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1.
土壤活性组分提取剂的研制及初步试验结果 总被引：2，自引：1，他引：1
土壤的活性组分能够反映土壤实际污染状况及对环境的危害,选择适当的土壤浸提剂是准确评价土壤活性组分的关键技术,已有的提取剂局限于不同元素和不同土壤类型,提取步骤繁琐,实验周期长,重现性不高。本文研制了一种提取土壤中活性组分的新型提取剂——AIE,提取剂组成为0.25 mol/L醋酸-0.25 mol/L醋酸铵-0.005 mol/L DTPA-0.2%对苯二酚混合溶液。国家标准物质提取实验表明,AIE提取剂能够有效提取土壤中多种元素的活性组分(有效态磷、有效态钾、有效态锰、有效态铜),具有很好的通用性。AIE提取剂与三种通用提取剂(Mehlich 3、AB-DTPA、盐酸)的实验比较表明,AIE对作物营养组分盐基离子(K、Na、Ca、Mg)的提取效果高于AB-DTPA和盐酸,与Mehlich 3的提取量变化规律基本一致;对Fe、Mn、P和重金属元素的提取值70%高于或相当于其他三种提取剂。应用AIE提取土壤的活性组分,适用于提取作物营养组分和重金属元素,既可提取有效态又可提取缓效态,且样品无需针对不同元素做分别处理,多种元素提取方法一致,比已有的提取剂实验周期缩短3~5倍,有利于大批量样品的分析测试;AIE实际应用的重现性较好,大多数元素提取量的相对标准偏差低于8%;AIE的缓冲能力强,提取液的pH值升高幅度(0.07~0.9)均未超过缓冲溶液的缓冲范围,可同时适用于酸性和碱性土壤。总体上AIE通用性优于Mehlich 3和AB-DTPA提取剂,是已有提取分析方法的补充和完善。 相似文献
2.
土壤重金属元素可提取态是衡量其生物有效性的重要指标,但其含量随着土壤酸碱性等环境条件的变化而改变,在提取土壤重金属元素可提取态时,不可避免地面临着提取剂与提取方法的选择。中国有关土壤重金属元素可提取态的标准分析方法或技术规范涉及的提取剂多达7种(pH=5.8盐酸溶液、0.1mol/L盐酸溶液、0.43±0.02mol/L硝酸溶液、0.11mol/L乙酸溶液、1mol/L硝酸铵溶液、0.005mol/L DTPA浸提剂、0.01mol/L氯化钙溶液),不同学者对不同提取剂有不同的研究结论,对于通用提取剂的系统研究未见报道。本文选择代表性农耕土壤样品,采用以上7种提取剂提取其中8种重金属元素(镉镍铜锌铬铅砷汞),电感耦合等离子体质谱法(ICP-MS)测定镉铬铜铅锌镍含量,原子荧光光谱法(AFS)测定砷和汞含量,对比了7种提取剂对各重金属元素的提取率,并研究了土壤酸碱性质对重金属元素提取率的影响。结果表明：(1)稀酸溶液对土壤重金属元素的提取率较高,且与土壤的酸碱性无关;(2) 1mol/L硝酸铵溶液虽然对镉的提取能力表征了镉在酸性土壤中的活性远大于碱性土壤的特点,但其对碱性土壤中铅的提取率... 相似文献
3.
砂岩铀矿成矿过程中有机质作用的实验研究--以吐鲁番-哈密盆地十红滩铀矿床为例 总被引：7，自引：2，他引：5
本文利用采自吐鲁番-哈密盆地西南部的样品,有针对性地做了一系列有机质抽提及分离实验,即①利用氯仿抽提岩石中有机质实验;②利用CS2-NmP(二硫化碳-N-甲基-2吡咯烷酮)抽提岩石中有机质实验;③腐殖质提取及分离实验。以上有机质抽提物及分离物分别做铀含量测试。通过实验发现,按以上实验顺序．岩石有机质提取物或分离物中铀含量依次有不同程度的提高,其中以腐殖质中分离出的黄腐酸(Fulvic acids)中铀含量最高,说明在吐哈盆地西南部砂岩铀矿的形成过程中有机质(主要是腐殖质和沥青质)的吸附作用起到部分作用．起最主要作用的是黄腐酸,而且与铀酰离子是以络合(或螯合)形式进行迁移。通过实验和分析,作者认为腐殖质(Humic substances)的络合作用和吸附作用在铀的迁移过程中是紧密相联的,而不是互相孤立的两种作用。在铀的迁移和沉淀富集过程中,黄腐酸(Fulvic acids)和腐殖酸(Humic acids)分别起到不同作用。 相似文献
4.
土壤中汞的生物有效性是决定土壤汞污染和农作物汞富集的重要指标。然而,采用不同提取方法所得到的有效态汞含量存在差异。为探索适用于汞矿区稻田土壤生物有效性汞的提取方法,研究对比了4种提取剂(超纯水、0.005 mol/L DTPA混合液、0.1 mol/L CaCl2和0.1 mol/L HCl)对万山汞矿区内两条典型河流沿岸稻田土壤生物有效态汞的测定结果。结果表明,万山汞矿区稻田土壤总汞含量均值为(12.7±0.42)mg/kg,超标率为93%。土壤生物有效态汞含量较低,4种试剂提取的有效态汞占总汞比例依次为0.005%、0.018%、0.003%和0.036%;超纯水提取的土壤生物有效态汞与稻田土壤、水稻根和茎的总汞浓度显著相关,表明超纯水提取方法最适用于测定万山汞矿区稻田土壤的生物有效态汞。本研究可为评估土壤汞污染风险提供技术和数据参考。 相似文献
5.
本文对云南先锋中新世木乃伊化木化石进行α-纤维素实验提取,以验证化石纤维素的可得性。实验利用有机溶剂分离、碱液分离、无机酸分离等方法分别对研究区5件木乃伊化化石样品进行处理,并采用红外光谱检测方法与现代木材α-纤维素和国际标准α-纤维素进行对比试验。实验结果显示,3种提取方法均可以从化石木材中提取出α-纤维素,但过程特征各有不同。其中,有机溶剂分离实验过程耗时最长,碱液分离方法样品损失最大。相比之下,无机酸分离方法对于木乃伊化木化石α-纤维素提取的效率最高。 相似文献
6.
四种浸提剂对果园与菜地土壤有效硒浸提效果的对比研究 总被引：2，自引：0，他引：2
有效硒是评价土壤中硒对植物供给能力的重要指标,我国目前尚无测试有效硒的国家标准方法。浸提剂的选择对于准确测定有效硒的含量至关重要,本文根据浸提的有效硒与硒形态的关联性来确定最优浸提剂种类。实验中选取了碳酸氢钠、磷酸二氢钾、硝酸和盐酸四种浸提剂,对天津果园和菜地的土壤进行有效硒浸提,采用原子荧光光谱法测定各形态硒的含量,并分别对浸提的有效硒与水溶态+离子交换态+碳酸盐结合态硒的最小值、25%处数据值、中位数、75%处数据值和最大值进行比较分析和差异性检验。结果表明:采用碳酸氢钠和磷酸二氢钾提取菜地土壤有效硒的平均含量均约为0.039mg/kg,高于硝酸和盐酸的提取量;采用碳酸氢钠、磷酸二氢钾、硝酸和盐酸提取果园土壤有效硒的含量依次降低。两种土壤中,磷酸二氢钾浸提有效硒的最小值、25%处数据值、中位数、75%处数据值和最大值与水溶态+离子交换态+碳酸盐结合态硒的含量最为接近,而且无显著差异性。研究认为,0.1mol/L磷酸二氢钾适合作为天津果园和菜地土壤有效硒的浸提剂。 相似文献
7.
8.
加速溶剂提取-气相色谱法同时测定土壤中的22种有机氯和有机磷农药 总被引：1，自引：0，他引：1
我国环境污染调查评价测试项目中开展了大量有关土壤中有机氯及有机磷农药残留的测定工作,多种有机污染物同时分析测试的方法是研究的新热点.本文以正己烷-丙酮(体积比1∶1)为提取剂,采用加速溶剂提取,毛细管柱气相色谱法测定土壤中六氯苯等9种有机氯及敌敌畏等13种有机磷农药残留.方法回收率为79.1％ ～ 107.7％,相对标准偏差为3.62％ ～9.94％ (n =7),检出限为0.02 ～ 0.45 μg/kg.本方法将两类农药同时提取且实现了各组分的完全分离,拓展了方法的适用范围,与传统的超声提取和索氏提取法相比,提取时间缩短至20 min,提取溶剂体积降至50 mL,缩短了分析时间,降低了成本,精密度和回收率能够满足全国环境污染调查评价的需要. 相似文献
9.
氢化物发生-原子荧光光谱法测定土壤样品中不同价态的硒 总被引：4，自引：4，他引：0
采用氢化物发生-原子荧光光谱法( HG - AFS)测定土壤样品中Se(Ⅳ)和Se(Ⅵ)时,提取剂的选择是技术的关键.以往的提取剂种类多且不具有针对性,本文对比了不同提取剂的提取能力,确定使用KH2PO4 - K2HPO4溶液(pH=8.5)为实验用提取剂,以6 mol/L HCl作为还原剂,沸水浴30 min后HG - AFS测定Se总量,不加热直接测定Se(Ⅳ)含量,以差减法得出Se(Ⅵ)含量.在本实验酸度条件下,加入三价铁盐,可消除共存元素的干扰.方法回收率为90.0％ ～ 112.5％,线性范围为0.00 ～6.00 μg/L,相对标准偏差为5.0％ ～ 12.6％ (n=11),方法检出限可达到0.347 μg/L.标准物质的测定值与标准值相符.实验证实此方法提取效果好,是测定土壤样品中硒不同价态的可行性方法. 相似文献
10.
土壤砷污染已成为我国严重的环境问题,淋洗法是修复土壤砷污染较为有效的手段之一。文中以砷污染土壤为研究对象,运用2种环境友好的淋洗剂KH2PO4和草酸进行振荡淋洗实验,探究两种淋洗剂对不同砷污染土壤的淋洗效果,在此基础上,通过2种不同的体外方法 (physiologically based extraction test,PBET;in vitro gastrointestinal,IVG),探索其生物可给性及对人体的健康风险。结果显示,KH2PO4和草酸对土壤中砷有不同程度的去除,草酸对土壤砷的去除率较高,平均去除率为54.3%。运用PBET方法得到的土壤砷的生物可给性高于IVG方法,KH2PO4淋洗后土壤砷的生物可给性高于草酸。与草酸相比,KH2PO4淋洗会在一定程度上增加土壤砷的健康风险。不同in vitro方法对不同淋洗剂修复后效果有不同的评估结果,应该根据不同的淋洗剂选择较为保守的体外方法来评估淋洗后土壤的生物可给性及健康风险。 相似文献
11.
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
12.
Effects of heat treatment on fluorescence properties of humic substances from sandy soil in arid land and their Hg(II) binding behaviors 总被引：1，自引：1，他引：0
Qinglong Fu Xiangliang Pan Daoyong Zhang Bin Zhou 《Environmental Earth Sciences》2012,66(8):2273-2279
The topsoil temperature in arid areas of Xinjiang, China can be up to about 80°C in summer. This may significantly affect the chemical properties of soil humic substances. However, the effects of high temperature on characteristics of soil humic substances and their complexation with toxic metals are still poorly known. In the present study, binding of Hg(II) to unheated soil humic substances and heated soil humic substances from sandy soils was comparatively investigated using three-dimensional excitation?Cemission matrix (EEM) fluorescence spectroscopy. Two fluorescent peaks (peak I at Ex/Em?=?365?C370/470?C474?nm; peak II at Ex/Em?=?270?C275/468?C472?nm) identified as humic-like fluorescence were observed in the EEM spectra of humic substances. Both peaks were clearly quenched by Hg(II), indicating the strong interaction of humic-like substances with Hg(II), and showed blue shifts after heat treatment. Heat treatment caused an increase of the fraction of accessible fluorophore (f a), binding sites number (n) and effective quenching constants (logK a), indicating that more binding sites in humic substances could bind Hg(II) and form more stable humic substances?CHg(II) complexes after heat treatment. However, a decrease of binding constants (logK b) suggested that heat treatment would reduce the binding capacity of each binding site of humic substances to Hg(II). This study implies the transport of Hg(II) may be affected by high temperature in the arid zone due to the modification of the physicochemical properties of humic substances in soil. 相似文献
13.
《Applied Geochemistry》2000,15(2):133-139
The sorption of Yb3+, UO2+2, Zn2+, I− and SeO2−3 onto Al2O3, Fe2O3 and SiO2 were determined by a batch technique in the presence and absence of fulvic acids. The effects of fulvic acid on sorption were compared. The existing general consensus, that humic substances tend to enhance metal cation sorption at low pH, reduce metal cation sorption at high pH and reduce inorganic anion sorption between pH values 3 to 10, was generally shown to be true. However, in this work many exceptions to the general consensus were found. The study indicated that the effect of humic substances on sorption of inorganic cations or anions depends not only on pH, but also on the nature of the oxide, the nature of humic substance, fractionation of the humic substance by sorption, the relative strength of complexes of both soluble and sorbed humic substances, the extent of surface coverage by humic substance, the initial concentration of humic substance and the inorganic electrolyte composition. 相似文献
14.
Cross-linking of humic substances with organic bridging groups is thought to contribute to the humification of soil organic matter. Model cross-linked humic substances were prepared by cross-linking Amherst soil humic acid by a diepoxide and a polycarboxylic acid, applying procedures established for cross-linking of polymers and textile fabrics. Products of the cross-linking reactions were analyzed by FTIR and 13C CPMAS NMR. Physicochemical properties of the products were determined by solubility experiments and thermal analysis. The incorporation of the cross-linker into the matrix of the humic acid by covalent linkages was confirmed by both the disappearance of bands of the reactive functional groups of the cross-linker in the FTIR spectrum and the increase of signals related to the incorporation of the cross-linker into the matrix of the humic acid in the FTIR and 13C CPMAS NMR spectra. The formation of covalent ester and ether linkages by the cross-linking reaction was indicated. Water solubilities at pH 6.2 of the cross-linked samples as determined by UV/Vis spectrometry were reduced compared to controls. Fewer water molecule bridges were formed in the cross-linked samples, which was attributed to a lower number of available functional groups and increased distances between humic acid strands caused by the cross-linking molecules. Reduced reactivities of humic acid strands in the cross-linked samples further indicated successful cross-linking. The reactions investigated in this study can be regarded as models for reactions occurring in natural soils to test the significance of cross-linking reactions in the humification process of soil organic matter and the physico-chemical properties and ecological function of organic matter in geosolids. 相似文献
15.
S.A. Visser 《Organic Geochemistry》1985,8(1):81-85
The incorporation of humic acid fractions in media designed for the enumeration of soil micro-organisms belonging to specific physiological groups was found to result for some groups in appreciably higher counts. It is suggested that by influencing the enzyme systems of certain micro-organisms, humic compounds may affect the range of substrates which they can utilize. The effect could have implications on the activity of organisms in environments in which humic substances are normally present, such as soils and natural waters. 相似文献
16.
Characterization of humic substances by advanced solid state NMR spectroscopy: Demonstration of a systematic approach 总被引：2，自引：0，他引：2
Characterization of humic substances is challenging due to their structural complexity and heterogeneity. Solid state nuclear magnetic resonance (NMR) is regarded as one of the best tools for elucidating structures of humic substances. The primary solid state NMR technique that has been used so far is the routine 13C cross polarization-magic angle spinning (CP-MAS) technique. Although this technique has markedly advanced our understanding of humic substances, the full potential of NMR for characterizing humic substances has yet to be realized. Recent technical developments and applications of advanced solid state NMR have revealed the promise to provide deeper insights into structures of humic substances. In this paper, we summarized and demonstrated the systematic solid state NMR protocol for characterization of humic substances using a humic acid as an example. This protocol included (1) identification of specific functional groups using spectral editing techniques, occasionally assisted by 1H13C two-dimensional heteronuclear correlation (2D HETCOR) NMR, (2) quantification of specific functional groups based on direct polarization-magic angle spinning (DP-MAS) and DP-MAS with recoupled dipolar dephasing, combined with spectral editing techniques, (3) determination of connectivities and proximities of specific functional groups by 1H13C 2D HETCOR or 2D HETCOR combined with spectral editing techniques, and (4) examination of domains and heterogeneities by 1H13C 2D HETCOR with 1H spin diffusion. We used a soil humic acid as an example to demonstrate how this protocol was applied to the characterization of humic substances step by step. Afterwards, based on typical 13C NMR spectra of humic substances we described how we could combine different NMR techniques to identify specific functional groups band by band from downfield to upfield. Finally, we briefly mentioned the potential new NMR techniques that could be developed to enrich the current systematic protocol. This systematic protocol is not only applicable to humic substances but also to other natural organic matter samples. 相似文献
17.
N. Plechanov 《Organic Geochemistry》1983,5(3):143-149
The system Sephadex LH 60/dimethylformamide/acetic acid was found to be useful for the determination of the molecular weights of humic substances. Fulvic and humic acids concentrated from natural waters, sediments and soil have number- and weight-average molecular weights less than 2000 and 4000, respectively. A theoretical model for the dependence of an experimental GPC curve on the relation between the measured property and the structure of heterogeneous polymers, is presented. The results from the examination of the molecular composition, obtained by using RI, UV, fluorescence and weight measurement as detection techniques, show that the apparent distributions of aromatic moities and fluorescent groups in the humic substances were similar to those of repeating structural subunits and end groups respectively, in synthetic polymers. 相似文献
18.
红壤中矿物表面对腐殖质吸附萘的影响 总被引：5，自引：1，他引：5
矿物表面可改变土壤腐殖质对疏水性有机污染物的结合能力。采用红壤和高岭石分别与胡敏酸结合制备得到的两种复合体对萘的吸附等温线非线性显著,其n=0.76或0.74,并且有机碳归一化吸附分配系数的实验值Koacds是采用Kow计算得出的理论值Koc的5倍以上,表明红壤、高岭石均对腐殖质吸附萘有强化作用,且红壤较之高岭石对腐殖质吸附萘的影响稍强些。主要原因是,红壤中除了高岭石外,还有与腐殖质结合力很强的铁氧化物,而且很可能是吸附态腐殖质组成结构形态发生了有利于对萘吸附的改变。 相似文献
19.
松嫩平原沼泽湿地区多目标地球化学调查方法试验 总被引：1，自引：1，他引：0
沼泽湿地属于一种特殊的生态景观条件。为了选择适合沼泽湿地区的多目标地球化学调查采样介质,在松嫩平原西部扎龙保护区开展了方法试验,采样介质主要采取沼泽湿地区的表层腐殖泥和基底冲积土2种介质。通过对比试验,反映出沼泽湿地区表层的腐殖泥是代表该景观区多目标地球化学调查的最佳采样介质。腐殖泥样品中的OrgC、N、S、Se、Hg、TC、U、Br、Au、TFe2O3、Bi、Cr、Ag、Li、Y、Mo、Cu、Sb等元素含量均高于其基底沉积物样品。这与沼泽湿地区的生态环境特征相吻合,而腐殖泥下部的冲积成因的基底物质属于外来物质,不能反映目前沼泽湿地区的生态环境特征,由此确定沼泽湿地区多目标地球化学调查最佳采样介质为表层的腐殖泥。 相似文献
20.
桂林毛村岩溶区自然植被土壤团聚体中腐殖质组成初步研究 总被引：1，自引：0，他引：1
探索土壤有机碳物理保护与化学保护的关系,有助于揭示土壤固碳和培肥机理,明确不同粒级团聚体和不同腐殖物质组分对土壤固碳和肥力的贡献。本研究对岩溶区自然植被土壤团聚体中腐殖质含量进行了研究,结果表明:(1)灌丛和林地土壤团聚体中有机碳含量总体上均表现为随着土层深度的增加逐渐下降,而在不同土层深度随着团聚体粒径范围的变化则有机碳含量的变化规律则不同,无明显一致的规律;(2)两种土地利用方式各粒径团聚体中胡敏酸和富里酸均比全土小。这可能是由于在湿筛分离团聚体的过程中溶于水的那部分胡敏酸和富里酸成分被损失掉;(3)各腐殖质组分随着团聚体粒径范围的减小在两种自然植被上均无明显一致的规律,但胡敏酸和富里酸总量则基本表现为随着团聚体粒径范围的减小而逐渐升高,即在0.25mm和0.5~0.25mm粒径范围团聚体中最大;(4)两种自然植被土壤各土层中和各团聚体中胡敏酸/富里酸(HA/FA)基本上表现为小于1,这主要是因为研究区温度相对较高,湿度较大,植被覆盖度大,微生物降解作用强所致。 相似文献