三苯基锗炔基膦酸酯的合成和表征

０IntroductionInrecentyears，thechemistryoforganogermaniumcompoundswasextensivelystudiedbecauseoftheirbiologicalactivity犤１，２犦．Organotinderivativesofoxyandthiophosphorusacidarewell－known犤３～５犦．Inourearlywork，theorganotinderivativesofalkynyloralkenylphosphateweresynthesizedandtheirstructuresandbiologicalactivitieswerealsostudied犤６～８犦．Sofar，tri－organogermaniumderivativesofphosphonicacidhavenotbeenreported．Inthispaper，O－bis（triphenylgermanium）alkynylphosphatesandO－trip…     

一个新的具有梯子型链状结构的有机二膦酸铜化合物的合成和结构

０IntroductionThemetalphosphonatechemistryhasbeenofin－creasinginterestinthepastdecadeduetotheirpoten－tialapplicationsinionexchanges，adsorptionsandsensors犤１～４犦．Anumberofphosphonatecompoundshavebeenprepared，amongwhichthecoppercompoundsareuniquebecauseoftheversatilecoordinationcapabilitiesofCuions犤５～７犦．Basedon１－hydroxyethylidenediphosp－honate犤hedp，CH３C（OH）（PO３）２犦，severalcopperph－osphonateshavebeenobtainedinourlaboratoryin－cluding犤NH３（CH２）２NH３犦Cu２（he…     

新型红色荧光粉Sr3Al2O6的合成和发光性能研究

稀土金属离子激活的多铝酸盐发光材料，在可见光区具有较高的量子效率犤１～４犦，充分显示出这类荧光发光材料，在高效节能、环保、电光源与新一代可见光显示器领域的应用前景犤４～９犦。特别是SrAl２O４∶Eu２＋的持续发光现象的发现犤２，３犦，激起了对以稀土金属离子为激活剂，碱土铝酸盐为基质的长余辉无机发光材料体系的兴趣。研究表明其发光强度和余辉时间是传统硫化物发光材料的十倍以上，利用其长余辉储光－发光特性，有望开发新型发光油漆、涂料、发光陶瓷、发光塑料、薄膜、发光纸、发光纤维犤４犦。早在七十年代，荷兰菲利…     

氰基桥联双核镝(Ⅲ)-铁(Ⅲ)配合物[DyFe(CN)_6(DMF)_4(H_2O)_3]·1.25H_2O的合成与结构表征(英文)

０IntroductionRecently，severalresearchgroupshaveemployedahybridapproach，inwhich犤M（CN）６犦n－buildingblockhavebeencombinedwithtransitionmetalionsorlanthanideionscomplexesinordertoexploitthefea－turesoftheligandsintheformationofdifferentstruc－tures犤１～８犦．Cyano－bridgedcomplexesaregenerallyob－tainedbyreactinghexacyanometalatewithmononuclearassemblercomplexinwhichsomeofthecoordinationsitescanbeoccupiedbysomeassistantligands（ortermsasthethirdligands）．Severalcyano－bridgeddin－uclear…     

MgSO_4·5Mg(OH)_2·3H_2O的水热合成及反应时间对其形貌的影响(英文)

０IntroductionWhiskerswithhighaspectratiohavebeenexten－sivelyusedascompositematerialsinalloys，ceramics，cementandplastic犤１～５犦，sincetheyhavespecificdesirepropertiessuchashighmeltingpoint，lowdensityandhighmodulus犤６犦．Magnesiumoxysulfate（MOS）com－poundshowsthehighcrystallinityandaspectratiotomakeitapotentialreinforcingmaterialforplastics，resinandrubber犤７，８犦．Inpastyears，MgSO４·５Mg（OH）２·３H２Ohasbeensynthesizedbyhydrothermalreactionusingmagnesiumhydroxideandmagnesium…     

Synthesis of [MoOS_3Cu_3I(3, 5-diMePy)_4]·CH_3CN and (Et_4N)_4[Mo_4Cu_8O_4S_(12){(Ph_2PS)_2N}_4] from Solid State Product [Et_4N] _4[Mo_2O_2S_6Cu_6I_4Br_2]

Awell－groundmixtureof犤NH４犦２犤MoS２O２犦,CuI,andEt４NBr,wasputintoareactiontubeandheatedat８０℃for４hunderanitrogenatmosphere．AfterextractingtheresultantblacksolidwithCH３CN,theextractwasfilteredtoaffordadeepredfiltratewhichcontainsatwin－nestshapeinter－mediate犤NEt４犦４犤Mo２O２S６Cu６I４Br２犦１犤１犦．Twin－nestshapeproductsareinterestingbecausetheirbridgegroupscleavagecanincorporatedifferentligandsintotheclusterspecieswithinterestingskeletalstructures．Takingadvantageo…     

锐钛相虫蛀状介孔二氧化钛的表征

0IntroductionMesostructuredtitania(TiO2)hasattractedagreatdealofattention,inviewofcontrolleddelivery,catalytic,photocatlytic,orenergyconversionapplica-tions犤1犦.Theuseoftitaniumisopropoxidebis-acetylace-tonateprecursors,combinedwithalkylphosphatean-ionicsurfactantsastemplate,ledtothefirstdocu-mentedpuremesoporousTiO2犤2犦.Insubsequentyears,moresyntheticstrategieshavebeendevelopedusingavarietyofstructure-directingagents,forexample,car-boxylicacids犤3犦,alkylamine犤4犦,aminium犤5犦,blockcop-o…     

正丁基黄原酸根合镉(Ⅱ)的合成和晶体结构

黄原酸配合物以及它们与各种路易斯碱反应的产物得到广泛的研究犤１～４犦。可溶性的黄原酸碱金属盐广泛用于汞、银、镉等金属的萃取分离犤５～７犦，并且这类盐对于汞中毒具有解毒作用犤８犦。E．D．Zelmon等犤９犦对过渡金属黄原酸配合物的非线性光学性质进行了研究。但迄今为止，对黄原酸镉配合物与路易斯碱的反应与结构研究较少。我们首先合成了一种配位聚合物犤Cd（S２CO－n－C４H９）２犦n晶体，然后利用吡啶与犤Cd（S２CO－n－C４H９）２犦n反应破坏其原有配位聚合物的结构，得到了犤Cd（C５H５N）２（S２CO－n－C４H９）…     

两个β-二酮Co(Ⅱ)配合物[Co(β-diketonate)2(py)2]的合成和晶体结构

钴是生物学上重要的微量元素，它能在一些酶中代替锌，而不改变原来酶的活性犤１犦，钴的光谱和磁性是酶活性部位的有效探针犤２犦。钴催化剂是单活性中心催化剂犤３犦，同时又是很好的乙烯齐聚催化剂犤４，５犦。β－二酮是重要的催化剂原料，徐德民等犤６犦报道了含有β－二酮金属配合物催化剂制备间规聚苯乙烯与聚丙烯共混复合物。宓霞等犤７犦报道了含β－二酮钛非茂催化剂催化降冰片烯聚合。近年来，已报道了一些β－二酮的Co?配合物犤８～１０犦的晶体结构，本文报道两个β－二酮的Co?配合物的合成和晶体结构。１实验部分１．１配合…     

MgO·3B2O3·3.5H2O的合成、表征及其溶液Raman光谱分析

硼是具有独特化学行为的稀有亲氧元素，在自然界中主要是以无机硼氧酸和硼氧酸盐形式存在。在硼酸盐晶体中，硼以聚合硼氧配阴离子形式存在，其中配位数为３和４的硼原子比可以有所不同，这使得硼酸盐种类繁多，结构复杂多样。至今，人们在自然界和实验室已发现了４种六硼酸镁盐犤１，２犦：MgO·３B２O３·nH２O（n＝７．５，７，６，５），它们的分子结构中都含有犤B６O７（OH）６犦２－基团。最近，我们在硼酸盐化学系列研究中，利用复盐氯柱硼镁石在沸点温度下的硼酸溶液中的相转化，合成了一种新的六硼酸镁盐MgO·３B２O３·３．…     

Residues and dissipation of guadipyr in rice ecological system

A modified QuEChERs method with liquid chromatography-tandem mass spectrometry for analysis of guadipyr residue and dissipation in rice matrices, paddy soil and paddy water was developed and validated. Mean recoveries and relative standard deviations in paddy soil, paddy water, rice plant, rice straw, rice hull and husked rice matrices at three spiking levels were 83.1–116.5% and 1.6–9.5%, respectively. The half-life of guadipyr was determined in 2 years at three different field sites in China via a dissipation experiment. The half-lives of guadipyr in paddy water were 0.22–0.37 days, 0.24–3.33 days in paddy soil and 0.44–1.90 days in rice plant. The terminal residues of guadipyr ranged from ND (concentrations of guadipyr were below limit of detection) to 50 μg kg^?1 in paddy soil, 10–470 μg kg^?1 in rice hull, ND70 μg kg^?1 in husked rice and ND to 110 μg kg^?1 in rice straw. The results would be helpful in fixing maximum residue limit of guadipyr, a new insecticide, in rice.     

Anomalously high activities of <Superscript>137</Superscript>Cs in soils and vegetation on and near a diabase outcrop in La Sierra de Lema,Venezuela

As a result of routine soil sampling to determine the ¹³⁷Cs background activities country-wide in Venezuela, it was decided to further investigate El Mirador (Lookout) area at the base of the Sierra de Lema mountain range. In April 2003 (A), soil samples were collected at eight sites on and around the edge of the diabase outcrop to confirm that this area had anomalously high ¹³⁷Cs activities. In July 2003 (B), not only soil samples were collected again, but also black mat, palm tree leaves and trunks, fruit bushes leaves and its fruit and fern leaves. The ¹³⁷Cs content was measured by high resolution gamma-ray spectroscopy by a comparative method with reference materials. The ¹³⁷Cs activity values range from 16.3 to 30.8 Bq·kg-1 in the soil samples collected in July 2003, 20.7–32.1 Bq·kg⁻¹ for the black mat, 26.3–38.4 Bq·kg⁻¹ for the palm leaves, 16.8–31.2 Bq·kg⁻¹ for the palm trunks and 17.6–27.3 Bq·kg⁻¹ for the fruit bush leaves, while, the ¹³⁷Cs activity values for the whole fruit were between 23.4 and 30.7 Bq·kg⁻¹; but, the value of the ¹³⁷Cs activity in the center of the fruit (the edible part) was 51.6 Bq·kg⁻¹, and the value of the ¹³⁷Cs activity for the fern leaves was 51.8 Bq·kg⁻¹. Thus, most of the ¹³⁷Cs activity values determined in the soil, black mat and vegetation samples from El Mirador (Lookout) were considered anomalously high with respect to those found near the equator and in other areas of Venezuela. Only the center of the fruit from the Clusia grandiflora bushes and the fern leaves had high activity ratios, about a factor of three and could be considered as biomonitors that concentrate and retain the ¹³⁷Cs. Finally, these anomalously high ¹³⁷Cs activities have been attributed not only to the rich organic soils, as sinks, but also due to the affect of the cloud forests.     

Re-evaluation of the thermodynamic activity quantities in aqueous alkali metal nitrate solutions at T = 298.15 K

The Hückel equation used in this study to correlate the experimental activities of dilute alkali metal nitrate solutions up to a molality of about 1.5 mol · kg⁻¹ contains two parameters being dependent on the electrolyte: B [that is related closely to the ion-size parameter (a∗) in the Debye–Hückel equation] and b₁ (this parameter is the coefficient of the linear term with respect to the molality and this coefficient is related to hydration numbers of the ions of the electrolyte). In more concentrated solutions up to a molality of 7 mol · kg⁻¹, an extended Hückel equation was used, and it contains additionally a quadratic term with respect to the molality and the coefficient of this term is parameter b₂. All parameter values for the Hückel equations of LiNO₃, NaNO₃, and KNO₃ were determined from the isopiestic data measured by Robinson for solutions of these salts against KCl solutions [J. Am. Chem. Soc. 57 (1935) 1165]. In these estimations, the Hückel parameters determined recently for KCl solutions [J. Chem. Eng. Data 54 (2009) 208] were used. The Hückel parameters for RbNO₃ and CsNO₃ were determined from the reported osmotic coefficients of Robinson [J. Am. Chem. Soc. 59 (1937) 84]. The resulting parameter values were tested with the vapour pressure and isopiestic data existing in the literature for alkali metal nitrate solutions. These data support well the recommended Hückel parameters up to a molality of 7.0 mol · kg⁻¹ for LiNO₃ and NaNO₃, up to 4.5 mol · kg⁻¹ for RbNO₃, up to 3.5 mol · kg⁻¹ for KNO₃, and up to 1.4 mol · kg⁻¹ for CsNO₃ solutions. Reliable activity and osmotic coefficients of alkali metal nitrate solutions can, therefore, be calculated by using the new Hückel equations, and they have been tabulated at rounded molalities. The activity and osmotic coefficients obtained from these equations were compared to the values suggested by Robinson and Stokes [Electrolyte Solutions, second ed., Butterworths Scientific Publications, London, 1959], to those calculated by using the Pitzer equations with the parameter values of Pitzer and Mayorga [J. Phys. Chem. 77 (1973) 2300], and to those calculated by using the extended Hückel equation of Hamer and Wu [J. Phys. Chem. Ref. Data 1 (1972) 1047].     

Synthesis,characterization, and antimicrobial activity of two Schiff base silver(I) complexes derived from 4-carboxybenzaldehyde

Two new Schiff base silver(I) complexes, {[Ag(L¹)][H₂O]}_∞ (1) and {[Ag(L²)][H₂O]}_∞ (2), where L¹ = 4-((2-diethylaminoethylimino)methyl)phenecarboxylate and L² = 4-([3-(morpholin-4-yl)propyl]iminomethyl)phenecarboxylate, have been synthesized and characterized. X-ray crystallographic analysis reveals that silver ions in 1 are bridged by L¹ to form a one-dimensional zigzag chain, while three silver ions in 2 are linked by L² to produce a two-dimensional coordination polymer. Guest water molecules in 1 generate a one-dimensional hydrogen-bonded chain. Both 1 and 2 offer high antibacterial activity against Gram-positive bacteria Staphylococcus aureus with MIC values of 0.26 and 0.24 mM and to exhibit good inhibitory activity against urease with the respective IC₅₀ values of 3.5 ± 0.1 and 3.8 ± 0.2 μM.     

Cytotoxic Podophyllotoxin Type-Lignans from the Steam Bark of <em>Bursera fagaroides </em>var. <em>fagaroides</em>

The hydroalcoholic extract of the steam bark of B. fagaroides var. fagaroides displayed potent cytotoxic activity against four cancer cell lines, namely KB (ED₅₀ = 9.6 × 10^-2 μg/mL), PC-3 (ED₅₀ = 2.5 × 10^-1 μg/mL), MCF-7 (ED₅₀ = 6.6 μg/mL), and HF-6 (ED₅₀ = 7.1 × 10^-3 μg/mL). This extract also showed anti-tumour activity when assayed on mice inoculated with L5178Y lymphoma cells. Bioactivity-directed isolation of this extract, afforded seven podophyllotoxin-type lignans identified as podophyllotoxin (1), β-peltatin-A-methylether (2), 5'-desmethoxy-β-peltatin-A-methylether (3), desmethoxy-yatein (4), desoxypodophyllotoxin (5), burseranin (6), and acetyl podophyllotoxin (7) by 1D and 2DNMR and FAB-MS analyses, and comparison with reported values. All the isolated compounds showed potent cytotoxic activity in the cell lines tested, especially compound 3, which exhibited greater activity than camptothecin and podophyllotoxin against PC-3 (ED₅₀ = 1.0 × 10^-5 μg/mL), and KB (ED₅₀ = 1.0 × 10^-5 μg/mL). This is the first report of the isolation of podophyllotoxin and its acetate in a Bursera species.     

Experimental Study on the Determination and Degradation of Pyoluteorin in Soil via CE with Soxhlet’s Extraction and Field-Amplified Sample Stacking

A sensitive analytical method based on capillary electrophoresis with field-amplified sample stacking, Soxhlet’s extraction and ultrasonic extraction for studying the degradation of trace amounts of pyoluteorin (Plt, a broad-spectrum fungicide produced by fluorescent Pseudomonas) in soil samples was first developed. The limits of detection and the limits of quantification for Plt of the developed method were 0.107 and 0.36 μg mL^?1, respectively. The recoveries of Plt at three spiking concentrations of 500, 200, and 50 μg kg^?1 were 94.18, 79, and 78.25%, respectively. In this communication, we successfully performed the investigation on the dynamic residue of Plt during its decomposition in agriculture soil using the method developed. The calculated t _1/2 values for Plt residue in near-surface and rhizosphere soil were 42.26 and 32.84 h, respectively. The results show that Plt has good environmental compatibility.     

Concentration of arsenic in soil samples collected around the monazite processing facility, Thailand

Arsenic (As) in soil is a contaminant originated from human activities including pesticide use, mining and ore processing operations. In this work, As concentration in soil samples collected around the monazite processing facility, Pathum Thani, Thailand, was investigated. The collections of 24 soil samples were collected from the monazite processing area and 7 soil samples were collected from the control area without the processing activity of the same facility. Soils were digested with the mixture of HNO₃, HClO₄ and HF using a microwave digester. Inductively coupled plasma mass spectrometer (ICP-MS) equipped with an octopole reaction system (ORS) was used to determine the concentration of As in soils after the acid digestion. JB-3 (igneous rock) was the standard reference material used to check the accuracy of the method. It was found that the analytical results showed good agreement with the certified values. As concentration in soils collected from the monazite processing area ranged from 3.85 to 36.01 mg kg^?1 with the mean of 13.06 mg kg^?1. The concentration of As higher than the US EPA cancer soil screening level (22 mg kg^?1) was observed for only one sample. The control area showed As concentration varied from 9.59 to 14.19 mg kg^?1 with the mean of 11.97 mg kg^?1. The obtained results from this work were compared with the contaminated soil data of Amphoe Ron Phibun, Nakhon Si Thammarat, Thailand.     

Synthesis,structure, and urease inhibitory activities of Co(III), Mn(II) and Zn(II) complexes with hydrazone derived from protocatechuic acid

[Co^III(L₁)₂·H₂O]NO₃ (1), [Mn^II(L₁)₂·H₂O] (2), and [Zn^II(L₁)₂·H₂O] (3) with a hydrazone derived from protocatechuic acid (HL₁ = C₁₅H₁₃N₃O₃) were designed, synthesized, and characterized by C, H, N elemental analyses, single-crystal X-ray diffraction, and IR spectra, which revealed that the three complexes are similar structures. Docking study has been done. The urease inhibitory activities of the three complexes were tested. Complexes 1 and 3 showed strong inhibitory activity against jack bean urease with IC₅₀ values of 45.9 and 11.64 μM. Complex 2 had no obvious inhibitory activity to urease; the IC₅₀ was > 50 μM.     

Assessment of effective radium content and radon exhalation rates in soil samples

Effective radium content and radon exhalation rates in soil samples have been measured by ??Sealed Can Technique?? using LR-115 type II plastic track detectors. The soil samples were collected from Farrukhabad city of Utter Pradesh, India. The values of effective radium content were found to vary from 5.39 to 34.56?Bq?kg^?1 with an average value of 16.58?Bq?kg^?1 and a standard deviation of 7.16. The mass and surface exhalation rate has been found to vary from 0.41?×?10^?6 to 2.64?×?10^?6?Bq?kg^?1?d^?1 and 1.41?×?10^?6 to 9.10?×?10^?6?Bq?m^?2?d^?1, respectively. All the values of radium content in soil samples of study area were found to be quite lower than the permissible value of 370?Bq?kg^?1 recommended by Organization for Economic Cooperation and Development.