Exchange reactions of copper complexes with amines

Square planar mixed ligand complexes of the type [CuLL′] where L = 5-chlorosalicylaldehyde and L′ = acetoacetanilide, have been synthesized on treatment with ammonia. Amine exchange of the above Schiff base complexes has been carried out on treatment with different amines. The reaction with ethanol amine is quite interesting compared to other amines. It reacts with 5-chlorosalicylaldehyde to form a Schiff base, while the β-diketone part is removed in the complex formation. All the complexes were characterized by elemental analysis, spectral studies, magnetic measurement, TLC, and conductane.     

综合性化学实验的线上线下混合式教学——以水泥分析为例

水泥熟料分析是一个经典的综合性实验,涉及重量分析和配位滴定分析的很多原理及操作。为了有效开展实验教学、缩短课堂讲解时间、客观评价学生实验数据及结果,我们开展了线上线下混合式教学,引导学生课前自主学习,训练学生综合和创新实验技能。这一改革提高了实验教学质量,取得了较好的教学效果。     

Anaerobic biological treatment of dye bearing water in anaerobic sequencing batch reactor: Performance and kinetics studies

Textile and dye industries are main sources of dye bearing effluent. In present studies the anaerobic biological degradation of Acid Red 3BN dye water (AR3BNDW) and mixed dye water (MDW) for reduction of color and COD were studied in sequential batch reactor (SBR). The sludge as sources of microorganism was arranged from maize processing bio methanation wastewater treatment plant, which was acclimatized for treatment of AR3BNDW and MDW. After the acclimatization, dyes degradation were studied in SBR At optimum operation condition of hydraulics retention time (HRT) = 2.5 d, and treatment time (t_R) = 16 h, AR3BNDW have gone maximum 87% color reduction of 500 mg/L dye, and 82.8% COD reduction of 380 mg/L COD. At same operating condition, 84.5% color reduction of 500 mg/L dye, and 79.42% COD reduction of 413 mg/L COD achieved for MDW. The second order Grau model was fitted well for COD and dye reductions. The kinetics parameter were evaluated for both the dye water.     

Covariate model-based fault tree analysis for risk assessment in chemical process industries: A case study of a chlorine manufacturing facility

Fault tree analysis (FTA) is a promising quantitative technique for risk analysis in chemical process industries (CPIs). In FTA, a certain sequence of basic events (causes) leads to one specific Top event (critical event of interest). However, the conventional fault tree analysis has the limitations of staticity and uncertainty. The staticity in conventional FTA arises due to its inability to accommodate time-dependent characteristics of the process system. Whereas uncertainty primarily lies in the failure probability data of basic events. This paper proposes an innovative methodology that uses a time-dependent covariate model to update the failure probability values of major contributing basic events in FTA. A novel subclass of the family of phase-type distributions is used to model the covariates corresponding to the basic events. The newly developed methodology is applied for a case study in a chlorine manufacturing facility to estimate the chlorine release probability. The blockage in the pipeline was identified as the significant reason for chlorine release from expert opinion and sensitivity analysis. The results of the proposed model of FTA are compared with that of conventional FTA.     

基于混酸回流制备碳点的中和过程

Carbon dots (C dots) are relatively novel carbon nanomaterials that have attracted significant interest due to their unique photoluminescence, good biocompatibility, and stability. The preparation methods of C dots was usually summarized into "top-down" and "bottom-up", and mixed acid reflux is a top-down strategy that can be used to synthesize C dots, during which neutralization is a necessary step that can significantly influence the properties and potential applications of the final product. Previously, this research area mainly focused on tuning the properties of C dots by changing the starting materials and/or varying the reaction conditions; the influence of the reagents used during neutralization has been largely ignored. As the previously reported C dots prepared by mixed acid reflux were obtained from different starting materials under varied conditions, a meaningful comparison is difficult. Herein, yellow-emitting C dots were prepared by mixed acid-refluxing a carbon-rich material derived from fullerene carbon soot. For the same batch of as-prepared C dots, the influences of four reagents, i.e., NaOH, Na₂CO₃, K₂CO₃, and NH₃·H₂O, during neutralization on the structures and photoluminescence of the resulting C dots were investigated in detail. The results of thermogravimetric analysis, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy clearly showed that the reagent used during neutralization can affect the degree of dissociation of the acidic functional groups on the C dots. This is further supported by examination of the C dot/surfactant mixtures where subtle changes in the phase behavior were observed. Structural changes of the C dots cause variations in their surface states, ultimately altering the optical characteristics, including UV-vis absorption and fluorescence. Among the treated C dots, the sample prepared with Na₂CO₃ showed the strongest emission under the same excitation wavelength, while that prepared with NH₃·H₂O exhibited a distinct red shift (~8 nm) in the emission curve. The results presented herein provide clear evidence that neutralization reagent selection is important for optimizing the properties of the resulting C dots obtained by mixed acid reflux. In addition, the photoluminescence of the C dots can be influenced by their counterions, providing a novel method for tuning the properties of C dots while explaining their behavior in saline solutions. In short, the basicity of the neutralizing reagent and the type of counterions affect the structure of the C dots surface, which brings different performances. This work reminds researchers that it is necessary to use the type of neutralizing reagent as an experimental condition when preparing C dots in the future.     

Magnetic solid‐phase extraction of angiotensin II receptor antagonists in human urine and plasma with a reversed‐phase/cation‐exchange mixed‐mode sorbent

Biocompatible magnetic nanoparticles that featured divinylbenzene and sulfonate functionalities were used for the magnetic solid‐phase extraction of five angiotensin II receptor antagonists from human urine and plasma samples based on a reversed‐phase and cation‐exchange mixed‐mode mechanism. Under the optimized extraction conditions, coupled to high‐performance liquid chromatography with fluorescence detection, this proposed method was found to be accurate and precise with relative standard deviations of less than 11.7%, and a good recovery of 80.1–119.5% for both samples. The linear ranges were 0.2–2000 and 0.2–2500 ng/mL along with correlation coefficients above 0.9923 and 0.9928 for urine and plasma samples, respectively. Limits of detection were 0.01–5.74 and 0.01–1.31 ng/mL, respectively. The proposed magnetic solid‐phase extraction based on the magnetic nanoparticles functionalized with divinylbenzene and sulfonate was a reliable and convenient sample pretreatment method and had the potential for isolating and enriching the angiotensin II receptor antagonists in biological samples.     

Two unprecedented inorganic-organic boxlike and chainlike hybrids based on arsenic-vanadium clusters linked by nickel complexes

Two novel organic-inorganic hybrid arsenic-vanadates, [{Ni(en)₂}₄(4,4′-bipy)₄{Ni(H₂O)₂}]₂[As₈V₁₄O₄₂(NO₃)]₄·16H₂O 1 and [Ni(en)₂(H₂O)₂]₂[{Ni(en)₂(H₂O)}₂As₈V₁₄O₄₂(NO₃)][{Ni(en)₂}As₈V₁₄O₄₂(NO₃)]·6H₂O 2 are reported in this study. Crystal data for compound 1: Tetragonal, I4/m, a=27.507(4) Å, b=27.507(4) Å, c=22.101(4) Å; V=16722(5) Å³, Z=2, R(final)=0.0508. Crystal data for compound 2: Triclinic, P-1, a=11.530(2) Å, b=14.883(3) Å, c=21.330(4) Å, α=76.94(3)°, β=76.58(3)°, γ=69.54(3)°, V=3293.4(1) Å³, Z=1, R(final)=0.0559. The boxlike structure of compound 1 is designed from [{Ni(en)₂}₄(4,4′-bipy)₄{Ni(H₂O)₂}] sheets pillared by [α-As₈V₁₄O₄₂] clusters, which represents the first mixed-organic ligand-decorated tetrameric As-V-O cluster. Compound 2 is constructed from the rarely [β-As₈V₁₄O₄₂] clusters and Ni coordination complex fragments. The electrochemical property and magnetic property of compound 1 have been studied.     

C12-2-En-C12•2Br与SDS混合水溶液的胶团化研究

与[C12H25N＋(CH3)2CH2]2•2Br－(简记为C12-2-C12•2Br)/ C12H25SO4Na(SDS)混合水溶液相比,随着联接链上乙氧基团(E)数目增加,[C12H25N＋(CH3)2]2C2H4(OC2H4)n•2Br－(简记为C12-2-En-C12•2Br, n=2,3)与SDS混合水溶液澄清区域明显增大. C12-2-E3-C12•2Br/SDS混合胶团化过程中二组分产生了协同效应,理论预测在澄清区域所能达到的最小临界胶团总浓度(cmcT,min)= 0.0339 mmol•L－1,对应的SDS在溶液体相中的摩尔分数(x2*)=0.447.当水溶液体相中SDS摩尔分数(x2)=0.5时,混合胶团总聚集数(NT)=36,混合胶团中SDS的摩尔分数(x2M)=0.43.     

离子液体[BMim]BF4对SDS水溶液表面活性和聚集能力的促进

采用表面张力测定法和核磁共振谱等方法研究了阴离子表面活性剂十二烷基硫酸钠(SDS)在水溶性室温离子液体[BMim]BF4/水混合溶剂中的表面性质及聚集行为, 发现极少量[BMim]BF4的介入就可以显著降低SDS的临界胶束浓度, 提高体系的表面活性; 且[BMim]BF4在混合溶剂中所占的摩尔分数(x1)在一定范围内(0相似文献   

A Novel Hybrid Solid Constructed from Tetramolybdate and Copper Complexes with Mixed Ligands: [{(Cu·phen)2(tp)}{(Cu·phen·H2O)2(tp)}{Mo4O14}]

A novel copper molybdate with mixed ligands, [{(Cu·phen)2(tp)}{(Cu·phen·H2O)2(tp)}{Mo4O14}] (phen=1,10-phenanthroline, tp=terephthalate) 1, has been hydrothermally synthesized and structurally characterized. The crystal belongs to monoclinic system, space group P21/c with a=13.1711(7), b=19.6132(10), c=13.6910(7) (A), β=117.6870(10)°, V=3131.8(3)(A)3, Z=2, C64H44Cu4Mo4N8O24, Mr=1946.99, Dc=2.065 g/cm3, F(000)=1920, μ(MoKα) (A) 2.198 mm-1, R=0.0810 and wR=0.2012 for 4233 observed reflections (Ⅰ ＞ 2σ(Ⅰ)). The structural analysis indicates that the title compound contains a discrete tetramolybdate cluster decorated with copper complex fragments and tp ligands bridging the clusters into a wave-like layer. The hydrogen bonding between adjacent layers further extends the compound into a 3-D framework.