Determination of lead by solid-phase spectrophotometry using Arsenazo III

Complexation of lead with Arsenazo III in a solid phase was studied. The results obtained were used for the development of a new procedure for determining trace lead.     

Radiolysis of aqueous solutions of cobalt(II) and cobalt(III)

Radiolysis of aqueous solution of di and trivalent cobalt with 1:2 (bis) carboxymethylaminodiethyltetraacetic acid (EGTA) was investigated, both in absence and in presence of oxygen. A radiolytic mechanism has been proposed. It has been shown that the degradation at the ligand of the chelate is due to OH only.     

Determination of tungsten with pyrocatechol violet by first-derivative solid-phase spectrophotometry

Derivative spectrophotometry was applied to solid-phase spectrophotometry in order to enhance its sensitivity and remove the large background caused by the absorbance of the resin layer. Determination of micro-amounts of tungsten with pyrocatechol violet to form a 21 green complex in acid medium which is fixed on a dextran-type anion-exchange resin (Sephadex QAEA-25) is described as an example for the application of this technique. The absorbance of the resin packed in a 1-mm spectrophotometric cell, was measured directly. The characteristic peak amplitude of the signal at 674 nm in the first-derivative spectrum is useful for quantitative determination of tungsten (3–16 g 1^–1; RSD 5.8%) in natural and industrial water samples.     

麦塔喇红催化光度法测定痕量钴的研究

基于在NH3-NH4Cl缓冲液中,柠檬酸存在下,痕量钴能灵敏地催化H2O2氧化麦塔喇红的反应,建立了一种测定痕量钴的新方法。考察了反应的影响因素,研究了该催化反应的最佳条件及动力学参数,探讨了反应机理。线性范围为0~0.050μg/mL,检出限为1.33×10-10g/mL。可用于蜂蜜和维生素B12中钴的测定。     

Co(Ⅱ)-棉红-H2O2体系测定痕量钴的研究与应用

基于在NH3-NH4Cl缓冲液中,柠檬酸存在下,痕量钴能灵敏地催化H2O2氧化棉红的反应,建立了一种测定痕量钴的新方法。考察了反应的影响因素,研究了该催化反应的最佳条件及动力学参数,探讨了反应机理。该方法线性范围为0~0.025μg/mL,检出限为3.33×10-10g/mL。可用于蜂蜜和维生素B12中钴的测定。     

固相萃取-分光光度法测定人体尿液中亚硝酸盐的含量

亚硝酸盐中毒发生时,为了快速准确测定人体尿液中的亚硝酸盐的含量,建立了固相萃取-分光光度的分析方法。本方法是基于亚硝酸盐的重氮偶合反应,采用固相萃取技术对尿液进行净化处理后,消除了基质干扰,提高了测试灵敏度,通过对比考察了固相萃取柱类型、重氮化剂种类、重氮化剂质量浓度、反应酸度、偶合剂质量浓度及反应时间等试验参数对测试结果的影响,得出了最佳的试验条件,确定了试验方法为尿液离心后经HLB固相萃取柱净化除杂,取过柱液2.0 mL于比色管中,用水定容至5.0 mL,依次加入0.5 mL对氨基苯磺酰胺酸性溶液（50.0 g/L）和0. 5 mL盐酸萘乙二胺溶液( 2.5 g /L)进行重氮偶合显色反应10 min,于波长544 nm 处进行吸光度的测定,以工作曲线外标法定量。 结果显示,亚硝酸盐在0.033-0.986 μg/mL范围内线性关系良好,相关系数为0.9998,尿液在0.246-2.054 μg/mL三种加标水平范围内亚硝酸盐的平均回收率为96.3%-106.1%,表明HLB固相萃取柱有效去除了影响重氮偶合反应的干扰物质,达到了满意的净化效果。日内和日间测定值的相对标准偏差（RSD）分别为2.01% -3.58%和2.21%- 4.75%,方法检出限为0.010 μg/mL,定量下限为0.033 μg/mL。该方法操作简单、快速,精密度和准确度良好,且检出限低,适用于人体尿液中亚硝酸盐含量的快速检测。     

Determination of cobalt in water samples by photoacoustic spectroscopy with a solid-phase spectrophotometry approach using 3-(2-pyridyl)-5,6-bis(4-sulfophenyl)-1,2,4-triazine

This work forms part of an investigation which seeks to determine metal complexes in a solid phase by photoacoustic spectrometry (PAS). Results of spectral determination of Co(II) complexes are introduced. The method is based on Co(II) colorimetric reaction with 3-(2-pyridyl)-5,6-bis(4-sulfophenyl)-1,2,4-triazine (FST, ferrozine) retained on an anion-exchange resin, DEAE Sephadex A-25. The immobilization of Co(II) on the solid phase is combined with PAS measurement. A numerical approach is applied to reduce noise in the spectral data. At λ = 477 nm, the calibration for Co(II) is linear over the range 14–300 μgL^{− 1}. The Co(II) concentration in water samples was determined by conventional photoacoustic measurement. The relative standard deviation (R.S.D.) of the method for the calibration is < 5%. Under optimized conditions, the obtained analytical features were LOD 14 μgL^{− 1} and LOQ 45 μgL^{− 1}.     

Determination of traces of aluminium with chrome azurol S by solid-phase spectrophotometry

A microdetermination method at sub-mug/1. level for aluminium by solid-phase spectrophotometry has been developed. Chrome azurol S was used as chromogenic reagent to form a blue complex which was easily and strongly sorbed and concentrated on a dextran-type anion-exchange resin. The resin-phase absorbances at 615 and 800 nm were measured directly. Aluminium can be determined in the 0.6-4.0 mug/1. range with a RSD of 2.1%. The method is applied to the determination of aluminium in micaschist, natural and tap water samples.     

Determination of total iodine in samples with an organic matrix by solid-phase spectrophotometry

A solid-phase spectrophotometry method is proposed for determining total iodine in samples with an organic matrix. The method involves the sorption of I₂ formed in oxidation of iodide with oxone (active ingredient potassium peroxomonosulfate) by polyurethane foams, followed by the registration of the adsorbent absorbance at 360 nm. Sample preparation includes treatment with an aqueous methanolic solution of tetramethylammonium hydroxide followed by thermostation at 90 ± 2°C for 3 h. The detection limit for iodine calculated using the 3s-test is 0.03 μg in a sample aliquot portion of ≤8 cm³. The relative standard deviation is 8–12% for iodine concentration in the range 0.3–5.0 μg/g.     

结晶紫-高碘酸钾体系催化动力学光度法测定痕量钌(Ⅲ)

测定金属元素主要的主法有光度法、原子吸收法、荧光法[1,2]等.近年来催化动力学光度法测定金属元素以其灵敏度高、检测限低倍受分析工作者重视,适合于痕量分析,尤其适合于痕量钌(Ⅲ),采用有机染料作为检测组分.     

Determination of unsulphonated quinoline yellow in soft drinks by solid-phase spectrophotometry

A spectrophotometric method for determination of quinoline yellow spirit soluble (QYSS) in the presence of sulphonated quinoline yellow water soluble (QYWS) in soft drinks at trace levels is reported. The method is based on the fixation of QYSS on C-18 silica gel, followed by measurement of its absorbance at = 418 nm in the solid phase after being packed in a 1-mm cell. The applicable concentration range was 1.5–15.0 ng/ml, the detection limit 0.4ng/ml and the relative standard deviation 5.2%. The method was applied satisfactorily to the determination of this compound in samples of commercial soft drinks.     

Simultaneous determination of iron(III) and cobalt(II) withN-phenylcinnamohydroxamic acid and thiocyanate by extraction and spectrophotometry

Simple, precise, sensitive, and highly selective methods for the separate determination of iron(III) and cobalt(II) and for the simultaneous determination of both metal ions are described. Iron(III) and cobalt(II) react with thiocyanate in the presence ofN-phenylcinnamohydroxamic acid (PCHA) to form pinkish red and blue coloured complexes, respectively. Both the iron(III) and cobalt(II) complexes having stoichiometric composition of 122 (FeSCN^–PCHA) and 14 (CoSCN^–), respectively, are quantitatively extractable into ethylacetate from 0.5–1.5 M hydrochloric acid solutions. The spectra of iron(III) and cobalt(II) complexes in the visible region exhibit absorption maxima at 495 and 625 nm, respectively. The coloured systems obey Beer's law in the concentration range of 0.2–4.0g/ml of iron and 2–40g/ml of cobalt. The effects of foreign ions and of various experimental parameters were studied to establish the optimum conditions for the extraction and determination of iron and cobalt. The methods have been applied successfully to the analysis of blood, vitamin B₁₂, and standard steels for iron and cobalt.     

Cleavage by halogens of carboncobalt bonds in organometallic complexes of cobalt(III) : II. Organobis(dimethylglyoximato)cobalt(III) complexes

The reaction between organocobaloximes and ICl in chloroform has been studied. In absence of an excess of added chloride ion the reaction is electrophilic in character; in presence of an excess of chloride ion both oxidative dealkylation and radical attack can occur.     

Determination of trace amounts of cobalt in water by solid-phase spectrophotometry after preconcentration on a nitroso R salt chelating resin

A sensitive method for the determination of microamounts of cobalt by ion-exchanger spectrophotometry has been developed. The chromogenic agent, Nitroso-R-Salt (NRS), was loaded on an anionic-exchange resin (Amberlite CG-400). The absorbance of the NRS-cobalt complex on the chelating resin was measured at 508 nm. The best conditions for the preconcentration of cobalt on the resin before the spectrophotometric determination were a pH value of 6, temperature of 80 °C, and heating times of 45 or 90 min for 50 and 400 ml of sample, respectively. The detection limits were 27 ng/ml (50-ml samples) and 1.8 ng/ml (400-ml samples). Interference by other metals was investigated. The method is useful for determination of cobalt in natural waters.     

反向流动注射阻抑动力学光度法测定微量锑(Ⅲ)

锑是一种广泛分布的有毒元素,许多研究证明锑对人体及生物具有毒性及致癌性,由于锑矿的开采和加工以及自然过程的影响,环境水样中锑污染日趋严重,而人体及生物对锑的摄取,一般来自饮用水、空气等,因此有效、快速、灵敏的测定环境水样中的锑具有实际的意义.     

Determination of free acid in antimony(III) and bismuth(III) solutions

A method for the determination of free acid in antimony(III) and bismuth(III) solutions is given. A solution of the disodium salt of EDTA, 2-3 % in excess of the stoichiometric amount, is added to the metal salt solution and titrated with sodium hydroxide solution potentiometrically or visually using a mixed indicator. The error in the method is less than 0.5 %.     

Three-component synthesis of amidoalkyl naphthols catalyzed by bismuth(III) nitrate pentahydrate

Bismuth(Ⅲ) nitrate pentahydrate catalyzed the three-component condensation ofβ-naphthol,aldehydes and amines/urea under solvent-free conditions to afford the corresponding amidoalkyl naphthols in excellent yields.     

Determination of fluoride by spectrophotometry of Arsenazo(III) complex of the back-extracted Th(IV)

A method based on the back-extraction of Th(IV) from its TTA complex in benzene by aqueous F^– followed by spectrophotometric measurement of Th(IV), for the determination of fluoride has been developed. The coefficients of variation obtained are 2.4% and 1.4% in 11 determinations at F^– concentration levels of 1.0 g ml^–1, respectively.