水浴振荡碱消解-火焰原子吸收法测定土壤中六价铬

建立了水浴振荡碱消解-火焰原子吸收法测定土壤中的六价铬的方法。称取经风干、研磨并过0.15 mm孔径筛的土壤样品2.0 g(精确至0.01 g)置于150 mL锥形瓶中,加入25.0 mL碱性提取溶液,再加入400 mg氯化镁和0.5 mL磷酸氢二钾-磷酸二氢钾缓冲溶液,用聚乙稀薄膜封口,置于水浴恒温振荡器中。常温振荡样品5 min后,开启加热装置,加热水浴振荡至90～95℃,保持90 min。取下,冷却至室温。过滤,用硝酸调节溶液pH至7.5±0.5,将此溶液定容至50 mL容量瓶中,摇匀,待测。该方法采用水浴振荡碱消解的前处理方式进行土壤中六价铬的全消解,代替了磁力搅拌加热方式的消解,优化了前处理条件,简化了试验步骤,节约了分析测试时间,提高了分析效率,此方法还有利于处理大批量土壤样品。探讨了样品前处理提取温度的优化选择、氯化镁加入量的研究优化、提取时间的优化选择、pH值的优化以及三价铬干扰试验的影响。确认了最优化的仪器条件,对六价铬做了线性范围测试,曲线相关系数均在0.999以上。依据HJ 168—2020方法做了检出限,六价铬的检出限为0.5 mg/kg,以4倍检出限做测定下限,则测定下限为2.0 mg/kg。(取样量为2.0 g,定容体积为50 mL)。选取GBW(E)07251—255系列标准物质进行测试试验,试验结果的精密度和准确度均可满足土壤环境监测技术规范的要求。     

饱和块状混合回填土地基的一维固结分析

用块状渣土置换软弱地基和回填低洼谷地等是处置工程渣土的有效途径。为了分析饱和块状混合回填土地基的固结性状，运用混合物理论建立了其一维固结模型。首先，假定块状土固相和充填土固相之间满足等应变条件，获得了饱和块状混合回填土中各相应变与块状土孔隙变形和充填土孔隙变形的关系式。其次，在小应变条件下，根据自由能势函数方程建立了饱和块状混合回填土的一维线弹性本构方程，再结合达西定律和应力平衡方程获得了一维固结控制方程。再次，利用分离变量法得到一维固结解析解，通过退化本文模型与已有模型进行对比，验证了本文模型的正确性。最后，基于所得解析解，分析了充填土孔隙渗透系数、块状土孔隙渗透系数以及流体交换参数等因素对饱和块状混合回填土地基固结性状的影响。分析结果表明：充填土孔隙渗透系数对饱和块状混合回填土地基整体固结性状起主导作用；在固结初期，块状土超孔压会有一定程度的上升，且3个参数具有相似的作用机理。     

The influence of FeNi nanoparticles on the microstructures and soft magnetic properties of FeSi soft magnetic composites

In this work, a new type of FeSi/FeNi soft magnetic powder core (SMPC) was successfully fabricated by coating FeNi nanoparticles on the surface of FeSi micrometer powder. The effects of different contents of FeNi nanoparticles on the micromorphology, internal structures, and soft magnetic properties of SMPCs were studied. The results show that FeNi nanoparticles adhere to the surface of FeSi powder, which can effectively fill the air gap between FeSi powder and is beneficial to the compaction of the powder cores during the pressing process. Thus, the density of the SMPCs is increased. Compared to FeSi SMPCs, the comprehensive soft magnetic properties of FeSi/FeNi SMPCs have been greatly improved. When adding 15 wt% FeNi nanoparticles, the SMPCs exhibit excellent magnetic properties with high effective permeability (increased by 43.8 %) and low core loss (decreased by 22.1 %). The high performance FeSi/FeNi SMPCs prepared in this work are expected to be widely used in power choke coils, uninterruptible power supplies, and boosts and inverter inductors.     

Synthesis of Hollow Three-Dimensional Channels LiNi_(0.5)Mn_(1.5)O_4 Microsphere by PEO Soft Template Assisted with Solvothermal Method

A appropriate size with three-dimension(3 D) channels for lithium diffusion plays an important role in constructing highperforming LiNi_(0.5)Mn_(1.5)O_4(LNMO) cathode materials, as it can not only reduce the transport path of lithium ions and electrons, but also reduce the side effects and withstand the structural strain in the process of repetitive Li~+ intercalation/deintercalation. In this work, an e fficient method for designing the hollow LNMO microsphere with 3 D channels structure by using polyethylene oxide(PEO) as soft template agent assisted solvothermal method is proposed. Experimental results indicate that PEO can make the reagents mingle evenly and nucleate slowly in the solvothermal process, thus obtaining a homogeneous distribution of carbonate precursors. In the final LNMO products, the hollow 3 D channels structure obtained by the decomposition of PEO and carbonate precursor in the calcination can provide abundant electroactive zones and electron/ion transport paths during the charge/discharge process, which benefits to improve the cycling performance and rate capability. The LNMO prepared by adding 1 g PEO possesses the most outstanding electrochemical performance, which presented an excellent discharge capacity of 143.1 mAh g~(-1) at 0.1 C and with a capacity retention of 92.2% after 100 cycles at 1 C. The superior performance attributed to the 3 D channels structure of hollow microspheres, which provide uninterrupted conductive systems and therefore achieve the stable transfer for electron/ion.     

Electric field-assisted synthesis/sintering cerium oxide: 5 wt.% gadolinium oxide

Gadolinium oxide ceramic powders were mixed to cerium oxide ceramic powders, pressed to pellets, and sintered either at 1450 °C or applying 200 V cm⁻¹ electric field at 800 °C, 900 °C and 1000 °C. The structural phases and the microstructure of the sintered pellets were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The formation of substitutional solid solution was followed by monitoring the increase of the electrical conductivity by impedance spectroscopy and X-ray diffraction. The main results show that Joule heating due to the flow through the pellets of the electric current, which was produced by the application of the electric field, allows for promoting partial solid solution as well as partial sintering the ceria-gadolinia pellets. Moreover, grain growth that occurred in the high temperature sintered pellets was inhibited in the electric field-assisted synthesized/sintered pellets, being an alternative technique for producing cerium oxide-gadolinium oxide solid solutions.     

Effect of sintering temperature on lightweight aggregates manufacturing from copper contaminated soil

Manufacturing lightweight aggregate (LWA) at high temperature is an effective way to immobilize heavy metals in solid waste. This work investigated the performance and solidification mechanism of LWA prepared from copper contaminated soil. The volume expansion of LWA could reach a maximum of 28%, and its lowest density accounted of 1.5 g/cm³, which met the standard requirements. Optical microscope and micro-CT test illustrated that the addition of Cu leaded to obvious phase separation in LWA. The Cu leaching result of LWA first increased and then dropped with the temperature. The XRD test found that the main formation phase of Cu in LWA were t-CuFe₂O₄ and amorphous phase that they had different acid resistance ability. XPS revealed that the main cause of the agglomeration of liquid phase in LWA was the chain broken reaction between Cu and Si–O tetrahedron. SEM-EDS results showed that the distribution of Cu and Si had a strong correlation, which meant that Cu mostly formed amorphous phase. This work showed the uniqueness of Cu in the high temperature immobilization and pointed out the best immobilization target phase.     

木质纤维与水泥共同改良软土的力学性能与微观机制分析

通过压实试验、无侧限抗压强度试验和劈裂试验,分析不同木质纤维含量、水泥含量和固化时间对软土力学性能的影响规律,探讨木质纤维、水泥改良软土的微观机制。结果表明,木质纤维的加入对水泥改良软土的击实特性有显著的影响;木质纤维与水泥可有效改善土体的抗压和劈裂抗拉强度,随着木质纤维含量的增加,改良土的抗压和劈裂抗拉强度呈现出明显的“驼峰”现象,并在木质纤维含量为0.25%时最大;木质纤维与水化产物、软土颗粒形成互锁效应,增大了改良土的摩擦力,同时木质纤维还承担一定的拉伸强度,使改良土的劈裂强度增加。     

不同消解方法对土壤中铜锌测定的影响

采用微波消解法和石墨消解法对土壤样品进行预处理,用火焰原子吸收分光光度法测定土壤中铜和锌的含量。对3个土壤标准物质(GSS-17、GSS-30、GSS-34)的精密度和准确度进行了分析,结果表明:微波消解法和石墨消解法的检出限、精密度和准确度均能满足土壤检测的要求,石墨消解法相对于微波消解法更加便捷,具有很好的精密度和准确度。