纳米TiO2/CNTs复合材料的制备及其光学性质

TiO2在碳纳米管上的复合材料可以增加材料的光催化性能,已成为新的研究热点.本文采用低温液相法成功地合成了TiO2/CNTs复合材料,并用TEM、XRD和UV-vis对材料进行了表征,结果表明,TiO2很好地分散在CNTs上,具有显著的催化效果,有很好的应用前景.     

纳米TiO_2固相萃取原子吸收光谱法测定工业废水中铅与镉

主要研究了纳米TiO2固相萃取与原子吸收光谱法测定工业废水中铅与镉的方法。合成了3种不同粒径的纳米TiO2,探讨了粒径对铅与镉离子分离富集效率的影响,发现其萃取效率随着粒径的增大而降低。在原子吸收光谱仪最佳操作条件下,工业废水样品中镉与铅的检出限分别为0.010和0.046μg/L。工业废水中铅与镉的分析结果表明,该方法具有灵敏度高、简便快速、相对误差较小等特点。     

纳米TiO 2 -碳纳米管复合膜修饰电极伏安法测定水中α -萘酚和β -萘酚

摘要：制备了一种新型的纳米TiO2-碳纳米管复合膜修饰电极，在pH值为5.57的NaAc-HAc缓冲溶液中，研究了α-萘酚和β-萘酚在该修饰电极上的电化学行为，据此建立了纳米TiO2-碳纳米管复合膜修饰电极伏安法测定水中α-萘酚和β-萘酚的方法。优化了试验条件，α-萘酚和β-萘酚分别在8.3×10^-7mol／L—1.0×10^-5mol／L和7.8×10^-7mol／L—1.0×10^-5mol／L范围内，浓度与氧化峰电流呈良好的线性关系，开路富集3min，检出限分别为3.5××10^-7mol／L和2.3×10^-7mol／L，模拟水样测定的回收率为97.6％—101％。     

自动电位滴定法测定水中氯离子

以银电极为响应电极，用硝酸银溶液滴定水中氯离子，等当点时，产生电位突跃，以此确定终点电位，在仪器上锁定的此终点电位值，从而完成样品的自动分析。     

纳米金修饰分子印迹聚合膜电极检测双酚A

以纳米金修饰玻碳电极为基础电极,以双酚A为模板分子,以邻氨基苯硫酚为聚合单体,采用循环伏安法电聚合制备分子印迹聚合膜,利用循环伏安和交流阻抗法研究电极的电化学特性。结果表明,双酚A在修饰电极表面的反应是一个受吸附控制的等电子、质子转移的不可逆反应。采用差分脉冲伏安法检测双酚A,线性范围为5. 0×10~(-6)mol/L～4. 0×10~(-4)mol/L,检出限为2. 3×10~(-7)mol/L。将该电极用于自来水和牛奶样品的测定,结果均为未检出,加标回收率分别为93. 5%和95. 4%,3次测定结果的RSD分别为4. 0%和5. 7%。     

电极法测定水中氟化物的几点体会

1由于温度对电极法的影响 ,测定样品时必须同时测定工作曲线 ,才能保证样品测定值的准确可靠。 2待测液的浓度愈低 ,电极响应时间愈长 ,有时达 1 0分钟以上才能读数。一般情况 ,从电极接触待测液时间起 5分钟左右 ,电极电位变化范围小于 0 .5 mv,就可记录电极电位。3为消除电极的“记忆性”每测一个样品前应洗电极到空白液电极电位以下 ,当样品浓度差别大时应备用两支氟电极 ,分别测定。电极法测定水中氟化物的几点体会@焦晓娟$河北省环境监测中心站!河北石家庄050051     

溶解氧测试中的稳定性研究

一、电极灵敏度的自然衰减 测氧电极是溶解氧测试仪最关键的部件,电极灵敏度的自然衰减是溶解氧测试主要的不稳定因素。测氧电极为隔膜式原电池型结构,阳极是纯铅做的圆筒,阴极为直径8mm的玻璃碳片,电极内注有1M NaOH支持电解质,玻璃碳面复有20μ厚的聚四氟乙烯薄膜。当空气或水中氧气透过薄膜扩散至玻璃碳表面,电极两端接有负载时,将产生电流,该电流称为扩散电流。扩散电流与试样中氧浓度、阴极面积、薄膜材料的性质、厚度、溶液温度有关。在一定的温度下,扩散电流可近似地写成下式:     

火焰原子吸收法测定土壤中的铅

建立了一种以 HNO3-HCl-HCl O4 -HF对土壤样品进行消化 ,火焰原子吸收测定铅的方法。该法用于实际样品的测定时 ,相对标准偏差小于 2 .3 % ,加标回收率为 98%～ 1 0 2 %。     

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。     

土壤中氰化物的快速测定——以江苏镇江电镀园区土壤监测为例

以电镀园区为例,利用流动注射仪对园区土壤中的氰化物进行了快速测定,并与传统分光光度法进行了比对.结果表明：流动注射法中准确度和精密度均满足监测要求;pH为3.8、蒸馏温度为125℃是氰化物测定的最佳实验条件;流动注射法和传统方法测试的结果相对标准偏差（RSD）均小于8％.该法具有分析速度快、稳定性好等特点,适用于大批量土壤样品测定.     

Performance of an electrochemical COD (chemical oxygen demand) sensor with an electrode-surface grinding unit

An electrochemical COD (chemical oxygen demand) sensor using an electrode-surface grinding unit was investigated. The electrolyzing (oxidizing) action of copper on an organic species was used as the basis of the COD measuring sensor. Using a simple three-electrode cell and a surface grinding unit, the organic species is activated by the catalytic action of copper and oxidized at a working electrode, poised at a positive potential. When synthetic wastewater was fed into the system, the measured Coulombic yields were found to be dependent on the COD of the synthetic wastewater. A linear correlation between the Coulombic yields and the COD of the synthetic wastewater was established (10-1000 mg L(-1)) when the electrode-surface grinding procedure was activated briefly at 8 h intervals. When various kinds of wastewater samples obtained from various sewage treatment plants were measured, linear correlations (r(2)> or = 0.92) between the measured EOD (electrochemical oxygen demand) value and COD of the samples were observed. At a practical wastewater treatment plant, the measurement system was successfully operated with high accuracy and good stability over 3 months. These experimental results show that the application of the measurement system would be a rapid and practical method for the determination of COD in water industries.     

Formation of a Mercury Plated Carbon Paste Electrode by Electroreduction of a Mercury(II) Diethyldithiocarbamate Modified Carbon Paste

A novel approach to formation of a mercury film electrode (MFE) at the surface of a carbon paste electrode is proposed in this paper. This MFE is easy to fabricate, has good reproducibility and avoids the use of a plating mercury solution. In this new type of MFE, mercuric diethyldithiocarbamate (Hg(DDTC)2) was mixed with graphite powder and paraffin oil to form a chemically modified carbon paste electrode. When a -0.95V potential was applied to the electrode, the Hg(II) (in Hg(DDTC)2) was reduced to metallic Hg, thus forming a mercury film at the surface of the carbon paste electrode. The characteristics of this MFE were studied. This modified electrode was used in anodic stripping voltammetry. Conditions for the simultaneous determination of trace amount of Pb(II) and Cd(II) were also investigated.     

Analysis of Pesticides Using a Polyppyrole Modified Electrode

Electrochemical methods can provide fast, sensitive and sometimes real time detection of pesticides. In the course of this work, a dispersed mercury electrode has been used to detect pesticides electrochemically. The electrode was prepared by depositing a thin mercury film on a glassy carbon disc and then coating a layer of polypyrrole on the disc. The effect of coating thickness on detection sensitivity was studied. A thin mercury film of 0.34 µm dispersed by one cycle polymerization of pyrrole was preferred. The influence of electrolyte, pH and organic solvent content on pesticide response was also investigated. The polypyrrole dispersed mercury electrode (Hg-PPy/GC) was not suitable for a pH above 6 but it can tolerate acetonitrile up to 10% at which concentration the mercury film coated glassy carbon electrode (Hg/GC) failed to response. Methyl parathion, methyl azinphos, parathion and fenitrothion were detected. The sensitivity of the dispersed mercury electrode was similar to a normal thin mercury film electrode in this case. A good response can be obtained for 1 ppm pesticides using fast linear sweeping voltammetry.     

Voltammetric determination of platinum at a lead film electrode in environmental water samples

The paper presents the first report on the application of a lead film electrode for the determination of ultratrace concentrations of platinum. The procedure is based on preconcentration of the Pt(IV)-formaldehyde complexes at an in situ plated lead film electrode held at ?0.9 V (vs. Ag/AgCl), followed by a negatively sweeping differential pulse voltammetric scan. The composition of the supporting electrolyte, the influence of accumulation potential and time on the sensitivity of platinum responses are discussed. The detection limit of Pt(IV) with the accumulation time of 60 was equal to 9.2?×?10^?12 mol L^?1. The application of this method was tested by recovery of Pt(IV) from spiked environmental water samples.     

电化学传感法测定水中亚硝酸盐

借助于简单可控的在线电聚合方法,溴酚蓝被修饰到玻碳电极表面,制备了聚溴酚蓝修饰玻碳电极。实验表明,聚溴酚蓝薄膜对于亚硝酸盐的电化学氧化具有很好的催化作用。经实验优化,聚溴酚蓝膜的最佳厚度为聚合20圈,最佳的检测底液为pH=4.0的0.01 mol/L磷酸盐缓冲溶液。亚硝酸盐在传感器上的电化学氧化是一个双电子双质子参与的过程。在最佳检测条件下,亚硝酸盐的氧化峰电流与其浓度在0.02~109.1μmol/L范围内有良好的线性关系,检测限低至5 nmol/L(S/N=3),所制备的亚硝酸盐传感器线性范围宽、检出限低、稳定性和重现性好、抗干扰能力强,将传感器应用于东湖水样中亚硝酸盐含量的测定,结果令人满意。     

Biomonitoring of testate amoebae (protozoa) as toxic metals absorbed in aquatic bryophytes from the Hg-Tl mineralized area (China)

A new method has been developed for the determination of chemical oxygen demand (COD) in pulping effluent using chemometrics-assisted spectrophotometry. Two calibration models were established by inducing UV-visible spectroscopy (model 1) and derivative spectroscopy (model 2), combined with the chemometrics software Smica-P. Correlation coefficients of the two models are 0.9954 (model 1) and 0.9963 (model 2) when COD of samples is in the range of 0 to 405 mg/L. Sensitivities of the two models are 0.0061 (model 1) and 0.0056 (model 2) and method detection limits are 2.02?C2.45 mg/L (model 1) and 2.13?C2.51 mg/L (model 2). Validation experiment showed that the average standard deviation of model 2 was 1.11 and that of model 1 was 1.54. Similarly, average relative error of model 2 (4.25%) was lower than model 1 (5.00%), which indicated that the predictability of model 2 was better than that of model 1. Chemometrics-assisted spectrophotometry method did not need chemical reagents and digestion which were required in the conventional methods, and the testing time of the new method was significantly shorter than the conventional ones. The proposed method can be used to measure COD in pulping effluent as an environmentally friendly approach with satisfactory results.     

Cu 2+ 对分光光度法测定水样中COD的影响

通过测定Cr^3＋、Cr2O7^2-和Cu^2＋吸收曲线及标准水样的COD值，研究了Cu^2＋对分光光度法测定COD的影响。结果表明，可改变吸收波长和量程消除较高质量浓度Cu^2＋对COD测定值产生的明显影响。当水样Cu^2＋质量浓度超过400mg／L时，须将水样稀释后采用低量程法进行测定。     

Measurement of chemical oxygen demand (COD) in natural water samples by flow injection ozonation chemiluminescence (FI-CL) technique

COD determination based on ozone oxidation of alpha-naphthol combined with UV radiation (UV-O3) has been studied in the present work. Utilizing the phenomenon that luminol can be oxidized by the dissolved ozone to produce luminescence, we have established a new method of utilizing aqueous chemiluminescence to determine COD. The kinetics and mechanism of the ozonation reaction of alpha-naphthol have been investigated in order to gain a better understanding of the general applicability and limitation of the technique. Real world samples were analyzed and the results show that the relative error of COD(FI-CL) measurement for water samples was < 10%. Compared with the results of the conventional potassium permanganate method, the COD values of the FI-CL method are consistently higher (0-20% relative). The higher COD values suggest that the ozone-UV system is a more effective oxidation technique.     

颗粒活性炭负载TiO2薄膜用于染料污水脱色的研究

研究了溶胶-凝胶法制备以活性炭为载体的TiO2膜。通过实验确定了溶胶一凝胶体系的最佳组成,对涂膜的次数、煅烧温度、保温时间等因素进行实验,确定了涂膜的最佳工艺,并用于处理有机染料污水,脱色率达92％。     

南四湖港口污染物扩散区COD降解系数的研究

本文对南四湖港口污染物扩散区内的ＣＯＤ降解规律进行了室内模拟试验研究，采用最小二乘法估计出了ＣＯＤ可降解部分的降解系数和不可降解部分的百分比，并通过方差分析验证了模型的可靠性。ＣＯＤ降解系数和不可降解百分比的获取，可以为预测各港口对南四湖水质变化趋势的影响，为制定相应的水污染防治规划和措施，提供了重要的基础数据。