Investigation of 2-[(<Emphasis Type="Italic">E</Emphasis>)-2-(4-diethylaminophenyl)-1-ethenyl]-1,3,3-trimethyl-3H-indolium as a new highly sensitive reagent for the spectrophotometric determination of nitrophenols

A new, simple, rapid, and sensitive spectrophotometric method has been developed for the determination of nitrophenols [picric acid (PA); dinitrophenols (DNP)] in wastewater samples. The method is based on the reaction of nitrophenols with 2-[(E)-2-(4-diethylaminophenyl)-1-ethenyl]-1,3,3-trimethyl-3 H-indolium chloride reagent to form the colored ion associates, which are extracted by organic solvents. The molar absorptivity of the ion associates of PA with the investigated reagent ranges from 8.3×10⁴ to 11.3×10⁴ L mol^–1 cm^–1, depending on the extractant. Because only PA is extracted in an acidic medium with the investigated reagent, but both PA and DNP are extracted in an alkaline medium, it is possible to determine both substances in a mixture. Appropriate reaction conditions have been established. The absorbance of the colored extracts obeys Beers law in the range of 0.04–4.58 mg L^–1 PA, 1.0–18.4 mg L^–1 2,4-DNP and 1.2–14.7 mg L^–1 2,6-DNP, respectively. The limit of detections, calculated from a blank test (n=10; P=0.95), are 0.05 mg L^–1 PA, 0.9 mg L^–1 (2,4-DNP), and 1.1 mg L^–1 (2,6-DNP), respectively.     

Thermal evolution of ferromagnetic metallic glasses

A traditional TG apparatus was modified by placing two permanent magnets producing a controlled magnetic field (TG(M): Magneto Thermogravimetry). This technique proved to be useful to study both structural relaxation and crystallisation of ferromagnetic metallic glasses. Results obtained for the amorphous alloys Fe₄₀Ni₄₀P₁₄B₆ and Fe_62.5Co₆Ni_7.5Zr₆Nb₂Cu₁B₁₅, are reported in this paper. Structural relaxation can be evaluated by measuring changes in Curie temperature induced by thermal treatments. Crystallisation in TG(M) is detected through a change in the measured apparent mass (difference between the sample mass and magnetic force driving it upward). These results were confirmed by DSC analysis. Whether the obtained crystalline phase is ferromagnetic, it can be identified through its Curie temperature, measured by TG(M). In fact the value of 770°C measured as Curie temperature of crystallised Fe_62.5Co₆Ni_7.5Zr₆Nb₂Cu₁B₁₅led to conclude that the only ferromagnetic crystalline phase is a-Fe. These hypothesis was confirmed by XRD analysis, showing that the first crystallisation yields to a-Fe nanocrystals. This revised version was published online in July 2006 with corrections to the Cover Date.     

WS2 超细粉体的固相法合成

WS2 超细粉体的固相法合成;WS2;固相反应;过硫系数;高能球磨;粒度     

四（五氟化苯基）卟啉氯化铁选择催化氧化超临界丙烷的反应机理

 以BHT为自由基捕捉剂，研究了四（五氟化苯基）卟啉氯化铁（Ⅲ）将超临界丙烷高选择性催化氧化为丙醇的反应机理．通过GC－MS分析发现，反应产物中有PBHT，故可认为在超临界丙烷氧化反应过程中有丙基自由基存在，初步推断反应涉及自由基机理．同时发现高浓度BHT抑制反应，低浓度BHT促进反应的现象，而以戊烷为底物时没有促进作用．这是由于BHT的位阻效应所致．并对BHT存在时超临界丙烷氧化反应机理进行了初步的推断．     

两种荧光LB膜的制备和光谱性能

制取了４－二氰基亚甲基－２－甲基－６－对二甲胺基苯乙烯基－４Ｈ－吡喃（ＤＣＭ）和１，２－双（５－甲基苯并恶唑）基乙烯（ＤＴ）两种荧光分子的ＬＢ膜以及两者的混合膜，以吸收光谱和荧光光谱探讨了膜中分子的构型，微环境，发光性能等特征，发现在ＬＢ膜的缀密排布环境中ＤＣＭ顺式构型的含量较之在溶液中大为增加。     

Williamson法合成两亲性聚醚砜酮-聚乙二醇接枝共聚物

含二氮杂萘酮结构的聚醚砜酮(PPESK)是一种新型的耐热可溶解工程塑料,其玻璃化温度高达263~305℃,可用来制造耐高温气体分离、超滤和纳滤膜,表现出优异的综合性能[1~4].然而,膜材料本身的疏水特性使PPESK膜在过滤操作中易遭受膜污染,导致膜性能下降,对膜材料进行亲水化改性以抑     

A Novel Green Preparation of a, a''''-Bis (substituted benzylidene)-cycloalkanones Promoted by FeCl_3 6H-2O in Ionic Liquid

a, a'-Bis(substituted benzylidene)cycloalkanones were efficiently prepared from cycloalkanones and benzaldehydes in [bmim][BF4] by using iron(III) chloride hexahydrate as a catalyst. It is shown that [bmim][BF4] and iron(III) chloride hexahydrate can be quantitatively recovered and be reused effectively for many times. Compared with the known methods, this novel process has the advantage of being an envkonmentally benign process together with good yields and mild reaction conditions.     

锰、铑原卟啉IX-二甲酯配合物共振拉曼光谱研究

合成了MnPPCl,RhPPCl,RhPPN3,RhPP(CO)Cl四种配合物 (PP =ProtophyrinIXDimethy1Ester) ,用元素分析、红外吸收光谱及紫外吸收光谱确定了配合物的组成 ,测定了它们的共振拉曼光谱 ,对特征谱带进行了归属。分析了拉曼谱带和电子吸收谱带变化的原因 ,提出了谱带频率的变化受金属离子外层d电子和轴配体的影响。     

Determination of selenoamino acids by gas chromatography-mass spectrometry

The application of the recently introduced ethylchloroformate derivatization method for the separation and determination of selenomethionine and selenocystein in selenium-enriched yeast and yeast-free tablets by means of a gas chromatography-mass spectrometry (GC-MS) system has been studied. The efficiency of three methods for the extraction of selenomethionine from the tablets were compared. Total selenium content of the same tablets were measured using inductively coupled plasma (ICP)-MS and it was found that in the selenized yeast tablets about 80% of the total selenium is present as selenomethionine. The results were in agreement with the values in the labels and with the literature. The accuracy of the total selenium analysis was controlled by the analysis of a reference material.