Substitution of toxicologically critical solvents in the residue analysis of acetamiprid: Towards green chemistry

The article presents the reduced use of toxicologically critical solvents for the extraction and clean-up of a neo-nicotinoid pesticide, acetamiprid from vegetables. Acetamiprid was extracted from spiked vegetable samples of cabbage by the use of different techniques like microwave-assisted extraction (MWAE), sonication and by the conventional method of homogenization. The study revealed that though higher percent recoveries of 78–92 were obtained in the blending method, solvent use was high as compared to MWAE. In MWAE, the percent recoveries recorded were in the range of 46–89 depending upon the solvent used and power employed. A mixture of methanol–water and methanol–acetone at 400 W power levels gave percent recoveries of 72 and 82, respectively, as compared to solvent mixtures, namely, acetone–hexane and acetone–hexane–water, which recorded recoveries of 49 and 67%. The study indicates that the choice of solvent and power employed plays a significant role in MWAE for enhanced recoveries.     

CuO/zeolite catalyzed oxidation of gaseous toluene under microwave heating

The development of a combined process of catalytic oxidation and microwave heating for treatment of toluene waste gas was described in this work. Toluene, a typical toxic volatile organic compound, was oxidized through a fixed bed reaction chamber containing zeolite-supported copper oxide (CuO/zeolite) catalyst mixed with silicon carbide (SiC), an excellent microwave-absorbing material. The target compound was efficiently degraded on the surface of the catalyst at high reaction temperature achieved by microwave-heated SiC. A set of experimental parameters, such as microwave power, air flow and the loading size of CuO etc., were investigated, respectively. The study demonstrated these parameters had critical impact on toluene degradation. Under optimal condition, 92% toluene was removed by this combined process, corresponding to an 80%–90% TOC removal rate. Furthermore, the catalyst was highly stable even after eight consecutive 6-h runs. At last, a hypothetical degradation pathway of toluene was proposed based on the experimental data obtained from gas chromatography-mass spectrum and Fourier transform infrared spectroscopy analyses.     

微波Sol-Gel制备TiO2的研究及其对活性艳红X-3B的降解

采用微波Sol-Gel法在石英表面制备了负载型TiO2光催化剂,通过紫外吸收光谱和X衍射分析表征了TiO2溶胶的变化过程及锐钛型TiO2的生成。以活性艳红X-3B为模拟污染物进行光催化降解,探讨了微波功率、反应温度和反应时间对微波Sol-Gel法制备TiO2光催化活性的影响。由因素试验确定了最佳工艺条件:微波功率400W,反应温度90℃,反应时间2min。在此条件下制备的TiO2催化剂对活性艳红X-3B溶液进行光催化降解,反应30 min的脱色率达93%,TOC去除率为55%。采用中空纤维膜三相液相微萃取-毛细管电泳(HF-LLLME-CE)联用技术对降解生成的小分子有机物进行了测定。     

固相萃取—微波衍生化—GC-MS法同时测定水中6种雌激素物质

建立了固相萃取—微波衍生化—气相色谱-质谱联用法快速同时测定水中雌酮（E1）、17α-雌二醇（α-E2）、17β-雌二醇（β-E2）、雌三醇（E3）、17α-乙炔基雌二醇（EE2）、双酚A（BPA）等6种雌激素物质的分析方法,对色谱柱升温程序、固相萃取及衍生化条件进行了优化。色谱柱最佳升温程序为：初始温度50 ℃,保持2 min;以20 ℃/min速率升至260 ℃,保持5 min;最后以10 ℃/min速率升至280 ℃,保持5 min。实验结果表明,在选取 HC-C18萃取小柱、添加双（三甲基硅烷基）三氟乙酰胺（BSTFA）+1%三甲基氯硅烷（TMCS）+吡啶作为衍生化试剂、微波315 W衍生化加热4 min的条件下,6种目标物标准曲线的相关系数均大于0.999,BPA、E1、EE2及E3的线性范围为3~300 ng/L,17α-E2及17β-E2的线性范围为5~300 ng/L,方法检出限为2.0~5.0 ng/L,加标回收率为76.45%~96.24%。     

不同微波条件对活性炭微波再生效率的影响研究

研究了吸附药厂废水COD的粉末活性炭在不同微波条件下的微波再生。以碘吸附值为指标,通过单因素实验考查了微波功率、微波辐照时间对粉末活性炭性能恢复率、再生损耗率、综合恢复率的影响,结合实验拟合曲线特点,分析了呈现的规律和原因。实验结果表明,在微波功率为648W、辐照时间为180s时活性炭性能恢复率达到最大,为99.73%;在功率为464W、时间为180s时综合恢复率最佳,为96.81%。     

The Effect of Starch Composition on Structure of Foams Prepared by Microwave Treatment

A microwave technique was used to prepare foams from different potato starches in granular form, with varying amounts of amylose content, and water. In addition to native potato starch (PN), high amylose potato starch (HAP) and potato amylopectin (PAP) were used, as well as mixtures thereof. In all cases the native crystallinity of starch granules was lost upon microwave treatment and an amorphous material was created. An increased concentration of starch in the initial water dispersion resulted in a less dense foam structure. The potato amylopectin formed open cell foams, whereas increased amylose content, as in native potato starch, yielded a more compact structure with irregular pore shapes. The high amylose potato starch yielded a structure with hardly any porosity. Foaming experiments were done to compare pre-gelatinized and granular starches dispersed in water. The pre-gelatinisation did not affect the pore formation process. These experiments indicated that the molecular architecture of starch polymers is more important for foam formation than starch polymer organization in the granules. Studies of temperature profile and dry matter content during microwave treatment showed that water evaporates more rapidly from a high amylose starch solution than native potato starch and potato amylopectin solutions. Rheological measurements showed that the amylose solution had much lower viscosity than starch and amylopectin. This confirms that polymer – water interaction, such as in amylopectin solution, favours stabilization of bubbles formed upon boiling and evaporation of water, which yields high porosity materials.     

高铁酸钾-微波耦合对印染污泥脱水性能的影响研究

分别采用微波、微波耦合高铁酸钾对印染污泥进行脱水预处理.结果表明,适宜的微波辐射可改善污泥脱水性能.2320、3240、4000 W·L-1对应的最适时间分别是140 s、100 s和80 s.在3240 W·L-1的微波下辐射100 s后,污泥的沉降速率(SV30)、污泥比阻(SRF)和粘度较原污泥分别减少4.00%、18.89%、35.05%.同时,高铁酸钾的加入能更好地提高污泥脱水性能,其最佳投加量为0.1767 g·g-1(以SS计,下同),对应的污泥SV30、毛细吸水时间(CST)、粘度相比原污泥分别降低了13.50%、51.18%、40.79%.泥饼含固率相比原污泥则增加14.58%.微波耦合高铁酸钾能有效破坏污泥絮体结构.随着高铁酸钾投量增加,上清液的蛋白质含量持续增加,多糖含量则先增加后减少.     

微波解吸-催化燃烧净化甲苯研究

以甲苯为目标污染物,采用活性炭做吸附剂对含甲苯废气进行吸附;吸附完成后利用微波辐照进行解吸;另外采用浸渍法制备Cu-Mn复合氧化物催化剂并对微波解吸后的废气进行催化燃烧处理从而达到对污染物进行彻底净化的目的.实验中甲苯的浓度由气相色谱(GC)测定.结果表明,采用微波解吸后,在以氮气为载气的解吸气体中加入空气来提供氧气从而实现催化燃烧是可行的,解吸气与空气配比为1∶1(体积比)时效果最好,此时对应的催化空速为2.67 s-1.解吸温度会影响解吸气体中的甲苯浓度进而影响催化燃烧效率,实验结果表明400℃解吸比较理想.当催化燃烧温度保持在300℃时,系统对甲苯的最终净化效率可以维持在90%以上,其中大部分时间是在95%以上.     

活性炭微波再生方法研究

以亚甲基兰为污染物污染活性炭滤芯,利用微波辐照的方法对失效的活性炭滤芯进行再生,通过实验分别测出新的、失效的活性炭滤芯的碘值,通过碘值计算出活性炭的性能恢复率、损耗率、综合恢复率等性能指标,并分析影响上述性能指标的单一因素：辐照功率、时间和活性炭用量。设计正交试验,找到微波再生活性炭滤芯的最佳再生条件：微波功率600W,辐照时间90s,辐照活性炭质量2g。经过再生的活性炭的综合恢复率达到94．30％。     

Treatment of simulated wastewater containing Reactive Red 195 by zero-valent iron/activated carbon combined with microwave discharge electrodeless lamp/sodium hypochlorite

A comparative study of treatment of simulated wastewater containing Reactive Red 195 using zero-valent iron/activated carbon (ZVI/AC), microwave discharge electrodeless lamp/sodium hypochlorite (MDEL/NaClO) and the combination of ZVI/ACMDEL/ NaClO was conducted. The preliminary results showed the two steps method of ZVI/AC-MDEL/NaClO had much higher degradation e ciency than both single steps. The final color removal percentage was nearly up to 100% and the chemical oxygen demand reduction percentage was up to approximately 82%. The e ects of operational parameters, including initial pH value of simulated wastewater, ZVI/AC ratio and particle size of ZVI were also investigated. In addition, from the discussion of synergistic e ect between ZVI/AC and MEDL/NaClO, we found that in the ZVI/AC-MEDL/NaClO process, ZVI/AC could break the azo bond firstly and then MEDL/NaClO degraded the aromatic amine products e ectively. Reversing the order would reduce the degradation e ciency.