Preparation of TiO_2/ITO film by liquid phase deposition and its photoelectrocatalytic activity for degradation of 4-aminoantipyrine

A thin layer of TiO2 film was deposited on ITO surface via the liquid phase deposition （LPD） process. The photocurrent and electrochemical impedance spectroscopy （EIS） measurements indicated that the as-prepared LPD TiO2/ITO film had an excellent photoelectrochemical performance, which showed a sensitive and rapid response to the UV irradiation. The photogenerated electron-hole pairs could be effectively separated by applying an external bias to the TiO2 film electrode. The LPD TiO2/ITO film was employed to study the photoelectrocatalytic （PEC） degradation of 4-aminoantipyrine. Compared with other techniques, the PEC technique based on such a LPD film electrode had a synergetic effect for 4-aminoantipyrine degradation. When the applied bias potential was＋0.8 V and the supporting electrolyte concentration of Na2SO4 was 0.1 mol/L, the highest degradation efficiency within 120 min could reach 95%for 0.1 mmol/L 4-aminoantipyrine solution at pH 2.0.

Synthesis,spectroscopic characterization and thermal studies of some lanthanide(Ⅲ) nitrate complexes with a hydrazo derivative of 4-aminoantipyrine

A heterocyclic ligand synthesized by the coupling of diazotized 4-aminoantipyrine with acetylacetone reacted with lanthanide(Ⅲ) nitrate to form complexes of the type [Ln(HAAP)2(NOз)з] where, Ln=La(Ⅲ), Ce(Ⅲ), Pr(Ⅲ), Nd(Ⅲ), Sm(Ⅲ), or Gd(Ⅲ) and HAAP=3-{[2-(N-1-phenyl-2,3-dimethylpyrazol-3-in-5-on-4-yl)]hydrazone}pent-2,3,4-trione. The ligand and metal complexes were characterized on the basis of elemental analysis, molar conductance, magnetic susceptibility measurements, UV-Visible, infrared, far infrared and proton NMR spectral data. The spectral data revealed that the ligand existed in the hydrazo form and coordinated to the metal ion without deprotonation in a neutral tridentate manner, through carbonyl oxygen of pyrazolone ring, hydrazo nitrogen and carbonyl oxygen of the acetylace-tone moiety. The molar conductance values adequately supported their non-electrolytic nature. The ligand and the praseodymium(Ⅲ) complex were subjected to X-ray diffraction studies. Thermal decomposition behavior of the lanthanum(Ⅲ) complex was also examined.

Crystal Structures of Schiff Base from 4-Aminoantipyrine and Pyridine-2-carboxaldehyde and Its Perchlorate

The Schiff base pyridine-2-carboxaldehyde-4-aminoantipyrine （CI7H16N4O 1） and its perchlorate （C17H17N4O·ClO4 2） have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray crystallography analysis. Both 1 and 2 crystallize in the monoclinic system, space group P21/c. For 1, a = 8.6820（12）, b = 24.934（3）, c = 7.0064（10） A,, β= 97.942（3）°, V = 1502.2（4） A^3, Z = 4, Dc = 1.293 g/cm^3, F（000） = 616,μ = 0.084 mm^-1, the final R = 0.0592 and wR = 0.1244. For 2, a = 5.9302（2）, b = 20.347（7）, c = 14.663（6） A, β= 90.200（9）°, V= 1769.201） A^3, Z = 4, Dc = 1.475 g/cm^3, F（000） = 816, μ = 0.254 mm^-1, the final R = 0.0533 and wR = 0.0819. As expected, both molecular structures of 1 and 2 adopt a trans configuration about the central C=N double bond. 2 is an ionic compound with the protonation at N（1） of pyridine-2-carboxaldehyde-4- aminoantipyrine.

流动注射-4-氨基安替比林分光光度法测定水中挥发酚不确定度评定

通过流动注射-4-氨基安替比林分光光度法对水中挥发酚测量不确定度来评定,结合流动注射-4-氨基安替比林分光光度法对水中挥发酚测量不确定度进行系统分析,研究其影响不确定因素并对其了评估。实验结果表明:使用该方法测定水中挥发酚样品含量平均值为0.103 1 mg/L,其扩展不确定度为1.7×10^(-2)mg/L,参考所有分量来看,发现进样系统的稳定性变化对测量结果影响较大。通过提高进样系统的稳定性从而降低不确定度是有效方法之一。

静注人免疫球蛋白(pH 4)中IgA残留量的不确定度分析

目的:紫外-可见分光光度法测定静注人免疫球蛋白中IgA残留量,并对其进行不确定度评定。方法:采用紫外-可见分光光度法,测定波长340 nm,比色皿狭缝1 nm,依据操作过程及测定环节引入的影响因素,对各个分量进行评估。结果:静注人免疫球蛋白(pH 4)中的IgA残留量结果为103μg·mL^(-1),扩展不确定度为10μg·mL^(-1)(k=2)。结论:本实验首次对静注人免疫球蛋白(pH 4)中的IgA残留量不确定度分量进行分析和评定,为血液制品检验提供了影响因素来源分析,为提高检验结果准确性提供了数据分析。

Spectrophotometric Determination of Aluminium with 2,3,7-Trihydroxy-9-[4-(2,4-dihydroxy)phenylazo] phenylfluorone

The conditions of color reaction of Aluminium(Ⅲ) with a new organic reagent 2,3,7 trihydroxy 9 [2,4 dihydroxy)phenylazo]phenylfluorone (ARPF) in the presence of cetyltrimethyammonium bromide(CTMAB) were studied. It was found that Aluminium(Ⅲ) reacts with ARPF and CTMAB in pH 6.5 HAc NaAc buffer solution to form a 1∶2 red complex with maximum absorption at 562 nm .The molar absorptivity is 1.10×10 5 L·mol -1 ·cm -1 . Beer's law is obeyed in the range of 0 5.5 μg Al(Ⅲ) per 25 mL. The method has been applied to determination of Aluminium in the limestone with satisfactory results.

Synthesis of meso-Tetra-(2-chloro-4-Sulfophenyl) Prophyrin and Spectrophotometric Determination of Trace Amounts of Cadmium

Synthesis of a new high sensitive water soluble chromogenic reagent mes o tetra (2 chloro 4 sulfophenyl)prophyrin and the conditions for the reaction of this reagent with cadmiun(Ⅱ) were studied. The apparent molar absorption coefficient at 434 nm is 5.20×10 5 L·mol -1 ·cm -1 . The method has been applied to the determination of 5.0×10 -9 (content by weight) Cadmium(Ⅱ) in honey.

Development of a Highly Sensitive Extractive Spectrophotometric Method for the Determination of Nickel(II) from Environmental Matrices Using 2-Acetylpyridine-4-methyl-3-thiosemicarbazone

Nickel(II) reacts with 2-acetylpyridine-4-methyl-3-thiosemicarbazone (APMT) and forms a yellow colored complex, which was extracted into n-hexanol from sodium acetate and acetic acid buffer at pH 6.0. The absorbance value of the Ni(II)-APMT complex was measured at different intervals of time at 375 nm to ascertain the time stability of the complex. The extraction of the complex into the solvent was instantaneous and stable for more than 72 hrs. The system obeyed Beer’s law in the concentration range of 0.235 - 2.43 μg·ml–1 of nickel(II), with an excellent linearity and a correlation coefficient of 0.999. The molar absorptivity and Sandell’s sensitivity of the extracted species were found to be 2.16 × 104 L mol–1 ·cm–1 and 0.003 μg·cm–2 at 375 nm, respectively. Hence a detailed study of the extraction of nickel(II) with APMT has been undertaken with a view to developing a rapid and sensitive extractive spectrophotometric method for the determination of nickel(II) when present alone or in the presence of diverse ions which are usually associated with nickel(II) in environmental matrices like soil and industrial effluents. Various standard alloy samples (CM 247 LC, IN 718, BCS 233, 266, 253 and 251) have been tested for the determination of nickel for the purpose of validation of the present method. The results of the proposed method are comparable with those from atomic absorption spectrometry and were found to be in good agreement.

Spectrophotometric Study for the Reaction of Pentoxifylline Hydrochloride with 1,2-Naphthoquinone-4-Sulphonate: Kinetics, Mechanism and Application for Development of High-Throughput Kinetic Microwell Assay for Pentoxifylline in Quality Control Laboratory

Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occurs in alkaline medium to activate the nucleophilic substitution reaction producing an orange-colored product measured spectrophometrically at λmax 472 nm. The variables affecting the reaction were carefully studied and the conditions were optimized. The kinetics of the reaction was investigated and its activation energy was found to be 0.262 cal/mol. Owing to its low activation energy, the reaction proceeded easily and was successfully used for simple and rapid assay of POX. The stoichiometry of the reaction was determined (1:1), and the reaction mechanism was suggested. To develop a high-throughput methodology used in quality control laboratory, a comparative study of the reaction using the conventional spectrophotometric versus microwell assay was applied. Under the optimum reaction conditions, the initial rate and fixed time methods were utilized for constructing the calibration graphs for determination of POX concentrations. The linear range was 10 - 120 μg/ml with good correlation coefficients (0.9987 - 0.9998). The LOD was 2.5 and 3.4 μg/ml for initial rate and fixed time methods, respectively. The intra- and inter-day accuracy and precision of the developed methods were satisfactory, where RSD was ≤3.94%. The present methods have been successfully applied to the determination of POX in its pharmaceutical tablets, and the percentage recovery values were 97.9% - 101.9%. Therefore, we strongly recommend the proposed methods for determination of POX in quality control laboratories.

4-甲基肉桂酸小檗碱共晶体外吸收特性、体内药动学研究

目的考察4-甲基肉桂酸小檗碱共晶体外吸收特性、体内药动学。方法荧光分光光度法测定4-甲基肉桂酸小檗碱溶解度、表观油水分配系数(P),Caco-2细胞单层模型、尤斯室系统测定其单位面积转运速率(Flux)、表观渗透系数(P app)。12只大鼠随机分为2组,分别灌胃小檗碱(80 mg/kg)、4-甲基肉桂酸小檗碱(118 mg/kg)的0.5%CMC-Na混悬液,于5、10、15、30、45 min及1、2.5、5、8、12、24 h采血,UPLC-MS/MS法测定小檗碱血药浓度,计算主要药动学参数。结果4-甲基肉桂酸小檗碱溶解度、log P显著高于小檗碱。在Caco-2细胞单层模型、尤斯室系统中,4-甲基肉桂酸小檗碱Flux、P app显著高于小檗碱。与小檗碱比较,4-甲基肉桂酸小檗碱T_(max)、t_(1/2)缩短(P<0.05),C_(max)、AUC_(0~t)、AUC 0~∞升高(P<0.05)。结论4-甲基肉桂酸小檗碱共晶可改善小檗碱吸收特性、生物利用度。

4-氨基安替比林光度法测定啫喱水中的甲萘酚

在碱性条件下,采用高碘酸钾为氧化剂,4-氨基安替比林(4-AAP)为显色剂,用分光光度法测定不同品牌啫喱水中甲萘酚的含量。实验最佳条件为:波长为500 nm,氧化剂用量为5.50 mL,缓冲液的用量4.50 mL,缓冲液的pH为10.0,显色剂用量为4.50 mL,常温反应10 min。结果表明:甲萘酚在0.2~8.0 mg/L范围内,呈良好线性关系,标准曲线为A=0.062c-0.004,相关系数R^(2)=0.999,平均回收率为99.2%。

1-(2,6-二溴-4-硝基苯)-3-(4-硝基苯)-三氮烯光度法测定铜

建立了用 1 - ( 2 ,6-二溴 - 4-硝基苯 ) - 3- ( 4 -硝基苯 ) -三氮烯 (DBNPNPT)分光光度法直接测定铜矿及铝合金样品中铜的方法。在表面活性剂TritonX - 1 0 0的存在下 ,pH在 9.5～ 1 1 .5的Na2 B4O7-NaOH介质中 ,DBNPNPT与Cu2 +可生成黄色络合物 ,以 5 35nm为参比波长 ,45 0nm为测定波长的双峰双波长法进行测定 ,表观摩尔吸光系数可达 1 .1 1× 1 0 5L·mol- 1 ·cm- 1 ,Cu2 +的质量浓度在 0～ 360 μg/L符合比尔定律。方法用于铜矿中铜的测定 ,结果与原子吸收法吻合。对于w(Cu)为 0 .1 1 %的BY2 1 70 - 1铝合金试样测定 1 0次 ,其RSD为3.4%。

新显色剂4-溴-2-磺酸基苯基重氮氨基偶氮苯的合成及其与镉(Ⅱ)的显色反应

报道了一种新型的三氮烯类偶氮染料的合成方法及其与Cd(Ⅱ )的显色反应。实验表明 ,在TritonX 1 0 0存在下的弱碱性介质中 ,试剂与镉 (Ⅱ )形成 2∶1的红色络合物 ,摩尔吸收系数为 2 .1× 1 0 5L·mol- 1 ·cm- 1 ;镉含量在 0 μg/2 5mL～ 2 5 μg/2 5mL范围内遵守比耳定律。

新显色剂4,4′-二偶氮苯重氮氨基偶氮苯测定水中微量锌的研究

本文报告在四硼酸钠体系中和Triton X-100存在下,锌与新显色剂4,4′-二偶氮苯重氮氨基偶氮苯有灵敏的显色反应。红色络合物在525nm处摩尔吸光系数为1.63×10~5L·mol^(-1)·cm^(-1),并研究了测定锌的各种条件和40余种共存离子对测定的影响。

新显色剂8-[杯(4)芳烃偶氮]氨基喹啉的合成及其与金的显色反应

合成了一种新的杂环偶氮类显色试剂 8 [杯 ( 4 )芳烃偶氮 ]氨基喹啉(CAQ) 1。研究了该试剂与金的显色反应的适宜条件 ,在碱性介质中 ,在CTMAB存在下 ,试剂与金生成 1∶1稳定络合物 ,建立了测定金的光度法新体系 ,体系至少可稳定 8h ,λmax =640nm ,ε =2 .0 6× 1 0 5L·mol-1·cm-1,金含量在 0～ 2 2μg 2 5mL内符合比尔定律。方法已用于金矿石中微量金的测定。

酱油中4-甲基咪唑含量测定方法的研究

建立了分光光度法测定酱油中4-甲基咪唑含量的方法。酱油样品经沉淀、离心、萃取、脱色、显色反应，利用分光光度计在波长440nm处测定其吸光度值。方法的平均回收率为85%-110％，标准偏差为0．14如．37，变异系数为0．007-0．014。结果表明，该方法设备简单、精密度和重复性较好。

meso-四(4-磺酸苯基)卟啉与铅显色反应及其应用

研究了铅与meso-四(4-磺酸苯基)卟啉(TPPS_4)的显色反应条件,试验发现,在盐酸羟胺存在下和碱性(pH 12)介质中,铅与TPPS_4在室温即可络合完全,络合比为1:1,摩尔吸光系数ε=2.64X10^5,铅含量在0～2.0μg/10ml范围内呈线性,经APDC/MIBK 萃取分离,排除干扰后,用于自来水、桃叶中痕量铅的测定,结果满意.

2-(2-喹啉偶氮)-4-二甲氨基苯甲酸光度法测定钢铁中镍

合成了新试剂 2 -(2 -喹啉偶氮 ) -4 -二甲氨基苯甲酸 (QADMABA) ,并研究了其与镍的显色反应 ,在 pH8 0硼酸-磷酸二氢钾缓冲介质中 ,吐温 80存在下 ,QADMABA与铜反应生成 2 :1稳定络合物 ,λmax=5 80nm ,ε =9 6× 10 4。镍含量在 0～ 10 μg/2 5mL内符合比尔定律 ,方法用于钢铁样品中镍含量的测定 。

新显色剂四(4-甲氧基-4-磺酸基苯基)卟啉与Fe^(3+)的高灵敏反应的研究与应用

本文提出以四 (4 -甲氧基 - 4 -磺酸基苯基 )卟啉 (p- OCH3TPPS4 )为显色剂 ,在 p H=3.5— 5 .5的条件下测定痕量铁的新体系 ,络合物最大吸收波长为 4 4 6nm,表观摩尔吸收系数ε=2 .0× 10 4 L· mol-1· cm-1,Fe3+ 在 0— 10 μg/ 2 5 m L 范围内符合比耳定律 ,应用本法测定花生仁皮中铁 ,回收率可达 95 .0 %—10 8.4 %

4-(邻-重氮氨基苯胂酸)-偶氮苯测定镉的高灵敏度方法

本文提出了用4-(邻-重氮氨基苯胂酸)偶氮苯分光光度法测定镉的高灵敏度新方法。此试剂可与Cd(Ⅱ)形成3:1的配合物,其表观摩尔吸光系数为1.85×10~5L·mol^-1·cm^-1,在0—12.50μg Cd(Ⅱ)/25ml范围内服从比尔定律,大多数离子不干扰,可满意地用于测定工业废水中的痕量Cd(Ⅱ)。