一种用于离子色谱系统的免脱气碳酸盐淋洗液发生器系统

报道了一种免脱气碳酸盐淋洗液发生器系统(含碳酸盐发生器和pH调节器)。碳酸盐淋洗液发生器可在线将纯水转变成设定浓度的碳酸盐淋洗液,该淋洗液再通过电致p H调节器调节pH进而改变淋洗液中碳酸盐/碳酸氢盐的比例,最终实现分离选择性的灵活调控。通过该碳酸盐淋洗液发生器系统可以得到0.5～8 mmol/L之间任意浓度、碳酸盐/碳酸氢盐任意比例的碳酸盐淋洗液;所得淋洗液纯度高,结合离子色谱系统,可用于分析7种常见阴离子,其保留时间的日间相对标准偏差均小于0.76%。     

三电极电致膜阴离子抑制器的构建

制作了一个三电极电致膜抑制器,考察了加电方式、串连电阻阻值、电极间距对改善噪声的影响。相较于传统两电极抑制器,优化得到的三电极抑制器在抑制CO_3~(2-)-淋洗液时在噪声(～2.5倍)和信噪比(2.5～3.6倍)方面皆有一定程度的改善;所得三电极抑制器稳定性好,可与离子色谱结合后检测饮料中6种常见阴离子含量。     

离子液体中聚3-己基噻吩的制备及电致变色性质和器件的研究

以室温离子液体1-丁基-3-甲基咪唑六氟磷酸盐[BMIM]PF₆为溶剂及支持电解质,通过电化学方法制备聚(3-己基噻吩)(PHexT)膜。采用循环伏安法和扫描电子显微镜,对膜的电化学性质及形貌结构进行表征。同时通过紫外可见光谱、计时电流、计时库仑以及计时吸收曲线等方法研究聚合物膜的光谱电化学和电致变色特性,并在此基础上制备PHexT膜的电致变色器件。实验结果表明,在离子液体中制备的PHexT膜光滑致密,掺杂态时为蓝色,脱掺杂时为桔红色,并且具有高的颜色对比度 (40%),较短的响应时间 (2.5 s) 和高的电致变色着色效率 (230cm²/C),该膜制成的固态电致变色器件具有很好的电致变色性能和长的循环寿命。     

烯烃取代的紫罗精合成及全固态电致变色器件

合成了2种烯烃取代的紫罗精分子,通过核磁、红外和紫外测试技术对其结构进行了确证。循环伏安表明,它们都有2个明显的可逆氧化还原峰;并以PEO胶体聚电解质为离子导电层组装出了基于所合成化合物,低能耗、无辐射的全固态电致变色器件,总厚度约2.35mm,同溶液型电致变色器件相比较,全固态化可以提高器件在变色-褪色和开路延时记忆等方面的性能,且固态电致变色器件制作工艺相对简单,便于规模化生产。经优化后制作的电致变色器件施加1.1～3V的电压可产生明显的蓝色或紫色,断电后开路延时记忆可以达到3d。实验测试出大多数器件响应时间小于50ms,循环次数在百万次以上,主要性能指标已经达到电子墨水的显示要求。     

多孔磺化树脂分离柱及其高效离子排斥色谱性能

近年来,由于高效分离柱和高灵敏检测器的研究与应用,使离子色谱技术的发展十分显著。在环境保护、工业生产和科学研究中得到广泛的应用。离子排斥色谱是离子色谱技术中的一个分支,其分离原理建立在Donnan排斥效应的基础上,即分离柱填料上的官能团趋向于在填料颗粒间空体积内的淋洗液和颗粒孔隙内吸留的淋洗液之间形成一种称为Donnan膜的半透膜。这种膜对于离子化程度不同的溶质具有不同的排斥能力而使之得以分离。离子排斥色谱不仅可使有机酸快速分离,也可以从有机酸中分     

可吸附紫精化合物电致变色器件

研究报道了一种基于可吸附的固态紫精化合物电致变色器件. 我们设计并合成了一种新型可吸附的不对称紫精化合物,其一端引入三苯胺基团用以修饰紫精化合物的电致变色性质,另一端引入膦酸基团使其固定于电极上,以提高变色速度,增加器件稳定性. 将所合成的材料应用于器件中,得到了高透过差值和高稳定的电致变色器件. 我们利用紫外-可见-红外分光光度计、电化学工作站以及CIE 1931 %Y_Lxy色度系统对其电致变色性能以及颜色进行了表征.     

活性炭-离子液体凝胶电致动膜材料制备及性能研究

本文通过湿法涂膜和热压复合的方法,制备了基于活性炭-离子液体凝胶的电致动膜材料。使用电化学循环伏安法和原位激光位移传感器分别测定了不同活性炭含量对电致动膜材料的界面电容和电致动位移性能的影响。结果显示膜材料的界面电容和电致动位移性能随着活性炭含量增加而增加。     

氧化铑电致变色薄膜的制备、结构及性能

采用溶胶_凝胶方法在ITO导电基底上制备氧化铑电致变色薄膜 .当在碱性溶液中对薄膜分别施加阴极和阳极电位时 ,薄膜即呈现由亮黄到深绿的可逆变化 .采用原位XRD、TG_DTA、IR、XPS等方法对薄膜的结晶态、热处理过程以及膜的化学组成进行分析 .应用交流阻抗法计算了薄膜变色过程的扩散系数 ,结果表明该膜基本可以用于变色器件     

基于无机电致变色材料的变色储能器件

电致变色和电化学储能的原理均是基于电荷在电极中的嵌入或脱出而发生的氧化还原反应,具有相同的电化学本质。将电致变色和电化学储能功能集成在一起的电化学器件即电致变色储能器件。以锂离子电池为代表的电化学储能器件已广泛商业化,单一功能的电致变色器件也已被广泛报道并有商业化应用,但有关电致变色储能器件的研究仍然停留在实验阶段。该类器件在电化学储能的同时,可以改变其在可见光甚至红外波段的透射率,并可用颜色指示器件的荷电状态,为电化学器件提供新的应用前景。电致变色储能器件主要包括电致变色超级电容器、电致变色电池和光驱动电致变色智能窗等。电致变色超级电容器和电致变色电池以同时具有电致变色效应和电荷存储性质的材料为正负电极,光驱动电致变色智能窗则还包括将光能转化为电能的光电转换部分。这些器件可用于建筑节能智能窗、静态显示、智能传感等。此外,在柔性基底上制备的可穿戴电致变色储能器件在智能服装、植入显示器和电子皮肤等方面具有应用潜力。本文从基本原理、研究进展和应用领域等方面对无机电致变色储能材料与器件进行综述,并提出未来的研究展望。     

苯胺四聚体薄膜的制备及其电致变色性能

以苯胺四聚体做为电致变色材料, 在保持ITO有效涂覆面积不变的情况下, 通过控制溶液浓度和用量的方式控制膜厚, 采用自然铺展的方式制备得到了均匀的电致变色膜. 循环伏安特性曲线表明, 在－0.2～0.8 V电压范围内, 随着电压的升高, 苯胺四聚体结构发生从还原态到中间态再到氧化态的转变, 并伴随着颜色从浅黄色到绿色再到蓝色的变化. 研究发现, 电解质溶液种类和膜厚对苯胺四聚体膜的电致变色性能有较大影响. 苯胺四聚体膜的对比度按照HCl, HNO₃, H₂SO₄, LiClO₄电解质溶液的顺序依次降低. 随着膜厚度增加, 苯胺四聚体膜的对比度增加, 响应时间延长. 当采用樟脑磺酸掺杂的苯胺四聚体制备电致变色膜时, 在其他条件相同的情况下可以提高苯胺四聚体膜的对比度并同时缩短响应时间.     

Simultaneous separation of alkali and alkaline-earth cations on polybutadiene-maleic acid-coated stationary phase by mineral acid eluents

The simultaneous separation of alkali and alkaline-earth cations on polybutadiene-maleic acid-coated silica columns can be achieved with mineral acid eluents. Simple ion-exchange retention mechanisms and the high selectivity of eluent hydronium ions towards the carboxylate group are the basis for the separation. Use of mineral acid eluents allows using this column in both single column and suppressor-based IC systems. Both types of ion chromatography systems provide detection limits in the low-ng/ml range with excellent linearity.     

Influence of multivalent ions on power production from mixing salt and fresh water with a reverse electrodialysis system

Reverse electrodialysis is a membrane-based technique for production of sustainable electricity from controlled mixing of a diluted electrolyte solution (e.g., river water) and a concentrated electrolyte solution (e.g., sea water). Reverse electrodialysis has been investigated with pure sodium chloride solutions. In practice, however, in most cases also other ions are present in both feed solutions. In the present paper, the effect of multivalent ions on the performance of a reverse electrodialysis stack was investigated. Results show that, besides a higher stack resistance in presence of multivalent ions, especially the presence of multivalent ions in the dilute solution has a lowering effect on the stack voltage. This can be explained by an observed transport of these ions from the diluted electrolyte solution to the concentrated electrolyte solution. In order to prevent or hamper this transport against the activity gradient, monovalent-selective membranes can be used. This shows indeed better results with respect to the stack voltage. Therefore, it would be beneficial to use monovalent-selective membranes in reverse electrodialysis, especially in the case of a relatively high content of multivalent ions in the dilute (i.e., in the first stages of the installation where the sodium chloride content in the dilute is still relatively low).     

Separation of oxyanions of phosphorus by single column ion chromatography

Separation of mixtures containing hypophosphite, phosphite, orthophosphate, chloride, nitrate and sulphate ions has been achieved using a Vydac 300 IC 405 column, refractive index detection and eluents which were 2mM in p-hydroxy benzoic acid or 4mM in p-amino benzoic acid (adjusted to ph 5.5). Calibration curves were linear over the concentration range 3 to 30 mg P/l.; and the precision (RSD for peak heights in mixtures) was < +/- 10%. Using p-hydroxy benzoic acid, detection of eluted peaks by indirect UV absorption was equally satisfactory. In an initial survey, the elution behaviour of nine oxyanions of phosphorus (simple ions and condensed species) was examined, using eluents containing different organic carboxylic acids (six aliphatic and nine aromatic), present at levels of 1 to 5m(M); with the pH adjusted to values between 3 and 8.6. No suitable conditions for separating mixtures containing condensed phosphates were identified.     

Using ultrapure water in ion chromatography to run analyses at the ng/L level

Thanks to enhanced capabilities, ion chromatography (IC) occupies an increasing position in many types of applications. Achieving ideal performances for an extended life-time can only be reached, however, if the IC system is operated in optimum experimental conditions. Among the various parameters that need to be controlled, water is particularly important, because it is used throughout the analysis, from sample preparation to column rinsing, elution, and mobile phase preparation. More and more, devices are included in IC systems to generate the eluent in situ, and ultrapure water becomes the major reagent. Data of pre-concentration of high purity water show that detection limits at the ng/L level can be expected with water purified using the right combination of technologies.     

毛细管离子色谱分析系统研究进展

离子色谱是目前分析离子型样品的成熟技术,其水相工作介质的特点相对于液相色谱更适合于生物样品的分析。毛细管离子色谱(CIC)由于其节省样品的特点在生物分析方面的优势更为明显。CIC大体上可分为开管型、填充柱型和整体柱型3种类型。本文以填充型CIC几大关键部件技术发展为主线,综述了近年来CIC的研究进展。     

Quantitative ion chromatography with an ultraviolet absorbance detector without standards

Samples of ions are studied by non-suppressed ion chromatography and an ultraviolet absorbance detector. When two eluents of similar properties but different absorptivities per normal concentration are used in succession, two distinct chromatograms are obtained for the same sample. This information can be used to predict the number of equivalents of each ion present, as well as its absorptivity. In conjunction with elution-time studies, molar concentrations can also be obtained. The procedure does not require knowledge of the identity or any physical properties of the ionic species, and is applicable to ions with arbitrary absorption strengths.     

Transport of ions of pyrophosphoric acid through chemically different anion-exchange membranes

Characteristics of mass transport of the anions of pyrophosphoric acid are investigated during electrodialysis through MA-40 and MA-41 anion-exchange membranes. It is established that the rate of mass transport for counterions is greater through the MA-41 membrane than the MA-40 membrane, and thus the former can be used for demineralizing solutions with salts of pyrophosphoric acid. Higher selectivity to pyrophosphate ions is found for the MA-40 membrane compared to the MA-41 membrane in the electrodialysis of mixtures of pyrophosphate and hydropyrophosphate ions, and thus the MA-40 membrane can be regarded as promising for the separation of such mixtures.     

Optimization of enantiomeric separations with chiral bonded phases

Summary The preparation and properties of chiral bonded phases with amino acid groups are described. These phases were used in non-polar eluents and in aqueous systems in the presence of Cu²⁺ ions in the ligand-exchange mode. The optimization of chiral resolution is demonstrated for both cases. With non-polar eluents similarity between bonded groups and solutes is required. The elution could be accelerated by non-protonic moderators. Ligand-exchange separation is influenced by the copper content of the eluent and the stationary phase, the organic moderator concentration, the pH and ionic strength of the buffer and by the temperature. Structural requirements of both the bonded groups and of the solutes for chiral separation are discussed.     

A separation scheme for the analysis of multicomponent samples

A sequential separation scheme has been devised for the quantitative analytical separation of 27 different metal ions. Five different Chromatographic and ion-exchange columns are used to separate the metal ions into groups. The metal ions of each group are eluted separately from each column by means of selective eluents. Following separation, the metal ions are determined by titrimetry, flame spectrometry or other appropriate analytical methods. The reliability of the proposed scheme has been demonstrated by extensive testing, including the analysis of U.S. National Bureau of Standards samples. The scheme can be used for macro or micro quantities.     

Separation of oxyanions of sulphur by single-column ion-chromatography

After stabilization of sulphite by addition of a five-fold excess of formaldehyde, mixtures of sulphite, sulphate and thiosulphate are readily separated by HPLC. For use with Vydac columns (302IC or 300IC) a suitable eluent is 1-3mM phthalic acid (pH 5-6), and the eluted ions may be detected by means of the change in refractive index or the absorbance at 290 nm. With a flow-rate of 2 ml/min, anion elution times are about 2.7 (0.7) min for HOCH(2)SO(-)(3), 7.5 (2.6) min for SO(2-)(4) and 8.4 (5.2) min for S(2)O(2-)(3), the values in parentheses being those for the shorter 300IC column. Detection limits for sulphite and sulphate were around 1 mg/l., with relative standard deviations of 2-3% at higher levels. The sensitivity for S(2)O(2-)(3) was an order of magnitude lower. The proposed method has advantages over earlier procedures based on alkaline eluents.