Capillary electrophoresis and circular dichroism study of trichosanthin and its mutants

A new chromogenic reagent, 2-(2-quinolylazo)-5-diethylaminoaniline (QADEAA) was synthesized. A highly sensitive, selective and rapid method for the determination of silver based on the rapid reaction of silver (I) with QADEAA has been developed. In the presence of sodium citrate-sodium hydroxide buffer solution (pH 6.5) and sodium dodecyl sulfonate (SDS) medium, QADEAA reacts with silver to form a violet complex of molar ratio 1:2 (silver to QADEAA). The molar absorptivity of the complex is 1.39x10(5) l mol(-1) cm(-1) at 580 nm. Beer's law is obeyed in the range of 0.01-0.6 mug ml(-1). The relative standard deviation for 11 replicate samples of 0.2 mug ml(-1) is 1.67%. This method can be applied to the determination of silver in water with satisfactory results.     

5—（2—苯并噻唑偶氮）—8—氨基喹啉作为镍的光度分析试剂及应用研究

研究了新试剂 5- (2 -苯并噻唑偶氮 ) - 8-氨基喹啉与镍的显色反应。在弱碱性介质中 ,阳离子表面活性剂溴化十六烷基三甲基铵存在下 ,试剂与镍形成 3∶ 1的蓝色配合物 ,其最大吸收波长位于 61 0 nm处 ,表观摩尔吸光系数为 1 .2 6× 1 0 5L· mol-1· cm-1,镍的浓度在 0～ 8.0μg/2 5ml范围内 ,符合比耳定律。应用于铝合金中微量镍的测定 ,获得了满意的结果。     

Sensitive spectrophotometric determination of nickel(II) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

A simple, selective and highly sensitive procedure for spectrophotometric determination of nickel has been developed. At pH 5.5, nickel reacts with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in water-ethanol medium to form a red-violet complex which has two absorption maxima, at 520 and 56Onm. The molar absorptivity at 56Onm is 1.26 x 10(5) l.mole(-1).cm(-1). Beer's law is obeyed for 0-15 mug of nickel. Nickel in aluminium alloys and electroplating waste-water has been determined by this method.     

Spectrophotometric determination of silver with 2-(2-quinolylazo)-5-diethylaminophenol as chromogenic reagent

A new chromogenic reagent, 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) was synthesized. A highly sensitive, selective and rapid method for the determination of silver based on the rapid reaction of silver(I) with QADEAP has been developed. In the presence of citric acid-sodium hydroxide buffer solution (pH=5.0) and sodium dodecyl sulfonate (SDS) medium, QADEAP reacts with silver to form a violet complex of a molar ratio 1:2 (silver to QADEAP). The molar absorptivity of the complex is 1.33x10(5) L mol(-1) cm(-1)at 590 nm. Beer' s law is obeyed in the range of 0.01-0.6 micro g mL(-1). The relative standard deviations for eleven replicate samples of 0.2 microg mL(-1) is 1.38%. This method was applied to the determination of silver in water with satisfactory results.     

Spectrophotometric determination of nickel in copper-base alloy with 2-(2-thiazolylazo)-p-cresol

A spectrophotometric method for determination of nickel in copper-base alloy with 2-(2-thiazolylazo)-p-cresol (TAC) is described. The interferences of foreign ions can be eliminated by masking with a mixture of sodium tartrate and sodium thiosulphate. The nickel-TAC complex has low solubility in water, but is soluble in aqueous ethanol. Beer's law is obeyed for 20-70mug of nickel in 50 ml of solution, at pH 5.7. The molar absorptivity at 580 nm is 2.6 x 10(4)l.mole(-1).cm(-1). The method has been applied successfully to determination of nickel in reference samples.     

Spectrophotometric determination of indium in nickel alloys and zinc ores with 1-(2-pyridylmethylideneamine)-3-(salicylideneamine)thiourea

A sensitive method for the spectrophotometric determination of indium with 1-(2-pyridylmethylideneamine)-3-(salicylideneamine)thiourea is proposed. A yellow complex is formed at pH 4.5 (succinate buffer) in a medium containing 40% dimethylformamide, and the absorbance is measured at 415 nm. The molar absorptivity is 6.2 x 10(4)l.mole(-1).cm(-1). The relative standard deviation of the procedure is 1.5%. The method has been applied to determination of indium in a nickel alloy and three zinc ores, with prior isolation of indium by co-precipitation with ammonia and extraction into n-butyl acetate from 5M hydrobromic acid.     

Highly sensitive colour-reaction of nickel with a new chromogenic reagent benzothiaxolyldiazoaminoazobenzene and its application

The synthesis of benzothiaxolyldiazoaminoazobenzene (BTDAB) is described, and a simple, rapid and sensitive procedure for spectrophotometric determination of nickel has been developed. At pH 9.4, in the presence of emulsifier p-octylpolyethyleneglycol phenylether (OP), the reagent reacts with nickel to form a red 1:3 (metal:ligand) complex. The nickel-BTDAB complex exhibit an adsorption maximum at 550 nm with an apparent molar absorptivity of 1.96 x 10(5) 1 mol(-1) cm(-1), Beer's law is obeyed for nickel in the range 0-7 mug per 25 ml. The proposed method has been applied to the determination of nickel in aluminum alloy with satisfactory results.     

新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸分光光度法测定微量钴

近年来,杂环偶氮苯甲酸类显色剂取得了较快的发展。由于氨基取代结构对试剂性能有较大的影响^[1],因此本文合成了新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸,(TAEB)并研究了它与钴的显色反应。     

Selective determination of cobalt using polyurethane foam and 2-(2-benzothiazolylazo)-2-p-cresol as a spectrophotometric reagent

The present work describes a selective, rapid and economical method for the determination of cobalt using the 2-(2-benzothiazolylazo)-p-cresol (BTAC) as a spectrophotometric reagent associated with a solid extraction on polyurethane foam. The BTAC reacts with Co(II) in the presence of Triton-X100 surfactant forming a green complex with maximum absorption at 615 nm. The reaction is used for cobalt determination within a pH range of 6.50-7.50, with an apparent molar absorptivity of 1.62 x 10(4) L mol(-1) cm(-1). Beer's Law is obeyed for a concentration of at least 1.60 microg ml(-1). A selective procedure is proposed for cobalt determination in the presence of Fe(II), Hg(II), Zn(II) and Cu(II) up to milligram levels using masking agents. Polyurethane foam is used for the preconcentration and separation of cobalt from thiocyanate media and this procedure is applied to its determination in nickel salts and steel alloys.     

Extraction and spectrophotometric determination of zinc in coal fly ash and pond sediments with 2-[2-(3,5-dibromopyridyl)azo]-5-dimethylaminobenzoic acid

An extraction-spectrophotometric method is described for the determination of traces of zinc with 2-[2-(3,5-dibromopyridyl)azo]-5-dimethylaminobenzoic acid. The reagent forms a stable, blue 1:2 zinc/reagent complex that can be extracted into chloroform. The apparent molar absorptivity of the zinc(II) complex is 1.26 × 10⁵ l mol^?1 cm^?1 at 610 nm in chloroform. The reagent is relatively selective; interferences from cobalt, copper and nickel can be masked with dimethylglyoxime and aluminium and iron with a mixture of sodium fluoride and triethanolamine. The method is applied to the determination of zinc in coal fly ash and pond sediments with good precision and accuracy.     

2-[2-(6-Methylbenzothiazolyl)azo]-5-Diethylaminobenzoic acid as a new analytical reagent for the spectrophotometric determination of nickel

A new thiazolylazo chromogenic reagent, 2-[2-(6-methylbenzo-thiazoly)azo]-5-diethylaminobenzoic acid (6-Me-BTAEB), has been synthesized. Its chromogenic reaction with microamounts of nickel in the presence of sodium dodecylsulfate (SDS) has been thoroughly studied. 6-Me-BTAEB reacts with nickel(II) in weak acid medium containing appropriate amounts of SDS to form a blue-violet complex with high sensitivity, good selectivity and high stability. The composition is found to be 1:2 (nickel to 6-Me-BTAEB) and its absorption maximum is at 650 nm with an apparent molar absorptivity of 1.67 × 10⁵l mole^–1 cm^–1. Beer's law is obeyed over the range 0-0.4 g of nickel per ml. The proposed method has been applied to the direct determination of nickel in aluminium alloys, pure magnesium and low alloy steels at the 0.2–0.3% (w:w) level with satisfactory results.     

Colour reaction of platinum(II) with 5-(4-nitrophenylazo)-8-(p-toluenesulphonamido)-quinoline and its analytical applications

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of platinum. 5-(4-Nitrophenylazo)-8-(p-toluenesulphonamido)quinoline (NPTSQ) reacts with platinum(II) almost instantaneously in alkaline solution to form a violet-red 1:2 complex with an absorption maximum at 640 nm. Beer's law is obeyed over the concentration range 0-1 mug/ml platinum. The molar absorptivity is 1.37 x 10(5) 1.mole(-1).cm(-1). The method has been used for the determination of microamounts of platinum in catalysts and anode slime.     

Extraction-spectrophotometric determination of trace iron (II) in sea water with 2-[2-(3,5-dibromopyridyl)azo]-5-diethylaminobenzoic acid

An extraction-spectrophotometric method is described for the determination of traces of iron(II) with 2-[2-(3,5-dibromopyridyl)azo]-5-diethyl-aminobenzoic acid. The reagent forms a stable and blue 12 iron/reagent complex that can be extracted into chloroform. The apparent molar absorptivity of the iron(II) complex is 1.09 × 10⁵ 1 mol^–1 cm^–1 at 624 nm in chloroform. The reagent is relatively selective; interferences from cobalt, copper, nickel and vanadium can be removed by using dimethylglyoxime and EDTA. The method is applied to the determination of iron (II) in sea water and aluminium alloys with good precision and accuracy.     

Study of the solid phase extraction and spectrophotometric determination of nickel using 5-(4′-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione in environmental samples

A rapid, sensitive and selective method for the determination of nickel based on the rapid reaction of nickel(II) with 5-(4′-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Ni(II)–CPAHPD complex with C18 membrane disks has been developed. In the presence of pH 6.8 buffer solution and cetylpyridinium bromide (CPB) medium, CPAHPD reacts with nickel to form a red complex of a molar ratio of 1:1 (nickel to CPAHPD). This complex was enriched by solid phase extraction (SPE) with C18 membrane disks. An enrichment factor of 100 was obtained by elution of the complex from the disks with the minimal amount of isopentyl alcohol. The molar absorptivity and Sandell sensitivity of the complex was 3.11 × 10⁵ L mol^?1 cm^?1 and 0.0189 ng cm^?2, respectively at 549 nm in the measured solution. Beer's law was obeyed in the range of 0.01–0.37 μg mL^?1, while that obtained by Ringbom plot was in the range of 0.025–0.35 μg mL^?1. The detection and quantification limits were calculated and found to be 0.003 and 0.01 μg mL^?1. The proposed method was applied to the determination of nickel in water, food, biological and soil samples with good results.     

Spectrophotometric determination of nickel(ii) with molybdophosphoric acid

A sensitive spectrophotometric method for the determination of nickel, based on the reduction of a complex formed between molybdophosphoric acid and Ni(II) at pH 4.3 has been developed. Excess of molybdophosphoric acid is eliminated by complexation with sodium citrate. The method is rapid and the system obeys Beer's law up to 5 ppm of Ni(II). The molar absorptivity is 1.30 x 10(3) 1.mole(-1).mm(-1). The technique compares favourably with existing photometric methods for nickel in sensitivity and is reasonably selective.     

Synthesis and spectrophotometric study of 2-[2-(3,5-dibromopyridyl,)azo] -5-dimethylaminobenzoic acid as an analytical reagent: Determination of nickel

2-[2-(3,5-Dibrornopyridyl)azo]-5-dimethyIam;nobenzoic acid (3,5-diBr-PAMB) has been synthesized and its potential for the spectrophotometric determination of metals studied. It reacts sensitively with nickel, cobalt, iron and copper, and is particularly useful for nickel. The apparent molar absorptivity in chloroform is 1.50 × 10⁵ l mol^-1 cm^-1 and the Sandell sensitivity is 0.4 ng Ni cm^-2. Nickel reacts with 3.5-diBr-PAMB at pH 4–10; at pH 4–7 the complex can be extracted into chloroform to give a stable purple solution. The optimal calibration range is 0.04–0.4 ppm Ni. Only Cu, Co, Fe, Pd and V interfere seriously but Pd, Cu and V can be masked by thiourea.     

Spectrophotometric determination of nickel in biological samples using 1-azobenzene-3-(3-hydroxyl-2-pyridyl)-triazene

A new sensitive and selective chromogenic reagent, 1-azobenzene-3-(3-hydroxyl-2-pyridyl)-triazene (ABHPT), was synthesized. It has been found that ABHPT reacts with nickel(II) in a borax buffer solution (pH 10.0) to form 2: 1 red complexes with the maximum absorption at 530 nm. The apparent molar absorptivity of the complex is 2.6 × 10⁵ L/(mol cm). Most metal ions can be tolerated in considerable amounts, whereby only zinc and mercury may interfere with the determination of nickel(II). Nevertheless, this can be easily eliminated by prior separation with sulfhydryl dextran gel. A new method for the spectrophotometric determination of trace nickel(II) was developed. Beer’s law is obeyed for 0–15 μg of nickel(II) in 25 mL of solution. The limit of quantification, limit of detection, and relative standard deviation are 0.74 ng/mL, 0.25 ng/mL, and 1.0%, respectively. The method has been applied to the determination of trace nickel(II) in biological samples with satisfactory results. The text was submitted by the authors in English.     

6-Chloro-3-hydroxy-2-(5'-methylfuryl)-4H-chromene-4-one as an analytical reagent for micro determination of molybdenum(VI).

6-Chloro-3-hydroxy-2-(5'-methylfuryl)-4H-chromene-4-one (CHMFC) has been used as an analytical reagent for the spectrophotometric determination of molybdenum. Molybdenum(VI) in the presence of several cations, anions and complexing agents forms a yellow 1:2 complex with CHMFC. The complex is quantitatively extractable into 1,2-dichloroethane from 1 mol dm(-3) acetic acid medium and is stable for more than 6 h. The complex shows an absorption maximum at 438 nm with a molar absorptivity of 5.36 x 10(4) dm3 mol(-1) cm(-1) and Sandell's sensitivity equal to 0.0017 microg Mo cm(-2). The method obeys Beer's law up to 1.9 microg Mo ml(-1). The relative standard deviations are 0.2% for solutions and 0.5-1.5% for solid samples. The method is simple, selective, precise and rapid, and has been satisfactorily applied to the micro determination of molybdenum in various synthetic and standard samples.     

Solid phase extraction and spectrophotometric determination of Au(III) with 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine.

A new chromogenic reagent, 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine (HNATR) was synthesized. A highly sensitive, selective and rapid method for the determination microg l(-1) level of Au(III) based on the rapid reaction of Au(III) with HNATR and the solid phase extraction of the colored complex with a reversed phase polymer-based C(18) cartridge have been developed. The HNATR reacted with Au(III) to form a red complex of a molar ratio 1:2 (Au(III) to HNATR) in the presence of 0.05 - 0.5 mol l(-1) of phosphoric acid solution and emulsifier-OP medium. This complex was enriched by the solid phase extraction with a polymer-based C(18) cartridge. The enrichment factor of 100 was achieved. The molar absorptivity of the complex is 1.37 x 10(5) l mol(-1) cm(-1) at 520 nm in the measured solution. The system obeys Beer's law in the range of 0.01 - 3 microg ml(-1). The relative standard deviation for eleven replicates sample of 0.5 microg l(-1) level is 2.18%. The detection limit, based on the three times of standard deviation is 0.02 microg l(-1) in the original sample. This method was applied to the determination of gold in water and ore with good results.     

8-喹啉偶氮显色剂QADCB的合成及其分析性能的研究

报道了8-喹啉偶氮显色剂2-(8-喹啉偶氮)-5-二羧甲氨基苯甲酸(QADCB)的合成、提纯与鉴定,研究了其与Co(Ⅱ)、Ni(Ⅱ)、Fe(Ⅲ)的显色反应,对QADCB与Co(Ⅱ)的显色反应作了研究。在pH5.9的缓冲体系中,试剂与Co(Ⅱ)形成棕红色配合物,其最大吸收波长位于650nm,表观摩尔吸光系数为4.2×104L.mol-1.cm-1,钴量在0~20μg/25mL范围内符合比耳定律。方法简便、快速,选择性较好,已用于纯铜、维生素B12中微量钴的测定,结果满意。