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作者改进了气提法富集水中痕量挥发性有机物装置。研究了实验条件对水中痕量有机物富集的影响,并确定了最佳富集条件。以气提法富集气相色谱/质谱法(GC/MS)测定了水样中痕量挥发性有机物,取得了满意的结果。 相似文献
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复合螯合剂—活性碳柱现场富集天然水中痕量元素 总被引:3,自引:0,他引:3
本文提出了一种适于野外条件下的富集天然水中多个痕量元素的方法。研究了四种螫合剂在活性碳上的吸附特性及多种溶剂、酸、碱洗脱螯合剂的特性。研究了20多个元素在不同pH值下的螯合剂——活性碳的静态和动态吸附性能。采用直径10mm,长80mm柱可在现场富集天然水中不同形态的痕量元素。加入回收率为90~108%。天然水中大量的Na、K、Ca、Mg等元素不被吸附。可用多种分析方法测定。 相似文献
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研究了柱流速和有机物对固相萃取富集水中痕量金属的影响,并比较了两种样品处理方式,发现MAD~(21)SPE的准确度和精确度均超过了传统的螯合-溶剂萃取。 相似文献
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CPA—mA形成纤维富集光度法测定稀土总量 总被引:3,自引:1,他引:3
稀土元素的分离富集方法除萃取法、沉淀法外,离子交换分离富集技术是目前常用的方法。本文拟定了偶氮氯膦—mA螯合形成纤维分离富集、偶氮胂Ⅲ分光光度法测定地质试样中痕量稀土总量。并研究了吸附酸度、柱高、溶液流速等对分离富集痕量稀土元素的影 相似文献
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活性炭柱吸附富集-分光光度法测定饮用水中痕量钼(Ⅵ) 总被引:1,自引:0,他引:1
提出了一种预富集水中痕量钼(VI)的新方法,研究了影响Mo α 安息香肟螯合物定量吸附于活性炭柱上的参数,找出了最佳吸附解吸时的条件。该方法避免了用活性炭作为吸附材料的常规方法中,活性炭只能使用一次的间歇式操作,以及用浓硝酸解吸这种费时污染大的解吸方法,同时用NaOH解吸时,大部分金属离子以氢氧化物沉淀的形式留在活性炭上,减少了干扰。该法已用于测定水中痕量钼(Ⅵ),加标回收率达到94.6%~101.4%,RSD3.6%~8.6%。 相似文献
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固相萃取-高效液相色谱法同时测定水中的对二氯苯与六氯苯 总被引:1,自引:1,他引:1
采用国产新型D4020 大孔吸附树脂作固定相,用自制的玻璃富集柱研究了柱长、上样速度、样品溶液的pH、盐度等因素对对二氯苯与六氯苯吸附率的影响,确定了最佳固相萃取条件,建立了固相萃取-高效液相色谱同时测定水中痕量对二氯苯与六氯苯的分析方法;不同加标水平的对二氯苯与六氯苯的回收率为86.4%~93.9%,RSD≤4.2%,检出限分别为0.85和0.10 ng/mL;方法已用于实际水样分析. 相似文献
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Large-bore coated (LBC) columns were used as sampling and concentrating traps in analyses for traces of organic volatiles in air and water. This simple technique utilizes long metal columns thinly coated with SE-30 for direct trapping of the organics. The sample is simply passed through the LBC column; the trapped organics are then thermally desorbed onto a conventional porous polymer pre-column or onto a second LBC column. If desired, this can be shorter or narrower bore than the initial LBC sampling column. The sample is finally desorbed onto the gas chromatographic column for analysis. Multiple transfers between LBC columns are possible, with increased concentration at each transfer, resulting in a "concentration pump" effect. The technique offers the advantages of great simplicity, efficiency and ease of sample transfer. Samples are obtained with low back-pressure and minimal interfering artifacts. The system shows almost complete imperturbability to moisture. Indifference to moisture and the low back-pressure enable direct sampling of very large volumes of air and even breath. Direct sampling of aqueous systems was also possible. The latter area was not fully investigated but offers potential for water pollution analysis and in direct examination of biological fluids and aqueous flavor extracts where heat sensitivity is a problem. With LBC columns the sampling and concentration sequence exposes the substances sought to no more drastic conditions than those they will be subjected to in the process of gas chromatographic analysis. 相似文献
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Song J Kahveci D Chen M Guo Z Xie E Xu X Besenbacher F Dong M 《Langmuir : the ACS journal of surfaces and colloids》2012,28(14):6157-6162
Use of biocatalysis for industrial synthetic chemistry is on the verge of significant growth. Enzyme immobilization as an effective strategy for improving the enzyme activity has emerged from developments especially in nanoscience and nanotechnology. Here, lipase from Burkholderia cepacia (LBC), as an example of the luxuriant enzymes, was successfully encapsulated in polycaprolactone (PCL) nanofibers, proven by X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Evaluated in both organic and aqueous medium, the activation factor of the encapsulated enzymes in the hydrolysis reaction was generally higher than that in the transesterification reaction. Enhanced catalytic activities were found when 5-20 w/w % of LBC was loaded. The effect of different solvents pretreatment on the activity of immobilized LBC was also investigated. The highest activation factor was found up to 14 for the sample containing acetone-treated LBC/PCL (10 w/w %). The encapsulated lipase reserved 50% of its original activity after the 10th run in the transesterification reaction in hexane medium. The mechanism of activation of lipase catalytic ability based on active PCL nanofiberous matrix is proposed. 相似文献
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金属螯合亲和色谱中的疏水作用 总被引:1,自引:0,他引:1
通过考察盐溶盐和盐析盐浓度对蛋白质在IDA裸柱和金属螯合柱上保留行为的影响,详细研究了金属螯合色谱中的疏水作用,疏水作用的发生、形成的条件以及不同条件下对蛋白质保留值的贡献。实验结果表明,在高浓度和低浓度的盐溶盐以及低浓度盐析盐中,蛋白质在金属螯合柱上的保留主要受静电和配位作用控制,而疏水作用对蛋白质的保留影响很小。对弱亲和性的金属螯合柱以静电作用为主,其大小可用参数Q表征;对强亲和性的IDA-Cu(Ⅱ)柱以配位作用为主。仅在高浓度的盐析盐中,金属螯合柱才呈现较强的疏水作用,支配蛋白质保留。实验证明,金属螯合色谱中疏水作用主要来自固定相间隔臂中的疏水碳链和盐析盐对蛋白质的增疏作用,利用这种疏水作用有可能改善金属螯合色谱分离的选择性。 相似文献
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The concentration sensitivity of a thermal conductivity detector (TCD) depends, among other factors, on the amount of sample mixture in the detector's sensing cell. Since the cell volume has to be appropriately matched with column diameter, it makes the concentration sensitivity of a TCD dependent on column diameter and, therefore, on the speed of gas chromatography. Through reduction of column diameter, higher speed tends to lead to a reduction in the concentration sensitivity of the cell. The factor which the most directly affects the concentration sensitivity of a TCD cell is the heat power conducted through the cell. The higher the power, the greater the sensitivity. The limit of detection of a TCD depends on the concentration-sensitivity of its cell and on the level of statistical errors in the measurement. The errors increase with increasing analysis speed. As the column diameter is reduced, the errors cause additional worsening (on top of the decrease in concentration sensitivity) of the detection limit, dynamic range, and other performance characteristics of the TCD. 相似文献
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采用简便易行的方法自制内径为100 μm的电色谱柱,并考察了其性能,同时研究了磷酸盐缓冲液浓度、乙腈体积分数、电压、柱温对中性化合物保留行为的影响。 相似文献
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Herman JL 《Rapid communications in mass spectrometry : RCM》2005,19(5):696-700
The use of turbulent flow chromatography in conjunction with column switching isocratic focusing was used to perform on-line sample cleanup and concentration of neat rat plasma for the identification of low-level metabolites. The concentration was achieved by focusing multiple injections, which were cleaned by a turbulent flow column, onto an analytical column prior to elution into the mass spectrometer. In addition, the first application of turbulent flow chromatography for on-line sample cleanup of neat bile samples is reported. The on-line cleanup and concentration method extracts and concentrates a sample 20-fold in 1 h, and is completely automated. 相似文献
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J. R. Conder 《Journal of separation science》1984,7(11):615-619
The original plate model of chromatography is extended to the sorption process occurring at the column inlet and the desorption process at the column exit. At the column inlet it is shown that sufficiently wide feed bands undergo no change in concentration but a fall in band width, i.e., the volume of mobile phase occupied by the solute band is reduced. The reduction factor is (1 + k) where k is the mass distribution ratio (capacity factor). Narrower bands suffer partial reduction in both band width and concentration. On desorption at the outlet, however, the change is always in band width and not concentration. A perfect detector registers the true concentration-time profile of the band in the column if the solute mass fraction in the stationary phase is below 10?3 at the column outlet. The risks of stripping the stationary phase at high solute concentrations in analytical and preparative or production gas chromatography are compared. 相似文献
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Enantiomeric resolution of amino acid derivatives on molecularly imprinted polymers as monitored by potentiometric measurements 总被引:2,自引:0,他引:2
L I Andersson A Miyabayashi D J O'Shannessy K Mosbach 《Journal of chromatography. A》1990,516(2):323-331
Potentiometric measurements have been applied to the detection of enantiomeric separations on molecularly imprinted polymers. A flow-through column electrode, based on the use of polymers imprinted against L-phenylalanine anilide, is described. The electrode consisted of a glass column in which the polymer was packed and where the end frits constituted the electrodes. The flow stream potential across the column can be continuously recorded as solvent is pumped through the system. The column resolved the enantiomers of phenylalanine anilide as detected by both UV absorption and potentiometric measurements and the recorded signals could be correlated with the concentration of phenylalanine anilide. The calibration graphs obtained for the UV absorption of phenylalanine anilide were linear over the concentration range investigated, whereas the potentiometric signal was shown to be exponentially linear with concentration. The application of molecular imprints to the preparation of supports suitable for chromatographic separations of enantiomers and for the preparation of specific electrodes is discussed. 相似文献