用二-2-乙基己基磷酸从盐酸溶液中萃取Th(Ⅳ)

用二-2-乙基己基磷酸(HDEHP)做萃取剂,Na2CO3做反萃剂,234Th为示踪剂,完成了从盐酸溶液中液-液萃取Th(IV)的实验研究。在不同萃取条件下(包括HDEHP和Na2CO3溶液浓度、震荡时间、有机相和水相比值等)对234Th百分萃取(或反萃取)作了一系列实验。发现,随HDEHP浓度的增加,234Th的萃取效率明显增加。当HDEHP的浓度≥20%时,234Th的萃取效率>97%;用Na2CO3溶液能有效地从有机相中反萃出234Th,当Na2CO3溶液的浓度≥0.5mol/L时,234Th的反萃效率>96%;反萃时,震荡周期长于4min时,两相能达到反萃平衡;随有机相和水相比值的增加,234Th的萃取效率也明显地增加,在合适的萃取条件下,有机相与水相比值≥4:1时,高达97%的234Th进入有机相。

用二-2-乙基己基磷酸和P_2O_5混合物从硝酸溶液中萃取Am(Ⅲ)

用二-2-乙基己基磷酸(HDEHP)和P2O5混合物做萃取剂,241Am3+为示踪剂,做了从硝酸溶液中液-液萃取Am的实验研究。完成了硝酸浓度和震荡时间的变化影响241Am3+萃取效率的条件实验。发现P2O5的浓度≥0.0125mol/L时,241Am3+的萃取效率大于98%;震荡时间≥30s,两相便可达到萃取平衡。分别用二乙撑三胺五乙酸(DTPA)-乳酸以及Na2CO3溶液对241Am3+进行反萃取。结果显示Na2CO3溶液能给出很高的反萃效率。而且,在很短的震荡时间内,两相都能达到反萃平衡。

Novel catalysis of TiO2 for the catalytic alcohols synthesis from CO and H2O

Direct synthesis of alcohols from CO and H2O was investigated using TiO2 catalyst. MeOH (about 24 mg g(-1) h(-1)) and EtOH (about 8 mg g(-1) h(-1)) could be produced under the reaction conditions of T= 573 K, P= 0.5 MPa, CO flow rate of 30 ml min(-1) and CO/H2O = 3/2 during the period of 12 to 44 h time-on-stream. Compared with PbO, TiO2 could preserve stable catalytic activity during a long time of reaction. For the same catalyst TiO2, the reaction performance of alkali carbonates increased with their solubility (K2CO3>Na2CO3>Li2CO3). The corresponding catalytic activity was found to increase with the alkalescence of solvent. The formation mechanism of alcohols was proposed as well. (C) 2004 Elsevier B.V. All rights reserved.

分光光度法测定蒙古栎叶中多酚的含量

以没食子酸为标准品,使用福林酚试剂(FC),通过分光光度法,对蒙古栎树叶中植物多酚含量进行了测定.首先从方法的稳定性、线性关系、精确性和准确性角度,对FC法进行了调整,确定了以没食子酸为标准的最佳反应条件.结果表明,最佳反应条件为0.15mL FC试剂(1mol/L),0.15mL 10%体积分数的Na2CO3,25℃反应80min后于760nm处测吸光值.使用调整后的方法测得结果为:蒙古栎叶中总酚含量为6.39%,RSD为1.90%.方法操作简单,结果重现性好,可用来测定蒙古栎叶中总酚的含量.

The study on a PVC membrane electrode for gemfibrozil

In this paper, a poly(vinyl chloride) (PVC) membrane electrode is prepared for gemfibrozil, 2, 2-dimethyl-5(2,5-xylyloxy) valeric acid, based on its ion pair complexes with hexadecyltrioctyl ammonium iodide (HTOA). The membrane composition of the electrode was optimized by using the sequential level elimination method for orthogonal experimental design. The electrode has a Nernstian response range from 2.5 X 10(-5) to 0.1 mol/l with an average slope of 55.3 mV/decade. The limit of detection is 7.1 X 10(-6) mol/l. The electrode responses were not affected by pH in the range 10.0-12.3. A Na2B4O7-Na2CO3 buffer of pH = 11.0 was selected as the background electrolyte solution for potentiometric measurements. The electrode was used for determining gemfibrozil in pharmaceutical preparations with satisfactory results.

复合厌氧工艺处理生活污水的快速启动研究

采用两段式UASB+AF复合厌氧反应器处理生活污水,着重研究了其快速启动的条件。结果表明,水解酸化段无需调节pH,运行20 d后对COD的去除率即可达60%左右且保持稳定;甲烷化段受pH的影响较大,利用Na2CO3和NaHCO3的混合液调节该段进水的pH值在6.8~7.2之间,6 d后对COD的去除率即可稳定地保持在30%左右。启动期内,温度对水解酸化段的影响不大,但显著影响甲烷化段,在试验条件下,甲烷化反应的最佳温度为30℃;在水解酸化段不设混合液回流、甲烷化段设置混合液回流的条件下,最佳的回流方式为:间隔2 h回流10 s。采取上述优化措施后,系统的启动时间可缩短到30 d以内,仅为常规厌氧工艺启动时间(3~6个月)的1/3~1/6,反应器的运行效率得到了大幅度提高。

Spectra and long-lasting properties of Sm3+-doped yttrium oxysulfide phosphor

We reported, for the first time to the best of our knowledge, the Sm3+ -doped yttriurn oxysulfide phosphors has reddish orange long-lasting phosphorescence. The phosphor show prominent luminescence in reddish orange due to the electronic transitions of (4)G(5/2) --> H-6(J) (J = 5/2, 7/2, 9/2), the afterglow color of this type of phosphors is a mixture of the three above mentioned electronic transition emissions and have a little different when the concentration of the Sm3+ dopant changes. Synthesis procedure of the Sm3+-yttrium oxysulfide reddish orange phosphor through the flux fusion method with binary flux compositions was presented. The synthesized phosphors were analyzed using X-ray diffraction (XRD) to interpret the structural characterization. The XRD analysis result reveal that the Y2O2S:Sm3+ phosphor synthesized with a binary flux composition containing (S and Na2CO3 at a ratio of 1: 1 at 30 wt.% of total raw material) at 1050degreesC for 3 h was in single-phase. Luminescence properties of the Y2O2S:Sm3+ long-lasting phosphor was analyzed by measuring the excitation spectra, emission spectra and afterglow decay curve. The mechanism of the strong afterglow from Y2O2S:Sm3+ was also discussed in this paper.

Extraction and separation of cerium(IV) from nitric acid solutions containing thorium(IV) and rare earths(III) by DEHEHP

The extraction behaviour of Ce(IV), Th(IV) and part of RE(III), viz., La, Ce, Nd and Yb, has been investigated using di(2-ethylhexyl) 2-ethylhexyl phosphonate (DEHEHP,B) in heptane as an extractant. Results show that extractability varies in the order: Ce(IV) > Th(IV) much greater than RE(III). Therefore, it is possible to find the appropriate conditions under which Ce(IV) can be effectively separated from Th(IV) and RE(III). Furthermore, stripping Ce(IV) from the loaded organic phase can be carried out by dilute H2SO4 with an aliquot of H2O2.Roasted bastnasite made in Baotou (China) by Na2CO3 and leached by HNO3, there is about 50% Ce mainly as tetravalent nitrate along with other RE(III) and Th(IV) in the leachings. Through fractional extraction, taking nitric acid leachings of roasted Bastnasite as feed and DEHEHP as an extractant, we can obtain the CeO2 products with high purity of 99.9-99.99%, with a yield of >85%, in which ThO2/CeO2 < 10(-4).

Electrocatalytic mechanism for formaldehyde oxidation on the highly dispersed gold microparticles and the surface characteristics of the electrode

Electrocatalytic mechanism for the electrochemical oxidation of formaldehyde (HCHO) on the highly dispersed Au microparticles electrodeposited on the surface of the glass carbon (GC) electrode in the alkaline Na2CO3/NaHCO3 solution and the surface characteristics of the Au microparticle-modified glass carbon (Au/GC) electrode were studied with in situ FTIR spectroscopy, scanning electron microscopy (SEM) and X-ray diffraction (XRD). It was found that the final products of HCHO oxidation is HCOO- at the Au/GC electrode and CO2 at the bulk Au electrode. The difference may be ascribed to the different surface characteristics between the Au/GC electrode and the bulk Au electrode. (C) 1999 Elsevier Science B.V. All rights reserved.

Catalysis of copper-containing transition metal hydrotalcite-like compounds in the phenol hydroxylation with hydrogen peroxide

Hydrotalcite-like compounds containing carbonate ion as the interlayer anion were prepared by coprecipitation under low supersaturation condition by mixing an aqueous solution of metal nitrates with an aqueous solutions of NaOH and Na2CO3, at room temperature, maintaining pH = 8-10 with vigorous stirring, Following the mixing, the resulting heavy slurry was aged at 353 K for 18 h with vigorous stirring, The precipitate was then filtered, washed several times with hot distilled water and dried in air at 353 K overnight, In this way, CuMI AlCO3-HTLcs and M-I AlCO3-HTLcs were synthesized and characterized by means of XRD and IR, The catalysis of the above mentioned HTLcs were investigated in the phenol hydroxylation with H2O2. The results indicated that all of the copper-containing HTLcs had a higher catalytic activity in the reaction, However, those catalysts that did not contain copper had no catalytic activity in this reaction, This means that copper was the active center in the phenol hydroxylation. Meanwhile, the mechanism was also proposed, which could be used to explain the main reason for higher activity for CuCuAlCO3-HTLcs in the phenol hydroxylation and the effect of Mg2+, Zn2+, Co2+, Ni2+ on activity of CuMI AlCO3-HTLcs.

Hydrogel-Forming Microneedles Prepared from ‘‘Super Swelling’’ Polymers Combined with Lyophilised Wafers for Transdermal Drug Delivery

We describe, for the first time, hydrogel-forming microneedle arrays prepared from "super swelling" polymeric compositions. We produced a microneedle formulation with enhanced swelling capabilities from aqueous blends containing 20% w/w Gantrez S-97, 7.5% w/w PEG 10,000 and 3% w/w Na2CO3 and utilised a drug reservoir of a lyophilised wafer-like design. These microneedle-lyophilised wafer compositions were robust and effectively penetrated skin, swelling extensively, but being removed intact. In in vitro delivery experiments across excised neonatal porcine skin, approximately 44 mg of the model high dose small molecule drug ibuprofen sodium was delivered in 24 h, equating to 37% of the loading in the lyophilised reservoir. The super swelling microneedles delivered approximately 1.24 mg of the model protein ovalbumin over 24 h, equivalent to a delivery efficiency of approximately 49%. The integrated microneedle-lyophilised wafer delivery system produced a progressive increase in plasma concentrations of ibuprofen sodium in rats over 6 h, with a maximal concentration of approximately 179 µg/ml achieved in this time. The plasma concentration had fallen to 71±6.7 µg/ml by 24 h. Ovalbumin levels peaked in rat plasma after only 1 hour at 42.36±17.01 ng/ml. Ovalbumin plasma levels then remained almost constant up to 6 h, dropping somewhat at 24 h, when 23.61±4.84 ng/ml was detected. This work represents a significant advancement on conventional microneedle systems, which are presently only suitable for bolus delivery of very potent drugs and vaccines. Once fully developed, such technology may greatly expand the range of drugs that can be delivered transdermally, to the benefit of patients and industry. Accordingly, we are currently progressing towards clinical evaluations with a range of candidate molecules.

Mass production of nitrifying bacterial consortia for the rapid establishment of nitrification in saline recirculating aquaculture systems

Two distinct nitrifying bacterial consortia, namely an ammonia oxidizing non-penaeid culture (AMO NPCU-1) and an ammonia oxidizing penaeid culture (AMOPCU-1), have been mass produced in a nitrifying bacterial consortia production unit (NBCPU). The consortia, maintained at 4 C were activated and cultured in a 2 l fermentor initially. At this stage the net biomass (0.105 and 0.112 g/l), maximum specific growth rate (0.112 and 0.105/h) and yield coefficients (1.315 and 2.08) were calculated respectively, for AMONPCU-1 and AMOPCU-1 on attaining stationary growth phase. Subsequently on mass production in a 200 l NBCPU under optimized culture conditions, the total amounts of NH4 ?–N removed by AMONPCU-1 and AMOPCU-1 were 1.948 and 1.242 g/l within 160 and 270 days, respectively. Total alkalinity reduction of 11.7–14.4 and 7.5–9.1 g/l were observed which led to the consumption of 78 and 62 g Na2CO3. The yield coefficient and biomass of AMONPCU-1 were 0.67 and 125.3 g/l and those of AMOPCU-1 were 1.23 and 165 g/l. The higher yield coefficient and growth rate of AMOPCU-1 suggest better energy conversion efficiency and higher CO2 fixation potential. Both of the consortia were dominated by Nitrosomonas-like organisms. The consortia may find application in the establishment of nitrification within marine and brackish water culture systems.

Preparation and magnetic properties of La–Mn and La–Co doped barium hexaferrites prepared via an improved co-precipitation/molten salt method

LaMn and LaCo doped barium hexaferrites of formula Ba(1-x)LaxFe(12-x)MxO19 (M=Mn, Co) (x=0.05 to 0.40) were prepared with an improved co-precipitation/molten salt method. For the synthesis, aqueous solutions of the appropriate metal chlorides were prepared in the ratio required except that the initial mole ratio of Fe and dopants to Ba was chosen to be 11:1, and then mixed with excess Na2CO3. The solutions were then cooled, filtered off, dried, then mixed with KCl flux, and heated at 450 degrees C and for 2 h. The temperature was then raised to 950 degrees C and kept for 4 h, then cooled. This new synthesis method, which employs a lower temperature and shorter reaction time, gives products with improved crystallinity and purity while the saturation magnetization and coercivity values are comparable with those synthesized via the high temperature method.

Stepwise construction of [Os6(CO)18(μ6-P)]-, a hexanuclear osmium cluster monoanion with trigonal-prismatic co-ordination for phosphorus: X-ray crystal structures of [Os6(μ-H)2(CO)20(MeCN)(μ3-PH)] and [PPh3Me][Os6(CO)18(μ6-P)]

Treatment of the labile cluster [Os3(CO)11(MeCN)] with PH3 affords the substituted product [Os3(CO)11(PH3)](1) in high yield. Subsequent reaction of (1) with Na2CO3 in MeOH, followed by acidification, gives the hydrido phosphido cluster [Os3(µ-H)(CO)10(µ-PH2)](2). When (2) is heated to 45–60 °C in the presence of [Os3(CO)11(MeCN)] a hexanuclear complex with the formulation [Os6(µ-H)2(CO)21(µ3-PH)](3) is obtained. If this reaction is repeated using [Os3(CO)10(MeCN)2] instead of [Os3(CO)11(MeCN)], an acetonitrile-containing product, [Os6(µ-H)2(CO)20(MeCN)(µ3-PH)](4), is obtained. An X-ray analysis of (4) shows that two Os3 triangular units are linked by a µ3-phosphinidene ligand, which symmetrically bridges an Os–Os edge of one triangle and is terminally co-ordinated to one Os atom of the second triangle. When (3) is treated with a weak base, such as [N(PPh3)2]Cl or [PPh3Me] Br, deprotonation to the corresponding cluster monoanion [Os6(µ-H)(CO)21(µ3-PH)]–(5) occurs. Treatment of (5) with a weak acid regenerates (3) in quantitative yield. Thermolysis of (3) leads to a closing up of the metal framework, affording the cluster [Os6(µ-H)(CO)18(µ6-P)], which readily deprotonates to give the anion [Os6(CO)18(µ6-P)]–(7) in the presence of [N(PPh3)2] Cl or [PPh3Me]Br. The same anion (7) may also be obtained by direct thermolysis of (5). An X-ray analysis of the [PPh3Me]+ salt of (7) confirms that the phosphorus occupies an interstitial site in a trigonal-prismatic hexaosmium framework, and co-ordinates to all six metal atoms with an average Os–P distance of 2.31 (1)Å. Proton and 31P n.m.r. data on all the new clusters are presented, and the position of the phosphorus resonance in the 31P n.m.r. spectrum is related to the changes in the environment of the phosphorus atom.

Estudo de adsorvente obtido de terras diatomáceas para remoção de metais pesados em águas produzidas: processamento, caracterização e dinâmica em leito fixo

The acceleration of industrial growth in recent decades on all continents aroused the interest of the companies to counter the impacts produced on the environment, spurred primarily by major disasters in the petroleum industry. In this context, the water produced is responsible for the largest volume of effluent from the production and extraction of oil and natural gas. This effluent has in its composition some critical components such as inorganic salts, heavy metals (Fe, Cu, Zn, Pb, Cd, ), presence of oil and chemicals added in the various production processes. In response to impact, have been triggered by research alternative adsorbent materials for water treatment and water produced, in order to removing oils and acids and heavy metals. Many surveys of diatomaceous earth (diatomite) in Brazil involve studies on the physico-chemical, mineral deposits, extraction, processing and applications. The official estimated Jazi are around 2.5 million tonnes, the main located in the states of Bahia (44%) and Rio Grande do Norte (37,4%). Moreover, these two states appear as large offshore producers, earning a prominent role in research of adsorbents such as diatomite for treatment of water produced. Its main applications are as an agent of filtration, adsorption of oils and greases, industrial load and thermal insulator. The objective of this work was the processing and characterization of diatomite diatomaceous earth obtained from the municipality of Macaíba-RN (known locally as tabatinga) as a low cost regenerative adsorbent for removal of heavy metals in the application of water produced treatment. In this work we adopted a methodology for batch processing, practiced by small businesses located in producing regions of Brazil. The characterization was made by X-ray diffraction (XRD), scanning electron microscopy (SEM) and specific surface area (BET). Research conducted showed that the improvement process used was effective for small volume production of diatomite concentrated. The diatomite obtained was treated by calcination at temperature of 900 oC for 2 hours, with and without fluxing Na2CO3 (4%), according to optimal results in the literature. Column adsorption experiments were conducted to percolation of the in nature, calcined and calcined fluxing diatomites. Effluent was used as a saline solution containing ions of Cu, Zn, Na, Ca and Mg simulating the composition of produced waters in the state of Rio Grande do Norte, Brazil. The breakthrough curves for simultaneous removal of copper ions and zinc as a result, 84.3% for calcined diatomite and diatomite with 97.3 % for fluxing. The calcined fluxing diatomite was more efficient permeability through the bed and removal of copper and zinc ions. The fresh diatomite had trouble with the permeability through the bed under the conditions tested, compared with the other obtained diatomite. The results are presented as promising for application in the petroleum industry