几种常见阴离子的高效毛细管电泳-电导分离检测

采用柠檬酸-柠檬酸钠作为缓冲体系,使用负高压,对Cl-、NO3-、HCO3-、H2PO4-几种常见阴离子进行了分离检测,研究了缓冲剂的种类、浓度、pH值及操作电压对分离的影响;在选定的条件下,定量线性范围为Cl-5.0×10-5～2.5×103md/L,NO3-6.0×10-5～2.0×10-3mol/L,HCO3-1.0×10-5～2.0×10-3mol/L,H2PO4-6.0×10-5～1.0×10-3mol/L;检出限为Cl-1.5×10-5mol/L,NO3-3.0×10-5mol/L,HCO3-1.0×10mol/L,H2PO4-2.0×10-5mol/L;4种离子的RSD(n=6)分别为3.1%、33%、2.6%和2.9%;应用选定条件对自来水样品进行了分析,结果令人满意.     

石墨炉原子吸收法测定水系中的铍

用石墨炉原子吸收法测定水系中的铍,以Mg(NO3)2为基体改进剂,提高了测定铍的灵敏度,增强了测定铍的抗干扰能力。方法的线性范围为0－1．0μg/L,检出限为0．05μg/L。用于水库水、黄河水、饮用水和地下水等水中铍的测定,回收率为95％－110％。     

双电极法现场快速检测地下水和湖水中碳酸氢根和碳酸根

地下水和湖水中碳酸氢根( HCO-3)和碳酸根( CO2-3)含量是地球化学碳行为和碳循环的重要表征,但两种离子的浓度易受环境影响而改变,因此,地下水和湖水中HCO-3和CO2-3真实含量的测定一直是个难题。实验利用CO2的水解平衡,通过pH电极和二氧化碳电极联用,建立了HCO-3和CO2-3现场快速测定的新方法,解决了地下水和湖水中HCO-3和CO2-3真实含量的测定难题。研究结果表明,在pH=4.8±0.1的底液中, HCO-3和CO2-3的线性范围分别为0.027~570 mg/L和1.25×10-8~39.7 mg/L。共存的金属离子、强酸阴离子(K+、Na+、Mg2+、Cl-、SO2-4,100 mg/L)、弱酸阴离子和弱酸(HSO-3、NO-2、HOAc,50 mg/L)对测定干扰小于5%。实际水样加标实验回收率在95.2%~99.2%之间,相对标准偏差为2.6%~3.7%。与酸碱滴定法进行对比,本方法的准确性良好。但方法受温度影响,因此标准溶液与样品应在同一温度下测量。总体而言,双电极法灵敏、快速、经济且电极携带方便、操作简单、对环境要求不高,十分适合现场和室内一般自然水体的快速检测。本方法已成功应用于青海省地下水和青海湖湖水中HCO-3和CO2-3的现场测定。实验表明,海东地区地下水样品pH在6.4~7.4之间,HCO-3含量为234~4096 mg/L,CO2-3含量为0.16~1.89 mg/L;青海湖湖水样品pH≈8.7,HCO-3含量范围在1.36~1.86 g/L,CO2-3含量在32.3~43.9 mg/L,与文献结果吻合。     

Ultrathin Co3S4 Nanosheets that Synergistically Engineer Spin States and Exposed Polyhedra that Promote Water Oxidation under Neutral Conditions

Development of efficient and affordable electrocatalysts in neutral solutions is paramount importance for the renewable energy. Herein, we report that the oxygen evolution reaction (OER) performance of Co₃S₄ under neutral conditions can be enhanced by exposed octahedral planes and self‐adapted spin states in atomically thin nanosheets. A HAADF image clearly confirmed that the active octahedra with Jahn–Teller distortions were exposed exclusively. Most importantly, in the atomically thin nanosheets, the spin states of Co³⁺ in the octahedral self‐adapt from low‐spin to high‐spin states. As a result, the synergistic effect endow the Co₃S₄ nanosheets with superior OER performance, with exceptional low onset overpotentials of circa 0.31 V in neutral solutions, which is state‐of‐the‐art among inorganic non‐noble metal compounds.     

杂多酸催化H2O/THF或乙醚中三组分一锅煮合成α-胺基膦酸酯

发现杂多酸是在水/四氢呋喃或乙醚中三组分一锅煮高产率合成α-胺基膦酸酯的有效催化剂.研究了催化剂用量、反应溶剂、醛和胺的结构对反应的影响.     

水蒸气超高温热泵系统的实验研究

近年来以低温室效应(GWP)的制冷剂的蒸汽压缩式高温热泵一直是余热回收领域的研究热点.为获得更高的输出温度,本课题组搭建了一台采用自然工质水作为循环冷媒的超高温热泵样机并进行了实验测试.实验结果表明蒸发温度为80℃,冷凝温度从115℃升至145℃时,热泵的COP从4.88降至1.89.在85℃蒸发,117℃冷凝时,最高...     

Synthesis,Structure and Photoluminescence of Co-crystal of Bis[2-(benz(oxa/imida)zol-2-yl)phenolato-κ2N,O]zinc(Ⅱ) Being Site Occupancy Disorder with a Heteroatom Ratio of NH to O (0.408/0.592)

The zinc(Ⅱ) complex with Hpbx (Hpbx = 2-(benzoxazol-2-yl)phenol) and Hpbm (Hpbm=2-(benzimidazol-2-yl)phenol),namely[Zn(pbm)2]1.633[Zn(bpx)2]2.367·DMF·2H2O1,has been synthesized and characterized by X-ray crystallography,FTIR and elemental analysis.The coordination structures are statistically disordered and can be regarded as a co-crystal of [Zn(pbm)2]and [Zn(pbx)2] with the ratio of ca.0.408/0.592.Solvate water and DMF molecules are also present in the lattice.Crystal data for 1:monoclinic,space group P21/c,Mr= 2049.02,Z = 2,α = 9,7571(6),b = 25.6415(16),c = 19.8675(10)(A),β = 111.342(2)°,V = 4629.7(5) (A)3,Dc = 1.470 g/cm3,μ =1.100 mm-1,F(000) = 2104,R = 0.0575 and wR = 0.1282 for 5528 observed reflections (I＞ 2σ(I)).The photoluminescent spectra for this compound have also been studied.     

Synthesis and Structural Characterization of a New Cadmium(Ⅱ) Complex Bridged by Endo-norbornene-cis-5,6-dicarboxylic Acid

A polynuclear complex [Cd(endc)(H2O)]n·nH2O (endc = endo-norbomene-cis5,6-dicarboxylate anion) has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbomene-cis-5,6-dicarboxylic acid in 1:1 molar ratio,and structurally characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a = 1.16471(7),b = 0.95334(7),c = 0.91109(9) nm,Z = 4,V= 1.01035(14)nm3,Dc.= 2.160 g/cm3,μ= 2.172 mm-1,F(000) = 648,R =0.0302 and wR = 0.0752.According to structural analysis,each Cd(Ⅱ) ion is coordinated to six O atoms from three endc anions and one water molecule,giving a distorted octahedral geometry.Two- dimensional layer arrangement of the title complex is constructed from the bridging nature of endc.It is worth notice that adjacent two-dimensional layers are joined together to form a three-dimensional supramolecular framework via intermolecular hydrogen bonding interactions.     

Synthesis and Crystal Structure of a Novel Manganese Coordination Polymer： 2,5-Bis（4-pyridyl）-3,4-diaza-2,4-hexadiene

A new manganese coordination polymer 1, [Mn(H2O)4(L)]n(ClO4)2n·2nH2O·3nL (L = 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene), has been synthesized and structurally characterized. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group Pn with a = 13.9176(8), b = 15.4754(9), c = 15.9670(9) , β = 99.5010(10)o, V = 3391.8(3) 3, Z = 2, C56H68Cl2MnN16O14 , Mr = 1315.10, Dc = 1.288 g/cm3, μ = 0.344 mm-1, F(000) = 1374, R = 0.0733 and wR = 0.2035. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene and four oxygen atoms from water molecules, completing an octahedral geometry. The title complex exhibits a novel supramolecular layer architecture sustained by the concurrence of coordination bonds, hydrogen bonds, and π-π stacking interactions.