离子色谱法测定地表水和饮用水中亚氯酸盐、溴酸盐和氯酸盐

采用KOH梯度淋洗离子色谱法测定地表水和饮用水中ClO2-、BrO3-和ClO3-,在试验确定的条件下,3种离子与F-、Cl-、NO2-、NO3-、SO2-4、Br-、I-等7种离子分离度良好。 ClO2-、BrO3-、ClO3-在50．0μg/L～1000μg/L范围内线性良好,检出限分别为5．2μg/L、8．9μg/L、7．6μg/L,环境水样加标平行测定的RSD分别为2．1％～5．4％、4．1％～5．4％、2．5％～4．8％,两个质量浓度水平加标的平均回收率分别为93．7％～96．5％、90．3％～94．8％、98．7％～111％。     

离子色谱法测定地表水中总氮

采用碱性过硫酸钾消解水样,OnGuardⅡBa柱萃取、过滤,去除消解液中大量硫酸盐,离子色谱法测定地表水中总氮含量。试验表明,方法在0ms／L～20．0mg／L之间线性良好,相关系数r为0．9994,方法检出限为0．007mg／L。该方法与国标法同时测定标准物质,测定值均在定值范围内,6次平行测定结果的RSD分别为2．3％和1．8％,地表水样的加标回收率为95．7％～105％。实际水样的测定结果与国标法比对,无明显差异。     

离子选择电极法测定水中氯化物

采用离子选择电极法测定水中氯化物,通过试验确定参比溶液、离子强度调节剂的配制,并用添加氯离子氧化剂和离子浓度调节剂的方法排除干扰离子对测定的影响,使得复合氯离子电极测得的能斯特曲线响应系数为93．2％。标准品的加标回收率为99．8％±0．6％,测定结果的 RSD为0．4％。用该方法与国标硝酸银滴定法同时测定实际水样,两方法的测定值绝对误差在允许范围内。     

三维电极法处理氯苯废水

采用三维电极法处理氯苯废水。研究了外加槽电流、停留时间、氯苯初始质量浓度、废水初始pH等对氯苯去除率的影响。实验结果表明：外加槽电流增大,氯苯去除率明显提高;停留时间延长,氯苯去除率提高;而废水初始pH和氯苯初始质量浓度的变化对氯苯去除率影响不大。在外加槽电流为2．0A、氯苯初始质量浓度为1～200mg／L、停留时间为40～60min、废水初始pH为7的条件下,氯苯去除率达83％以上。并探讨了氯苯的电化学降解机理。     

不同涂层电极和抑制剂对电化学氧化降解苯酚的影响

采用热分解法和电沉积法2种工艺制得4个二氧化铅电极,用扫描电镜（SEM）观察了电极表面形貌.以水杨酸(2-HBA)为捕获剂,用高效液相色谱仪测定羟基自由基与水杨酸的羟基化产物2,5-二羟基苯甲酸(2,5-DHBA)的量作为产生的羟基自由基的浓度.通过羟基自由基的浓度的测定和苯酚的降解,研究了不同涂层电极和抑制剂对电化学氧化对苯酚降解的影响.热分解电极、无掺杂电极、掺铋电极和掺镧电极产生羟基自由基的最大浓度分别为0.781、1.048、1.838、2.044 μmol/L,以这4个电极为阳极对苯酚进行电解, 1.5　h苯酚去除率分别为87.30%、93.55%、97.95%、98.70%,5　h　TOC去除率分别为86.75%、94.26%、98.53%、99.60%;以掺镧电极为阳极,加入抑制剂CO^2-₃、PO^3-₄、CH₃ＣＯＯ^-产生的羟基自由基的最大浓度分别为无检出、0.170 μmol/L、0.270 μmol/L,对苯酚进行电解,5 h苯酚去除率分别为99.06%、99.98%、99.79%.电沉积法制得电极对苯酚的降解效果优于热分解法制得的电极,而掺杂的电极优于无掺杂的电极,掺镧电极对苯酚降解效果最好,抑制剂CO^2-₃、PO^3-₄、CH₃ＣＯＯ^-存在时会对苯酚的降解起到阻碍作用,CO^2-₃阻碍作用最强.不同制备方法和掺杂不同添加剂制得的电极的催化性能不同,对苯酚的降解效果也不同;羟基自由基的浓度越大,苯酚的降解效果越好,抑制剂捕获了产生的羟基自由基,不利于苯酚的降解.     

离子色谱法测定工作场所空气中的草铵膦

用玻璃纤维滤纸采集工作场所空气中的草铵膦,经Metrosep A Supp 5-150型阴离子色谱柱分离,以1.92mmol/L碳酸钠-0.60mmol/L碳酸氢钠混合溶液为流动相,用离子色谱法测定。该方法在0mg/L~1.04mg/L范围内线性良好,方法检出限为0.012mg/L,按采集30 L空气计算,最低检出值为0.004mg/m3。空白玻璃纤维滤纸的加标回收率为93.7%~102%,标准溶液6次测定结果的RSD为0.8%~4.3%。     

Electroreduction of hexavalent chromium using a porous titanium flow-through electrode and intelligent prediction based on a back propagation neural network

● Titanium-based flow-through electrode achieved high Cr(VI) reduction efficiency. ● Flow-through pattern enhanced the mass transfer and reduced cathodic polarization. ● BPNN predicted the optimal electroreduction conditions of flow-through cell. Flow-through electrodes have been demonstrated to be effective for electroreduction of Cr(VI), but shortcomings are tedious preparation and short lifetimes. Herein, porous titanium available in the market was studied as a flow-through electrode for Cr(VI) electroreduction. In addition, the intelligent prediction of electrolytic performance based on a back propagation neural network (BPNN) was developed. Voltametric studies revealed that Cr(VI) electroreduction was a diffusion-controlled process. Use of the flow-through mode achieved a high limiting diffusion current as a result of enhanced mass transfer and favorable kinetics. Electroreduction of Cr(VI) in the flow-through system was 1.95 times higher than in a parallel-plate electrode system. When the influent (initial pH 2.0 and 106 mg/L Cr(VI)) was treated at 5.0 V and a flux of 51 L/(h·m²), a reduction efficiency of ~99.9% was obtained without cyclic electrolysis process. Sulfate served as the supporting electrolyte and pH regulator, as reactive CrSO₇²⁻ species were formed as a result of feeding HSO₄⁻. Cr(III) was confirmed as the final product due to the sequential three-electron transport or disproportionation of the intermediate. The developed BPNN model achieved good prediction accuracy with respect to Cr(VI) electroreduction with a high correlation coefficient (R² = 0.943). Additionally, the electroreduction efficiencies for various operating inputs were predicted based on the BPNN model, which demonstrates the evolutionary role of intelligent systems in future electrochemical technologies.     

离子色谱法同时测定水中的甲酸、乙酸、丙烯酸和氯乙酸

建立了离子色谱电导同时检测水中甲酸、乙酸、丙烯酸和氯乙酸的方法,当采用1.0mL/min、1mmol/L KOH淋洗液梯度洗脱时可达到样品中甲酸、乙酸、丙烯酸和氯乙酸分离分析的目的;乙酸、甲酸、丙烯酸和氯乙酸的线性范围分别为0.01～10.0、0.01～20.0、0.01～20.0和0.01～20.0mg/L,检出限分...     

Bi_2MoO_6薄膜电极光电催化氧化处理氰化物的研究

本文采用非晶态配合物法及浸渍提拉法在导电玻璃基底上制备了Bi2MoO6薄膜电极,采用此电极在可见光(λ420 nm)照射下进行了光电催化氧化处理氰化物的研究.通过场发射扫描电子显微镜和X射线衍射对电极的晶体结构进行了表征,发现导电玻璃基底上充分而平均地覆盖着黄色的纳米Bi2MoO6颗粒,形成了γ-Bi2MoO6相.在Bi2MoO6电极处理络合态氰化物Cu(CN)2-3实验中,总氰化物的去除率和Cu的回收率大致是随着电压的升高而增大,当电压为2.0 V,反应时间为120 min时,处理效果最好,剩余总氰化物和Cu的含量分别为30%和35%.破络合后的Cu2+一部分以Cu(Ⅱ)形式沉积在阳极上,一部分转化为Cu单质沉积在阴极上.在Bi2MoO6电极处理自由态氰化物NaCN实验中,总氰化物的去除率大致也是随着电压的升高而增大,当电压为2.0 V,反应时间为120 min时,剩余总氰化物含量为5%.     

离子选择电极法测定粉煤灰中的氟

建立了用离子选择电极测定粉煤灰中氟含量的方法,用硝酸钾—柠檬酸钠作为离子强度调节剂,并采用碱熔法处理样品,测定结果的相对标准偏差为1.55%～2.06%,回收率93.89%～98.35%,表明方法的准确度较高,可用于粉煤灰样品中氟的简单分析。