Gold leaf electrochemical flow cell for determination of iodide in nuclear emergency tablets.

This work introduces an innovative gold-leaf flow cell for electrochemical detection in flow injection (FI) analysis. The flow cell incorporates a hammered custom gold leaf electrochemical sensor. Hammered gold leaves consist of pure gold and are readily available in Thailand at affordable prices (approximately $0.085 for a sheet measuring 40 mm × 40 mm). Four sensing devices can be made from a single sheet of this gold leaf, resulting in a production cost of approximately $0.19 per sensor. Each electrochemical sensor has the gold leaf as the working electrode, together with a printed carbon strip, and a printed silver/silver chloride strip as the counter and reference electrodes, respectively. Initial investigations using cyclic voltammetry of a standard 1000 µmol L⁻1 iodide solution in 60 mmol L⁻1 phosphate buffer (PB) solution at pH 5, demonstrated performance comparable to that of a commercial screen-printed gold electrode. The hammered gold leaf electrode was then installed in a commercial flow cell as part of an FI system. A sample or standard iodide solution (100 µL) is injected into the first carrier stream of phosphate buffer (PB) solution, which then merges to mix with the second stream of the same buffer solution before flowing into the flow cell for amperometric detection of iodide. The optimized operating conditions include a fixed potential of +0.39 V (vs Ag/AgCl), and a total flow rate of 3 mL min⁻1. A linear calibration is obtained in the concentration range of 1 to 1000 µmol L⁻1 I- with a typical equation of µA = (0.00299 ± 0.00004) × (µmol L-1 I-) + (0.021 ± 0.020), and R2 = 0.9994. Analysis of iodide using this gold leaf-FI system is rapid with sample throughput of 86 samples h⁻1 and %RSD of a sample of 100 µmol L⁻1 I⁻ of 1.2 (n = 29). The limit of detection, (calculated as 2.78 × SD of regression line/slope), is 27 µmol L⁻1 I-. This method was successfully applied to determine iodide in nuclear emergency tablets.

Determination of promethazine in forensic samples using multi-walled carbon nanotube-gold nanoparticle electrochemical sensor.

An electrochemical sensor was developed based on a glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNTs) and gold nanoparticles (AuNPs) for the determination of promethazine (PMZ) in 'purple drank', pharmaceutical formulations, and synthetic saliva. The oxidation of PMZ at the modified electrode occurred at a higher cathodic potential and produced a higher sensitivity compared to the unmodified GCE. The morphology of the modified electrode was characterized using field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The presence of MWCNTs and AuNPs was confirmed. The optimized parameters included the concentration and pH of the supporting electrolyte, amount of modifiers used to fabricate the electrode, deposition potential, and time. Using these optimized conditions, the method has a linear range from 0.5 to 100 µmol L-1, with a R2 value of 0.9991. The limit of detection (3SDblank/slope) was 0.13 µmol L-1. The proposed electrochemical sensor was successfully applied for the determination of PMZ in 'purple drank', pharmaceutical formulations, and spiked synthetic saliva samples. The results obtained from this sensor were in statistical agreement with the values obtained using the reference gas chromatography-flame ionization method.

Smart dual imprinted Origami 3D-ePAD for selective and simultaneous analysis of vanillylmandelic acid and 5-hydroxyindole-3-acetic acid carcinoid cancer biomarkers using graphene quantum dots coated with dual molecularly imprinted polymers.

Measuring the levels of the biomarkers vanillylmandelic acid (VMA) and 5-Hydroxyindole-3-acetic acid (5-HIAA) is a valuable tool for clinical diagnosis not only of neuroblastoma or carcinoid syndrome, but also of essential hypertension, depression, migraine, and Tourette's syndrome. Herein, we explore using graphene quantum dots (GQDs) coated with molecularly imprinted polymer (MIP) as novel dual-imprinted sensors for selective and simultaneous determination of VMA and 5-HIAA in urine and plasma samples. The dual-MIP was successfully coated on the GQDs core via co-polymerization of (3-aminopropyl) triethoxysilane (APTES) and tetraethyl orthosilicate (TEOS), acting as functional and cross-linking monomers, respectively. In addition, we successfully created the dual imprinted VMA and 5-HIAA shell on the GQDs' core via a one-pot synthesis. We fabricated a facile and ready-to-use Origami three-dimensional electrochemical paper-based analytical device (Origami 3D-ePAD) for simultaneous determination of VMA and 5-HIAA using a GQDs@dual-MIP modified graphene electrode (GQDs@dual-MIP/SPGE). The Origami 3D-ePAD was designed to form a voltammetric cell on a three-layer foldable sheet with several advantages. For example, they were quickly assembled and enhanced the device's physical durability with the hydrophobic backup sheet. The developed dual imprinted Origami 3D-ePAD leads to substantially enhanced sensitivity and selectivity to electrochemical signal amplification generated from increasing the electrode-specific surface area, electrocatalytic activity, and the large numbers of dual imprinted sites for VMA and 5-HIAA detection. The synthetic recognition sites are highly selective for 5-HIAA and VMA molecules with an imprinting factor of 8.46 and 7.10, respectively. Quantitative analysis relying on square wave voltammetry reveals excellent linear dynamic ranges of around 0.001-25 µM, with detection limits of 0.023 nM for 5-HIAA and 0.047 nM for VMA (3Sb, n = 3). The Origami 3D-ePAD provides high accuracy and precision (i.e., recovery values of 5-HIAA ranged from 82.98 to 98.40 %, and VMA ranged from 83.28 to 104.39 %), and RSD less than 4.37 %) in urine and plasma samples without any evidence of interference. Hence, it is well suited as a facile and ready-to-use disposable device for point-of-care testing. It is straightforward, cost-effective, reproducible, and stable. Furthermore, it allows for rapid analysis (analysis time ∼20s) useful in medical diagnosis and other relevant fields.

Exploitations of Schiff's test and iodoform test for an effective quality assessment of alcohol-based hand sanitizers.

In the period of the corona virus disease 2019 (COVID-19) outbreak, an alcohol-based hand sanitizer is one of the most in-demand products for disinfection purposes. Two major concerns are adulteration of methanol, which causes toxicity to human health, and the concentration of legal alcohol in hand sanitizers due to their effect on antivirus. In this work, the first report of the entire quality assessment of alcohol-based hand sanitizers in terms of detection of methanol adulteration and quantification of ethanol is presented. Detection of adulterated methanol is carried out based on Schiff's reagent after the oxidation of methanol to formaldehyde, giving a bluish-purple solution to detect at 591 nm. In cases where a colorless solution is observed, an iodoform reaction with turbidimetric detection is then performed for quantitative analysis of legal alcohol (ethanol or isopropanol). To comply with the regulation of quality assessment of alcohol-based hand sanitizers, a regulation chart with four safety zones is also presented, employing a combination of two developed tests. The coordinates of a point (x, y) obtained from the two tests are extrapolated to the safety zone in the regulation chart. The regulation chart also showed consistency of analytical results as compared with the gas chromatography-flame ionization detector.

Transparent Cross-Flow Platform as Chemiluminescence Detection Cell in Cross Injection Analysis.

This work presents the use of a transparent 'Cross Injection Analysis' (CIA) platform as a flow system for chemiluminescence (CL) measurements. The CL-CIA flow device incorporates introduction channels for samples and reagents, and the reaction and detection channels are in one acrylic unit. A photomultiplier tube placed above the reaction channel detects the emitted luminescence. The system was applied to the analysis of (i) Co(II) via the Co(II)-catalyzed H2O2-luminol reaction and (ii) paracetamol via its inhibitory effect on the catalytic activity of Fe(CN)63- on the H2O2-luminol reaction. A linear calibration was obtained for Co(II) in the range of 0.002 to 0.025 mg L-1 Co(II) (r2 = 0.9977) for the determination of Co(II) in water samples. The linear calibration obtained for the paracetamol was 10 to 200 mg L-1 (r2 = 0.9906) for the determination of pharmaceutical products. The sample throughput was 60 samples h-1. The precision was ≤4.2% RSD. The consumption of the samples and reagents was ca. 170 µL per analysis cycle.

Origami 3D-microfluidic paper-based analytical device for detecting carbaryl using mesoporous silica-platinum nanoparticles with a molecularly imprinted polymer shell.

Herein, we present a novel Origami 3D-µPAD for colorimetric carbaryl detection using a super-efficient catalyst, namely mesoporous silica-platinum nanoparticles coated with a molecularly imprinted polymer (MSN-PtNPs@MIP). Morphological and structural characterization reveals that coating MIP on the MSN-PtNPs surface significantly increases the selective area, leading to larger numbers of imprinting sites for improved sensitivity and selectivity in determining carbaryl. The as-prepared MSN-PtNPs@MIP was used for catalytic oxidation of 3,3',5,5'-tetramethylbenzidine (TMB) by H2O2. Carbaryl selectively binds to the cavities embedded on the MSN-PtNPs surface and subsequently inhibits TMB oxidation leading the color to change to light blue. The change of reaction color from dark blue to light blue depends on the concentration of carbaryl within the 3D-µPAD detection zone. This design integrates the advantages of highly efficient sample delivery through micro channels (top layer) and efficient partition/separation paths (bottom layer) of the cellulose substrate to achieve both improved detection sensitivity and selectivity. Assay on the Origami 3D-µPAD can determine carbaryl by ImageJ detection, over a dynamic range of 0.002-20.00 mg kg-1, with a very low limit of detection at 1.5 ng g-1. The developed 3D-µPAD exhibit high accuracy when applied to detect carbaryl in fruits, with satisfactory recoveries from 90.1% to 104.0% and relative differences from the reference HPLC values less than 5.0%. Furthermore, the fabricated Origami 3D-µPAD provides reliable durability and good reproducibility (3.19% RSD for fifteen devices).

Facile and Compact Electrochemical Paper-Based Analytical Device for Point-of-Care Diagnostic of Dual Carcinogen Oxidative Stress Biomarkers through a Molecularly Imprinted Polymer Coated on Graphene Quantum-Dot Capped Gold.

Nanoscale imprinting significantly increases the specific surface area and recognition capabilities of a molecularly imprinted polymer by improving accessibility to analytes, binding kinetics, and template removal. Herein, we present a novel synthetic route for a dual molecularly imprinted polymer (dual-MIP) of the carcinogen oxidative stress biomarkers 3-nitrotyrosine (3-NT) and 4-nitroquinolin-N-oxide (4-NQO) as coatings on graphene quantum-dot capped gold nanoparticles (GQDs-AuNPs). The dual-MIP was successfully coated on the GQDs-AuNPs core via a (3-mercaptopropyl) trimethoxysilane (MPTMS) linkage and copolymerization with the 3-aminopropyltriethoxysilane (APTMS) functional monomer. In addition, we fabricated a facile and compact three-dimensional electrochemical paper-based analytical device (3D-ePAD) for the simultaneous determination of the dual biomarkers using a GQDs-AuNPs@dual-MIP-modified graphene electrode (GQDs-AuNPs@dual-MIP/SPGE). The developed dual-MIP device provides greatly enhanced electrochemical signal amplification due to the improved electrode-specific surface area, electrocatalytic activity, and the inclusion of large numbers of dual-imprinted sites for 3-NT and 4-NQO detection. Quantitative analysis used square wave voltammetry, with an oxidation current appearing at -0.10 V for 4-NQO and +0.78 V for 3-NT. The dual-MIP sensor revealed excellent linear dynamic ranges of 0.01 to 500 µM for 3-NT and 0.005 to 250 µM for 4-NQO, with detection limits in nanomolar levels for both biomarkers. Furthermore, the dual-MIP sensor for the simultaneous determination of 3-NT and 4-NQO provides high accuracy and precision, with no evidence of interference from urine, serum, or whole blood samples.

Determination of phosphorus in water and chemical fertilizer samples using a simple drawing microfluidic paper-based analytical device.

A simple one-step drawing for the cost-effective fabrication of microfluidic paper-based analytical devices (µPADs) for the determination of phosphate content in water and fertilizer samples is presented in this paper. The hydrophobic barrier of µPAD was patterned using a 2-mm tip marker pen using a transparent acrylic sheet template. The molybdenum blue reaction using ascorbic acid as a reducing agent was used. A pre-concentration step of samples is proposed to improve the sensitivity of the measurement. The blue complex produced on the µPADs was recorded using a smartphone camera. The color intensities (red, green, blue and gray) were analyzed using ImageJ program. The proposed µPAD method provides a linear calibration range from 0 to 100 mg L-1 P. The limit of detection (LOD) was found to be 0.7 mg L-1 P with a precision of 3.1%RSD for 50 mg L-1 P (n = 10). The proposed method was successfully applied to the determination of phosphorus contents in water and liquid chemical fertilizer samples. The results obtained from µPAD agreed with a spectrophotometric method using paired t test at a 95% confidence level.

A simple cost-effective paper-based electrochemical device for detection of adulterated sibutramine in slimming products.

This work presents the first paper-based electrochemical device, or ePAD, for direct detection of adulterated sibutramine in slimming products. The ePAD was fabricated using a screen-printing technique for defining the hydrophilic area for sample loading and for the working, reference and counter electrodes. The ePAD gave reproducible responses comparable to both conventional rod electrodes and commercial screen-printed electrodes (SPEs). Use of paper to fabricate the ePAD device provides advantages over the conventional SPE platforms (e.g. glass, ceramics and polymers) in terms of biocompatibility, strong capillary action and environmental friendliness. To detect sibutramine, square wave voltammetry was employed after sample loading on the circular hydrophilic area. The linear range is 2.51 to 83.7 mg L-1 sibutramine, with a precision of 6 %RSD (n = 3) and an instrumental limit of detection (3SD of intercept/slope) of 2.46 mg L-1 sibutramine. Recovery of spiked samples ranged from 83 to 116%. The samples were capsules, slimming coffee powders and nutraceutical beverages. The samples were appropriately diluted to give concentrations within the linear calibration range. Filtration of undissolved solids found with the capsules and coffee powder samples was not required, demonstrating that the method is not susceptible to solid particles. The ePAD is cost-effective (

Disposable Microchamber with a Microfluidic Paper-Based Lid for Generation and Membrane Separation of SO2 Gas Employing an In Situ Electrochemical Gas Sensor for Quantifying Sulfite in Wine.

This work presents a fully disposable microchamber for gas generation of a sample solution. The microchamber consists of a cylindrical well-reactor and a paper-based microfluidic lid (µFluidic lid), which also serves as the reagent loading and dispensing unit. The base of the reactor consists of a hydrophobic membrane covering an in-house graphene electrochemical gas sensor. Fabrication of the gas sensor and the three-layer µFluidic lid is described. The µFluidic lid is designed to provide a steady addition of the acid reagent into the sample solution instead of liquid drops from a disposable syringe. There are three steps in the procedure: (i) acidification of the sample in the reactor to generate SO2 gas by the slow dispensing of the acid reagent from the µFluidic lid, (ii) diffusion of the liberated SO2 gas through the hydrophobic membrane at the base of the reactor, and (iii) in situ detection of SO2 by cathodic reduction at the graphene electrode. The device was demonstrated for quantitation of the sulfite preservative in wine without heating or stirring. The selectivity of the analysis is ensured by the combination of the gas-diffusion membrane and the selectivity of the electrochemical sensor. The linear working range is 2-60 mg L-1 SO2, with a limit of detection (3SD of intercept/slope) of 1.5 mg L-1 SO2. This in situ method has the shortest analysis time (8 min per sample) among all voltammetric methods that detect SO2(g) via membrane gas diffusion.

An application study of membraneless-gas separation microfluidic paper-based analytical device for monitoring total ammonia in fish pond water using natural reagent.

The membraneless-gas separation microfluidic paper-based analytical device (ML-GS µPAD), consisting of donor, spacer, and acceptor layers, was developed to monitor total ammonia in fish pond water. The principle of the analysis involved the addition of sodium hydroxide solution to the sample zone in the donor layer containing ammonia/ammonium, and the produced ammonia gas diffuses through the spacer to the detection zone in the acceptor layer containing red rose extract to produce a color change from pink to blue corresponding to the ammonia/ammonium concentration. Under optimum conditions, the proposed method provided good linearity of ammonia in the range concentration of 0-100 mg L-1 (R2 = 0.9993) with LOD and LOQ of 2.25 and 7.51 mg L-1, respectively. This method was successfully applied to fish pond water samples without significant influence of interfering compounds with recoveries in the range of 103-110%, indicating good selectivity and accuracy of the proposed method.

Smart sensor for assessment of oxidative/nitrative stress biomarkers using a dual-imprinted electrochemical paper-based analytical device.

We present a novel dual-imprinted electrochemical paper-based analytical device (Di-ePAD) to simultaneously determine 8-hydroxy-2'-deoxyguanosine (8-OHdG) and 3-nitrotyrosine (3-NT) and assess oxidative and nitrative biomarkers in urine and plasma samples. The Di-ePAD was designed with hydrophobic barrier layers formed on filter paper to provide three-dimensional circular reservoirs and assembled electrodes. The molecularly imprinted polymer (MIP) was synthesized using a silica nanosphere decorated with silver nanoparticles (SiO2@AgNPs) as a core covered with dual-analyte imprinted sites on the polymer to recognize selectively and bind the target biomarkers. This strategy drives monodispersity and enhances the conductivity of the resulting MIP core-shell products. 3-NT-MIP and 8-OHdG-MIP were synthesized by successively coating the surface of SiO2@AgNPs with l-Cysteine via the thiol group, then terminating with MIP shells. The dual imprinted core-shell composites possess attractive properties for the target biomarkers' sensing, including catalytic activity, selectivity, and good conductivity. The Di-ePAD revealed excellent linear dynamic ranges of 0.01-500 µM for 3-NT and 0.05-500 µM for 8-OHdG, with detection limits of 0.0027 µM for 3-NT and 0.0138 µM for 8-OHdG. This newly developed method based on the synergistic effects of SiO2@AgNPs combined with promising properties of MIP offers outstanding selectivity, sensitivity, reproducibility, simplicity, and low cost for quantitative analysis of 3-NT and 8-OHdG. The proposed Di-ePAD showed good accuracy and precision when applied to actual samples, including urine and serum samples validated by a conventional HPLC method.

Simple gunshot residue analyses for estimating firing distance: Investigation with four types of fabrics.

This work presents two simple methods for estimating the firing distance from the gunshot residues (GSRs) on fabric targets. Four types of fabric targets, namely twill weave denim cotton-polyester (80/20), jersey knitting 100% cotton, plain weave cotton-polyester (80/20) and plain weave cotton-polyester (60/40), were employed. The firing tests were carried out using these white fabrics as targets at distances of 5-100 cm, respectively. In the first method, digital images of the black GSRs on fabric materials were recorded inside an illuminated box and the inverted gray intensity values were plotted against the firing distances. Since the plots of all fabrics are not significantly different, the estimation of firing distance employs the same exponential curve for all test fabrics. Although simple, the imaging method is not suitable for dark-colored materials. A chemical-based method was therefore developed as an alternative method. In the second method, a small disposable microfluidic paper-based analytical device (µPAD) was employed for detecting Pb(II) extracted from the GSRs. The µPAD method uses the measurement of the length of a narrow band of a pink color resulting from reaction between rhodizonate reagent and the Pb(II) extract. The plots indicated that the data of thick denim material are significantly different to other test fabrics which are much thinner. These three fabrics share the same estimation curve. However, it is recommended that the separate estimation curve for denim materials must be used. Both methods are suitable for short range firing distance, no further than 60 cm, since at greater distances the inverted gray intensity and the 'band-length' methods are unable to detect the GSRs.

Simple and Equipment-Free Paper-Based Device for Determination of Mercury in Contaminated Soil.

This work presents a simple and innovative protocol employing a microfluidic paper-based analytical device (µPAD) for equipment-free determination of mercury. In this method, mercury (II) forms an ionic-association complex of tetraiodomercurate (II) ion (HgI42-(aq)) using a known excess amount of iodide. The residual iodide flows by capillary action into a second region of the paper where it is converted to iodine by pre-deposited iodate to liberate I2(g) under acidic condition. Iodine vapor diffuses across the spacer region of the µPAD to form a purple colored of tri-iodide starch complex in a detection zone located in a separate layer of the µPAD. The digital image of the complex is analyzed using ImageJ software. The method has a linear calibration range of 50-350 mg L-1 Hg with the detection limit of 20 mg L-1. The method was successfully applied to the determination of mercury in contaminated soil and water samples which the results agreed well with the ICP-MS method. Three soil samples were highly contaminated with mercury above the acceptable WHO limits (0.05 mg kg-1). To the best of our knowledge, this is the first colorimetric µPAD method that is applicable for soil samples including mercury contaminated soils from gold mining areas.

Gold leaf electrochemical sensors: applications and nanostructure modification.

This work presents the first planar three-electrode electrochemical sensor comprising local gold leaf as the working electrode and printed, or hand-drawn, counter and reference electrodes, respectively. The gold leaf was mounted on a polyvinyl chloride (PVC) adhesive sheet (15 mm × 30 mm) and covered with a second PVC sheet printed with the counter and reference electrodes. This sheet has a 3 mm circle and a 2 mm × 3 mm rectangle removed to expose the gold electrode area and electrical contacts, respectively. A third shorter insulating layer with a 10 mm circular hole was placed on top to delineate the sensing area of all electrodes. The sensor displayed expected performances in various modes of operation, such as cyclic voltammetry, square wave voltammetry and anodic stripping voltammetry. For the latter mode, the limit of detection of Pb(ii) was 3.2 µg L-1, compliant with regulation for drinking water (10 µg L-1 Pb(ii)). Although designed as a disposable unit, the electrode is effective for up to 200 cycles and applicable for multiple use. The gold leaf was modified by electrodeposition of the gold network and large nano-size gold particles which significantly enhanced the sensitivity of all voltametric sensing, giving lower limits of detection. For stripping voltammetry, the electroplating structure modification improved the simultaneous detection of lead and copper, with the copper response increasing 6-fold. The device has the capability of on-site identification of copper/lead bullets from gunshot residues within 6 min.

Rapid detection of Clostridium perfringens in food by loop-mediated isothermal amplification combined with a lateral flow biosensor.

Clostridium perfringens is a key anaerobic pathogen causing food poisoning. Definitive detection by standard culture method is time-consuming and labor intensive. Current rapid commercial test kits are prohibitively expensive. It is thus necessary to develop rapid and cost-effective detection tool. Here, loop-mediated isothermal amplification (LAMP) in combination with a lateral-flow biosensor (LFB) was developed for visual inspection of C. perfringens-specific cpa gene. The specificity of the developed test was evaluated against 40 C. perfringens and 35 other bacterial strains, which showed no cross-reactivity, indicating 100% inclusivity and exclusivity. LAMP-LFB detection limit for artificially contaminated samples after enrichment for 16 h was 1-10 CFU/g sample, which was comparable to the commercial real-time PCR kit. The detection performance of LAMP-LFB was also compared to culture-based method using 95 food samples, which revealed the sensitivity (SE), specificity (SP) and Cohen's kappa coefficient (κ) of 88.0% (95% CI, 75.6%-95.4%), 95.5% (95% CI, 84.8%-99.4%) and 0.832 (95% CI, 0.721-0.943), respectively. Area under the receiver operating characteristic (ROC) curve was 0.918 (95% CI, 0.854-0.981), indicating LAMP-LFB as high relative accuracy test. In conclusion, LAMP-LFB assay is a low-cost qualitative method and easily available for routine detection of C. perfringens in food samples, which could serve as an alternative to commercial test kit.

Simple Flow-Based System with an In-Line Membrane Gas-liquid Separation Unit and a Contactless Conductivity Detector for the Direct Determination of Sulfite in Clear and Turbid Food Samples.

This study presents a simple flow-based system for the determination of the preservative agent sulfite in food and beverages. The standard method of conversion of sulfite ions into SO2 gas by acidification is employed to separate the sulfite from sample matrices. The sample is aspirated into a donor stream of sulfuric acid. A membrane gas-liquid separation unit, also called a 'gas-diffusion (GD)' unit, incorporating a polytetrafluoroethylene (PTFE) hydrophobic membrane allows the generated gas to diffuse into a stream of deionized water in the acceptor line. The dissolution of the SO2 gas leads to a change in the conductivity of water which is monitored by an in-line capacitively coupled contactless conductivity detector (C4D). The conductivity change is proportional to the concentration of sulfite in the sample. In this work, both clear (wine) and turbid (fruit juice and extracts of dried fruit) were selected to demonstrate the versatility of the developed method. The method can tolerate turbidity up to 60 Nephelometric Turbidity Units (NTUs). The linear range is 5-25 mg L-1 SO32- with precision < 2% RSD. The flow system employs a peristaltic pump for propelling all liquid lines. Quantitative results of sulfite were statistically comparable to those obtained from iodimetric titration for the wine samples.

Dual-Purpose Photometric-Conductivity Detector for Simultaneous and Sequential Measurements in Flow Analysis.

This work presents a new dual-purpose detector for photometric and conductivity measurements in flow-based analysis. The photometric detector is a paired emitter-detector diode (PEDD) device, whilst the conductivity detection employs a capacitively coupled contactless conductivity detector (C4D). The flow-through detection cell is a rectangular acrylic block (ca. 2 × 2 × 1.5 cm) with cylindrical channels in Z-configuration. For the PEDD detector, the LED light source and detector are installed inside the acrylic block. The two electrodes of the C4D are silver conducting ink painted on the PEEK inlet and outlet tubing of the Z-flow cell. The dual-purpose detector is coupled with a sequential injection analysis (SIA) system for simultaneous detection of the absorbance of the orange dye and conductivity of the dissolved oral rehydration salt powder. The detector was also used for sequential measurements of creatinine and the conductivity of human urine samples. The creatinine analysis is based on colorimetric detection of the Jaffé reaction using the PEDD detector, and the conductivity of the urine, as measured by the C4D detector, is expressed in millisiemens (mS cm-1).

Contactless conductivity sensor employing moist paper as absorbent for in-situ detection of generated carbon dioxide gas.

This work presents an unconventional use of capacitively coupled contactless conductivity detector (C4D) for detection of gas absorption by moist paper with potential application for chemical analysis. To be suitable for measuring conductivity of moist paper absorbent, the C4D sensor was therefore designed in planar configuration. A layer of dry filter paper, only 20 mm × 25 mm in size, was placed on the C4D sensor and the device installed inside a specifically designed vaporization chamber. A vial (16 mm i.d., 8 mm high) containing a 150-µL solution of sodium bicarbonate was placed alongside. The filter paper was loaded with 110 µL of deionized water through an injection hole in the cover lid. A 100-µL aliquot of 2 M hydrochloric acid solution was directly dispensed into the vial through a second hole in the lid to generate CO2 gas from the bicarbonate solution. It was observed that the C4D sensor gave real-time response that corresponded to the absorption of the gas and subsequent production of H+ and HCO3- in the moist paper. The monitored signal reached a constant value at 160 s after the addition of the acid. Chemistry of the absorption process and equivalent circuit for the C4D are proposed. Direct measurement of cement powder was chosen to demonstrate the potential use of this device for quantifying the CaCO3 content of the cement. The calibration curve for 0.5-3 mg CaCO3 was linear for signals recorded at 160 s: Vdc = (0.172 ± 0.005) · (mg CaCO3) + (0.016 ± 0.009), with coefficient of determination of 0.9965. Linear calibrations were also observed when the signals were monitored at various time less than 160 s. The limit of quantitation (3 SD of intercept/slope) was 0.17 mg CaCO3. The method provided acceptable precision with %RSD of 4.6 (2 mg CaCO3, n = 10).

Micro-PAD card for measuring total ammonia nitrogen in saliva.

This work presents a portable microfluidic paper-based analytical device (micro-PAD) card for the quantification of total ammonia nitrogen in human saliva. The amount of total ammonia nitrogen in saliva can be an indicator of the status of the oral microbiome with potential correlation to kidney health problems. The developed micro-PAD card comprises twenty units consisting of three stacked layers of circular discs: the sample layer, paper discs impregnated with sodium hydroxide solution, the PTFE membrane layer, and the detection layer, paper discs impregnated with bromothymol blue. The twenty units were aligned on transparent laminating pouches laminated to form the micro-PAD card (7.5 cm × 10.5 cm). Saliva samples can be directly dispensed onto the micro-PAD card and the detection was achieved by the BTB indicator color change, from yellow to blue, after conversion of ammonium into ammonia and diffusion of the ammonia gas through a hydrophobic layer. The determination of total ammonia nitrogen in saliva using the developed micro-PAD card intended to be very simple method and operated without the need of laboratory equipment. A quantification limit of 11.3 NH4+mg L-1 and linear application range from up to 150 NH4+mg L-1 were obtained making it suitable for the expected concentrations of total ammonia nitrogen in human saliva. It was successfully applied to saliva samples and its validation obtained by comparison against a potentiometric method. The card is stable for at least 1 month making it ideal as a portable device for point-of-care diagnosis. Graphical Abstract.