A flow injection analysis method for iodate and iodide in sea water is described. The system involves spectrophotometric detection based on the catalytic, fading effect of either iodate or iodide on the indicator reaction of iron (III) thiocyanate and nitrite. With and without an anion-exchange column in the flow conduit, the system allows the determination of iodate and total iodine, respectively; iodide can be found by difference. Both iodate-iodine and total iodine can be determined in the range 0.75 to 150 g/1 on the sea water basis with analysis times of 20 min for iodate-iodine and 9 min for total iodine. The RSDs are within 1.3% for both iodate and iodide. Results are presented for the determination of iodate and iodide in sea waters and some brines associated with natural methane gas evolution. 相似文献
An automated analysis system is described for the measurement of hydrogen peroxide based on a chemiluminescence reaction with phenyl 10-methylacridinium-9-carboxylate (PMAC). A reversed FIA experimental arrangement is used to establish the operating conditions for the measurement of submicromolar levels of hydrogen peroxide. The carrier stream consists of hydrogen peroxide standards prepared in a pH 9.0, boric acid buffer and the flow rate for this carrier/sample stream is 4 ml/min. Twenty microliters of a 10 mM PMAC solution, prepared in a pH 3 phosphate buffer, are injected into the carrier/sample stream. Hydrogen peroxide mixes with the PMAC reagent in an incubation coil that is constructed by wrapping 107 cm of polyethylene tubing around a 1 cm o.d. plastic rod. The chemiluminescence reaction is then initiated by adding base just before the sample passes in front of a photomultiplier tube (PMT) detector. The calculated limit of detection (S/N = 3) for hydrogen peroxide is 0.25 M. In addition, the pH dependent hydrolysis of the PMAC reagent is characterized by an HPLC method which has been specifically developed for the separation and detection of the hydrolysis products of PMAC. Results indicate that a pH of 3.0 is required for long term stability of the PMAC reagent. Finally, this system has been successfully extended to the measurement of glutamate by coupling a bioreactor column of glutamate oxidase with the hydrogen peroxide detection scheme. A detection limit (S/N = 3) of 0.5 M has been established for glutamate with a throughput of 200 samples per hour. 相似文献
The development and improvement of a gas chromatography inductively coupled plasma mass spectrometry system, GC-ICP-MS, is described. The GC and ICP-MS are coupled with a heated stainless steel transfer line. Xe, present in the GC carrier gas, is used to facilitate the nebuliser gas flow rate setting and the positioning of the torch. Alkyltin compounds are separated by GC using a 30 m capillary column within 9 min. The necessity of applying double internal standardisation (use of Bu3PeSn and Xe gas as internal standards) is shown. The repeatabilities at 50 g/l concentration for both retention time and peak are better than 0.25% and 5%, respectively. The detection limits for alkyltin compounds are better than those of existing methods and range between 15 and 35 fg Sn. Finally, GC-ICP-MS is applied to the determination of mono-, di- and tributyltin in some harbour waters, after extraction and Grignard derivation with PrMgCl. Concentrations between 1 and 20 ng/l are found. 相似文献
A flow injection system incorporating an alumina microcolumn has been coupled to inductively coupled plasma mass spectrometry (ICP-MS) for on-line preconcentration and determination of platinum (IV) in natural waters. Depending on the nature of the sample, a nominal preconcentration factor of up to 600 can be achieved by eluting with 50l of 2 mol/l NH4OH. The limit of detection after a 5 min preconcentration time was 4 ngl-1, with a relative standard deviation of 4% (100 ngl-1 working solution). The proposed method was assessed for the determination of platinum (IV) in natural waters, motor car exhaust and some common analytical reagents. 相似文献
A procedure based on differential pulse cathodic stripping voltammetry on the graphite electrode is described for the determination of dissolved manganese in natural waters buffered at pH about 6.5 with acetate solution. In order to avoid interference of iron(II) the addition of fluoride is used. The limit of detection is 3 g/l for a deposition time of 6 min. Acidification and UV-irradiation are recommended for samples containing dissolved organic matter. Results of manganese determination in table mineral waters are reported and the possibility of manganese speciation is discussed. 相似文献
Summary An HPLC procedure is described for the determination of caffeine in pharmaceutical preparations. A Spherisorb octadecylsilane ODS-2 C18 analytical column and spectrophotometric detection at 273 nm were used. The chromatographic behaviour of caffeine with different micellar eluents containing sodium dodecyl sulphate (SDS) is described. The determination of caffeine in pharmaceutical preparations was performed by use of a mobile phase containing 0.05 M sodium dodecylsulphate (SDS) and 1.5% propanol at pH7. At a 6.0 g mL–1 concentration level the peak area and peak height repeatability were 2.6 and 2.4%, respectively. The application of the proposed method to the analysis of five pharmaceutical formulations, using peak heights as the dependent variable, gave recoveries between 85 and 104% of the values declared by the manufacturers. The proposed procedure for the determination of caffeine is rapid (15 min per sample), reliable and free from interferences. 相似文献
Summary The application of a sensitive electroanalytical technique for the analysis of N-methyl-N-nitro-N-nitrosoguanidine (MNNG) in aerosol was investigated. Cyclic voltammetric studies of the reduction of MNNG in acidic media showed three reduction waves. The first reduction step was assigned to be the reduction of the nitroso group and the second and third steps the reduction of the nitro group. The second peak was selected for the analysis as it was found to give a constant high current at pH below 1 and it was stable up to 40 days under normal daylight exposure and bubbling air at slow flow rate. Optimised parameters for the sensitive differential pulse polarographic technique were determined and the sampling conditions were investigated. The standard addition method was used to reduce the marix interference and the peak current was measured by the difference of current before and after UV irradiation so as to eliminate the interference caused by trace metals and electroactive and UV stable organic compounds present in air. The developed method was used to analyse MNNG aerosol in an animal room. The detection limit was found to be about 3 g/m3 for a sampling period of 48 h with a flow rate of 100 ml/min for the scrubbing method, whereas for the membrane filter method it was about 0.1 g/m3 for a sampling period of 8h at a flow rate of 4.9 l/min.
Bestimmung von N-Methyl-N-nitro-N-nitrosoguanidin in Aerosol mit Hilf der Differentialpuls-Polarographie
A kinetic method was developed for the determination of iodide ions. The method is based on the catalytic effect of iodide ions on the oxidation reaction of o-phenylenediamine with Chloramine B in an acidic solution and has a detection limit of 1 × 10–4 g/mL. It was demonstrated that the method could be used for the determination of iodides in natural waters. 相似文献
This work describes the characterization of a solid-phase extraction (SPE) and liquid-chromatography-tandem mass spectrometry-based method for the analysis of acrylamide (AA) in complex environmental waters. The method involved the SPE of AA using activated carbon, and the AA was detected with tandem mass spectrometry after separating on an ion exclusion high-performance liquid chromatography column. The method incorporated two labeled AA standards for quantification using isotope dilution and to assess absolute extraction recovery. The method was evaluated for inter- and intra-day precision and accuracy. The method was both accurate (i.e., <30 % error) and precise (i.e., <20 % relative standard deviation), with absolute extraction recoveries averaging 37 %. The mass spectrometry provided excellent sensitivity, with instrumental limits of detection and quantitation values of 23 and 75 pg, respectively. The method detection limit was determined to be 0.021 μg/L. The analysis of AA was successfully performed in real-world samples that contained total dissolved solids concentrations ranging from 23,600 to 297,000 mg/L and AA concentrations ranging from 0.082 to 1.0 μg/L.
Figure
Product ion spectra of, from top to bottom, acrylamide, acrylamide-1-13C, and acrylamide-2,3,3-d3. The predominant peak in each spectrum was used for quantitation 相似文献
A simple, sensitive and accurate reversed-phase high-performance liquid chromatographic (HPLC) method for simultaneous determination of three naturally occurring estrogenic steroids including estrone (E1), 17β-estradiol (E2) and estriol (E3) in environmental water samples was developed. Analytes were extracted with ethyl acetate solvents and preconcentrated prior to HPLC analysis. Separations were accomplished in <20 min using a reversed-phase C(18) column (4.6×250 mm id, 5 μm) with a gradient elution of mobile phase containing 3.0 mM ammonium acetate/acetonitrile mixtures (flow rate, 1.0 mL/min). UV light absorption responses at 205 nm were linear over a wide concentration range from 100,000 μg/L to the detection limits of 0.96 μg/L E1, 0.64 μg/L E2 and 0.78 μg/L E3. Quantitation was carried out by the peak area method. The relative standard deviation for the analysis of three estrogens was <3.0%. This method was applied for the simultaneous determination of estrogens in environmental water samples collected in Zhejiang, China. The higher concentrations of both E2 and E3 were found in Tang River and West Lake waters, and E1 was detected in lake water only. All three estrogens were below the detection limits in rain waters. 相似文献
Summary For monitoring the ammonium content in environmental waters an optical sensor was developed. The sensor is based on a glass rod coated with a caoutchouc layer in which bromophenolblue was immobilized as indicator. A detection limit of 3 mol/l ammonium is obtained. 相似文献
Summary The polarographic behaviour of 10-bromo-11 b-(2-fluorophenyl)-2,3,7,11 b-tetrahydrooxazolo [3,2-d][1,4] benzodiazepin-6(5H)-one (Haloxazolam) was studied in the pH range 1–13. Haloxazolam suffers a hydrolysis process, which can be followed by polarography. The reduction processes of Haloxazolam and its hydrolysis products are irreversible and their currents are diffusion-controlled. This behaviour was compared with that observed for other members of benzodiazepinooxazoles. Two polarographic methods have been developed upon the basis of the reduction of both the protonated iminium form (0.05 mol/l HCl, measurement time: 5 min) and the benzophenone produced in the hydrolysis process (pH 13.25, measurement time: 17 min). The relationship between reduction peak current and concentration is linear up to at least 6.62×10–5 mol/l for both methods. A higher sensitivity was obtained for the method based on the benzophenone reduction (detection limit 1.06×10–7 mol/l; 40 g/l). The reproducibility of the both methods in terms of relative standard deviation was inferior to 2%. 相似文献
A rapid chemiluminescence method for the determination of iodate has been developed, based on the reaction with an excess of iodide in acidic solutions, gas extraction of the iodine formed and detection in the stream of carrier gas by alkaline luminol solution. The limit of detection for IO–3 is 0.7 g/l. The time required for analysis is 2 min. 相似文献
Summary Chromium(VI) is one of the major pollutants of waters and unfortunately, at the present time, it cannot be determined with a simple and fast method. The use of the ultraviolet multiwavelength absorptiometry (UVMA) for chromium determination is very convenient for that purpose because of the well known absorption properties of chromium. Two methods are proposed which lead to different sensitivity. The first one needs hydroxide sodium addition for the measurement of the chromate form and has a detection limit of 4 g/l. The second does not use any reagent and determines directly both dichromate and chromate forms, whose sum gives the concentration of chromium(VI). This last procedure is faster but the characteristics are slightly less precise. These proposed methods have been compared with a reference method, for natural waters and treated wastewaters, with good agreement. These procedures can be used for water quality monitoring. 相似文献
A Spectrofluorimetric method for the determination of traces of bromide has been developed. The method is based on the bromination of fluorescein after bromide and hypochlorite form bromine, giving the less fluorescent eosin. The fluorescence decrease is used as the analytical signal. The calibration graph is linear over the range 10 to 80 g/1. The detection limit is 3 g/1 and the relative standard deviation 1.0%. The method has been satisfactorily applied to the determination of bromide in natural waters. 相似文献
Summary The derivatizing procedure of Moody et al. [20] for valproic acid has been simplified and applied to the simultaneous HPLC determination of valproic acid (VPA), barbital (B), primidone (PRM), phenobarbital (PB) and carbamazepine (CBZ) in serum or plasma of epileptic patients. The sample is deproteinized with acetonitrile containing esterification agents and an aliquot of the supernatant is heated to 70°C for 15 min with 4-bromophenacyl bromide. The reaction mixture is analysed on a C18 column at ambient temperature, with gradient elution and with detection at 205 nm. The time required for the chromatographic analysis is 13 min; identification is based on retention time and quantification is by peak area determination with an internal standard. The calibration curves show good linearity in the range 6.25 to 100 mg/L. The detection limits at a signal: noise ratio 3, ranged from 1 mg/L for B and CBZ to 2–3 mg/L for PRM, PB and VPA. The method described for the simultaneous determination of the five drugs in the same plasma pool, correlated well with isocratic HPLC methods specific for each drug. The simultaneous procedure described allows a reproducible (CVs6.5% within run) and rapid (25 min for sample preparation: 13 min for chromatographic run) therapeutic monitoring of patients treated with VPA and two or more antiepileptic drugs. 相似文献
A simplified method for the determination of chlorothalonil (I) and its metabolite 4-hydroxy-2,5,6-trichloroisophthalonitrile (II) in mustard crop is described. It involves extraction, derivatisation, clean-up on a silica-gel column and gas-liquid chromatography. The retention times and detection limits are 4.49, 5.39 min and 0.01, 0.005 g/g for I and II, respectively. 相似文献
Summary A simple method for the determination of barium in natural waters by flameless atomic absorption spectrometry using the carbon rod is proposed. Barium in highly salted waters is previously separated from the interfering ions by ion-exchange chromatography, using Dowex 50 W-X8 resin, and eluted with 0.1M EDTA solution. Mineral waters with low salinity are transferred directly to the furnace and the standard addition method is performed. The detection limit is 90 pg Ba for 10l injections. The method was applied to samples from the Atlantic Ocean and from Araruama Lake. Barium in commercially available waters was also determined.
Bestimmung von Barium in natürlichen Wässern durch flammenlose Atomabsorptionsbestimmung unter Verwendung des Standard-Zugabe- Verfahrens
Zusammenfassung In salzreichen Wässern enthaltenes Barium wird von störenden Ionen durch Ionen-Austausch-Chromatographie über Dowex 50 W-X8 getrennt und mit 0,1M EDTA ausgewaschen. Mineralwässer mit geringem Salzge- halt werden unmittelbar in den Ofen eingebracht und die Standard-Zugabe- Methode angewendet. Die Nachweisgrenze liegt bei 90pg/10l. Die Methode wurde zur Untersuchung von Proben aus dem Atlantischen Ozean sowie aus dem Araruama-See angewendet. Außerdem wurde Barium in handelsüblichen Trinkwässern bestimmt.
A single-wall carbon nanotubes (SWNT) film coated glassy carbon electrode (GCE) was fabricated for the direct determination of 4-nitrophenol (4-NP). The electrochemical behaviors of 4-NP at the SWNT-film coated GCE were examined. In 0.1M phosphate buffer with a pH of 5.0, 4-NP yields a very sensitive and well-defined reduction peak at the SWNT-modified GCE. It is found that the SWNT film exhibits obvious electrocatalytic activity towards the reduction of 4-NP since it not only increases the reduction peak current but also lowers the reduction overpotential. Based on this, an electrochemical method was proposed for the direct determination of 4-NP. The reduction peak current varies linearly with the concentration of 4-NP ranging from 1×10–8 to 5×10–6M, and the detection limit is 2.5×10–9M after 3min of open-circuit accumulation. The relative standard deviation at 2×10–7M 4-NP was about 6% (n=10), suggesting excellent reproducibility. This new method was successfully employed to determine 4-NP in several lake water samples. 相似文献
Polycyclic aromatic hydrocarbons (PAHs) are USEPA regulated priority pollutants. Their low aqueous solubility requires very sensitive analytical methods for their detection, typically involving preconcentration steps. Presented is the first demonstrated ‘proof of concept’ use of condensed phase membrane introduction mass spectrometry (CP-MIMS) coupled with direct liquid electron ionization (DEI) for the direct, on-line measurement of PAHs in aqueous samples. DEI is very well suited for the ionization of PAHs and other nonpolar compounds, and is not significantly influenced by the co-elution of matrix components. Linear calibration data for low ppb levels of aqueous naphthalene, anthracene, and pyrene is demonstrated, with measured detection limits of 4 ppb. Analytical response times (t10%–90% signal rise) ranged from 2.8 min for naphthalene to 4.7 min for pyrene. Both intra- and interday reproducibility has been assessed (<3% and 5% RSD, respectively). Direct measurements of ppb level PAHs spiked in a variety of real, complex environmental sample matrices is examined, including natural waters, sea waters, and a hydrocarbon extraction production waste water sample. For these spiked, complex samples, direct PAH measurement by CP-MIMS-DEI yielded minimal signal suppression from sample matrix effects (81%–104%). We demonstrate the use of this analytical approach to directly monitor real-time changes in aqueous PAH concentrations with potential applications for continuous on-line monitoring strategies and binding/adsorption studies in heterogeneous samples.
