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1.
干法灰化和微波消解-电感耦合等离子体发射光谱法测定植物样品中22个主次量元素 总被引：13，自引：6，他引：7
采用干法灰化和微波消解两种样品分解方法处理植物试样,用电感耦合等离子体发射光谱法测定样品中铝、钡、钙、铜、钾、镁、钠、铁等22个主、次量元素的含量,用两种前处理方法对国家一级标准物质进行测定,比对测定值与标准值,验证两种方法的准确度和精密度。结果表明,不同的样品分解方法对各元素的测定结果会产生不同程度的影响。选择适宜的分解方法可以大大提高植物样品中铝、铁、硫等元素测定结果的准确度。干法灰化和微波消解两种前处理方法的精密度(RSD,n=11)均小于5%。 相似文献
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3.
有机溶剂辅助微波消解-电感耦合等离子体质谱法测定多种原油中微量金属元素 总被引：2，自引：2，他引：0
建立了二氯甲烷溶剂辅助微波消解-电感耦合等离子体质谱法测定原油中V、Cr、Fe、Ni、Cu、Zn、Mo、Co、Pb等16种微量金属元素。研究表明,用CH2Cl2分散原油样品,以浓HNO3-H2O2为消解体系,采用CEM微波消解系统消解样品,各元素线性关系良好,相关系数≥0.9995;检出限可达ng/L;方法精密度较高,相对标准偏差(RSD,n=3)<5.0%;回收率为92%～110%。以w(Ni)/w(V)与w(Fe)/w(V)比值为变量参数对不同原油样品进行聚类分析,表明国内与国外不同地区原油样品中各金属元素含量差异较大。 相似文献
4.
微波消解-电感耦合等离子体发射光谱法同时测定白云石中铁铝钙镁钾钠硫 总被引：2，自引：2，他引：2
采用微波消解白云石样品，电感耦合等离子体发射光谱法测定其中铁、铝、钙、镁、钾、钠、硫的氧化物，对微波消解条件和等离子体发射光谱仪的工作条件进行了选择，克服了常规化学分析方法步骤繁琐、耗时长、工作量大的不足。利用所建立的方法快速分析了白云石中铁、铝、钙、镁、钾、钠、硫的含量，结果与标准值或化学法相符，10次测定的相对标准偏差（RSD）7种元素均小于1％，可以满足生产和科研的要求。 相似文献
5.
微波消解-高分辨电感耦合等离子体质谱法测定土壤中8种金属元素 总被引：1，自引：0，他引：1
微波消解结合电感耦合等离子体质谱(ICP-MS)是土壤样品中金属元素测定的常用方法,其前处理可以采用不同的消解体系,但是消解体系对分析结果的准确性影响较大。此外,应用ICP-MS测定某些元素时干扰的存在会影响结果的准确性。基于上述问题,本文优选三个酸体系微波消解溶样,采用高分辨电感耦合等离子体质谱(HR-ICP-MS)测定土壤样品中8种金属元素(Cr、Co、Ni、Cu、Zn、Pb、Cd和U)的含量,对比研究了由不同用量硝酸、盐酸、氢氟酸混合组成的三个酸消解体系对国家土壤标准物质的消解效果,确定了最优前处理方法。结果表明：经国家土壤标准物质验证,采用HR-ICP-MS检测,在不需要干扰校正的情况下,酸体系Ⅰ(6mL硝酸+3mL盐酸+3mL氢氟酸)和酸体系Ⅱ(2mL硝酸+6mL盐酸+1mL氢氟酸)的测定值与标准值相吻合,方法检出限为0.001～0.715μg/g,精密度(RSD,n=6)小于7.0%。从消解情况、准确度和精密度比较,酸体系Ⅰ稍优于酸体系Ⅱ;从酸用量比较,酸体系Ⅱ酸用量最少。两种酸体系的样品处理方法均具有较高的适用性和可靠性,都可用于土壤样品中8种金属元素含量的直接测定。 相似文献
6.
测定植物样品中的钾和磷,通常采用高压密闭微波消解-电感耦合等离子体发射光谱法(ICP-OES),但复杂的基质会增加消解难度,如花生、核桃等含有高油脂类大分子聚合物的样品难以快速消解彻底,易使测定结果偏低。为了提高植物中钾和磷的检测效率,本文采用硫酸-过氧化氢消解法和高压密闭微波消解处理样品,将待测元素磷转化成磷酸盐,钾成为游离的钾离子,形成单相单价态消解溶液,通过对比实验确定了应用ICP-OES快速、准确测定不同类型样品中钾和磷含量的前处理方法。经实际样品分析验证表明：(1)对于高油脂类样品,硫酸-过氧化氢消解法通过强酸破坏植物外层结构,使有机物快速炭化,随后滴加过氧化氢快速消解(约2.5h),能直接消解样品,且消解更安全和彻底;而高压密闭微波消解法耗时较长(约4.5h);与大多学者研究结果对比,硫酸-过氧化氢消解法准确度优于高压密闭微波消解法,建议优先采用。(2)对于非油脂类样品,2种处理方式均适宜,钾和磷测定结果无显著性差异,并且与目前大多学者的研究结果较为一致,其中高压密闭微波消解法试剂消耗少、空白值低、操作简便,建议优先采用。(3)硫酸-过氧化氢消解法测定钾和磷的方法检出限分别... 相似文献
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全反射X射线荧光光谱法同时测定复混肥料中钒铬锰铁镍铜锌铅 总被引：1，自引：0，他引：1
样品经硝酸微波消解,以镓为内标,采用全反射X射线荧光光谱法(TXRF)同时测定复混肥料中的钒、铬、锰、铁、镍、铜、锌、铅,方法检出限从铅的1.0μg/g到钒的7.0μg/g,精密度(RSD)铬为2.5%,铅为16%,除铅以外,其余元素的RSD均小于10%;方法回收率为80%～120%,Pb的回收率略低主要是由于化肥中As Kα谱线对Pb Lα谱线的干扰导致测定结果偏低。用TXRF和电感耦合等离子体发射光谱法(ICP-AES)测定不同复混肥料中各元素的含量,经统计检验,两种方法测定结果在95%置信区间内无显著性差异。对于金属元素含量较高的样品,TXRF法测定结果的相对标准偏差小于ICP-AES法。对于不同的复混肥料,在微量、痕量元素检测范围内,TXRF法具有较高的准确度和适用性,仪器使用和维护成本低,方法快速准确。 相似文献
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灰岩样品的主要成分为碳酸钙,而镁、钾、钠、铝、钛、铁、锰的含量非常低,测试的灵敏度要求很高。该文采用一次溶矿电感耦合等离子体法直接测试灰岩中的镁、钾、钠、铝、钛、铁、锰。实验表明：在5％的盐酸介质中测试镁、钾、钠、铝、钛、铁、锰能取得很好的效果。通过测试国家标准样品,与国家标准值相比较,分析结果基本一致,准确度和精密度均令人满意,镁、钾、钠、铝、钛、铁、锰元素的相对标准偏差≤0．07％。钙元素的标准偏差≤0．15％。 相似文献
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运用电感耦合等离子体发射光谱法(ICP-AES)分析磷矿石样品中的多元素,通常采用氢氟酸+盐酸+硝酸混合酸分解石样品,其中的氢氟酸是为了彻底分解地质样品中以硅酸盐形式存在的待测元素,但赶除氢氟酸的程序繁琐。本文在实际工作中发现,仅需测定磷矿石中的磷、镁、铝、铁元素时,可不加氢氟酸,四种元素的分析结果已能满足要求,这可能是与样品处理过程中生成的少量氢氟酸有关。为了验证不加氢氟酸的样品分解能力,采用浓硝酸-浓盐酸混合酸(体积比1∶1)加热分解试样,稀酸浸取,溶液冷却定容后直接用ICP-AES测定。分析结果显示溶样酸中是否含有氢氟酸,对磷、镁、铝、铁的测定结果不存在显著影响。方法检出限为磷100μg/g、镁0.3μg/g、铝20μg/g和铁6μg/g。经国家一级标准物质分析验证,方法精密度(RSD)小于5.0%,相对误差小于1.5%。本方法针对性强,分析快速准确,适用于实际工作中不包括钙和硅元素在内的磷矿石简项测定。 相似文献
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生物样品中微量元素硒的分析检测,经典方法是湿法消解-氢化物发生原子荧光光谱法(HGAFS)。湿法消解处理生物样品需使用大量试剂,并且消解时间长,样品背景值高;HG-AFS的分辨率较低,已经不能满足微量硒的分析需求。解决生物样品的消解过程缓慢、试剂用量大的问题是提高样品中微量元素硒的检出限和分辨率的前提。本文采用湿法消解和微波消解两种消解体系处理样品,对两种方法制备的溶液分别采用HG-AFS和电感耦合等离子体质谱法(ICP-MS)进行测定,通过对比试验确定了微波消解ICP-MS方法可以实现生物样品中微量硒的准确测定。对比试验表明:采用高压密闭微波消解前处理样品技术可以大大缩短消解时间,减少试剂用量,降低了样品背景值;利用ICP-MS直接进行测定,方法检出限为0.01μg/g,精密度(RSD,n=12)小于4%,低于HG-AFS的检出限(0.03μg/g)和精密度(10%)。微波消解ICP-MS方法操作简单快捷,降低了方法检出限,提高了样品分析的准确度和精密度。 相似文献
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The weathering of a late Tertiary volcanic ash near Jackson, Wyoming, was studied by sampling water percolating through the ash with suction lysimeters, and by examination of the associated solid phases. Soluble organic compounds derived from vegetation control the release and transport of solutes by complexing Al and Fe, and by causing low pH values. The concentrations of Na, K, Ca, and Mg, as well as those of Al and Fe correlate with the dissolved organic carbon concentrations (DOC) and follow an annual cycle with a maximum in spring. DOC concentrations averaged 5O mg C per liter, and values as high as 260 mg/l were observed. Al and Fe concentrations ranged as high as 5 mg/l. The dissolved organic matter was largely in the form of humic acids, although minor amounts of oxalate, acetate, and formate were also present. The pH of the percolating waters ranged from 4.3 to 6.5 with a mean of 5.2.During laboratory weathering experiments with the same ash in the absence of dissolved organic compounds, pH values ranged from 7.3 to 9.5, dissolved Al and Fe concentrations were below the detection limit, and there was little resemblance between the compositions of the solutions and the compositions observed in the field. Any model attempting to describe weathering in a comparable setting must incorporate biological mechanisms as the dominant controls. 相似文献
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Mobilization and redistribution of elements in soils developed from extreme weathering basalt on Hainan Island 总被引：1，自引：0，他引：1
Major, trace and organic elements of a South China were reported to investigate elements laterite profile developed on Neogene basalt on Hainan Island, mobilization and redistribution in tropical regions. The results indicate that strong acid environment and organic matter （OM） can remarkably improve the transfer of insoluble elements. Among all the elements, Th is the least mobile. As for the general conservative elements during incipient chemical weathering, such as Ti, Zr, Hf and Nb, the removals are up to 30%-40% in the upper profile. And for Fe, A1, Cu and Ni, that tend to be combined with secondary minerals and to be retained in temperate zone, they are re- moved from the upper profile, transferred downwards, and then precipitated in the lower profile. In addition, atmos- pheric inputs, including sea salt aerosols and dust, have a profound effect on the budgets of elements that are susceptible to leaching losses （e.g. K, Na and Sr）. Excluding the possibilities of groundwater and erosion, the remarkable increase of K, Na and Sr concentrations in the upper profile, together with dramatically upward increasing trends of the percentage changes of Sr/Th, K/Th and Na/Th ratios, show that atmospheric inputs, especially sea salt aerosols, contribute much extraneous seawater derived elements, such as K, Na and Sr to the soils. The overall elemental be- haviors in this profile suggest that organic matter and atmospheric inputs play a very important role in the mobiliza- tion and redistribution of elements during extreme weathering in tropical regions. 相似文献
13.
中太平洋PC5222孔岩芯地球化学特征及物源探讨 总被引：1，自引：0，他引：1
通过对中太平洋PC5222孔45个岩芯样品进行常微量元素的测试分析与研究,发现元素含量在垂向上有4次比较明显的变化。早期沉积物中,随着Al2O3、Fe2O3、K2O、MnO、TiO2、CaO、CaCO3含量的增加,SiO2含量呈递减趋势;晚期变化不明显。元素的相关性分析和R型因子分析表明,Al2O3、Fe2O3、K2O、MnO、TiO2之间存在明显的正相关关系,而与SiO2为负相关。前者主要受陆源碎屑沉积的影响,后者与生物作用及火山活动有关。进一步探讨了晚渐新世沉积环境的演变规律。 相似文献
14.
《Applied Geochemistry》1997,12(4):465-472
Permafrost is a common feature in the Canadian Subarctic, resulting in the development of distinctive wetland forms, such as peat plateaux, which are perennially frozen peatlands. The geochemistry of a peat plateau bog in East Little Bear River Valley, Northwest Territories, is discussed, including variations in botanical and mineralogical composition, and the influence of permafrost. The riparian margin of the plateau bog is unfrozen, but permafrost occurs at 0.68 m depth 10 m inland. Cores taken in these 2 sites exhibit variations in peat stratigraphy, but possess a similar C-shape ash distribution. In the core not affected by permafrost, most elements studied (Al, Ba, Cr, Fe, K, Mg, Na, Si, Th, Ti, V) also display a C-shape distribution, and their concentration can be explained in terms of mineral matter abundance and variety. Halogens (Cl, I, Br), on the other hand, are mainly associated with the organic fraction, whereas Ca and Se appear to be associated with both the organic and inorganic fraction. In the permafrost-affected core, all elements, independently of their organic or inorganic affinity, exhibit a substantial enrichment immediately above the permafrost table, whereas they are depleted immediately below. This is inferred to be the result of solute redistribution linked with ice formation caused by upward permafrost growth and downward seasonal freezing. 相似文献
15.
《Quaternary International》2006,142(1):162-171
A geochemical study of oligotrophic Lake Sanabria (NW Iberian Peninsula) allows us to distinguish the geochemical response of a lacustrine system to catastrophic events and climatic events. The main major elements analysed were: K, Na, Mg, Ca, Ti, Al, Fe, Mn, P and S. The organic matter content in the sediment of Lake Sanabria is determined by the rainfall regime of the region. Periods when sediments were enriched in Ti, Mg, K, and Al are indicative of relatively wet paleoenvironmental conditions, whereas intervals when sediments were enriched in S and P (associated with organic matter) are indicative of dry conditions. A factor analysis of the geochemical data shows a progressive temporal displacements from organic rich conditions (relatively high values of S and P) to inorganic rich conditions (relatively high values of Ti, Mg, K, Al, and Na). Maximal inorganic content occurred at the beginning of two discrete sedimentary levels: the LOL2 (cal. 1160–1230 yr AD) and the LOL1 (cal. 1510–1680 yr AD) horizons. The LOL2 and LOL1 horizons constitute two discrete events related to climatic changes during the beginning and end of the Little Ice Age, respectively. In contrast, the geochemical analysis provides evidence that the samples associated with the 1959 catastrophic event that occurred in the catchment area of Lake Sanabria do not follow the long-term geochemical evolution paths of the climate driven system. 相似文献
16.
电感耦合等离子体发射光谱法同时测定长石矿物中钾钠钙镁铝钛铁 总被引：3，自引：3，他引：0
样品用HCl-HNO3-HClO4-HF分解,电感耦合等离子体发射光谱法同时测定长石矿物中的K、Na、Ca、Mg、Al、Ti、Fe。对元素的分析谱线、溶解用酸的量等工作条件进行了优化,选择了各元素的最佳分析谱线及背景校正模式,探讨HF的用量,试验加内标和不加内标两种测定方法对测定结果的影响。结果表明,对于样品中含量较高的Al,选用次灵敏线396.152 nm,用内标法补偿非光谱干扰,以长石中含量极低的Au作为内标元素(测定谱线为242.795 nm)可以获得满意的结果,方法检出限为0.45～3.56μg/g。经国家一级标准物质GBW03134、GBW 3116验证,测定值的相对误差(RE)为-1.32%～10.0%,ICP-AES法与其他测定方法的测定结果无显著性差异,方法精密度(RSD,n=10)为0.55%～7.2%,能够满足长石矿物中相关组分的准确测定。 相似文献
17.
通过LL-4孔沉积环境指标研究表明,近100年来龙感湖地区人类活动加强,导致营养元素磷、碳、氮以及铁在沉积物中的浓度均呈增长趋势,特别是1950年以来,随着大量人口的迁入,围湖造田、破坏湖滨湿地等造成水土流失加剧,沉积物质量累积速率加快,同时营养元素累积量急剧增加。根据营养元素与参比元素Al, Fe和Ti之间的关系,以及不同营养元素之间的相互关系,人类活动引起的累积量得以从自然背景上区分出来,结合沉积物质量累积速率计算,人类活动引起的磷、有机碳和氮的累积通量分别在151.0~889.4mg/m2a,4.3~149.0g/m2a和0.5~18.6g/m2a间变化。碎屑物质的累积稀释了沉积物中营养盐的富集浓度,龙感湖草型湖泊的特点,使湖泊沉积环境易于呈氧化环境,生物和地球化学作用,也削弱了人类活动累积营养盐的变化幅度,使沉积中营养盐呈平稳上升的趋势。 相似文献
18.
The La Luna Formation (Maraca section), Maracaibo Basin, was studied by means of V and Ni analysis of the bitumen, total organic carbon (TOC), total sulfur (St), major elements (Si, Al, Fe, Mg, Mn, Ca, Ti, Na, K, P), trace elements (V, Ni, Co, Cr, Cu, and Zn), and electron microprobe analysis (EPMA) of the whole rock, and St, major elements (Si, Al, Fe, Mg, Mn, Ca, Ti, Na, K, P), trace elements (V, Ni, Co, Cr, Cu, Zn, Mo, Ba, U, Th) and rare earth elements (La, Ce, Nd, Sn, Eu, Th, Yb, Lu) of the carbonate-free fraction. The results are discussed based on the organic and inorganic association of trace elements and their use as paleoenvironmental indicators of sedimentation. An association between V and organic matter is suggested by means of correlation between V and Ni vs. TOC, the use of EPMA (whole rock) and V and Ni concentrations (carbonate-free fraction), whereas Ni is found in the organic matter and the sulfide phase. Fe is present as massive and framboidal pyrite, whereas Zn precipitates into a separate phase (sphalerite), and Ni, Cu and, in some cases, Zn, can be found as sulfides associated with pyrite. Concentrations of V and Ni (bitumen), TOC, St, V, Ni, Cr, Cu and Zn (whole rock), U, Th, Mo (carbonate-free fraction) are indicative of changes in the dysoxic sedimentation conditions in the chert layers (TOC, St, V, Ni, Cu and low Zn and V/Cr <4) to euxinic anoxic conditions in the argillaceous limestone (TOC, St, V, Ni, Cu and high Zn and V/Cr >4). In the sequence corresponding to the argillaceous limestone, variations in the concentrations of TOC, St, V, Ni, Zn, Cu and Cr (whole rock) can be observed, also suggesting variable sedimentation conditions. The following is proposed: (i) sedimentation intervals under euxinic conditions associated with high contribution and/or preservation of organic matter, allowing a high concentration level of V and Ni in the organic phase and the accumulation of Cu, Zn and Ni (in a smaller proportion) in the sulfide phase; (ii) sedimentation intervals under anoxic conditions and in the presence of relatively lower H2S, which allowed lower concentrations of V and Ni in the organic phase and higher concentrations of Cu, Zn, and Ni in the sulfide phase. Rare earth elements (REE) concentrations exhibit a marked increase in Ce, Nd, Sm, Eu, Y and Lu for the QM-3 interval, relative to Post-Archean Average Shale (PAAS). REE enrichment in shales has been related to the presence of phosphate minerals such as monazite or apatite. However, these minerals were not detected through XRD or EPMA in the whole rock or in the carbonate-free fraction. The association of REE with organic matter is suggested due to the absence of phosphate minerals, although assessment of these elements require further analysis. 相似文献
19.
Surface slices of 20 sediment cores, off southwestern Taiwan, and bed sediment of River Kaoping were measured for major and
trace elements (Al, As, Ca, Cd, Cl, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, S, Si, Ti, V, and Zn) to evaluate the geochemical
processes responsible for their distribution, including elemental contamination. Major element/Al ratio and mean grain size
indicate quartz-dominated, coarse grained sediments that likely derived from sedimentary rocks of Taiwan and upper crust of
Yangtze Craton. Bi-plot of SiO2 versus Fe2O3T suggests the possible iron enrichment in sediments of slag dumping sites. Highest concentrations of Cr, Mn, P, S, and Zn
found in sediments of dumping sites support this. Correlation analysis shows dual associations, detrital and organic carbon,
for Cr, P, S, and V with the latter association typical for sediments in dumping sites. Normalization of trace elements to
Al indicates high enrichment factors (>2) for As, Cd, Pb, and Zn, revealing contamination. Factor analysis extracted four
geochemical associations with the principal factor accounted for 25.1% of the total variance and identifies the combined effects
of dumped iron and steel slag-induced C–S–Fe relationship owing to authigenic precipitation of Fe–Mn oxyhydroxides and/or
metal sulfides, and organic matter complexation of Fe, Mn, Ca, Cr, P, and V. Factors 2, 3, and 4 reveal detrital association
(Ti, Al, Ni, Pb, Cu, and V), effect of sea salt (Cl, Mg, Na, and K) and anthropogenic component (As and Zn)-carbonate link,
respectively, in the investigated sediments. 相似文献
20.
对赣南三百山盆地晚侏罗世武夷群火山岩的岩石地球化学特征进行了系统研究。根据岩石Na2O K2O含量9.84%～10.74%,K2O/Na2O值1.99～2.52,高铝(ω(Al2O3)>15%)、低钛(ω(TiO2)<0.50%)、贫铁(TFeO=3.15%～3.50%),确定三百山盆地火山岩属长英质橄榄玄粗岩系列。同时根据岩石富集大离子亲石元素、铕正异常等稀土元素、微量元素特征,认为三百山盆地火山岩是挤压构造环境下,深部地幔含石榴石斜长角闪岩部分熔融的产物。 相似文献