Digital image colorimetric detection of ceftazidime based on azo compound formation on a polyethyleneimine-modified cotton sponge.

A novel colorimetric platform using cotton sponges modified with polyethyleneimine (PEI) was fabricated for the detection of ceftazidime through the diazotization and coupling reaction. In this work, cotton sponges were initially prepared by freeze drying using 2 w/w% cotton fibers modified with 3-aminopropyl triethoxysilane (APTES), followed by grafting of PEI through a crosslinking reaction using epichlorohydrin (ECH). The optimal concentrations of modifying agents were 170 mM APTES for 1.0 g of cotton fibers and 210 µM PEI for 0.5 g of APTES sponges. With a sample volume of 150 mL, the extracted ceftazidime was detected through the reactions with 0.5 M HCl, 30 mM NaNO2, and 25 µM chromotropic acid on the sponge surface. The PEI-sponge platform provided good selectivity and sensitivity for ceftazidime determination within 30 min. The linear working range for ceftazidime determination was in the range of 0.5-3.0 mg L-1 with a limit of detection (LOD) of 0.06 mg L-1. The proposed method was successfully applied to detect ceftazidime in water samples with satisfactory recovery (83-103%) and reproducibility (<4.76% RSD).

Miniaturized sensor for electroanalytical and electrochemiluminescent detection of pathogens enabled through laser-induced graphene electrodes embedded in microfluidic channels.

High performance, laser-induced graphene (LIG) electrodes were integrated into adhesive tape-based microfluidic channels to realize both electrochemical (EC) and electrochemiluminescent (ECL) detection approaches. This provides strategies for low limits of detection, simple hardware requirements and inexpensive fabrication, which are characteristics required for assays in the competitive point-of-care (POC) sensor field. Here, electrode design and microchannel dimensions were studied and a DNA hybridization assay with liposomes for signal amplification was developed for the specific detection of DNA derived from Cryptosporidium parvum as the model analyte. Liposomes entrapped either Ru(bpy)32+ or K4[Fe(CN)6] generating ECL- and EC-signal amplification, respectively. This new microchip provided all desirable analytical figures of merit needed for POC applications. Specifically, a desirable one-step assay was designed which provided a limit of detection of 3 pmol L-1 for the ECL and 47 pmol L-1 for the EC approach and furthermore enabled highly specific detection considering that at room temperature in this simple setup a single nucleotide polymorphism resulted in a signal decrease of 58%, whereas a decrease of > 98% was observed for non-matching sequences present in 10-fold excess. Direct detection in various matrices ranging from drinking water to soil extracts was also achieved. It is concluded that the simple and inexpensive fabrication in combination with signal amplification strategies makes these concepts relevant for on-site pathogen detection in resource-limited environments.

Silver-doped hydroxyapatite for formaldehyde determination by digital-image colorimetry.

Silver-hydroxyapatite material (Ag-HAP) was first proposed as material for trace-level formaldehyde detection based on Tollens' reaction on the material surface. By using this Ag-HAP material, the chemical reduction caused by formaldehyde occurred directly on the solid surface. The material color changed from off-white to the yellow or brown of silver nanoparticles depending on the formaldehyde concentration. The color intensity of the materials was measured from their smartphone digital images using Image-J software. The effect of silver ion concentration, sodium hydroxide concentration, contact time, and sample volume on formaldehyde detection were investigated. Under optimized conditions, the working range for formaldehyde detection was determined to be 15 to 200 µg L-1. The method was successfully applied to detect trace formaldehyde in water samples and a recovery of 86 to 111%, with an RSD of 3 to 8%, was observed. With a lowest concentration for the detection of 15 µg L-1 and good accuracy and precision, the method showed promise for formaldehyde determination.

Paper-based Platform for Urinary Creatinine Detection.

A new paper platform was developed for the colorimetric detection of creatinine. The filter paper was coated with 3-propylsulfonic acid trimethoxysilane and used as the platform. Creatinine in a cationic form was extracted onto the paper via an ion-exchange mechanism and detected through the Jaffé reaction, resulting in a yellow-orange color complex. The color change on the paper could be observed visually, and the quantitative detection of creatinine was achieved through monitoring the color intensity change. The color intensity of creatinine complexes on the paper platform as a function of the creatinine concentration provided a linear range for creatinine detection in the range of 10 - 60 mg L(-1) and a detection limit of 4.2 mg L(-1). The accuracy of the proposed paper-based method was comparable to the conventional standard Jaffé method. This paper platform could be applied for simple and rapid detection of creatinine in human urine samples with a low consumption of reagent.

Detection of urinary creatinine using gold nanoparticles after solid phase extraction.

Label-free gold nanoparticles (AuNPs) were utilized in the detection of creatinine in human urine after a sample preparation by extraction of creatinine on sulfonic acid functionalized silica gel. With the proposed sample preparation method, the interfering effects of the urine matrix on creatinine detection by AuNPs were eliminated. Parameters affecting creatinine extraction were investigated. The aggregation of AuNPs induced by creatinine resulted in a change in the surface plasmon resonance signal with a concomitant color change that could be observed by the naked eye and quantified spectrometrically. The effect of AuNP concentration and reaction time on AuNP aggregation was investigated. The method described herein provides a determination of creatinine in a range of 15-40mgL(-1) with a detection limit of 13.7mgL(-1) and it was successfully used in the detection of creatinine in human urine samples.

Automated on-line preconcentration of trace aqueous mercury with gold trap focusing for cold vapor atomic absorption spectrometry.

A fully automated system for the determination of trace mercury in water by cold vapor atomic absorption spectrometry (CVAAS) is reported. The system uses preconcentration on a novel sorbent followed by liberation of the mercury and focusing by a gold trap. Mercury ions were extracted from water samples by passage through a solid phase sorbent column containing 2-(3-(2-aminoethylthio)propylthio)ethanamine modified silica gel. The captured mercury is released by thiourea and then elemental Hg is liberated by sodium borohydride. The vapor phase Hg is recaptured on a gold-plated tungsten filament. This is liberated as a sharp pulse (half-width<2 s) by directly electrically heating the tungsten filament in a dry argon stream. The mercury is measured by CVAAS; no moisture removal is needed. The effects of chloride and selected interfering ions were studied. The sample loading flow rate and argon flow rates for solution purging and filament sweeping were optimized. An overall 50-fold improvement in the limit of detection was observed relative to direct measurement by CVAAS. With a relatively modest multi-user instrument we attained a limit of detection of 35 ng L(-1) with 12% RSD at 0.20 µg L(-1) Hg level. The method was successfully applied to accurately determine sub-µg L(-1) level Hg in standard reference water samples.

Removal of heavy metal ions by iron oxide coated sewage sludge.

The municipal sewage sludge was modified with iron oxide employed in metal ions removal. The surface modification method was proposed and the effect of parameters in the preparation was studied. The iron oxide coated sludge had higher surface area, pore volume and iron content, compared to uncoated sludge. The suitable conditions for removal of Cu(II), Cd(II), Ni(II) and Pb(II) ions from solutions were investigated using batch method. The suitable pH value in the extraction was 7 for adsorption of Cd(II) and Ni(II), 6 for Cu(II) and 5 for Pb(II) ions. The presence of NaNO(3), Ca(NO(3))(2) and Na(2)SO(4) in metal solution in the concentration of 0.01 M and 0.50 M could reduce the removal efficiency. The adsorption isotherms for the adsorption of the metal ions were defined by Langmuir relation. The maximum adsorption capacity of the iron oxide coated sludge for Cu(II), Cd(II), Ni(II) and Pb(II) was 17.3, 14.7, 7.8 and 42.4 mg g(-1), respectively. The adsorption kinetics for every metal ions followed pseudo-second order model. The metal removal from wastewater by iron oxide coated sludge was also demonstrated.

A cold plasma dielectric barrier discharge atomic emission detector for atmospheric mercury.

An automated atmospheric elemental mercury analyzer based on the dielectric barrier discharge (DBD) atomic emission technique was developed. The instrument is based on a gold-on tungsten coiled filament preconcentrator fashioned from commercial quartz-halogen lamps, a DBD excitation source and a radiation detector. An in-house program provided system control and data collection. Several types of radiation detectors, e.g., charge coupled device (CCD) array spectrometers, photomultiplier tubes (PMTs) and phototube (PT) are investigated. An argon plasma provided better performance than a nitrogen plasma. With approximately 0.88 standard liters per min sampling rate and preconcentration for 2min, the estimated (S/N=3) detection limit was 0.12ng/L (Hg(0)), the linear range extended at least to 6.6ngHg/L. Typical RSD values for determination at the single digit ng/L level ranged from 2.8 to 4.9%. In 19 separate calibrations conducted over 7 days, the calibration slope had a standard error of 1%. The system was applied to the determination of atmospheric mercury in two different locations.

Synthesis of MPTS-modified cobalt ferrite nanoparticles and their adsorption properties in relation to Au(III).

Cobalt ferrite magnetic nanoparticles (Co-MNP) were prepared by a co-precipitation method and subsequently coated with (3-mercaptopropyl)trimethoxysilane (MPTS) for the extraction and recovery of Au(III) from aqueous chloride solutions. Physical characterization of the MPTS-modified particles (Co-MPTS) was performed using FT-IR, TGA, and SEM. Results from FT-IR confirmed that MPTS was present on the surface of the magnetic nanoparticles. The amount of MPTS was 0.36 mmol g(-1) of Co-MPTS, obtained by elemental analysis. SEM images revealed aggregates composed of nanocrystalline Co-MPTS particles. The extraction efficiency as a function of the pH, contact time, and initial Au(III) concentration was evaluated. The modified particles showed maximum adsorption in the pH range from 1.0 to 4.0. The adsorption behavior of Co-MPTS toward Au(III) followed a Langmuir isotherm and the maximum adsorption capacity was found to be 120.5 mg g(-1). The stability of the modified materials was improved as compared to that of bare Co-MNP. The subsequent desorption of gold could be achieved by using acidified thiourea solution; the highest gold recovery reached 85%.

Preparation and use of chemically modified MCM-41 and silica gel as selective adsorbents for Hg(II) ions.

Adsorbents for Hg(II) ion extraction were prepared using amorphous silica gel and ordered MCM-41. Grafting with 2-(3-(2-aminoethylthio)propylthio)ethanamine was used to functionalize the silica. The functionalized adsorbents were characterized by nitrogen adsorption, X-ray diffraction, 13C MAS NMR spectroscopy and thermogravimetric analysis. The adsorption properties of the modified silica gel and MCM-41 were compared using batch method. The effect of pH, stirring time, ionic strength and foreign ions were studied. The extraction of Hg(II) ions occurred rapidly with the modified MCM-41 and the optimal pH range for the extraction by the modified materials was pH 4-7. Foreign ions, especially Cl- had some effect on the extraction efficiency of the modified silica gel and the modified MCM-41. The adsorption behavior of both adsorbents could be described by a Langmuir model at 298 K, and the maximum adsorption capacity of the modified silica gel and MCM-41 at pH 3 was 0.79 and 0.70 mmol g(-1), respectively. The modified MCM-41 showed a larger Langmuir constant than that of the modified silica gel, indicating a better ability for Hg(II) ion adsorption. The results indicate that the structure of the materials affects the adsorption behavior. These materials show a potential for the application as effective and selective adsorbents for Hg(II) removal from water.

Reuse of waste silica as adsorbent for metal removal by iron oxide modification.

Silica gel is widely used in research laboratories, especially for the purification of organic compounds. Consequently, waste silica gel is generated in increasing amounts. In this work, waste silica was modified by coating its surface with iron oxide aiming to obtain an effective adsorbent for metal removal from wastewater. In the preparation of the adsorbent, the optimal pretreatment temperature and iron concentration were investigated. The coated waste silica was characterized for BET surface area, pore size, specific pore volume and iron content. Iron oxide-coated waste silica was tested for the adsorption of Pb(II), Cu(II), Cd(II) and Ni(II) from solutions in a batch system. The effect of contact time, pH and salt concentration on metal adsorption was investigated. It was found that the adsorption of metals occurred rapidly and reached equilibrium within 30 min. The pH suitable for metal adsorption was between 6 and 7 and leaching of iron from the coating was observed only at pH 3 or lower. The presence of salt reduced the adsorption efficiency of the adsorbent. The adsorption behavior followed both Langmuir and Freundlich isotherms (25 degrees C). Finally, the efficacy of the adsorbents was investigated using aqueous lab waste where removal efficiencies ranging from 62 to 89% were achieved when the initial metal concentrations ranged from 13 to 42 mg L(-1).

Multi-element preconcentration of heavy metal ions from aqueous solution by APDC impregnated activated carbon.

Ammonium pyrrolidinedithiocarbamate impregnated activated carbon (APDC-AC) has been used for the preconcentration of Cd(II), Cu(II), Ni(II), and Zn(II) from aqueous solution by column solid phase extraction (SPE) technique. Trace metal ions in aqueous solution were quantitatively sorbed onto APDC-AC packed in a SPE column at pH 5.0 with a flow rate of 1.0mLmin(-1). The sorbed metals were eluted with 1M nitric acid in acetone solution at a flow rate of 0.6mLmin(-1) and analyzed by flame atomic absorption spectrometry. The effects of sample volume, amount of APDC-AC, volume of eluent and ionic strength of working solution on metal ion recovery have been investigated. The present methodology gave recoveries from 90 to 106% and R.S.D. from 0.6 to 5.5%.