用自行设计的自动分析系统测定高含量SO3--对硫酸钡浊度测定法的改进

为了解决湿法磷酸生产中高含量SO3的测定,对硫酸钡浊度测定法的反应条件进行了改进,并自行设计制造了自动化的分析系统。测定时样品由蠕动泵(P)推入酸化盘管(AC)中进行酸化和稀释,由定量环(Sv)取样25μL,注入反应系统。在第一反应盘管(RC1)中,SO3与第一混合试剂中的BaCl2溶液反应生成BaSO4悬浊液,该溶液中的聚乙二醇-4000(PEG-4000)和乙醇通过协同作用避免了BaSO4颗粒的团聚,降低粒子间的相互作用,使BaSO4的生成减少,降低了测定的灵敏度,提高了稳定性。在第二反应盘管(RC2)中,BaSO4与第二混合试剂中的NH3·H2O/乙二胺四乙酸二钠(Na2EDTA)溶液发生络合反应同时被Na2EDTA包裹,进一步降低其灵敏度。最后反应溶液进入流通式光度检测器,在680.0nm波长处测试BaSO4悬浊液的吸光度。经优化试验条件,上述第一混合试剂中3种组分的质量分数或体积分数为:BaCl24%,PEG-4000 3%和乙醇2%;第二混合试剂中Na2EDTA的质量分数为6%,NH3·H2O的体积分数为6%。对实际按本方法及重量法分析进行测定,两种方法所得结果的相对偏差在±2%以内,且不受共存的高含量PO43-和F-的干扰。     

纳米丝光沸石分子筛的合成及表征

在水热条件下制备丝光沸石的纳米晶.研究了合成条件、不同添加剂、动态晶化等对沸石粒径的影响.结果表明,反应物中较高的碱度,较低的晶化温度,加入NaCl和Na2SO4金属盐做成核助剂,及动态晶化有利于纳米丝光沸石分子筛的合成.     

AOT微乳液中通过水化电子产额调控合成BaSO_4纳米纤维

通过γ-辐照含有K2S2O8和BaCl2的二(2-乙基己基)琥珀酸酯磺酸钠(AOT)反相微乳液,将S2O82-通过辐射还原实现了SO42-的原位缓释,从而成功制备出BaSO4纳米纤维单晶,并进一步制得多层次的纳米纤维束结构.在此基础上,通过改变水与表面活性剂物质的量之比(ω值)、改变钡盐阴离子和在微乳液连续相添加芳香化合物等手段来调节水化电子(e-aq)产额,控制微乳液水池中S2O82-的还原和SO42-的缓释速率,成功实现了对BaSO4纳米粒子形貌的调控:随着ω值的增加或剂量率的增加,e-aq产额增加,从而加快了SO42-的释放,不利于BaSO4纳米纤维的生成;采用Ba(NO3)2为钡源时,NO3-能有效地降低e-aq产额和S2O82-的还原速率,因而在较高的剂量率和较高ω值下能得到BaSO4纳米纤维;在微乳液油相中加入甲苯来捕获油相中过量电子(e-oil),降低e-aq产额,从而在较高的剂量率下得到BaSO4纳米纤维.研究结果表明:通过e-aq产额调控纳米粒子形貌的机理在BaSO4纳米粒子的制备中得到很好体现.     

高纯纳米氧化钛的制备及催化活性

以工业级硫酸钛为原料,在酸性环境下以EDTA作为络合剂,采用控制沉淀法制备高纯度纳米TiO2。考察了pH值、反应温度、煅烧温度等工艺条件对TiO2颗粒晶型、大小和分布影响。利用TEM、XRD、ICP等手段对产物进行表征,TiO2纯度超过99.9%,粒径为10-20nm,分布均匀。经过对其光催化降解苯酚反应活性实验,结果表明样品具有较好的光催化活性。     

丙三醇存在下硫酸钡微粒体系的光谱特性研究及其分析应用

0.10 mol/L HCl-4.0 mol/L丙三醇-0.05 mol/L BaCl2溶液体系的瑞利散射很弱.当有SO4^2-存在时,（BaSO4）n微粒体系在470 nm处产生一较强的瑞利散射峰,SO4^2-浓度在1.0～80μg/mL浓度范围内与I470nm呈线性关系.据此,建立了一个测定水中硫酸根的简便、灵敏的瑞利散射光谱分析新方法.研究结果表明：SO4^2-与Ba^2＋由于静电引力可形成BaSO4分子,而BaSO4分子间存在较强疏水作用力和分子间作用力,可聚集形成（BaSO4）n微粒和固液界面,（BaSO4）n微粒和固液界面的形成是导致体系瑞利散射强的根本原因.     

全硅MEL纳米分子筛的合成及物化性质I．全硅MEL纳米分子筛的合成

在TEOS-TBAOH-H_2O反应物体系中,水热条件下制备了全硅MEL （Silicalite- 2）沸石纳米晶。详细讨论反应物中TBAOH/TEOS摩尔比、H_2O/TEOS摩乐比、反应温 度等对沸石粒径的影响。结果表明,反应物中较高的碱度和TEOS（硅源）浓度,及 较低的晶化温度有利于MEL纳米分子筛的合成。     

超声波法制备超细铜粉

在40k Hz超声波作用下,使用以Na BH4作为还原剂的化学还原法制备具有粒径约300 nm~500 nm、产率约为80~90%的超细铜粉,其具有反应温度低反应速率快的优点。最佳制备条件为Cu SO4溶液初始浓度为20 g/L、Na BH4的加入量为1.5 g/L、p H值为11.5、反应温度20~30℃;反应时间20~25 min。通过XPS、XRD、SEM对超细铜粉表面进行检测发现分析表明所制备的超细铜粉呈类球状,其表面有少量Cu2O和Cu(OH)2存在。     

全硅MEL纳米分子筛的合成及物化性质I.全硅MEL纳米分子筛的合成

在TEOS-TBAOH-H_2O反应物体系中，水热条件下制备了全硅MEL （Silicalite- 2）沸石纳米晶。详细讨论反应物中TBAOH/TEOS摩尔比、H_2O/TEOS摩乐比、反应温 度等对沸石粒径的影响。结果表明，反应物中较高的碱度和TEOS（硅源）浓度，及 较低的晶化温度有利于MEL纳米分子筛的合成。     

六方相W03纳米带的制备与表征

以Na2WO4、K2SO4和H2C2O4为原料,采用两步水热合成法制备了六方相W03纳米带。首先,在探索pH值、K2SO4加入量、反应温度和时间以及表面活性剂等因素对WO3纳米带的前驱物钨酸盐形貌的影响后,给出了前驱物钨酸盐纳米带的合成条件,并讨论了纳米带的形成机理;然后,在180℃的水热条件下对前驱物再处理48h获得六方相WO3纳米带。测试结果表明,WO3纳米带的形貌保持较好,宽度在100—300nm间,长度可达数微米,沿纳米带长轴方向为[001]方向。     

六方相WO3纳米带的制备与表征

以Na2WO4、K2SO4和H2C2O4为原料,采用两步水热合成法制备了六方相WO3纳米带.首先,在探索pH值、K2SO4加入量、反应温度和时间以及表面活性剂等因素对WO3纳米带的前驱物钨酸盐形貌的影响后,给出了前驱物钨酸盐纳米带的合成条件,并讨论了纳米带的形成机理;然后,在180℃的水热条件下对前驱物再处理48 h获得六方相WO3纳米带.测试结果表明,WO3纳米带的形貌保持较好,宽度在100～300 nm间,长度可达数微米,沿纳米带长轴方向为[001]方向.     

Synthesis of nanosized BaSO4 and CaCO3 particles with a membrane reactor: effects of additives on particles

Nanosized BaSO(4) particles, about 15 nm in size, were synthesized successfully by a membrane reactor at the aids of additives, in which Na(2)SO(4) solutions were added into BaCl(2) solutions gradually through the micropores of ultrafiltration membranes to control the saturation ratio, subsequently the nucleation and growth rates. The effects of additives species, additives concentrations, and membranes molecular weight cut-off (MWCO) on the particle morphology, along with the formation processes of particles, were investigated. CaCO(3) nanoparticles of 30-60 nm in size were also prepared by the reactor. The results revealed that the addition of methyl alcohol, ethanol etc. favor the synthesis of nanoparticles with small size. The particles size decreases with the increase in ethanol concentrations. With the increase in membrane MWCO, the products tend from nanoparticles towards aggregates.     

Effect of background electrolytes and pH on the adsorption of Cu(II)/EDTA onto TiO2

Cu(II)/EDTA adsorption onto TiO2 has been studied with a variation of pH, ionic strength, and type of background electrolytes. Cu(II) adsorption onto TiO2 increased as ionic strength increased when NaClO4 was used as a background electrolyte. This can be explained by the increase of exp(-FPsi/RT) as a part of the electrostatic correction within a surface complexation model. Model predictions described experimental adsorption trends. Types of background anions (ClO4, Cl, NO2, NO3, SO3, and PO4) did not affect adsorption trends and adsorption amounts of Cu(II) onto TiO2. However, different trends were observed with various types of background ions used as ionic strength in EDTA and Cu(II)-EDTA adsorption. EDTA adsorption was decreased by using Na2SO3 and Na3PO4 as background ions, while NaClO4, NaCl, NaNO2, and NaNO3 showed negligible interference on the EDTA adsorption, which matched well with model predictions. The presence Na2SO3 and Na3PO4 also interfered with Cu(II)-EDTA adsorption, to a somewhat greater extent compared to EDTA adsorption, especially at lower pH. This interference was also noted in Cu(II)-EDTA adsorption with a variation of Cu(II)-EDTA concentration at constant ionic strength (3 x 10(-3) M) by using Na2SO3 and Na3PO4, especially at lower ratios of Cu(II)-EDTA to Na2SO3 and Na3PO4. These results suggest that the ratio of Cu(II)-EDTA to Na2SO3 and Na3PO4 is an important factor for the controlling of competition between these background ions and Cu(II)-EDTA onto TiO2. Model prediction generally matched well with experimental adsorption using NaClO4, NaCl, NaNO2, and NaNO3 as backgrounds ions, while a severe deviation was observed in the presence of Na2SO3 and Na3PO4. These results suggest that the mobility of copper ions as Cu(II)-EDTA can be increased from polluted area in the presence of multivalent background ions, especially as the ratio of adsorbates/background ions decreased.     

超声化学法制备BaF_2纳米粒子及纳米方块

<正>0引言BaF2的用途非常广泛,可用于光学玻璃、陶瓷色料、玻璃光导纤维、激光发生器、助熔剂及防腐剂等。BaF2是最快的闪烁体,在核物理和核技术中用来检测γ射线和带电粒子[1]。将掺杂稀土金属的纳米BaF2粒子嵌入有机或玻璃基体以发挥其发光性能的研究越来越引起重视[2]。碱土氟化物和许多半导体的晶格匹配性良好,可以用不同碱土氟化物层来连接晶格常数不同的半导体[3]。     

钨酸钙核/卤化银壳微晶乳剂的二次定影研究

近２０年来,随着卤化银微晶合成技术的进步,合成出了诸如Ｔ－颗粒、核壳乳剂和外延复合颗粒乳剂等性能优异的微晶体,极大地提高了乳剂的感光性能．但这些乳剂也有一个共同的缺点,即大量消耗贵金属银,且未成影像的银均随定影过程而浪费．为改善此类乳剂的不足,各国科...     

A new preparation method of gold nanoparticles by intra-reduction of sodium gold（I） sulfite

In this study, well-dispersed gold nanoparticles were prepared by using intra-molecular reduction of sodium gold sulfite, without using additional reductants and chloride free. The technical parameters including transformation temperature, pH, and concentration were optimized by the single-factor method as 90 C, pH 1, and 0.01 mmol/L [Na3Au（SO3）2], respectively. The resultant colloidal transmission electron microscopy images （TEM） and UV-vis absorption spectrophotometer spectra were acquired to check their properties, and the results show this kind of colloidal gold is controlled to 6 nm in sizes and has good stability in solution.     

溶液中铝还原制备Fe-Co合金纳米粉体

为了获得价廉而方便的制取Fe-Co纳米粉体的方法,在pH～3, 40 ℃条件下用铝粉还原FeSO4•(NH4)2SO4和CoSO4•(NH4)2SO4的混合溶液,制得了平均粒径为15 nm的Fe-Co固溶体粉体.用XRD鉴定了合金的物相和粒度,ICP方法分析了合金的成份.实验表明,固溶体的成份可以通过改变溶液中Fe2＋和Co2＋的比例而得以调整.     

Fast removal and recovery of Cr(VI) using surface-modified jacobsite (MnFe2O4) nanoparticles

In this work, the effectiveness of surface-modified jacobsite (MnFe2O4) nanoparticles was investigated for the removal and recovery of Cr(VI) from synthetic wastewater. Ten nanometer modified MnFe2O4 nanoparticles were produced to be a new adsorbent using a co-precipitation method followed by a surface redox reaction. The equilibrium time for Cr(VI) adsorption onto modified MnFe2O4 nanoparticles was as short as 5 min, and the adsorption data fit the Langmuir model well. The maximum uptake of 31.5 mg of Cr(VI)/g of modified MnFe2O4 was obtained at pH 2, which was comparable with other common adsorbents such as activated carbon and sawdust. The effects of ligands (EDTA, SO4(2-), NH4+) and ionic strength were studied in a pH range of 2-10. EDTA and SO4(2-) inhibited the adsorption of Cr(VI) over the entire pH range studied, whereas NH4+ enhanced the uptake of Cr(VI) at pH greater than 6.5. The mechanisms leading to Cr(VI) adsorption by modified MnFe2O4 nanoparticles were determined by X-ray diffraction and X-ray photoelectron spectroscopy to be a combination of electrostatic interaction and ion exchange. Regeneration studies indicated the potential reuse of the modified MnFe2O4 nanoparticles without sacrificing adsorption capacity and the possible recycling of Cr(VI) without changing the valence.     

Influence of EDTA on the Morphology of Barium Carbonate Using High Gravity Technology

The superfine BaCO3 particles were synthesized by high gravity technology with BaCl2·2H2O and Na2CO3 as the raw materials. The changes of particle size and morphology were studied by adding different amount of EDTA, and rod-like, near-spherical and cylindrical shape BaCO3 were prepared. The BaCO3 particles were analyzed and characterized by TG/SDAT, SEM, XRD and FT-IR. The results indicated that the crystal transformation temperature and decomposition temperature of BaCO3 had increased because of EDTA addition. With the increase of EDTA amount, the shape of BaCO3 changed from irregular rod-like to near-spherical then to cylindrical shape. All different shape BaCO3 adopts orthorhombic crystal systems.