Validation of spectrophotometric method for Se(IV) determination: analytical applications

As selenium is an important part of the antioxidant enzymes and also because there are several studies suggesting a possible link between cancer and selenium deficiency, this paper presents a spectrophotometric method for the assay of Se(IV), using N,N-diethyl-p-phenylenediamine monohydrochloride as reagent. The proposed method is based on the reaction between the selenium and potassium iodide in low acidic medium, when iodine is released. This last product will further oxidise the new reagent. The final obtained product is strongly coloured in red and has an absorption maximum at 552 nm and molar extinction coefficient (ε) of 6.1?×?10⁴ L mol^?1 cm^?1. The optimum working conditions were established, and the developed method was validated, being characterised by a good linearity (in the range of 0.5–3.0 μg/mL), a limit of detection (0.0573 μg/mL) and a limit of quantification (0.1737 μg/mL). At the same time, the repeatability, the precision of the method and the accuracy were established. The proposed and validated method was applied with good results for the determination of Se(IV) in spring and bottled water from Iasi and also in pharmaceutical and cosmetic products.     

A nanosilver-based spectrophotometric method for determination of malachite green in surface water samples

A new spectrophotometric method is reported for the determination of nanomolar level of malachite green in surface water samples. The method is based on the catalytic effect of silver nanoparticles on the oxidation of malachite green by hexacyanoferrate (III) in acetate–acetic acid medium. The absorbance is measured at 610 nm with the fixed-time method. Under the optimum conditions, the linear range was 8.0?×?10^?9–2.0?×?10^?7?mol?L^?1 malachite green with a correlation coefficient of 0.996. The limit of detection (S/N?=?3) was 2.0?×?10^?9?mol?L^?1. Relative standard deviation for ten replicate determinations of 1.0?×?10^?8?mol?L^?1 malachite green was 1.86 %. The method is featured with good accuracy and reproducibility for malachite green determination in surface water samples without any pre-concentration and separation step.     

钼酸铵分光光度法测定废水中的元素磷

利用钼酸铵分光光度法测定了水样中的元素磷,发现该方法的灵敏度、准确度和稳定性都可以满足分析的要求,并且用元素磷标准样品进行了对比实验,分析误差在10%以内.     

Development of simple and sensitive spectrophotometric method for the determination of bendiocarb in its formulations and environmental samples

Facile, selective and sensitive spectrophotometric method has been developed for the determination of bendiocarb in its insecticidal formulations, fortified water, food grains, agriculture wastewater and agriculture soil samples with prepared reagents. The method was based on alkaline hydrolysis of the bendiocarb pesticide, and the resultant hydrolysis product of bendiocarb was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with λmaxof457 nmorcouplingwith2, 6−dibromo−4−nitroanilinetoproducearedcoloredproductwithλ_max of474~nmorcouplingwith2, 4, 6−tribromoanilinetoformorangeredcoloredproducthasaλ_max of465 nm.Underoptimalconditions, Beer'slawrangefor2, 6−dibromo−4−methylaniline(DBMA)wasfoundtobe0.6−−14.0~μgmL ^-1, 0.8−−10.0 μgmL ^-1 for2, 6−dibromo−4−nitroaniline(DBNA)and0.4−−10.0 μgmL ^-1 for2, 4, 6−tribromoaniline(TBA).Themolarabsorptivityofthecolorsystemswerefoundtobe4.126~×~10⁴ lmol ^-1 cm ^-1 forDBMA, 3.254×10⁴ l~mol ^-1 cm ^-1 forDBNAand2.812×10⁴ lmol ^-1 cm ^-1 forTBA.Sandell'softhecolorreactionsare0.018 μgcm ^-2(DBMA), 0.052 μgcm ^-2(DBNA)and0.065 μgcm ^-2$ (TBA) respectively. The effect of the non-target species on the determination of bendiocarb was studied. The formation of colored derivatives with the coupling agents is instantaneous and stable for 18 h, 30 h, and 12 h. Performance of the proposed methods were compared statistically in terms Student's F and t-tests with the reported methods.     

双波长分光光度法同时测定叶绿素a、b

介绍了同时测定叶绿素ａ、ｂ 的双波长分光光度法。该法不进行预分离,直接测定,操作简便,结果与先分离、再以强氧化剂消解后分别测定镁离子浓度进而推算叶绿素ａ、ｂ 浓度的原子吸收法有一定可比性,本法具有进一步推广应用的价值。     

流动注射分光光度法测定废水中硫化物的研究

在硫化物的直接显色分光光度法 (GB/T1 71 3 3 -1 997)的基础上 ,对在线气体扩散 -流动注射分光光度测定废水中硫化物的管路参数等条件作了探讨。实验结果表明 ,硫化物的浓度在 0～ 1 0 mg/L范围内 ,具有良好线性关系。通过在线气体扩散分离技术 ,提高了分析速度 ,分析频率达 2 6次 /小时 ,方法的相对标准偏差在 3 .0 3 %～ 8.5 3 %之间 ,回收率在97.0 %～ 1 0 4.0 %之间。     

间接光度法测定水中硫酸根

介绍了用一定过量的氯化钡沉淀SO2-4,余下的Ba2+与加入一定过量的铬酸钾反应,存在于溶液中的铬酸根在pH3.4的HAc-NaAc介质中与联邻甲苯胺生成蓝绿色的产物,并且溶液的颜色随硫酸根的量呈线性关系,借此进行光度法测定硫酸根.本法选620nm为测定波长,硫酸根含量在0～125μg/10ml范围符合比尔定律.方法在用于测定自来水中硫酸根时,结果满意.     

Flow injection spectrophotometric determination of methamidophos using online hydrolysis

A new protocol for the online spectrophotometric determination of methamidophos has been developed. The method is based on online hydrolysis of methamidophos, and the resulting hydrolyzed product is reacted with sodium nitroproside to form a colored complex. The calibration curve is linear over the concentration range of 0.5–20 μgml^?–?1, with a molar absorptivity of 2.5×10⁴ L mol^?1 cm^?1. The method is fast and reproducible with a sample throughput of 90 samples/h. The method is successfully applied to formulations and real samples.     

A field-based spectrophotometric flow-injection system for automatic determination of chloride in soil water

The use of chloride as a tracer for soil water investigations is discussed. Limitations with laboratory based soil core and field based sampling are considered with respect to the poor suitability of the data for rigorous assessment of mechanistic models. Investigation of water movement in soil has been restricted by limitations in spatial and temporal sampling. Fine resolution sampling generates large numbers of samples which cause problems with post sampling laboratory analysis. This paper describes a field-based system for the analysis of chloride in soil water. There are three component parts to the system, (i) a custom sampling sub-system comprising of ceramic cup suction samplers and sample traps, (ii) a sample routing sub-system to channel sample to (iii) a sample analysis sub-system utilizing a flow injection method for sample analysis using a custom built photo-diode detector. The three sub-systems were controlled by a suitably equipped personal computer. A calibration procedure is described with a third order polynomial equation derived to convert millivolt response from the detector into chloride concentration. Field and laboratory data from a tracer experiment are presented and discussed, and it is concluded that the system is well suited to field-based applications. Finally it is noted that the photo-detector is suitable for colourimetric analysis of any tracer with suitable chemical determination.     

火焰原子吸收法测定水中总铬

水中铬的测定有一定的技术难度。本文采用原子吸收测定方法,以铵盐作基体改进剂,可以有效地抑制铁与镍对水中铬的干扰。在仪器最佳工作条件下,对混合标准样进行了对比测定,获得了满意的测定结果     

多元配合物胶束增溶光度法测定微量氰化物

根据CN-对丁二酮肟-Ni-OP-10体系的增色作用,建立了一种测定微量氰化物的新方法.该方法操作简便,选择性好,不需要蒸馏和萃取.CN-量在0～5μg/25ml内符合比尔定律,用于环境水中氰化物的测定,结果满意.     

Dibenzazepin hydrochloride as a new spectrophotometric reagent for determination of hydrogen peroxide in plant extracts

A rapid, simple, accurate, and sensitive visible spectrophotometric method for the determination of trace amounts of hydrogen peroxide in acidic buffer medium is reported. The proposed method is based on the oxidative coupling of Ampyrone with dibenzazepin hydrochloride by hydrogen peroxide in the buffer medium of pH?4.0 which is catalyzed by ferrous iron. The blue-colored product formed with maximum absorption at 620?nm was found to be stable for 2?h. Beer's law is obeyed for hydrogen peroxide concentration in the range of 0.03-0.42?μg?ml(-1). The optimum reaction conditions and other important optical parameters are reported. The molar absorptive and Sandell's sensitivity are found to be 5.89?×?10(4)?mol(-1)?cm(-1) and 0.57?g/cm(2), respectively. The interference due to diverse ions and complexing agents was studied. The method is successfully applied to the determination of hydrogen peroxide in green plants satisfactorily.     

A new nanosilver-based spectrophotometric method for monitoring Eriochrome black T in river water

In this paper, a new spectrophotometric method is reported for the determination of nanomolar levels of Eriochrome black T in environmental samples. The method is based on the catalytic effect of silver nanoparticles on the oxidation of Eriochrome black T by hexacyanoferrate (III) in acetate–acetic acid medium and at 25 °C. The absorbance is measured at 512 nm with the fixed-time method. It relies on the linear relationship between the absorbance difference (?A) and Eriochrome black T amounts in the range of 40–1,250 nM. Under optimum conditions, the sensitivity of the proposed method, i.e., the detection limit corresponding to 80 s, is about 25 nM. The method is featured with good accuracy and reproducibility for Eriochrome black T determination in river water samples without any pre-concentration and separation step.     

铋磷钼蓝分光光度法测定土壤中磷含量

土壤中磷含量的分析是土壤环境监测的主要项目之一.建立了铋磷钼蓝分光光度法测定土壤中磷含量的新方法,与现有的《土壤全磷测定方法》(GB 9837-88)和土壤总磷快速检测仪方法进行了比较讨论.方法的检出限为5.0 mg/kg,对磷含量为475 mg/kg和292 mg/kg的标准土壤样品进行测定,结果与标准值吻合,其相对...     

废水中总氰化物测定的新方法

研究了用气提法测定废水中总氰化物的条件的方法.实验结果表明,与蒸馏法相比,气提法简便安全,分析结果的准确度和精密度能满足监测要求.     

FIA-coupled spectrophotometric method for determination of Cr (VI) traces in natural waters: application of in-line dissolution of 1,5-diphenylcarbazide after heat treatment and activated alumina as adsorbent for preconcentration

This work proposes the quantification of Cr (VI) ions in natural waters in trace level, using activated alumina (Al₂O₃) as preconcentration support, controlled in-line dissolution of the solidified chromophore diphenylcarbazide after heat treatment and spectrophotometric detection. The manifold ensures high sensitivity of analytical response, good repeatability, and stability. In this work, optimization of experimental conditions of a flow injection system was chosen as the parameters for greater sensitivity and better selectivity. The selected optimized conditions were 0.30 mol L^?1 for H₂SO₄ concentration, system flow rate as 0.40 mL min^?1, sample injection volume of 192.50 μL, 2 min for preconcentration time, and 0.10 mol L^?1 for eluent concentration. The analytical curves obtained for real sample analysis show linear range from 0.192 to 0.961 μM, linear correlation coefficient R?=?0.9997 and LOD?=?0.024 μM. The preconcentration factor of about four times was obtained through the passage of 800 μL of a standard solution containing 0.961 μM of Cr (VI) through mini-column of preconcentration followed by elution at 192.5 μL of NH₄OH 0.1 mol L^?1 solution. The solid chromogenic reagent presented high durability (weeks in daily use with mass of 0.0993 g) and good reproducibility in analytical signal. The reactivation of the mini-column of alumina should be executed after ten injections of eluent, using 800 μL of HCl 0.02 mol L^?1 solution in flow through the same. Each cycle of injection and elution of the sample takes about 5 min on the proposed terms. Despite the length of each cycle still be high, low concentrations can be detected using a technique of relatively low cost. This is due in part, the association dissolution of the chromogenic reagent directly in the line and the preconcentration step. Another important factor is the economy of reagent chromogenic, low generation of reject contributing to better quality of the environment, and the high potential for applications to work in field.     

Interlaboratory comparability of copper complexation capacity determination in natural waters

The results of a test of interlaboratory comparability for the determination of copper complexation capacity and copper-ligand complex formation constant are presented. Eight water samples comprising, six natural waters, a synthetic ligand solution and a blank solution were analysed by seven laboratories using their own methods of complexation titration. Given the wide variation that might have been possible, relatively good comparability was demonstrated amongst the variety of methods for determining copper complexation capacity. The complexation capacity data largely satisfied the predefined criterion of agreement to within 50%. This provides support for the use of metal speciation criteria in the regulation of copper in the environment. Data for the determination of complex formation constants were of poorer comparability, ranging between 10(7) and 10(12) for the same water.     

A spectrophotometric assay method for vanadium in biological and environmental samples using 2,4-dinitrophenylhydrazine with imipramine hydrochloride

A simple, rapid, and sensitive method involving the interaction of 2,4-dinitrophenylhydrazine with imipramine hydrochloride in presence of vanadium (V) in sulfuric acid medium has been proposed for the determination of vanadium. The purple-colored product developed showed an absorption maximum at 560 nm and was stable for 24 h. The working curve was linear over the concentration range of 0.1–2.8 μg ml^− 1, with sensitivity of detection of 0.0124 μg ml^− 1. Molar absorptivity and Sandell’s sensitivity were found to be 2.6 × 10⁴ l/mol cm and 0.0039 μg cm^− 1, respectively. The accuracy of the proposed method was assessed by Student’s t test and variance ratio F test, and the results were on par with the reported method. The method was successfully used in the determination of V in water, human urine, soil, and plant samples, and it was free from interference by various concomitant ions.