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萃取树脂作为一种化学分离手段,国外七十年代就有报导,近年国内兄弟单位研制合成了各类型萃取树脂,并相继用于分析工作中,P_(507)萃取树脂最近问世,给稀土元素的分离富集带来了佳音。该树脂是在P_(507)萃取色层的基础上研制而成的,并具有离子交换的优点。 本文研究了P_(507)萃取树脂分离稀土的条件及偶氮氯膦—PN与稀土元素的显色反应;拟定了一个分离效果良好、简便、灵敏度比偶氮胂Ⅲ高一倍的稀土总量的分析流程,可作为稀土分析的新方法。 实验部分 相似文献
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萃淋树脂作为一种化学分离手段,国外七十年代已有报导。上海最近合成的P_(507)萃淋树脂,具有溶剂萃取和离子交换的双重优点,该树脂对稀土元素有良好的萃取性能,柱上分离周期短而简便,是目前较好的稀土分离试剂之一。 本文研究了P_(507)萃淋树脂分离富集稀土元素的条件,采用大色散率的光栅摄谱仪,着重选择了对稀土元素有较高灵敏度的缓冲剂,在柱上色层制备的总稀土氯化物中测定15个微量稀土分量。拟定的矿石分析流程简便、柱上分离只需2小时,单一稀土的检测下限为0.3—0.001微克、均方误差为±O.2—13.2％。 相似文献
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中子活化分析测定岩石中13个稀土元素 总被引：1，自引：0，他引：1
本文报道了用中子活化分析法测定岩石中13个稀土元素。试样经混酸溶解后通过TBP萃淋树脂住分离铀、钪和铁等干扰元素,富集的稀土元素经中子辐射后再用P_(507)萃取色谱柱将稀土分成La—Tb和Ho—Lu两组。最后使用SCOIRPI—3000多道计算机Ge(Li)γ谱仪系统进行测量。 相似文献
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P507萃取色谱分离三溴偶氮胂光度法测定矿石中痕量铈组稀土 总被引：3，自引：0，他引：3
本文改进了三溴偶氮胂与铈组稀土的显色反应条件,提高了铈组稀土测定的选择性并采用P_(507)萃淋树脂分离富集稀土元素。所拟定的矿石中痕量铈组稀土的测定方法,操作简便快速,易于掌握,适于矿石中0.000x～0.x％含量的铈组稀土的测定。经标准矿样验证,精密度、准确度均符合要求。 相似文献
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甲基膦酸二甲庚脂(简称P_(350))作为镓、金的萃取剂已有报道,但迄今未见P_(350)萃取色谱分离镓的报导。本文研究了以聚二乙烯苯(X—5)型大孔吸附树脂为担体,P_(305)为固定相,考查对镓的反向色谱行 相似文献
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甲基膦酸二甲庚脂(简称P_(350))作为镓、金的萃取剂已有报道,但迄今未见P_(350)萃取色谱分离镓的报导。本文研究了以聚二乙烯苯(X—5)型大孔吸附树脂为担体,P_(350)为固定相,考查对镓的反向色谱行为,以及盐析剂效应等,试验表明P_(350)是分离镓的良好固定相,痕量镓可从大量Fe、Al、Cu、Pb、Zn、Hg、Sn、Ag、Bi,Cd,Cr、In、Tl等分离出来,最后以Ga—CAS— 相似文献
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《吉林地质》2015,(4)
本文围绕金属元素的溶剂萃取进行了一系列研究,考察了8-羟基喹啉与羧酸有机萃取剂仲辛基苯氧基乙酸(以下简称CA12)对稀土元素的萃取效应。研究了8-羟基喹啉与羧酸萃取剂CA12的混合体系在硝酸介质中对稀土金属的萃取,对不同的稀土元素,存在不同的协同萃取效应。具体研究了混合体系对15种稀土元素的萃取行为。考察了混合萃取体系对不同稀土元素的分离系数,并与CA12的分离稀土元素的分离系数进行了比较。通过实验证明对于这15种稀土元素均有着较强的协同效应,并进行了反萃实验。通过实验得出在较低的硝酸浓度下具有较高的反萃率。因此,比较低的硝酸浓度说明8-羟基喹啉+CA12的混合体系能够用于实际的分离应用中。 相似文献
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A series of batch-type experiments with acetate acid as the primary substrate were performed using enrichment cultures developed from the anaerobic sludge to investigate the effect of acetate acid on tetrachloroethylene （PCE） biodegradation. Experimental results indicated that acetate acid was an efficient electron donor in affecting the biotransformability of PCE. Trichloroethylene （TCE） was the primary dehalogenation product, and small amounts of dichloroethylenes （DCEs） were also detected. No significant further DCEs degradation was detected. PCE degradation rate in the experiment was 36.6 times faster than background rate in natural groundwater. 相似文献
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Aquatic fulvic acid, isolated from a North Carolina bay lake, was reacted with ozone, an alternative oxidant in drinking water treatment. Ozonated samples were acidified, extracted with ether, dried, concentrated, and methylated prior to GC-MS analysis. Identified reaation products include mono-, di- and tribasic aliphatic acids and benzene tricarboxylic acids. The products with the highest relative concentrations were succinic and malonic acid, although all products were at relatively low concentration levels. Many of the products identified in this study have also been seen among the reaction products of fulvic acid and other oxidants, such as Cl2, CIO2 and KMnO4. 相似文献
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重氮甲烷衍生气相色谱-质谱法检测地下水中17种酸性除草剂 总被引：2，自引：1，他引：1
通过水体中酸性除草剂存在形态的改变,衍生试剂的选择及定量离子的确定,建立了重氮甲烷衍生气相色谱-质谱法检测水中卤代酸类、苯酚类、氮硫杂环类酸性除草剂的方法。重氮甲烷与酸性除草剂发生衍生反应,生成易于气相色谱-质谱测定的酯类化合物,反应条件温和,副产物少。采用自行设计制造的重氮甲烷发生装置,有效控制了二甲基亚硝基苯磺酰胺的反应用量,减少了有害气体的排放。对重氮甲烷连续鼓泡法和间断鼓泡法进行了试验对比。方法检出限为4.95~9.80 ng/L,精密度(RSD,n=7)为1.7%~7.9%,对不同添加水平的回收率进行对比,回收率控制在67.5%~126.3%。 相似文献
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自动电位滴定测定锰矿石中锰的方法研究 总被引：3，自引：3，他引：0
多批次的锰矿石锰含量滴定分析消耗大量人工,随着自动化电位滴定仪的普及,利用仪器完成容量滴定成为可能,而将手工滴定向自动电位滴定移植是当前需要解决的课题。本文建立了一套自动电位滴定仪测定锰矿石中锰含量的方法,确定了相关滴定参数和等当点识别标准。锰矿石样品采用盐酸、磷酸分解,硝酸去除碳和有机物,高氯酸氧化,形成样品溶液。自动电位滴定仪先用硫酸亚铁铵标准溶液对预先移取的重铬酸钾标准溶液和标定空白溶液分别进行氧化还原滴定,用铂复合电极指示,计算得到硫酸亚铁铵标准溶液浓度,再对样品空白溶液和样品溶液进行氧化还原滴定,得到样品锰含量,方法检测范围为5%～60%。采用本法分析国家一级标准物质,测定结果的准确度和精密度高;分析多个产地不同水平的锰矿石样品,测定结果与手工方法进行对照,经t检验无显著性差异。建立的滴定方法自动化程度高、方法稳健,适用于冶炼企业、港口商检等行业,具有推广价值。 相似文献
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Phosphonoformic acid, oxalic acid, glyoxylic acid, and 10 additional organic compounds that are structurally related to them have been reacted with synthetic MnO2 (birnessite), consisting of 22% MnIII and 78% MnIV, and synthetic MnOOH (manganite), consisting solely of MnIII. Significant concentrations of dissolved MnIII were detected in reactions of phosphonoformic acid with MnOOH, indicating that ligand-assisted dissolution took place. Reaction of phosphonoformic acid with MnO2, and reaction of all other organic reactants with either MnOOH or MnO2, yielded only MnII, indicating that reductive dissolution was predominant. As far as reductive dissolution reactions are concerned, MnO2 yields a range of reactivity that is nearly 20-times greater than that of MnOOH. Oxidation converts phosphonoformic acid into orthophosphate ion, glyoxylic acid into formic acid, pyruvic acid into acetic acid, and 2,3-butanedione into acetic acid. When differences in surface area loading are accounted for, oxalic acid, pyruvic acid, and 2,3-butanedione yield virtually the same dissolution rates for the two (hydr)oxides. At pH 5.0, glyoxylic acid reacts 14-times faster with MnO2 than with MnOOH. MnO2 reacts more slowly than MnOOH by a factor of 1/16th with oxamic acid, 1/20th with lactic acid, and 1/33rd with dimethyl oxalate. Adsorptive, complexant, and reductant properties of the 13 organic reactants are believed responsible for the observed reactivity differences. 相似文献
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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
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通过尾矿砂微波加热硫酸溶解新方法的实验,研究了硫酸浓度、液固比及反应时间等因素对尾矿砂酸蚀率的影响。结果显示,在无需搅拌的情况下,微波加热实验的最佳条件酸浓度5mol/L、液固比5.0mL/g都较传统水热法有优势,在反应时间上,微波加热15min就能达到传统水热法2～3h的效果。在酸蚀率相同的情况下,微波加热所用时间仅为传统水热法的1/6,而所用的酸浓度、液固比都较传统水热法小很多。先对尾矿砂直接微波辐照一段时间,然后再加入硫酸进行微波辐照加热溶解,能够促进尾矿砂的溶解,提高尾矿砂的酸蚀率。微波加热条件下,尾矿砂在硫酸浓度8mol/L、液固比5.0mL/g条件下无需搅拌,反应1h后,除透闪石没有完全溶解外,绝大部分的矿物被溶解。与传统加热方式相比,微波加热可显著提高尾矿砂酸溶解速率。 相似文献
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微波消解-等离子体发射光谱法同时测定水中硅铁钠 总被引：1，自引：0，他引：1
讨论使用电感耦合等离子体发射光谱法测定水样中si、Fe、Na时，四种水样前处理方法对测试结果的影响。提出采用HNO3^-HF体系微波消解、H3BO3掩蔽HF的方法前处理水样，用等离子体发射光谱法可同时准确快速地测定水中Si、Fe、Na三种元素的含量。5次测定的相对标准偏差小于4％，加标回收率为89．2％-106％。 相似文献
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HDEHP萃淋树脂,其载体是苯乙烯二乙烯苯的共聚合物,固定相是HDEHP[即二-(2-乙基已基)—磷酸]。这种萃淋树脂的主要优点是萃取容量较大、有机固定相不易脱落、洗脱曲线形状良好,但能否用于矿石中稀土元素的分组,尚未见有报导。本实验选用此种萃淋树脂,以不同浓度的盐酸为流动相,进行了铈组、钇组稀土的分离洗脱条件试验。然后分别加大掩蔽剂,直接用光度法测定各组稀土。 相似文献
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B. Garrido-Rodríguez D. Fernández-Calviño J. C. Nóvoa Muñoz M. Arias-Estévez M. Díaz-Raviña E. Álvarez-Rodríguez M. J. Fernández-Sanjurjo A. Núñez-Delgado 《International Journal of Environmental Science and Technology》2013,10(5):983-994
The aim of this study was to assess the influence of pH on copper mobilization in two copper-rich acid soils (from vineyard and mine) amended with crushed mussel shell. Crushed mussel shell amended soils (0–48 Mg ha?1) were subjected to the effect of several acid and alkali solutions in a batch experiment in order to study their copper release. Copper distribution was studied in decanted soils from batch experiments using a sequential extraction procedure, whereas the effect of crushed mussel shell on copper release kinetics was studied using a stirred flow reactor. When soils were treated with acid solutions, the copper mobilization from non-amended soils was significantly higher than from the amended samples. Major changes in copper fractionation were an increase of the acid soluble fraction in acid-treated vineyard soil samples with shell dose. For the mine soil, the oxidable fraction showed a relevant diminution in acid-treated samples at the highest crushed mussel shell dose. For both soils, copper desorption rates diminished up to 86 % at pH 3 when crushed mussel shell was added. At pH 5, copper release rate was very slow for both soils decreasing up to 98 % for the mine soil amended with the highest shell dose, whereas no differences were observed at pH 7 between amended and non-amended soils. Thus, crushed mussel shell addition could contribute to reduce potential hazard of copper-enriched soils under acidification events. 相似文献