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.     

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 rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples

A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, λ-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, τ-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L⁻¹ with RSDs values ≤3–25% (n = 5). The coefficients of estimation of the calibration curves obtained following the proposed methodology were ≥0.998. Recovery values were in the range of 45–106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L⁻¹.     

A method for the determination of tritium distribution in environmental and biological samples

A method for the determination of the tritium distribution in environmental and biological samples is described. Tritium as HTO is removed by freeze-drying and the residue is combusted to obtain organically bound tritium. Each tritium fraction is electrolytically enriched and determined by liquid scintillation spectrometry. Enrichment and large sample sizes are required due to the low environmental tritium levels. During the analyses of more than 600 samples over a two-year period all aspects of the method (freeze-drying, combustion, enrichment and counting) have provided reproducible and precise results.     

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.     

Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C₆mim][PF₆] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L⁻¹, while the relative standard deviation (RSD) was 3.4% (at 1 μg L⁻¹ Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.     

Rapid determination of antimony in biological and environmental samples using instrumental neutron activation analysis

A rapid non-destructive activation analysis method has been developed for the determination of antimony. A high resolution low energy Ge detector is used to measure the 61.6 keV γ-ray from^122mSb (T=4.2 min). Sensitivities and detection limits for biological and environmental samples activated with thermal and epithermal neutrons are listed. The time required for the anlaysis is about 12 min per sample using thermal activation and 22 minutes using epithermal activation analysis.     

A sensitive spectrophotometric method for the determination of dithiocarbamate fungicide and its application in environmental samples

A sensitive spectrophotometric method based on the evolution of CS₂ and colour development by leuco crystal violet is described for the determination of dithiocarbamate fungicides, e.g. thiram, ziram and zineb. Dithiocarbamate fungicides release CS₂ on acid hydrolysis. This CS₂ is absorbed in ethanolic sodium hydroxide and forms xanthate. The xanthate formed is subsequently treated with potassium iodate and N-chlorosuccinimide, during which free iodine is liberated. Crystal violet dye was formed through selective oxidation of leuco crystal violet by liberated iodine, which has an absorbance maxima at 595 nm. The colour systems obey Beer's law in the range of 0.02–0.20, 0.02–0.24 and 0.04–0.32 ppm for thiram, ziram and zineb respectively. The molar absorptivity of the colour system were found to be 9.6×10⁵, 1.1×10⁶ and 6.8×10⁵±100 l mol⁻¹ cm⁻¹ for thiram, ziram and zineb respectively. The method has been successfully applied to the determination of these dithiocarbamate fungicides in various environmental samples.     

Investigating the antimony determination in environmental samples by NAA

In recent years, environmental concerns regarding antimony have grown considerably due to anthropogenic processes that have resulted in increasing concentration of Sb in the environment, and also because of its impacts and possible adverse effects to living organisms. Several techniques have been used, to obtain reliable results for Sb, since Sb is present at low level concentration, requiring analytical instrumentation with low detection limits. The neutron activation analysis (NAA) technique has a high metrological level for the determination of several elements in different matrices. However, Sb determination in environmental and biological samples presents some analytical difficulties due to its low concentrations and gamma ray spectrum interferences. The objective of this research was to study on Sb determination in environmental reference materials by NAA. Ten environmental reference materials were selected and analyzed using long period irradiation at IEA-R1 research nuclear reactor. The induced gamma activities of ¹²²Sb and ¹²⁴Sb were measured. Relative errors of the results demonstrated that the accuracy depends mainly on Sb radioisotope measured, the decay time for counting and the sample composition.     

A simple and rapid hydride generation—atomic absorption method for the determination of arsenic in biological,environmental and geological samples

An inexpensive 50-ml disposable (hypodermic) syringe is used as the arsine generation vessel. The arsine is passed into a 10-cm long. 10-mm i.d. electrically heated silica tube atomizer with nitrogen carrier gas. Excess of hydrogen is burned off in a hydrogen diffusion flame at the ends of the tube. Samples containing appreciable silica are fused with KOH—MgO_XXX while organic samples are digested with H₂SO₄—H₂O₂. Parameters affecting the determination of arsenic as arsine have been investigated. Collaborative results on a variety of standard reference materials agree well with literature values. The advantages of the proposed method are that it is sensitive, selective, fast, simple, inexpensive, precise and accurate.     

A simple spectrophotometric method for the determination of copper in industrial, environmental, biological and soil samples using 2,5-dimercapto-1,3,4-thiadiazole.

A simple spectrophotometric method is presented for the rapid determination of copper at a trace level using 2,5-dimercapto-1,3,4-thiadiazole (DMTD) as a new spectrophotometric reagent. The method is based on the reaction of non-absorbent DMTD in a slightly acidic (0.002-0.014 mol dm(-3) sulfuric acid) aqueous solution with copper(II) to produce a highly absorbent greenish-yellow chelate product that has an absorption maximum at 390 nm. The reaction is instantaneous and the absorbance remains stable for 24 h. The average molar absorption coefficient and Sandell's sensitivity were found to be 5.65 x 10(4) dm3 mol(-1) cm(-1) and 10 ng cm(-2) of CuII, respectively. Linear calibration graphs were obtained for 0.1-20 microg cm(-3) of CuII; the stoichiometric composition of the chelate is 1:2 (Cu:DMTD). A large excess of over 50 cations, anions and complexing agents (e.g. tartrate, oxalate, citrate, phosphate, thiourea, SCN-) do not interfere in the determination. The method was successfully used for the determination of copper in several Standard Reference Materials as well as in some environmental water samples, biological samples, soil samples and solutions containing both copper(I) and copper(II) and complex synthetic mixtures. The method has high precision and accuracy (s = +/-0.01 for 0.5 microg cm(-1)).     

A cloud point extraction for spectrophotometric determination of ultra- trace antimony without chelating agent in environmental and biological samples

We report on a simple, sensitive and reliable method for the cloud point extraction of antimony (Sb) and its subsequent spectrophotometric detection. It is based on the color reaction of Sb (III) with iodide in acidic medium and subsequent micelle-mediated extraction of tetraiodoantimonate using a non-ionic surfactant in the absence of any chelating agent. The effects of reaction and extraction parameters were optimized. The calibration plot is linear in the range of 0.80–95?ng?mL^?1 of antimony in the sample solution, with a regression coefficient (r) of 0.9994 (for n?=?9). The detection limit (at SNR?=?3) is 0.23?ng?mL^?1, and the relative standard deviations at 10 and 70?ng?mL^?1 of antimony are 3.32 and 1.85?% (at n?=?8), respectively. The method compared favorably to other methods and was applied to determine antimony in seawater, anti-leishmania drug (glucantime), and human serum.

A simple and sensitive spectrophotometric method for the determination of trace amounts of nitrite in environmental and biological samples using 4-amino-5-hydroxynaphthalene-2,7-disulphonic acid monosodium salt

A very simple, sensitive, fairly selective and rapid spectrophotometric method for the determination of trace amounts of nitrite has been described. This method is based on the diazotized intramolecular coupling of electrophilic diazonium cation with the phenolic group of 4-amino-5-hydroxynaphthalene-2,7-disulphonic acid monosodium salt (AHNDMS) in a phosphate buffer solution of pH 7.5. The cyclic product has a purple color with maximum absorbance at 560 nm and is stable for 6 h. Optimum reaction conditions and other important analytical parameters for the maximum color development were established. Beer's law was found to obey for nitrite in the concentration range of 0.1–1.6 μg ml^?1 with molar absorptivity of 2.6 × 10⁴ l mol^?1 cm^?1 and Sandell's sensitivity of 0.0075 μg ml^?1. The effect of interfering ions on the determination is described. The recommended method was applied for the determination of nitrite in different water, soil and human saliva samples. The performance of the recommended method was evaluated in terms of Student's t-test and variance ratio F-test, which indicated the significance of proposed method over the reference method.     

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.     

A simple and sensitive method for the determination of hydroxylamine in fresh-water samples using hypochlorite followed by gas chromatography.

A new and simple method for the determination of hydroxylamine in environmental water, such as fresh rivers and lakes using hypochlorite, followed by its gas choromatographic detection, has been developed. A glass vial filled with sample water was sealed by a butyl-rubber stopper and aluminum cap without head-space, and then sodium hypochlorite solution was injected into the vial through a syringe to convert hydroxylamine to nitrous oxide. The head-space in the glass vial was prepared with 99.9% grade N2 using a gas-tight syringe. After the glass vial was shaken for a few minutes, nitrous oxide in the gas-phase was measured by a gas chromatograph with an electron-capture detector. The dissolved nitrous oxide in the liquid-phase was calculated according to the solubility formula. The proposed method was applied to the analysis of fresh-water samples taken from Iu river and Hii river, flowing into brackish Lakes Nakaumi and Shinji, respectively.     

一种简单灵敏的盐酸文拉法辛测定方法

四苯硼钠对罗丹明B具有荧光猝灭作用,使其荧光信号强度减弱甚至消失,而盐酸文拉法辛可以跟四苯硼钠反应生成更稳定的疏水性离子缔合物沉淀,使罗丹明B重新释放出来,又使该体系荧光信号强度增强,且荧光信号的增强程度与盐酸文拉法辛的加入量成正比关系,据此建立了一种反荧光猝灭法测定盐酸文拉法辛新方法。以365nm为激发波长,610nm为发射波长,测量了试液和空白液荧光强度之差ΔF。盐酸文拉法辛的质量浓度在2.423～43.94mg/L范围内与△F值呈线性关系,线性回归方程为△F=1.1789ρ-9.158,相关系数R为0.9995,检出限为0.7268mg/L,方法 RSD为0.87%。用本方法对不同厂家生产的盐酸文拉法辛缓释片及盐酸文拉法辛胶囊样品进行测定,测定值与药品标示量基本相符,加标回收率在95%～103%之间。     

A simple radiochemical determination of90Sr in environmental samples

A simple procedure for the determination of⁹⁰Sr in environmental samples is described. The method uses the different solubilities of the oxalates of calcium and strontium in presence of a large excess of calcium. For this reason the method is especially suited for Ca-rich samples, as e.g., bones or soils. However, after addition of supplementary calcium it works equally well for other types of samples. The method was tested by analyzing the IAEA Certified Reference Materials soil, animal bone and algae.     

A simple and sensitive gas chromatographic method for the determination of clonazepam in human plasma.

A simple gas chromatographic method for the determination of clonazepam in human plasma has been developed. After solvent extraction, the compound is measured by an electron capture detector on an OV-17 column. The electron-capture response is linear for 5-120 ng/ml of plasma. There is no interference from other commonly used anti-epileptic drugs or endogenous substrates. Preliminary data from routin monitoring of epileptic patients shows a 10-fold variation in their clonazepam plasma levels.