1-(2-噻唑偶氮)-2-萘酚螯合物反相高效液相色谱法分离测定铜(Ⅱ)、铁(Ⅱ)和镍(Ⅱ)

以１－（２－噻唑偶氮）－２－萘酚（ＴＡＮ）作柱前显色剂，于ＯＤＳ柱上，用内含０．１ｍｏｌ／ＬＬｉＣｌ，５×１０－６ｍｏｌ／Ｌ ＴＡＮ和ＨＡｃ－ＮＨ４Ａｃ缓冲溶液（ｐＨ ５．５）的甲醇－水溶液（８０：２０，Ｖ／Ｖ）作流动相，流速为０．６ｍＬ／ｍｉｎ，并以紫外－可见检测器于５９０ｎｍ处进行检测，发展了一种ＲＰ－ＨＰＬＣ法同时分离测定铜（Ⅱ）、铁（Ⅱ）、镍（Ⅱ）的方法，方法灵敏度高，对于铜、铁、镍的检测限分别为１μｇ／Ｌ， ２ μｇ／Ｌ和 ０．４ μｇ／Ｌ。用于实际样品测定，结果满意。     

电镀液和电镀层中钯和钴的分光光度法同时测定

在ＰＨ＝４．５的ＨＡｃ－ＮａＡｃ介质中,钴和钯都能与２－「２－（６－甲基苯并噻唑）偶氮」－５－「Ｎ－甲基－Ｎ－乙羧基」苯甲酸（简称ＭＣＢ）形成络合物。在λ＝７１０ｎｍ处Ｃｏ－ＭＣＢ不吸收;在６１０．５ｎｍ处Ｃｏ－ＭＣＢ有最大吸收,而Ｐｄ－ＭＣＢ也有一定的吸收值。利用这一差异,在可６１０．５ｎｍ处测定Ｐｄ和Ｃｏ的合量,而在７１０ｎｍ处测定Ｐｄ的含量学与化学传感再利用系数法算出Ｃｏ的含量。测定了纯性范     

钕（Ⅲ）与对－氨基苯甲酸、邻菲咯啉混配配合物的晶体结构和激光拉曼光谱

报道了钕与对－氨基苯甲酸、邻菲咯啉的配合物［（Ｎｄ（ｐ－ＡＢＡ）４·２Ｐｈｅｎ］Ｈ３Ｏ·２Ｐｈｅｎ的合成。测定了它的结构和激光拉曼光谱。配合物属单斜晶系，空间群为Ｃ２／ｃ，ａ＝１９０６７（５）ｎｍ，６ｂ＝１，９１９２（３）ｎｍ，ｃ＝２．０１９０（４）ｎｍ，Ｂ＝２１１７．２５（２）℃，Ｖ＝６．５６８（５）ｎｍ３Ｍ＝１４２８．６３，ｚ＝４，Ｄｘ＝１．４５ｇ·ｃｍ－３。钕离子的配位数为１０，钕原子周围的配位原子形成畸变的四帽三角棱柱体。     

双波长分光光度法同时测定贵金属钯和锇

本文提出了在对羟基苯基荧光酮和溴化十六烷基三甲烷基甲胺存在下，双波长分光光度法同时测定微量和锇的新方法，在ｐＨ＝７．６～８．０的磷酸盐介质中，钯和锇的对羟基苯基荧光酮－ＣＴＭＡＢ配合物吸收光谱相互重叠，选择测定钯配合物的波长对为５８０．５ｎｍ与５３０．５ｎｍ，测定锇配合物的波长对为５５３．５ｎｍ与６０４．５ｎｍ，钯含量在０～７．０μｇ／１０ｍＬ范围内，锇含量在０～９．０μｇ／ｍＬ范围内，与ΔＡ值呈     

反相HPLC测定钒,铌,钽的2—（2—吡啶偶氮）—5—二乙氨基苯酚配合物

以２－（２－吡啶偶氮０－５－二乙氨基苯酚（ＰＡＤＡＰ）为柱前衍生试剂，在含０．１％酒石酸的１０ｍｍｏｌ／Ｌ（ｐＨ３．５）ＨＡｃ－ＮａＡｃ缓冲溶液的甲醇／水（５０∶５０，Ｖ／Ｖ）中（５８０ｎｍ检测），在Ｃ１８柱上于１１ｍｉｎ内实现了Ｖ、Ｎｂ、Ｔａ的同时分离及测定，检出限（Ｓ／Ｎ＝３）杰０．３４、０．２９、７．３０ｎｇ／ｍＬ．该法灵敏度高，用于矿样分析所得民推荐值相行，标准加入回收率为９９．０％～１０     

一阶导数分光光度法同时测定镀层中的铁和镍

１引言在铁镍合金中添加适量的稀土元素能提高合金的机械性能，使其具有良好的抗蚀性和耐磨性。本文研究了以二甲酚橙为试剂和在适量表面活性剂ＣＴＭＡＢ存在下利用一阶导数分光光度法同时测定铁镍合金镀层中的铁和镍的最佳实验条件，并应用于含有微量稀土元素的铁镍合金镀层中铁和镍含量的同时测定，获得满意的结果。２仪器与试剂美国ＢｅｃｋｍａｎＤＵ－７ＨＳ型分光光度计；ＨＭ－２０Ｅ型ｐＨ计。５０ｍｇ／Ｌ铁标准溶液；５０ｍｇ／Ｌ镍标准溶液；ｐＨ为４．４的ＨＡｃ－ＮａＡｃ缓冲溶液（其中ＮａＡｃ的浓度为０．５ｍｏｌ／Ｌ）；…     

新显色剂5－NO_2－PADAP与镍的显色反应研究

本文研究了新显色剂２－（５－ＮＯ２－２－吡啶偶氨）－５－二乙氨基酚（５－ＮＯ２－ＰＡＤＡＰ）与镍的显色反应及分光光度测定镍，在ＰＨ３．５乙醇水溶液中，镍与５－ＮＯ２－ＰＡＤＡＰ形成稳定的深色配合物，最大吸收在５６５ｕｍ处，摩尔吸光系数为．１．５７×１０５Ｌ·ｍｏｌ（－１）·ｃｍ（－１），镍在０～１２μｇ／２５ｍＬ范围内服从比尔定律，用此法测定钢铁及茶叶中的微量镍，结果令人满意。     

二阶导数光度法同时测定微量镍和铜的研究

用２－（２－噻唑偶氮）－５－二甲氨基苯甲酸作为显色剂，在ｐＨ５．６，波长在６２０ｎｍ和５９０ｎｍ处，用于阶导数光度法，同时测定微量镍和铜。回收率镍为１００％￣１０２％，铜在９２％￣１０５％，Ｎｉ＾２＋、Ｃｕ＾２＋在０￣１６μｇ／２５ｍｌ均呈线性关系。     

对偶氮苯重氮氨基偶氮苯磺酸分光光度法测定水和土壤中的痕量镍

在ＴｒｉｔｏｎＸ－１００和四硼酸钠介质中，题示试剂与镍产生灵敏的显色反应，所生成的紫红色络合物最大吸收波长５４６ｎｍ，摩尔吸光系数为２．３×１０＾５Ｌ．ｍｏｌ＾－＾１．ｃｍ＾－＾１，镍在０－１２μｇ／２５ｍｌ范围内遵守比耳定律。干扰离子可用丁二酮肟－正丁醇萃取法消除。拟定的方法应用于水样和土壤样品中镍的测定。结果满意。对水样２＾＃和土壤样５＾＃６次测定的相对标准偏差分别为６．２％和４．９％。     

新试剂5－氟偶氮胂Ⅰ荧光法测定铝的研究

本文报道了新试剂５－氟偶氮胂Ⅰ（５－ＦＡｓＡ－Ⅰ）的合成方法，研究了荧光光度法测定铝的反应条件。Ａｌ（Ⅲ）与试剂在ｐＨ５．６０ＨＡｃ－ＮａＡｃ缓冲介质中形成１＋１红色配合物并呈现荧光，λｅｘ／λｅｍ＝３４８．６／３９１．４ｎｍ，线性范围为０～０．２μｇ／ｍＬ，检测限为３．０ｎｇ／ｍＬ。用于分析茶叶样品中的铝，结果满意。     

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.     

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.     

Simultaneous spectrophotometric determination of nickel and iron in copper-base alloy with bromo-PADAP

The reaction of nickel (II) with Br-PADAP, in the presence of tergitol NPX surfactant, forms a complex with absorption peaks at 520 and 560 nm. The iron(II)-Br-PADAP system at the same conditions forms a chelate with absorption peaks at 560 and 748 nm. This allows the simultaneous spectrophotometric determination of nickel and iron by measuring the absorbance at 560 and 748 nm. The proposed method, at ph 4.0-5.7, shows a molar absorptivity of 1.22 x 10(5)l . mole(-1) . cm(-1) for nickel at 560 nm and 8.20 x 10(4)l . mole(-1) . cm(-1) at 560 nm and 3.35 x 10(4)l . mole(-1) . cm(-1) at 748 nm for iron(II). Beer's law is obeyed up to 0.40 mu/ml of nickel(II) and up to 0.65 mu/ml of iron(II). Thiosulphate as masking agent allows the simultaneous determination of iron and nickel in the presence of high concentrations of copper. The ethylene glycol 2-(2-amino-ethyl) tetracetic acid provides the elimination of many other interferences. The method has been applied successfully to the simultaneous determination of nickel and iron in reference samples.     

Spectrophotometric determination of aluminium and nickel

A simple spectrophotometric method, based on the complexes with xylenol orange (XO) and EDTA, is presented for the rapid determination of aluminium and nickel, respectively, in synthetic samples of hydrotalcite. The method only requires the solubilization in sulphuric acid of the inorganic material before the ligand addition. Under optimum conditions, the complexes Al-XO and Ni-EDTA showed maximum absorption at 554 nm and 380 nm, respectively. The method obeyed Beer's law in the concentration range 0.14-1.8 microg mL(-1) of aluminium, and 30-2730 microg mL(-1) of nickel. Molar absorptivities were 2.45 x 10(4) and 14.85 L mol(-1) cm(-1) while Sandell's sensitivities were 1.1 x 10(-3) and 3.9 microg cm(-2) for aluminium and nickel, respectively. The standard addition technique was used and the recoveries obtained revealed that the proposed procedure shows good accuracy.     

Use of 3-hydroxy-1,3-diphenyltriazine in the spectrophotometric determination of copper, palladium, iron, cobalt, nickel, and molybdenum

3-Hydroxy-1,3-diphenyltriazine (HDPTA) forms brightly coloured complexes with copper, palladium, iron, cobalt and nickel ions, which are readily extractable in benzene. The deep yellow molybdenum complex is completely soluble in 60% ethanol. All the chelates have a definite absorption maximum between 398 and 422 nm, the reagent absorption being negligible above 415 nm. The molar composition of the chelates is ML(2), except for iron and cobalt which form ML(3) complexes. Microquantities of these metals can be determined spectrophotometrically with HDPTA.     

Novel use of doublet peaks in flow injection analysis : Simultaneous Spectrophotometric Determination of Nickel(II) and Iron(II)

A simple, non-separation method for the simultaneous, single-injection determination of nickel(II) and iron(II) is described. The method is based on doublet peaks in a single-line system, with multiple vertical (absorbance) measurements of the doublet peak profile. Doublet peaks occur when the center of the sample zone remains unmixed. Nickel(II), 0.17–0.24 M, in the presence of 2.7–5.4 mM iron(II) is determined by direct spectrophotometry of the nickel(II) ion at the center of the sample zone, Iron(II) is first oxidized on-line by peroxodisulfate to iron(III), which complexes with thiocyanate to form the intensely red complex; this is measured at the peak maximum corresponding to the trailing edge of the sample zone. Correction are made for absorbance of nickel and its reduction in the iron thiocyanate complex formation. The absorbance of nickel(II) ion and the iron thiocyanate complex are both measured at 395 nm from a single injected sample. The general utility of the doublet peak method is discussed.     

o-Diketonedioxime compounds as analytical reagents for the spectrophotometric determination of nickel

Sixteen dioxime compounds, including six new compounds, were synthesized and their reactions with nickel, cobalt, iron(II, III) and copper ions were examined. The nickel chelates of the glyoxime derivatives show hardly any absorption in the visible region, and are therefore unsuitable as color reagents. The nickel chelates of the benzildioxime derivatives can be extracted into organic solvents and provide a selective color reaction, so that useful extraction-spectrophotometric methods are possible. The metal complexes of quinonedioximes are extracted into some organic solvents, and the complexes have relatively large molar absorptivities in the visible region, but the reagents are not selective. However, the molar absorptivity of the ternary complex, Ni²⁺-reagent-zephiramine, with 1,2-naphthoquinonedioxime-4-sulfonic acid was 2.03·10⁴ at 480 nm, and that of the nickel complex of 9,10-phenanthrenequinonedioxime was 2.49·10⁴at 456 nm. The compositions of the nickel-dioxime complexes were examined spectrophotometrically.     

Simultaneous third-derivative spectrophotometric determination of copper and nickel in iron alloys and aluminium alloy

A method is proposed for the simultaneous determination of copper and nickel by third-derivative spectrophotometry based on the absorption spectra of their complexes with cyanide ion in the ultraviolet range. The method allows the determination of 0.55-5.8 mug/ml of copper and 0.55-6.8 mug/ml of nickel. The relative standard deviation for 11 determinations of 1.5 mul/ml of copper and nickel were 0.78 and 0.72%, respectively. The detection limits were 0.10,mug/ml for nickel and 0.13 mug/ml for copper. The method has been applied to direct determination of copper and nickel in iron alloys and an aluminium alloy without any separation.     

Simultaneous determination of lanthanum and cerium in mixed rare earths with p-acetylarsenazo by spectrophotometry

A new method has been developed for the simultaneous spectrophotometric determination of small amounts of lanthanum and cerium in the presence of large amounts of rare earth elements. Lanthanum (III) and cerium (III) were determined spectrophotometrically with p-acetylarsenazo as the color reagent in the chloroacetic acid medium at pH 3.1 by measuring the absorbances of the complexes at 670 nm. The remained rare earths were masked with ethylenediaminetetracetic acid and ethylenediaminetetracetic acid-zinc during the analysis. The optimum conditions for the simultaneous determination of lanthanum and cerium have been defined. The individual content of lanthanum (III) and cerium (III) were determined by varying the amounts of EDTA and EDTA-Zn used in the analysis and solving the simultaneous absorbance equations based on the Beer's law. The proposed method has been successfully applied to the determination of lanthanum and cerium in Longnan mixed rare earth oxides and other heavy rare earths without preliminary separation with satisfactory results. The relative errors of all analytical results of the method were not more than 2% with good precision. The procedure does not require separation of lanthanum, cerium and the other rare earth elements.     

Spectrophotometric simultaneous determination of cobalt, copper and nickel using nitroso-R-salt in alloys by partial least squares

Partial least squares modeling as a powerful multivariate statistical tool applied to spectrophotometric simultaneous determination of cobalt, copper, and nickel in aqueous solutions. The concentration range for cobalt, copper and nickel were 0.4-2.6, 0.6-3.4, 0.5-5.5 ppm, respectively. The experimental calibration set was composed with 36 sample solutions using a mixture design for three component mixtures. The absorption spectra were recorded from 470 to 600 nm. The effect of pH on the sensitivity and selectivity was studied according to net analyte signal (NAS). The values of root mean square difference (RMSD) for cobalt, copper and nickel using partial least squares (PLS) were 0.0192, 0.0263 and 0.0446 ppm, respectively. The effects of various cations and anions were investigated. The method was used to determination of cobalt, copper and nickel in two sample alloys based on copper, nickel and cobalt (known as cunico) and based on cobalt, nickel and iron (known as conife).