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1.
A flow injection on-line sorption preconcentration method for the electrothermal AAS determination of platinum has been developed. The pyrrolidine dithiocarbamate complexes of either Pt4+ or Pt2+, formed in 0.7 mol L–1 HNO3, are on-line adsorbed on the inner walls of a PTFE knotted reactor and subsequently eluted with methanol. An enhancement factor of 112 and a detection limit (3 σ) of 10 ng L–1 along with a sampling frequency of 21 h–1 are achieved with a 90 s preconcentration time at a sample flow rate of 8.8 mL min–1. The relative standard deviation is 2.5% for 0.4 μg L–1 Pt. The method has been applied to the determination of platinum in blood samples. Received: 6 October 1997 / Revised: 26 November 1997 / Accepted: 3 December 1997  相似文献   

2.
A flow-injection analysis (FIA) system incorporating a micro-column of ZrO2 has been used for the development of an on-line multi-element method for the simultaneous preconcentration and determination of Al, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Tl, V, Sb, Sn, and Zn by inductively coupled plasma atomic emission spectrometry (ICP–AES). The conditions for quantitative and reproducible preconcentration, elution, and subsequent on-line ICP–AES determination were established. A sample (pH 8) is pumped through the column at 3 mL min–1 and sequentially eluted directly into the ICP–AES with 3 mol L–1 HNO3. With a sample volume of 100 mL and an elution volume of 1 mL signal enhancement 100 times better than for conventional continuous aspirating systems was obtained for the elements studied. The reproducibility (RSD %) of the method at the 10 ng mL–1 level in the eluate is acceptable – less than 8% for five replicates. Recoveries between 95.4% and 99.9% were obtained for the elements analysed. ZrO2, with a specific surface area of 57 m2 g–1 and a capacity of approximately 5 mg g–1 for the elements studied, was synthesized by hydrolysis of ZrCl4. The preconcentration system was evaluated for several simple synthetic matrices, standard water samples and synthetic seawater. The effect of foreign ions on the efficiency of preconcentration of the elements studied was investigated. The application of a micro-column filled with high-surface-area ZrO2 and flow injection inductively coupled plasma atomic emission spectrometry enables preconcentration and simultaneous determination of 18 elements at low concentrations (ng L–1) in different water samples.  相似文献   

3.
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   

4.
An on-line column preconcentration method based on the combined use of ammonium O,O-diethyldithiophosphate and activated carbon or polyurethane foam as adsorbents has been developed for the determination of Pb in water samples. The complexed Pb was eluted with ethanol and determined by flame atomic absorption spectrometry. The optimum preconcentration conditions are given for each adsorbent. The enrichment factors were 63 and 294, and the detection limits (3σ) 3?μg?L–1 and 0.8?μg?L–1, respectively, for the carbon and foam systems. When the optimized procedures were applied to the determination of Pb in water samples the recovery efficiency was > 96%.  相似文献   

5.
In the present study, the ?5-(4-dimethylaminobenzylidene)rhodanin-modified SBA-15? was applied as stable solid sorbent for the separation and preconcentration of trace amounts of cobalt ions in aqueous solution. SBA-15 was modified by ?5-(4-dimethylaminobenzylidene)rhodanin reagent. The sorption of Co2+ ions was done onto modified sorbent in the pH range of 6.8–7.9 and desorption occurred in 5.0 mL of 3.0 mol L?1 HNO3. The results exhibit a linear dynamic range from 0.01 to 6.0 mg L?1 for cobalt. Intra-day (repeatability) and inter-day (reproducibility) for 10 replicated determination of 0.06 mg L?1 of cobalt was ±1.82% and ?±1.97%?. Detection limit was 4.2 µg L?1 (3Sb, n = 5) and preconcentration factor was 80. The effects of the experimental parameters, including the sample pH, flow rates of sample and eluent solution, eluent type and interference ions were studied for the preconcentration of Co2+. The proposed method was applied for the determination of cobalt in standard samples, water samples and agricultural products.  相似文献   

6.
A flow injection on-line preconcentration system was developed for the determination of lead by hydride generation atomic fluorescence spectrometry (HG-AFS). It is based on a simple micro-column filled with multiwalled carbon nanotubes (MWCNTs). The preconcentration of lead on the MWCNTs was carried out based on the adsorptive retention of analyte via on-line introducing the sample into the micro-column system. A 0.3 mol L?1 HNO3 was introduced to elute the retained analyte and merged with KBH4 solution for HG-AFS detection. Under the optimal experimental conditions, an enhancement factor of 26 was obtained with a sample consumption of 14.4 mL. The limit of detection was 2.8 ng L?1 and the precision (RSD) of 11 replicate measurements of 0.2?μg L?1 Pb was 4.4%. The method was validated by analyzing three certified reference materials, and was successfully applied to the determination of trace lead in natural water samples.  相似文献   

7.
A flow injection on-line coprecipitation preconcentration system with diethyldithiocarbamate (DDTC) chelate of copper used as the coprecipitate carrier was coupled with flame atomic absorption spectrometry (FAAS) for the determination of trace silver. Silver was on-line coprecipitated with DDTC-Cu(II) in 0.5 moL · L−1HCl, and the precipitate was collected in a knotted reactor. The precipitate was then dissolved by isobutyl methyl ketone and transported directly into the nebulizer–burner system of a flame atomic absorption spectrometer. A detection limit (3ς) of 0.6 μg · L−1was achieved for a loading period of 30 s, a relative standard derivation of 2.0% was obtained for 11 determinations of 20 μg · L−1Ag(I). Interference-free levels were 10 mg · L−1for Cd2+, 50 mg · L−1for Cu2+, 50 mg · L−1for Mn2+, 25 mg · L−1for Ni2+, 100 mg · L−1for Pb2+, 50 mg · L−1for Zn2+, 500 mg · L−1for Fe3+, and 2000 mg · L−1for Fe2+reduced from Fe3+by ascorbic acid. The developed method has been successfully applied to the determination of trace amount of silver in geological samples.  相似文献   

8.
A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L–1 levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min–1. The trapped complex was then eluted with 3.6 mol L–1 HCl at a flow rate of 4.9 mL min–1. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L–1 HCl stabilized with 1 % triton X-100, 4.9 mL min–1) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h–1, the enhancement factor was 97, the detection limit was 0.25 μg L–1, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L–1), whereas for 300 s of the preconcentration time and a sample frequency of 10 h–1, the enhancement factor of 357, the detection limit (3σ) of 0.069 μg L–1 and the precision of 1.32 % (at 10 μg L–1) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.  相似文献   

9.
A sensitive and rapid on-line method has been developed for the determination of trace amounts rare earth elements (REEs), lanthanum, cerium, neodymium and yttrium, by microwave plasma torch-atomic emission spectrometry (MPT-AES) combined with micro-column separation/preconcentration. A strong basic cinnamene anion exchange resin is used for matrix elimination and enrichment of the analytes. The adsorbed metal ions are subsequently eluted from the column and transferred into the detector with nitric acid solution for simultaneous multi-element determination. Various factors influencing the separation/preconcentration, sample flow rate, loading time, acidity and eluent flow rate, concentration, have been studied in detail. Under the optimized conditions, the detection limits for lanthanum, cerium, neodymium and yttrium based on three times of standard deviations of blank by 7 replicates are 0.89, 2.02, 1.56 and 0.78 μg·L 1, and the relative standard deviations are determined as 1.54, 4.29, 4.95 and 3.90%, respectively. The proposed method has been applied to the analysis of the four REEs in high purity Sm2O3, Eu2O3, Gd2O3, Tb2O3, Dy2O3, Yb2O3, and Lu2O3 samples with a recovery range of 95.1-104.8%.  相似文献   

10.
Polychlorotrifluoroethylene (PCTFE) in the form of beads was applied, as packing material for flow injection on-line column preconcentration and separation systems coupled with flame atomic absorption spectrometry (FAAS). Its performance characteristics were evaluated for trace copper determination in environmental samples. The on-line formed complex of metal with diethyldithiophosphate (DDPA) was sorbed on the PCTFE surface. Isobutyl methyl ketone (IBMK) at a flow rate of 2.8 mL min−1 was used to elute the analyte complex directly into the nebulizer-burner system of spectrophotometer. The proposed sorbent material reveal, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates up to 15 mL min−1 without loss of retention efficiency. For copper determination, with 90 s preconcentration time the sample frequency was 30 h−1, the enhancement factor was 250, which could be further improved by increasing the loading (preconcentration) time. The detection limit (3s) was cL = 0.07 μg L−1, and the precision (R.S.D.) was 1.8%, at the 2.0 μg L−1 Cu(II) level. For lead determination, the detection limit was cL = 2.7 μg L−1, and the precision (R.S.D.) 2.2%, at the 40.0 μg L−1 Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials and by recovery measurements on spiked natural water samples.  相似文献   

11.
A new method has been developed for the determination of trace rare earth elements (REEs) in water samples based on preconcentration with a microcolumn packed with multiwalled carbon nanotubes (MWNTs) prior to their determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimum experimental parameters for preconcentration of REEs, such as pH of the sample, sample flow rate and volume, elution solution and interfering ions, have been investigated. The studied REEs ions can be quantitatively retained by MWNTs when the pH exceed 3.0, and then eluted completely with 1.0 mol L−1 HNO3. The detection limits of this method for REEs was between 3 and 57 ng L−1, and the relative standard deviations (RSDs) for the determination of REEs at 10 ng mL−1 level were found to be less than 6% when processing 100 mL sample solution. The method was validated using a certified reference material, and has been successfully applied for the determination of trace rare earth elements in lake water and synthetic seawater with satisfactory results.  相似文献   

12.
The efficiencies and performances of silver nanoparticle loaded activated carbon modified with 2-(4-isopropylbenzylideneamino)thiophenol (IPBATP-Ag-NP-AC) and activated carbon modified with IPBATP (IPBATP-AC), as new sorbents, were evaluated for separation and preconcentration of Cu2+, Zn2+, Co2+, Cd2+ and Pb2+ ions from real environmental samples. The retained metals content was reversibly eluted using 5?mL of CH3COOH (6.0?mol?L?1) and/or 10?mL of 4.0?mol?L?1 HNO3 for IPBATP-Ag-NP-AC and IPBATP-AC, respectively. The experimental parameters influence the recoveries of metal ions including pH, amounts of ligand and supports, condition of eluents, sample and eluent flow rates of has been investigated. The preconcentration factors were found to be 100 for Zn2+, Cd2+, Co2+, Cu2+ and 50 for Pb2+ ions using IPBATP-Ag-NP-AC, and 50 for Zn2+, Cd2+, Co2+, Cu2+ and 25 for Pb2+ ions using IPBATP-AC. The detection limit of both SPE-based sorbents was between 1.6–2.5?ng?mL?1 for IPBATP-AC and 1.3–2.5?ng?mL?1 for IPBATP-Ag-NP-AC. The proposed methods have been successfully applied for the extraction and determination of the understudy metal ions content in some real samples with extraction efficiencies higher than 90% and relative standard deviations (RSD) lower than 2.4%.  相似文献   

13.
An on-line preconcentration procedure for the determination of bismuth by flame atomic absorption spectrometry (FAAS) has been described. Lewatit TP-207 chelating resin, including iminodiacetate group, packed in a minicolumn was used as adsorbent material. Bi(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L−1 HNO3 and then introduced directly to the nebulizer-burner system of FAAS. Best preconcentration conditions were established by testing different resin quantities, acidity of sample, types of eluent, sample and eluent solution volumes, adsorption and elution flow rates, and effect of interfering ions. The detection limit of the method was 2.75 μg L−1 while the relative standard deviation was 3.0% for 0.4 μg mL−1 Bi(III) concentration. The developed method has been applied successfully to the determination of bismuth in pharmaceutical cream, standard reference materials and various natural water samples with satisfactory results.  相似文献   

14.
A flow injection analysis system incorporating a microcolumn of nanometer-sized TiO2 loaded with 1-(2-pyridylazo)-2-naphthol (PAN) has been used for the development of an on-line multi-element method for simultaneous separation and preconcentration and subsequent determination of Cu2+, Co2+, Cr3+, Y3+, Yb3+ and Bi3+ by ICP-AES. Effects of pH, sample flow rate and volume, elution conditions, adsorption capacity and interfering ions on analyte recovery were examined. The adsorption capacity of nanometer-sized TiO2 loaded with PAN was 4.73, 18.57, 3.81, 6.14, 4.52 and 20.35mgg–1 for Cu2+, Cr3+, Y3+, Yb3+, Co2+ and Bi3+, respectively. The method has been applied to the analysis of trace elements in standard reference biological samples, and the results are in good agreement with the certified values.  相似文献   

15.
A novel ion imprinted polyvinylimidazole-silica hybrid copolymer (IIHC) was synthesized and used as a selective solid sorbent for Pb2+ ions preconcentration using an on-line solid phase extraction (SPE) system coupled to TS-FF-AAS. The ionic hybrid sorbent was prepared using 1-vinylimidazole and 3-(trimethoxysilyl)propylmethacrylate as monomers, Pb2+ ions as template, tetraethoxysilane as reticulating agent and 2,2′-azobis-isobutyronitrile as initiator. The best on-line SPE conditions concerning sorption behavior, including sample pH (6.46), buffer concentration (9.0 mmol L−1), eluent (HNO3) concentration (0.5 mol L−1) and preconcentration flow rate (4.0 mL min−1), were optimized by means of full factorial design and Doehlert matrix. The analytical curve ranged from 2.5 to 65.0 μg L−1 (r = 0.999) with limit of detection of 0.75 μg L−1; the precision (repeatability) calculated as relative standard deviation (n = 10) was 5.0 and 3.6% for Pb2+ concentration of 10.0 and 60.0 μg L−1, respectively. From on-line breakthrough curve, column capacity was 3.5 mg g−1. Preconcentration factor (PF), consumptive index (CI) and concentration efficiency (CE) were 128.0, 0.16 mL and 25.6 min−1, respectively. The selective performance of the sorbent, based on relative selectivity coefficient, was compared to NIC (non imprinted copolymer) for the binary mixture Pb2+/Cd2+, Pb2+/Cu2+ and Pb2+/Zn2+. The results showed that ion imprinted polyvinylimidazole-silica hybrid polymer had higher selectivity for Pb2+ than NIC at 64.9, 16.0 and 8.8 folds. The developed method was successfully applied for highly sensitive and selective Pb2+ determination in different kinds of water samples, parenteral solutions and urine. Accuracy was also assessed by analyzing certified reference fish protein (DORM-3) and marine sediment (MESS-3 and PACS-2) with satisfactory results.  相似文献   

16.
In this study a method for the determination of low concentrations of silver in waters using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed. Moringa oleifera seeds were used as a biosorbent material. Chemical and flow variables of the on-line preconcentration system such as sample pH and flow rate, preconcentration time, eluent concentration and sorbent mass were studied. The optimum preconcentration conditions were obtained using sample pH in the range of 6.0-8.0, preconcentration time of 4 min at a flow rate of 3.5 mL min− 1, 0.5 mol L− 1 HNO3 eluent at a flow rate of 4.5 mL min− 1 and 35 mg of sorbent mass. With the optimized conditions, the preconcentration factor, precision, detection limit and sample throughput were estimated as 35 (for preconcentration of 14 mL sample), 3.8% (5.0 μg L− 1, n = 7), 0.22 μg L− 1 and 12 samples per hour, respectively. The developed method was successfully applied to mineral water and tap water, and accuracy was assessed through analysis of a certified reference material for water (APS-1071 NIST) and recovery tests, with recovery ranging from 94 to 101%.  相似文献   

17.
A sol-gel thiocyanatopropyl-functionalized silica sorbent was synthesized and employed for an automated on-line microcolumn preconcentration platform as a front-end to inductively coupled plasma atomic emission spectroscopy (ICP-AES) for the simultaneous determination of Cd(II), Pb(II), Cu(II), Cr(III), Co(II), Ni(II), Zn(II), Mn(II), Hg(II), and V(II). The developed system is based on an easy-to-repack microcolumn construction integrated into a flow injection manifold coupled directly to ICP-AES’s nebulizer. After on-line extraction/preconcentration of the target analyte onto the surface of the sorbent, successive elution with 1.0 mol L−1 HNO3 was performed. All main chemical and hydrodynamic factors affecting the effectiveness of the system were thoroughly investigated and optimized. Under optimized experimental conditions, for 60 s preconcentration time, the enhancement factor achieved for the target analytes was between 31 to 53. The limits of detection varied in the range of 0.05 to 0.24 μg L−1, while the limits of quantification ranged from 0.17 to 0.79 μg L−1. The precision of the method was expressed in terms of relative standard deviation (RSD%) and was less than 7.9%. Furthermore, good method accuracy was observed by analyzing three certified reference materials. The proposed method was also successfully employed for the analysis of environmental water samples.  相似文献   

18.
An on-line flow injection preconcentration-ETAAS method is developed for trace determination of cobalt in biological materials and natural samples by ion-pair sorption on the inner walls of a PTFE knotted reactor. The ion-pair is formed between the negatively charged cobalt-nitroso-R-salt complex and the tetrabutylammonium counter-ion. An enhancement factor of 15, a sampling frequency of 17 and a concentration efficiency of 4 are obtained for a preconcentration time of 60 s and a sample loading flow rate of 5 mL min–1. The detection limit (3σ) is 5 ng L–1. The relative standard deviation at the 0.2 μg L–1 level is 2.3%. The analytical results obtained for standard reference materials are in good agreement with the certified or indicated values and satisfactory recoveries of spiked cobalt in tap water are obtained.  相似文献   

19.
In the present paper novel column solid phase extraction procedure was developed for the determination of Cd(II) and Pb(II) in cows', goats', ewes', buffalos' and humans' milk samples using newly synthesized reagent 2,2′‐DPED3P (2,2′‐{[1,2‐diphenylethane‐1,2‐diylidene]dinitrilo}diphenol) for preconcentration and separation prior to differential pulse polarography using amberlite XAD‐2 in the ranges of pH 4.0–5.0. The sorbed elements were subsequently eluted with 10 mL of 2 M HCl elutes were analysed by differential pulse polarography (DPP). The interference of foreign ions has also been studied. Effects of various instrumental parameters are investigated and received conditions are optimized. The total metal concentration of the milk samples in the study area were in the following ranges 0.030–0.090 μg L?1 of Cd(II), 0.009–0.026 μg L?1 of Pb(II) respectively. The limits of detections were found to be 0.020 and 0.024 μg L?1 for Cd(II) and Pb(II) respectively by applying a preconcentration factor ~40. The proposed enrichment method was applied successfully for the determination of metal ions in cows', goats', ewes', buffalos' and humans' milk samples.  相似文献   

20.
In this work a solid phase on-line uranium ion preconcentration system coupled with spectrophotometry has been developed. The method is based on uranyl ion preconcentration at pH 3.75 onto multiwall carbon nanotubes treated with HNO3. After preconcentration, the uranyl ions are eluted with 0.32?mol?L?1HCl followed by reaction with 3,6-bis[(2-arsonophenyl)-azo]-4,5-dihydroxy-2,7-naphthalendisulfonic acid 0.08%[w/v] (Arsenazo III), which had maximum monitored absorbance of 650?nm. Effects of the pertinent experimental parameters on the system were investigated by means of 26?2 fractional factorial design, while optimization was carried out using the Doehlert matrix. Under optimized conditions, detection and quantification limits were found to be 0.21 and 0.7?µg?L?1, respectively. The analytical curve ranged from 5 to 150?µg?L?1 (r?=?0.998), while the relative standard deviations (RSD) were 3.27 and 2.56% for the respective uranium concentrations of 10 and 100?µg?L?1 (n?=?10). The features obtained for the on-line preconcentration system were: preconcentration factor of 228, concentration efficiency of 57?min?1, consumption index of 0.13?mL and sample throughput of 15?h?1. In order to assess the accuracy of the proposed method, addition and recovery studies were carried out on spring water samples from different sources and synthetic seawater with satisfactory results ranging from 94.85 up to 103.65%.  相似文献   

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