同多酸和杂多酸修饰微电极的电化学研究——Ⅳ.1:2-磷钼杂多酸薄膜修饰碳纤维微电极的制备和电化性质

本文报道了1:12-磷铜杂多酸(PMo_(12)薄膜修饰碳纤维(CF)微电极的制备及其电化学性质。采用简单,快速的浸渍吸附制备的PMo_(12)薄膜修饰CF电极在酸性介质中具有很高的稳定性和氧化还原活性,电解质溶液的pH值和扫描电位范围对PMo_(12)膜的稳定性和电化学性质产生较大的影响。另一方面,PMo_(12)薄膜修饰CF微电极对酸性水溶液中的PMo_(12)和氯酸根离子(ClO)_3~-)的电催化还原作用也进行了描述。     

Ion chromatographic determination of chloride,chlorate, and perchlorate in sulfuric acid solutions

Summary The determination of chloride and perchlorate by non-suppressed ion chromatography in aqueous process solutions containing a high sulfate background is described. The method is reliable and fast. The sensitivity for perchlorate is lower than for other anions like nitrate, nitrite and chlorate. The detection limits are about 0.3 g/ml with linear calibration curves within a concentration range from 1 to 50 g/ml.     

Use of ion chromatography with post-column reaction for the measurement of tribromide to evaluate bromate levels in drinking water

A user-friendly ion chromatography method in conjunction with a post-column reaction (PCR) achieves practical quantitation limits for the oxyhalides bromate and chlorite of 0.05 μg/l and 0.10 μg/l, respectively. This level of measurement allows for the accurate assessment of bromate contributed to finished drinking waters that have been chlorinated using sodium hypochlorite. The target sensitivity of oxyhalides in the presence of other major ion species typically found in drinking water is achieved by PCR using excess bromide under acidic conditions to form a tribromide species that is detected by ultraviolet spectrometry. The method setup involves non-hazardous materials, as opposed to other recently developed methods that employ somewhat hazardous chemicals for generating the reaction necessary for the detection of bromate at sub-μg/l levels. No pretreatment of the samples is required, other than filtration and quenching of oxidant residual.     

Electroanalysis of Bromate,Iodate and Chlorate at Tungsten Oxide Modified Platinum Microelectrode Arrays

This article describes the direct detection of Bromate, but also of chlorate and iodate, using modified arrays of platinum ultramicroelectrodes. The detection limits for these ions are IO =0.76 μM; BrO =2.34 μM and ClO =133.2 μM. The formation of a suitable tungsten oxide layer and the optimum analytical conditions are described. These oxide layers are formed electrochemically from hydrogen peroxide‐tungstanate solutions in acid conditions. Although film stability may be an issue, particularly at pH>3, these modified arrays of microelectrodes can be used for analytical purposes. After the analysis, the modifying oxide is easily removed and the Pt microelectrode array recovers its original properties.     

A novel stopped flow injection-amperometric procedure for the determination of chlorate

A novel stopped flow injection—amperometric (sFI-Amp) procedure for determination of chlorate has been developed. The reaction of chlorate with excess potassium iodide and hydrochloric acid, forming iodine/triiodide that is further electrochemically reduced at a glassy carbon electrode at +200 mV versus Ag/AgCl electrode is employed. In order to increase sensitivity without using of too high acid concentration, promoting of the reaction by increasing reaction time and temperature can be carried out. This can be done without increase of dispersion of the product zone by stopping the flow while the injected zone is being in a mixing coil which is immersed in a water bath of 55 ± 0.5 °C. In a closed system of FIA, a side reaction of oxygen with iodide is also minimized. Under a set of conditions, linear calibration graphs were in the ranges of 1.2 × 10⁻⁶-6.0 × 10⁻⁵ mol l⁻¹and 6.0 × 10⁻⁵-6.0 × 10⁻⁴ mol l⁻¹. A sample throughput of 25 h⁻¹ was accomplished. Relative standard deviation was 2% (n = 21, 1.2 × 10⁻⁴ mol l⁻¹ chlorate). The proposed sFI-Amp procedure was successfully applied to the determination of chlorate in soil samples from longan plantation area.     

磷钼钒类杂多酸—聚吡咯薄膜修饰电极及其电催化性能研究

合成了磷钼类杂多酸，采用电化学方法首次在导电基体玻碳电极上研制了磷钼钒类杂多酸－聚吡咯薄膜修饰电极，该电极性能稳定，经久耐用，对膜修饰电极的电化学行为进行了表征，研究了膜修饰电极酸性水溶液中的氯酸根、溴酸根，、磺酸根，亚硝酸根，三阶铁离子，     

A review on the electrochemical production of chlorine dioxide from chlorates and hydrogen peroxide

Chlorine dioxide is one of the most interesting oxidants because it combines a strong capacity of oxidation with low formation of hazardous byproducts such as chlorinated organics during its application. Because of that, it is widely used in disinfection of drinking water and, currently, it is aimed to be used in the disinfection of surfaces or buildings. Although it is usually produced by the chemical interaction of chlorite with hypochlorite/chlorine or hydrochloric acid, one interesting alternative for its production is the combination in strongly acidic media of chlorate and hydrogen peroxide. Both compounds are known to be efficiently manufactured with electrochemical technology, opening the possibility of a complete electrochemical process to produce this important oxidant. This review summarizes the recent progress in the electrochemical production of the two raw materials, as well as the complete electrochemical production of chlorine dioxide, not only paying attention to the scientific literature but, most importantly, to recent patents, trying to see in which technology readiness level are each of the technologies and what are the elements of the value chain required for a complete implementation of the technology.     

Reversed flow injection spectrophotometric determination of chlorate

An interfacing has been developed to connect a spectrophotometer with a personal computer and used as a readout system for development of a simple, rapid and sensitive reversed flow injection (rFI) procedure for chlorate determination. The method is based on the oxidation of indigo carmine by chlorate ions in an acidic solution (dil. HCl) leading to the decrease in absorbance at 610 nm. The decrease in absorbance is directly related to the chlorate concentration present in the sample solutions. Optimum conditions for chlorate were examined. A linear calibration graph over the range of 0.1-0.5 mg L⁻¹ chlorate was established with the regression equation of Y = 104.5X + 1.0, r² = 0.9961 (n = 6). The detection limit (3σ) of 0.03 mg L⁻¹, the limit of quantitation (10σ) of 0.10 mg L⁻¹ and the RSD of 3.2% for 0.3 mg L⁻¹ chlorate (n = 11) together with a sample throughput of 92 h⁻¹ were obtained. The recovery of the added chlorate in spiked water samples was 98.5 ± 3.1%. Major interferences for chlorate determination were found to be BrO₃⁻, ClO₂⁻, ClO⁻ and IO₃⁻ which were overcome by using SO₃²⁻ (as Na₂SO₃) as masking agent. The method has been successfully applied for the determination of chlorate in spiked water samples with the minimum reagent consumption of 14.0 mL h⁻¹. Good agreement between the proposed rFIA and the reference methods was found verified by Student's t-test at 95% confidence level.     

离子色谱法同时测定饮用水中溴酸盐、亚氯酸盐、氯酸盐、亚硝酸盐氮、磷酸盐含量

建立了梯度淋洗-离子色谱法同时测定饮用水中的溴酸盐、亚氯酸盐、氯酸盐、亚硝酸盐氮、磷酸盐等多种离子的方法。选用IonPac AS19型分析柱,采用0~45mmol/L的KOH淋洗液梯度淋洗,流速为1.0mL/min,抑制型电导检测器。方法的线性相关系数r0.999 3,相对标准偏差RSD小于6.0%,样品加标回收率为92.8%~111.8%。结果表明,方法具有操作简单、分析快速、结果准确等优点。