Fluorimetric determination of aluminium in water by sequential injection through column extraction

A fluorimetric procedure for the determination of aluminium with matrix removal in drinking water is proposed. The system is based both on the solid phase extraction of aluminium on a new chelating resin (XAD-4 modified by grafting salicylic acid) and the fluorimetric detection of a complex formed between 8-hydroxyquinoline-5-sulfonic acid (HQS) and Al(III), after elution of the resin by hydrochloric acid. The sorption and elution of aluminium were studied in both competitive and non-competitive conditions, varying pH, flow-rates, volume and concentration of reagents, as well as time contact. The optimised procedure allows determination of Al³⁺ at the sub-ppb level (LOD: 0.2 g L^–1 for 1 ml of sample) within a working range of 0.2–500 g L^–1. The analytical procedure was successfully employed for the determination of aluminium in drinking water during and after flocculation/coagulation treatment processes.     

Neutron induced radiography in the determination of boron in drinking water

Neutron induced radiography has been applied to the determination of boron concentrations in drinking water, collected from natural springs of Reshian and Muzaffarabad areas of Azad Kashmir, Pakistan, using CR-39 etched track detectors. The technique is based upon the simultaneous irradiation with thermal neutrons of a sample of unknown concentration and a standard of known boron concentration, fixed on a track detector. The subsequent counting of alpha and ⁷Li tracks in the detector resulting from the ¹⁰B(n,)⁷Li nuclear reaction is done after chemical etching. Boron concentration in the sample is determined by comparing ⁷Li and alpha-particle track density with that of a standard of known boron concentration. Boron concentrations in drinking water samples from Muzaffarabad and Reshian area of Azad Kashmir have been found to vary from (0.054±0.001) mg/l to (0.250±0.004) mg/l with an average of (0.16±0.002) mg/l. The observed concentration of boron in drinking water has been found to be less than the provisional Maximum Acceptable Concentration level (0.4 mg//l) of WHO. The drinking water from the reported area has been found to be within safe limits as far as boron related health hazards are concerned.This revised version was published online in November 2005 with corrections to the Cover Date.     

饮用水中氯酸盐、亚氯酸盐的离子色谱测定方法

建立了饮用水中微量氯酸盐以及亚氯酸盐的离子色谱测定方法。结果表明,亚氯酸盐和氯酸盐在0～0.50 mg/L范围内线性良好,精密度高,亚氯酸盐r2=0.999 8,样品加标平均回收率91.5%～99.4%,相对标准偏差(RSD)0.64%～1.78%,检出限为3.98μg/L;氯酸盐r2=0.999 6,样品加标平均回收率94.7%～101.6%,相对标准偏差(RSD)0.94%～1.35%,检出限为4.65μg/L;方法操作简单、快速、准确、灵敏度高、干扰少,适用于饮水消毒副产物亚氯酸盐和氯酸盐的检测。     

Determination of low concentrations of chlorite and chlorate ions by using a flow-injection system

A flow-injection method is reported for the determination of chlorite ion and chlorite and chlorate ions in mixtures at the submilligram per liter level in drinking water. The chlorite ion concentration is selectively determined by using its reaction with iodide ion at pH 2, which liberates iodine. Both species react with iodide ion in6 M HCl to produce iodine, the concentration of which is measured spectrophotmetricaly at 370 nm. The individual species are determined using multiplel regression. The method exhibits a linear range from 2 to 150 μM (0.1–10.1 mg l^-1) for chlorite ion and from 2 to μM (0.1–8.3 mg l^-1 for chlorate ion, with relative standard deviations of 0.4 and 1.2%, respectively.     

Detection and quantification of PAH in drinking water by front-face fluorimetry on a solid sorbent and PLS analysis

The direct determination in drinking water of perylene, chrysene, pyrene, benzo[a]pyrene, and benzo[k]fluoranthene, by front-face synchronous fluorimetry on a commercial SPE disk, has been evaluated. Sorbent treatment, influence of humic substances, and pH effect are discussed. In pure water the detection limits were estimated to be in the range 0.03–0.01 g L^–1. A working pH in the range 10–11 was found to minimize the fluorescence quenching effect of humic substances. The proposed method combined with a partial-least-square (PLS) treatment was tested for quantitative analysis of mixtures of four PAH in a spiked drinking water.     

Online Flow-Injection Determination of Trace Zinc in Natural Waters

A procedure for the flow-injection determination of trace zinc in natural waters with sorption preconcentration is developed. The procedure provides the determination of zinc in the concentration range from 5 to 100 g/L with RSD no higher than 25%. A single determination of zinc in water at the lower limit of analytical range takes 15 min.     

Rapid Determination of Mercury in Water by Stripping Voltammetry at a Gold-Modified Carbon Electrode

A procedure was developed for determining mercury in natural water by stripping voltammetry on a gold-modified carbon electrode. The concentration dependence of the anodic stripping current of mercury is linear in the range 0.02–5 g/L Hg(II). The interference of Fe(III), Cu(II), Cl^–, Br^–, I^–, and F^– ions with the determination of mercury was studied. Ozonation was used for rapid sample preparation. The detection limit for mercury was 0.02 g/L at an electrolysis time of 5 min.     

Rapid radiochemical analysis of 131I in environmental samples using a well-type Ge-detector

Large-scale production of ¹³¹I in a nuclear reactor, the gaseous nature of ¹³¹I, and its selective uptake by the human thyroid gland, make this radioisotope a health hazard in the event of a nuclear accident. The maximum concentration of ¹³¹I in drinking water has been set at 1 pCi/l. Human ingestion of ¹³¹I through the grass-cow-milk pathway makes milk an environmentally significant matrix to be monitored for. In this paper, we report a simple and a rapid radiochemical procedure for the analysis of ¹³¹I in water and milk samples. A quick single-step separation on anion-exchange resin concentrates radioiodine from large sample volumes. The resin is then directly counted in the cavity of a low-background well-type HPGe detector that has high counting efficiency for X-rays and low-energy -radiation. Chemical recovery is evaluated from the intensity of the 29.6 keV X-rays of the ¹²⁹I spike, and ¹³¹I is assayed through the intensity of its 364.5 keV g-peak. The method's minimum detection limit is 0.5 pCi ¹³¹I based on a 1 liter sample and a 200-minute count.     

Spin–Spin Relaxation in the 17O NMR Spectra of Na+ and K+ Water Clusters

Relaxation characteristics of Na⁺ and K⁺ water clusters were studied by ¹⁷O NMR spectroscopy. The influence of viscosity and pH of solution was taken into account; for both electrolytes in the concentration range -4 M, spin–spin relaxation times are greater than those for pure water. For K⁺ clusters, maxima of the concentration dependence of ¹⁷O spin–spin relaxation time have been found.     

Determination of aluminium in chewing gum samples using electrothermal atomic-absorption spectrometry and slurry sample introduction

A slurry-based electrothermal atomic absorption spectrometric procedure for the rapid determination of aluminium in chewing gum samples is discussed. To achieve a sufficiently small particle size, the samples have been first submitted to a mild calcination stage. Suspensions have been then prepared from the ground carbonaceous residues in a medium containing 8% v/v ethanol, 1% v/v concentrated nitric acid, 0.2% m/v magnesium nitrate and 4% v/v concentrated hydrogen peroxide. Aliquots of 10 l have been introduced in the furnace and dried at 200° C for 20 s. No ashing step has been used. Wall atomization has been performed at 2600° C. Calibration has been carried out with aqueous standards. The reliability of the procedure has been checked by analyzing standard reference materials and by comparing the results for eight commercial samples with those found by a conventional procedure based on the complete dissolution of the samples. The results for the commercial samples are in the 36–64 g g^–1 range, only one of the samples giving a higher value of 123 g g^–1.     

3-Hydroxy-2-(2"-Thienyl)-4H-Chromon-4-one as a Spectrophotometric Reagent for the Trace Determination of Zirconium in an Aqueous Phase

A rapid, simple, selective, and sensitive method for the trace determination of zirconium has been developed based on the reaction of 3-hydroxy-2-(2"-thienyl)-4H-chromon-4-one in an hydrochloric acid medium to form a yellow–colored complex which is rendered water soluble by the micellar action of Triton X-100 and measured at 415 nm. Most of the metal ions do not interfere with the determination. Beer's law is obeyed in the concentration range 0–2.0 g/mL and the molar absorptivity of the complex is 2.73 × 10⁴L mol^–1cm^–1; Sandell's sensitivity is found to be 0.0034 g cm^–2. The method has been applied for the determination of zirconium in various samples, and satisfactory results have been obtained.     

Thorium in man and environment uptake and clearance

The intake and tissue distribution of thorium (^{2 3 2}Th) was studied in an urban (Bombay) population in India. From the analysis of 16 whole diet samples, the average daily intake through food was found to be 2 g (range 0.8–4.3 g·d^–1). The estimated intake through drinking water and inhalation comes out to be 0.03 and 0.02 g per day. From the analysis of human autopsy tissue samples it is observed that the concentration ranges in lungs and bone are 1.5–16 g/kg and 0.2–9.0 g/kg fresh weight respectively. The average urinary concentration is 12 ng/1 (range 7–22 ng/l for 10 samples). Among the different body tissues, pulmonary lymph nodes were found to contain the highest concentration (geometric mean 53.4 g/kg, range 31.4–85.5 g/kg for 6 samples). Analysis of the samples was done by the neutron activation technique. 311.8 keV gamma photons of^{2 3 3}Pa which is the activation product of^{2 3 2}Th, were counted after chemical separation. A 54 cm³ intrinsic Ge detector coupled to 1024-channel analyser was used. Using the average lung content and the daily average intake values of thorium through inhalation, the clearance half-time from lung was estimated.     

On-line sample preparation and determination of phenols with a Flow-Analysis method

Summary A Flow-Analysis system has been developed to automate the phenol determination according to the German standard method DIN 38409-H16-2. The automation leads to a significant acceleration of the procedure. One analysis only lasts 3 min while the complete manual determination requires 3 h. Also the sample, solvent and reagent volumes are reduced to a tenth of the volumes demanded by the standard method. The described phenol determination is based on the integration of an airsegmented (Airsegmented-Flow-Analysis SFA) part in a Flow-Injection-Analysis (FIA) system. The main steps of the analytical procedure are: Reproducible inserting of the sample in a carrierstream, sample pretreatment and sample measuring. In the first step the sample is injected into the carrierstream. It transports the sample in the reactioncoil and than through the distillation unit. The steam distillation represents the sample preparation step; therefore an airsegmented stream is necessary. Afterwards the different phases (liquid and gas) were singled again and the distilled solution is fed into the FIA manifold. The determination itself takes place inside the FIA system. The limit of determination amounts to 0.01 mg l^–1 with a standard deviation of 1.5%. Different waste, surface and drinking water samples have been analyzed without any problems. The results correspond very well to those obtained by manual procedure.     

Passive sampling for volatile organic compounds (VOCs) in air at environmentally relevant concentration levels

A sensitive and reliable method is described for the determination of aromatic and chlorinated hydrocarbons (benzene, toluene, o-, m-, p-xylene, trichloromethane, trichloroethane, trichloroethene and tetrachloroethene) in indoor and outdoor air at environmental concentration levels. The procedure can be easily extended to other VOCs. Using passive samplers the VOCs have been adsorbed onto charcoal during a four-week sampling period and subsequently desorbed with carbon disulfide. After injection with a cold split-splitless multi-injector the VOCs have been separated by capillary gas chromatography. Quantification has been achieved using an electron capture detector (ECD) and a flame ionization detector (FID) switched in series. A limit of about 1 g/m³ for aromatic hydrocarbons and of about 0.01 g/m³ for chlorinated hydrocarbons has been obtained. The procedure has been successfully applied in the framework of a field study to measure indoor and outdoor air concentrations in Essen and Borken, two differently polluted areas of Northrhine-Westphalia.     

3,3′,5,5′-Tetramethylbenzidme for the colorimetric determination of manganese in water

Manganese can be determined by colorimetry with previous oxidation of Mn(II) in a strong basic medium, using 3,3,5,5-tetramethylbenzidine as a chromogenic reagent. The molar absorptivity of the reaction product is 3.4 × 10⁴ mol^–1l cm^–1l, the detection limit 3 ng/ml, the RSD (0.5 mg/l,n = 8) 0.9% and the calibration range (1-cm cells) 0.02–0.8 mg/1 V(V), Cr(VI) and Co(II) are the most significant interferences. The new method was compared with an AAS procedure (air-acetylene flame) with previous solvent extraction and also with a colorimetric method for the determination of manganese in sea and drinking water.     

Determination of 222Rn in Iranian mineral waters using liquid scintillation alpha-spectrometry

Liquid scintillation counting (LSC) method has been used for the measurement of ²²²Rn in mineral water samples under a pilot project for the first surveillance in Iran. Low level background LSC counter Quantulus and pulse-shape analysis method have been employed. The concentration of ²²²Rn found in mineral waters of the studied areas ranges from about 1 to 75 Bq/l. The best lower limit of detection obtained with the applied technique was 0.069 Bq/l for a counting time in the range of 236–296 minutes.     

Spectrophotometric and atomic absorption determination of Ni(II) in fresh and sea waters after preconcentration by flotation

A highly selective and sensitive procedure for flotation separation followed by spectrophotometric determination, confirmed by AAS, of Ni(II) traces is proposed. The maximum flotation separation (100%) is achieved at 25° C in the pH range of 1–3 using sodium diethyldithiocarbamate (as a collector) and oleic acid surfactant. The floated (1 : 2) colored complex is measured spectrophotometrically at 430 nm over a concentration range of 0.5–4.0 g/g with a molar absorptivity of 0.44 × 10⁴ L mol^–1 cm^–1. The procedure was successfully applied for the separation and determination of Ni(II) in fresh and sea waters.     

Determination of Carotenoids in the Chinese Medical Herb Jiao-Gu-Lan (Gynostemma Pentaphyllum MAKINO) by Liquid Chromatography

A QSTAR Pulsar quadrupole time-of-flight mass spectrometer was used for the determination of chlorophenols in surface water samples. The investigated compounds were: 2-chlorophenol; 4-chloro-3-methylphenol; 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol. Each analyte is listed by the US-EPA as a priority pollutant. Sample enrichment of water samples was achieved by a solid-phase extraction procedure, using a Waters Oasis HLB cartridges followed by LC-Tandem-MS. A narrow-bore 2.1-mm-i.d. reversed phase LC C-18 column operating with a mobile phase flow rate of 0.2 mL min^–1. was used to separate the analytes. The whole column effluent was diverted to the ion spray interface source. For the determination of the analytes the hybrid quadrupole time-of-flight spectrometer operated in product ion scan acquisition mode. Average recoveries from 2 L samples varied from 91 to 110% and relative standard deviations (RSD) were less than 10% for all samples. The limit of detection (signal-to-noise ratio=3) of the method for the phenols in drinking water samples is less than 10 ng L^–1. In real environmental samples, levels of the selected analytes varied from non-detected up to 0.5 g L^–1 for pentachlorophenol.     

Liquid chromatography — Particle beam mass spectrometry for identification of unknown pollutants in water

Summary Trace enrichment on a precolumn packed with copolymer material, coupled on-line with reversed-phase, column liquid chromatography-particle beammass spectrometry (RPLC-PB-MS) has been used for both target and non-target analysis of water samples. RPLC is carried out on a C-18-bonded silica column using a linear acetonitrile-0.1 M ammonium acetate gradient. Using optimised PB-MS conditions and 100–250 ml water samples, the detection limits for several phenylureas are in the 0.03–0.05 g l^–1 range using the full-scan mode; repeatability is good and the LC-PB-MS system is robust. Several surface and drinking water samples have been analysed and low levels of various environmental contaminants have been identified using electron impact mass spectra. Applying chemical ionisation with methane as reagent gas in both the positive and negative mode in conjunction with PB-MS provides relevant confirmatory information.     

Making Analytical Chemistry Simpler by Rediscovering Cheap Analytical Reagents: Micro-Spectrophotometric Determination of Palladium in Catalysts Using the Food Additive Dye (Yellow-6)

Simple spectrophotometric and extracto-spectrophotometric micro-methods have been developed in order to assess quality control in palladium catalysts by means of a cheap soft drink additive dye (yellow-6, Y6). In the pH range of 3 to 9.5, Y6 forms a red colored complex with Pd(II) with a maximum at 553nm and a molar absorptivity of 1.14× 10⁴M^–1cm^–1 at pH 7.0. The ratio of the metal ion to the ligand and its stability constant were found to be 1:2 and 3.92×10¹¹, respectively. Extraction of the complex was carried out with the cationic surfactant Aliquat-336 by using methyl isobutyl ketone as organic solvent. The effect of pH, ionic strength, organic phase volume, Y6 and surfactant concentration on complex formation was studied, and the tolerance limits for many cations have been determined. Finally, the micro-methods were successfully applied to determine palladium content in commercial catalyst samples by using a commercial drinking soda containing Y6.