3-硝基偶氮氟膦与铬的褪色反应及其应用

报道了新显色剂3一硝基偶氮氟膦（偶氮氟膦-mN）的合成及与铬（Ⅶ的褪色反应，并将其应用于铬的形态分析。在硝酸介质中，于85℃热水浴中加热8min，铬（Ⅷ可使偶氮氟膦-mN显著褪色，且试剂空白与褪色溶液在528nIyl处的吸光度差与0．006～0．2μg／mL范围内的铬（Ⅷ符合比尔定律，表观摩尔吸光系数e为1．87×10^5L·mol^-l·cm^-1，方法检出限为1．5×10^-3μg／mL。应用该显色体系可直接测定样品中铬（Ⅶ含量，同时加入过硫酸铵将铬（Ⅲ）氧化成铬（Ⅷ，再进行测定可得总铬的含量，两者之差即为铬（Ⅲ）含量。该显色体系用于测定多种比例的铬（Ⅷ和铬（Ⅲ）混合标准溶液中铬（Ⅷ和铬（Ⅲ）的测定，测定值均与理论值一致。该显色体系应用于电镀厂及钢铁厂的工业废液显色体系中铬（Ⅷ的测定，结果的相对标准偏差（RSD，n=5）为2．2％～3．4％，加标回收率为98％～1O3％，测定结果与二苯碳酰二肼光度法测定值一致。

铬黑T-溴酸钠催化动力学分光光度法测定铼

基于在硫酸介质中,铼催化溴酸钠氧化铬黑T的褪色反应,建立了测定铼的光度分析新方法。确定了催化体系的动力学条件,计算得出催化反应的表观活化能Ea=39.12KJ/mol,反应速率常数为K=1.248×10-3/s。在选定的试验优条件下,铼的浓度在0-10.02mg/L范围内与相对吸光度呈良好的线性关系,检出限为2.7675mg/L。方法所用仪器简单,操作简便。

溴酸钾氧化铬天青S催化光度法测香肠中痕量亚硝酸盐

在H2 SO4介质中，亚硝酸盐对KBrO3氧化铬天青S 褪色反应有催化作用，基于此建立了催化光度法测定亚硝酸盐的新方法。讨论了 H2 SO4用量、铬天青S 用量、KBrO3用量、加热温度及反应时间的影响，确立了最佳反应条件。在选择的条件下，该方法的线性范围为0．04～1．35 mg/L，检出限为6．6＆#215;10-3 mg/L。该方法用于香肠中亚硝酸盐的测定，结果满意。

Anesthesia Management in Hereditary Pheochromocytoma and Paraganglioma:Updated Insights into Clinical Features and Perioperative Care

Approximately 40%of pheochromocytoma and paraganglioma(PPGL)cases are familial,typically presenting earlier with more complex symptoms.This paper synthesizes literature and guidelines to inform on clinical characteristics and perioperative care for PPGL.Pheochromocytoma in von Hippel-Lindau(VHL)disease exhibits heightened secretion activity without significant perioperative hemodynamic changes.Tumors in multiple endocrine neoplasia type 2(MEN2)have a stronger endocrine function,which may induce hemodynamic fluctuations during surgery Therefore,pheochromocytoma screening is essential at all stages of MEN2.Neurofibromatosis type 1(NF1)often presents multisystem lesions and can result in dificult airway.Pheochromocytoma should be evaluated when NF1 patients present hypertension.Pheochromocytoma and paraganglioma type 5 may present multiple lesions of pheochromocytoma or paraganglioma.In summary,hereditary PPGLs may present with severe lesions in other systems,beyond tumor function.A multi-disciplinary team(MDT)approach is often invaluable in perioperative management.

Research and prospect on extraction of vanadium from vanadium slag by liquid oxidation technologies

A series of innovative green metallurgical processes using novel reaction media including the NaOH/KOH sub-molten salt media and the NaOH-NaNO3 binary molten salt medium, for the extraction of vanadium and chromium from the vanadium slag have been developed. In comparison with the traditional sodium salt roasting technology, which operates at 850 ℃, the operation temperatures of these new processes drop to 200-400 ℃. Further, the extraction rates of vanadium and chromium utilizing the new approaches could reach 95% and 90%, respectively, significantly higher than those in the traditional roasting process, which are 75% and approximate zero, respectively. Besides, no hazardous gases and toxic tailings are discharged during the extraction process. Compared with the conventional roasting method, these new technologies show obvious advantages in terms of energy, environments, and the mineral resource utilization efficiency, providing an attractive alternative for the green technology upgrade of the vanadium production industries.

Behaviors of vanadium and chromium in coal-based direct reduction of high-chromium vanadium-bearing titanomagnetite concentrates followed by magnetic separation

The reduction behaviors of FeO·V2O3 and FeO·Cr2O3 during coal-based direct reduction have a decisive impact on the efficient utilization of high-chromium vanadium-bearing titanomagnetite concentrates. The effects of molar ratio of C to Fe n(C)/n(Fe) and temperature on the behaviors of vanadium and chromium during direct reduction and magnetic separation were investigated. The reduced samples were characterized by X-ray diffraction(XRD), scanning election microscopy(SEM) and energy dispersive spectrometry(EDS) techniques. Experimental results indicate that the recoveries of vanadium and chromium rapidly increase from 10.0% and 9.6% to 45.3% and 74.3%, respectively, as the n(C)/n(Fe) increases from 0.8 to 1.4. At n(C)/n(Fe) of 0.8, the recoveries of vanadium and chromium are always lower than 10.0% in the whole temperature range of 1100-1250 °C. However, at n(C)/n(Fe) of 1.2, the recoveries of vanadium and chromium considerably increase from 17.8% and 33.8% to 42.4% and 76.0%, respectively, as the temperature increases from 1100 °C to 1250 °C. At n(C)/n(Fe) lower than 0.8, most of the FeO·V2O3 and FeO·Cr2O3 are not reduced to carbides because of the lack of carbonaceous reductants, and the temperature has little effect on the reduction behaviors of FeO·V2O3 and FeO·Cr2O3, resulting in very low recoveries of vanadium and chromium during magnetic separation. However, at higher n(C)/n(Fe), the reduction rates of FeO·V2O3 and FeO·Cr2O3 increase significatly because of the excess amount of carbonaceous reductants. Moreover, higher temperatures largely induce the reduction of FeO·V2O3 and FeO·Cr2O3 to carbides. The newly formed carbides are then dissolved in the γ(FCC) phase, and recovered accompanied with the metallic iron during magnetic separation.

Fretting wear and friction oxidation behavior of 0Cr20Ni32AlTi alloy at high temperature

The fretting wear behavior of 0Cr20Ni32AlTi alloy was investigated with crossed cylinder contact under 80 N at 300 and 400 °C.Wear scar and debris were analyzed systematically by scanning electron microscopy and X-ray photoelectron spectroscopy.The results show that the friction logs are mixed fretting regime and gross slip regime with the magnitudes of displacement of 10 and 20 μm,respectively.Severe wear and friction oxidation occur on the material surface.A large number of granular debris produced in the fretting process can be easily congregated and adhered at the contact zone after repeated crushes.The resultant of friction oxidation is mainly composed of Fe3O4,Fe2O3,Cr2O3 and NiO.Temperature and friction are the major factors affecting the oxidation reaction rate.The fretting friction effect can enhance the oxidation reaction activity of surface atoms of 0Cr20Ni32AlTi alloy and reduce the oxidation activation energy.As result,the oxidation reaction rate is accelerated.

Migration and transfer of chromium in soil-vegetable system and associated health risks in vicinity of ferro-alloy manufactory

Study was carried out to analyze the distribution and migration patterns,soil-to-plant transfer and potential health risks of chromium in soil-vegetable system in areas near a ferro-alloy manufactory in Hunan province.The results show that soils near sewer outlet,sewer channel and in control area are averaged 2 239.5,995.33 and 104.9 mg/kg,respectively.The total Cr has a relative accumulation in soil depth of 200-400 mm near the sewer outlet,mainly enriches in the surface layer（0-200 mm） near the sewer channel and decreases gradually in unpolluted soils.The differential concentration level of enrichment between layers is little.The results also indicate that the three vegetables of celery,lettuce and Chinese cabbage are able to convert the potentially toxic Cr（Ⅵ） species into the non-toxic Cr（Ⅲ） species,and the chromium contents in the edible parts of the vegetables are averaged 11.95 mg/kg.The transfer factors of the three vegetables follow the order：Chinese cabbage lettuce celery.The estimated total daily intake of chromium substantially exceeds the dietary allowable value,which may pose health risks to local population.

膨化食品中铝含量的测定与研究

用铬天青-S分光光度法测定膨化食品中的铝含量,利用三价铝离子在乙二胺-盐酸缓冲溶液中与铬天青-S及溴化十六烷基三甲基铵反应生成绿色三元络合物在610nm处测其吸光度,利用标准曲线方程计算出其含量.结果发现:样品中87.5%符合标准,品牌膨化食品铝含量较低,不合格产品为散装的膨化食品.

Absorption capacity of major urban afforestation species in north-eastern China to heavy metal pollutants in the atmosphere

Totally 24 arbor tree species and 6 shrub species were measured on their absorption capacities to heavy metal Pb, Cd, Cr, and Hg by collecting and analyzing the leaves of trees along different streets in Harbin city in Sept. to Oct. of 2003. The results showed that all the measured species had certain absorbency to the pollutants (Pb, Cd, Cr and Hg), but there existed significant difference in absorption capacity for different species to different pollutants. The measured tree species were classified into three categories by their absorption quantum of heavy metal pollutants. Among the species measured,Betula platyphylla, Ulmus pumila var.pendula, andPrunus persicaf.rubro-plena had high capacity in absorbing Pb;Populus xiahei, P. nigra var.Italica, P. alba x P. berolinensis andSalix matsudana had had high capacity in absorbing Cd;Phellodendron amurense, Syringa oblata, Salix matsudana, Pinus tabulaeformis var.mukdensis, Picea koraiensis, Prunus persica f.rubro-plena, P. triloba andAcer negundo, etc. had high capacity in absorption of Cr;Prunus triloba, Quercus mongolica, Salix matsudana, Sambucus williamsii, Pyrus ussuuriensis andSpiraea fritschiana were good at absorption of Hg. This study might offer scientific foundation for selection of urban afforestation species in different polluted conditions caused by heavy metals. Keywords Greening tree species - Heavy metal - Pollutants - Plumbum - Cadmium - Chromium - Mercury - Absorptivity CLC number S731.2 - X501 Document code A Foundation item: This study is financially supported by the Special Programme for Agriculture under Ministry of Chinese Science and Technology (No. 2002BA516A15-01).Biography: MU Li-qiang (1966-), female, Associate professor in Northeast Forestry University, Harbin 150040, P. R. China.Responsible editor: Zhu Hong

Electron beam welding of 304 stainless steel to QCr0.8 copper alloy with copper filler wire

Electron beam welding （EBW） of 304 stainless steel to QCr0.8 copper alloy with copper filler wire was carried out. Orthogonal experiment was performed to investigate the effects of process parameters on the tensile strength of the joints, and the process parameters were optimized. The optimum process parameters are as follows：beam current of 30 mA, welding speed of 100 mm/min, wire feed rate of 1 m/min and beam offset of-0.3 mm. The microstructures of the optimum joint were studied. The results indicate that the weld is mainly composed of dendriticαphase with little globularεphase, and copper inhomogeneity only occurs at the top of the fusion zone. In addition, a melted region without mixing exists near the weld junction of copper side. This region with a coarser grain size is the weakest section of the joints. It is found that the microhardness of the weld decreases with the increase of the copper content in solid solution. The highest tensile strength of the joint is 276 MPa.

Phosphate film free of chromate, fluoride and nitrite on AZ31 magnesium alloy and its corrosion resistance

A phosphate solution free of chromate, fluoride and nitrite was prepared and an environment-friendly film was obtained on AZ31 magnesium alloy surface via the chemical deposition method. The morphology, composition, phase structure and its corrosion resistance were studied. The effects of film-forming temperature and free acid on corrosion resistance, microstructure and electrochemical behavior of the film were discussed. The results indicate that the corrosion resistance of AZ31 with the phosphate film was better than blank AZ31 substrate, which was most attributed to the great inhibitive action on the anodic dissolution and cathodic hydrogen evolution of the film.

Determination of Chromium and Zinc in Soil by Microwave Digestion and Flame Atomic Absorption Spectrometry

[Objective] The aim was to develop a rapid, simple method for determination of chromium and zinc in soil samples by flame atomic absorption spectrometry.[Method] The method for determination of Cr and Zn in soil by combined flame atomic absorption spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-0.8 mg/L for Cr and 0-0.8 mg/L for Zn, the detection limits of Cr and Zn was 0.0025 mg/L and 0.002 3 mg/L, respectively. Recoveries of 102.4%-103.2% for Cr and 97.7%-98.3% for Zn were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of Cr and Zn in soil samples.

Preparation of potassium chromate by roasting of carbon ferrochrome

The oxidizing roasting process of carbon ferrochrome to prepare potassium chromate in the presence of potassium carbonate and air was investigated. The effects of reaction temperature, reaction time, mole ratio of potassium carbonate to carbon ferrochrome were studied, and thermodynamics and kinetics were also discussed. It was observed that the reaction temperature and reaction time had a significant influence on the roasting reaction of carbon ferrochrome. The reaction mechanism changed greatly as the temperature varied. A two-stage roasting process was favorable for the roasting reaction, and a chromium recovery rate of 97.06% was obtained through this two-stage roasting method. The chromium residue yielded from this method was only 1/3 of the product. Moreover, the component of Fe in the residue was as high as 55.04%. Therefore, it can be easily recovered to produce sponge iron, realizing complete detoxication and zero-emission of chromium residue.

Preparation of UV-visible light responsive photocatalyst from titania-bearing blast furnace slag modified with(NH_4)_2SO_4

Sulfate-modified titanium dioxide-bearing blast furnace slag（STBBFS） photocatalysts were prepared by the high energy ball milling method with（NH4）2SO4 and titanium dioxide-bearing blast furnace slag（TBBFS） as raw materials.X-ray photoelectron spectroscopy（XPS）,X-ray diffraction（XRD）,scanning electron microscopy（SEM）,thermogravimetric analysis（TGA）,UV-visible diffuse reflectance absorption spectra（UV-Vis）,adsorption experiment and photocatalytic degradation measurement were conducted to characterize the structure,surface status,light absorption capacity,adsorption capacity and photocatalytic activity of the obtained photocatalysts.The adsorption equilibrium was described by the Langmuir isotherm model with a maximum adsorption capacity of 8.25 mg/g of Cr（VI） ions onto the STBBFS photocatalysts.As a result,sulfation of TBBFS improved the photocatalytic activities of STBBFSx photocatalysts.At a low calcination temperature,the photocatalytic activity of STBBFS300 photocatalyst was markedly higher compared with TBBFSx prepared at high calcination temperature,indicating that the photocatalytic activity of STBBFSx photocatalyst was determined by the balanced result between adsorption capacity and perovskite content.

Effect of standard heat treatment on microstructure and properties of borided Inconel 718

Boronizing was applied to Inconel 718. In order to obtain the optimal combination of strength and ductility, the borided Inconel 718 was subjected to standard heat treatment. This consists of solution treatment and then a two-step aging treatment. The borided layer is composed of the compound layer and the boron diffusion zone. Because of the superior hardness of borides, the borided Inconel 718 exhibits a significant reduction in its wear rate and relatively low coefficient of friction （COF） compared with the unborided Inconel 718. The standard heat treatment efficiently promotes the diffusion of boron into the interior of the material and the generation of new borides （Fe2B, CrB）. The borided layer with standard heat treatment shows much better wear resistance due to the thicker borided layer （313.76 μm）.

Crystallization behaviors of bayerite from sodium chromate alkali solutions

In order to clean production of chromium compounds, it is a critical process to remove aluminates and utilize aluminum compounds from artificial chromate alkali solutions. The effects of Na2 Cr O4 on the neutralization curve, Al（OH）3 precipitation efficiency and induction period of bayerite were investigated. The results indicate that the neutralization curve of the artificial chromate alkali solutions shows three distinct regions and its induction period is longer than that of pure sodium aluminate solutions at the same aluminum concentration. And the decreased temperature and volume fraction of CO2 enhance the particle size of bayerite β-Al（OH）3. Bayerite composed of agglomerates of rods and cone frustums was obtained from alkali metal chromate solutions with 28.5% CO2（volume fraction） at temperatures ranging from 50 °C to 70 °C. Coarse bayerite with particle size（d50） from 24.2 μm to 29.3 μm extremely has few impurities, which is suitable for comprehensive utilization.

Dechromization and dealumination kinetics in process of Na_2CO_3-roasting pretreatment of laterite ores

A novel process was proposed for the activation pretreatment of limonitic laterite ores by Na2CO3 roasting. Dechromization and dealumination kinetics of the laterite ores and the effect of particle size, Na2CO3-ore mass ratio, and roasting temperature on Cr and Al extraction were studied. Experimental results indicate that the extraction rates of Cr and Al are up to 99%and 82%, respectively, under the optimal particle size of 44–74μm, Na2CO3-to-ore mass ratio of 0.6：1, and temperature of 1000 ℃. Dechromization within the range of 600–800 oC is controlled by the diffusion through the product layer with an apparent activation energy of 3.9 kJ/mol, and that it is controlled by the chemical reaction at the surface within the range of 900–1100 ℃ with an apparent activation energy of 54.3 kJ/mol. Besides, the Avrami diffusion controlled model with on apparent activation energy of 16.4 kJ/mol is most applicable for dealumination. Furthermore, 96.8%Ni and 95.6%Co could be extracted from the alkali-roasting residues in the subsequent pressure acid leaching process.

Cyclic oxidation and hot corrosion of Al_2O_3 or Y_2O_3-dispersed low-temperature chromizing coating

Chromium coatings with and without Al_2O_3 or Y_2O_3 particles were prepared by chromizing the as-deposited Ni-film with and without Al_2O_3 or Y_2O_3 particles using a conventional pack-cementation method at 800 ℃. The cyclic oxidation at 800 ℃ and hot corrosion in molten 75% Na2SO4＋25% NaC1 at 800 ℃ of the three different chromizing coatings were investigated. The effects of Al_2O_3 or Y_2O_3 on the cyclic oxidation and hot corrosion behavior of the chromizing coatings were discussed. Microstructure results show that the codeposited Al_2O_3 or Y_2O_3 particles significantly retard the grain growth of the chromizing coating, which increases the cyclic oxidation and hot corrosion resistance of the chromizing coatings, due to the more rapid formation of purer and denser chromia scnle

Effect of different fillers on oxidation behavior of low-temperature chromizing coating

Three different chromizing coatings were produced on Ni substrate using a conventional pack-cementation method with Al2O3,Al2O3＋CeO2 and CeO2 acting as filler,respectively,at a greatly decreased temperature（700 ℃）.Effects of different fillers on the isothermal and cyclic oxidation resistance of chromizing coating in air at 850 ℃ were comparably investigated.Microstructure results show that the addition of CeO2 into the filler significantly retards the grain growth of the chromizing coating.Oxidation results indicate that the chromizing coating using CeO2 as filler exhibits somewhat increased oxidation resistance than the normal chromizmg coating,while the chromizing coating using Al2O3＋CeO2 as filler exhibits much better oxidation resistance.The effects of different fillers on the oxidation behaviors were discussed in detail.