Spectrophotometry Determination of Cobalt after Extraction of its Ternary Complex with 3-(4-Phenyl-2-Pyridyl)-5,6-Diphenyl-1,2,4-Triazine and Tetraphenylborate into Molten Naphthalene

The reaction of 3-(4-phenyl-2-pyridyl)-5,6-diphenyl-1,2,4-triazine (PPDT) and tetraphenylborate (TPB) with cobalt (II) has been studied to determine the optimum conditions for the extraction and quantitative spectrophotometry determination of this metal. The ternary complex is extracted into molten naphthalene at pH 3.6–7.4. The solid naphthalene containing the cobalt associated complex is separated by filtration and dissolved in acetonitrile. Beer's law is obeyed in the concentration range 8–140 μg cobalt in 10 ml of acetonitrile solution. The molar absorptivity and sensitivity are 4.2×10³ l·mol^?1·cm^?1 and 0.01408 μg/cm², respectively. The other factors such as pH, amounts of reagents and naphthalene, shaking and standing times, and the effect of diverse ions are studied. The method has been applied to the determination of cobalt in iron steel alloys.     

Atomic Absorption Spectrophotometric Determination of Copper(II) after Adsorption of its Oxinate on Microcrystalline Naphthalene

A New Atomic Absorption Spectrophotometric Procedure Has Been Developed For The Microdetermination Of Copper(Ii) As Its Oxinate By Its Adsorption On Micro-Crystalline Naphthalene And Dissolution In 1 N Nitric Acid. Copper(Ii) Oxinate Is Quantitatively Adsorbed In The PH Range Of 3.2–10.1 And Trace Amounts Of Copper Can Be Determined. The Effect Of Variables Such As Reagent And Naphthalene, Shaking Time, Digestion Time, And Diverse Ions Are Studied. The Proposed Method Has Been Applied To The Determination Of Copper In Standard Reference Material (Zinc Alloy), And Metallic Zinc And Lead.     

Atomic Absorption Spectrophotometric Determination of Copper (I) after Adsorption of its 4′-(p-Methoxyphenyl)-2, 2′:6′, 2″-Terpyridine Tetraphenylborate Ion-Associated Complex on Microcrystalline Naphthalene

A new atomic absorption spectrophotometric method has been developed for the trace determination of copper after adsorption of its 4′-(p-methoxyphenyl)-2, 2′:6′,2″-terpyridine tetraphenylborate ion-associated complex on microcrystalline naphthalene. This complex is adsorbed on microcrystalline naphthalene in the pH range 0.5-11.0 by shaking for a few seconds. The solid mass so formed is separated by filtration, dissolved in dimethylformamide and the absorbance is measured at 324.7 nm. Beer's law is obeyed in the concentration range 5.0-60.0 μg of copper in 10 ml of the final dimethylformamide solution. The replicate determinations of a sample containing 30 μg of copper gave a mean absorbance of 0.171 with a standard deviation of 0.0019 and a relative standard deviation of 1.11%. The method has been applied to the determination of copper in certain standard reference materials.     

微晶萘固相萃取分离富集及ICP—AES测定Cu,Mn的研究

报道以微晶萘作吸附载体的固相萃取分离及ＩＣＰ－ＡＥＳ测定Ｃｕ，Ｍｎ的新方法，详细研究了溶液酸度，试剂浓度，萘用量及共存离子对待测物回收率的影响，考查了加入适量的Ｃｏ＾２＋，对富集痕量Ｃｕ＾２＋Ｍｎ＾２＋辅助作用，本法用于生物样品马尾藻及小牛肝中Ｃｕ，Ｍｎ的测定，分析结果与标准值吻合。     

Trace Analysis of Nickel by Extraction-Atomic Absorption Spectrophotometry Determination of its Acenaphthenequinone Dioxime Complex in Molten Naphthalene

A procedure is described for the trace analysis of nickel using the liquid-liquid extraction of nickel acenaphthenequinone dioxime complex with molten naphthalene followed by solid-liquid separation. Nickel complex cannot be extracted into any non-aqueous organic solvents, but can be quantitatively extracted into molten naphthalene. It is very stable at high temperature and is dissolved in the mixed solvent (HNO₃-DMF). The absorbance of the solution was measured at 231.5 nm against a reagent blank. Beer's law is followed in the concentration range of 5–100 μg of nickel in 10 ml of the final solution. The sensitivity for 1% absorption is 0.155 μg/ml nickel. The relative standard deviation is 1.0% for ten replicate determinations of 60 μg of nickel. The interference of various ions has been studied and the method has been applied to the determination of nickel in aluminium alloys.     

Complex Formation Equilibria of Iron(III) With 2-Hydroxy-3- Pyridinol and 2-Mercapto-3-Pyridinol. Spectrophotometry Determination of Iron(III) In Multivitamins

ABSTRACT

The complex equilibria of iron(III) with 2-hydroxy-3-pyridinol (HHP), and 2-mercapto-3-pyridinol (MHP) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaCIO₄). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance pH-graphs. After considering all the different parameters a simple, rapid, sensitive and selective method for spectrophotometric determination of trace levels of iron(III) was proposed based on the formation of (Fe -MHP) complex at pH 2.5 (λ_max = 640 nm, ? = l×10⁴ L mol^?1 cm^?). The interference of a large number of foreign ions was investigated. The method has been applied successfully for the determination of iron content in some multivitamins with mineral preparations and infant milk products.     

2-(2-喹啉偶氮)-4-甲基-1, 5-苯二酚测定银的研究

合成了新试剂2-(2-喹啉偶氮)-4-甲基-1,5-苯二酚(QAMDHB),研究了其与银的显色反应.在pH=4.7的乙酸-乙酸钠缓冲介质中,QAMDHB与银反应生成2∶1的稳定络合物,λmax=558 nm,ε=5.8×104 L*mol-1*cm-1,银含量在0～1.6 mg/L内符合比耳定律.方法用于环境废水中银含量的测定,结果满意.     

Direct and Second Order Analogue Derivative Extraction-Spectrophotometric Determination of Iron with 2 (4, 5-Dimethyl-2-Thiazolylazo)-4, 6-Dimethylphenol

Abstract

An extraction-spectrophotometric method for the determination of trace amounts of iron based on its extraction into chloroform with 2-(4, 5-dimethyl-2-thiazolylazo)-4, 6-dimethylphenol has been developed, which allows the determination of 5–28 μg Fe (?₇₇₃ = 1.38×10⁴ 1. mol^?1. cm^?1). The use of second order analogue derivative spectrophotometry allows the determination of down to 0.2–5 μg, Fe. The methods are quite selective and have been applied to the determination of iron in mineral waters.     

新试剂5-(4-氯苯基偶氮)-8-苯磺酰氨基喹啉光度法测定微量铜

在 p H 8.5的 Na2 B4 O7- HCl介质及有氯化十六烷基吡啶 ( CPC)存在时 ,室温下铜 ( )与 5 - ( 4 -氯苯基偶氮 ) - 8-苯基磺酰氨基喹啉 ( CPBSQ)迅速反应 ,生成络合比为 1∶ 3的有色络合物。研究了反应的最佳条件 ,建立了一个测定 Cu( )的光度分析新方法。Cu( )的浓度在 0～ 1 4.0 μg/2 5 m L 范围内符合比耳定律 ,其摩尔吸光系数为 8.1 2× 1 0 4 L· mol- 1· cm- 1。方法用于面粉、茶叶及奶粉中铜的测定 ,其相对标准偏差为 0 .5 8%～ 1 .2 % ,标准加入回收率为 95 .5 %～ 1 0 4 .5 %。     

水中痕量钼(Ⅵ)的4-(2-吡啶偶氮)-间苯二酚螯合活性炭吸附富集分光光度法测定

提出了一种简单快速预富集水中痕量钼（Ⅵ）的新方法，方法的机理在于4－（2－吡啶偶氮）－间苯二酚（PAR）与钼（Ⅵ）螯合后被活性炭中附，然后用NaOH解吸下来，再用水杨基荧光酮与钼（Ⅵ）显色，分光光度法测定钼（Ⅵ）的含量；详细研究了影响Mo-PAR螯合物定量吸附于活性炭上的各种参数，找出了最佳吸附－解吸条件，包括吸附酸度、PAR用量、吸附时间、解吸酸度等；该法的主要优点是操作简单、快速，干扰小，避免了常规方法中用浓硝酸消化活性炭费时和污染大的解吸方法，该法已用于测定水中痕量钼（Ⅵ），加标回收率达到94％－97％。     

铟(Ⅲ)-7-(1-苯偶氮)-8-羟基喹啉-5-磺酸钠的配位吸附波及其应用

在ｐＨ４．５的 ０．０１５ ｍｏｌ／Ｌ ＨＡｃ－ＮａＡｃ介质中，Ｉｎ铟（Ⅲ）－７－（１－苯偶氮）－８－羟基喹啉－５－磺酸钠（ＢＱ）在滴汞电极上于－０．６６５－０．７０ Ｖ（ｖｓ．ＳＣＥ）电位处得到络合物的吸附还原波，其一阶导数峰电流Ｉ＇ｐ与Ｉｎ（Ⅲ）浓度在４．０× １０~（－８）～３．５ × １０~（－６）ｍｏｌ／Ｌ范围内呈良好的线性关系，检测限为１．６ × １０~（－８）ｍｏｌ／Ｌ Ｉｎ（Ⅲ）．应用该法测定了铅粉和氢氧化铝样品中的微量铟，结果令人满意。对电极反应机理进行了探讨。     

Determination of Lithium in Pharmaceutical preparations with 1-(2-Arsenophenylazo)-2-Hydroxy 3, 6-Naphthalendisulfonic Acid

Abstract

This paper reports the characteristics, in acetonic medium, of the lithium complex with 1-(2-arsenophenylazo)2-hydroxy 3,6-naphthalenedisulfonic acid (APHNDS).The analytical optimization is also reported. The coloured product was measured spectrophotometrically at 468 nm. The Beer's law was realized at 0.1–4.0 μg ml^?1. The method was used for the determination of lithium in pharmaceutical preparation. The reproducibility of the described method was efficient. The accuracy of the procedure was evaluated measuring the recovery, between 86.0–97.9 %.     

2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚-BrO_3~--SCN-三元离子缔合物测定微量BrO_3~-的研究

本文研究了5-Br-PADAP在酸性介质中质子化,与BrO_3~-和SCN~-形成三元离子缔合物的最佳条件,其表观摩尔吸光系数ε_(540)=4.3×10~4L·mol~(-1)·cm~(-1),缔合物组成比为:5-Br-PADAP:BrO_(3-)SCN~-=1:1·1。提供了测定微量BrO_(3-)的新方法,可应用于化学试剂中微量BrO~(3-)的测定。此外,本文还探讨了反应机理。     

新试剂1-(6-硝基-2-苯并噻唑)-3-(4-硝基苯)-三氮烯与锌的显色反应研究及应用

研究了新显色剂１－（６－硝基－２－苯并噻唑）－３－（４－硝基苯）－三氮烯（ＮＢＴＮＰＴ）与锌的显色反应，在非离子表面活性剂ＴｒｉｔｏｎＸ－１００存在下，ｐＨ１０．１～１０．８的Ｎａ２Ｂ４Ｏ７－ＮａＯＨ缓冲溶液中，Ｚｎ２＋与试剂能形成１∶２的橙黄色配合物，最大吸收波长为４４６ｎｍ，同时在５２８ｎｍ处配合物表现有最大负吸收，其表观摩尔吸光系数分别为ε＝７．０３×１０４Ｌ·ｍｏｌ－１·ｃｍ－１和ε＝１．０６×１０５Ｌ·ｍｏｌ－１·ｃｍ－１．用拟定的方法测定了人发和婴儿奶粉中的微量锌，结果令人满意．     

1—（2—羟基—3,5—二硝基苯基）—3—［4—（苯基偶氮）苯基］—三氮烯与汞的显色反

研究了1-（2-羟基-3,5-二硝基苯基）-3-[4（苯基偶氮）苯基]-三氮烯（HDNPAPT）试剂与汞离子的显色反应。在非离子表面活性剂TritonX-100存在下,pH10．3的NH3·H2O-NH4Cl介质中,汞与HDNPAPF形成1：4的红色络合物,表观摩尔吸光系数ε525＝1．63×105·mol-1·cm－1,汞离子浓度在0～0．64mg/L范围内符合比尔定律。方法应用于废水中微量汞的测定。     

BTAB与铁形成的配合物组成的研究

研究了3 -(6-溴苯并噻唑-2-偶氮)- 2,6-二羟基苯甲酸(简称BTAB)与铁的配合反应.用摩尔比法、等摩尔连续变化法、平衡移动法和双峰双波长法四种方法详细研究并测定了3 -(6-溴苯并噻唑 -2-偶氮)- 2,6-二羟基苯甲酸与铁显色形成配合物的配合比和稳定常数,建立了光度法测定铁的新方法.结果表明,在溴代十六...     

Selective Spectrophotometric Determination of Palladium (II) With 2-(5-Bromo-2-Pyridylazo)-5-(Diethylamino)-Phenol

Abstract

A spectrophotometric study of the Pd(II) complex of a reagent 2-(5-Bromo-2-Pyridylazo)-5-(diethylamino)-Phenol (5-Br-PADAP) is presented. A violet complex is formed at pH 3.53, and shows maximal absorbance at 585 nm with molar absorptivity of 3.86 × 10⁴ 1. mol^?1 cm^?1. Beer's law is obeyed up to 50 μ of Pd(II). The method offers the advantages of simplicity, high precision, requires no extraction and is very selective, where 5.0 mg Pt(VI) and 0.3 mg Au(III) ions do not interfere.     

Iron(II) complex of 2-(1H-pyrazol-1-yl)pyridine-4-carboxylic acid (ppCOOH) suitable for surface deposition

Abstract

The synthesis, structural and magnetic characterization of the tris iron(II) complex of 2-(1H-pyrazol-1-yl)pyridine-4-carboxylic acid (ppCOOH) ligand are reported in [Fe(ppCOOH)₃](ClO₄)₂·0.5H₂O·2EtOH. Single crystal structure and magnetic characterization of the bulk compound show that the low-spin state is dominant from 2 to 400 K. ESI-MS and UV–Vis spectroscopy experiments indicate that acetonitrile solutions of this complex are stable with time. ESI-MS confirms the presence of the tris complex in solution. This complex can be deposited onto SiO₂ surfaces due to the presence of carboxylic acid groups by immersing the substrates into acetonitrile solutions of the complex. XPS spectra of the deposited complex are similar to those of the bulk sample. AFM images show a slight increase in roughness with respect to the naked substrate and the absence of aggregates. These results are consistent with the formation of a monolayer of the complex on the surface.     

新显色剂2-(2-咪唑偶氮)-5-二甲氨基苯甲酸与镍(Ⅱ)的显色反应研究

研究了新显色剂2-(2-咪唑偶氮)-5-二甲氨基苯甲酸(IZDBA)与Ni(Ⅱ)的显色反应。结果表明,在pH 6.0的HAc-NaAc缓冲溶液中,IZDBA可与Ni(Ⅱ)形成一种配合比为2∶1的稳定红色配合物,其最大吸收波长位于580 nm处,而试剂的最大吸收波长为390nm,对比度为190 nm。配合物的表观摩尔吸光系数为2.95×104L.mol-1.cm-1;Ni(Ⅱ)量在0~0.8 mg/L范围内遵守比耳定律。在硫脲和氟化铵存在下,方法可直接用于测定镍催化剂和铸造铝合金中的微量镍。本法与原子吸收光谱法相对照,结果基本一致。     

1-(6-硝基-2-苯并噻唑)-3-(5-溴-8-喹啉)-三氮烯与Co(Ⅱ)的高灵敏显色反应及其应用

报道了在CPB 存在下,新试剂1-(6-硝基-2-苯并噻唑)-3-(5-溴-8-喹啉)-三氮烯(NBTBQT)与钴的显色反应.在pH 9.5的硼砂-NaOH缓冲介质中,试剂与钴形成2:1 深蓝色络合物,其最大吸收波长位于655 nm处,表观摩尔吸光系数为1.94×105 L·mol-1·cm-1,钴的质量浓度在0～0.24 mg/L 的范围内符合比尔定律.方法应用于维生素B12注射液和水系沉积物的测定.