crust will be described by two ratios:^186Os/^188Os and ^187Os/^188Os .The coupled ^187Re-^187Os and ^190Pt-^186Os systematics will be a powerful tool in the investigation of the geodynamic history of the Earth because the ^187Re-^187Os system is sensitive to the interactions between the mantle and the crust,while the ^190Pt-^186Os system is a good tracer for mantle processes. 相似文献
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The ground waters circulating in the Apulian mesozoic carbonate aquifer, of coastal type, show high concentrations of 222Rn everywhere. Considering their variation during the different phases of a hydrological year, such high concentration values can reach activity of 20 Bq/L, in the more internal zones of the aquifer. Moreover, it is often observed that, in correspondence of wells and springs nearest the coast, the concentrations of radioactive gas reach values greater than 400 Bq/L and vary considerably during the course of a day and with withdrawals. The research carried out over the last few years, has confirmed that 226Ra and 222Rn concentrations in the karst groundwater of Apulia, are mainly related to the occurrence of Terra Rossa inside the aquifer and the capacity of these paleosols to fix the salts of 226Ra coming from the dissolution of the calcareous and calcareous-dolomitic rocks. This paper shows the results of the analysis performed to define 222Rn increase in the brackish waters that come in contact with carbonate rocks and terra rossa. It also indicates the results of surveys performed in a coastal zone with well-known hydrogeological features. The controls performed during one hydrological year, have confirmed the relationships between the salt content of the ground waters and the enrichment of 222Rn and have highlighted that the manner of increase of this radioisotope is related to cases of ionic exchange and adsorption regulated by the dynamics of marine intrusion. 相似文献
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Mark Quigley Yu Liangjun Liu Xiaohan Christopher J.L. Wilson Mike Sandiford David Phillips 《Tectonophysics》2006,421(3-4):269-297
Structural and thermochronological studies of the Kampa Dome provide constraints on timing and mechanisms of gneiss dome formation in southern Tibet. The core of Kampa Dome contains the Kampa Granite, a Cambrian orthogneiss that was deformed under high temperature (sub-solidus) conditions during Himalayan orogenesis. The Kampa Granite is intruded by syn-tectonic leucogranite dikes and sills of probable Oligocene to Miocene age. Overlying Paleozoic to Mesozoic metasedimentary rocks decrease in peak metamorphic grade from kyanite + staurolite grade at the base of the sequence to unmetamorphosed at the top. The Kampa Shear Zone traverses the Kampa Granite — metasediment contact and contains evidence for high-temperature to low-temperature ductile deformation and brittle faulting. The shear zone is interpreted to represent an exhumed portion of the South Tibetan Detachment System. Biotite and muscovite 40Ar/39Ar thermochronology from the metasedimentary sequence yields disturbed spectra with 14.22 ± 0.18 to 15.54 ± 0.39 Ma cooling ages and concordant spectra with 14.64 ± 0.15 to 14.68 ± 0.07 Ma cooling ages. Petrographic investigations suggest disturbed samples are associated with excess argon, intracrystalline deformation, mineral and fluid inclusions and/or chloritization that led to variations in argon systematics. We conclude that the entire metasedimentary sequence cooled rapidly through mica closure temperatures at 14.6 Ma. The Kampa Granite yields the youngest biotite 40Ar/39Ar ages of 13.7 Ma immediately below the granite–metasediment contact. We suggest that this age variation reflects either varying mica closure temperatures, re-heating of the Kampa Granite biotites above closure temperatures between 14.6 Ma and 13.7 Ma, or juxtaposition of rocks with different thermal histories. Our data do not corroborate the “inverse” mica cooling gradient observed in adjacent North Himalayan gneiss domes. Instead, we infer that mica cooling occurred in response to exhumation and conduction related to top-to-north normal faulting in the overlying sequence, top-to-south thrusting at depth, and coeval surface denudation. 相似文献