增效试剂在动力学分析法中的应用研究Ⅱ: 锰(Ⅱ)-氨三乙酸-十二烷基硫酸钠-高碘酸钾-罗丹明B催化体系

基于存在活化剂氨三乙酸和增敏剂十二烷基硫酸钠,锰(Ⅱ)催化高碘酸钾氧化罗丹明B的反应,拟定了测定痕量锰的新催化光度法.讨论了有关的反应机理.本法由于添加了表面活性剂,灵敏度提高3.4倍.测定锰含量线性范围为10～120ng·25mL~(-1),相对标准偏差为2.6%(n=9),检出限为8.O×10~(-11)g·mL~(-1).用于测定水样和酒样中锰.     

催化动力学分光光度法测定痕量锰(Ⅱ)

研究了氢氧化钠介质中 ,痕量锰催化过氧化氢氧化桑色素褪色反应及其动力学条件 ,建立了催化动力学测定痕量锰的新方法。Mn (Ⅱ )的测定线性范围为 0 0 0 5～ 0 0 60 μg/2 5mL ,检出限为 7 8× 1 0 - 10 g·mL- 1。用于大米中痕量Mn (Ⅱ )的测定 ,结果满意。     

用锰(Ⅱ)-氨三乙酸-溴代十六烷基三甲胺-高碘酸钾-灿烂甲酚蓝体系催化光度法测定锰

基于存在活化剂氨三乙酸和增敏剂溴代十六烷基三甲胺，锰（Ⅱ）催化高碘酸钾氧化灿烂甲酚蓝的反应，拟定了测定痕量锰的催化光度法，讨论了有关反应机理。本法由于添加了溴代十六烷基三甲胺，灵敏度揭高2．5倍，测定锰含量线性范围为8．0×10－4～8．0×10－3mg／L，检出限为7．0×10－5mg／L，相对标准偏差为4．7％（n＝11），可用于测定茶叶和水样中的锰。     

流动注射催化光度法测定痕量锰——NTA-Mn(Ⅱ)-碱性品红-KIO_4体系

本文基于在pH4.6的乙酸-乙酸钠缓冲体系中,氨三乙酸存在下,Mn(Ⅱ)对KlO_4氧化碱性品红褪色有显著地催化作用,将这一新指示反应和流动注射分析技术结合起来,建立了流动注射催化光度法测定痕量锰的新方法.该法灵敏、快速、操作简便.线性范围为Mn(Ⅱ)0～0.35μg·ml~(-1),分析速度为24次·h~(-1).用于水样、土壤、粮食中锰的测定,结果令人满意.对环境水质标样(CWO108)五次平行测定的相对标准偏差为1.3%.     

催化光度法测定痕量Mn(Ⅱ)的研究——Mn(Ⅱ)-铍试剂Ⅲ-H_2O_2体系

研究了0.10mol·L~(-1)氨水介质中,Mn(Ⅱ)催化H_2O_2氧化铍试剂Ⅲ退色的反应,选择了最佳反应条件下。方法的检出限为2.0×10~(-10)g·ml~(-1),线性范围为0.4～20.0ng·ml~(-1)。本法简单灵敏、选择性较好,可直接测定茶叶中Mn(Ⅱ)含量。     

溴酸钾-溴酚蓝-锰(Ⅱ)催化体系的研究及其在测定抗坏血酸中的应用

基于在pH 3.6的HOAc-NaOAc介质中,抗坏血酸对溴酸钾、溴酚蓝、锰(Ⅱ)催化体系具有显著的活化作用,建立了测定抗坏血酸的方法。线性范围为10~125μg/25 mL,检出限为3.44×10-5g.L-1,用于药品、饮料中抗坏血酸的测定,结果满意。     

催化光度法测定痕量猛——高碘酸钾-Mn(Ⅱ)-邻菲啰啉-溴酚蓝体系

本文以高碘酸钾-溴酚蓝为指示反应,在活化剂邻菲(口罗)啉存在下建立了催化光度法测定痕量锰(Ⅱ)的新方法,方法灵敏度为6×10~4μg/ml。线性范围为0.00—0.60μg/15ml,应用于标准铝合金及茶叶中痕量锰的测定,结果令人满意。     

高灵敏催化光度法测定痕量锰

研究了痕量Mn2 + 催化KIO4 氧化棉红的反应动力学 ,测定了反应级数、表观速率常数和表观活化能 ,确立了速率方程 ,探讨了反应机理 ,建立了测定痕量锰的方法 ,方法灵敏度为 7.5×10 - 9g·L- 1,线性范围为 0 .0～ 6.0× 10 - 6g·L- 1。方法选择性好 ,直接用于化学试剂、井水及蒸馏水中痕量锰的测定 ,结果满意     

流动注射催化吸光光度法测定人发中痕量锰

探讨实现结晶紫-KIO4-NTA-Mn2+体系的流动注射催化吸光光度测定痕量锰的条件,方法的检出限为3×10-4μg·ml-1,线性范围0～8×10-3μg·ml-1。采用停流法测定人发中锰的结果与石墨炉原予吸收法相近,回收率为102%,RSD为4.2％(n=6),采样速率为10次·h-1。     

锰(Ⅱ)存在下用二安替比林苯乙烯甲烷分光光度法测定水中微量铬(Ⅵ)

文献[1]报道了二安替比林苯乙烯甲烷测定部分变价元素有较高灵敏度。章道昆指出有锰(Ⅱ)存在时钒(Ⅴ)、铈(Ⅳ)灵敏度显著增加。本研究同样发现有锰(Ⅱ)存在时该试剂使铬(Ⅵ)的摩尔吸光系数由2.5×10~4l·mol~(-1)·cm~(-1)增至1.5×10~5l·mol~(-1)·cm~(-1),为微量铬(Ⅵ)的测定提供了迄今为止文献尚未报道的新方法。     

新型固相分光光度法测定茶叶中痕量锰的研究

系统地研究了 Mn( ) -1 -( 2 -吡啶偶氮 ) -2 -萘酚 ( PAN)在石蜡相中的显色反应。在 NH3-NH4Cl( p H=1 0 .0 )缓冲介质中 ,此有色络合物能定量被石蜡萃取 ,锰量在 0～ 1 0μg/30 m L范围内符合比耳定律 ,建立了测量锰的新型固相分光光度法。方法的检出限为1 .6× 1 0 - 9g/m L。应用于茶叶中痕量锰的分析 ,结果良好。     

铜(Ⅱ)催化PHA的褪色反应特性及应用

本文研究了铜(Ⅱ)催化抗坏血酸还原多卤代变色酸双偶氮胂类试剂(PHA)的褪色反应特性, 讨论了试剂结构对褪色反应动力学特性的影响, 探讨了反应机机。以三氯偶氮胂为代表, 拟定了测定痕量铜(Ⅱ)的新方法, 其检出限为3.06×10^-^1^2g/mL, 线性范围为0~28ng/10mL。用于生物材料中痕量铜(Ⅱ)的测定, 结果满意。     

分光光度法测定化学试剂中痕量钙

在pH10.4的NH3 NH4Cl介质中,Ca2+与DBC 偶氮氯膦生成1∶1蓝色络合物.络合物的最大吸收波长位于624nm,方法的表观摩尔吸光系数ε624nm=3.82×104L·mol-1·cm-1,钙量在0～25μg/25mL范围内遵守比尔定律.本法用于化学试剂KCl,NaCl及NaNO3中痕量钙的测定,得到了满意的结果.     

Rapid spectrophotometric determination of chromium(III)

A spectrophotometric procedure is suggested for the determination of Cr(III). The reaction between Cr(III) and 2-(5-bromo-2-pyridylazo)-5-dimethylaminophenol is accelerated by sodium dodecyl sulphate(SDS), sodium benzoate causes a further increase in the absorbance of the chelate. The optimum pH range for the reaction is 5-5.8(benzoate buffer). The chelate exhibits maximum absorbance at 590 nm, obeys Beer's law over the concentration range 0.02-0.56 microg/ml of Cr(III), has molar absorptivity of 7.8 x 10(4) 1. mol(-1) cm(-1) and a Sandell sensitivity of 0.66 ng/cm. The metal to ligand ratio is 1:2 in the absence of SDS and 1:1 in its presence. A procedure for the determination of Cr(III) and Cr(VI), when present together, is described. The method has been applied to the analysis of Cr(III) in tap water.     

Determination of procaine hydrochloride by ion-pairing flow injection analysis with piezoelectric detection

A fast and simple method for the determination of procaine hydrochloride by ion-pairing flow injection analysis has been developed. It is based on the formation of an ion-pair with sodium dodecyl phenylsulphonate and piezoelectric detection. The calibration curve was linear between 0.02 and 2.00 mg/mL, with a detection limit of 0.01 mg/mL, a relative standard deviation of 0.3% (10 replicates) and a sampling frequency of 120/h. The proposed method has been satisfactorily applied to the determination of procaine hydrochloride in pharmaceutical preparations.     

新显色剂对胂酸基苯基重氮氨基偶氮苯的合成 及其与Cd(Ⅱ)的显色反应研究

合成了对胂酸基苯基重氮氨基偶氮苯并对其与Cd(Ⅱ)的显色反应进行了初步研究。在pH 10．5的碱性介质中，在Triton X-100存在下，试剂与Cd(Ⅱ)的显色反应有较高灵敏度，摩尔吸光系数ε472=9．1×104L·mo1-1·cm-1，在0～10μg／25 mL范围内遵守比耳定律。方法应用于分离后的井水和湖水中Cd(Ⅱ)的测定，结果满意。     

Determination of procaine hydrochloride by ion-pairing flow injection analysis with piezoelectric detection

A fast and simple method for the determination of procaine hydrochloride by ion-pairing flow injection analysis has been developed. It is based on the formation of an ion-pair with sodium dodecyl phenylsulphonate and piezoelectric detection. The calibration curve was linear between 0.02 and 2.00 mg/mL, with a detection limit of 0.01 mg/mL, a relative standard deviation of 0.3% (10 replicates) and a sampling frequency of 120/h. The proposed method has been satisfactorily applied to the determination of procaine hydrochloride in pharmaceutical preparations. Received: 19 August 1996 / Revised: 6 November 1996 / Accepted: 12 December 1996     

Simultaneous determination of digoxin and digitoxin by micellar electrokinetic chromatography and application to drug formulations

A simple micellar electrokinetic chromatographic method is described for simultaneous determination of digoxin and digitoxin. The simultaneous analysis of digoxin and digitoxin was performed in Tris buffer (10 mM; pH 9) with 90 mM sodium dodecyl sulfate and 10% isopropyl alcohol as an anionic surfactant and organic modifier. Under these conditions, good separation with high efficiency is achieved in short analysis times. Several parameters affecting the separation of the drugs were studied, including the pH and concentrations of the Tris buffer and sodium dodecyl sulfate. The linear range of the method for the determination of digoxin and digitoxin was over 0.01–0.3 mg/mL; the detection limit (signal to noise ratio = 3; injection 3.5 kPa 3 s) was 4 and 6 μg/mL, respectively. Application of the proposed method to the determination of digoxin in commercial tablets and in injections proved to be feasible.     

Spectrofluorimetric determination of trace amounts of Ga(III) in aluminium and biological samples with 1-(2-pyridylazo)-2-naphthol in sodium dodecyl sulphate micellar medium

Summary A spectrofluorimetric method is proposed for the determination of gallium with 1-(2-pyridylazo)-2-naphthol as derivative reagent in sodium dodecyl sulphate micellar medium. Sensitivity is increased by a factor of 20 with respect to that obtained in 20% ethanol medium. The stoichiometry of the complex is 11. Optimum working conditions are about pH 4, 0.3% sodium dodecyl sulphate and absence of ethanol. The calibration graph is linear in the range 5–400 ppb of Ga(III) with a variation coefficient of 1.5% at 210 ppb of Ga for 10 replicates, and detection limit is 0.8 ppb. Main interferences are from copper and cobalt. Results obtained in the determination of Ga(III) in urine and aluminium samples show the validity of the method proposed.

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Spektrofluorimetrische Bestimmung von Spuren Ga(III) in Aluminium und biologischen Proben mit 1-(2-Pyridylazo)-2-naphthol in micellarem Natriumdodecyl-sulfatmedium

     

高碘酸钾氧化酚藏花红催化光度法测定痕量钴(Ⅱ)

在HAc-NaAc(pH=4.0)缓冲溶液中,以氨三乙酸为活化剂,痕量钴(Ⅱ)可催化KIO4氧化酚藏花红褪色反应。研究了反应的最佳条件,测得反应表观活化能为65.23kJ.moL-1,据此建立了一种测定痕量钴(Ⅱ)的新方法。方法线性范围为0.010～1.20μg/25mL,检出限为8.84×10-10 g.mL-1,回收率为94%～103%,相对标准偏差(RSD)为3.6%～5.1%。该法用于粮食样品中钴(Ⅱ)的测定,结果满意。