Spectrophotometric Study on the Interaction between Arsenazo M and Proteins

Arsenazo M could bind with bovine serum albumin to form a complex in Clark-Lube buffer at pH 2.3 and room temperature, which gives a maximum absorption peak at 625 nm with a red shift of 75 nm compared with that of Arsenazo M itself. The apparent molar absorptivity of the BSA-Arsenazo M complex is 3.21105 Lmol-1cm-1. The linear ranges for protein determination are wide (at least 0-100 mg/mL).

Catalytic Spectrophotometry for Vanadium Determination Based on Oxidation of Arsenazo Ⅲ by Bichromate

A catalytic spectrophotometry for the determination of trace amount of vanadium was developed based on its catalytic effect on the oxidation of arsenazo by potassium bichromate in weak acidic medium. The optimized conditions for determinations are: cK2Cr2O7=3.010-5 molL-1, carsenazo =3.010-5 molL-1, pH=4.0, t=90. The calibration graph is linear for 0.020.2 gml-1, and the detection limit is 0.02 gml-1 V. The apparent active energy of this catalytic reaction is 21.72 kJmol-1. Most foreign ions do not interfere with the determination of vadadium, except for Fe() and Co(), and their interferences could be eliminated by ion exchange. The present method has been used to make the determination of vanadium in human hair, tea, potato and wastewater, and the results were satisfactory.

钌催化高碘酸钾氧化偶氮胂I动力学光度法测定痕量钌

在 H3 PO4、90± 0 .5°C水浴条件下 ,Ru( )催化高碘酸钾氧化偶氮胂 I的褪色反应基础上 ,提出了测定钌的新催化光度法。钌质量浓度在 0～ 0 .0 8μg/1 0 m L范围内符合比尔定律 ,检出限为3.47× 1 0 -4μg/m L。对 0 .0 5 μg/1 0 m L Ru( )测定的相对标准偏差为 1 .47% ( n=1 0 )。该催化反应是一级反应 ,表观活化能为 5 8.82 k J/mol。此法已用于了某些冶金产品和矿石中钌的测定 ,相对标准偏差为 1 .73%～ 2 .0 3% ,标准加入回收率为 97%～ 1 0 5 %。

蛋白质-偶氮胂I复合物的光度性质研究

研究了蛋白质与偶氮胂 的显色反应 .在 p H3 .2的 Britton-Robinson缓冲溶液中 ,偶氮胂 I与蛋白质形成红色复合物 ,λmax为 551 nm,ε为 2 .5× 1 0 5 L· mol- 1· cm- 1 ,蛋白质含量在 1 3 .2～ 2 3 1 mg/L范围内服从Beer定律 .所提出的方法可直接用于血清、花生等生物样品中蛋白质的测定 .

用Arsenazo Ⅲ比色法测定血清钙

在pH 5.5条件下,钙与过量的ArsenazoⅢ以1:2结合形成蓝紫色复合物,在650nm处有一吸收峰,籍以比色测定之,此法重复性得CV 1.2%～1.3%,回收率在94.2～104.0%。用Beckman 700型自动分析仪测定血清钙线性范围在0～6 mmol/L。高胆红素血,高游离血红蛋白和高脂血对此法干扰较小。150名正常人参考位为2.39±0.14 mmol/L,正常范围定为2.11～2.67mmol/L。只要测定条件控制得当,此法可以信赖。

Dual-wavelength dual-indicator catalytic kinetic spectrophotometry for determination of trace Ru(Ⅲ)

A new dual-wavelength dual-indicator catalytic kinetic spectrophotometric method for the determination of trace Ru(III)was studied.This method was based on Ru(III)-catalyzing oxidation of Arsenazo I and indigo carmine by potassium bromate in sulfuric acid.The absorbances of the catalytic and noncatalytic systems were measured at 510 and610 nm,respectively.Under the optimum conditions,the linear range of determination is 0–0.12 lgáml-1and the detection limit is 1.21 9 10-4lgáml-1.The method was applied for the determination of trace Ru(III)in ore samples with satisfactory results.

Catalytic spectrophotometric determination of trace vanadium in fly ash and coal gangue by Triton X-100 enhancing effect

Trace Ⅴ(Ⅴ) catalyzes mightily the decolorization reaction of arsenazo Ⅲ(AsA Ⅲ) by oxidizing with H_2O_2 in a pH 4.0 HAc-NaAc buffer solution, and the addition of TritonX-100 can further increase the sensitivity of the reaction and its catalytic extent is linear withthe content of Ⅴ(Ⅴ). A catalytic spectrophotometric procedure for determining trace Ⅴ(Ⅴ)wasdeveloped. The results show that the maximun absorption of the color solution is at 560 nm and thedetection limit of the method for Ⅴ(Ⅴ) is 0.014 mg·L^(-1). Beer's law is obeyed for Ⅴ(Ⅴ) in therange of 0.00-0.20 mg·L^(-1). The recoveries are 99.0%-104.6%, and the relative standarddeviations (RSD) are 2.7%-3.7%. Combined with ion-exchange resin, the method has been applied to thedetermination of trace vanadium in fly ash and coal gangue with satisfactory results.

Sensitivity Enhancement in Uranium Determination by UV-Visible Spectroscopy Using Ion Imprinted Polymer

There is need to determination of uranium concentration at ppb level in environmental matrices.Due to low sensitivity of FAAS,UV-Visible Spectroscopy is generally used as measurement technique.In this study,ion-imprinted polymers(IIP)were prepared for uranyl ion(imprint ion)by formation of ternary(salicylaldoxime and 4-vinylpyridine)complex in 2-methoxy ethanol(porogen)following copolymerization with methacrylic acid(MAA)as a functional monomer and ethylene glycol dimethacrylate(EGDMA)as crosslinking monomer using 2,2-azobisisobutyronitrile as initiator.The synthesized polymers were characterized by FTIR and TGA analysis.ArsenazoⅢin 3M HClO_4 was used as complexing agent in the measurement step.The optimal pH for preconcentration was found to be between 3.5~6.5values.The developed method was applied to uranium(Ⅵ)determination in natural water samples.

自配Arsenazo Ⅲ试剂测定血清钙──在全自动生化分析仪上的应用

我们对自配ＡｒｓｅｎａｚｏⅢ单一试剂检测血清钙这一方法进行较系统研究。测定波长为６５０ｎｍ，５０ｍｍｏｌ／Ｌ，ｐＨ６．３，ＰＩＰＥＳ缓冲液配制ＡｒｓｅｎａｚｏⅢ浓度为２００μｍｏｌ／Ｌ。线性范围从０～３，７５ｍｍｏｌ／Ｌ（０～１５ｍｇ／ｄｌ）。在ＣＸ４全自动生化分析仪上使用双波长消除了胆红素、血红蛋白的干扰。本法与原子吸收法有良好的一致性。

Simple Spectrophotometric Sequential Injection Analysis System for Determination of Serum Calcium

A sequential injection analysis (SIA) system for the determination of total calcium in blood has been implemented. The assay principle is based on the arsenazo III method, in which the indicator’s complex with calcium forms a blue-purple colour. The absorbance peak height at 650 nm was proportional to the calcium content in samples. A linear range was obtained from 2.5 - 15 mg?dL–1 (r2 = 0.999), with a detection limit of 0.430 mg?dL–1 (3σ). Magnesium, glucose, hae-moglobin, and bilirubin at 123, 1,000, 50, and 0.5 mg?dL–1, respectively, were not found to interfere with the proposed system significantly (recovery 99.1% - 104.4%). The sampling frequency was 30 h–1, in which the carry-over effect was negligible (0.69%). The proposed SIA system was successfully applied to the determination of calcium from serum samples (r2 = 0.970;n = 30).

微波消解试样-催化动力学光度法测定腌菜中亚硝酸根

腌菜试样用稀磷酸及过氧化氢置于PTFE罐中,在微波炉先后在400 W及500 W消解2 min及4 min,所得试样溶液于100 mL容量瓶中定容供光度测定。在稀磷酸介质中偶氮胂Ⅰ溶液与溴酸钾溶液的氧化褪色反应因亚硝酸根的存在而催化加速。有及没有亚硝酸根存在的两份相同试液的吸光度A及A_0之差△A与亚硝酸根质量浓度在50μg·L^(-1)以内呈线性关系,其检出限为0.82μg·L^(-1)。用此方法分析3件腌菜试样,测定结果的相对标准偏差(n=6)均小于2%。以此样品为基体,加入亚硝酸根标准溶液进行回收试验,测得的回收率在98.0%～102.0%之间。

稀释溶液吸光度比值法测定不稳定络合物的稳定常数

本文利用溶液的稀释度与其吸光度的关系,导出一个适用于不稳定络合物稳定常数的测定方法。当络合物的摩尔吸光系数(ε)不能直接测定时,本法可直接求算它的稳定常数及摩尔吸光系数。本文还讨论了方法误差与络合物离解度以及溶液稀释度的关系。

阳离子胶束介质中次磷酸钠还原偶氮胂Ⅰ褪色催化动力学光度法测定痕量硒(Ⅳ)

基于0.02 mol/L的H2SO4介质中存在阳离子胶束时,痕量硒（IV）对次磷酸钠还原偶氮胂I（AsA I）的褪色反应有明显的催化作用,建立了测定痕量硒（IV）的动力学光度法。在固定加热时间段（8 min）后,于500 nm处测定AsA I的吸光度减少值监控反应速率。方法检出限为0.053μg/L,线性范围为0.0~1.0μg/L。讨论了酸度、反应物浓度、表面活性剂的种类和用量、温度、反应时间、干扰离子等因数的影响。研究了反应的最佳条件,并测定了一些动力学参数,催化反应的表观活化能为45.69 kJ/mol。在25 mL溶液中,分别测定0.01μg、0.02μg硒（IV）的相对标准偏差为2.1%、1.9%（n=11）。结合巯基葡聚糖凝胶分离富集,方法用于测定食品和人发样品中的痕量硒（IV）,结果与ICP-AES值相符。相对标准偏差为2.7%~5.8%,加标回收率为96.0%~101.5%。

偶氮胂Ⅰ负载树脂对铀酰吸附特性及应用

用 D-290大孔阴离子交换树脂吸附有机试剂偶氮胂Ⅰ制备了含有偶氮胂Ⅰ基团的负载树脂。用静态法和柱法研究了负载树脂对铀酰吸附反应的最佳 pH、吸附的平衡速度、交换容量等吸附特性。在柱操作条件试验基础上,拟定了用 EDTA 作为掩蔽剂从大体积溶液中定量富集微量铀酰的方法,并用于富集铀矿废水中微量铀取得较好结果。

铬(Ⅵ)—溴酸钾-偶氮胂Ⅰ催化光度法测定水中痕量铬(Ⅵ)

基于在乙酸—乙酸钠缓冲介质中,铬(Ⅵ)对溴酸钾氧化偶氮胂Ⅰ的催化作用,建立了测定水中微量铬的新方法,研究了影响催化褪色反应速度的最佳条件,方法的检出限4.8×10-7g/L,线性范围为0.12～2.2μg/25mL铬(Ⅵ)。多数常见的离子均不干扰测定。用于水中微量铬的测定,快速、准确、简便。

银(Ⅰ)催化抗坏血酸还原偶氮胂Ⅲ反应的研究及痕量银的测定

研究了在柠檬酸 K2HPO4介质中,银(Ⅰ)催化抗坏血酸还原偶氮胂Ⅲ的褪色反应。考察了影响反应的条件,探讨了有关动力学问题,建立了一种测定痕量银的新方法。方法的检出限为9.35×10-11g mL,测定范围为0～0.04μg mL,相对标准偏差为2.6%,回收率在98.5%～101%。

Resonance Rayleigh Scattering Spectra of Thorium(IV)-bisazo Dye of Chromotropic Acidprotein Systems and Their Analytical Applications

In acidic medium, thorium(IV) can react with a bisazo dye of chromotropic acids such as arsenazo III (AA III), arsenazo M (AA M), chlorophosphonazo III (CPA III) and chlorosulphonphenol S (CSP S) to form an anionic chelate which further interacts with some proteins to produce a complex. This results in a significant enhancement of intensity of the resonance Rayleigh scattering (RRS) and the appearance of a new RRS spectrum. There are a few obvious RRS peaks in the range of 400-470 nm and the most intensive peak of them is located at 470 nm. The intensity of RRS is directly proportional to the concentration of protein in the range of 0-1.6 μg·mL -1 for Th(IV)-CPA III system, 0-2.8 μg·mL -1 for Th(IV)-AA M system, 0-2.0 μg·mL -1 for Th(IV)-AA III system and 0-0.28 μg·mL -1 for Th(IV)-CSP S system, respectively. The detection limits for BSA (3σ) are 10.7 ng·mL -1 for Th(IV)-CPA III, 6.3 ng·mL -1 for Th(IV)-CSP S, 13.6 ng·mL -1 for Th(IV)-AA III and 22.1 ng·mL -1 for Th(IV)-AA M, respectively. This new RRS method has high sensitivity and fairly good selectivity and can be applied to the direct determination of proteins in human serum with satisfactory results.

Decomposed characteristic of azo dyes by ozonization with ultrasonic enhancement

Azo dyes have been used in many industries (textile mill, printing and dyeing mill, paper and pulp mill) and have caused great environmental pollution due to complicated constitution and high chemical stability. The construction of azo dyes can be destroyed by ozonization, but not thoroughly when the ozone dosage is controlled to a certain extent and the operating cost is higher. Ozonization decomposed ability with ultrasonic enhancement on azo dyes has been demonstrated in the study. The conclusion derived from this investigation may be summarized as follows: (1) The decoloration rate of arsenazo I solutions during sono-zone treatment is more rapid than the rate obtained with ozone alone because the complicated constitution has been destroyed by the O free radical from ozone decomposition. (2) The destructing pathway of arsenazo I by ozone with ultrasound is identical with that of by ozone alone: the breakdown of-N=N-bonds, the conversion of benzene ring to car-boxylic acid, and-HSO3 bonds to H2SO4. So,

阻抑过氧化氢氧化偶氮胂I褪色反应动力学光度法测定痕量锌

基于pH=10.3NH3-NH4Cl缓冲介质中,反应温度为100℃时,痕量锌(II)阻抑H2O2氧化偶氮胂I(AsAI)的褪色反应,建立了测定痕量锌(II)的阻抑反应动力学光度法。在固定加热时间段(4min10s)后,于515nm处测定AsAI的吸光度增加值,监控反应速率。方法检出限为1.72μg/L,校准曲线的浓度线性范围为0.0～2.0μg/25mL。讨论了酸度、反应物浓度、温度、反应时间、干扰离子等因数的影响,研究了反应的最佳条件,并测定了一些动力学参数,阻抑反应的表观活化能为84.00kJ/mol。方法用于奶粉样品中痕量锌(II)的测定,相对标准偏差为2.4%～3.1%,加标回收率为98.2%～103.2%。

偶氮胂Ⅰ分光光度法测定替米沙坦的含量

在pH7.90的Britton-Robinson缓冲介质中,替米沙坦与偶氮胂Ⅰ染料反应,形成离子缔合物,溶液颜色发生明显改变,最大吸收波长在558nm,从而建立测定替米沙坦的分光光度法。在最大波长558nm处,替米沙坦浓度在0—2.25×10^(-5)mol/L时遵守比耳定律,表观摩尔吸光系数ε为3.14×10~4L/(mol·cm),检出限为5.93×10^(-7)mol/L。本法操作简便,体系稳定,灵敏度较高,选择性较好,用于临床用药和合成样中替米沙坦含量的测定,结果满意。