A simple method for the spectrophotometric determination of atrazine using p-aminoacetophenone and its application in environmental and biological samples

A spectrophotometric method is described for the determination of the widely used herbicide, atrazine. Atrazine reacts with pyridine and forms a quaternary halide which adds a hydroxyl group in the presence of alkali to form a carbinol base. The heterocyclic ring of the resulting carbinol breaks forming a glutaconic dialdehyde which is subsequently coupled with p-aminoacetophenone (PMP) to form a yellow orange polymethine dye. Beer's law is obeyed in the range 0.16–1.6 ppm of atrazine at 470 nm. The method is sensitive and free from the interference of most of the foreign species. The analytical parameters have been optimised and the method has been successfully applied to the determination of atrazine in various environmental and biological samples.     

A sensitive spectrophotometric determination of atrazine in micellar medium and its application in environmental samples

A sensitive analytical procedure based on solid phase extractive-spectrophotometry has been established for the determination of the widely used herbicide atrazine .The method is based on the Konig reaction in which atrazine reacts with pyridine reagent to form a quaternary pyridinium halide, which further forms glutaconic aldehyde in the presence of alkali. Glutaconic aldehyde is subsequently coupled with 4-aminoacetanilide in the micellar medium of anionic surfactant sodium dodecyl sulphate to give a yellow-orange dye. The produced dye was enriched on a C₁₈ cartridge and is measured spectrophotometrically at 460 nm. The sensitivity and selectivity of the method was largely enhanced in the micellar media and SPE on the C₁₈ cartridge and avoids the use of toxic solvents. Beer’s law was obeyed in the range 0.012–0.12 μg mL^?1. Molar absorptivity and Sandell’s sensitivity were found to be 1.52 × 10⁶ L mol^? 1 cm^?1 and 0.0002 μg cm^?2, respectively. The limit of detection and quantification were 0.001 and 0.003 μg mL^?1, respectively. The proposed method was applied successfully for the determination of atrazine in environmental and biological samples with a recovery range of 96–101 %. The method was found to be free from interference of a large number of foreign species. The accuracy and reliability of the method was further established by parallel determination by the reference method, and by recovery studies.     

A new reagent system for the highly sensitive spectrophotometric determination of selenium

Highly sensitive and simple spectrophotometric determination of selenium is described for the determination of selenium(IV) using a new reagent leuco malachite green. The method is based on the reaction of selenium(IV) with potassium iodide in an acidic condition to liberate iodine, the liberated iodine oxidizes leuco malachite green to malachite green dye. The green coloration was developed in an acetate buffer (pH 4.2–4.9) on heating in a water bath (∼ 40 °C). The formed dye exhibits an absorption maximum at 615 nm. The method obeys Beer’s law over a concentration range of 0.04–0.4 μg mL⁻¹ selenium. The molar absorptivity and Sandell’s sensitivity of the color system were found to be 1.67 × 10⁵ L mol⁻¹ cm-¹ and 0.5 ng cm⁻², respectively. The optimum reaction conditions and other analytical parameters have been evaluated. The proposed procedure has been successfully applied to the determination of selenium in real samples of water, soil, plant material, human hair, and cosmetic samples. The results were compared to those obtained with the reference method. Statistical analysis of the results confirms the precision and accuracy of the proposed method. In addition, the developed method is cost-effective and involves easily accessible instrumentation technique which can be used by ordinary research laboratories.     

A new and sensitive method for the spectrophotometric determination of ethion in environmental and biological samples

A new and sensitive spectrophotometric method is described for the determination of sub ppm levels of the organophosphorus pesticide ethion based on the oxidation of ethion by potassium permanganate in phosphoric acid to sulphones and its hydrolysis under acidic condition at 100°C to release formaldehyde, which is then determined by a reaction with 1,3,5-trihydroxybenzene (phloroglucinol) in alkaline medium. Beer's law is obeyed in the range of 0.1–0.8 ppm of ethion at 460 nm. The analytical parameters have been optimized.     

A sensitive spectrophotometric method for lead determination by flow injection analysis with on-line preconcentration

A new flow injection (FI) system for the determination of Pb(II) at trace level with a preconcentration step and spectrophotometric detection is proposed. It is based on preconcentration of lead ions on chitosan and dithizone-lead complex formation in aqueous medium (pH 9). The chemicals and FIA variables influencing the performance of the system were optimized and applied to the determination of lead in natural, well, and drinking water samples. It is a simple, highly sensitive, and low cost alternative methodology. The method provided a linear rage between 25 and 250 μg l⁻¹, a detection limit of 5.0 ng ml⁻¹ and a sample throughput of 15 h⁻¹. The obtained results of spiked samples are in good agreement between the proposed method and ICP-AES.     

一种简单灵敏的光度法测定环境水样中痕量对苯二酚

在SCN -存在下,控制溶液pH5.0,对苯二酚使Cu(Ⅱ)还原生成的Cu(Ⅰ)与SCN -反应生成CuSCN沉淀,通过测定溶液中剩余Cu(Ⅱ)的量,可以测定对苯二酚的含量.吸光度与对苯二酚含量之间存在良好线性关系.线性方程:A =4.567 +0.9726ρ(μg/mL),线性范围为0.16～4.0μg/mL,相关系...     

A new spectrophotometric method for the determination of hydrazine in environmental samples

Summary Hydrazine is determined spectrophotometrically by using veratraldehyde (3,4-dimethoxybenzaldehyde) as a new reagent. The reaction is based on the condensation of veratraldehyde with hydrazine in acidic medium. The resulting yellow coloured condensation product has maximum absorption at 410 nm. The colour system obeys Beer's law in the range of 0.065 to 0.3 g/ml of hydrazine. Molar absorptivity and Sandell's sensitivity are found to be 6.72×10⁴ l mol^–1 cm^–1 (±100) and 0.0004 g cm^–2, respectively. The method is successfully applied for the determination of hydrazine in polluted water, biological samples, in isoniazide tablets and in air. It is compared with other reported spectrophotometric methods and is found to be of comparable sensitivity.     

New reagents for the facile and sensitive spectrophotometric determination of carbofuran in its formulations and environmental samples

Facile and sensitive spectrophotometric methods were developed for the determination of carbofuran in its formulations and environmental samples by using new reagents. The methods were based on the coupling reaction of hydrolysed product of cabofuran with diazotized reagents, namely, 2,6-dibromo-4-methylaniline, 2,6-dibromo-4-nitroaniline, and 2,4,6-tribromoaniline in basic medium to give color derivatives having the absorption maximum at 468, 474, and 410 nm, respectively. The color derivatives were correspondingly stable for 40, 30, and 16 h. Beer’s law was obeyed in the carbofuran concentration range 0.2–10.0 μg/mL. The proposed methods have been found to be applicable to the determination of carbofuran in its formulations, tap and distilled water, grains, polluted water, plant material (cabbage), and soil samples. The text was submitted by the authors in English.     

铟的灵敏光度测定法

我国对微量铟的显色反应研究得较少.最常用的是碱性染料萃取光度法,但操作冗繁而且苯的毒性较大.因此寻找灵敏度高而又能在水相测定铟的新方法是很有必要的. 用苯荧光酮(2,3,7-三羟基-9-苯基-6-荧光酮,PF)作显色剂的胶束增溶分光光度法已应用于锗、钼、锡、镓等的测定,但用类似的方法测铟则尚未见报道.我们的实验证明,在pH为7.7～8.9的醋酸-氢氧化铵缓冲介质中,铟与PF及氯化十六烷基吡啶(OPC)生成玫瑰红色的三元配合物,其配合比为In(III):PF:CPC=1:2:2,表观稳定常数为8.6×10~(10),摩尔吸收系数达1.28×10~5.提出用乙酸乙酯萃取分离杂质.利用本显色反应测定微量铟,方法灵敏且稳定,准确度和精密度均较好.     

A sensitive method for the ultraviolet spectrophotometric determination of chloride

A new method for the determination of chloride ion is based on the formation of phenylmercury(II) chloride, its extraction into chloroform and reaction with sodium diethyldithiocarbamate to form phenylmercury(II) diethyldithiocarbamate. This complex has spectral maxima at 257 and 297 nm. either of which can he used for quantitative purposes. The molar absorptivities are 21.3·10³ and 6.5·10³ respectively. referred to the chloride ion. The method is especially suitable for the determination of trace amounts of chloride in aqueous solution and has been applied to samples of drinking water. Amounts of chloride in the range 0.04 0.32 p.p.m. can be determined in 250-ml aqueous samples with an average relative mean error of 12%. The method can be used also for bromide and iodide, and for organomercury(11) compounds. Interferences are minimal and the method compares favourably with the standard mercury(II) thiocyanate procedure.     

Surfactant-mediated extraction of iron and its spectrophotometric determination in rocks, minerals, soils, stream sediments and water samples

An extraction spectrophotometric method for iron determination in rocks, minerals, soils, stream sediments and water samples has been developed. At pH 3-4, iron (III) forms a 1:2:1 ternary complex with thiocyanate and cetyltrimethylammonium bromide (Fe/SCN/CTAB) which is extracted into ethyl acetate. The readily formed purple complex is suitable for extraction spectrophotometric determination of iron in rocks and related materials from submicrogram to milligram levels. The method is free from any interference due to commonly associated ions present in the matrices of rock samples. The present method is at least fourfold more sensitive (ε=3.2×10⁴ l mol⁻¹ cm⁻¹) than the conventional thiocyanate method and, in addition to the enhanced sensitivity and selectivity, it has got definite advantages over the corresponding binary thiocyanate system in terms of substantial improvement in the stability of the complex formed and broadening of Beer's law adherence range (0-6.0 mg/l). The method has been applied to a number of geological and hydrogeochemical samples for the determination of iron and the results obtained have been found to be favourably comparable with those obtained from the standard methods.     

A sensitive spectrophotometric method for the determination of desloratadine in tablets

A simple, rapid, and sensitive visible spectrophotometric method was developed, for the first time, for analysis of desloratadine (DE) in tablets. The method is based on the deep-blue colored TCNQ*- radical anion formed by interaction of the drug (n-donor) with 7,7,8,8-tetracyanoquinodimethane (TCNQ, pi-acceptor) in acetonitrile at ambient temperature. Optimum conditions for the reaction were investigated, absorbances were read at 843 nm, and the linearity range for concentrations of DE was found to be 1.5-13 microg/mL. The reaction product remains stable up to 8 h when kept at room temperature in the dark. The developed method was validated and successfully applied to the determination of DE in tablets. The tablets were also analyzed with a column liquid chromatography method reported in literature. The results from both methods were statistically compared by t- and F-tests. No significant difference was found for the means and standard deviations at 95% confidence level. Accuracy was examined through recovery studies. Being very simple and reliable, the method can be recommended for routine quality control analysis of DE in tablets.     

Micellanized spectrophotometric method for the determination of beryllium using haematoxylin

A simple and sensitized spectrophotometric method for the determination of trace amounts of beryllium has been described. The method is based on the formation of a ternary complex by the reaction of beryllium with haematoxylin in the presence of micellar medium (cationic surfactant, cetyltrimethylammonium bromide). The ternary complex of beryllium has a maximum absorbance at 592 nm and showed an excellent sensitivity (molar absorption coefficient of 7.07 x 10(4)L mol(-1)cm(-1) and the Sandell's sensitivity being 1.27 x 10(-4) microg cm(-2)) and reproducibility (within-day precision: R.S.D.相似文献   

A membraneless gas-diffusion unit-multisyringe flow injection spectrophotometric method for ammonium determination in untreated environmental samples

A new design of a membraneless gas-diffusion (MGD) unit coupled to a multisyringe flow injection system is proposed. The spectrophotometric determination of ammonium using an acid-base indicator was chosen to show the feasibility of this approach. Hence, in alkaline medium, ammonium ions are transformed into ammonia (donor channel) which diffuses through the headspace into the acceptor stream (bromothymol blue solution), causing a pH change and subsequently a colour change. The exploitation of the enhanced potentialities of this re-designed MGD device was the main purpose of the present work. Hence, several strategies concerning flow management were studied seeking to characterize and improve the analytical features of the methodology and moreover, untreated environmental samples were analysed without previous filtration. Consequently, stopped flow in acceptor channel with continuous flow in donor channel was chosen for the application to wastewater and spiked river water samples. A linear concentration range between 10.0 and 50.0 mg L⁻¹ of NH₄⁺, a limit of detection of 2.20 mg L⁻¹ and a determination frequency of 11 h⁻¹ were obtained.     

Kinetic spectrophotometric method for rapid determination of trace formaldehyde in foods

A simple and sensitive kinetic-spectrophotometric method was developed for the determination of ultra trace amount of formaldehyde in food samples. The method was based on the oxidation of rhodamine B (RhB) by potassium bromate in sulfuric acid medium (formaldehyde as catalyst). The reaction was monitored by measuring the decrease in absorbance of the dye at 515 nm after 6 min. The developed method allowed the determination of formaldehyde in the range of 10–100 μg L⁻¹ with good precision, accuracy and the detection limit was down to 2.90 μg L⁻¹. The relative standard deviations for the determination of 10 and 60 μg L⁻¹ of formaldehyde were 3.0% and 1.9% (n = 10), respectively. The method was found to be sensitive, selective and was applied to the determination of formaldehyde in foods with satisfactory results.     

Cloud-point extraction,preconcentration, and spectrophotometric determination of palladium in water samples

The possibility of using Thio-Michler's Ketone (TMK), 4,4′-bis(dimethylamino) thiobenzophenone, for palladium(II) concentrated by micellar extraction at the cloud-point temperature, and later spectrophotometric determination, was investigated. Under the optimum conditions, preconcentration of 50?mL of water samples in the presence of 0.1% (w/v) octylphenoxy polyethoxy ethanol (Triton X-114), 2?×?10^?6?mol?L^?1?TMK and 1?×?10^–3?mol?L^?1 buffer solution (pH?=?3.0) gave the limit of detection of 0.47?ng?mL^?1, and the calibration graph was linear in the range of 2–50?ng?mL^–1. The recovery under optimum working conditions was higher than 97%. The proposed method has been applied to the spectrophotometric determination of palladium(II) in natural water samples after cloud-point extraction with satisfactory results.     

A simple and sensitive analytical method for the determination of antimony in environmental and biological samples.

The results of a study and application of leucocrystal violet for the determination of antimony in parts per million levels is described here. The proposed method is based on the reaction of antimony(III) with acidified potassium iodate to liberate iodine. The liberated iodine selectively oxidizes leucocrystal violet to crystal violet dye. The formed dye shows maximum absorbance at 590 nm. The color system obeys Beer's law in the concentration range from 0.4 - 3.6 microg antimony per 25 ml of final solution. The molar absorptivity and Sandell's sensitivity were found to be 7.32 x 10(5) l mol(-1) cm(-1) and 0.0016 microg cm(-2), respectively. All variables were studied in order to optimize the reaction. The proposed method is satisfactorily applicable for the analysis of antimony in various environmental and biological samples. The method is simple, highly sensitive, accurate and reliable.     

两相体系分光光度法测定聚乙二醇化蛋白质混合物中游离聚乙二醇

建立了用硫氰酸铁胺-氯仿两相体系分光光度法测定游离聚乙二醇含量的方法。确定了最大吸收波长，考察了混合振荡时间、其他生物大分子存在对测定结果的影响，并与三硝基苯磺酸(TNBS法)进行了比较。     

高效液相色谱快速测定水产品中孔雀石绿、结晶紫及其无色产物的残留量

采用高效液相色谱同时检测水产品中孔雀石绿、结晶紫及无色孔雀石绿和无色结晶紫的残留量,样品经提取、净化处理后所得残渣用乙腈溶解后,通过采用C_(18)色谱柱,以乙腈(A)和pH3.0的0.02 mol·L~(-1)磷酸二氢钾缓冲溶液(B)按不同比例混合进行梯度淋洗,实现孔雀石绿、结晶紫及其代谢物的分离。用自制的二氧化铅柱氧化无色孔雀石绿及无色结晶紫。在588 nm波长处,测定4种物质的质量浓度在0.3～6.0 mg·L~(-1)范围内与其峰面积呈线性关系,相对标准偏差(n=6)小于2.5%,检出限(3S/N)小于1.9μg·kg~(-1),分析时间20 min。以凤尾鱼罐头为基体进行回收试验,方法的回收率在71.5%～88.6%范围。     

Rapid and sensitive spectrophotometric determination of trace amounts of iron(III) using leuco Xylene cyanol FF

A new, simple, sensitive, and reliable method is presented for the rapid spectrophotometric determination of trace amounts of iron(III) using leuco Xylene cyanol FF. The method is based on the oxidation of leuco Xylene cyanol FF (LXCFF) to its blue form of xylene cyanol FF by iron(III) in sulfuric acid medium (pH 2.0–3.0), the absorbance of the formed dye is measured in an acetate buffer medium (pH 2.8–4.4) at 615 nm. The method obeys Beer's law over a concentration range of 0.15–0.9 g mL^-1 iron, having a molar absorptivity of 5.6×10⁴ L mol^-1 cm^-1 and a Sandell's sensitivity of 0.0001 g cm^-2. The optimum reaction conditions and other analytical parameters have been evaluated. The developed method has been successfully applied to the determination of iron in water, soil, industrial effluent, plant material, pharmaceutical preparations, synthetic mixtures, and aluminum alloys.