Flow Injection System For Determination Research Articles

An exploiting of cost-effective direct current conductivity detector in gas diffusion flow injection system

In this work, a homemade direct current (DC) conductivity detector as an alternative cost-effective detection device has been fabricated and investigated to use in flow analysis system. Under the selected appropriate conditions of flow system, the electrolysis of a carrier stream at the conductivity detector was negligible and provides well-defined signal. The cost-effective DC conductivity detector was demonstrated to couple with gas diffusion flow injection system for determination of dissolved inorganic carbon (DIC) in water. The method is based on the conversion of DIC (dissolved CO2, HCO3- and CO32-) presented in the injected sample to carbon dioxide in an acidic donor stream and then CO2 gas diffuses through a hydrophobic porous membrane to an acceptor stream. As a result, the change of conductivity signal was observed corresponding to DIC concentration. A linear calibration range of DIC in 1.0–10mmolL−1, with limit of detection of 70µmolL−1, repeatability of <3% RSD and 15 injections h−1 sample throughput can be obtained. This method was applied for DIC determination in natural water.

A microfabricated electroosmotic pump coupled to a gas-diffusion microchip for flow injection analysis of ammonia

We have microfabricated two functional components toward developing a microchip flow injection analysis (FIA) system, i.e., an open-channel electroosmotic pump and a gas-diffusion chip, consisting of two microfabricated glass wafers and a porous polytetrafluoroethylene membrane. This is the first application of gas-diffusion separation in a microchip FIA system. To demonstrate the feasibility of using these two components for performing gas-diffusion FIA, we have incorporated them together with a regular FIA injection valve and a capillary electrophoresis absorbance detector in a flow injection system for determination of ammonia in environmental water samples. This system has a limit of detection of 0.10 mg L−1 NH3, with a good repeatability (relative standard deviation of less than 5 % for 4.0 mg L−1 NH3). Parameters affecting its performance are also discussed.

On-line solid–phase extraction using a C18 minicolumn coupled to a flow injection system for determination of caffeine in green and roasted coffee beans

A novel and fast method based on the solid phase extraction (SPE) coupled to a flow injection system for the determination of caffeine in coffee beans was developed. The caffeine extraction of coffee beans was carried out with hot water. A C18 reverse-phase mini-column was coupled to a continuous flow manifold to carry out the on-line SPE and the quantification of caffeine from aqueous extracts. Column length, retention time, elution volume, extracting solution and injection volume were evaluated. The retention time was of 90s and the elution was carried out with 400μL of a methanol:water mixture (25:75). The proposed on-line SPE was compared against a chloroform extraction from aqueous extracts. With the proposed method the sample preparation was minimised and the sample throughput was increased (10determination/h) because no dilution was required. Green coffee beans and beans with different roasting degree were analyzed.

Potentiometric flow injection system for determination of reductants using a polymeric membrane permanganate ion-selective electrode based on current-controlled reagent delivery

A polymeric membrane permanganate-selective electrode has been developed as a current-controlled reagent release system for potentiometric detection of reductants in flow injection analysis. By applying an external current, diffusion of permanganate ions across the polymeric membrane can be controlled precisely. The permanganate ions released at the sample-membrane interface from the inner filling solution of the electrode are consumed by reaction with a reductant in the sample solution thus changing the measured membrane potential, by which the reductant can be sensed potentiometrically. Ascorbate, dopamine and norepinephrine have been employed as the model reductants. Under the optimized conditions, the potential peak heights are proportional to the reductant concentrations in the ranges of 1.0 × 10 −5 to 2.5 × 10 −7 M for ascorbate, of 1.0 × 10 −5 to 5.0 × 10 −7 M for dopamine, and of 1.0 × 10 −5 to 5.0 × 10 −7 M for norepinephrine, respectively with the corresponding detection limits of 7.8 × 10 −8, 1.0 × 10 −7 and 1.0 × 10 −7 M. The proposed system has been successfully applied to the determination of reductants in pharmaceutical preparations and vegetables, and the results agree well with those of iodimetric analysis.

Spectrophotometric flow injection system for determination of Zn2+ in ophthalmic formulations using Alizarin red S

A spectrophotometric flow injection method for the determination of Zn(II) in ophthalmic formulations was developed. In this work, Zn(II) ion was complexed with Alizarin red S in borate buffer solution (pH 9.0) and the chromophore produced was monitored at 520 nm. The analytical curve was linear in the Zn(II) concentration range from 6.05 x 10-6 to 1.50 x 10-4 mol L-1 with a detection limit of 3.60 x 10-6 mol L-1. Recoveries ranged from 96.3 to 105 % and a relative standard deviation of 1.2 % (n = 10) for 5.5x10-5 mol L-1 Zn(II) reference solution were obtained. The sampling rate was 60 h-1 and the results obtained of Zn(II) in ophthalmic products using this procedure are in close agreement with those obtained using a comparative spectrophotometric procedure at 95 % confidence level.

Spectrophotometric flow injection system for determination of Zn2+ in ophthalmic formulations using Alizarin red S

A spectrophotometric flow injection method for the determination of Zn(II) in ophthalmic formulations was developed. In this work, Zn(II) ion was complexed with Alizarin red S in borate buffer solution (pH 9.0) and the chromophore produced was monitored at 520 nm. The analytical curve was linear in the Zn(II) concentration range from 6.05 x 10-6 to 1.50 x 10-4 mol L-1 with a detection limit of 3.60 x 10-6 mol L-1. Recoveries ranged from 96.3 to 105 % and a relative standard deviation of 1.2 % (n = 10) for 5.5x10-5 mol L-1 Zn(II) reference solution were obtained. The sampling rate was 60 h-1 and the results obtained of Zn(II) in ophthalmic products using this procedure are in close agreement with those obtained using a comparative spectrophotometric procedure at 95 % confidence level.

On-line preconcentration system using a microcolumn packed with Alizarin Red S-modified alumina for zinc determination by flame atomic absorption spectrometry

A simple and sensitive on-line flow injection system for determination of zinc with FAAS has been described. The method is based on the separation and preconcentration of zinc on a microcolumn of immobilized Alizarin Red S on alumina. The adsorbed analyte is then eluted with 250 µL of nitric acid (1 mol L-1) and is transported to flame atomic absorption spectrometer for quantification. The effect of pH, sample and eluent flow rates and presence of various cations and anions on the retention of zinc was investigated. The sorption of zinc was quantitative in the pH range of 5.5-8.5. For a sample volume of 25 mL an enrichment factor of 144 and a detection limit (3S) of 0.2 µg L-1 was obtained. The precision (RSD, n=7) was 3.0% at the 20 µg L-1 level. The developed system was successfully applied to the determination of zinc in water samples, hair, urine and saliva.

Preparing of Iridium Oxide Film Modified Microelectrode as an Amperometric Detector in FIA for Determination of Epinephrine

Iridium oxide film modified microelectrode with a tip diameter of 25 µm was constructed using anodically grown iridium oxide film. The iridium oxide film, which was formed at the tip of the iridium wire by cyclic voltammetry in dilute sulfuric acid, showed excellent catalytic activity towards the oxidation of epinephrine. The stability and electrochemical properties of iridium oxide film modified microelectrode along with catalytic oxidation of epinephrine was studied. An oxidation peak was observed at 0.28 V. The electron‐transfer number (n) was 2. The iridium oxide film modified microelectrode was used as a detector in flow injection system for determination of epinephrine. Under the optimized conditions, the calibration curve was linear in the concentration range of 1.0×10−8 to 1.0×10−5 mol/l for epinephrine, with a detection limit of 1.0×10−9 mol/l. The iridium oxide film modified microelectrode was used for direct determination of the epinephrine in human serum samples. The flow injection analysis was precise detection method of epinephrine and time saving device.

Potentiometric multi-syringe flow injection system for determination of exchangeable potassium in soils with in-line extraction

A multi-syringe flow injection system for the potentiometric determination of exchangeable potassium in soil samples is proposed. Firstly, a manifold was devised to allow determination in soil extracts prepared off-line. It was possible to analyze samples prepared in extractants with different composition (Mehlich or Morgan) without physical or chemical modification of the manifold. A linear dynamic concentration range of 6–391 mg L − 1 was obtained, allowing the direct introduction of soil extract without dilution. A determination frequency of 50 h − 1 was achieved, with good repeatability for 10 consecutive injections of soil extracts (RSD < 3.0%). The in-line preparation of soil extract was implemented by automatic addition of extractant solution to a previously weighed portion of soil, followed by in-line filtration. Good repeatability was attained as the variance of the extraction procedure was not significantly different from the variance obtained in consecutive measurements of the same extract. Furthermore, results comparable to those obtained by off-line extraction and determination by flame emission spectrometry were attained for the two soil samples tested. Using this procedure, a determination frequency of 13 h − 1 and a sampling rate of 4 h − 1 were achieved.

Novel analytical applications of porphyrin to HPLC post-column flow injection system for determination of the lanthanides

A novel indirect substitution spectrophotometric methodology using porphyrin is developed for the determination of some metals that do not react with porphyrin directly. The methodology is concerned with a multistep reaction system, which consists of 3 complexation reactions that occur in a sequence of EDTA with metal, EDTA with Cu(II) and porphyrin with Cu(II). The complexation reaction of Cu(II) with a cationic porphyrin, meso-tetrakis (4- N-trimethylaminophenyl)-porphine (ttmapp), which has a high molar absorptivity about 5 × 10 5 l mol −1 cm −1, serves for spectrophotometric detection. This methodology was verified through individual determinations of 14 species of lanthanides following a batchwise procedure, which was further developed to an automatic procedure on a HPLC post-column flow injection system for simultaneous analysis of the lanthanides. Compared with the conventional post-column derivatization method using 4-(2-pyridylazo) resorcinol (PAR), the analytical sensitivity was greatly improved in this method and the results also showed good linearity.

Determinação condutométria de carbonato residual do calcário aplicado no solo por análise em fluxo

The objective of this study was to evaluate a flow injection system for determination of residual CO32- in soil amended with lime material. It was used a closed system were the CO2 released from soil sample acidified with 0.5 mol L-1 HCl was capted in a 0.2 mol L-1 NaOH solution. After 16h the capted CO2 was determined by conductivimetry using a flow injection system. The results obtained by the proposed method were significantly correlated with those reported in soil samples used by the International Soil Analytical Exchange Programe. The regression equation was: y = 0.987x ¾ 0.075 r = 0.996, P > 0.01. For acid soils amended with CaCO3 the method showed a deviation error of 2.7%, detection limit was 0.077 mmol kg-1 of CO32-, and a recovery of 99.7% of the total CO32- added in soil sample. The method was easily adapted for routine determination of residual CO32- in soil samples with an analytical frequency of 40 samples per hour.

Eletrodissolução anódica em sistema de injeção em fluxo: uma alternativa rápida e eficiente para dissolução de ligas metálicas

Anodic electrodissolution procedure in a flow injection system for determination of constituents in alloys is discussed. This approach implement sample preparation procedure by using a chamber and a DC power supply with constant direct current. Solid sample was attached to chamber as anode. In this review a general overview of these procedure is presented. The procedure presented a good performance characterized by a high sample throughput determinations, good accuracy and relative standard deviation.

Highly-sensitive flow injection determination of hydrogen peroxide with a peroxidase-immobilized electrode and its application to clinical chemistry

A flow injection system for determination of hydrogen peroxide was constructed using a peroxidase/ferrocene-embedded carbon paste (POD-Fc-CP) electrode covered with a membrane. H 2O 2 was reduced bioelectrocatalytically at 100 mV (versus Ag/AgCl/sat. KCl). A Nafion ®-coated cellulose acetate membrane prepared on the surface of water proved to be suitable for the covering membrane. The detection limit (signal : noise = 6) for H 2O 2 was 200 fmol (10 nM × 20 μl) and the response linearity was retained at least up to 25 μM. The relative standard deviation was 4.4% for 1.0 μM H 2O ( n = 7). The flow injection system was successfully applied to the determination of glucose and urate in serum by using the corresponding oxidase-immobilized pre-column. The detection limits were 1.5 pmol for glucose and 2 pmol for urate.

Eletrodissolução de ligas de latão empregando sistemas de análise em fluxo para a determinação de cobre, zinco e chumbo por ICP-AES

An on-line electrodissolution procedure implemented in a flow injection system for determination of copper, zinc and lead in brasses alloys by ICP-AES is described. Sample dissolution procedure was carried out by using a PTFE chamber and a DC power supply with constant current. Solid sample was attached to chamber as anode and a gold tubing coupled in the chamber was used as cathode. An electrolytic solution flowing through the gold tubing closed the electric circuit with sample, in order to provide condition for electric dissolution when the DC power supply was switched on. The best results were achieved by using a 1.5 mol l-1 nitric acid solution as electrolyte and a 2.5 A current intensity. The procedure presented a good performance characterized by a relative standard deviation better than < 5% (n=5) and a sample throughput of 180 determinations per hour for Cu, Zn and Pb. Results were in agreement with those obtained by conventional acid dissolution (99% confidence level).

Merging Zones Standard Addition Technique for Determination of Copper in Beer by Flow Injection Atomic Absorption Spectrophotometry

A flow injection system for determination of copper in beer by atomic absorption spectrophotometry by the standard additions method is described. The manifold, based on the merging zone technique, prevents the burner head from clogging, as observed with the conventional reference method. With 5 standard additions, results are comparable with those of the reference method. Relative deviations were less than 5.8%, precision was better than 6.4%, and sampling rate was about 30 samples/ h. A less precise, less accurate, but faster procedure (75 samples/h) is possible with only 2 standard additions. The detection limit was 5 micrograms/L.

Immobilization of glucose oxidase and acetylcholinesterase onto modified polyamide sorbent

Two types of polyamide (PA) sorbents with high specific area were prepared. The effects of solvent type, concentrations of formic acid, and polymer on the porosity characteristics were studied. The sorbent with the highest specific area was obtained by using C 2 H 5 OH-HCOOH solvent (60% HCOOH ) and the rest of the experiments were carried out with this type of sorbent. The possibility of applying the PA sorbent as carrier for immobilization of glucose oxidase ( GOD ) and acetylcholinesterase (AChE) was investigated. In order to increase the active groups content (necessary for enzyme immobilization), the sorbent was modified with dimethylaminoethylmethacrylate (DMAEM) and 2-acrylamido-2-methylpropensulfonic acid. The amount of the active groups introduced during the modification and the degree of hydrophilicity were determined. The quantity of bound protein and relative activity of GOD and AChE immobilized onto unmodified and modified sorbents were studied. Optimum pH and temperature of the immobilized GOD and AChE were also determined. The influence of three phosphoroorganic compounds on the activity of the immobilized AChE was investigated. Tetrachlorvinvos was found to be the strongest inhibitor, while AChE immobilized onto PA sorbent modified with DMAEM showed the highest stability. The possibility of using immobilized GOD and AChE in a flow-injection system for determination of the concentrations of glucose and phosphoroorganic compounds was studied.

Process monitoring of acetic acid in Escherichia coli cultivation using electrochemical detection in a flow injection system

A flow-injection system for determination of acetic acid in Escherichia coli cultivations with electrochemical detection based on immobilized acetate kinase (AK), pyruvate kinase (PK) and lactate dehydrogenase (LDH) was developed to cope with the problems related to measurements under process conditions such as interferences from pyruvate, drift of electrode baseline and making the cultivation medium and reagents compatible. The results obtained by flow injection analysis were compared with those obtained with an enzymatic test kit.

Flow injection determination of metrifonate by immobilised acetylcholinesterase inhibition

A flow injection system for determination of metrifonate by inhibition of immobilised acetylcholinesterase (AChE) is described. Acetylthiocholine is hydrolysed by AChE, and the thiocholine produced is mixed with the chromogen 5,5-dithiobis(2-nitrobenzoic acid) and the absorbance is measured at 405 nm. The decrease in absorbance due to decrease in enzymatic activity after injecting metrifonate as an inhibitor is measured. On-line re-activation of the inhibited enzyme by buffer, substrate and pyridine-2-aldoxime methiodide is also studied so that system can be reused continuously. The calibration graph is linear in the range of 1 × 10 −6 to 1 × 10 −5 M metrifonate ( r = 0.998, n = 5), the 3σ limit of detection is 8 × 10 −7 M and the relative standard deviation for 5 determinations of 6 × 10 −6 M metrifonate is 2.0%. Common blood components did not interfere.

Membrane-based flow injection system for determination of sulfur(IV) in atmospheric water

A single flow channel analysis system that employs the formaldehyde-S(IV)-pararosaniline color reaction has been developed for the determination of aqueous S(IV). The system employs a passive cation-exchange membrane reactor for the introduction of base and a pressurized porous membrane reactor for the introduction of acidic pararosaniline. The detection limit is 1.6 x 10/sup -7/ M S(IV); the sample size is 200 ..mu..L, and the throughput rate is 15/h. Results for cloudwater samples are presented. 15 references, 3 figures, 1 table.