Interaction of nickel with 4-(2'-benzothiazolylazo) salicylic acid (BTAS) and simultaneous first-derivative spectrophotometric determination of nickel(II) and iron(III)

The solution properties of nickel complex with 4-(2'-benzo-thiazolylazo) salicylic acid (BTAS) have been studied by zero-order absorption spectrophotometry in 40% (v/v) ethanol at 20 degrees C and an ionic strength of 0.1 mol dm(-3) (KNO(3)). The equilibria that exist in solution were established and the basic characteristics of complexes formed were determined. A new direct spectrophotometric method for the determination of trace amounts of the nickel is proposed based on the formation of the Ni (BTAS) complex at pH 7.0. The absorption maximum, molar absorbtivity, and Sandell's sensitivity of 1:1 (M:L) complex are 525 nm, 0.6 x 10(4) l mol(-1) cm(-1) and 2.824 x 10(-9) microg cm(-2), respectively. The use of first-derivative spectrophotometry eliminates the interference of iron and enables the simultaneous determination of nickel and iron using BTAS. Quantitative determination of Ni(II) and Fe(III) is possible in the range (0.59-7.08) and (2.1-8.4) microg ml(-1), respectively with a relative standard deviation of 0.5%. The proposed method has been successfully applied to the simultaneous spectrophotometric determination of nickel and iron in steel alloys and aluminum alloys.     

Determination of nickel with 2-(2-quinolylazo)-5-diethylaminoaniline as a chromogenic reagent.

A sensitive, selective and rapid method for the determination of nickel based on a rapid reaction of nickel(II) with 2-(2-quinolylazo)-5-diethylaminoaniline (QADEAA) has been developed. In the presence of pH = 6.0 ammonia-ammonium chloride buffer solution and sodium dodecyl sulfonate (SDS) medium, QADEAA reacts with nickel to form a violet complex having a molar ratio of 1:2 (nickel to QADEAA). The molar absorptivity of the complex is 1.38 x 10(5) l mol(-1) cm(-1) at 595 nm. Beer's law is obeyed in the range of 0.01-0.4 microg/ml. This method had been applied to the determination of nickel with good results.     

Quinoline-2-aldehyde thiosemicarbazone (QAT) as spectrophotometric reagent for palladium and nickel

A procedure is described for the extractive spectrophotometric determination of nickel and palladium with quinoline-2-aldehyde thiosemicarbazone. At pH 7.5 nickel forms a 1:2 complex which is soluble in chloroform and has an absorption maximum at 460 nm. Palladium forms a 1:2 complex with maximum absorbance at 510 nm which can be extracted into MIBK from 1M HCl. Both complexes are stable and conform to Beer's law. The molar absorptivities for nickel and palladium are 1.58 x 10(4) and 2.6 x 10(3) 1.mole(-1). cm(-1) respectively. The proposed method is suitable for detection and determination of nickel and palladium in the presence of associated metal ions. The results of the analysis of synthetic mixtures and standard samples are reported.     

镍—亚硝基红盐—氯化癸基吡啶体系的络合物吸附波研究及应用

在0.020mol/硼砂-0.0030％亚硝基红盐-0.0040％氯化癸基吡啶体系中,镍有一灵敏的络合物吸附波,峰电位-0.55V(υs. Ag/AgCl),线性范围0.2～1600ng/ml,可用于水样和发样的测定。镍与亚硝基红盐形成1:3的二元络合物。络合物在滴汞电极上的吸附,低浓度符合Langmuir吸附等温线,高浓度符合Frumkin吸附等温线。     

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。     

Cathodic stripping voltammetric determination of 2-mercaptobenzothiazole using the catalytic cobalt peak

Previously, thiols have been determined indirectly by cathodic stripping voltammetry (CSV) after accumulation as their mercury and copper(I) salts. Following a previous report of the first use of the catalytic nickel peak (for the determination of cysteine), this paper reports the first use of the catalytic cobalt peak in CSV (for the determination of 2-mercaptobenzothiazole (MBT)): only a very ill-defined catalytic cobalt peak had been observed previously with cysteine, and was unreported. MBT is accumulated at pH 4 (Britton-Robinson buffer) as its cobalt(II) complex at -0.1 V, and is then determined indirectly by observing the reduction of the cobalt(II) in the complex at -0.95 V, i.e., with a much lowered overpotential: hydrated cobalt(II) is reduced at -1.2 V. The peak is catalytic because the thiol released on reduction of the complex complexes further cobalt ions and causes their reduction. The detection limit for the determination of MBT was calculated to be 2.5 x 10(-9) M (3sigma) using an accumulation time of 1 min. The sensitivity is about three times that obtained with the corresponding catalytic nickel peak.     

Sequential extraction and determination of copper and nickel with 2,4-dihydroxyacetophenone thiosemicarbazone

2,4-Dihydroxyacetophenone thiosemicarbazone (DAPT) forms a 1:1 complex with copper(II) which can be extracted into n-butanol or ethyl acetate from acetic acid-sodium acetate (pH 5.0) buffer, and a 1:1 nickel(II) complex which can be extracted into n-butanol from ammonium chloride-ammonia (pH 7.5) buffer. The difference between the pH(1 2 ) values for extraction of the two complexes is 3.4 and this has been exploited for their sequential extraction and determination. The molar absorptivities for the copper and nickel complexes are 1.5 x 10(4)l.mole(-1).cm(-1) at 390 nm and 8.2 x 10(3)l.mole(-1).cm(-1) at 385 nm respectively. The procedure has been applied to the analysis of cupronickel.     

Zero-crossing second derivative spectrophotometry for simultaneous determination of palladium and nickel using 1-(2-pyridylazo)-2-naphthol in mixed micellar solutions

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous determination of nickel and palladium at trace levels. PAN complexes of nickel and palladium in the pH 1.98 form red and green colored complexes, respectively, which are soluble in aqueous 4:1 Triton X-100 to sodium dodecylsulfate (SDS) micellar media with total detergent concentration of 3.2%. Under optimum conditions, calibration graphs for the simultaneous determination by second derivative spectrophotometry were obtained. Zero crossing second derivative spectrophotometry at 668 and 572 nm, respectively for palladium and nickel was used for the simultaneous determination. The method is able to determine palladium to nickel ratio 70:1 to 1:6 (Wt/Wt), accurately. Accuracy and reproducibility of the determination method on the known various amounts of palladium and nickel in their binary mixtures were tested. Effects of diverse ions on the determination of palladium and nickel to investigate selectivity of the method also were studied.     

Spectrophotometric determination of nickel with p-acetylarsenazo

A spectrophotometric method for the determination of trace amounts of nickel is described. At pH 6, nickel reacts with p-acetylarsenazo to form a 1:2 coloured complex with an absorption maximum at 630 nm. The apparent molar absorptivity is 6.5 x 10(4) l.mol(-1) . cm(-1) . Beer's law is obeyed over the concentration range of 0-0.8 microg/ml. The proposed method is selective, sensitive and can be applied to the determination of nickel in aluminum alloy.     

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.     

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.     

Determination of nickel in biological samples spectrophotometrically involving complexation reaction with some thiazolylazo compounds

Three new heterocyclic azo compounds, 5(2-benzothiazolylazo)2,2 biphenyldiol (I), 5-(2-benzothiazolylazo)-8-hydroxyquinolene (II) and 4-(2-benzothiazo-lylazo)3-hydroxy-2-naphthoic acid (III) were synthesized. The formation constant of the reagents in 30% (v/v) ethanol and reactions with various metal ions were studied. These reagents (I-III) reacts with nickel ion to form (2:1) colored complex with an absorption band at 604, 635 and 643 nm. The apparent stability constants and the optimum conditions for complete color development were investigated. Beer's law is obeyed over the concentration ranges of 0.05-3.50, 0.05-4.00 and 0.05-3.10 micrograms ml-1. For more accurate analyses, Ringbom optimum concentration ranges were found to be 0.20-3.25, 0.20-3.80 and 0.20-2.90 micrograms ml-1 using reagents I, II and III, respectively. The apparent molar absorptivity and Sandell sensitivity were also calculated. The interference of various foreign ions on the determination of nickel was investigated. The proposed method has been successfully applied to the determination of nickel substrates in various biological samples.     

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.     

Determination of nickel in alloys and plant leaves with salicylaldehyde 3-oxobutanoylhydrazone by spectrophotometry.

A simple and highly sensitive reagent of salicylaldehyde 3-oxobutanoylhydrazone (salicylaldehyde acetoacetic acid hydrazone, SAAH) was synthesized and studied for the spectrophotometric determination of nickel in detail. In the pH range 6, which greatly increased the selectivity, nickel reacted with SAAH to form a 1:1 yellow complex, having a sensitive absorption peak at 405 nm. Under the optimal conditions, Beer's law was obeyed over the range from 0.0117 to 0.1174 microg cm(-3). The apparent molar absorptivity was 3.025 x 10(5) dm3 mol(-1) cm(-1). The detection limit and the variation coefficient were found to be 1.752 ng cm(-3) and 1.0%, respectively. The method has been applied to the quantitative determination of nickel in different alloys and leaves.     

Spectrophotometric determination of nickel in vegetable oil with ammonium 2-amino-1-cyclohexene-1-dithiocarboate

The reaction between nickel and ammonium 2-amino-1-cyclohexene-1-dithiocarboate in aqueous acetone medium at pH 3.0-8.0 results in a stable dark red complex. The ratio of reagent to nickel in the complex is 2:1 and the formation constant is 7.38 +/- 0.12 x 10(10). Beer's law is obeyed up to 4 microg/ml nickel at the absorption maximum at 535 nm. The apparent molar absorptivity is 2.8 x 10(4) l.mole(-1). cm(-1), and the detection limit is 10 ng/ml nickel. The method is applied to the determination of nickel in vegetable oil.     

Spectrophotometric determination of nickel by extraction of the complex nickel-purpurin

A simple, sensitive procedure for extractive spectrophotometric determination of nickel has been developed. At pH 8.5, nickel reacts with purpurin (1,2,4-trihydroxyanthraquinone) to form a 1:1 red complex, extractable in methyl isobutyl ketone, with an absorption maximum at 525 nm. The characteristics of the complex, including optimum conditions of formation and extraction, and the adherence to Beer's law, are described. Nickel in cobalt and in iron and aluminum alloys has been determined by this method.     

High-performance liquid chromatographic determination of uranium using solvent extraction and bis(salicylaldehyde) tetramethylethylenediimine as complexing reagent

The reagent bis(salicylaldehyde)tetramethylethylenediimine has been used for the determination of dioxouranium(VI), based on complexation in aqueous solution at pH 6, followed by extraction in chloroform and HPLC determination on a Hypersil ODS (3 μm) column. The complex was eluted with the ternary mixture methanol-acetonitrile-water (40:30:30, v/v/v), with UV detection at 260 nm. Oxovanadium(IV), iron(III), copper(II), cobalt(II), nickel(II) and palladium(II) were completely separated and did not interfere in the determination of uranium. The linear calibration range and detection limits have been obtained. The method has been applied to the determination of uranium together with copper, iron and nickel in mineral ore samples.     

The Spectrophotometric Determination of Nickel and Cobalt in Mixtures with Picolinaldehyde 4-Phenyl-3-Thiosemicarbazone

Abstract

The properties of nickel complex of picolinaldehyde 4-pheny1-3-thiosanicarbazone are described. The optimal conditions for a selective and sensitive spectrophotometric determination of nickel are discussed, A photometric method for the determination of traces of cobalt(II) and nickel(II) ions in mixtures has also been developed.     

Ternary Complex Nickel(II)/3-(4′,5′-Dimethyl-2′-Thiazolylazo)-2,6-Dihydroxybenzoic Acid/Cyanide. Spectrophotometric Determination of Nickel

Abstract

A spectrophotometric method for nickel has been developed based on the formation of a ternary complex in the system Ni(II)/3-(4′,5′-dimethyl-2′-thiazolylazo)-2,6-dihydroxybenzoic acid/cyanide at pH 9.2 (borate buffer), which allows the determination of 0.05–0.47ppm of nickel (ε = 3.53×10⁴ 1.mol^?1. cm^?1) at 538nm. Interferences have been studied and the method applied to the determination of nickel in low alloy steels.     

一个新的测定镍的分光光度法——-以2-4-溴-2-苯骈噻唑偶氮)-5-二乙胺基苯酚作试剂

At pH 9.5 nickel reacts with 2-(6-bromo-2-benzothiazolylazo)-5 diethylamino-phenol (Br-BTAE) in the presence of Tween-80 and sodium lauryl sulfate to form a red-violet complex which has an absorption maximum at 540 nm (e 2.5X10^5). Though this is also the absorption maximum of the reagent, yet the reagent will readily decompose at 40-50`C within 20 min. The reagent blank is low and the error is negligible. Beer's law is obeyed for 0.01-0.125 \mγ nickel in a 1mL solution. The composition of the complex was found to be Ni/Br-BTAE=1:2 by the continuous-variation method. This method can be applied to the determination of nickel in electroplating waste-water and in copper-aluminium alloy and steel samples after extraction with dimethylglyoxime. The results of the analysis agree with that from AAS and dimethylglyoxime method