钴掺杂Sr1.5La0.5MnO4的合成及高温电化学性能研究

采用EDTA-柠檬酸法合成了中温固体氧化物燃料电池阴极材料Sr_1.5La_0.5Mn_1-xCo_xO₄（SLMCO_x）,并利用粉末X射线衍射（XRD）、X射线光电子能谱（XPS）以及电化学交流阻抗谱（EIS）进行表征。结果表明,该材料与Ce_0.9Gd_0.1O_1.95（CGO）在1 200℃烧结12 h不发生化学反应。随着Co掺入量的增加,氧化物中Mn³⁺和Co²⁺含量增多,晶格氧含量降低,晶格畸变率增大。交流阻抗谱（EIS）测试结果显示,钴的掺杂明显降低电极的极化电阻,其中Sr_1.5La_0.5Mn_0.7Co_0.3O₄阴极在700℃空气中的极化电阻为0.62 Ω·cm²,明显小于Sr_1.5La_0.5MnO₄阴极在750℃的极化电阻（1.5 Ω·cm²）,表明钴掺杂的Sr_1.5La_0.5Mn_1-xCo_xO₄是一种潜在的IT-SOFC阴极材料。     

(Pr0.9La0.1)2(Ni0.74Cu0.21Ga0.05)O4+δ-Ce0.9Gd0.1O2-δ复合阴极的制备及电化学性质

采用EDTA-柠檬酸盐法制备了（Pr_0.9La_0.1）₂（Ni_0.74Cu_0.21Ga_0.05）O_4+δ（PLNCG）,并与Ce_0.9Gd_0.1O_2-δ（CGO）形成复合阴极PLNCG-CGO。XRD和SEM分析结果表明PLNCG与CGO在1 000℃具有较好的化学相容性。电化学阻抗测试结果表明PLNCG-30% CGO复合阴极在700℃的极化电阻为0.092 Ω·cm²;过电位为39.3 mV时,电流密度达到113.3 mA·cm^-2。氧分压分析表明电极反应的速率控制步骤为电荷转移过程。阳极支撑单电池（Ni-CGO/CGO/PLNCG-30% CGO）在700℃的最大输出功率密度达到569 mW·cm^-2,开路电压（OCV）为0.76 V。综上结果预示PLNCG-30% CGO复合阴极是一种有发展前景的电极材料。     

2-巯基苯并噻唑对铜缓蚀行为的表面增强红外光谱研究

2-巯基苯并噻唑(MBT)是Cu的高效缓蚀剂,但是缓蚀机理存在较大争议.本文通过电化学极化曲线从宏观角度对缓蚀效率进行评估,并利用原位衰减全反射-表面增强红外光谱技术结合理论计算研究了电位控制下的微观吸附构型.结果表明:在较高电位(大于0 V,相对饱和甘汞电极(SCE))下,MBT和金属Cu之间发生电子转移,MBT以硫醇式的环外S和N与金属Cu(I)离子配位在表面形成聚合物膜;在较低电位(小于0 V,vs SCE)下,MBT通过环外S原子以硫醇离子形式在金属Cu表面直立吸附.表面膜阻止了腐蚀介质的侵蚀,起到了较好的缓蚀效果.     

Effects of High Salt Concentration and Residue on Copper and Aluminum Corrosion

Traditional researches on metal corrosion under salt solutions deposit conditions are usually carried out by visual, electron microscopic observations and simple electrochemical measurement via a traditional one-piece electrode. These techniques have difficulties in measuring localized corrosion that frequently occur in inhomogeneous media. This paper reports the results from the experiments using specially shaped coupons and a relatively new method of measuring heterogeneous electrochemical processes, namely, the wire beam electrode(WBE). Preliminary results from copper and aluminum corrosion in highly concentrated sodium chloride solutions with and without solid deposits show that the method is useful in simulating and studying corrosion especially localized corrosion in pipelines.     

试纸法快速测定高粱中单宁的研究

探讨了试纸与单宁反应的最佳条件,提出了用Fe(SCN)3-壳聚糖试纸法快速检测高粱中单宁的方法。结果表明,在pH 7.0～9.0的条件下,单宁与试纸上的显色物质反应生成紫红色稳定络合物,试纸颜色深浅与样品中单宁浓度成正比,通过与标准色阶图谱比较确定单宁浓度。试纸最低检出限达1.0μg/mL,5 min即可实现检测。应用于7种高粱样品中单宁含量的测定,并通过与国标法测定结果比较,本方法可实现半定量检测,已应用于高粱样品中单宁的实时、快速检测。     

相变微胶囊型吸热剂MPCM-2的制备及其控热效果

以十二水合磷酸氢二钠为芯材,乙基纤维素为壁材,采用原位聚合工艺制备了相变微胶囊型吸热剂MPCM-2,其结构和性能经IR、 DSC、TG和粒度分析表征。结果表明：MPCM-2的相变温度为43.34和58.77 ℃,总相变焓值为144.82 J·g^-1,包裹率为67.5%; MPCM颗粒中径为57.26 μm,同时,MPCM-2应用于深水固井水泥浆体系可实现对水化热及水化温升的有效控制。     

Self-cleaning Anti-fouling TiO2/Poly(aryl ether sulfone) Composite Ultrafiltration Membranes

A series of novel TiO2/poly(aryl ether sulfone) ultrafiltration membranes with anti-fouling and self-cleaning properties was designed and prepared. First, anti-photocatalytic degraded fluorine contained polv(aryl ether sulfone) matrix(PAES-F) was synthesized. Then the composite membranes were prepared via TiO2 nanopartides and PAES-F polymer matrix by solution blending and non-solvent induced phase inversion methods. Further, separation efficiency, fouling behavior and self-cleaning property of the composite ultrafiltration(UF) membranes were investigated by dead-end filtration experiments using a polyacn lamide solution. The composite UF membranes exhibited outstanding self-cleaning efficiency and anti-photocatalytic degraded property after exposure to simulated sunliglit irradiation.The water flux recovery ratios(FRR)of the optimal composite UF membranes could reach 74.24%, which was attributable to photocatalytic degradation of the organic contaminant by TiO2. And the retention rates of the composite UF membranes could maintain over 97%, which indicated the excellent photocatalytic degradation resistance of the fluorine contained PAES-F matrix. The novel high perfomiance composite UF membranes have a broad application prospect in water treatment.     

不同助剂对CuO-ZnO/SBA-15催化CO_2加氢制甲醇性能影响的研究

以硅质骨架结构介孔分子筛SBA-15为载体,采用浸渍法合成CuO-ZnO/SBA-15(CZ/SBA-15)、CuO-ZnO-MnO_2/SBA-15(CZM/SBA-15)、CuO-ZnO-ZrO_2/SBA-15(CZZ/SBA-15)三组多孔催化剂,在固定床反应器上评价了各组催化剂催化CO_2加氢合成甲醇的性能,同时结合N_2吸附-脱附(BET)、X射线衍射(XRD)、H_2程序升温还原(H_2-TPR)、程序升温脱附(H_2-TPD、CO_2-TPD)、N_2O滴定、X射线光电子能谱(XPS)、透射电子显微镜(TEM)等表征研究了不同助剂对CO_2催化加氢制甲醇的影响。结果表明,催化剂中的金属氧化物改变了SBA-15分子筛载体的孔径大小和比表面积;催化剂CuO-ZnO-MnO_2/SBA-15、CuO-Zn O-ZrO_2/SBA-15中铜的分散度(D_(Cu))和比表面积(A_(Cu))更大,表面CuO粒径更小,更易被还原;相比Mn-O簇,Zr-O簇为增强了碱性位点,提高了甲醇选择性。此外,CuO-ZnO-ZrO_2/SBA-15具有更高的氧空位浓度,催化活性更好,其甲醇选择性为25.02%,与CuO-ZnO/SBA-15、CuO-ZnO-Mn O_2/SBA-15相比分别提高了28%和136.9%,催化效果最好。     

烤鳗中6种农药残留量的液相色谱-质谱/质谱法同时测定

建立了烤鳗中苯胺灵、嘧菌酯、氨苯乙酯、氟酮唑草、丙蝇驱、唑螨酯6种农药残留的同时检测方法.烤鳗样品采用乙腈、中性氧化铝超声基体分散吸附、涡旋混合提取,Florisil固相萃取小柱净化、浓缩,以乙腈-乙酸铵缓冲液为流动相进行色谱分离,串联质谱检测.结果表明,6种化合物在0.5 ～1 000 μg/L范围内线性关系良好,方法的检出限为0.03 ～2.3 μg/kg,定量下限为0.09 ～7.7 μg/kg,平均加标回收率为75% ～104%,相对标准偏差(RSD)为1.6% ～15%,满足当前进出口残留控制要求.     

2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺的合成及其与铑(Ⅲ)的高灵敏显色反应的研究

合成了新显色剂2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺(5-I-PADMA),并研究了其与铑(Ⅲ)的显色反应。结果表明,在pH4.0~6.2的乙酸-乙酸钠缓冲介质中,铑(Ⅲ)与5-I-PADMA可形成稳定的1∶2配合物,该配合物呈现2个吸收峰,分别位于557、597 nm处。配合物形成后,以适量HClO4(0.24~5.57 mol.L-1)酸化,可转变为另一种具有较高吸收特性的质子化形体,其吸收峰分别红移至564、613 nm处。表观摩尔吸光系数达ε613=1.86×105L.mol-1.cm-1,铑的质量浓度在0~0.56 mg.L-1范围内符合比尔定律。该法是目前测定痕量铑的高灵敏显色体系之一,且具有良好的选择性。所建立的方法操作简单,应用于催化剂中微量铑的测定,结果满意。