Thermal investigation of iron(III) and manganese(II,III) complexes of dianils derived from 6-formylkhellin

Manganese and iron complexes of Schiff bases derived from 6-formylkhellin were prepared and characterized. Complexes of o-phenylenediamine derivative (ligand (I)) are monomeric or dimeric whereas those of p-phenylenediamine derivative (ligand (II)) are polymeric. The complexes obtained are characterized by a lower magnetic moment values. The complexes also have different solvent of crystallization with different nature of interaction. The thermal behaviour of the ligands and their metal complexes was investigated by means of DTA, TG, IR and X-ray diffraction spectroscopy. Ligand (I) shows different thermal behaviour from that of ligands (II) and (III). The complexes of ligand (II) give abnormal oxides as a final product during their thermal decomposition. This revised version was published online in August 2006 with corrections to the Cover Date.     

Progress on phthalocyanine-conjugated Ag and Au nanoparticles: Synthesis,characterization, and photo-physicochemical properties

Phthalocyanine (Pc) complexes are an important class of dyes with numerous (e.g., biological, photophysical, and analytical) applications. Among the methods used to improve the properties of these complexes, one should mention the introduction of different substituents, variation of the central metal ion, ligand exchange, and conjugation to nanomaterials (e.g., carbon-based nanomaterials and metal nanoparticles (NPs)). This work briefly reviews Pc complex conjugation to Ag and Au NPs, highlights the different NP shapes, and discusses the diversity of conjugation approaches. Moreover, the use of UV–Vis spectroscopy, powder X-ray diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy, atomic force microscopy, dynamic light scattering and Fourier transform infrared spectroscopy to characterize Pc-NP hybrids is summarized. The effect of conjugation on Pc photo-physicochemical properties (fluorescence, singlet oxygen generation, triplet state formation, and optical limiting behavior) is discussed, and future perspectives for the synthesis and applications of new hybrids are provided.     

N,N'-二(二乙氧基硫代磷酰基)-1,4-苯二胺的合成、晶体结构及热性能研究

通过二乙氧基硫代磷酰氯与对苯二胺反应生成了标题化合物N,N'-二(二乙氧基硫代磷酰基)-1,4-苯二胺，并应用元素分析, FTIR及¹H NMR对标题化合物进行了表征. 利用X射线单晶衍射测定了其晶体结构, 同时应用TG分析法对其热性能进行了分析. 标题化合物的相对分子质量M_r＝412.42, 为正交晶系, Pbca空间群, 晶胞参数为a＝0.86936(16) nm, b＝1.2787(2) nm, c＝1.8897(3) nm, β＝90°, V＝2.1006(7) nm³, Z＝8, D_c＝1.304 g/cm³, μ(Mo Kα)＝0.425 mm^－1, F(000)＝872, S＝1.052. 最终偏离因子R＝0.0628, wR＝0.1860, 可观测衍射点1852个[I＞2σ(I)]. 该晶体通过对苯二胺连接并以中心对称分布, 并形成层状结构, 且存在弱的分子内氢键N—H…S. TG分析表明该化合物有很好的热稳定性及成炭性, 通过其阻燃聚丙烯腈表明, 该物质是一种高效能的膨胀型阻燃剂.     

染发剂中4种p-苯二胺N位取代衍生物的高效液相色谱测定法

建立了高效液相色谱(HPLC)同时测定染发剂中N,N-双(2-羟乙基)-p-苯二胺硫酸盐(DHPD)、N,N-二甲基-p-苯二胺硫酸盐(DMPD)、N,N-二乙基-p-苯二胺硫酸盐(DEPD)、N-苯基-p-苯二胺盐酸盐(PPD)4种p-苯二胺N位衍生物的方法。采用Agilent Eclipse XDB-C18柱(150 mm×4.6 mm,5μm)为固定相,25 mmol/L磷酸缓冲液(pH 6.0,含0.1%的辛烷磺酸钠)和乙腈为流动相,梯度洗脱,流速1.0 mL/min,柱温25℃,进样量20μL,检测波长250 nm和280 nm。各组分的线性范围为0.1～400 mg/L,相关系数r为0.999 2～0.999 9,检出限为18～108 mg.kg-1,定量下限为42～320 mg.kg-1,RSD<10%,加标回收率为83%～115%。该方法具有简便、快速、准确等特点,基本满足实际样品的分析要求。     

葡萄糖在聚对苯二胺/铜修饰电极上的电化学行为及测定

在静态法合成聚对苯二胺纳米片的基础上,经一步水热将铜微球均匀锚定于其上,成功合成了具有良好导电性、大比表面积、大孔径和孔容的铜/聚对苯二胺(Cu/Pp PD)复合物,其独特的结构有利于电子的转移、活性位点的充分利用以及反应物、电解质等的输运。复合物对葡萄糖氧化表现出很高的电催化活性,在最优测试条件下,所构建的葡萄糖无酶传感器响应时间短(达到稳定电流的95%所需时间小于3 s)、线性范围宽(0.003~6.44 mmol/L)、灵敏度高(929μA·mmol-1·L·cm-2)、检出限低(4.48×10-7mol/L)、重现性和选择性好,对血清样品进行检测,回收率为99.5%~101.1%。所制备Cu/Pp PD复合物能实现对葡萄糖的简单、快速、灵敏、准确无酶检测,在临床医学上糖尿病人的早期诊断和治疗监测领域具有很好的应用前景。     

大环Schiff碱化合物的合成、表征及其荧光活性研究

含乙酰丙酮类大环Schiff碱化合物一般都具有良好的荧光活性．采用模板合成法,用对苯二胺与乙酰丙酮反应合成得到的Schiff碱配体（H2L）与烷基二胺（即1,2-乙二胺,1,3-丙二胺,1,4-丁二胺）反应合成了3种新型大环Schiff碱化合物,通过元素分析,^1H NMR,IR,MS,UV,摩尔电导等手段对合成得到的化合物进行了组成和结构表征,同时在DMF溶液中对大环Schiff碱锌（Ⅱ）配合物的荧光活性进行了初步研究．     

间甲基苯胺电化学聚合以及它与对苯二胺电化学共聚的 原位紫外-可见光谱

在0.5 mol&#8226;dm－3硫酸介质中, 循环伏安法电解间甲苯胺的原位紫外可见光谱图表明聚间甲基苯胺产生在氧化铟锡导电玻璃电极表面上. 在恒电位条件下, 用原位紫外-可见光谱较详细地研究了间甲基苯胺在氧化铟锡(ITO)上的电化学聚合. 结果表明间甲基苯胺只能在较高电解电位和单体浓度足够大的条件下才能发生电化学聚合. 在0.7 V(相对于饱和的Ag/AgCl), 0.2 mol&#8226;dm－3的间甲基苯胺和0.9 V, 20 mmol&#8226;dm－3的间甲基苯的实验条件下, 尽管在ITO电极上没有发生电化学均聚合, 但原位紫外-可见光谱表明在电极表面上可能还形成低分子量的齐聚物. 在低电位0.8 V下, 电化学聚合200 mmol&#8226;dm－3间甲苯胺时, 有明显的诱导期存在. 在恒电位电解的条件下, 相应的原位紫外-可见光谱和聚合物的傅立叶变换红外光谱(FTIR)表明间甲基苯胺和对苯二胺能发生电化学共聚反应, 由于对苯二胺可能与间甲基苯胺形成了具有较强反应活性的中间体, 使得对苯二胺的加入不但促进和加速了聚合反应, 而且还结合进聚合物中形成了phenazine或类似于phenazine的环结构.     

Fabrication of Orange Fluorescent Boron-Doped Graphene Quantum Dots for Al3+ Ion Detection

Aluminum is a kind of metal that we often encounter. It can also be absorbed by the human body invisibly and will affect our bodies to a certain extent, e.g., by causing symptoms associated with Alzheimer’s disease. Therefore, the detection of aluminum is particularly important. The methods to detect metal ions include precipitation methods and electrochemical methods, which are cumbersome and costly. Fluorescence detection is a fast and sensitive method with a low cost and non-toxicity. Traditional fluorescent nanomaterials have a high cost, high toxicity, and cause harm to the human body. Graphene quantum dots are a new type of fluorescent nanomaterials with a low cost and non-toxicity that can compensate for the defects of traditional fluorescent nanomaterials. In this paper, c-GQDs and o-GQDs with good performance were prepared by a bottom-up hydrothermal method using o-phenylenediamine as a precursor and citric acid or boric acid as modulators. They have very good optical properties: o-GQDs exhibit orange fluorescence under UV irradiation, while c-GQDs exhibits cyan fluorescence. Then, different metal ions were used for ion detection, and it was found that Al³⁺ had a good quenching effect on the fluorescence of the o-GQDs. The reason for this phenomenon may be related to the strong binding of Al³⁺ ions to the N and O functional groups of the o-GQDs and the rapid chelation kinetics. During the chelation process, the separation of o-GQDs’ photoexcited electron hole pairs leads to their rapid electron transfer to Al³⁺, in turn leading to the occurrence of a fluorescence-quenching phenomenon. In addition, there was a good linear relationship between the concentration of the Al³⁺ ions and the fluorescence intensity, and the correlation coefficient of the linear regression equation was 0.9937. This illustrates the potential for the wide application of GQDs in sensing systems, while also demonstrating that Al³⁺ sensors can be used to detect Al³⁺ ions.     

SURFACE ENHANCED RAMAN SCATTERING EFFECT OF SEMIQUINONEDIIMINE OF CD-2 ADSORBED ON SILVER CLUSTER

The development process is very compicated. The detailed mechanism of color development is not very clear. In the present work, the interaction of the color developer and the silver sol was studied by absorption spectroscopy, normal Raman and surface enhanced Raman spectroscopy.