新钽酸盐K_6FeTa_(15)O_(42)的合成与表征

在K2O -Fe2O3-Ta2O5 三元系统中 ,新发现存在钽酸盐K6FeTa15O42,使用X射线衍射(XRD)、电子探针微区分析(EPMA)、扫描电镜(SEM)、差热分析(DTA)等方法对该化合物的晶体结构、成分、形态、光学性质、溶解性、熔点及密度进行了研究。新化合物K6FeTa15O42 晶体属于六方晶系,空间群P63/mcm,晶胞参数a=0.91221(1)nm,c=1.21084(4)nm,Z=1,V=0.87258nm3。     

新钽酸盐K6FeTa15O42的合成与表征

在K2O－Fe2O3-Ta2O5三元系统中,新发现存在钽酸盐K6FeTa15O42,使用X射线衍射（XRD)、电子探针微区分析（EPMA）、扫描电镜（SEM）、差热分析（DTA）等方法对该化合物的晶体结构、成分、形态、光学性质、溶解性、熔点及密度进行了研究。新化合物K6FeTsa14O42晶体属于六方晶系,空间群P63／mcm,晶胞参数a=0.91221(1)nm,c=1.21084(4)nm,Z=1,V=0.87258nm^3。     

类钙钛矿结构新钽酸盐KSr2Ta3O10的合成、结构与层间特性

类钙钛矿结构氧化物是由钙钛矿结构基元与其它类型结构基元组合而成的一种超结构复合氧化物.     

新钽酸盐Ba3TiTa4O15的结构与介电性能

在BaO Ta2O5系统通过掺Ti4＋合成了新钽酸盐Ba3TiTa4O15,用粉晶XRD对其结构进行了分析,并测试了其烧结体的介电特性.结果表明:Ba3TiTa4O15在室温下属于填满型四方钨青铜结构,晶胞参数a=1.256 27(6)nm, c=0.395 86(4)nm; Ba3TiTa4O15在－35 ℃从铁电相转变为顺电相.     

新钽酸盐Ba_3TiTa_4O_(15)的结构与介电性能

在 ＢａＯ－Ｔａ２Ｏ５系统通过掺Ｔｉ４＋合成了新钽酸盐 Ｂａ３ＴｉＴａ４Ｏ１５,用粉晶ＸＲＤ对其结构进行了分析,并测试了其烧结体的介电特性．结果表明：Ｂａ３ＴｉＴａ４Ｏ１５在室温下属于填满型四方钨青铜结构,晶胞参数α＝１．２５６ ２７（６）ｎｍ,ｃ＝０．３９５ ８６（４）ｎｍ;Ｂａ３ＴｉＴａ４Ｏ１５在－３５℃从铁电相转变为顺电相     

K9TaW11O40.15H2O的合成及性质

迄今为止,有关钨钽杂多阴离子的报道极少。由于杂多酸在石油化工、颜料等领域有重要用途,人们对研究新的杂多阴离子的合成一直有着浓厚兴趣,也是杂多酸化学的重要内容。本文报道粉状白钨酸和可溶性钽酸钾溶液反应以合成十二聚系列的钨钽酸钾化合物。 钽酸钾按文献[1]制备,以Ta_2O_5(99.9%)与K_2CO_3之比1∶2的混合物于970℃熔融后     

用TPAC重量法测定钽的新方法

研究了TPAC作为沉淀剂用重量法测定含铌复杂基体中钽的可能性. 结果表明,TPAFTa经分解定量地转化为五氧化二钽, 并以此为称量形式. 对20多种共存离子的吸附或共沉淀的杂以质量均小于万分之四. 随着老化时间的增加晶体明显增大, 吸附或共沉淀的杂质显著减少. 选择了最佳实验条件、详细研究了TPAFTa的物理化学性质. 钽的回收率为98.1-101.8%、镍基高温合金试样分析结果为1.80±0.027%, 可认为TPAC是钽的特效沉淀剂.     

高频红外吸收法测定钽粉、铌粉和碳化钽中的碳

用HCS-140型高频红外碳硫分析仪测定钽粉、铌粉、碳化钽中的碳,进行了助熔剂、称样量、氧气流量试验,在不需测硫的情况下,采用铜和钨作助熔剂、称样量为0．5g、氧气流量为2L／min时,测定结果满足分析要求。     

有机胺柱类钙钛矿型钽酸盐的制备与表征

采用分步交换法，合成了新型的正丙胺、正丁胺柱层状类钙钛矿型钽酸盐C3H7NH3-Sr2Ta3O10与C4H9NH3-Sr2Ta7O10，采用X射线衍射(XRD)、扫描电镜(SEM)、红外光谱(IR)对该类化合物的结构与形貌进行了表征，并测定了其比表面积。     

钴-二氮菲一硫脲体系的极谱催化波

In 8*10^-^7M phenanthroline-0.02M thiourea medium (ethanolamine buffer, pH =8.3), by using Na2SO3 to remove dissolved oxygen, cobalt ion can produce a sensitive catalytic wave with a peak shape on dc polarography. Ep=1.62V (vs. S.C.E.), detection limit is 1 X 10^-^1^0M. There is a linear dependence of peak height on cobalt concentration over a range of 2 X 10^-^1^0 - 4 X 10^-^8 M. Common ions which are not more than 1000-fold of Co^2^+ do not interfere the determination of cobalt, except Ni^2^+ and As^3^+ which are permitted to only 125 and 300-fold respectively. Good results are obtained in determining traces of cobalt in various samples by this method.     

Mercury(II) ion-selective electrodes based on p-tert-butyl calix[4]crowns with imine units.

A PVC membrane incorporating p-tert-butyl calix[4]crown with imine units as an ionophore was prepared and used in an ion-selective electrode for the determination of mercury(II) ions. An electrode based on this ionophore showed a good potentiometric response for mercury(II) ions over a wide concentration range of 5.0 x 10(-5) - 1.0 x 10(-1) M with a near-Nernstian slope of 27.3 mV per decade. The detection limit of the electrode was 2.24 x 10(-5) M and the electrode worked well in the pH range of 1.3 - 4.0. The electrode showed a short response time of less than 20 s. The electrode also showed better selectivity for mercury(II) ions over many of the alkali (Na+, -1.69; K+, -1.54), alkaline-earth (Ca2+, -3.30; Ba2+, -3.32), and heavy metal ions (Co2+, -3.67; Ni2+, -3.43; Pb2+, -3.31; Fe3+, -1.82). Ag+ ion was found to be the strongest interfering ion. Also, sharp end points were obtained when the sensor was used as an indicator electrode for the potentiometric titration of mercury(II) ions with iodide and dichromate ions.     

PVC膜修饰电极上零电流示波电位滴定法测定硼的研究

以氯化十六烷基吡啶（ＣＰＣ）和氟硼酸钠形成的离子缔合物为活性物质，制成ＰＶＣ膜涂层石墨电极，提出了一个快速测定硼的零电流示波电位滴定法。以ＣＰＣ为滴定剂，用ＰＶＣ膜电极为指示电极，甘汞电极为参比电极，利用阴极射线示波器荧光屏上荧光点的突然位移来指示ＣＰＣ滴定硼的终点，具有灵敏、准确、快速等特点，用该法测定玻璃中的硼，结果良好。     

Novel potentiometric membrane sensor for the determination of trace amounts of chromium(III) ions.

A plasticized Cr3+ ion sensor by incorporating 2,3,8,9-tetraphenyl-1,4,7,10-tetraazacyclododeca-1,3,7,9-tetraene (TTCT) ionophore exhibits a good potentiometric response for Cr3+ over a wide concentration range (1.0 x 10(-6)-1.0 x 10(-1) M) with a slope of 19.5 mV per decade. The sensor response is stable for at least three months. Good selectivity for Cr3+ in comparison with alkali, alkaline earth, transition and heavy metal ions, and minimal interference are caused by Li+, Na+, K+, Co2+, Hg2+, Ca2+, Pb2+ and Zn2+ ions, which are known to interfere with other chromium membrane sensors. The TTCT-based electrode shows a fast response time (15 s), and can be used in aqueous solutions of pH 3-5.5. The proposed sensor was used for the potentiometric titration of Cr3+ with EDTA and for a direct potentiometric determination of Cr3+ content in environmental samples.     

Potentiometric sensor array for the determination of lysine in feed samples using multivariate calibration methods

A potentiometric sensor array has been developed for the determination of lysine in feed samples. The sensor array consists of a lysine biosensor and seven ion-selective electrodes for NH4+, K+, Na+, Ca2+, Mg2+, Li+, and H+, all based on all-solid-state technology. The potentiometric lysine biosensor comprises a lysine oxidase membrane assembled on an NH4+ electrode. Because the selectivity of the lysine biosensor towards other cation species is not sufficient, there is severe interference with the potentiometric response. This poor selectivity can be circumvented mathematically by analysis of the richer information contained in the multi-sensor data. The sensor array takes advantage of the cross-selectivity of lysine for each electrode, which differs from the other species and quantification of lysine in complex feed sample extracts is accomplished with multivariate calibration methods, such as partial least-squares regression. The results obtained are in a reasonable agreement with those given by the standard method for amino acid analysis.     

邻苯二酚紫修饰电极示差脉冲伏安法测定水中铝

利用吸附的方法在热解石墨电极上制得邻苯二酚紫(PCV)修饰电极。在NH~3.H~2O-NH~4Cl底液(pH8.5)中,该电极具有很好的电化学活性,其示差脉冲氧化峰电位为E~p~a=+80mV。对铝进行检测,只是峰电流降低,而峰电位不变,氧化峰电流的降低值与铝浓度在1×10^-^8-1×10^-^7mol.dm^-^3和1×10^-^7-1×10^-^6mol.dm^-^3范围内成正比,检测限为5×10^-^9mol.dm^-^3,标准偏差为5.0%(4×10^-^8mol.dm^-^3Al,n=8),对实际水样进行测定,结果令人满意。对其检测机理进行了研究后认为:(1)PCV修饰电极表面是PCV单分子层吸附,具有很好的电化学活性;(2)铝与PCV在电极表面形成一1:3的配合物,该配合物在修饰电极上本身没有电化学活性,仅覆盖住原有的PCV电活性点,从而使峰电流降低,而峰电位没有变化;因此,在有铝和无铝时,电极过程没有变化,都对应于PCV的电化学行为。我们用电化学方法、扫描电镜、X射线光电子能谱和X射线荧光光谱法对此进行了证明。     

Cetylpyridinium-iodomercurate PVC membrane ion selective electrode for the determination of cetylpyridinium cation in Ezafluor mouth wash and as a detector for some potentiometric titrations

A potentiometric method is described for the determination of cetylpyridinium (CP) cation using a polyvinyl chloride powder (PVC) membrane sensor based on CP-iodomercurate ion pair as an electroactive material. The sensor shows a linear response for CP ion over the concentration range of 2x10(-6)-1x10(-3) M at 25 degrees C. The electrode posses a sub-Nernstian slope of 29.0+/-0.4 mV decade(-1), which has been thoroughly discussed.The electrode shows a fast potential response of approximately 50 s, which is almost constant over a pH range of 3.0-6.0. Selectivity coefficient data for some common ions show negligible interference, however, cetyltrimethylammonium bromide (CTMAB) interferes significantly. An average recovery of 98.8% for CP with an average relative standard deviation (R.S.D.) of 1.2% has been achieved. The determination of CPC in Ezafluor mouth wash gave result that compare favorably with those obtained by the British Pharmacopoeia method. The CP electrode has been utilized as an end point indicator electrode in potentiometric titration of some anions, and applied for the determination of anionic surfactants in some commercial detergents and waste water.     

Potentiometric determination of cetylpyridinium chloride using a new type of screen-printed ion selective electrodes

A new type of screen-printed ion-selective electrode for the determination of cetylpyridinium chloride (CPC) is presented. These new electrodes involve in situ, modified and unmodified screen-printed ion-selective electrodes for the determination of CPC. The screen-printed electrodes (SPEs) show a stable, near-Nernstian response for 1 × 10⁻² to 1 × 10⁻⁶ M CPC at 25 °C over the pH range 2-8 with cationic slope 60.66 ± 1.10. The lower detection limit is found to be 8 × 10⁻⁷ M and response time of about 3 s and exhibit adequate shelf-life (6 months). The fabricated electrodes can be also successfully used in the potentiometric titration of CPC with sodium tetraphenylborate (NaTPB). The analytical performances of the SPEs are compared with those for carbon paste electrode (CPE) and polyvinyl chloride (PVC) electrodes. The method is applied for pharmaceutical preparations with a percentage recovery of 99.60% and R.S.D. = 0.53. The frequently used CPC of analytical and technical grade as well as different water samples has been successfully titrated and the results obtained agreed with those obtained with commercial electrode and standard two-phase titration method. The sensitivity of the proposed method is comparable with the official method and ability of field measurements.     

金属有机电荷转移盐(CpFeBz)n[M(L)2](L=mnt或dmit)的合成及其三阶非线性光学性质

合成了两种类型共九个新的金属有机电荷转移盐(CpFeBz)n[M(mnt)2]和(CpFeBz)n[M.(dmit)2](M=Ni, Pd, Pt,Cu, Co; Cp代表环戊二烯基; Bz代表苯; 通过元素分析、IR和1H NMR对化合物进行了鉴定。用简并四波混频的方法首次研究了金属有机电荷转移盐的三阶非线性光学性质。结果表明, 这类金属有机电荷转移有较大的近共振三阶非线性光学响应。     

混合溶剂中性载体镁离子选择性微电极的研究

用氯化石腊和邻硝基苯辛醚为混合溶剂制备中性载体ETH5214的镁离子选择性微电极,相对于钾离子的电位选择性系数较单独以邻硝基苯辛醚为溶剂的ETH5214镁微电极改善0.9个数量级。在纯MgCl~2和在含细胞内典型离子背景的MgCl~2溶液中,响应斜率为Nernst响应,检测下限分别为4×10^-^7mol.dm^-^3和2×10^-^5mol.dm^-^3。在pH3.5-9.5范围内,氢离子对电极的电位响应无影响。测量的重现性良好。电极的实用响应时间(t~9~5)≤3s,有效寿命长于5天。