氟硅酸溶液中氟硅酸及氢氟酸含量的测定

基于生成氟硅酸钾沉淀和该沉淀水解均析出不同量酸，用碱滴定完成氟硅酸及氢氟酸的连续测定。该方法用于生产实践，结果令人满意。     

磷酸三丁酯在酸水溶液中溶解度的测定

在20~70℃之间,用浊点法测定了磷酸三丁酯在水、盐酸和硫酸溶液体系中的溶解度.水在TBP-煤油有机相中的溶解度D(H2O)是TBP在水中溶解度δ的60倍;随着温度升高纯TBP和煤油稀释的TBP在水相中的溶解度δ都增加,符合Apelblat溶解度模型,即纯TBP在水中的溶解度与温度的关系:lgδ=3.509 4-1 328.31/T;用煤油稀释TBP可以降低TBP在水相中的溶解度δ;随着盐酸和硫酸的浓度的增加,纯TBP在酸液中的溶解度也增加,盐酸的影响更显著.     

金、银、铂、钯合金中钯的选择性滴定方法的研究与应用

建立了丁二肟选择性沉淀分离和析出EDTA-Pd络合物中的EDTA,Pb(NO3)2返滴定测定Pd的新方法,系统地研究了在硝酸或盐酸介质中测定Pd的条件,并对比了本法与《国家标准》分析方法的结果.研究表明:2种方法测得Pd的结果吻合,测定5～30mg Pd,相对误差-0.17% ～ 0.20%;但拟定方法的选择性好,适用性强,分析快速,操作简便、易于掌握.方法已应用于Au、Ag、Pt、Pd合金中5%～99%的Pd含量的测定,结果满意.     

Effect of La2CuO4 electrode area on potentiometric NOx sensor response and its implications on sensing mechanism

The intent of this work is to look at the effects of varying the La₂CuO₄ electrode area and the asymmetry between the sensing and counter electrode in a solid state potentiometric sensor with respect to NO_x sensitivity. NO₂ sensitivity was observed at 500-600 °C with a maximum sensitivity of ∼22 mV/decade [NO₂] observed at 500 °C for the sensor with a La₂CuO₄ electrode area of ∼30 mm². The relationship between NO₂ sensitivity and area is nearly parabolic at 500 °C, decreases linearly with increasing electrode area at 600 °C, and was a mixture of parabolic and linear behavior 550 °C. NO sensitivity varied non-linearly with electrode area with a minima (maximum sensitivity) of ∼−22 mV/decade [NO] at 450 °C for the sensor with a La₂CuO₄ electrode area of 16 mm². The behavior at 400 °C was similar to that of 450 °C, but with smaller sensitivities due to a saturation effect. At 500 °C, NO sensitivity decreases linearly with area.We also used electrochemical impedance spectroscopy (EIS) to investigate the electrochemical processes that are affected when the sensing electrode area is changed. Changes in impedance with exposure to NO_x were attributed to either changes in La₂CuO₄ conductivity due to gas adsorption (high frequency impedance) or electrocatalysis occurring at the electrode/electrolyte interface (total electrode impedance). NO₂ caused a decrease in high frequency impedance while NO caused an increase. In contrast, NO₂ and NO both caused a decrease in the total electrode impedance. The effect of area on both the potentiometric and impedance responses show relationships that can be explained through the mechanistic contributions included in differential electrode equilibria.     

NOx adsorption behavior of LaFeO3 and LaMnO3+δ and its influence on potentiometric sensor response

NO_x adsorption behavior on LaFeO₃ (LFO) and LaMnO_3+δ (LMO) was characterized using temperature controlled methods and mass spectrometry. Temperature program desorption revealed decomposition of complex surface species formation when NO or NO₂ was adsorbed on LFO and LMO. LFO exhibited higher adsorption capacity for NO_x species than LMO and was shown to be more active for NO_x surface conversion. Both effects were attributed to the different B-site cations, with iron in LFO in the 3+ valence state, and manganese in LMO in the 3+ and 4+ valence states. Results from diffuse reflectance infrared spectroscopy were used to identify specific nitrite and nitrate species that are formed on the surfaces of LFO and LMO at room temperature. Temperature programmed reaction revealed a complex NO₂ decomposition mechanism to NO and O₂ for LFO and LMO in which the formation of nitrite and nitrate species serve as intermediates below ∼600 °C. NO_x sensing mechanisms were considered and predicted based on the types and quantities of surface species formed.     

Selective potentiometric determination of uric acid with uricase immobilized on ZnO nanowires

In this study, a potentiometric uric acid biosensor was fabricated by immobilization of uricase onto zinc oxide (ZnO) nanowires. Zinc oxide nanowires with 80-150 nm in diameter and 900 nm to 1.5 μm in lengths were grown on the surface of a gold coated flexible plastic substrate. Uricase was electrostatically immobilized on the surface of well aligned ZnO nanowires resulting in a sensitive, selective, stable and reproducible uric acid biosensor. The potentiometric response of the ZnO sensor vs Ag/AgCl reference electrode was found to be linear over a relatively wide logarithmic concentration range (1-650 μM) suitable for human blood serum. By applying a Nafion^® membrane on the sensor the linear range could be extended to 1-1000 μM at the expense of an increased response time from 6.25 s to less than 9 s. On the other hand the membrane increased the sensor durability considerably. The sensor response was unaffected by normal concentrations of common interferents such as ascorbic acid, glucose, and urea.     

A technique for monitoring SO2 in combustion exhausts: Use of a non-Nernstian sensing element in combination with an upstream catalytic filter

Detection of sulfur dioxide (SO₂) at high temperature (600–750 °C) in the presence of some interferents found in combustion exhausts (NO₂, NO, CO₂, CO, and hydrocarbon (C₃H₆)) is described. The detection scheme involves use of a catalytic filter in front of a non-Nernstian (mixed-potential) sensing element. The catalytic filter was a Ni:Cr powder bed operating at 850 °C, and the sensing elements were pairs of platinum (Pt) and oxide (Ba-promoted copper chromite ((Ba,Cu)_xCr_yO_z) or Sr-modified lanthanum ferrite (LSF)) electrodes on yttria-stabilized zirconia. The Ni:Cr powder bed was capable of reducing the sensing element response to NO₂, NO, CO, and C₃H₆, but the presence of NO₂ or NO (“NO_x”, at 100 ppm by volume) still interfered with the SO₂ response of the Pt–(Ba,Cu)_xCr_yO_z sensing element at 600 °C, causing approximately a 7 mV (20%) reduction in the response to 120 ppm SO₂ and a response equivalent to about 20 ppm SO₂ in the absence of SO₂. The Pt–LSF sensing element, operated at 750 °C, did not suffer from this NO_x interference but at the cost of a reduced SO₂ response magnitude (120 ppm SO₂ yielded 10 mV, in contrast to 30 mV for the Pt-(Ba,Cu)_xCr_yO_z sensing element). The powder bed and Pt–LSF sensing element were operated continuously over approximately 350 h, and the response to SO₂ drifted downward by about 7%, with most of this change occurring during the initial 100 h of operation.     

化学因子分析法测定液体推进剂A

基于测定推进剂Ａ现有分析方法准确度低,神经网络法对仪器要求高等不足,提出了的一种新的分析方法。该方法利用已知酸的电位滴定数据建立多元线性回归数学模型,利用化学因子分解该模型,对未知样进行浓度测定。实际测定结果表明本方法的最大分析误差不超过０．１７％,标准偏差不超过１．９％,满足样品分析要求。     

多元分析法在沉淀滴定中的应用

将多元分析法应用于沉淀滴定之中 ,提出固定电位的方法 ,建立了沉淀滴定中各组分浓度与体积之间关系的数学模型 ,对卤素和硫氰酸盐混合体系进行了测定。     

库仑滴定法测定工业废水中微量砷

以库仑滴定法测定工业废水中微量砷，以死停终点法确定滴定终点，最后以EXCEL处理实验数据，本方法具有灵敏度高，准确，简便快速，仪器便宜，易于推广的特点，特别适用于工厂及县级以下环境监测站进行水中微量砷的检测，方法的回收率为99．3％。