共查询到19条相似文献，搜索用时 218 毫秒
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湿碱消解-等离子体发射光谱法测定海洋沉积物中的生物硅 总被引：2，自引：1，他引：1
利用湿碱式化学提取技术和电感耦合等离子体发射光谱仪,优化样品碱式消解方法,确定仪器最佳工作条件,建立了测定海洋沉积物中不同含量级别生物硅的方法。结果表明,仪器检出限为0.724μmol/L,方法检出限为0.942μmol/L。用于测定硅酸盐-硅溶液成分分析国家一级标准物质(GBW08648和GBW 08649,标准值分别为50.0μmol/L和100.0μmol/L),测定值分别为(49.888±0.275)μmol/L、(99.578±0.651)μmol/L,相对标准偏差为0.443%、0.527%;对于不同生物硅含量级别海洋沉积物样品的平行、独立测量,其相对标准偏差8.9%。方法快速、简便、准确,可满足古海洋学不同时空尺度气候和环境分析的应用。 相似文献
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碱提取法分析海洋沉积物生物硅方法中碎屑组分污染的评估及校正 总被引：2，自引：0，他引：2
利用电感耦合等离子体质谱 (ICP- MS)和电感耦合等离子体原子发射光谱 (ICP- AES)方法分析了常规碱液提取海洋沉积物中的生物硅所获取的溶液中的 Si、 Al和 Ti含量.分析结果显示 , 碱液提取法获取的溶液中 Si和 Al明显地由两种来源混合而成,其中, Si有较大比例的陆源碎屑成分的贡献,并不能直接代表沉积物中的生物硅含量,而需要对其中的陆源碎屑贡献进行扣除.通常使用 Al来代表陆源碎屑进行扣除的方法无法给出正确结果,因为碱提取液中 Al存在明显的非碎屑组分.对数个土壤及水系沉积物标准样品物质的试验发现,碱提取可以优先溶解其中的 Si和 Al,而提取液中的 SiO2/TiO2比值相对于土壤和沉积物全样的 SiO2/TiO2比值有一个比较固定的富集系数 (约 14左右 ).对南海沉积物而言,根据这个富集系数和区域的碎屑物质的化学组成算得碱提取液中碎屑组分 SiO2/TiO2比值约为 748,这与根据二端员混合估计的比值相当.这样,根据提取液中的 Ti含量可以较好地扣除出碎屑组分对生物硅的污染,对于更准确测定海洋沉积物中低含量的生物硅具有重要意义. 相似文献
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沉积物中有机质及相关元素含量、重金属含量等是研究环境污染和古环境的依据。利用近红外漫反射光谱测定沉积物中的化学成分,方法简便、快捷、价廉。本文概述了近红外漫反射光谱测定沉积物中化学成分的基本流程、样品制备及建模方法,介绍了如何通过选择建模样品、利用光谱预处理及回归分析等方法提高近红外光谱模型的定量能力,综述了近红外漫反射光谱分析沉积物中的有机碳、总氮、总磷、生物硅、重金属含量等方法。但是利用近红外光谱分析沉积物中的化学成分研究起步较晚,仍存在很多问题,有必要深入探讨近红外光谱分析沉积物的化学成分时产生误差的机理,进一步开展建模样品的计算机选择方法、光谱预处理方法和数学模型优化等方面的研究,提高近红外漫反射光谱分析沉积物中化学成分的精密度和准确度。 相似文献
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中国北方第四纪孢粉提取方法研究 总被引：3，自引：0，他引：3
孢粉提取方法是第四纪孢粉学研究的基础和前提，中国北方地区具有独特的自然地理条件，第四纪以来形成了特有的沉积物类型，不同沉积物的孢粉提取研究一直以来是中国孢粉学研究的难点和热点。本文选取了中国北方不同沉积相的沉积物样品（黄土与古土壤样品17个、湖泊样品沉积物20个、风成砂样品11个、泥炭沼泽样品10、考古点文化层6个、表土样品10个）共74个，通过对同一种样品不同处理方法的对比研究，就中国北方不同沉积物的孢粉提取方法进行了探讨。对比研究发现，黄土及古土壤中的孢粉提取是以氢氟酸筛选法效果佳，值得注意的是盐酸与氢氟酸对样品的处理过程，进行多次彻底处理才能达到很好的效果；湖泊沉积物孢粉提取可采用传统的氢氟酸法，对干旱区含砂量较高的湖泊沉积物及风成砂样品需要配合重液浮选法进行；泥炭、沼泽中孢粉提取应采用重液浮选法，配合筛选法进行；考古点文化层沉积物孢粉提取应采用重液浮选法，并将重液浮选出来的样品配合以氢氟酸处理能达到很好效果；表土样品可以采用无酸碱重液浮选法。同时还探讨了孢粉提取中的分散剂和硝酸的使用及酸碱的使用顺序。 相似文献
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青海湖沉积物生物硅的环境意义初步研究 总被引：1，自引：0，他引：1
湖泊沉积物中生物硅含量的变化已经被广泛应用于评价湖泊生产力和古气候变化研究,但大型湖泊不同位置生物硅含量的时空变化及其与环境要素之间的关系仍缺乏详细的现代过程研究.通过对青海湖不同位置表层沉积样品的生物硅含量测定,建立其空间分布模式及最近数百年生物硅含量的时间序列.结果表明,青海湖表层沉积物生物硅含量变化范围是1.75%～2.98%,平均值为2.25%.与世界其他湖泊相比,青海湖生物硅含量处于相对较低水平,可能与其特殊的地理位置和气候条件有关.青海湖生物硅含量的空间分布规律与沉积物质量堆积速率以及陆源组分含量(如SiO2)相反,而与化学/生物沉积组分(如CaCO3)含量的空间分布规律大体一致,说明生物硅的空间分布受到陆源碎屑物质的"稀释效应"影响.时间序列上,生物硅含量与SiO2含量呈相反变化趋势,与指示降雨量变化的C/N比值也是反相变化,说明生物硅含量在时间序列上也受与气候条件密切相关的陆源输入的影响.青海湖湖心低沉积速率区域的生物硅指标具有指示古气候变化的潜力. 相似文献
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以采自大同盆地野外试验场的含水层沉积物为研究对象,调查高砷含水层中生物可利用性砷的含量及其影响因素。经实验室测定,沉积物总体呈碱性,Al、Fe等金属元素含量较高。利用连续提取法发现沉积物中砷结合形态主要为无定形和低结晶铁铝氧化物结合态,其次是残余态砷。其中铁铝氧化物形态的砷所占比例达53.54%,非专性吸附态和专性吸附态占14.33%,生物可利用形态的砷较少,这与体外模拟方法测定的生物可利用性砷含量较低吻合。体外模拟实验还发现：肠阶段生物可利用性砷含量比胃阶段低,生理学提取法(PBET)和体外消化法(IVG)测定的生物可利用性砷差异较小。 相似文献
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还原性无机硫是沉积物硫中最活跃的部分,其含量变化控制沉积物中铁、磷及重金属等元素的地球化学行为,在地质过程和环境污染方面都具有至关重要的影响。化学连续提取法是目前沉积物中硫形态提取基本方法,但常用的冷扩散法处理单个样品耗时长,难以实现对大批量样品的快速连续提取。为实现快速、准确地测定沉积物样品各形态还原性无机硫的含量,本文采用热蒸馏法,改进基于前人的三步提取过程,通过优化实验装置预先制备实验所需的二氯化铬溶液,实现了样品还原性无机硫形态的快速连续提取;以过氧化氢为氧化剂,将提取的各形态硫氧化为SO24-后采用离子色谱进行检测。选取三峡库区沉积物样品进行重复实验检验,得到提取酸挥发性硫、黄铁矿硫、元素硫的标准偏差(RSD,n=3)分别为5.26%、1.22%和3.09%,重复性较好。进一步对酸挥发性硫、黄铁矿硫、元素硫的加标回收率进行测定,得到这三种硫形态的回收率分别为92.8%、93.6%、94.1%。本实验方法采用的热蒸馏法对单个硫形态提取时间为1.5h,用时较短,玻璃装置连接便捷、操作简单,分析检测准确度好,实现了一套装置对沉积物还原性无机硫形态的连续提取,可适用于大批量样品的硫形... 相似文献
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《矿物岩石地球化学通报》2015,(6)
依托第3次、第4次、第5次北极科学考察在北极楚科奇海采集的表层沉积物样品,通过碱液连续提取法对生物硅含量进行分析,以探讨楚科奇海的生物硅分布及硅质泵过程。结果显示,楚科奇海表层沉积物中生物硅的含量为1.23%~10.60%。高值区位于楚科奇海陆坡处72°N附近和楚科奇海南部阿纳德尔流和西伯利亚沿岸流的交界处68°N附近,低值区位于楚科奇海东部阿拉斯加沿岸流影响区域,其生物硅含量小于3%。楚科奇海表层沉积物中生物硅的分布与上层水体的初级生产力的分布格局较一致,而影响上层水体浮游植物生产的两个重要因素分别为楚科奇海环流格局(尤其是太平洋入流水的影响)和海冰融化。生物硅和有机碳之间存在很好的正相关关系,表层沉积物中蛋白石/有机碳(Sibio/Corg)的比值为1.6~2.02,与北太平洋中该比例相当,表明上层海洋硅质泵过程对楚科奇海碳埋藏的贡献较大,使得楚科奇海成为全球海洋吸收大气CO2重要的汇之一。 相似文献
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凯氏蒸馏法和元素分析仪法测定沉积物中全氮含量的异同及其意义 总被引：2，自引：0，他引：2
氮循环是生物地球化学研究领域中最重要的课题之一,全氮含量的测定是农业、生物和环境等多领域研究中的常规测试项目。凯氏蒸馏法和元素分析仪法作为常规方法通用于上述领域的全氮含量测定,但两种方法在实际应用中的差异却常被忽视。通过对中国北方某盐湖沉积物序列近百个样品的全氮含量分析,对两种方法测定结果的异同进行了对比研究。凯氏蒸馏法的分析精密度高于元素分析仪法(前者标准偏差为0.007,后者为0.024),但在样品硝态和亚硝态氮的含量较高时,凯氏蒸馏法所测结果显著低于元素分析仪法的测定结果,此时选择元素分析仪法进行全氮含量的测定更为可靠和准确;对硝态和亚硝态氮含量极低的样品,两种方法的测定结果无显著差异。研究表明,选择全氮含量的测定方法,必须对所测样品的无机氮含量有初步的了解。对于中国北方的多数盐湖和地表环境样品,由于其无机氮的含量较高,选择凯氏蒸馏法进行全氮含量的测定是不适当的。尽管如此,对所研究的湖泊沉积物剖面而言,两种方法的对比却可以提供有价值的气候和环境演变信息。随着沉积物剖面的由深到浅,两种方法的测定结果由一致变化到存在显著差异,表明了湖泊水体从早期的淡水向今天的盐湖演化的过程。因此,凯氏蒸馏法和元素分析仪法测定结果的差异可以作为一种独立的地球化学气候代用指标。 相似文献
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古环境研究中深海沉积物粒度测试的预处理方法 总被引：12，自引：1，他引：11
对深海沉积物样品进行粒度测试前,应根据研究目的,在预处理过程中有效去除碳酸盐和生物硅,同时完好保留陆源碎屑组分,才能使测试结果准确反映古气候和古环境变化。对采于南海的样品分别加入不同剂量浓度为10％的盐酸或浓度为25％的醋酸,以及不同剂量的NaOH或Na2CO3,同时利用有机元素分析仪、硅钼蓝比色法、环境扫描电子显微镜分析、观察不同方法的预处理效果,并结合粒度测试的结果认为,对于碳酸盐,盐酸和醋酸均可将其有效去除,但由于少量盐酸仍会对陆源矿物组分造成破坏,因此应使用酸性较弱的醋酸;对于生物硅,大剂量的Na2CO3仍难将其有效去除,而使用小剂量的NaOH即可去除干净,但需控制剂量以避免破坏矿物组分。针对南海沉积物中的各种生物组分含量,确定了醋酸和NaOH的使用剂量并建立了预处理流程。 相似文献
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A. M. Sulej-Suchomska Ż. Polkowska A. Przyjazny Z. J. Kokot J. Namieśnik 《International Journal of Environmental Science and Technology》2016,13(6):1475-1488
Determination of xenobiotics in samples of airport runoff water is both a complex and indispensable task due to an increasing threat resulting from the activities of numerous airports. The aim of this study was to develop, optimize, and validate a procedure based on liquid–liquid extraction (LLE) coupled with gas chromatography–mass spectrometry (GC–MS) for the determination of polycyclic aromatic hydrocarbons (PAHs). So far, no procedure was available that would ensure reliable data about concentration levels of these toxic pollutants in a new type of environmental samples, such as airport stormwater. The most difficult step in the analytical procedure used for the determination of fuel combustion products in airport stormwater samples is sample preparation. In this work, eight different protocols of sample preparation were tested. The evaluation of the LLE demonstrated that the best extraction conditions were as follows: dichloromethane (extraction solvent), solvent volume of 15 mL and sample volume of 250 mL. The percent recovery values ranged from 66 to 106 %, which shows that the LLE technique is a powerful method for extracting PAHs from airport runoff water samples with a complex matrix composition. Moreover, the developed procedure was characterized by satisfactory selectivity and a relatively low LOQ (0.17–0.52 μg/L). The procedure has been successfully applied to the analysis of stormwater samples collected from different sites at international airport in Poland. The procedure can thus be used as a tool for tracking the environmental fate of these compounds and for assessing the environmental effect of airports. 相似文献
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The sequential extraction procedure was proposed and used to study of mercury speciation in real samples of soil. Samples
of soil profiles together with bedrock and coal were taken from sampling spots in the vicinity of surficial coal beds in an
area with natural coal outcrops. The proposed sequential extraction procedure involves the following fractionation: organic
mercury compounds, extractable mercury in an acidic medium, mercury bound to humic substances, elemental Hg and mercury bound
to complexes, HgS and residual mercury. The significant distribution of mercury between the two portions—mercury bound to
humic substance and HgS was determined in the majority of samples. The mercury bound to humic substances created a significant
contribution, especially to the top layer of soil. On the other hand, HgS was the dominant form in the samples from lower
layers of the soil profile. The mercury content in the samples did not show a distinct mobility. The influence of soil parameters
on the mercury distribution in the studied samples was investigated and discussed. 相似文献
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新疆某地浸砂岩型铀矿中铀赋存形态的研究 总被引：3，自引：2，他引：1
以新疆某地浸砂岩型铀矿为研究对象,参考Tessier逐级化学提取方法,对10件矿芯试样进行铀赋存形态的研究。将铀赋存形态分为可交换离子态、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残渣态,其中前4种形态铀为活性铀,残渣态铀为惰性铀。研究结果显示,无论是试样间还是同一试样内,铀的形态分布特征都存在明显的差异。各形态铀的含量(平均值)占总量铀的比例为:残渣态(37.75%,RSD为1.80%)>碳酸盐结合态(20.56%,RSD为2.72%)>可交换离子态(15.51%,RSD为1.85%)>硫化物及有机物结合态(14.26%,RSD为2.08%)>铁锰氧化物结合态(11.91%,RSD为1.75%),表明残渣态铀是砂岩型铀矿石中铀的重要赋存形式。针对目前酸法地浸工艺,活性铀是可被浸出的部分,而惰性铀对资源回收是无效的,对于残渣态铀所占比例较高的铀矿石,铀的浸出值较低,在地浸过程中依靠提高溶浸剂的酸度和增加氧化剂对提高浸出率是无益的。 相似文献
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目前国内外比较先进的岩心无损测试,主要采用高光谱技术及XRF扫描技术,这两种扫描范围较大的快速分析方法,均存在着精度要求越高测试时间越长、完整岩心数据精度较高、不完整岩心及岩石标本数据精度较差的问题,难以满足馆藏地质标本取样范围小、快速、准确的要求。本文应用手持式X射线荧光光谱分析技术,以多点测试加权平均的计算方法,改善复杂的样品岩性、矿物种类等因素的影响,提高了分析结果的准确性。结果表明:本方法与定量分析结果比较,具有指示半定量范围作用的测试结果超过82%,加权平均值比算术平均值的指示效果提高了近22%,多点测试的准确度得到了明显提高。并且,该方法具有测试元素较多、粗糙标本经微处理后便可随时测试等优点,较好地解决了馆藏地质标本取样的应用问题。通过这次预研究,新发现了部分铅锌矿标本银元素含量较高、Zk0901钻孔(黄沙坪矿区)168.46~171.24 m的Mo元素平均值为0.3%等具有实际意义的研究数据,为馆藏地质标本再利用提供了重要的找矿信息。 相似文献
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Determining Biogenic Silica in Marine Samples by Tracking Silicate and Aluminium Concentrations in Alkaline Leaching Solutions 总被引：5，自引：0，他引：5
This study introduces an alkaline leaching technique for the simultaneous analysis of biogenic silica and aluminium in sediments. Measuring aluminium facilitates the discrimination between silica from the biogenic (BSiO2) and the non-biogenic fraction, because it originates almost solely from the lithogenic phase. The method was tested using fine-grained silicagel, standard clay minerals, artificial sediments, and natural samples ranging from fresh diatoms to aged sediment from different depositional settings. To determine the BSiO2 content, four different models each describing the dissolution curves, but of increasing complexity, were applied and for each different type of sample the optimum model was selected on the basis of F-test statistics. For mixtures of silicagel and clay minerals, the contribution of Si from the dissolution of clay was negligible compared to Si originating from silicagel. For natural samples with high clay content, complex dissolution curves were observed and single-phase first order dissolution was the exception. This deviation from `ideal' behavior could only be recognized because of high-resolution sampling, especially in the first 20 minutes of the experiment. For most of the samples, the distinction between the biogenic silica fraction and the silica originating from dissolution of clays could be made on the basis of the Si/Al ratios and reactivity constants of the dissolving phases calculated with the models. Clay minerals typically dissolve slowly at a Si/Al ratio close to 1–2, depending on the type of clay mineral. In contrast, biogenic silica displays a wide range of reactivities and Si/Al ratios. Fresh biogenic silica from the water column usually has a high reactivity and a low Al content. Aged biogenic silica from the sediments has a lower reactivity, but Si/Al ratios as low as 5 were found. The method as described here therefore presents an accurate method to analyze biogenic silica in marine sediments with a relatively high clay mineral content. 相似文献
17.
A sequential extraction procedure was carried out in columns using reagents that are known to be reliable from batch tests. The intention was to distinguish between different chemical forms of iron and heavy metals in samples from reduced porous aquifers, which demands anaerobic conditions for the extraction procedure and the determination of small amounts of reactive mineral phases in a quartz dominated sediment system. By means of the developed method, anaerobic conditions can be guaranteed in the columns, which could not be realized to full satisfaction in batch tests that were carried out in a glove box. In order to distinguish between the fractions that were water soluble, exchangeable, bound to carbonates and bound to hydroxides, different reagents were pumped through the sediments and sampled after passage of the columns. Sediment samples of 10 kg each were investigated in this way. The extraction steps were known to be complete when analyses revealed that no further major and trace elements were leached out of the columns. This approach enabled well-adjusted amounts of reagents to be used. By means of the sequential extraction procedure in columns the composition of even small amounts of reactive mineral phases can be determined successfully, which contributes to a deeper understanding of the hydrogeochemical processes in aquifers. In batch tests this accuracy cannot be reached because of the surplus of the extraction solution in relation to the amount of sediment (higher solution-sediment ratio). Furthermore, larger samples are much more representative of the composition of the aquifers than smaller ones and the heterogeneity of the sediment does not limit the accuracy of the results as much as in batch tests. In addition, the technique of flushing sediment in a column is much more typical for the situation in an aquifer than suspending a few grams of a sample in the extracting reagents in batch extraction tests. In order to demonstrate the methodical improvements and field applications, the newly developed method was used to investigate the changing binding forms and mobility of iron and trace metals in samples from a lignite overburden dump, which are influenced by pyrite oxidation processes (acidification) followed by the addition of crushed limestone (neutralization) (see "Sequential extraction procedure in columns. Part 2: Application of a new method"). 相似文献
18.
Tobias F. Ertefai Verena B. Heuer Christoph Vogt Jeffrey Seewald 《Geochimica et cosmochimica acta》2010,74(21):6033-6048
Sorption of volatile hydrocarbon gases (VHCs) to marine sediments is a recognized phenomenon that has been investigated in the context of petroleum exploration. However, little is known about the biogeochemistry of sorbed methane and higher VHCs in environments that are not influenced by thermogenic processes. This study evaluated two different extraction protocols for sorbed VHCs, used high pressure equipment to investigate the sorption of methane to pure clay mineral phases, and conducted a geochemical and mineralogical survey of sediment samples from different oceanographic settings and geochemical regimes that are not significantly influenced by thermogenic gas. Extraction of sediments under alkaline conditions yielded higher concentrations of sorbed methane than the established protocol for acidic extraction. Application of alkaline extraction in the environmental survey revealed the presence of substantial amounts of sorbed methane in 374 out of 411 samples (91%). Particularly high amounts, up to 2.1 mmol kg−1 dry sediment, were recovered from methanogenic sediments. Carbon isotopic compositions of sorbed methane suggested substantial contributions from biogenic sources, both in sulfate-depleted and sulfate-reducing sediments. Carbon isotopic relationships between sorbed and dissolved methane indicate a coupling of the two pools. While our sorption experiments and extraction conditions point to an important role for clay minerals as sorbents, mineralogical analyses of marine sediments suggest that variations in mineral composition are not controlling variations in quantities of sorbed methane. We conclude that the distribution of sorbed methane in sediments is strongly influenced by in situ production. 相似文献
19.
An effective novel ultrasonic extraction procedure coupled with gas chromatography and negative chemical ionization mass spectroscopy has been developed for quantitative recovery of polar herbicides in soil. This rapid one-step sample preparation methodology was named accelerated ultrasonic extraction (AUE), and is based on elevated temperatures, increased power and dispersing intimate contact. Simultaneously, in-situ derivatization was achieved by the addition of derivatization reagent, chelating agent and dispersing agent. The extraction efficiency was enhanced by the multiple applied force and elevated ultrasonic temperature. The in-situ derivatization efficiency was enhanced considerably by the use of ultrasonic energy. Dozens of samples can be extracted simultaneously with this method. The sensitivity was improved because of the remarkable reduced background noise achieved using GC-MS in negative chemical ionization (NCI) mode. The amount of reagent and various ultrasonic parameters, such as ultrasonic energy, ultrasonic time and ultrasonic temperature, were optimized. The reproducibility of replicate soil extraction determination of 9 herbicides in different matrix samples and at different concentrations (n=7) was in the range of 4.9-12.6% of the relative standard deviation. The obtained LOD values ranged between 0.02-0.37 g/kg for all herbicides. Here, we present an improved ultrasonic extraction procedure, which we have termed AUE, can serve as a rigorous high efficiency preparation methodology for polar organic contaminants and can be applied to solid sample pre-treatment extensively 相似文献