极谱法测定锌、锑渣氧粉中的铟

提出了以溴化钾-水杨酸-硫酸羟胺-硫酸溶液为底液,采用单扫描极谱法测定锌、锑渣氧粉中铟的新方法。实验条件下,铟于-0.59V(相对于饱和甘汞电极)处产生一个灵敏的极谱波。结果表明,铟的峰电流与其浓度在0.008—40μg/mL范围内有良好的线性关系,检出限为0.002μg/mL。用本法测定实际样品中的微量铟,其相对标准偏差为0.6%—1.5%,加标回收率为95.3%—102.8%,结果满意。     

离子交换分离3,5-二溴水杨基荧光酮-EDTA-CTMAB分光光度法测定微量钍

在EDTA和CTMAB存在下 ,在pH 8 8～ 10 2NH4 Cl NH3 ·H2 O缓冲体系中 ,钍 (Ⅳ )与 3,5 二溴水杨基荧光酮 (3,5 DBSF)形成红紫色多元配合物 ,其最大吸收波长为 5 5 7nm ,表观摩尔吸光系数ε为 2 19× 10 5L·mol-1·cm-1,钍含量在 0～ 7μg·(2 5mL) -1范围内 ,符合比耳定律。经离子交换分离除去干扰离子 ,用本法测定了稀土精矿和寻乌矿中的微量钍。     

Spectrophotometric Determination of Cobalt with Di-2-Pyridyl Ketone Benzoylhydrazone

Abstract

A method for the spectrophotometric determination of cobalt (II) by complexation with di-2-pyridyl ketone benzoylhydrazone (DPKBH) in 50% (v/v) ethanolic solution is described. Cobalt (II) forms a 1:2 complex with DPKBH. The complex has maximum absorbance at 370 nm. Beer's law is obeyed over the range 0.1 – 2.8 μg.ml^?1. The effect of pH, effect of excess reagent, stability of the complex and the tolerance limit of many metal ions have been reported. The method is applied to the determination of cobalt in different alloys containing other metals ions.     

Derivative Spectroscopy in Conjunction with Thin Layer Chromatography Applied for Determination of Mixtures of Amino Acids in Baby Food.

The preparative thin layer chromatography using silica gel and solvent systems n. butanol : acetic acid: water (4:1:1 V/V) and 96% ethanol : water (70 : 30 v/v) were used to separate the amino acids mixture into groups that can be eluted and one or two of amino acids can be determined by derivative spectroscopy. This was done for determining histidine in presence of cystine, arginine in presence of lysine and ornithine, tryptophan in presence of tyrosine and phenylalanin, and methionine in presence of aspartic acid. The proposed method is applied for determination of these amino acids in baby food, Neslac, Dialac and Nestogen. The statistical analysis of the results were found to be good and in agreement with the ion exchange chromatographic method.     

石墨探针采集／石墨探针炉原子吸收法直接测定APM中痕量铟

采用一定气孔性的石墨探针直接收集大气微粒物质（ＡＰＭ），然后，立即采用石墨探针炉原子吸收法测定收集在探针上的ＡＰＭ中痕量烟。方法准确，灵敏，简便，快速。在０－５０ｎｇ／ｍｌ范围内，铟的浓度与峰面积吸光度呈良好的线性关系。铟的浓度大于３００ｎｇ／ｍｌ时，产生记忆效应。铟的特征量为４．８ｐｇ，检测限为２１．５ｐｇ。分析标准参比材料，铟的回收率为９２．４－１０８．４％，相对标准偏差为８．１％。     

荷移反应用于对氨基水杨酸钠的测定

本研究了对氨基水杨酸与２，６－二氯醌氯亚胺的荷移反应，确定了反应条件，反应在丙酮介质中进行，二形成１：１的络合物，其最大吸收波长为６６０ｎｍ，表观摩尔吸光系数为１．１７×１０＾３Ｌ．ｍｏｌ．ｃｍ＾－１，用拟定方法测定对氨基水杨酸钠制剂的含量，获得满意的结果。     

析相光度法测定铁(Ⅲ)的研究

本研究了铁（Ⅲ）－ＰＥＧ（聚乙二醇－２０００）－铬锖Ｒ－Ｎａ２ＳＯ４体系的上光度法并应用于测定Ｆｅ（Ⅲ）。最适酸并为４．５￣６．５（ＮａＡｃ－ＨＡｃ）缓冲溶液,其络合物的最大吸收位于５６０ｎｍ,表观摩尔吸光系数为５．３６×１０＾４Ｌ·ｍｏｌ＾－１·ｃｍ＾－１,Ｆｅ（Ⅲ）浓度在０￣４μｇ范围内服从比尔定律,铁与铬菁Ｒ形成组成为１：２的稳定络合物。该方法用于蔡叶中铁的测定,获得了满意的结果。     

Simultaneous Spectrophotometric Determination of Iron(II) and Iron(III) in Mixtures Using Di-2-pyridyl Ketone Benzoylhydrazone

A method for simultaneous spectrophotometric determination of total iron, iron(II) and iron(III) in mixtures containing other metal ions has been described. The method is based on the complexation of iron with di-2-pyridyl ketone benzoylhydrazone (DPKBH) in 50% (v/v) ethanolic solution. Iron(II) complex with DPKBH exhibits two absorption maxima at 360 and 650 nm. meanwhile iron(II1) complex with DPKBH exhibits only one maximum at 360nm. Iron(II) and iron(III) complexes with DPKBH have similar behaviour at 360nm. Iron forms 1:2 complexes with the reagent. Beer's laws are obeyed over the ranges 0.1–2 μgml-1 and 0.4–5 μgrn1-l for iron(II) complexes at 360 and 650nm respectively. Iron(III) showed results similar to those obtained for iron(II) at 360nm. The effect of pH, effect of excess reagent. the stability of complexes. and the tolerance limit of many metal ions have been reported. The method is applied to the determination of total iron, iron(I1). and iron(II1) in synthetic solutions.     

正己烷萃取-湿法消解-ICP-MS测定印刷电路板中有机锡

利用正己烷萃取-湿法消解-电感耦合等离子体-质谱(ICP-MS)测定印刷电路板中的有机锡。对ICP-MS测定条件进行了最佳化的选择,选取铟作为内标物,实验表明无机锡不溶于正己烷中。与气相色谱质谱法(GC-MS)对比,本方法可实现有机锡的快速测定。该方法的回收率、精密度和检出限分别为85.6%—96.8%、2.6%—6.5%和0.5mg/kg。     

氟罗沙星荷移络合物在胶束体系中的紫外光谱特性及应用

采用紫外光谱法研究了π电子受体四氯对苯醌(TCBQ)与电子供体氟罗沙星的荷移反应,结果表明,氟罗沙星与TCBQ在十二烷基硫酸钠(SDS)胶束体系中能形成稳定的荷移反应络合物,使其吸光度明显增强。据此建立了氟罗沙星简单、快速、准确和灵敏的分析方法。氟罗沙星浓度在0. 6～24 mg·L-1范围内符合比尔定律。r= 0.999 3。荷移络合物在326 nm处的表观摩尔吸光系数为3.3×104 L·mol-1·cm-1。本方法用于片剂中氟罗沙星含量的测定, 其回收率为99.3%～99.8%, 相对标准偏差为0.9%～2.3%。     

Smooth surface morphology and low dislocation density of p-GaN using indium-assisted growth

Mg-doped, 1-μm-thick, p-type GaN films were grown by metal-organic chemical vapor deposition using indium-assisted method. The influence of flow rate ratio of indium to magnesium (In/Mg ratio) on the quality of p-GaN thin films was investigated by atomic force microscope, X-ray diffraction, Hall measurement and secondary ion mass spectroscopy. The surface roughness, crystalline quality and hole concentrations of p-GaN present a different variation tendency below and above 0.183 In/Mg ratio. The evolution process of indium-adlayer model considering adsorption, desorption and the transformation of indium mono-adlayer was proposed to explain the above phenomenon. Indium-assisted growth method can improve surface smoothness and crystalline quality of p-GaN effectively without affecting its electrical properties.     

负载苯基荧光酮纤维柱富集-GFAAS测定痕量铟

研究负载苯基荧光酮(PF)滤纸纤维柱预富集痕量铟,确立了制备负载苯基荧光酮纤维的最佳条件,对铟的富集、洗脱和测量条件进行了优化。含In待富集液在pH 5时,以2.0 mL·min-1的速率过柱,用8 mL 5.00 mol·L-1的HNO₃以1.0 mL·min-1的速率可以完全洗脱。用涂钨普通石墨管GFAAS测量In,选Ag作基体改进剂,提高了灵敏度。该方法检出限为0.32 ng·mL-1,回收率为95.0%～101%,RSD 1.8％～7.0％,测定自来水样品和人工合成锌、铝等样品的In,得到满意的结果。     

琥乙红霉素与水杨基荧光酮的荷移配合物生成光度法分析

琥乙红霉素与水杨基荧光酮（SAF）在乙醇溶液中发生荷移反应,荷移络合物在522nm处有最大吸收,表观摩尔吸光系数ε为8.5×103L.mol^-1.cm^-1,荷移络合物的组成比为1∶1,稳定常数是105.2,药物浓度在1.724—129.3mg/L范围内服从比耳定律。当琥乙红霉素的浓度为68.96mg/L时,8次测定结果的相对标准偏差为0.52%。测定了琥乙红霉素片剂中有效成分的含量,并与药典法比较,结果基本吻合,回收率在98.3%以上。     

电感耦合等离子体发射光谱法测定烟道灰中的铟

铟是一种银白色稀有稀散金属,在地壳中的平均质量分数为0.000 01%,为了准确测定烟道灰样品中低含量的铟,通过对样品成分的初步分析,确定实验中溶解样品所用的酸及其比例。依次逐步加入HCl, HNO3, HF和HClO4(V∶V∶V∶V=15∶5∶2∶2),将样品完全溶解后,冷却至室温并移入分液漏斗,在HBr介质中,以溴化铵做盐析剂(溶液体积控制在25 mL左右);移取25 mL乙酸乙酯作为萃取剂和稀释剂,萃取液直接导入配备有机进样系统的电感耦合等离子体原子发射光谱仪(ICP-AES),选择In 230.606 nm为分析谱线,对烟道灰样品中的铟进行测定,从而建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定烟道灰样品中铟的方法。实验样品溶解后,采用萃取分离法消除基体元素及共存元素的干扰。通过对萃取酸度、萃取剂、萃取方法、盐析剂、分析谱线等条件试验,确定了最优的实验条件。铟的质量浓度在0.25~4.00 mg·L^-1范围内与其发射强度呈线性关系,校准曲线线性相关系数为0.999 3,检出限为0.03 mg·L^-1,测定结果的相对标准偏差(n=11)小于5%,回收率在92%~102%之间。按照上述试验步骤测定5个烟道灰样品中的铟含量,其测定结果与ICP-MS法比较吻合。另外,与现有的分析方法(EDTA滴定法、分光光度法、原子吸收光谱法、 X射线荧光光谱法、电感耦合等离子体原子发射光谱法及质谱法等)相比,该法具有简便,快速,灵敏,准确度较高的优点,可用于铟含量在0.000 8%~0.10%之间烟道灰样品的批量检测。     

萃取荧光法测定药物及体液中硫酸氢氯吡格雷含量

提出了简单、灵敏的测定药物及体液中硫酸氢氯吡格雷含量的荧光新方法。利用荧光法研究了硫酸氢氯吡格雷与茜素红的作用,基于在盐酸介质中硫酸氢氯吡格雷能与茜素红形成离子对化合物,该化合物能被二氯甲烷萃取,当用428 nm波长激发时在550 nm左右能发射较强的荧光。因荧光强度与硫酸氢氯吡格雷浓度在一定范围内存在定量关系,从而建立了测定硫酸氢氯吡格雷含量的新方法。当盐酸溶液的浓度为0.3 mol·L-1时,形成的离子对比较稳定,硫酸氢氯吡格雷浓度在1.0～11.0 μg·mL-1 范围内时离子对荧光强度与硫酸氢氯吡格雷浓度呈良好的线性关系,线性方程为F=53.32+35.01c(μg·mL-1),r=0.994,检出限为0.11 μg·mL-1。硫酸氢氯吡格雷在药物和人血清、尿液中的回收率分别为90.6%～99.3%,104.6%～109.3%,96.3%～105.0%,干扰实验表明常用药物辅料对它的测定没有干扰。用本法测定了硫酸氢氯吡格雷片、人血清及尿样中硫酸氢氯吡格雷含量,结果令人满意。实验结果表明本法快速,灵敏度高,准确度好,可用于实际样品中硫酸氢氯吡格雷含量的测定。     

Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography

A rapid method for quantitative determination of atrazine and simazine in honey samples was investigated. The procedure was based on the extraction of pesticides by sonication with benzene:water = 1:1 (v/v) mixture, thin-layer chromatographic separation and quantification by CAMAG Video Documentation system in conjunction with the Reprostar 3. The extraction procedure was optimized with regard to the amount of solvent, duration of sonication and the number of extraction steps. The apparent recovery of pesticides from honey was 92.3 ± 2.4 for atrazine and 94.2 ± 2.8 for simazine, when they were extracted in three steps for 20 min using 20 ml of solvent. Ultrasonic solvent extraction was compared with traditional shake-flask extraction method.     

A Solid Phase Extraction Application of Hybrid Nano B_2O_3/ZrO_2 for Separation and Determination of Trace Indium in Environmental Samples

Hybrid nanomaterials have attracted considerable interest in environmental science, analytical chemistry and atomic spectroscopy. In the present study, a column solid phase extractioo procedure was developed for the separation and preconcentration of indium in various matrixes by using hybrid nanomaterial B₂O₃/ZrO₂ (HNMBZ). Various experimental and analytical parameters such as sample solution pH, sample solution volume, flow rate of sample solution and eluent, volume and concentration of eluent aod amount of HNMBZ, effect of common matrix ions and capacity of sorbent were investigated. The adsorbed metal ions on HNMBZ were eluted with 6 mL of 1 mol·L-1 HNO₃ solutions and their concentrations were determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimized conditions, detection limits for indium for 3 pixels and 5 pixels were found as 0.20 and 0.16 μg·L-1, respectively. The accuracy of the procedure was checked by spiked water samples. The developed procedure was successfully applied to real samples for the separation and determination of indium.     

Simultaneous Determination of Sn and S in Methyltin Mercaptide by Microwave-Assisted Acid Digestion and ICP-OESSCIEI北大核心CSCD

Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4(v/v/v=9 : 3 : 1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181, DX-990, DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%-102%).