We have demonstrated a PM2.5 analysis method that adds information on the number concentration and size by using microfluidic-based ionic current sensing with a bridge circuit. The bridge circuit allows for suppression of the background current and the detection of small PM2.5 particles, even if a relatively large micropore is used. This is the first demonstration of the detection of PM2.5 particles via ionic current sensing; our method enables analyses of both the number concentration and size.
HPLC-FTIR analysis using a novel apparatus with CuO powder as an interface is reported. This apparatus initially serves as a reservoir for the dilute eluted solution of HPLC, and then acts as an enrichment device by combining diffusion and evaporation processes. It can be used not only to effectively remove the mobile phase of the eluted solution, but also to enrich the analyte within a tiny spatially resolved separated sample spot whose size is suitable for obtaining spectra using an FTIR microscope. An experimental demonstration using benzamide and sodium dodecyl benzene sulfonate shows that this apparatus is readily applicable in the analysis of real-world mixture samples.
In an effort to elucidate the deposition pathway of Pd in river sediments, we analyzed the amount of Pd in the river water and sediments of the Yukawa and Yazawa rivers, as well as in the sediments of the Shinaki dam-lake of the Kusatsu hot-spring area, which is located northwest in Gunma Prefecture of Japan. The crystal structures and elemental compositions of the river sediment samples differed significantly before and after neutralization. This was attributed to the lime input, which also affected the Pd abundance ratio obtained by the sequential extraction procedure. Additionally, the low leachability of Pd in the sediment suggested possible difficulties in its recovery. Considering the analysis of the Pd variation in the environments, it was concluded that the Pd content in the sediment of the Shinaki dam-lake was mainly supplied by the Yukawa river water inflowing the surrounding tributary rivers and hot-spring waters before neutralization, rather than the lime input.
The effect of long-time heating for elements from flame retardants (FRs) such as dechlorane plus (DP), tetrabromobisphenol A (TBBPA), triphenyl phosphate (TPhP) and antimony trioxide (Sb2O3) in both acrylonitrile-butadiene-styrene (ABS) and polycarbonate (PC) resin disks was examined in the present study. The heating temperature by a drying oven was 80°C, which was expected to be a harder environment than that of usual dump site to discard electric and electronic equipment, and the long-time heating was carried out for up to 722 days. As a result, the increases for both ether (C–O–C) and ketone (C=O) groups and the decrease of C=C double bond as well as methylene group (=CH2) were found for an ABS resin disk by fourier transform infrared (FTIR) spectrometry, which was expected to result in an increase of mass of the disk up to ca. 4% due to oxidation during the long-time heating. The changes in concentrations for bromine (Br), chlorine (Cl), phosphorous (P) and Sb, which were originated elements from FRs contained, were also evaluated by energy dispersive X-ray fluorescence (ED-XRF) spectrometry and the decreases in concentrations of ca. 5% in ABS resin disk were observed which could be almost explained by increasing ca. 4% mass of the disk. On the contrary, the mass and chemical form of a PC resin disk as well as the concentrations of elements contained did not change during the long-time heating. From these results, it could be considered that most of the elements from DP, TBBPA, TPhP and Sb2O3 contained as FRs in the ABS and PC resin disks examined in the present study were not lost during the long-time heating, even though the color, shape, mass and chemical form of ABS resin disk were changed.
A liquid-membrane type nitrate-selective electrode was constructed, in which the responding membrane contained polyvinylchloride, o-nitrophenyloctylether and tetraheptylammonium nitrate. The NO3−-selective electrode displayed a linear response to the concentration of NO3− with a Nernstian slope of −53.3 ± 1.0 mV decade−1, in the 10−5 – 10−1 mol dm−3 (M) NO3− concentration range. The NO3− detection limit was about 10−6 M. The electrochemical response of this electrode was stable for more than 30 days. Measurements performed using the NO3−-sensor indicated that in the presence of green plants, the concentration of NO3− in a hydroponic solution decreased from 0.20 to 0.05 mM over a three-day period.
A new type of fluorescent coordination polymer (NCPCd) based on disulfide carboxylate ligand was prepared by using one-pot synthesis for sensitive detection of reactive oxygen species (ROS). With the reaction between NCPCd and ROS, the morphology of the NCPCd was transformed from nanorods to hexagon particles, then broken into nano-fragments. Meanwhile, the fluorescence of NCPCd (at 421 nm) was quenched accordingly. For designing the highly sensitive probe for ROS, Rhodamine 6G (R6G) was doped in NCPCd. In the presence of ROS, the fluorescence of NCPCd moiety at 421 nm was quenched, but the R6G moiety was released from the broken nanorods and the fluorescence at 555 nm from R6G moiety was recovered. The R6G doped NCPCd (NCPCd-R) can be used as a highly sensitive and selective probe for hydrogen peroxide (H2O2) with detection limit of 12.4 nM. Moreover, the NCPCd-R was further extended to the glucose sensing combined with glucose oxidase (GOx) to oxidate glucose and generate H2O2, demonstrating the potential for practical applications.
In this work, sodium dodecyl benzene sulfonate (SDBS) was used as a dispersing agent; a WO3 nanoparticle suspension was used as a sensing material. The SDBS-WO3 thin film/Sn-doped glass optical waveguide sensor element was prepared by spin coating. The sensing material was characterized by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and field-emission scanning electron microscopy (FESEM). The gas-sensing characteristics of the fabricated sensors were studied at room temperature for various gases. The experimental results indicate that the sensor exhibited a high selective response toward SO2 and H2S and a low detection limit of 10 ppb to SO2 and H2S. The response/recovery times for SO2 and H2S were 2/23 and 2/18 s. However, during an electrochemical gas-sensing performance test of the SDBS-WO3 film at room temperature, the results indicated that the trend of the variation in resistance was consistent with the variation in the output light.
Adsorption of protein molecules into the pores of a porous material is an important process for chromatographic separation of proteins and synthesis of nanoscale biocatalyst systems; however, there are barriers to developing a method for analyzing the process quantitatively. The purpose of this study is to examine the applicability of differential scanning calorimetry (DSC) for quantitative analysis of protein adsorption into silica mesopores. For this purpose myoglobin, a globular protein (diameter: 35.2 Å) was selected, and its adsorption onto mesoporous silica powders with uniform pore diameters (pore diameters: 39 and 64 Å) was measured by adsorption assay and DSC experiments. Our results confirmed that the adsorption of myoglobin into the silica mesopores induced significant changes in the positions and areas of freezing/melting peaks of the pore water. The decrease in heat of fusion of the pore water after myoglobin adsorption could be utilized to quantify the amount of myoglobin inside the silica mesopores. The advantages of DSC include its applicability to small wet mesoporous silica samples.
A method is presented for the detection of a trace amount of cyanocobalamin (vitamin B12) using a combination of solid-phase extraction and the measurement of cobalt in vitamin B12 by a portable total-reflection X-ray fluorescence spectrometer. Using this combination, a detection limit of 1 ng/mL was achieved for vitamin B12.
A surface-enhanced Raman spectroscopy (SERS) based method was developed for the quantification of Cd2+ in rice. Gold nano-particles (AuNPs) modified with trimercaptotriazine served as a ratiometric SERS probe for the detection of Cd2+. A conical holed substrate was used to further enhance SERS signals, and hence to improve the sensitivity. A calibration model based on the spectral shape deformation quantitative theory was employed to mitigate the influence of variations in the number and distribution of “hot spots”. The proposed SERS method was applied to quantitative analysis of Cd2+ in three types of rice, and achieved satisfactory quantitative results with accuracy comparable to that of the reference method—inductively coupled plasma mass spectrometry. The limit of detection of the proposed method was estimated to be 8 μg kg−1. The proposed SERS method has the potential to become a fast screening method for the detection of Cd2+ in rice.
A highly selective and sensitive probe, DAC-Hg, has been designed and synthesized for the naked-eye detection of Hg2+ in practical applications. DAC-Hg showed applicative “turn-off” sensing for Hg2+ over other ions. The detection limit was determined to be 5.0 nM, the same as the strictest standard of Hg2+ measurements. A naked-eye evaluation with test strips demonstrated the potential of DAC-Hg for conveniently handled in-situ detection. The application of this established method for analyzing environmental and seafood samples supplied satisfactory results. Therefore, DAC-Hg offered a promising approach for Hg2+ detection as well as hints for sensing other heavy and transition metal ions.
Cannabis is an important industrial plant, in addition to its illicit drug use. Compound Δ9-THC (Δ9-tetrahydrocannabinol) is mainly responsible for the hallucinogenic effect on humans. The aminoalkylindole group cannabimimetics targets at the same physiological receptors to mimic the analgesic effects of Δ9-THC. Since there is no reliable colorimetric test to detect these synthetic cannabimimetics on site, a simple colorimetric assay for (aminoalkyl)indole group-containing drugs was developed, based on the silica/sulfuric acid-catalyzed Ehrlich reaction of (aminoalkyl)indoles with p-dimethylaminobenzaldehyde. The electrophilic substitution reaction of indoles with carbonyl compounds resulting in the formation of bis(indolyl)alkanes in an acid-catalyzed reaction has been used for the first time for their spectrophotometric determination by color change from yellow to purple/blue. The method was statistically validated against liquid chromatography tandem mass spectrometry, and applied to certain (aminoalkyl)indole derivatives, with 0.5 – 2.5 μg mL−1 detection limits for AM-2201, JWH-081, MAM-2201, JWH-018, JWH-210, JWH-122, 5F-PB-22 and XLR-11.
A novel fluorescent staining protocol to detect phosphoproteins in sodium dodecyl sulfate-polyacrylamide gels using a fluorescence sensor, 1-(2-hydroxy-1-naphthylazo)-2-naphthol-4-sulfonic acid sodium salt (Calcon), was developed. This method yields results within 135 min, with the sensitivities of 15 ng of α-casein and β-casein, and 62.5 ng of κ-casein, respectively. Since non-phosphoproteins have shown negative signals that are distinctly different from positive signals of phosphoproteins, this detection method allows one to monitor phosphoproteins with high specificity. Furthermore, a total protein profile can be achieved before a destaining step using a scanner with rapid and low-cost without further total protein staining.
This study investigated and proposed the use of trehalose extraction and a detection method for the determining of active sludge trehalose in sewage treatment. Seven extractants (trichloroacetic acid, ethanol, methanol, acetone, pure water, formaldehyde and trichloromethane) were used separately to extract the active sludge trehalose, and their trehalose contents were determined. The results shown in standard curves plotted for all seven extractants demonstrated good linearity, and the regression coefficients varied insignificantly. Using trichloroacetic acid, active sludge trehalose was extracted within a period of only 40 min at 40 centigrade. In view of that, trichloroacetic acid proved to be as the most efficient extractants in extracting trehalose from active sludge. Its extraction rate was 4 to 11-times faster than that of other extractants for the same amount of active sludge. From our results, trichloroacetic acid was substantiated as the optimal extractant for determining active sludge trehalose.
An ionic liquid (IL)-based microextraction method was developed for the preconcentration of paraquat traces in water samples prior to HPLC determination. On the basis of the relationship between the aqueous solubility and the extractability of known ILs, 1-ethyl-3-methylimidazolium bis(nonafluorobutanesulfonyl)amide ([EMIm][NNf2]) was selected as the extractant for paraquat. The distribution ratio of paraquat dication in the [EMIm][NNf2]/water biphasic system was theoretically estimated to be nearly 108 at its maximum level, indicating that [EMIm][NNf2] was suitable for the ultra-high preconcentration (a maximum of 106-fold concentration) of paraquat with a quantitative recovery (more than 99%). The extraction procedure could be performed easily and quickly following the in situ solvent formation microextraction technique, and the paraquat traces in the IL phase could be determined by hydrophilic interaction chromatography with good detection limits and linearity ranges (0.16 and 1 – 50 ng mL−1 for paraquat, respectively). The combined method was successfully applied to four real environmental water samples spiked with paraquat and its analog, diquat at 5.0 ng mL−1.
Micro-organic ion-associate phase (IAP) extraction was combined with a micro-volume back-extraction (MVBE) to reduce coexisting components and viscosity in the concentrates. Heavy metals were converted into a complex with 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)phenol in a 40-mL sample solution, and were extracted into ion associates. After centrifugation and discarding the aqueous phase, trace metals were stripped from IAP into a nitric acid solution, followed by GF-AAS determination. Only one vessel was required for 400-fold enrichment. The detection limits (3σb) for Cd, Ni, and Pb were 0.6, 3.7, and 0.8 ng/L, respectively. This method was applied in recovery tests in seawater.
Herein, we evaluated the quality of a double-layer coating method to stably immobilize photocatalysts by photodecomposition of dimethyl sulfoxide (DMSO) on a stainless-steel wire mesh using a flow analytical system, which included the reactor and conductimetric detector (FAS-CD). The prepared photocatalyst consisted of an amorphous titanium peroxide sol layer and a layer of a sol mixture containing TiO2 and amorphous titanium peroxide. Stable photocatalytic activity was demonstrated through successive photodecomposition tests of DMSO using FAS-CD/equipment.