Synthesis and Crystal Structure of t he Complex of Antimony Trichloride and Dioxane

New solid complex of the antimony trichloride and dioxane was obtained th rough a reaction of the dioxane and the absolute methanol solution of the antimony trichloride.The formula of the complex is[SbCl_(3)·{(CH_(2))_(4)O_(2)}_(1.5)].The crystal structure of the comple x belongs to cubic system,space group I-43d,a=17.1417(5)?,Z=16.The trivalent antimony ion not only bonds directly to three chlorine anions,but also is co ordinated by three oxygen atoms of th e dioxane molecules.Two oxygen atoms in a dioxane molecule wi ll coordinate to different antimony ions,respectively.

Simultaneous Determination of Melamine, Ammelide, Ammeline, and Cyanuric Acid in Milk and Milk Products by Gas Chromatography-tandem Mass Spectrometry

Objective To develop an analytical method for simultaneously qualitative and quantitative determination of melamine and triazine-related by-products including ammelide, ammeline, and cyanuric acid in milk and milk products by gas chromatography- tandem mass spectrometry （GC-MS/MS）. Methods Melamine and triazine-related by-products namely ammelide, ammeline and cyanuric acid in the samples were extracted in a solvent mixture of diethylamine, water, and acetonitrile （10：40：50, V/V/V）. After centrifugation, an aliquot of the supernatant was evaporated to dryness under a gentle stream of nitrogen gas, and then melamine and triazine-related by-products were derivatized using BSTFA with 1% TMCS. The derivatives of melamine and its analogues were determined by gas chromatography/tandem mass spectrometry using multiple reactional monitoring （MRM） with 2, 6-Diamino-4-chloropyrimidine （DACP） being used as an internal standard. Results The linear detectable ranges were from 0.004 mg/kg to 1.6 mg/kg for melamine, ammelide, ammeline, and cyanuric acid with a correlation coefficient no less than 0.999. The recovery rates of the tour compounds in spiked blank milk powder at concentrations 0.5, 1, 2 mg/kg were between 61.4%-117.2%, and the relative standard deviation was no more than 11.5% （n=6）. The detection limits of melamine, ammelide, ammeline and cyanuric acid in milk powder were 0.002 mg/kg with a ratio of signal to noise of 3. Conclusion This GC-MS/MS method for simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products is sensitive and specific.

Gallium trichloride-catalyzed conjugate addition of indole and pyrrole to α,β-unsaturated ketones in aqueous media

Michael addition of indole and pyrrole to a variety of α, β-unsaturated ketones was efficiently promoted by a catalytic amount of GaCl3 in aqueous media to afford the corresponding products in good to excellent yields.

Wet cyanuric chloride promoted efficient synthesis of amidoalkyl naphthols under solvent-free conditions

An efficient and direct procedure has been developed for the preparation of amidoalkyl naphthols by a one-pot condensation of aryl aldehydes, 2-naphthol and urea or amides, in the presence of wet-cyanuric chloride （wet-TCT） as a catalyst. The reactions were carried out under solvent-free media. The present methodology offers several advantages such as excellent yields, simple procedure and eco-friendly reaction condition.

Induction of Apoptosis in the Immature Mouse Testes by a Mixture of Melamine and Cyanuric Acid

The toxicity of melamine has attracted much attention since the recent outbreaks of renal injury in pets and infants. Previous studies indicated that melamine by itself had low toxicity, whereas a mixture of melamine and cyanuric acid （M＋CA） could cause serious renal damage. At present, most researches on the toxicity of M＋CA are focused on the kidney. However, little is known about the adverse effects of this mixture on the reproductive system. In the present study, the toxicity of M＋CA to testes was investigated. Immature male mice were orally dosed with 0, 0.6, 3, and 15 mg kg-1 d-1 of a 1：1 M＋CA for 28 d. Pathological changes occurred in germ cells, such as loose arrangement, reduced numbers and karyopyknosis, indicating that this mixture was toxic to spermatogenesis. Compared with the control group, the TUNEL- positive germ cells increased significantly and the ratio of Bcl-2 to Bax, total antioxidant capacity and superoxide dismutase activity decreased significantly in the 3 and 15 mg kg-1 d- M＋CA treated group, while the activities of caspase-3, caspase- 8 and caspase-9 remained unchanged. The results suggest that M＋CA can induce apoptosis in the mice testes. The downregulation of Bcl-2/Bax and oxidative stress may play a pivotal role in the induction of apoptosis by M＋CA in mice testes.

Crystal and Molecular Structure of Cyanuric Acid

The title compound [C3H3N3O3·2H2O] was synthesized by the reaction of urea with hydrogen peroxide, and characterized by elemental analysis, infrared spectra and nuclear magnetic resonance. The crystal belongs to monoclinic system,space group C2/c, with a=12. 538(3)i, b=6. 685(1),c=8.807 (3) , β= 116.11(2)°;V=662. 9(4), Z=4, Mr=165.11, Dc=1.65g/cm3, (MOKα)=0. 71069,μ=1. 47 cm-1, F(000) = 344,final R=0. 046 and Rω=0.061 for 493 observable reflections with I>3σ(I). All atoms lie in plane giving the molecule a planar configuration. The bond length of C-O is 1.214(3), C-N is 1.366(3). Every two cyan-uric molecules in the cell are connected by two intermolecular hydrogen bonds N-H…O, with N…O distance of 2.763 , N-H…O angle of 180.0°.

A facile synthesis of 2,4,6-trichloroborazine from boron trichloride-dimethylsulfide complex and ammonium chloride

2,4,6-Trichloroborazine has been recognized as a desirable monomer for the preparation of high-performance boron nitride fibers through polymer derived ceramics route.So a high yield and facile synthesis of 2,4,6-trichloroborazine is essential in practice. Using boron trichloride-dimethylsulfide complex((CH_3)_2S·BCl_3) and ammonium chloride(NH_4Cl) as starting materials and toluene(C_6H_5CH_3) as solvent,the synthesis of 2,4,6-trichloroborazine to give high yield is reported.

Crystal Structure of Calcium Complex with Cyanuric Acid Ligand［Ca（C3H3N3O3－O）（H2O）6］［（OH）（C3H2N3O3）］

The title compound[Ca(C3H3N3O3)(H2O)6][(OH)(C3H3N3O3)] crystallizes in the triclinic system,space group P1,with a=6.501(5),b=10.814(6),c=11.803(1) A,α=103.64(1),β=92. 72(3),γ=98. 82(4)°,V=793- 9(7) A3,Dc=l.77 g/cm3,Z=2,Mr=422. 32,λ(MoKα)=0.71069 A,μ=4.65 cm-1,F(000)=440,final R=0.045 and Rω=0.058 for 3422 observable reflections with I≥3σ(I).In the complex cation [Ca (C3H3N3O3)(H2O)6]2+,the Ca2+ is coordinated by an oxygen atom from cyanuric acid ligand and six oxygen atoms from water molecules forming a distorted pentagonal bipyramid geometry.The complex anions, OH- and C3H2N3O3-,are bound with the complex cation[(Ca(C3H3N3O3)(H2O)6]2+ by electrostatic force to form the title compound.

Iron trichloride as oxidizer in acid slurry for chemical mechanical polishing of Ge_2Sb_2Te_5

The effect of iron trichloride （FeC13） on chemical mechanical polishing （CMP） of Ge2Sb2Te5 （GST） film is inves- tigated in this paper. The polishing rate of GST increases from 38 nm/min to 144 nm/min when the FeC13 concentration changes from 0.01 wt% to 0.15 wt%, which is much faster than 20 nm/min for the 1 wt% H2O2-based slurry. This polish- ing rate trends are inversely correlated with the contact angle data of FeCl3-based slurry on the GST film surface. Thus, it is hypothesized that the hydrophilicity of the GST film surface is associated with the polishing rate during CMP. Atomic force microscope （AFM） and optical microscope （OM） are used to characterize the surface quality after CMP. The chemical mechanism is studied by potentiodynamic measurements such as Ecorr and Icorr to analyze chemical reaction between FeCl3 and GST surface. Finally, it is verified that slurry with FeCl3 has no influence on the electrical property of the post-CMP GST film by the resistivity-temperature （RT） tests.

Synthesis, Structure and Transesterification of the Derivatives of β-Alkoxycarbonylethyltin Trichlorides with Diethyldithiocarbamate

The derivatives of β-alkoxycarbonylethyltin trichlorides with diethyldithiocarbamate,ROCOCH2CH2Sn(S2CNEt2)Cl2, were synthesized and characterized by the means of elemental analysis, IR, 1H NMR and X-ray single crystal diffraction. The structural features of the compounds were described, and the possible mechanism of transesterification for compound 2a was suggested.

Synthesis and Structure of the Complexes of 2-Alkoxycarbonylalkyltin Trichlorides with 2-Salicylideneaminophenol

The complexes of 2-Alkoxycarbonylalkyltin Trichlorides with 2-Salicylideneamino-phenol have been synthesized and characterized by means of elemental analysis, lR, 1H-NMR andX-ray single crystal diffraction. The structural features of the complexes are described.

Research Progress on Detection Methods of Melamine and Cyanuric Acid Residue in Dairy Products and Feedstuff

[Objective] More accurate, rapid and sensitive method of melamine and cyanuricacid residue in dairy products and feedstuff were re- viewed. [ Method] Physicochemical properties, metabolism, uses, harm and detection methods of melamine and cyanuric acid were analyzed and described. [ Result] Melamine and cyanuric acid, when used alone, were slightly toxic, but long -term intake could lead to animal reproductive and urinary system damage. [ Condusion] Establishing a more sensitive, fast and easy to popularize detection method for elarnine and cyanuricacid res- idue in dairy products and feedstuff was necessary.

Effects of Aluminum Trichloride on Structure and Function of Kidney in Chickens

To investigate the effects of aluminum trichloride （AlCl3） on renal structure and function in chickens, the chickens were injected continuously with different gradient AlCl3 for 60 days to establish sub-chronic aluminum （Al） intoxication model. The AI concentration in serum and kidney, contents of creatinine （Cr） and blood urea nitrogen （BUN） in serum were detected, and the renal structure was also observed by optical microscope. The results showed that the A1 concentration in serum and kidney, the contents of Cr and BUN in serum were significantly higher in Al-treated chickens than those in the control group （P〈0.05; P〈0.01） and there was an AlCl3 dose-depended manner. Histopathologically, in the low dose group, acinus renis swelled mildly and there were no apparent pathological changes in nephric tubule and proximal convoluted tubule. In the middle and high dose group, acinus renis swelled, glomerular cells increased, nephric tubule cloudy swelled, and epithelial cells of proximal convoluted tubule swelled. The results indicated that sub-chronic Al exposure impaired the renal structure and function in chickens.

SYNTHESIS AND CHARACTERIZATION OF THE COMPLEXES OF β－ALKOXYCARBONYLETHYLTIN TRICHLORIDES WITHDBSO AND HMPA

A convenient approach on transesterification to preparing the complexee of β-alkoycarbonylethyltin trichlorides with dibenzylsulfoxide (DBSO) andhexametkylphosphoramide (HMPA) was reported. The structures of complexes were characterized by elemental analysis, IR, 1HNMR and X-ray single crystal diffraction.The possible mechanism for the transesterification of complexes of β-onylethyltin trichloride with an alcohol was suggested

Biodegradation of Melamine and Cyanuric Acid by a Newly-Isolated <i>Microbacterium</i>Strain

We searched for a superior melamine-degrading bacterium for the bioremediation of melamine. Cyanuric acid, which is a by-product produced during the biodegradation of melamine, shows strong nephrotoxicity. Therefore, the melamine-degrading bacterium is also required to show a high ability to degrade cyanuric acid. We selected a melamine-degrading strain (MEL1) among ten cyanuric acid-degrading bacteria isolated from the soil. The species of MEL1 strain was Microbacterium esteramaticum or was extremely similar to that species, and the enzymatic activity of the melamine deaminase in the MEL1 strain was similar to that in the NRRLB-12227 strain. The ability of the MEL1 strain to degrade cyanuric acid was higher than its ability to degrade melamine, and therefore, the accumulation of by-products (ammeline, ammelide and cyanuric acid) during the degradation of melamine was minimal. These results suggest that the MEL1 strain is useful for the bioremediation of melamine.

ACYLATIVE CLEAVAGE OF CYCLIC ETHERS CATALYZED BY SAMARIUM TRICHLORIDE

Oxiranes as well as four and five membered rings of cyclic ethers were cleaved with acyl chloride in the presence of samarium trichloride or Eu(hfe)_3 as Lewis-acid catalyst under mild conditions,the oorresponding chloroesters were obtained readily and smoothly in excellent yields.

THE SOLUBILITY OF FERROALLOYED NEODYMIUM IN MOLTEN SALT CONTAINING NEODYMIUM TRICHLORIDE

The solubility of ferroalloyed neodymium in molten salt containing neodymium trichloride and the de- pendence of solubility on temperature and composition of the melt are determined by means of electrochemical method.The data obtained are in good agreement with result of chemical analysis of the quenched molten salt samples.

Synthesis and Surface Active Properties of Cyanuric Chloride-based Branched Surfactant

A series of novel branched sodium carboxylate surfactants were synthesized from cyanuric chloride, behera amine, alcohol amine and 1,4-Bis (3-aminopropyl) piperazine through seven steps, and the total yield is about 25%. The chemical structures of target products were confirmed by 1H NMR, 13C NMR, FT-IR and ESI-MS. Their critical micelle concentrations (CMC) were also determined by surface tension tests in the aqueous solutions at 22 ℃. The results showed that the CMC value of multi-carboxylate anionic surfactants decreased with the increase of hydroxyl. Additionally, the branched structure of end group can reduce surface tension more than straight-chain type, which was determined by γCMC. The decomposition temperature of the target compound was 250 ℃, which was also tested by TG/DTA curve.

An Evaluation of Genotoxicity and Cytotoxicity of Melamine in Combination with Cyanuric Acid at Three Mass Ratios

Melamine in combination with cyanuric acid has been considered to be more toxic than either melamine or cyanuric acid alone. The objective of this study was designed to evaluate the combined genotoxicity and cytotoxicity of melamine （M） and cyanuric acid （C） at three mass ratios （1：1, 1：2, 2：1）. MC （1：1）, MC （1：2）, and MC （2：1） were evaluated for their potential genotoxic risk, at gene level by Ames test, and at chromosomal level by micronucleus test. In order to evaluate cytotoxicity in HEK-293 cells, the MTT assay was included. Western blot was also employed to investigate the renal injury molecule-1 （Kim-1） expression in HEK-293 cells exposed to MC. Neither genotoxicity at gene level nor at chromosomal level was observed for MC （1：1）, MC （1：2）, and MC （2：1）. Based on MTT assay, three ratios of MC at 82.5 and 165 μg/mL slightly inhibited viability of HEK-293 cells （P〈0.05）. MC （1：1） at 41.25 and 82.50 IJg/mL could elevate the Kim-1 expression in HEK-293 cells.

三氯化钒还原-分光光度法测定海水中硝酸盐的含量

为解决铜镉柱还原法在测定海水中硝酸盐时的操作繁琐、耗时、毒性大、难以适应大批量样品的快速测定等问题,提出了题示方法。取5 mL样品(海水样品用水稀释至盐度不大于7)和1 mL还原剂(体积比5∶1∶1的10 g·L^(-1)三氯化钒溶液、40 g·L^(-1)磺胺溶液和1.0 g·L^(-1)盐酸萘乙二胺溶液的混合溶液)于10 mL试管中,于45℃的水浴锅中加热60 min,取出,置于冰水混合物中冷却5 min,在543 nm波长下测定体系的吸光度差值。结果表明:方法的硝酸盐还原率在95%以上;当样品盐度不大于7时,基本消除盐效应对测定的影响,可用于淡水和海水中硝酸盐的测定。硝酸盐的质量浓度在300.0μg·L^(-1)以内与对应的吸光度差值呈线性关系,检出限为1.0μg·L^(-1)。对50.0,200.0μg·L^(-1)的加标样品溶液进行准确度和精密度试验,测定值与已知值基本一致,测定值的相对标准偏差(n=10)小于0.50%。采用本方法与HY/T 147.1-2013测定实际海水样品,两种方法的测定结果具有一致性,不存在显著性差异。本方法降低了试剂对环境的污染,避免了铜镉柱制备和过柱操作,可用于海水中硝酸盐的快速、批量测定。