钯的PAR-氯化四苯鉮的萃取光度法测定

本文报道了钯与4-(2-吡啶偶氮)间苯二酚(PAR=H_2R,下同)和四苯钟离子形成离子缔合物的化学条件,经氯仿萃取后,建立了一种测定微量钯的萃取光度法。萃取的最佳pH为4.4,络合物的化学式为[(C_6H_5)_4As~+,PdClR~-],其最大吸收峰波长为532nm,表观摩尔吸光系数e_(532)=3.3×10~4L·mol~(-1)·cm~(-1),10mL萃取液中钯量在0～25μg内遵守比耳定律。方法简便,选择性好,用于催化剂中钯的测定,结果满意。     

meso－四（4－甲基－3－磺基苯）卟啉分光光度法测定痕量钯的研究

本文研究了Ｐｄ（Ⅱ）与ｍｅｓｏ－四（４－甲基－３－磺基苯）卟啉（Ｔ（４Ｍ３ＳＰ）Ｐ）的显色反应在表面活性剂十二烷基磺酸钠（ＳＤＳ）和抗坏血酸存在下，ｐＨ４８的ＨＡｃ－ＮａＡｃ介质中，沸水浴加热，Ｐｄ（Ⅱ）与Ｔ（４Ｍ３ＳＰ）Ｐ形成１∶１（Ｍ∶Ｌ）配合物配合物最大吸收波长４１４ｎｍ，表观摩尔吸光系数ε＝２０×１０５Ｌ·ｍｏｌ－１·ｃｍ－１钯量在０－２．２５μｇ／１０μＬ范围内符合比耳定律本法应用于催化剂中痕量钯的测定，结果满意     

Non-Extractive Simultaneous Spectrophotometric Determination of Trace Quantities of Palladium(II) and Tungsten(VI)

A second order derivative spectrophotometric method has been developed for the simultaneous determination of Palladium(II) and Tungsten(VI) using 3,4-dihydroxybenzaldehyde isonicotinoylhydrazone (3,4-DHBINH) as a new complexing agent. The Pd(II) reacts with 3,4-DHBINH in the pH range from 3 to 7 to form green colored solution. The absorbance calibration curves were constructed for palladium(II) at 362 nm (0.53～6.40 μg/ml) and tungsten(VI) at 374 nm (0.92～11.40 μg/ml). The metal ions interfere with each other in determination of zero order as well as the first order spectrophotometry. The optimum condition for maximum color development and other analytical parameters were evaluated. The method was applied successfully for the determination of palladium in hydrogenation catalyst and tungsten in industrial waste water samples.     

Spectrophotometric Determination of Palladium(II) with n-Hydroxy-N,N-Diphenylbenzamidine and 1 -(2-Pyridylazo)-2-Naphthol

A spectrophotometric method to determine palladium(II) at trace levels is based on the extraction of palladium(II) as a binary complex with N-hydroxy-N,N′-diphenylbenzamidine (HDPBA) in chloroform at pH 5.0 ± 0.2. The complex shows maximum absorbance at 400 nm with molar absorptivity 6.4 × 10³ L mol^?1 cm^?1. The sensitivity of the Pd(II)-HDPBA complex was enhanced by the addition of l-(2-pyridylazo)-2-naphthol (PAN). The green coloured complex shows maximum absorbance at 620 nm with molar absorptivity 1.58 × 10⁴ L mol^?1 cm^?1. Sandell's sensitivity and the detection limit of the method are 0.0067 μg cm^?2and 0.1 μg Pd(II) mL^?1, respectively. Most common metal ions associated with palladium metal do not interfere. The effects of various analytical parameters on the extraction of the metal are discussed.     

Simultaneous Spectrophotometric Determination of Trace Palladium and Rhodium with2，4－TADAT

ＳｉｍｕｌｔａｎｅｏｕｓＳｐｅｃｔｒｏｐｈｏｔｏｍｅｔｒｉｃＤｅｔｅｒｍｉｎａｔｉｏｎｏｆＴｒａｃｅＰａｌｌａｄｉｕｍａｎｄＲｈｏｄｉｕｍｗｉｔｈ２,４－ＴＡＤＡＴＺＨＡＮＧＸｉａｏ－ｌｉｎｇ;ａｎｄＺＨＡＮＧＧｕａｎｇ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈ...     

2,6—二氯—4—溴偶氮胂光度法测定微量铀（Ⅵ）

本报道用了２，６－二氯－４－溴偶氮胂作显色剂测定微量铀（Ⅵ）的光度法。在Ｈ２ＳＯ４介质中，铀（Ⅵ与）２，６－二氯－４－溴偶氮胂形成１：２络合物，其λｍａｘ＝６４０ｎｍ；表观摩尔吸光系数为１．１×１０＾５Ｌ．ｍｏｌ＾－＾１．ｃｍ＾－＾１；铀的浓度在０．０－２２．０μｇ／ｍｌ内符合比耳定律。方法具有灵敏度高，选择性好，操作方便等特点并已用于废水及矿样中微量铀（Ⅵ）的测定。     

Spectrophotometric Study of 1,2,7-Trihydroxyanthraquinone-Mg(II) Complex. Determination of Mg(II)

Abstract

The spectrophotometric study of violet complex Anthrapurpurin-Mg(II) in a basic medium and a hydroalcoholic solution was made (δ_max - 530 nm., ? = 3.5 × 10³ 1 mol^?1 cm^?1, stoichiometry 1:1, apparent constant of stability log K = 9. 26). A new method for the spectrophotometric determination of Mg(II) is proposed for concentrations between one and six ppm. Relative errors between replicate samples were 0.90 %.     

长光路萃取光度法测定痕量氟

以新型氟树脂长光纤作吸收池，用二甲苯胺的异戊醇作萃取剂，氟、硝酸镧与茜素络合剂形成三元络合物。为保持有机相的清澈，加入０．１０ｍＬ无水乙醇代替ＨＡｃ－ＮａＡｃ缓冲溶液洗涤有机相，并以乙醇稀释有机相后测定。用１１０ｃｍ长的毛细管５８０ｎｍ处测定吸收，氟的线性范围在０－３２μｇ／Ｌ服从比尔定律。该法具有高灵敏度，高稳定性等优点，于天然水中氟，对含氟０．１０ｍｇ／Ｌ－０．１３ｍｇ／Ｌ的水样，其回收率在９     

一种新的测定痕量铁的分光光度法——利用 Fe(Ⅲ)对 H_2O_2氧化还原型罗丹明 B 的催化效应测定铁

本文基于在弱酸性介质中及活化剂硫氰酸钾存在条件下,痕量铁(Ⅲ)对H_2O_2氧化还原型罗丹明B这一显色反应的催化作用,建立了一个灵敏度,线性范围分别为4.0×10~(-11)gFe/ml、0—1.5μgFe/25ml的催化光度新方法。用于水样中微量铁的测定,结果满意,RSD.回收率分别为2.6％、90—103％。     

Some Arylidene-2-Pyridylhydrazone Derivatives as Reagents for Spectrophotometric Determination of Palladium (II)

Abstract

A method for spectrophotometric determination of palladium by complexation with Arylidene-2-pyridylhydrazone derivatives in 50% (V/V) ethanolic solution are described-Pd(II) forms a 1:1 complex with the reagents. Beer's law is obeyed over the range 0.2-6.5 μg ml^?1. The effect of pH, effect of excess reagent, stability of complexes as well as the tolerance amount of many metal ions have been reported. The method is applied, with fair accuracy, to the determination of pd(II) in synthetic solutions.     

测定水中痕量Cr(Ⅵ)的电渗泵顺序注射分光光度法

采用电渗泵顺序注射－分光光度法对水中痕量Cr(Ⅵ）进行了测定，方法通过改变电渗泵流量，流动方向及阀注入时间，实现试剂和样品的定量注入和反应时间的控制；泵工作电压为直流200V，流量为0．45mL/min显色剂采用二苯碳酰二肼，显色剂进样时间为30s，样品进样时间为15s，反应生成的紫红色配合物在540nm处检测，该法线性范围为0．010－1．20mg/L Cr(VI)，检出限为3．4μg/L，应用该法成功地进行了地表水中Cr(Ⅵ）的测定。     

新催化动力学光度法测定痕量钯

在磷酸－邻苯二甲酸氢钾缓冲溶液（ｐＨ２．０）中,利用钯（Ⅱ）对次磷酸钠还原二甲苯蓝ＦＦ褪色的催化作用,建立了用斜率法测定痕量钯的新动力学分光光度法。在加入金（Ⅲ）的条件下,钯（Ⅱ）的检测下限为２．７×１０－１１ｇ／ｍＬ,线性范围为０．０４～６．０ｎｇ／ｍＬ。该法已应用于测定二次阳极泥中钯的含量。     

4, 5-二溴苯基荧光酮光度法测定微量钯

研究了在十二烷基磺酸钠存在下,Pd(Ⅱ)与4,5 二溴苯基荧光酮的显色反应.试验表明,在pH6 3醋酸 醋酸钠缓冲溶液中,Pd(Ⅱ)与试剂形成1∶4的暗黄色配合物,配合物的最大吸收峰位于376nm波长处,表观摩尔吸光系数ε为1 06×105L/(mol·cm).Pd(Ⅱ)含量在0～12μg/10mL范围内符合比尔定律.所拟方法用于钯催化剂和钯矿样中微量钯的测定,结果满意.     

甲基紫用作光度法测定亚硝酸根

研究了在稀盐酸介质中亚硝酸根对甲基紫的退色反应，建立了一个简单，灵敏，选择性高的亚硝酸根测定方法。在５７０ｎｍ处亚硝酸根的浓度在２０－８００μｇ／Ｌ范围内，与甲基紫吸光度的减小呈线性关系。检测限为２０μｇ／Ｌ。研究了实验条件下甲基紫与ＮＯ＾－２的反应摩尔比，３４种共存离子的影响及反应机理。     

显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸与钯(Ⅱ)的显色反应研究

研究了显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸(CTZDBA)与钯(Ⅱ)的显色反应。结果表明,Pd(Ⅱ)与CTZDBA生成稳定的1∶2的紫红色配合物,其最大吸收波长为548 nm,配合物的表观摩尔吸光系数为9.32×104L.mol-1.cm-1,Pd(Ⅱ)质量浓度在0.08~0.8 mg/L范围内符合比耳定律。该方法可不经分离直接测定钯碳催化剂和钯纳米碳催化剂中的微量钯,测定结果与原子吸收法(AAS)基本相符。     

Meso—四—（3,5—二溴—4—羟基苯）卟啉分光光度测定食品中微量铅

研究了溴代卟啉试剂（ＤＢＨＰ）Ｐ分光光度法测定食品中微量铅。在０．０８ｍｏｌ／ＬＮａＯＨ介质中,铅与Ｔ（ＤＢＨＰ）Ｐ反应生成一橙黄色配合物,λｍａｘ＝４７９ｎｍ,ε＝２．２×１０＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。铅在０－１２μｇ／２５ｍＬ范围内符合比耳定律,用于食品中微量铅的测定,获得满意结果。     

Spectrophotometric Determination of Sulfate Ion Through Copper(II)-azide System

Abstract

An indirect and alternative method for the determination of sulfate ion has been established by spectrophotometry. The procedure is based on the formation of copper(II) monoazido species, in water/acetone medium, in which a discoloration effect of system is caused by sulfate presence. In the recommended conditions, sulfate ions can be determined in the concentration range from 40 to 5000 mg/l (ppm), at 375 nm, in natural samples of waters. The best experimental conditions were determined analysing the different factors involved. Studies about the formation equilibria of the CuN₃ ⁺ and CuSO₄ species were realized in water and their respective stability constants (β₁ = 225 M^?1 and 7.15 M^?1) were determined by spectrophotometry at 25.0° C and ionic strength 1.0 M (NaClO₄). Equilibrium investigations were also made in presence of acetone. Additional studies on the ternary system Cu(II)/N₃ ^?/SO₄ ^2-) indicated some evidences of mixed complexes.     

HCl－KSCN体系季胺盐（TOMA·Cl）萃取光度法测定痕量铜的研究

研究了以氯化三辛基甲基胺的二甲苯溶液为萃取剂，在ＨＣｌ－ＫＳＣＮ介质中痕量铜的萃取和分光光度测定。对萃取、分离定量的最适条件，选用适宜的反萃取剂以及铜的萃取体系等进行了详细研究。结果表明，桑德尔灵敏度为４．５×１０~（－４）μｇ／ｃｍ~２，相比Ｖ_ｗ／Ｖ_０＝４０，铜量在０．０２～１μｇ／ｍＬ范围遵守郎伯－比尔定律，成功地建立了一个新的测定微量铜的方法。