Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2–4.0 µg L^?1) and low detection limits (1.1–2.9 ng L^?1). The high extraction efficiency was determined with enrichment factors ranging from 1.2–2.9 for the lowest level, 1.3–4.9 intermediate level and 1.2–3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.     

钙钛矿型催化剂催化湿式氧化处理煤气化废水纳滤浓缩液

采用溶胶-凝胶法制备了Mn掺杂钙钛矿型催化剂LaFexMn1-xO3,并以其为催化剂催化湿式双氧水氧化处理煤气化废水纳滤浓缩液。采用XRD,SEM,FTIR技术对催化剂进行了表征。表征结果显示：制备的催化剂均具有标准的钙钛矿型结构,其中,LaFe0.9Mn0.1O3的结构稳定,比表面积大。实验结果表明：制备的催化剂中LaFe0.9Mn0.1O3的催化活性最高,且稳定性好,连续使用5次后催化活性未见明显减弱;在H2O2投加量3.0 g/L、n（H2O2）∶n（LaFe0.9Mn0.1O3）=12∶1、反应温度160 ℃、反应压力1 MPa、浓缩液pH 3、反应时间60 min的最优条件下,COD、UV254和TOC的去除率分别达到80.9%、95.2%和68.0%,BOD5/COD由0.02提升至0.40,可生化性大幅提高。     

粉煤灰基层状金属氧化物对水中活性红X-3B的吸附

以粉煤灰(FA)为原料,采用共沉淀法制备了层状双金属氢氧化物(LDH)和层状金属氧化物(LMO,也称LDO),并采用XRD和BET技术进行了表征。比较了FA、LDH、LMO对活性红X-3B染料(X-3B)的吸附效果;考察了LMO吸附X-3B的影响因素,并探讨了吸附机理。XRD表征结果表明,LMO在吸附X-3B后重新恢复LDH层状结构。BET表征结果表明,LMO的比表面积大于LDH。吸附实验结果表明,3种吸附剂对X-3B吸附效果的优劣顺序为:LMOLDHFA;在初始X-3B质量浓度为50 mg/L、LMO投加量为2.0 g/L、吸附温度为25℃、吸附pH为7、吸附时间为30 min的条件下,X-3B去除率可达98.1%;LMO对X-3B的吸附符合Langmuir等温吸附方程,饱和吸附量为129.53 mg/g,且吸附过程可用准二级动力学方程描述。     

金属冶炼进口物料的固体废物鉴别方法

建立了金属冶炼进口物料的固体废物鉴别方法,并利用该方法对海关查扣的3种金属冶炼进口物料进行了固体废物鉴别。鉴别结果显示:物料1、2和3的自然属性分别为砷含量超标铜精矿、锰阳极泥、回转窑氧化锌,产生来源分别为有害物质超标的产品、污染控制设施产生的物质、有意识加工的目标产物;物料1和2属于我国禁止进口的固体废物,物料3不属于固体废物。本文建立的固体废物鉴别方法可行,可为金属冶炼进口物料的固体废物鉴别和监管提供参考。     

铁氧化物复合氧化铝催化臭氧化过程中溴酸盐的生成控制

以市售活性炭、硅藻土和氧化铝小球为载体,考察了负载铁基活性组分对催化臭氧化过程中溴酸盐的控制情况,其中,铁基复合氧化铝小球体现出更好的溴酸盐还原特性和催化剂稳定性,证实催化剂中铁氧化物是溴酸盐得到有效控制的主要活性组分。进一步考察了铁基复合氧化铝小球催化臭氧化处理实际原水过程中对溴酸盐的生成控制,以及反应过程中溶解性有机碳（DOC）的去除情况。结果表明,与单独臭氧化相比,该催化剂既能有效去除水中的溶解性有机物,又能明显抑制溴酸盐的生成,反应50h,其活性并没有明显下降。催化剂失活主要归因于吸附位点数量的下降,可以通过负载铁氧化物来实现催化剂的再生。     

模拟阳光下Ag／I-TiO2光催化预处理山核桃加工废水

研究了在模拟太阳光下,采用银修饰的碘掺杂二氧化钛光催化剂（Ag／I—TiO2）对某食品厂山核桃加工废水进行光催化预处理的效果。结合x射线衍射（XRD）、比表面积分析（BET）、紫外-可见漫反射光谱（uV—Vis）的表征结果,来分析催化剂结构对于废水处理效果的影响。探讨了Ag含量、废水初始pH（pHi）和光照时间等因素对化学需氧量（COD）去除及水质可生化性（B／C）提高的影响。并得出适宜的反应参数为：3％Ag含量;pHi为6;光照时间为240min。在最佳条件下,COD去除率45％,废水B／C比由0．17上升到0．31。光催化氧化法能够有效降低山核桃加工废水的COD含量,并达到显著提高废水可生化性的目的。     

钛基金属氧化物电极的制备及性能

采用聚合物前驱体法制备了Ti/SnO₂-Sb₂O₃电极,再通过恒电流电沉积法制备了 Ti/SnO₂-Sb₂O₃/PbO₂和Ti/SnO₂-Sb₂O₃/MnO₂电极。采用SEM技术对3种金属氧化物电极表面的形貌进行了表征,并分别以3种电极为阳极进行了苯酚的电催化氧化实验。实验结果表明：电解时间为2.5 h时,Ti/SnO₂-Sb₂O₃电极、Ti/SnO₂-Sb₂O₃/PbO₂电极和Ti/SnO₂-Sb₂O₃/MnO₂电极对苯酚的降解率分别为85.9%,83.2%,44.6%;苯酚在3种电极上的电催化氧化反应均遵循一级反应动力学方程;苯酚在Ti/SnO₂-Sb₂O₃ 电极和Ti/SnO₂-Sb₂O₃/PbO₂电极上的反应速率较快,并具有较高的析氧电位;Ti/SnO₂-Sb₂O₃/PbO₂电极具有更好的耐腐蚀性和更长的使用寿命。     

TiO2-Cu2O/蒙脱土复合光催化剂的制备与性能

以钠基蒙脱土（MMT）为载体,先采用溶胶-凝胶法将纳米TiO₂引入到MMT层间,再采用化学沉积法将纳米Cu₂O负载在TiO₂/MMT上,制备出TiO₂-Cu₂O/MMT纳米复合光催化剂。采用XRD、SEM、紫外-可见漫反射技术对催化剂进行了表征。以甲基橙为目标污染物,考察了催化剂的光催化性能。表征结果显示：TiO₂与Cu₂O均匀分布在MMT的表面与片层孔隙中;TiO₂-Cu₂O/MMT结合了TiO₂和Cu₂O的特性,拓宽了催化剂的光吸收范围。实验结果表明,在光源为可见光、初始甲基橙质量浓度为20 mg/L、光催化剂加入量为2 g/L的条件下,TiO₂-Cu₂O/MMT纳米复合光催化剂对甲基橙的光催化降解效果明显优于单一负载的Cu₂O/MMT和TiO₂/MMT,大幅提高了催化剂的光催化效率,反应300 min时TiO₂-Cu₂O/MMT对甲基橙溶液的脱色率达到93%。     

A/O工艺N_2O的产生与释放的影响因素

采用A/O工艺,在连续运行条件下,以DO、SRT和硝化液回流比(R)为影响因素,对A/O生物脱氮工艺处理模拟城市生活污水过程中N2O的释放进行了研究。实验结果表明,SRT对A/O工艺N2O释放的影响最大,其次是DO,R的影响最小。N2O转化率随着SRT的升高而降低,当SRT从10 d升高到20 d时,总N2O平均转化率从0.319%下降到0.002%。总N2O转化率随着好氧池DO的升高先降低后有所升高,当DO分别为0.6 mg O2/L、1.2 mg O2/L、2.5 mg O2/L时,反应器的总N2O平均转化率分别为0.306%、0.007%和0.013%。R对N2O释放的影响差异不明显,总N2O平均转化率在300%时最低,为0.007%。N2O释放量最低的工艺运行条件组合是SRT为20 d、DO为1.2 mg O2/L、R为300%。     

A two-generational reproductive toxicity study of zinc in rats

A two-generation reproductive toxicity study of zinc chloride (ZnCl₂) was conducted in rats. F_o male and female rats were administered 0.00 (control), 7.50 (low), 15.00 (mid) and 30.00 (high) mg/kg/day of ZnCl₂. Selected F₁ male and female rats were exposed to the same doses received by their parents (F_o). Exposure of F₀ parental rats to ZnCl₂ showed significant reduction in fertility, viability (days 0 and 4), and the body weight of F₁ pups from the high-dose group but caused no effects on litter size, weaning index, and sex ratio. Similarly, the continued exposure of F₁ parental rats to ZnCl₂ also reduced fertility, liter size, viability (day 0), and the body weight of F₂ pups within the high-dose group but caused no effects on weaning index and sex ratio. Exposure of ZnCl₂ to F₀ and F₁ parental males resulted in a significant reduction in their body weights, and the F₀ and F₁ parental females did not show any significant difference in their body weights compared to their control groups. However, the postpartum dam weights of both F₀ and F₁ female rats were significantly reduced compared to their controls. Exposure of ZnCl₂ to F_o and F₁ generation parental rats did not produce any significant change of their clinical signs as well as their clinical pathology parameters, except the alkaline phosphotase (ALK) level, which showed an upward trend in both sexes of both generations. Exposure of ZnCl₂ to F₀ rats resulted in a reduction of brain, liver, kidney, spleen and seminal vesicles weights of males and in the spleen and uterus of females. Similarly, exposure of F₁ rats to ZnCl₂ also resulted in reduction of brain, liver, kidney, adrenal, spleen, prostate and seminal vesicles weights of males and in spleen and uterus of females. ZnCl₂ exposure resulted in grossly observed gastro-intestianla (GI) tract, lymphoreticular/hematopoietic, and reproductive tract lesions in parental rats in both generations. Reduced body fat was also recorded in F₁ parental rats.