Flame retardancy of poly(styrene-co-acrylonitrile) by the synergistic interaction between clay and phosphomolybdate hydrates

A combination of montmorillonite (MT) clay and catalysts was used to explore possible synergistic effects in reducing the flammability of poly(styrene-co-acrylonitrile) (SAN). Several catalysts, including ammonium phosphomolybdate hydrate (NHPMo), melamine phosphomolybdate hydrate (MEPMo), zinc phosphomolybdate hydrate (ZnPMo) and sodium phosphomolybdate hydrate (NaPMo), were used. The combination of MT (Cloisite 20A) with NHPMo showed synergistic enhancement in improving the char formation and reducing the peak mass loss rate of SAN40 as compared with SAN40 composites containing MT or NHPMo alone, while similar synergistic performance was not obtained between MT and NaPMo or ZnPMo or MEPMo. The better flame retardancy with this combination is probably due to the two primary aspects. One is the increased catalytic activity of the combination of Cloisite 20A and NHPMo probably due to the overlapping degradation temperature range of the combination of 20A/NHPMo and SAN40, which probably results in more char formation; the other is more NHPMo being around or on the clay stacks while less is in the galleries of the clay; this probably bridges the clay stacks and strengthens the clay network with char formed during the degradation process. High temperature rheological data confirmed the formation of a stronger network structure in SAN40/20/NHPMo; this benefits flame retardancy by allowing fewer cracks to form in the outer char layer on the polymer mass. The more continuous char layer suppresses bubbles transport of fuel vapors and heat transfer through the char layer, thereby reducing the mass loss rate.     

磷钼酸铵分光光度法测定茶多酚

在pH=5.3的醋酸-醋酸铵(HAc-NH4Ac)介质中,茶多酚与磷钼酸铵结合形成磷钼酸酯,溶液最大吸收波长为320nm。茶多酚的浓度在0.01—0.20mg/mL范围内遵守比耳定律,其表观摩尔吸光系数为ε=1.22×105L.mol-1.cm-1。方法选择性较好,用于茶汤中总茶多酚含量的测定,所得结果与标准方法测定结果基本一致。     

A Novel Sensor Based on Layer‐by‐Layer Hybridized Phosphomolybdate and Poly(ferrocenylsilane) on a Cysteamine Modified Gold Electrode

A novel sensor have been constructed by layer‐by‐layer hybridizing phosphomolybdate (POM) and poly(ferrocenylsilane) (PFS) on a cysteamine modified gold electrode. The properties and performance of the sensor have been measured by electrochemistry and atomic force microscopy in detail. The results showed that the constructed multilayers modified gold electrode combined the properties of POM and PFS, and exhibited good electrocatalytic ability to a series of inorganic ions, including BrO , IO , NO , Fe³⁺, ascorbic acid and SO . The well catalytic activity of the sensor was ascribed to the porous structure of hybrid POM‐PFS multilayer. The resulted sensor exhibited extremely fast amperometric response, low detection limit, high selectivity and wide linear range to these analyses.     

The molybdenum blue reaction for the determination of orthophosphate revisited: Opening the black box

The molybdenum blue reaction, used predominantly for the determination of orthophosphate in environmental waters, has been perpetually modified and re-optimised over the years, but this important reaction in analytical chemistry is usually treated as something of a 'black box' in the analytical literature. A large number of papers describe a wide variety of reaction conditions and apparently different products (as determined by UV–visible spectroscopy) but a discussion of the chemistry underlying this behaviour is often addressed superficially or not at all. This review aims to rationalise the findings of the many 'optimised' molybdenum blue methods in the literature, mainly for environmental waters, in terms of the underlying polyoxometallate chemistry and offers suggestions for the further enhancement of this time-honoured analytical reaction.     

Hydrothermal assembly and structural characterization of an unprecedented one-dimensional chain constructed from nickel diphosphopentamolybdate clusters

A novel molybdenum phosphate complex, [Ni(1)(en)₂(PO₄)₂Mo₅O₁₅][Ni(2)(en)₂- (H₂O)₂]?·?H₂en?·?3H₂O (1), has been synthesized under hydrothermal conditions. The complex was characterized by elemental analysis, FT-IR, DTA/TG and single crystal X-ray diffraction. The compound is orthorhombic, space group P2₁2₁2₁, with a?=?12.580(3), b?=?17.676(4), c?=?17.969(4)?Å, V?=?3995.5(15)?ų, Z?=?4, and was refined to R ₁?=?0.0301, wR ₂?=?0.0715. It possesses an unprecedented one-dimensional chain structure constructed from molybdenum phosphate clusters and nickel complex fragments.     

磷钼蓝共振散射光谱分析法测定抗坏血酸

在硫酸介质中,抗坏血酸可以定量地将磷钼酸铵还原成磷钼蓝,磷钼蓝在390nm波长处产生强烈的共振光散射峰,在0.15—5.00mg/L范围内,随着抗坏血酸浓度的增加,共振散射强度线性增强,回归方程为ΔIRS=21.45ρ+2.63,相关系数为0.9986,检出限0.12mg/L。由此建立了一种简单、灵敏检测抗坏血酸的方法,该方法用于测定饮料中的抗坏血酸,具有方便、快速的特点和较高的准确度和重现性。     

固体石蜡碳糊—磷钼酸根电极的研制与应用

研究了以固体石蜡作粘和剂的碳糊电极,在磷钼酸溶液中活化一定时间后,该电极对1.0×10~(-6)～5.0×10~(-4)mol·L~(-1)的磷钼酸有能斯特响应,斜率约为30mV,检出限为3.2×10~(-7)mol·L~(-1).电极的稳定性和选择性较好,已用于矿石、水样中磷的测定,结果满意.     

Electrochemical charging and electrocatalysis at hybrid films of polymer-interconnected polyoxometallate-stabilized carbon submicroparticles

Using the layer-by-layer technique, carbon submicroparticles, that have been modified and stabilized with monolayers of Keggin-type phosphododecamolybdate (PMo₁₂O₄₀³⁻), can be dispersed in multilayer films of organic polymers, poly(3,4-ethylenedioxythiophene), i.e., PEDOT, or poly(diallyldimethylammonium) chloride, i.e., PDDA, deposited on glassy carbon or indium-tin oxide conductive glass electrodes. The approach involves alternate treatments in the colloidal suspension of PMo₁₂O₄₀³⁻-covered carbon submicroparticles in the solution of monomer, 3,4-ethylenedioxythiophene or in solution of PDDA polymer. Electrostatic attractive interactions between anionic phosphomolybdate-modified carbon submicroparticles and cationic polymer layers permit not only uniform and controlled growth of the hybrid organic–inorganic film but also contribute to its overall stability. The system composed of PMo₁₂O₄₀³⁻-covered carbon submicroparticles dispersed in PEDOT is characterized by fast dynamics of charge transport and has been used to construct symmetric microelectrochemical redox capacitor. The PDDA-based system has occurred to be attractive for electrocatalytic reduction of hydrogen peroxide.     

含磷无机盐添加剂对甲醇羰基化反应的助催化作用研究

以Rh(OAc) 2 为催化剂,以钠、锌和铵的磷酸盐以及钠的磷钼酸盐和磷钨酸盐作为添加剂,在催化甲醇羰基化制乙酸的反应中系统考察了不同添加剂对反应的影响。实验表明,加入添加剂后可显著提高该反应体系的催化活性。其中磷酸盐系列以磷酸铵的助催化效果最好,该催化体系醋酸的时空收率能达到40mol (L·h)以上。磷钼酸钠催化体系在温度较高时醋酸的时空收率高于磷钨酸钠,达到3 5mol (L·h)以上。     

Preparation of Keggin‐type phosphomolybdate by a one‐step solid‐state reaction at room temperature and its application in protein adsorption

Keggin‐type phosphomolybdate ((C₁₉H₄₂N)₃PMo₁₂O₄₀) is prepared by a one‐step solid‐state reaction at room temperature and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X‐ray diffraction, thermogravimetric analysis, and elemental analysis. The as‐prepared phosphomolybdate is demonstrated to be an efficient adsorbent for proteins. In this particular case, the selective adsorption of neutral protein hemoglobin is achieved. While under the same conditions virtually no adsorption of acidic and basic proteins, represented by bovine serum albumin and cytochrome c, are observed. A solid‐phase extraction procedure is developed for the selective isolation of hemoglobin. At pH 6, a sorption efficiency of 91.4% is achieved for 100 μg/mL hemoglobin in 1.0 mL solution by using 5.0 mg of the phosphomolybdate. The adsorption behavior of hemoglobin fits well with a Langmuir adsorption model, corresponding to a theoretical adsorption capacity of 55.86 mg/g. The retained hemoglobin could be readily recovered by using a 60 mmol/L imidazole solution at pH 7, giving rise to a recovery of 64.7%. The practical application of phosphomolybdate for protein adsorption is demonstrated by the selective isolation of hemoglobin from human whole blood followed by a sodium dodecyl sulfate polyacrylamide gel electrophoresis assay.