新催化动力学光度法测定痕量铑

在ＰＨ５．１的ＨＡｃ－ＮａＡｃ介质中,铑（Ⅲ）催化高碘酸钾氧化偶氮胂Ⅲ褪色,据此建立了一个以偶氮胂Ⅲ褪色反应为基础的新催化动力学测定铑的方法。     

新显色剂5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯与铑(Ⅲ)高灵敏显色反应的研究及其应用

合成了新试剂碘代吡啶偶氮胺类化合物5-(5-碘-2-吡啶偶氮)-2,4-二氨基甲苯(5-I-PADAT),用红外光谱、元素分析和核磁共振波谱对其进行了鉴定,并研究了该试剂与铑(Ⅲ)的显色反应。结果表明,在pH=4.0～5.2的乙酸-乙酸钠缓冲溶液中,铑(Ⅲ)与5-I-PADAT形成1∶2的紫红色络合物。该络合物在1.2mol·L-1高氯酸介质中转变为另一稳定的蓝色配合物,其最大吸收峰位于580nm波长处,铑(Ⅲ)含量为0～0.8μg/mL范围内符合比耳定律,表观摩尔吸光系数为1.81×105L·moL-1·cm-1。该反应具有很高的灵敏度和良好的选择性,大量常见金属离子在一定范围内无干扰。所拟方法操作简单,用于催化剂中微量铑的测定,结果满意。     

KIO4-四硼酸钠系统阻抑亮绿褪色动力学光度法测定痕量Ir（Ⅳ）

基于H2SO4介质及四硼酸钠缓冲溶液中,80℃水浴中,Ir(Ⅳ)对KIO4氧化亮绿褪色反应具有阻抑作用,据此建立了阻抑动力学光度法测定痕量Ir(Ⅳ)的新方法。阻抑反应(吸光度A)与非阻抑反应(吸光度A0)吸光度差值△A与Ir(Ⅳ)的质量浓度ρ在0.0002～0.08μg/mL范围内呈良好的线性关系,检出限为2.969×10-10g/mL。对1μg/25 mL Ir(Ⅳ)标准溶液测定的相对标准偏差为1.7%(n=11)。测定了动力学参数,反应对Ir(Ⅳ)为一级反应,试验条件下,总反应为准一级反应,表观速率系数为2.883×10-4/s,表观活化能为52.2 kJ/mol。方法用于分子筛和活性炭样品中痕量Ir(Ⅳ)测定,加标回收率在98.1%～104.9%范围,符合痕量分析要求。     

Sequential spectrophotometric determination of rhodium and iridium with 1,5-diphenylcarbazide

Rhodium and iridium in mixtures are determined sequentially with 1,5-diphenylcarbazide at pH 5.0. The rhodium complex is formed at 70°C and is extracted into isobutanol for measurement. The iridium complex is then formed by heating for 45 min and measured in aqueous solution. Beer's law is obeyed over the ranges 0.56–2.8 μg ml^?1 for rhodium and 0.53–3 μg ml^?1 for iridium. Pt, Pd, Sn, Co, Ni and Cr can be tolerated in small amounts.     

双氧水活化-面粉酶抑制法测定蔬菜中有机磷农药

基于α-乙酸萘酯和固蓝B在面粉酶的催化作用下生成紫红色的偶氮化合物,而有机磷农药在双氧水的活化下会抑制酶的催化作用,其抑制程度与农药的浓度在一定范围内呈线性关系,由此建立了一种快速测定有机磷农药的方法。探讨了最佳的反应条件,测定甲基对硫磷和甲胺磷的线性范围分别为1~10μg/mL,1~50μg/mL,最低检出限分别为0.1136μg/mL,0.3525μg/mL。该法具有试剂廉价易得、操作简便、迅速的特点,适合果蔬中常见有机磷农药的快速检测。     

Extraction of iridium (IV) from hydrochloric acid media with crown ether in chloroform, and its determination by ICP-AES

A new method for the quantitative extraction and determination of trace amounts of iridium from hydrochloric acid media has been established based on the formation of an ion-association complex of iridium hexachloro anion IrCl6(2-) with dicyclohexyl-18-crown-6 (DC18C6) oxonium cation in chloroform, then determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). The effect of various factors (solvent, acid concentration, crown ether, reagent concentration, shaking time, composition of the extracted species, foreign ions, etc.) on the extraction and back-extraction of iridium has been investigated. The procedure was used to determine traces of iridium in palladium chloride and rhodium chloride.     

Extraction of iridium(IV) from hydrochloric acid media with crown ether in chloroform, and its determination by ICP–AES

A new method for the quantitative extraction and determination of trace amounts of iridium from hydrochloric acid media has been established based on the formation of an ion-association complex of iridium hexachloro anion IrCl₆ ^2– with dicyclohexyl-18-crown-6 (DC18C6) oxonium cation in chloroform, then determination by inductively coupled plasma atomic emission spectrometry (ICP–AES). The effect of various factors (solvent, acid concentration, crown ether, reagent concentration, shaking time, composition of the extracted species, foreign ions, etc.) on the extraction and back-extraction of iridium has been investigated. The procedure was used to determine traces of iridium in palladium chloride and rhodium chloride.     

荧光黄的示波极谱特性研究及其在催化反应-示波极谱分析中的应用

在pH4.9HOAc-NaOAc缓冲溶液中, 荧光黄于-0.50V(vs.SCE)产生一灵敏的单扫描示波极谱波。在100℃弱碱性介质中, 铱(IV)对KIO~4氧化荧光黄这一反应具有强烈催化作用。本文研究了荧光黄的示波极谱行为及利用该催化反应测定痕量铱的各种影响因素,拟定了铱的催化反应-示波极谱分析新方法, 它们的检出限和测定范围分别为0.04ng/mL和0.08-8.0ng/mL。     

甲基绿-高碘酸钾系统催化动力学光度法测定痕量铱(Ⅳ)

基于以H3PO4为反应介质,用HAc-NaAc(1+8)(pH5.7)作缓冲溶液,在沸水浴中加热条件下,痕量铱(Ⅳ)能灵敏地催化高碘酸钾氧化甲基绿的褪色反应,建立了一种测定痕量铱(Ⅳ)的新催化光度法。研究了反应的最佳条件。催化反应吸光度A与非催化反应吸光度A0的差值ΔA与铱(Ⅳ)的质量浓度ρ在0～2.0μg/25mL范围内呈良好的线性关系。检出限为2.97×10-10g/mL。对1μg/25mL铱(Ⅳ)测定的相对标准偏差为1.7%(n=11)。测定了动力学参数。该催化反应对铱(Ⅳ)为一级反应,总反应为准一级反应。反应的表观速率常数为4.613×10-4/s,表观活化能为40.56kJ/mol。该方法用于分子筛样品和活性炭中痕量铱(Ⅳ)的测定,回收率97.9%～104.4%。     

Kinetic Spectrophotometric Determination of Ranitidine

Two spectrophotometric methods were developed for the determination of ranitidine. The first method was a kinetic spectrophotometric method based on the catalytic effect of ranitidine on the reaction between sodium azide and iodine in an aqueous solution. The calibration graph was linear from 4–24 μg/mL. The drug was determined by measuring the decrease in the absorbance of iodine at 348 nm using a fixed time method. The decrease in the absorbance after 1 minute from the initiation of the reaction was related to the concentration of drug. The detection limit of the procedure was 0.76 μg/mL. The proposed procedure was successfully utilized in the determination of the drug in pharmaceutical preparations with mean recovery in the range of 99.83 ? 101.16%. The second method is a colorimetric method, which depends on the measurement of absorbances of tris (o‐phenanthroline) iron(II) [method 2A] and tris (bipyridyl) iron(II) [method 2B] complexes at 512 nm. The complexes obeyed Beer's law over the concentration range of 2–16 μg/mL and 4–40 μg/mL for methods 2A and 2B, respectively. The developed method has been successfully applied for the determination of ranitidine in bulk drugs and pharmaceutical formulations. The common excipients and additives did not interfere in its determination.     

Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples

In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra‐trace amounts of rhodium after adsorption of its 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015–0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values.     

Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aquesous Solution

A selective and sensitive method for determination of platinum and palladium(Ⅱ）in an aqueous solution simultaneously by laser thermal lens spectrometry,based on the complex reaction of 2-(3,5-dichloropyridylazo)-5-dimethylaminoamiline(3,5-diCl-PADMA) with platinum and palladium,has been developed.It is shown that the palladium complex can be fromed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath.By using this difference of reaction temperature and the characteristic of the complexes mentioned above,the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation.The results show that the dynamic linear ranges of determination for platinum and palladium are 0.005-0.04μg/mL and 0.005-0.25μg/mL respectively,and that the detection limits are both 0.002/μg/mL.The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.     

鲁米诺-AuCl4体系化学发光法测定美洛西林钠

在NaOH介质中, AuCl4-氧化鲁米诺产生化学发光, 美洛西林钠显著增强该体系的发光, 据此建立了一种测定美洛西林钠的流动注射化学发光新方法. 在优化的实验条件下, 该法测定美洛西林钠的线性范围为0.01～30 μg/mL, 检出限为3.0 ng/mL, 对1.0 μg/mL美林钠进行了11次平行测定, 其相对标准偏差为1.0%. 方法已用于生物体液和粉针剂中美洛西林钠的测定.     

铑-钨酸盐-罗丹明B缔合显色反应的研究及应用

在聚乙烯醇 (PVA)存在下 ,铑 ( )与钨酸盐及罗丹明 B(RB)形成的离子缔合物在 570 nm处产生最大吸收。建立了测定铑 ( )的光度分析方法 ,其表观摩尔吸光系数 ε达 1 0 7(L·mol-1·cm-1)数量级。方法的检测范围为 0～ 50ng/2 5m L ,检出下限为 0 .2 9ng/2 5m L。大量存在的常见离子对 Rh( )的测定不干扰。用此方法测定了催化剂及工业产品中铑的含量 ,结果与标准方法 (Sn Cl2法 )一致。     

双波长双指示剂催化动力学光度法测定痕量铁

铁是人体健康所必须的微量元素,它对人体的生理功能有一定影响.如果体内可利用的铁不能满足血红蛋白正常合成的需要,致使红细胞增殖能力下降,就会造成缺铁性贫血.相反,体内铁含量过高,又易产生癌症~([1]).     

催化激光热透镜光谱法测定南阳恐龙蛋化石中痕量铱

催化激光热透镜光谱法测定南阳恐龙蛋化石中痕量铱阎宏涛,杨胜科（西北大学化学系,西安,７１００６９）关键词恐龙蛋化石,热透镜光谱法,催化反应,痕量铱的测定近年来,地质学界对白垩－第三纪界线（Ｋ－Ｔ界线）全球性铱的异常给予极大的关注［１］．化石中痕量铱的...     

KBrO3氧化甲基紫褪色动力学光度法测定食品中痕量钒

基于0.004 mol/L的柠檬酸介质中,痕量V(Ⅴ)催化KBrO3氧化甲基紫的褪色反应,建立了测定痕量V(Ⅴ)的动力学光度法。方法的检出限为1.23μg/L,线性范围为0～0.16μg/mL。讨论了酸度、反应物浓度、温度、反应时间、干扰离子等因素的影响,确定了该体系反应的最佳条件。在25 mL溶液中,测定2.0μg V(Ⅴ)的RSD为1.9%(n=11)。方法可用于测定小麦和苹果中的痕量V(Ⅴ),RSD为1.1%～2.7%,标准加入回收率为97.6%～99.0%。     

Flow-injection chemiluminescence determination of tryptophan using galangin-potassium permanganate–polyphosphoric acid system

A high sensitive flow-injection chemiluminescence （FI-CL） method for the determination of tryptophan has been developed. The method is based on the chemiluminescence reaction of galangin-potassium permanganate-tryptophan in polyphosphoric acid （PPA） media. Under the optimized conditions, tryptophan was determined in the range 0.05-10 μg/mL with the detection limit （3tr） of 5.0 × 10^-3 μg/mL. The relative standard deviation （RSD） was 1.0% for 11 replicate determinations of 1.0 μg/mL tryptophan. Three synthetic samples were determined selectively with recoveries in the range from 99.6% to 102.0% in the presence of other amino acids.     

刚果红-孔雀石绿-左氧氟沙星分光光度法测定左氧氟沙星的含量

在pH=3.55的NaAc-HAc缓冲溶液中,左氧氟沙星对刚果红(CR)和孔雀石绿(MG)反应生成的产物在可见光区有明显的作用,在618 nm波长处测定其吸收强度,结果表明体系的吸光度与左氧氟沙星的浓度在2～60μg.mL-1范围内呈现良好的线性关系,线性相关系数R=0.9905,检出限为0.053μg.mL-1。该方法可用于盐酸左氧氟沙星片剂、胶囊以及尿液中左氧氟沙星含量的测定。     

荧光桃红分光光度法测定微量盐酸异丙嗪

在pH 1.85的HCl-NaAc缓冲溶液中,荧光桃红与盐酸异丙嗪依靠静电引力和疏水作用力相互作用形成离子缔合物,其组成比为1∶2,最大褪色波长537 nm,表观摩尔吸光系数ε=4.07×104L.mol-1.cm-1,研究了体系的光谱特征,适宜的反应条件和影响因素,发现体系的吸光度与盐酸异丙嗪的质量浓度在0.04~3.6μg/mL范围内呈良好的线性关系,线性回归方程A=-0.04991-0.1269ρ(μg/mL),线性相关系数r=0.9998,检出限和RSD分别为0.0177μg/mL和2.2%。本法可用于药物制剂中盐酸异丙嗪含量的快速测定。