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1.
A simple flow injection on line separation and preconcentration system coupled to hydride generation atomic fluorescence spectrometry
(HG-AFS) was developed for ultra-trace cadmium determination in seawater. With the sample pH kept at 3.0, the preconcentration
of cadmium on the inner walls of the knotted reactor was carried out based on the retention of cadmium complex with 1-phenyl-3-methyl-4-benzoylpyrazol-5-one.
A 0.2 mol L−1 HCl was introduced to elute the retained analyte complex and merge with KBH4 solution for HG-AFS detection. Under the optimal experimental conditions, an enhancement factor of 12 was obtained with a
sample consumption of 12.0 mL. The limit of detection was 3.2 ng L−1 with a sample frequency of 24 h−1. The developed method was validated by the analysis of cadmium in certified reference materials, and was applied to the determination
of cadmium in four seawater samples with R.S.D. of around 10%.
Correspondence: Hong Wu, Department of Chemistry, Xuzhou Normal University, Xuzhou 221116, P.R. China 相似文献
2.
Erdal Kendüzler Özcan Yalçınkaya Sıtkı Baytak Ali Rehber Türker 《Mikrochimica acta》2008,160(4):389-395
The preconcentration of chromium(III) by solid phase extraction and its determination from aqueous solutions by flame atomic
absorption spectrometry (FAAS) is investigated by applying an experimental design. The optimization of the preconcentration
variables such as pH of the sample solution, flow rate of the sample solution and concentration of elution solution was carried
out using 23 full factorial design. The most important parameter affecting the preconcentration of chromium is the concentration of eluent.
In the established experimental conditions, chromium can be determined with a relative standard deviation of 2.0% (N = 7) for a chromium concentration of 100 μg L−1. The detection limit for chromium was 1 μg L−1 (N = 20). The adsorption capacity of Amberlyst 36 is found to be 90.9 mg g−1 for chromium. Effect of other ions on the procedure was also evaluated. The method was validated by the analysis of certified
reference materials (tea leaves GBW 07605 and fish tissue IAEA-407). The method was applied to the determination of chromium
in waste water, dam water, carrot, parsley and lettuce.
Correspondence: Ali Rehber Türker, Department of Chemistry, Faculty of Science and Arts, Gazi University, TR-06500 Ankara,
Turkey 相似文献
3.
Design of a field flow system for the on-line spectrophotometric determination of phosphate, nitrite and nitrate in natural water and wastewater 总被引:1,自引:0,他引:1
Ioannis A. Tsoulfanidis George Z. Tsogas Dimosthenis L. Giokas Athanasios G. Vlessidis 《Mikrochimica acta》2008,160(4):461-469
This study describes the design and optimisation of a field flow system for the in-situ collection and on-line determination
of phosphate, nitrate and nitrite by flow injection analysis-spectrophotometry. The method is based on the initial determination
of phosphate as its phosphoantimonylmolybdenum blue complex which is then oxidized on-line by nitrite and the decrease in
absorbance is monitored at 880 nm. Nitrate is determined as the difference between total and initial nitrite content in a
separate flow after reduction to nitrite in a cadmium reductive column. The calibration curves were linear in the range 0–2.00 mg L−1 P-phosphate, 0–10.00 mg L−1 nitrite and 0–7.00 mg L−1 nitrate with correlation coefficients of 0.9979, 0.9993 and 0.9995, respectively. The detection limits, calculated as 3S/N,
were 0.15 mg L−1 for P-phosphate, 0.17 mg L−1 for nitrite and 0.09 mg L−1 for nitrate. The reproducibility was below 3.0% (n = 7). Method validation in the analysis of natural water and wastewater samples revealed that it can efficiently be applied
to the determination of the target analytes, with recoveries in the range of 92–108%.
Correspondence: Athanasios G. Vlessidis, Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina,
Ioannina 45110, Greece 相似文献
4.
Natalia García-Otero Carmen Teijeiro-Valiño Jacobo Otero-Romaní Elena Peña-Vázquez Antonio Moreda-Piñeiro Pilar Bermejo-Barrera 《Analytical and bioanalytical chemistry》2009,395(4):1107-1115
Nickel(II) and lead(II) ionic imprinted 8-hydroxyquinoline polymers were synthesized by a precipitation polymerization technique
and were used as selective solid phase extraction supports for the determination of nickel and lead in seawater by flow injection
solid phase extraction on-line inductively coupled plasma-optical emission spectrometry. An optimum loading flow rate of 2.25 mL min−1 for 2 min and an elution flow rate of 2.25 mL min−1 for 1 min gave an enrichment factor of 15 for nickel. However, a low dynamic capacity and/or rate for adsorption and desorption
was found for lead ionic imprinted polymer and a flow rate of 3.00 mL min−1 for 4-min loading and a flow rate of 2.25 mL min−1 for 1-min elution gave a enrichment factor of 5. The limit of detection was 0.33 μg L−1 for nickel and 1.88 μg L−1 for lead, with a precision (n = 11) of 8% (2.37 μg Ni L−1) for nickel and 11% (8.38 μg Pb L−1) for lead. Accuracy was also assessed by analyzing SLEW-3 (estuarine water) and TM-24 (lake water) certified reference materials,
and the values determined were in good agreement with the certified concentrations. 相似文献
5.
Joyce Nunes Bianchin Renata Mior Cleide Sandra Tavares Araújo Eduardo Carasek 《Talanta》2009,78(2):333-2300
In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L−1, a sample flow rate of 4.5 mL min−1 and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 μg L−1 and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 μg L−1, with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 μg L−1, n = 7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%. 相似文献
6.
Preconcentration Systems Using Polyurethane Foam/Me-BDBD for Determination of Copper in Food Samples
Valfredo Azevedo Lemos Daniel Rodrigues Vieira Cleber Galvão Novaes Marcelo Eça Rocha Moacy Selis Santos Regina Terumi Yamaki 《Mikrochimica acta》2006,153(3-4):193-201
A new reagent, 6-[2′-(6′-methyl-benzothiazolylazo)]-1,2-dihydroxy-3,5-benzenedisulfonic acid (Me-BDBD), was synthesised and
used in on-line and off-line systems for copper preconcentration by solid-phase extraction. Spectrophotometry and Flame Atomic
Absorption Spectrometry (FAAS) were the detection techniques. Polyurethane foam loaded with Me-BDBD packed in a minicolumn
was used as sorbent in both systems. The spectral characteristics of Me-BDBD were investigated. The optimum pH values for
maximum sorption of the metal are between 7.0 and 8.5. Copper was desorbed with 0.05 and 0.50 mol L−1 hydrochloric acid solutions, for on-line and off-line systems, respectively. The effects of several foreign substances on
the adsorption of copper are reported. The enrichment factors obtained were 7 (on-line) and 26 (off-line) for the systems.
The proposed procedures allowed the determination of copper with detection limits of 3.4 and 1.4 μg L−1 (0.85 and 0.35 μg per gram of sample) for on-line and off-line systems, respectively. The precision of the procedures was
also calculated: 3.2 (on-line) and 1.9% (off-line). The validation of the procedures was carried out by analysis of certified
reference material. The copper contents in corn and rice flour and black tea samples were determined by applying the proposed
procedures. 相似文献
7.
A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h−1. The detection limit was 0.01 μg L−1 and the precision (RSD at 0.1 μg L−1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material. 相似文献
8.
A new flow injection (FIA) procedure for the preconcentration of cadmium in urine using multiwalled carbon nanotubes (MWCNT) as sorbent and posterior electrothermal atomization atomic absorption spectrometry (ETA-AAS) Cd determination has been developed. Cadmium was retained in a column filled with previously oxidized MWCNTs and it was quantitatively eluted with a nitric acid solution. The parameters influencing the adsorption-elution process such as pH of the sample solution, amount of sorbent and flow rates of sample as well as eluent solutions have been studied. Cd concentration in the eluent was measured by ETA-AAS under the optimized conditions obtained. The results indicated the elimination of urine matrix effect as a consequence of the preconcentration process performed. Total recovery of cadmium from urine at pH 7.2 using a column with 45 mg of MWCNTs as sorbent and employing a HNO3 0.5 mol L−1 solution for elution was attained. The detection limit obtained was 0.010 μg L−1 and the preconcentration factor achieved was 3.4. The method showed adequate precision (RSD: 3.4-9.8%) and accuracy (mean recovery: 97.4-100%). The developed method was applied for the determination of cadmium in real urine samples from healthy people (in the range of 0.14-2.94 μg L−1) with satisfactory results. 相似文献
9.
A novel molecularly imprinted polymer solid-phase extraction (MISPE) with flow-injection chemiluminescence (CL) was developed
for the determination of pazufloxacin mesilate (PZFX). The molecularly imprinted polymer (MIP) was synthesized by using PZFX
as the imprinting molecule. A glass tube packed the particles of the MIP was employed as MISPE micro-column, which was connected
into the sampling loop of the eight-way injection valve for on-line selective preconcentration and extraction of PZFX. The
eluent of acetonitrile:acetic acid (9:1, v:v) was used as carrier for eluting the adsorbed PZFX to react with the mixture
of cerium(IV) and sodium sulfite in the flow cell to produce strong CL. The relative intensity of CL was linear to PZFX concentration
in the range from 2.5 × 10−9 to 2.5 × 10−7 g mL−1. The limit of detection was 7 × 10−10 g mL−1 (3 σ) and the relative standard deviation for 5 × 10−8 g mL−1of PZFX solution was 3.7% (n = 7). This method has been applied to the determination of PZFX in human urine. 相似文献
10.
An on-line solid phase extraction (SPE) preconcentration system coupled to flame atomic absorption spectrometer (FAAS) was developed for determination of copper and cadmium at μg L−1 level. The method is based on the on-line retention of copper and cadmium on a microcolumn of alumina modified with sodium dodecyl sulfate (SDS) and 1,10-phenanthroline and subsequent elution with ethanol and determination by FAAS. The effect of chemical and flow variables that could affect the performance of the system was investigated. The relative standard deviation (n = 6) at 20 μg L−1 level for copper and cadmium were 1.4 and 2.2% and the corresponding limits of detection (based on 3σ) were 0.04 and 0.14 μg L−1, respectively. The method was successfully applied to determination of copper and cadmium in human hair and water samples. 相似文献
11.
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
12.
A novel method for rapid HPLC-ICP-MS analysis of oxaliplatin in human urine was developed implementing a stationary HPLC phase
with a particle size of 1.8 μm. The method allowed a cycle time of <1 min at a HPLC flow rate of 0.9 mL min−1. Procedural limits of detection of 0.05 μg L−1 oxaliplatin (150 fg on column) were obtained. Analysis of oxaliplatin in patient urine showed that accurate quantification
of the intact drug demanded for storage at −80 °C and rapid measurement after thawing. 相似文献
13.
García-Ruiz S Petrov I Vassileva E Quétel CR 《Analytical and bioanalytical chemistry》2011,401(9):2785-2792
The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08
and 0.25 μg L−1 depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real
samples, and we hereby propose a validated method capable of addressing cadmium content below μg L−1 level in natural water. It is based on solid-phase extraction using TiO2 nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from
the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS).
The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility.
Procedural blanks for the whole measurement process were 5.3 ± 2.8 ng kg−1 (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including
loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery
rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency
for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter
5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios
measured after our separation procedure to the reference values obtained with a different protocol for the digested test material
IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties
associated to our results were estimated according to ISO-GUM guidelines (typically, 3–4% k = 2 for a cadmium content of around 100 ng kg−1). We applied the developed method to the groundwater and wastewater samples ERM-CA615 and BCR-713, respectively, and results
agreed with certificate values within uncertainty statements. 相似文献
14.
A novel hydrophobic sorbent material for on-line column preconcentration and separation systems coupled with atomic spectrometry was developed. Poly(etheretherketone) (PEEK) in the form of turnings was used as packing material and evaluated for trace lead determination in environmental samples. Sample and ammonium diethyl-dithiophosphate (DDPA) reagent were mixed on-line and the Pb(II)-DDPA complex was retained effectively on PEEK-turnings. Isobutyl methyl ketone (IBMK) was adopted for efficient analyte complex elution and subsequently transportation into the nebulizer-burner system for atomization. The developed sorbent material has shown, excellent chemical and mechanical resistance, fast adsorption kinetics permitting the use of high sample flow rates without significant loss of retention efficiency. For 120 s sample preconcentration time the sampling frequency was 20 h−1, the enhancement factor was 110, the detection limit (3 s) was cL = 0.32 μg L−1, and the relative standard deviation (RSD) was sR = 2.2%, at the 50.0 μg L−1 Pb(II) level. The accuracy of the developed method was evaluated by analyzing certified reference materials. 相似文献
15.
Xiangbing Zhu Dong Yang Xijun Chang Yuemei Cui Zheng Hu Xiaojun Zou 《Mikrochimica acta》2008,161(1-2):115-122
A new method using acetylsalicylic acid (aspirin) modified SiO2 nanoparticles (nanometer SiO2-aspirin) as a solid-phase extractant (SPE) has been developed for the preconcentration of trace amounts of Fe(III) prior
to their determination by inductively coupled plasma optical emission spectrometry. The preconcentration conditions of analytes
were investigated, including the pH value, the shaking time, the mass of sorbent, the sample flow rate and volume, the elution
condition and the interfering ions. At pH 4, the sorption capacity of nanometer SiO2-aspirin was found to be 1.28 mmol g−1. The preconcentration factor is 50. The detection limit (3σ) for Fe(III) was 0.49 ng mL−1. The method was validated by analyzing two certified reference materials (GBW 08301, river sediment and GBW 08303, polluted
farming soil), and the results obtained are in good agreement with standard values. The method was also applied to the determination
of trace Fe(III) in biological and water samples with satisfactory results.
Correspondence: Xiangbing Zhu, Department of Chemistry, Lanzhou University, Lanzhou 730000, P.R. China 相似文献
16.
Cleide S.T. Araújo 《Microchemical Journal》2010,96(1):82-85
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.
Effect of Substrate Concentration on Dark Fermentation Hydrogen Production Using an Anaerobic Fluidized Bed Reactor 总被引:1,自引:0,他引:1
The effect of substrate (glucose) concentration on the stability and yield of a continuous fermentative process that produces
hydrogen was studied. Four anaerobic fluidized bed reactors (AFBRs) were operated with a hydraulic retention time (HRT) from
1 to 8 h and an influent glucose concentration from 2 to 25 g L−1. The reactors were inoculated with thermally pre-treated anaerobic sludge and operated at a temperature of 30 °C with an
influent pH around 5.5 and an effluent pH of about 3.5. The AFBRs with a HRT of 2 h and a feed strength of 2, 4, and 10 g L−1 showed satisfactory H2 production performance, but the reactor fed with 25 g L−1 of glucose did not. The highest hydrogen yield value was obtained in the reactor with a glucose concentration of 2 g L−1 when it was operated at a HRT of 2 h. The maximum hydrogen production rate value was achieved in the reactor with a HRT of
1 h and a feed strength of 10 g L−1. The AFBRs operated with glucose concentrations of 2 and 4 g L−1 produced greater amounts of acetic and butyric acids, while AFBRs with higher glucose concentrations produced a greater amount
of solvents. 相似文献
18.
Shabnam Shahida Akbar Ali Muhammad Haleem Khan Muhammad Mufazzal Saeed 《Journal of Radioanalytical and Nuclear Chemistry》2011,289(3):929-938
A flow injection on-line determination of uranium(VI) after preconcentration in a minicolumn having amberlite XAD-4 resin
impregnated with dibenzoylmethane (DBM) is described. Uranium(VI) is selectively adsorbed from aqueous solution of pH 5.5
in the minicolumn (5.5 cm long with 5.0 mm i.d.) at a flow rate of 13.6 mL min−1. The uranium(VI) complex was desorbed from the resin by 0.1 mol dm−3 HCl at a flow rate of 4.2 mL min−1 and mixed with arsenazo-III solution (0.05% solution in 0.1 mol dm−3 HCl, 4.2 mL min−1), and taken to the flow through cell of spectrophotometer where its absorbance was measured at 651 nm. Various parameters
affecting the complex formation and its elution were optimized. Peak height (absorbance) was used for data analyses. The preconcentration
factors of 36 and 143, detection limits of 0.9 and 0.232 μg L−1, sample throughputs of 40 and 10 were obtained for preconcentration time of 60 and 300 s, respectively. The tolerance limits
of many interfering cations like Th(IV) and rare-earth elements were improved. The proposed method was applied on different
water (spiked tap, well and sea water) and biological samples and good recovery was obtained. The method was also validated
on mocked uranium ore sample and the results were in good agreement with the reported value. 相似文献
19.
Silica gel was prepared by the sol–gel method, modified with nanometer-sized zirconium oxide, and this material was characterized
by X-ray diffraction. A micro-column packed with silica gel modified with nanometer zirconium oxide as sorbent has been developed
for the quantitative separation and preconcentration of trace amounts of chromium(III) prior to their determination by electrothermal
atomic absorption spectrometry. Total chromium was determined after the reduction of chromium(VI) to chromium(III) by 10%
(m/v) of aqueous ascorbic acid as reducing reagent. The adsorption capacity for chromium(III) was found to be 2.36 mg g−1. The detection limit for chromium(III) was 15 ng L−1 with an enrichment factor of 100. The relative standard deviation was 3.2% (n = 7, c = 2.0 ng mL−1). 相似文献
20.
Vanessa Nunes Alves Nívia Maria Melo Coelho Kalya Cravo Di Pietro Roux Eduardo Carasek 《Talanta》2010,80(3):1133-1138
In this study a new method for determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line preconcentration system coupled to flame atomic absorption spectrometry (FAAS) was developed. Flow and chemical variables of the proposed system were optimized through multivariate designs. The limit of detection for cadmium was 5.50 μg L−1 and the precision was below 2.3% (35.0 μg L−1, n = 9). The analytical curve was linear from 5 to 150 μg L−1, with a correlation coefficient of 0.9993. The developed method was successfully applied to spiked alcohol fuel, and accuracy was assessed through recovery tests, with recovery ranging from 97.50 to 100%. 相似文献