共查询到20条相似文献，搜索用时 673 毫秒
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W.L. Campbell 《Journal of Geochemical Exploration》1981,15(1-3)
False readings, apparently caused by the presence of high concentrations of manganese dioxide, have been observed in our current flame atomic-absorption procedure for the determination of gold. After a hydrobromic acid (HBr)-bromine (Br2) leach, simply heating the sample to boiling to remove excess Br2 prior to extraction with methyl-isobutyl-ketone (MIBK) eliminates these false readings. 相似文献
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《Applied Geochemistry》2006,21(6):964-976
Hopanoids have been widely used as characteristic biomarkers to study inputs of bacterial biomass to sediments because they are preserved in the geologic record. A limited number of studies have been performed on hopanoid biomarkers in soils. The present study examined the distribution and potential preservation of hopanoids in soils that are developed under different climatic conditions and varying vegetative inputs. Solvent extraction and sequential chemical degradation methods were employed to extract both “free” and “bound” hopanoids, from three grassland soils, a grassland–forest transition soil, and a forest soil from Western Canada. Identification and quantification of hopanoids in the soil samples were carried out by gas chromatography–mass spectrometry. Methylbishomohopanol, bishomohopanol and bishomohopanoic acid were detected in all solvent extracts. The base hydrolysis and ruthenium tetroxide extracts contained only bishomohopanoic acid at a concentration range of 0.8–8.8 μg/gC and 2.2–28.3 μg/gC, respectively. The acid hydrolysis procedure did not release detectable amounts of hopanoids. The solvent extraction yielded the greatest amounts of “free” hopanoids in two of the grassland soils (Dark Brown and Black Chernozems) and in the forest soil (Gray Luvisol). In contrast, the chemical degradation methods resulted in higher amounts of “bound” hopanoids in the third grassland soil (Brown Chernozem) and the transition soil (Dark Gray Chernozem), indicating that more hopanoids exist in the “bound” form in these soils. Overall, the forest and the transition soils contained more hopanoids than the grassland soils. This is hypothesized to be due to the greater degradation of hopanoids in the grassland soils and or sorption to clay minerals, as compared to the forest and transition soils. 相似文献
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By comparing three sequential extraction procedures, a new optimized extraction scheme for the molybdenum association in environmental samples was proposed. Five operational steps were described as exchangeable (KH2PO4 + K2HPO4: including water-soluble), associated with organic matter (NaOH), Fe–Mn oxides and/or carbonates (HCl), sulfides (H2O2) and residue (HNO3 + HF + H2O2). An optimized extraction scheme was compared with Tessier’s procedure and the Commission of European Communities Bureau of Reference (BCR) was applied to black shales. Results showed Tessier’s procedure gave the lowest concentration values for exchangeable molybdenum and the highest values for the residual molybdenum, which could not present the efficiency of the extraction reagents. BCR’s procedure showed the highest values in oxidizable molybdenum and presented four fractions of molybdenum, which did not demonstrate the fractions of molybdenum in the black shales in detail. The optimized extraction scheme demonstrated a certain improvement on extraction efficiency over Tessier’s procedure for the lowest residual molybdenum, and revealed more featured fraction information of molybdenum in black shales than BCR’s. Therefore, after a comparison with other two extraction procedures, the optimized extraction scheme proved suitable for the molybdenum in black shales and it also showed an accurate determination of the molybdenum in the fractions and source of bioavailable Mo. 相似文献
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A study of literature reports of the concentrations of amino acids in extracts from the Murchison meteorite shows that many of the concentration ratios are constant. There are two possible interpretations of these ratios. One is that they are controlled by the pathways through which the amino acids formed, from which it follows that the amino acids are distributed in the same proportions throughout the meteorite. The other interpretation is that the ratios result from the analytical procedures used to extract the amino acids from the meteorite. These methods rely heavily on high-temperature (100 degrees C) aqueous extraction and subsequent high-temperature acid hydrolysis. A correlation was observed in the present study between the relative concentrations of several amino acids in the meteorite extracts and their relative aqueous solubilities at 100 degrees C (alanine, valine, leucine, isoleucine, norleucine, aspartic acid, glutamic acid and glycine). The extract solutions are dilute, and far from the saturation limits, but these correlations suggest that the sampling procedure affects directly the reported concentrations for these amino acids. Ratios of the concentration of serine to those of glycine are also constant but cannot be accounted for solely by relative solubilities, and, as suggested elsewhere, serine as well as phenylalanine and methionine may be terrestrial contaminants. Data for beta-alanine, alpha-aminobutyric acid, proline, sarcosine, alloisoleucine, beta-aminoisobutyric acid, beta-aminobutyric acid, and threonine also show constant abundances relative to glycine, but lack of solubility data at extraction conditions prohibits evaluating the extent of possible sampling bias for these amino acids. If the extraction process does not bias the results, and all extractable amino acids are removed from meteorite samples, then the properties of amino acids which control both their solubilities and their concentrations in the meteorite need to be established. The possibility of sampling bias needs to be tested experimentally before concluding that extraction is complete, and that the constant relative abundances indicate that the relative concentrations of amino acids are homogeneous in the meteorite. 相似文献
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A comparison was made between the composition of the recalcitrant organic matter (ROM) isolated from a sandy forest soil, as revealed with microwave assisted extractions and/or hydrolysis, and using common pyrolysis techniques. Successive microwave irradiation treatments were performed in H2O, 0.1 and 1 M HCl and 0.1 and 1 M KOH. At each step the insoluble residue was examined via Curie point pyrolysis (CuPy) and Curie point thermally assisted hydrolysis and methylation (CuTHM). Sequential irradiation treatment resulted in ca. 35% degradation of the ROM. Compounds released on microwave irradiation in H2O and in HCl were dominated by glucose, suggesting the occurrence of carbohydrate-containing molecular associations in the soil organic matter (SOM) which were not disrupted during acid hydrolysis and extraction as applied for the isolation of the ROM. The product distribution from the microwave irradiation in KOH showed an important contribution to the ROM from the higher plant polyesters cutin and suberin, and to a lesser extent from lignin. Different lignin-derived compounds were specifically released upon microwave acid or base hydrolysis. This suggested that two types of lignin monomers, ether- or ester-linked, occurred in the ROM. The changes in the composition of the CuPy pyrolysates of the residues from the different microwave hydrolyses are consistent with the near complete removal of carbohydrates by microwave HCl hydrolysis. The changes in the composition of the CuTHM pyrolysates of the residues from the different microwave acid and base hydrolyses are in agreement with a major release of cutin- and suberin-derived compounds upon microwave KOH hydrolysis. The CuPy and CuTHM pyrolysates of the final residue consist predominantly of lignin-derived compounds. The study emphasizes the potential of microwave assisted hydrolysis to give a better estimate of the actual contribution of cutin to ROM than pyrolysis. However, the technique appears to be unable to completely release the lignin-based constituent of the ROM. Microwave irradiation appears to provide great potential as a tool for extraction and chemical characterisation of complex OM and could be an attractive additional technique to pyrolysis. 相似文献
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The USGS reference sample marine mud MAG-1 has been subjected to a sequential extraction procedure designed to partition the constituent trace metals into five fractions: I-exchangeable; II- bound to carbonates; III-bound to Fe-Mn oxides; IV- bound to organic matter; V- residual. The analytical approach involved successive chemical extractions and the subsequent determination of trace metal concentrations (Co, Cu, Ni, Pb, Zn; Fe, Mn) in the leachates by atomic absorption spectrophotometry. The chemical speciation results obtained on four replicate sub-samples demonstrate that the coefficients of variation for metal concentrations in the individual fractions are generally better than + 10%. Comparison with published values for total trace metal concentrations in the MAG-1 sample suggests that the overall accuracy of the chemical extraction procedure is satisfactory. 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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传统的液液萃取技术主要采用与水不相溶的有机溶剂作萃取剂,这种异相萃取的传质速率一般较低,需反复振荡或多次萃取.本文建立了以乙腈-硫酸铵-水的双水相萃取体系高效液相色谱法测定地下水中苯并(a)芘和苯并(e)芘的方法,以密度比水小的乙腈为萃取剂,将其与水样混合(互溶)获得乙腈-水体系,然后加入硫酸铵,溶液澄清、分相后取上层有机相(乙腈)进样分析.考察了萃取剂的选择、双水相的形成条件、离子强度以及pH等对测定结果的影响.两种化合物线性范围为2.00～ 400.00 ng/mL,相关系数大于0.999.方法检出限为0.012～0.020 ng/mL,平均回收率为94.6％～97.3％,相对标准偏差为1.3％ ～2.5％.与传统萃取方法相比,该方法具有操作流程简单、快速的特点,可实现对野外环境水样进行原地样品前处理. 相似文献
10.
Off-line solid-phase extraction procedure for the determination of polycyclic aromatic hydrocarbons from aqueous matrices 总被引：1，自引：0，他引：1
I. Limam M. R. Driss 《International Journal of Environmental Science and Technology》2013,10(5):973-982
An off-line solid-phase extraction procedure followed by high-performance liquid chromatography with ultraviolet detection for the determination of 16 priority polycyclic aromatic hydrocarbon pollutants in aqueous matrices was described. Diverse aspects determining extraction efficiency such as packing type (disk or cartridge), elution solvents and addition of organic modifiers to the sample were evaluated. Elution with acetonitrile yields the highest recoveries. Rinsing the sample bottle with acetonitrile and combining the rinse with the sample extract avoids the adsorption of polycyclic aromatic hydrocarbons on the walls of the water containers. The use of isopropanol or methanol 10 % (V/V) was the most appropriate amount for the enrichment of 2- to 6-ring aromatic compounds only on C18 cartridge. The recoveries for all studied polycyclic aromatic hydrocarbons are ranged from 71.4 to 95.2 % for a treated water samples of 500 mL. The proposed method gives very low detection limits (subnanograms per liter) and it has been applied to drinking water, surface water and industrial effluent (oil refinery) samples with good results. 相似文献
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The determination of neutralization potential (NP) of mining wastes is an essential part of waste characterization for acid
rock drainage (ARD) prediction. Interpretation of NP values requires consideration of the mineralogical composition of the
waste. Different minerals can neutralize acid drainage at different rates and in different pH ranges. The test conditions
of widely used laboratory procedures to determine NP do not distinguish between such differences and overestimation of NP
can often result. A simple procedure is proposed in which the effective NP is calculated based on mineralogical composition
and the relative reactivities of component minerals. Mineralogical composition is calculated from easily determined analytical
values using a CIPW normative procedure. Comparison of calculated NP values for 92 samples with experimentally determined
values from tests designed to prevent the overestimation of NP indicates that the method is successful in predicting an effective
NP value in most cases. The procedure is considered to be a cost-effective means of providing confident routine ARD prediction
when used in combination with other tests and analyses.
Received: 1 August 1996 / Accepted: 11 November 1996 相似文献
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A method of extraction for amino acids from soils and sediments involving superheated water has been investigated. About 75–97 per cent of the amino acids contained in four soils of a soil profile from Illinois were extracted by this method. Deep penetration of water into soil aggregates and partial hydrolysis of peptide bonds during this extraction by water at high temperature are likely mechanisms responsible for the release of amino acids from samples. This extraction method does not require subsequent desalting treatments when analyses are carried out with an ion-exchange amino acid analyzer. 相似文献
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F. Khanramaki A. S. Shirani J. Safdari R. Torkaman 《International Journal of Environmental Science and Technology》2018,15(7):1467-1476
This paper presents a comprehensive study of the liquid–liquid extraction of uranium from 0.2 M sulfuric acid solution by tertiary amine (Alamine 336) and kerosene as an extractant and a diluent, respectively. For this purpose, the effects of operating parameters on the uranium extraction efficiency such as Alamine 336 concentration, contact time, initial aqueous phase pH, sulfate ion concentration, temperature and stripping process by different agents are investigated. The Gibbs energy change (ΔG), enthalpy change (ΔH) and entropy change (ΔS) have been determined as thermodynamic parameters to prove exothermic and spontaneous reaction. Also, equilibrium constants, reaction equation and stoichiometric coefficients for uranium extraction with Alamine 336 in sulfate medium are specified. The proposed procedure can be applied to the recovery of uranium from low-grade ore processing and from wastewater in the different stages of the nuclear fuel cycle. 相似文献
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We tested the accuracy of the chloroform fumigation–extraction method, which is commonly used to determine soil biomass C concentrations. Accurate and precise determination of total microbial biomass is important in order to characterize soil properties and to develop predictive metal transport models for soils. Two natural soils, and individual soil components, including silica sand, montmorillonite, kaolinite, a humic acid, and Bacillus subtilis bacterial cells, were fumigated for 24 h. Following the fumigation, C from fumigated and unfumigated samples was extracted using a 0.5 M K2SO4 solution. The difference between the C content in the fumigated and unfumigated samples ideally represents C due to biomass because the fumigation procedure should lyse cells and release biomass C. We observed increased C release upon fumigation for bacteria-only samples, confirming the ability of fumigation to lyse cells. There was no difference in extracted C concentration between fumigated and unfumigated samples of silica sand and of humic acid, confirming that the fumigation process does not introduce additional organic C to samples of these soil components. However, the fumigated clay samples both showed increased C release relative to the unfumigated controls, indicating that significant concentrations of the fumigant, chloroform, adsorbed onto the clay minerals studied here. Additionally, we found significant chloroform remaining in the extracts from two fumigated natural soils. Attempts to remove the chloroform from the soils or soil components prior to extraction by increasing the evacuation time, or to remove chloroform in the extracts by sparging them vigorously with nitrogen gas, both failed. This research reveals that chloroform gas may adsorb significantly to clays and the clay fraction of natural soils. Thus, the fumigation–extraction method must be corrected to account for the added chloroform C and accurately assess the concentration of biomass C in soils that contain significant concentrations of clays. 相似文献
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混合酸敞开或高压密闭溶样-ICPMS测定地质样品中稀土元素 总被引：9，自引：9，他引：0
测定地质样品中的稀土元素时,用碱熔法处理样品过程繁琐,混合酸敞开酸溶法的酸种类多,用量较大,而微波消解法批次处理样品少,效率不高。本文比较了7种混合酸敞开酸溶体系、硝酸-氢氟酸高压密闭体系对样品溶样的效果,采用电感耦合等离子体质谱测定15个稀土元素的含量,建立了一套样品前处理体系简单、酸用量少、相对快捷的测定地质样品中稀土元素的方法。通过对59件国家标准物质的测试分析,结果表明硫酸-氢氟酸敞开酸溶和硝酸-氢氟酸高压密闭溶样两套体系的方法检出限、精密度、准确度均能达到地质行业相关标准测试要求。硫酸-氢氟酸敞开酸溶体系对于样品中钡含量较高,或样品量较少时适用;硝酸-氢氟酸高压密闭溶样体系的检出限更低,适用于大批量样品的分析测试。两套体系均不需要进行数学干扰校正,且酸用量少（最多6 mL）,分析效率高（平均每日分析测试300件）,有较大的推广应用价值。 相似文献
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电感耦合等离子体发射光谱法测定黑钨矿精矿和中矿中的锰 总被引：2，自引：2，他引：0
样品采用过氧化钠熔融,酒石酸络合提取,电感耦合等离子体发射光谱法测定黑钨精矿和中矿中的锰含量,碱熔络合体系避免了酸处理样品时大量钨酸沉淀的生成,解决了钨酸沉淀导致的溶矿不完全和夹杂、吸附待测元素的问题。在优化的工作条件下,方法检出限为0.019μg/mL,精密度(RSD,n=11)为0.92%～1.50%,并且具有较高的回收率(97.5%～104.0%),单次测定结果与协同定值结果的偏差小于国家标准GB/T 6150.14—2008硫酸亚铁铵法实验室间允许差。方法简便快速,无明显基体干扰,满足了国家标准黑钨精矿中锰的检测要求,可用于高、中品位钨矿石样品中低含量锰的准确测定。 相似文献
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Georgios Papastergios Jose-Luis Fernandez-Turiel Anestis Filippidis Domingo Gimeno 《Environmental Earth Sciences》2011,64(3):743-751
The procedure proposed in this study is based on the extraction of elements in soils by analytical grade HNO3, the distribution of the elemental data displayed on probability graphs (Q–Q plots) and the visualization of the results
spatially by GIS software. The applicability of the procedure is demonstrated in an urban area and its surroundings (Kavala,
northern Greece). A major (Ca) and a trace (Ag) element are used as examples in order to demonstrate the applicability of
the proposed procedure. Normal probability and lognormal probability plots of Ca and Ag show that their concentrations are
lognormally distributed and that their geochemical baseline and anomaly threshold values can be calculated with the aid of
their geometric mean and geometric deviation. The advantages of the proposed procedure are simplicity, comprehensiveness,
and low cost. It can be applied to environmental geochemical studies of soils in a variety of areas. 相似文献
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Jean King Whelan 《Geochimica et cosmochimica acta》1977,41(6):803-810
The amino acids in a 56 cm sphincter core (K-19-4-9, Woods Hole Oceanographie Institution) from 30°N latitude, 60°W longitude—approximately 300 miles southeast of Bermuda—at a water depth of 5454m were analyzed by gas and liquid chromatography. Amino acids decreased rapidly with depth with β-alanine and γ-aminobutyric acid predominating in deeper sections. Most of the amino acids are tightly bound in the sediment and are released only upon hydrolysis with 6N HC1. Amino acids accounted for only 0.40% of total nitrogen in the non-carbonate minerals in the top 0–8 cm and 7.9 × 10?4 percent in the bottom 48–56 cm. The remaining nitrogen is removed from the sediment by amino acid extraction. 相似文献