CHARACTERIZATION OF POWDER FLOWABILITY USING MEASUREMENT OF ANGLE OF REPOSE

In response to the need in industry for a quick and reproducible method of measuring the flowability of powders in processes involving transport and storage, the apparently simple idea of measuring angle of repose has been revived. The simple tester first used has evolved over a number of years into the present version which is shown to be capable of handling quite small samples of powders that are even slightly cohesive. Experimental data are presented and results shown to compare consistently with the better known Hausner ratio.     

氮化物陶瓷颗粒增强铜基复合材料的干摩擦磨损性能研究

采用粉末冶金工艺制备了纯铜以及AlNp／Cu和TiNp／Cu系列铜基复合材料，研究了2种复合材料在不同颗粒含量、不同载荷及滑动速度等条件下与45^#钢对摩时的干摩擦磨损性能，用扫描电子显微镜观察其磨损表面形貌，用能谱仪分析了磨损表面的元素组成．结果表明：与纯铜相比，AlNpCu及TiNp／Cu复合材料的耐磨性能显著提高，随着氮化物颗粒含量增加，2种复合材料的磨损率先下降而后趋于稳定；载荷与滑动速度提高引起的热效应使得纯铜及其复合材料的磨损率增高；由于TiNp的硬度高于AlNp以及本身具有一定的自润滑性能，使得TiNp／Cu复合材料的耐磨减摩性能优于AlNp／Cu复合材料．     

A three‐dimensional cadmium(II) coordination polymer with unequal homochiral double‐stranded concentric helical chains

A homochiral helical three‐dimensional coordination polymer, poly[[(μ₂‐acetato‐κ³O,O′:O)(hydroxido‐κO)(μ₄‐5‐nicotinamido‐1H‐1,2,3,4‐tetrazol‐1‐ido‐κ⁵N¹,O:N²:N⁴:N⁵)(μ₃‐5‐nicotinamido‐1H‐1,2,3,4‐tetrazol‐1‐ido‐κ⁴N¹,O:N²:N⁴:N⁵)dicadmium(II)] 0.75‐hydrate], {[Cd₂(C₇H₅N₆O)₂(CH₃COO)(OH)]·0.75H₂O}_n, was synthesized by the reaction of cadmium acetate, N‐(1H‐tetrazol‐5‐yl)isonicotinamide (H‐NTIA), ethanol and H₂O under hydrothermal conditions. The asymmetric unit contains two crystallographically independent Cd^II cations, two deprotonated 5‐nicotinamido‐1H‐1,2,3,4‐tetrazol‐1‐ide (NTIA⁻) ligands, one acetate anion, one hydroxide anion and three independent partially occupied water sites. The two Cd^II cations, with six‐coordinated octahedral and seven‐coordinated pentagonal bipyramidal geometries are located on general sites. The tetrazole group of one symmetry‐independent NTIA⁻ ligand links one of the independent Cd^II cations into 6₁ helical chains, while the other NTIA⁻ ligand links the other independent Cd^II cations into similar but unequal 6₁ helical chains. These chains, with a pitch of 24.937 (5) Å, intertwine into a double‐stranded helix. Each of the double‐stranded 6₁ helices is further connected to six adjacent helical chains through an acetate μ₂‐O atom and the tetrazole group of the NTIA⁻ ligand into a three‐dimensional framework. The helical channel is occupied by the isonicotinamide groups of NTIA⁻ ligands and two helices are connected to each other through the pyridine N and carbonyl O atoms of isonicotinamide groups. In addition, N—H...O and O—H...N hydrogen bonds exist in the complex.     

Crystal structures of the pyrazinamide–p‐aminobenzoic acid (1/1) cocrystal and the transamidation reaction product 4‐(pyrazine‐2‐carboxamido)benzoic acid in the molten state

The synthesis of pharmaceutical cocrystals is a strategy to enhance the performance of active pharmaceutical ingredients (APIs) without affecting their therapeutic efficiency. The 1:1 pharmaceutical cocrystal of the antituberculosis drug pyrazinamide (PZA) and the cocrystal former p‐aminobenzoic acid (p‐ABA), C₇H₇NO₂·C₅H₅N₃O, (1), was synthesized successfully and characterized by relevant solid‐state characterization methods. The cocrystal crystallizes in the monoclinic space group P2₁/n containing one molecule of each component. Both molecules associate via intermolecular O—H...O and N—H...O hydrogen bonds [O...O = 2.6102 (15) Å and O—H...O = 168.3 (19)°; N...O = 2.9259 (18) Å and N—H...O = 167.7 (16)°] to generate a dimeric acid–amide synthon. Neighbouring dimers are linked centrosymmetrically through N—H...O interactions [N...O = 3.1201 (18) Å and N—H...O = 136.9 (14)°] to form a tetrameric assembly supplemented by C—H...N interactions [C...N = 3.5277 (19) Å and C—H...N = 147°]. Linking of these tetrameric assemblies through N—H...O [N...O = 3.3026 (19) Å and N—H...O = 143.1 (17)°], N—H...N [N...N = 3.221 (2) Å and N—H...N = 177.9 (17)°] and C—H...O [C...O = 3.5354 (18) Å and C—H...O = 152°] interactions creates the two‐dimensional packing. Recrystallization of the cocrystals from the molten state revealed the formation of 4‐(pyrazine‐2‐carboxamido)benzoic acid, C₁₂H₉N₃O₃, (2), through a transamidation reaction between PZA and p‐ABA. Carboxamide (2) crystallizes in the triclinic space group P with one molecule in the asymmetric unit. Molecules of (2) form a centrosymmetric dimeric homosynthon through an acid–acid O—H...O hydrogen bond [O...O = 2.666 (3) Å and O—H...O = 178 (4)°]. Neighbouring assemblies are connected centrosymmetrically via a C—H...N interaction [C...N = 3.365 (3) Å and C—H...N = 142°] engaging the pyrazine groups to generate a linear chain. Adjacent chains are connected loosely via C—H...O interactions [C...O = 3.212 (3) Å and C—H...O = 149°] to generate a two‐dimensional sheet structure. Closely associated two‐dimensional sheets in both compounds are stacked via aromatic π‐stacking interactions engaging the pyrazine and benzene rings to create a three‐dimensional multi‐stack structure.     

Crystal Structure of Cesium Phenylacetylide,CsC2C6H5, Solved and Refined from Synchrotron Powder Diffraction Data

The crystal structure of cesium phenylacetylide, CsC₂C₆H₅, was solved and refined from synchrotron powder diffraction data (Pbca, Z = 8). Each Cs⁺ cation is coordinated by five ligands: four acetylide groups coordinate side‐on and one end‐on. A similar arrangement is found in the crystal structure of NaC₂H (P4/nmm, Z = 2). There is a group‐subgroup relationship between both structures. Most importantly, the crystal structure of CsC₂C₆H₅ could only be solved with the help of synchrotron data, as the very good peak:noise ratio allowed the assignment of several very weak reflections, which finally led to the correct space group, in which a structural solution was possible using direct space methods.     

Nitrogen uptake of nickel free austenitic stainless steel powder during heat treatment—an XPS study

In austenitic stainless steel nitrogen stabilizes the austenitic phase, improves the mechanical properties and increases the corrosion resistance. Nitrogen alloying enables to produce austenitic steels without the element nickel which is high priced and classified as allergy inducing. A novel production route is nitrogen alloying of CrMn‐prealloyed steel powder via the gas phase. This is beneficial as the nitrogen content can be adjusted above the amount that is reached during conventional casting. A problem which has to be overcome is the oxide layer present on the powder surface which impedes both the sintering process and the uptake of nitrogen. This study focuses on whether heat treatment under pure nitrogen is an appropriate procedure to enable sintering and nitrogen uptake by reduction of surface oxides. X‐ray photoelectron spectroscopy (XPS) in combination with scanning electron microscopy (SEM) and energy dispersive X‐ray spectrometry (EDS) are used to investigate the surface of powdered FeMn19Cr17C0.4N heat treated under nitrogen atmosphere. The analyses showed reduction of iron oxides already at 500 °C leading to oxide‐free metallic surface zones. Mn and Cr oxides are reduced at higher temperatures. Distinct nitrogen uptake was registered, and successful subsequent sintering was reached. Copyright © 2014 John Wiley & Sons, Ltd.     

离子色谱法同时测定沙棘果粉中7种有机酸含量

采用离子色谱法同时测定沙棘果粉中7种有机酸含量。样品与氢氧化钾溶液经振荡反应后过0.22μm离子滤膜,采用IonPac AG19阴离子保护柱和IonPac AS19阴离子分析柱分离,以氢氧化钾溶液进行梯度淋洗,电导检测器检测。7种有机酸的质量浓度在一定范围内与其峰面积呈线性关系。对沙棘果粉样品进行加标回收试验,7种有机酸的回收率在94.0%~109%之间,测定值的相对标准偏差(n=11)在0.20%~3.1%之间。     

三角帆蚌贝壳粉与其珍珠粉的微结构及其光谱学特征

采用扫描电镜(SEM)、热重分析(TG)、傅里叶变换红外光谱(FTIR)及白度测试对三角帆蚌贝壳与其养殖的珍珠研磨粉进行了对比研究。结果表明:1珍珠粉的υ2谱带较于贝壳粉的该谱带存在约1~3cm-1的蓝移,两者文石中的υ1与υ4谱带具有较好的一致性;2 SEM观察下,粉体的颗粒粒径大小与形貌特征并不能作为贝壳粉与珍珠粉区分鉴别的依据。3随煅烧温度的升高,贝壳粉与珍珠粉的白度先下降后升高,珍珠粉白度降低的速率高于贝壳粉,且煅烧后珍珠粉的白度最低值低于煅烧贝壳粉的白度最低值。     

选择性激光烧结高分子粉末的制备方法

综述了用于选择性激光烧结(SLS)的高分子粉末的制备方法。首先介绍了选择性激光烧结工艺对粉末在粒径、形貌、粒径分布、流动性等方面的性能要求,然后综述了常用的高分子粉末的制备方法包括机械粉碎法、直接聚合法、溶液法,以及一些较为新颖的粉末制备方法,如相分离法、微流体技术、"溶胀"粉碎法、水分散法,并对不同种类的高分子粉末的应用作了介绍。     

表面增强拉曼光谱法同时检测奶粉中三聚氰胺和二聚氰胺

本文建立了奶粉中同时检测三聚氰胺及二聚氰胺的表面增强拉曼光谱法.奶粉样品经15％三氯乙酸溶液提取,中性氧化铝吸附杂质后进行拉曼光谱检测.三聚氰胺线性范围为0.0050～0.075 mg/L,检出限为0.0015 mg/L,回收率在79.5％～124％之间,相对标准偏差小于8.8％(n=5);二聚氰胺线性范围为0.50～l0mg/L,检出限为0.15 mg/L,回收率在76.5％～112％之间,相对标准偏差小于9.4％(n=5).该方法相比常规表面增强拉曼光谱法,仅通过一种样品前处理手段即可对奶粉中的三聚氰胺或二聚氰胺进行定性检出及定量分析,相比色谱等检测方法具有样品前处理过程简单、耗时短等优点,在奶粉质量监控方面具有良好的应用前景.