菲咯嗪分光光度法测定食品中的铁

本文建立了菲咯嗪分光光度法测定食品中铁含量的方法.在pH 4.5的乙酸-乙酸钠缓冲介质中,Fe(II)与菲咯嗪络合,生成紫色的络合物,其最大吸收波长是562nm,摩尔吸光系数ε=2.65×104 L ·mol-1·cm-1,Fe(II)含量在0～50μg/25mL之间符合比尔定律.该方法操作简单,灵敏度高,选择性好,准确度高,重现性好,用于测定茶叶、奶粉中铁的含量,结果令人满意.     

分光光度法测定猪肾中的硒

在盐酸介质中3—3’二氨基联苯胺与硒反应生成黄色络合物,λ_(max)=420nm,ε=4×10~4L·mol~(-1)·cm~(-1),硒含量在0.5～50μg/25ml内符合比尔定律,本方法用于猪肾样品中硒的测定结果令人满意。     

反相高效液相色谱法同时测定洁康舒洗剂中三组分的含量

建立反相高效液相色谱法同时测定洁康舒洗剂中大黄酸、大黄素和大黄酚含量的方法。采用反相高效液相色谱法。symmctry C18柱(3.9×150mm,5μm)流动相为甲醇—水—磷酸(80:20:0.1);流速为1.0mL·min-1;检测波长为432nm。大黄酸、大黄素和大黄酚的回归方程分别为:C1=7.3159×10-1+1.8966×10-5A,r=9994,C2=1.0513+1.5680×10-5A,r=0.9999C3=1.2260-1.4684×10-5A,r=0.9999三者分别在7.60~38.0μg·mL-1、1.75~8.75μg·mL-1、2.4~12.OOμg·mL-1范围内呈线性关系。平均回收率和RSD分别为98.02%、96.63%、97.05%和1.78%、1.20%、1.15%。该方法操作简便,测定结果准确可靠,可用于测定洁康舒洗剂中大黄酸、大黄素和大黄酚的含量。     

金属—PAN—S配合物的极谱研究——Ⅱ:Fe~(3+)—PAN—S—TEA—NH_3·H_2O—NH_4Cl体系配合吸附波

在NH_3·H_2O—NH_4Cl—三乙醇胺底液中Fe(Ⅲ)与PAN—S产生一灵敏的配合吸附波,峰电位在—0.50伏(vs.SCE)。峰电位与铁离子浓度在2.8×10~8～3.4×10~(-6)mol/L范围内线性良好,检出下限可达2.8×10~(-8)mol/L。该法用于乳粉、头发、血清等样品的测定,结果满意。     

微量镁的Mg~(2+)—BPR—CTMAB分光光度法测定

本文研究了Mg~(2+)—溴邻苯三酚红(BPR)—溴化十六烷基三甲基氯化铵(CTMAB)的显色反应,探讨了Mg2+—BPR—CTMAB体系的最佳测定条件。实验表明Mg~(2+)—BPR—CTMAB体系的最佳pH=9—10,λ_(max)=680nm,ε=1.3×10~4L·mol~(-1)·cm~(-1),镁量在0—80μg/50mL内符合比尔定律,该法用于测定铝合金中镁获得满意的结果。     

火焰原子吸收光谱法测定孕多维胶囊中钙、铁和锌的含量

用火焰原子吸收光谱法测定孕多维胶囊中钙,铁和锌的含量。结果表明,钙在8～16μg·mL~(-1)浓度范围,锌在0.5～3.5μg·ml~(-1)浓度范围,铁在3～11μg·mL~(-1)浓度范围内呈线性。钙,铁和锌的平均回收率分别为99.3％(RSD=0.93％),102.2％(RSD=0.57％)和100.6％(RSD=1.18％)。该方法快速、灵敏、准确,样品处理简便易行,可用于药品的质量控制。     

等度高效液相色谱测定大豆异黄酮中大豆甙元和金雀异黄酮

本文介绍了等度高效液相色谱(HPLC)测定大豆异黄酮中二种主要成份:大豆甙元(Daidzein)和金雀异黄酮(Genistein)的方法。采用Atlantis C18色谱柱和EasyGuard C18,保护柱;以甲醇:0·1%醋酸(pH3·11)=51·5:48·5(v/v)为流动相;检测波长λ=254nm;流速1mL/min。在测定范围内(10-200ng)峰面积与质量浓度线性关系良好。大豆甙元和金雀异黄酮的相关系数分别为0·9984,0·9997·两组份回收率为97·0—102·92%·     

Triton X-100-5-Br-PADAP分光光度法选择性测定乳粉中微量铁

报道了以2-(5-溴-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂,应用分光光度法高选择性测定铁(Ⅲ)的新方法。实验结果表明,在pH4.0的乙醇介质中和Triton X—100、盐酸羟氨存在下,以746nm为测定波长,可选择性测定铁(Ⅲ)含量。本法线性范围为0～1.3μg/ml,表观摩尔吸收系数为2.94×10~4L·mol~(-1)·cm~(-1),批内和批间精密度cv%分别为1.2%、2.3%,平均回收率为98.9%。已用于乳粉中微量铁的直接测定,常见共存成分对测定无干扰。     

微分脉冲极谱法测定饮料的总酸量

本文采用微分脉冲极谱法于浓度为0.5mol·L~(-1)的KCl底液,5.84×10~(-4)mol·L~(-1)的柠檬酸标准液,pH为5.65,CdCO_3粉末加入量为0.2g,通N_27min的条件下测定饮料中的总酸量。本法的线性方程为y=9.0288x+0.4192,线性浓度范围1.2×10~(-5)～8.4×10~(-5)mol/L,相关系数R=0.9995,标准偏差为0.142,测定结果与中和滴定法和电位滴定法对比,表明微分脉冲极谱法可以简单、快速、准确测定饮料中的总酸量。     

反相高效液相色谱法测定肾康口服液中黄柏的小檗碱含量

建立反相高效液相色谱法测定肾康口服液中黄柏的小檗碱含量。采用反相高效液相色谱法,Novapak C18柱(3.9×150mm,5μm)流动相为甲醇一乙腈(0.05mol·L-1)-磷酸二氢钠溶液(20∶3S∶45),流速为1.0mL·min-1,检测波长为346nm。小檗碱的回归方程为C=1.2616+1821X10-6A,r=0.9992,在4.00~20.00μg·mL-1范围内呈线性关系。平均回收率和RSD分别为101.32%和1.18%(n=5)。方法操作简便,测定结果准确可靠,可用于测定肾康口服液中黄柏的小檗碱含量。     

Development of P/M Fe–P soft magnetic materials

Phosphorous is treated as an impurity in conventional steels owing to segregation of phosphorous and formation of brittle phosphides along the grain boundaries. It is responsible for cold and hot shortness in wrought steels. In conventional powder metallurgy, involving compaction and sintering, high phosphorous content (up to 0·7%) in Fe-based alloys exhibit attractive set of mechanical and magnetic properties. These powder-processed alloys suffer from increasing volumetric shrinkage during sintering as phosphorous is increased beyond 0·6%. Thus both cast as well as conventional powder metallurgy routes have their own limitations in dealing with iron?Cphosphorous alloys. Hot-powder forging was used in the present investigation for the development of high-density soft magnetic materials containing 0·3?C0·8% phosphorous to overcome these difficulties. It was observed that phosphorous addition improves the final density of the resulting product. It was further observed that hot-forged iron?Cphosphorous alloys have excellent hot/cold workability and could be easily shaped to thin strips (0·5?C1·0?mm thick) and wires (0·5?C1·0?mm diameter). The powder hot-forged alloys were characterized in terms of microstructure, porosity content/densification, hardness, soft magnetic properties and electrical resistivity. Magnetic properties such as coercivity 0·35?C1·24?Oe, saturation magnetization 14145?C17490 G and retentivity 6402?C10836 G were observed. The obtained results were discussed based on the microstructures evolved.     

Mössbauer and XRD studies on the effect of doping iron in KCaY(PO4)2

The effect of doping iron at the yttrium site in hexagonal KCaY(PO₄)₂ is studied for various concentrations ofx (0≤x≤1), of iron using Mössbauer and X-ray diffraction methods. For low iron concentrations, very little changes in structure are seen but atx≈0·1, onset of new peaks in the XRD pattern is observed. The Mössbauer study of the doped samples reveals that iron has a solubility of up to 2·5% in the parent phase with any excess iron precipitating out to form a new and unknown phase. From a detailed analysis of the X-ray diffraction pattern (corresponding tox=1) of the latter phase, it is found that this phase is rhombohedral with the possible space groupR3.     

Iron-substituted AB5-type MH electrode

The present investigation is aimed to study MmNi₅-type (Mm = Mischmetal) hydrogen storage alloys with composition, Mm_0·8La_0·2Ni_3·7Al_0·38Co_0·3Mn_0·6?x Mo_0·02Fe _x (x = 0, 0·1, 0·2 and 0·3). The alloys are synthesized by radio-frequency induction melting. To study their electrochemical properties via measurements of discharge capacity, activation process, rate capability and cyclic stability, electrodes are fabricated using as-synthesized and annealed version of the alloys. The maximum discharge capacity is recorded as 288 mAhg^?1 for the iron concentration, x = 0·1, as compared to 270 mAhg^?1 for the alloy electrode without iron. Similarly, 99% cyclic stability is observed in annealed alloy electrode (x = 0·1) as compared to 78% in the alloy electrode without iron. Hence, small amount of iron-substitution (x = 0·1) in the alloy is found to improve the electrochemical properties. This improvement is thought to be due to less pulverization of the alloy in electrochemically-cycled alloy, as confirmed through structural and microstructural characterizations carried out by X-ray diffraction phase analysis and scanning electron microscopy of as-fabricated and electrochemically-cycled electrodes.     

Mechanomaking of nanostructured hypereutectic white irons: powder fabrication

Abstract

White irons containing 5·7 wt-%C were produced by room temperature, high energy milling from iron and carbon elemental powders. Both iron and cementite phases have crystal sizes of less than 10 nm in the powders which have fully dense particles of 50 μm mean size. The gas content is 0·5 wt-% and the powder is stable up to 550°C. Above 550°C decomposition of cementite occurs, involving a decrease in combined carbon content from 5·7 to 3·5 wt-% (annealing at 1050°C). The crystal growth kinetics has two temperature regions with lower activation energies in the high temperature (above 800°C) region. Crystal sizes still below 100 nm were observed for annealing up to 800°C. The size distribution in mechanosynthesised powders was modified by tumbling (dry) and attritor (wet) milling down to mean sizes of 4 μm and 1·4 μm respectively. Whereas tumbling milling does not alter the properties of MS powders, wet attritor milling produced higher gas content (7 wt-%) and much decreased thermal stability. Mechanosynthesised and tumbling milled powders can be degassed prior to consolidation, while wet attritor milled ones cannot.     

Selective flocculation of iron oxide-kaolin mixtures using a modified polyacrylamide flocculant

High molecular weight polyacrylamides were synthesized and successfully modified to contain up to 8·3% hydroxamate functional groups. The selective flocculation tests carried out on 1:1 iron oxide/kaolin mixtures using parent polyacrylamide, polyacrylic acid and the modified polyacrylamide, confirm the possibility of enhancing selectivity through introduction of iron chelating functional groups in commercially available polymers. Starting with a feed grade of 35% iron, 92% recovery with acceptable grade of 60% iron has been achieved using the modified polyacrylamide. NCL communication No. 4415     

Superplasticity of Fe3Al(Cr)

Abstract

The superplasticity of an Fe₃Al based intermetallic alloy with 3 at.-% chromium has been investigated in the strain rate range 10^-5-10^-2 s^-1 at test temperatures between 700 and 900°C. The composition of the iron aluminide was Fe–28Al–3Cr (at.-%) with additions of titanium and carbon. After thermomechanical processing the material possessed a coarse grained microstructure with an average grain size of 55 ± 10 μm. Strain rate exponents of 0·33≤m≤0.42 were recorded at strain rates of approximately 10^-5-10^-3 s^-1 in the temperature range 750-900°C. Superplastic elongations of 350% and more were achieved. From thermal activation analysis of superplastic flow, an activation energy of 185 ± 10 kJ mol^-1 was derived. This value is comparable to activation energies of superplastic flow in Fe₃Al(Ti) alloys. However, in unalloyed Fe₃Al the activation energy is higher, ~ 263 kJ mol^-1. Optical microscopy showed grain refinement to ~ 30 ± 5 μm in size in superplastically strained tensile specimens. Transmission electron microscopy gave evidence of the formation of subgrains of 0·3–0·5 μm in size. Superplasticity in this iron aluminide is mainly attributed to viscous dislocation glide, controlled by solute drag in the transformed B2 lattice at the deformation temperatures. During superplastic deformation, subgrain formation and grain refinement in the gauge length were revealed. From this it is concluded that dynamic recrystallisation makes an important contribution to the deformation mechanism of superplastic flow in this material.     

Effect of cerium sulphide particle dispersions on acicular ferrite microstructure development in steels

Abstract

Of the phases found in wrought steels, cerium sulphide particles are notable in that they can be both stable at liquid metal temperatures and exhibit good lattice coherency with α iron. An investigation has been carried out to determine the effectiveness of cerium sulphide particle dispersions in nucleating intragranular acicular ferrite microstructures in steels. Vacuum melts of 50 kg have been manufactured of appropriate base steel compositions with varying additions of cerium (0·04–0·18%) and sulphur (0·01–0·04%). The work has shown that 0·02–0·12% cerium and 70–340 ppm sulphur may be retained in steels after deoxidation and desulphurisation reactions while oxygen can be reduced to <20 ppm. Resulting inclusions are largely spheroidal in shape and consist of several crystalline compounds, notably CeS, Ce₃S₄ and Ce₂O₂S. The inclusion numbers are of the order of 0·68–6·12 × 10⁶ mm^?3 with mean diameters of 0·63–1·70 μm. The densities of these inclusion dispersions are approaching those in weld metals where acicular ferrite is the dominant microstructure constituent. Significant volume fractions of acicular ferrite (up to 65%) have been obtained in steels after thermally cycling in a dilatometer and cooling at rates simulating transformation conditions ranging from high heat input welding to air cooling of forgings and water cooling of plate. A potential beneficial effect of acicular ferrite on mechanical properties in high heat input welding (heat affected zone grain refinement) and in thermo-mechanically processed steels (relaxed schedules) has been highlighted. A pilot plant billet cast of steel has shown the feasibility of achieving the required particle dispersions and acicular ferrite microstructure in tonnage steelmaking.     

Modifying high Cr–Mn cast iron with boron and rare earth–Si alloy

Abstract

By modifying 13Cr–4Mn (wt-%) white cast iron with boron and rare earth (RE)–Si complex, the carbide morphology of the iron can be changed from interconnected, coarse clusters of rods into a parallel distribution of isolated, fine rods, and the impact toughness of the iron can reach 6–7 × 10⁴ J m^?2. In a pin wear test, the relative abrasion resistance of the iron is 1·01 and in a repeated impact abrasive wear test it is 0·95, in comparison with 15Cr–3Mo cast iron. Thus, it is stated that modifying high Cr–Mn cast iron with boron and RE–Si complex is very cost effective, and has almost the same abrasion resistance, when compared with 15Cr–3Mo cast iron.

MST/957