Spectrophotometric determination of beryllium in water samples after micelle-mediated extraction preconcentration

A new micelle-mediated phase preconcentration method for preconcentration of ultra-trace quantities of beryllium as a prior step to its determination by spectrophotometry has been developed. Chrome Azurol S (CAS) and cetyltrimethylammonium bromide (CTAB) were used as chelating agent and cationic surfactant, respectively. The method evaluates and eliminates the blank bias error present in such procedures using mean centering of ratio spectra. This procedure gives more accurate results than the traditional approach using absorbance values against reagent blank. The optimal extraction and reaction conditions were studied and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration and improvement factors) were obtained. Linearity was obeyed in the range of 0.9-18.0 ng mL⁻¹ (1.00 × 10⁻⁷-2.00 × 10⁻⁶ mol L⁻¹) of beryllium. The detection limit of the method is 0.51 ng mL⁻¹ (5.66 × 10⁻⁸ mol L⁻¹) of beryllium. The interference effect of some anions and cations was also tested. The method was applied to the determination of beryllium in spring water samples.     

An improved ion chromatographic method for determination of trace levels of perchlorate in environmental water

An improved ion chromatographic (IC) method was developed to determine trace levels of perchlorate in environmental water samples. Perchlorate was separated in the hydroxide selective column IonPac AS16 using NaOH as an eluent with an organic modifier. To eliminate the coelution of perchlorate and 4-chlorobenzene sulfonate (4-CBS), an organic solvent as modifier was added to the eluent. Of four organic solvents studied, acetonitrile proved to be the most efficient based on the retention time of perchlorate and 4-CBS. To improve the method sensitivity, a concentrator column (AG19) was used to concentrate perchlorate online. With the adoption of a preconcentration step, the sensitivity of our method was improved and the method detection limit (MDL) was reduced to 0.1 μg/L. The linear range was from 0.2 μg/L to 200 μg/L with a linear correlation coefficient of 0.9989 and the relative standard deviation (RSD) of peak area for eleven successive injections of 0.5 μg/L perchlorate was 4.2%. The method had been applied to the determination of perchlorate in some real environmental water samples and recovery was between 93% and 113%. __________ Translated from Chemical Journal of Chinese Universities, 2007, 28(7), 1246–1250 [译自: 高等学校化学学报]     

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   

Purge-and-trap ion chromatography for the determination of trace ammonium ion in high-salinity water samples

It has always been assumed that purge-and-trap (P&T) method is only used for the analysis of volatile organic compounds (VOCs) in aqueous samples. In this paper, a novel P&T preconcentrator has been developed for the determination of trace amounts of ammonium ion in high-salinity water samples by ion chromatography (IC). Method performance is evaluated as a function of concentration of assistant purging material, purging time, and flow rate. Under the optimum P&T conditions with the purified nitrogen gas at flow rate 40 mL/min for 15.0 min at 40 degrees C, the overall collection efficiency is independent of the concentration of ammonium over the range 1.2-5.9 microM. The enrichment factor (EF) of ammonium correlates the ratio of the sample volume to the acceptor solution volume in the trap vessel, providing potentially unlimited increase of the ammonium signal. Our results indicate that environmental samples with low levels of ammonium in matrices with high concentrations of sodium can be easily analyzed and the detection limit down to 75 nM (1.35 ppb) level, corresponding to picomole of ammonia in the injected sample. Calibration graph was constructed with ammonium standards ranging from 0.05 to 6.0 microM and the linearity of the present method was good as suggested by the square of correlation coefficients being better than 0.997. Thus, we have demonstrated that the P&T-IC method allows the routine determination of ammonium ion in seawater samples without cation interferences.     

Separation and preconcentration of ultra trace amounts of beryllium in water samples using mixed micelle-mediated extraction and determination by inductively coupled plasma-atomic emission spectrometry

In the present study a cloud point extraction process using mixed micelle of the cationic surfactant cetyl-pyridinium chloride (CPC) and non-ionic surfactant Triton X-114 for extraction of beryllium from aqueous solutions is developed. The extraction of analyte from aqueous samples was performed in the presence of 1,8-dihydroxyanthrone as chelating agent in buffer media of pH 9.5. After phase separation, the surfactant-rich phase was diluted with 0.4 mL of a 60:40 methanol-water mixture containing 0.03 mL HNO₃. Then, the enriched analyte in the surfactant-rich phase was determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The different variables affecting the complexation and extraction conditions were optimized. Under the optimum conditions (i.e. 1.6 × 10⁻⁴ mol L⁻¹ 1,8-dihydroxyanthrone, 1.2 × 10⁻⁴ mol L⁻¹ CPC, 0.15% (v/v) Triton X-114, 50 °C equilibrium temperature) the calibration graph was linear in the range of 0.006-80 ng mL⁻¹ with detection limit of 0.001 ng mL⁻¹ and the precision (R.S.D.%) for five replicate determinations at 18 ng mL⁻¹ of Be(II) was better than 2.9%. In this manner the preconcentration and enrichment factors were 16.7 and 24.8, respectively. Under the presence of foreign ions no significant interference was observed. Finally, the proposed method was successfully utilized for the determination of this cation in water samples.     

Partial least-squares regression for the simultaneous determination of aluminum and beryllium in geochemical samples using xylenol orange

A partial least-squares regression (PLS) was developed for the simultaneous spectrophotometric determination of aluminum and beryllium in geochemical samples by xylenol orange as the chromogenic reagent in water media and in micellar media. The effects of pH, xylenol orange concentration and surfactant concentration on the complexes formation reactions were studied. In the absence of surfactant the complex color development takes place at 2 h after mixing the reagents. By using CTAB as micellar media the complexes formation was improved and the rate of the complexation reactions increased. By using PLS-1 algorithm satisfactory results were obtained. The proposed procedure showed to be useful for prediction of Al and Be values from 0.1 to 1.0 mg L(-1).     

环境水样中痕量肼的荧光分析

基于在硫酸介质中，肼与罗丹明6G反应，使其荧光增强，建立了一种荧光测定痕量肼的新方法。该方法线性范围2．0－14．0μg/L，检出限为0．62μg/L。可用于环境水样中肼含量的测定，并进行了回收实验，回收率为97％－107％。     

Sensitive and selective ion exchange-combined atomic absorption: Spectrometric determination of trace elements in rocks

Ion-exchange precipitation was used in geochemical analysis where the various trace elements can be determined by prior separation over an ion-exchange column. By application of the principles of classical wet analysis the presence of trace elements was verified and their quantitative determination performed in rock samples by converting an anion exchanger into the respective ionic forms to obtain the insoluble salts through the action of counterion (an anion) of the resin and the metal ion in the solution. The metal ions are then eluted by suitable eluting reagents that form soluble salts. The columns of 5 g Amberlite IR-400 were used and were converted into the desired anionic forms. The different forms used were sulfide, hydroxyl, carbonate, chromate, and sulfate. Flow rate was maintained at 1 ml/min. Different rock samples were examined for Mn, Zn, Ba, Ni, Cu, and Sr, etc. The results have been compared with the standard results.     

Sensitive adsorptive stripping voltammetric method for direct determination of trace concentration of lead in the presence of cupferron in natural water samples

This paper reports the use of an adsorptive voltammetric technique for Pb(II) determination using cupferron as a selective complexing agent. After accumulation of the complex onto a hanging mercury drop electrode, the electrode potential was scanned with differential pulse modulation and the reduction current of lead was observed at about??0.5?V. Under optimum conditions (5?×?10^?4?mol?L^?1 cupferron concentration, 0.1?mol?L^?1 acetate buffer (pH 5.5), adsorption at??50?mV for 30?s) the detection limit was 5.1?×?10^?10?mol?L^?1. The relative standard deviation of five measurements for low lead concentration was 3.1%. The accuracy of the method was tested by analysing certified reference material (SPS-WW1 Waste Water). Finally, the method was successfully applied to the determination of Pb(II) in river water samples without any pretreatments.     

Development of an analytical method for beryllium in airborne dust by micellar electrokinetic chromatography

The separation of diacetylacetonato–beryllium [Be(acac)₂] from acetylacetone was achieved with micellar electrokinetic chromatography (MEKC) followed by subsequent beryllium analysis carried out using capillary electrophoresis. Analysis using a separation and absorption detector, with a 50 μm capillary cell, could detect approximately 1000 ppb of beryllium in the final sample. Be(acac)₂ is a promising reagent for absorption spectrophotometry, because its molar absorption coefficient, (32 000 l mol⁻¹ cm⁻¹) is very large. As the complex and acetylacetone have a similar absorption wavelength, the excess free ligand must removed from the sample to be measured. Acetylacetone is a weak acid with keto–enol tautomerism in aqueous solution. Acetylacetone and neutral Be(acac)₂ should be separated with capillary zone electrophoresis (CZE) using a neutral or basic buffer solution as the mobile phase. Although the pH and temperature of the mobile phase were optimized, separation with CZE was interfered with by a portion of acetylacetone. This interfering portion seems to be a neutral keto-form with the same migration time as Be(acac)₂. As a neutral species separation method, MEKC with sodium dodecyl sulfate was tried and the separation was completed. The optimum pH value and buffer temperature are pH 7.8 and 15°C, respectively.     

Sensitive and selective spectrophotometric method for the determination of trace amounts of osmium with 1,2,3-indanetrione monothiosemicarbazone

Summary Sensitive and Selective Spectrophotometric Method for the Determination of Trace Amounts of Osmium with 1,2,3-Indanetrione Monothiosemicarbazone A simple, sensitive and selective spectrophotometric method has been developed for the determination of osmium using 1,2,3-indane-trione monothiosemicarbazone (ITMT). The method is based on the colour reaction between ITMT and osmium(VIII) in hydrochloric acid (0.32–0.60 M) medium. The calibration graph for measurement at 440 nm is linear in the range 1.4–33.6g of osmium per 25ml, with a molar absorptivity of 6.43×10⁴l·mole^–1·cm^–1. The effect of interferences has been studied and the method applied to the determination of osmium in synthetic samples whose composition correspond to osmiridium or syserkite, with good results.     

Gas chromatographic methods for the determination of trace organic pollutants in environmental samples

Some problems, special features, and tendencies of the determination of trace organic compounds in various environmental samples with the use of chromatographic methods are considered.     

Instrumental method for the determination of trace elements in water samples by neutron activation analysis

Thermal neutron activation analysis and a large-volume high-resolution Ge(Li) gammaray spectrometer, connected on-line to a DEC PDP 8/L computer, have been used to measure the concentrations of Na, Sc, Cr, Fe, Co, Ni, Zn, As, Se, Br, Rb, Ag, Sb, Cs, W and Hg in some Italian subsurface water samples. The instrumental method requires neither a chemical separation technique nor a pre- or post-concentration of the trace elements to be detected. As a consequence, this method eliminates many inherent errors associated with chemical determinations. The technique is sensitive, precise and particularly suitable for routine analysis of many trace elements at both natural and pollution levels in water samples. The interferences due to fast neutron (n, p) and (n, α) reactions are not appreciable, with the only exception of the⁵⁴Fe(n, p)⁵⁴Mn and⁵⁸Ni(n, p)⁵⁸Co reactions. Losses of volatile, elements, e. g. As, Br and Hg, during irradiation proved to be negligible.     

A simple flow-injection chemiluminescence method for the determination of trace pentavalent vanadium in water samples

A simple method for rapid determination of trace pentavalent vanadium in natural water was presented by flow-injection chemiluminescence (CL). Through water injection, luminol and potassium permanganate were eluted from the anion exchange column to generate the CL, which was enhanced in the presence of V(V). Under the optimum conditions, the increased CL intensity was linear with V(V) concentration in the range from 0.1 to 100?ng?mL^?1. The limit of detection was 50?pg?mL^?1 (3σ) and the relative standard deviation (RSD) was 2.24% (n?=?5) for a 1.0?ng?mL^?1?V(V). At a flow rate of 2.0?mL?min^?1, one cycle of analysis could be performed in 0.5?min with a RSD of less than 3.0%. The proposed method was successfully applied to the determination of vanadium in natural water.     

Matrix removal for the ion chromatographic determination of some trace elements in milk

An ion chromatographic method has been developed for the determination of some microelements in different types of milk. It involves oxidative photodegradation of the organic matrix with H₂O₂ in a UV digester, equipped with a high-pressure mercury lamp. The temperature of the sample is maintained at 85±5 °C by a combined air/water cooling system. This procedure provides an efficient alternative to traditional dry ashing and wet digestion methods. Milk degrades in less than 2 h, while inorganic constituents, except for iodide, nitrate, nitrite, sulfite and manganese (II), are unaffected by UV radiation. Depending upon the type of milk (whole, skimmed, powdered, evaporated, etc.) to be analysed, the amount of sample and the UV photolysis time can be adjusted as per requirements. The clear solution resulting from the UV digestion is diluted, filtered and injected onto an ion chromatograph equipped with both conductivity and variable-wavelength UV-Vis detectors. The method has been tested with standards and real milk samples and has been found to be satisfactory for the determination of total chloride, bromide, phosphorus (as phosphate) and sulfur (as sulfate), and of copper, nickel, zinc, cobalt, iron and lead.     

Sensitive detection of beryllium using a fiber optic liquid waveguide cell

The metallochromic chelating agent, Chromazurol S, has been utilized in conjunction with a fiber optic liquid waveguide capillary cell to enable the sensitive detection of beryllium in solution (30 ng l⁻¹ detection limit) and following extraction from a contaminated plexiglas surface (0.5 ng cm⁻² detection limit). The addition of a cationic surfactant, cetylpyridinium chloride, to Chromazurol S at pH 10 in Tris-HCl buffer results in the formation of two bathochromic peaks in the visible spectrum following metal chelation by beryllium. The first absorbance band, at 515 nm, is intermediate in nature, permitting maximal sensitivity for low beryllium concentrations, but diminishing in intensity at concentrations above 100 μg l⁻¹. The second absorbance band, centered at 610 nm, dominates for beryllium concentrations of 100 μg l⁻¹ and above. Experimental conditions including pH, buffer type, additive surfactants, masking agents, and dye concentration were investigated in order to optimize detection sensitivity and selectivity. A fiber optic spectrometer is used with both a liquid waveguide capillary cell and 1 cm cuvette cell, to give a sensitive and broad dynamic range for beryllium detection that capitalizes on both beryllium metal chelate absorbance bands formed under these conditions.     

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.