Novel single-cell mega-size chambers for electrochemical etching of panorama position-sensitive polycarbonate ion image detectors

NASA Astrophysics Data System (ADS)

Sohrabi, Mehdi

2017-11-01

A novel development is made here by inventing panorama single-cell mega-size electrochemical etching (MS-ECE) chamber systems for processing panorama position-sensitive mega-size polycarbonate ion image detectors (MS-PCIDs) of potential for many neutron and ion detection applications in particular hydrogen ions or proton tracks and images detected for the first time in polycarbonates in this study. The MS-PCID is simply a large polycarbonate sheet of a desired size. The single-cell MS-ECE invented consists of two large equally sized transparent Plexiglas sheets as chamber walls holding a MS-PCID and the ECE chamber components tightly together. One wall has a large flat stainless steel electrode (dry cell) attached to it which is directly in contact with the MS-PCID and the other wall has a rod electrode with two holes to facilitate feeding and draining out the etching solution from the wet cell. A silicon rubber washer plays the role of the wet cell to hold the etchant and the electrical insulator to isolate the dry cell from the wet cell. A simple 50 Hz-HV home-made generator provides an adequate field strength through the two electrodes across the MS-ECE chamber. Two panorama single-cell MS-ECE chamber systems (circular and rectangular shapes) constructed were efficiently applied to processing the MS-PCIDs for 4π ion emission image detection of different gases in particular hydrogen ions or protons in a 3.5 kJ plasma focus device (PFD as uniquely observed by the unaided eyes). The panorama MS-PCID/MS-ECE image detection systems invented are novel with high potential for many applications in particular as applied to 4π panorama ion emission angular distribution image detection studies in PFD space, some results of which are presented and discussed.

Novel single-cell mega-size chambers for electrochemical etching of panorama position-sensitive polycarbonate ion image detectors.

PubMed

Sohrabi, Mehdi

2017-11-01

A novel development is made here by inventing panorama single-cell mega-size electrochemical etching (MS-ECE) chamber systems for processing panorama position-sensitive mega-size polycarbonate ion image detectors (MS-PCIDs) of potential for many neutron and ion detection applications in particular hydrogen ions or proton tracks and images detected for the first time in polycarbonates in this study. The MS-PCID is simply a large polycarbonate sheet of a desired size. The single-cell MS-ECE invented consists of two large equally sized transparent Plexiglas sheets as chamber walls holding a MS-PCID and the ECE chamber components tightly together. One wall has a large flat stainless steel electrode (dry cell) attached to it which is directly in contact with the MS-PCID and the other wall has a rod electrode with two holes to facilitate feeding and draining out the etching solution from the wet cell. A silicon rubber washer plays the role of the wet cell to hold the etchant and the electrical insulator to isolate the dry cell from the wet cell. A simple 50 Hz-HV home-made generator provides an adequate field strength through the two electrodes across the MS-ECE chamber. Two panorama single-cell MS-ECE chamber systems (circular and rectangular shapes) constructed were efficiently applied to processing the MS-PCIDs for 4π ion emission image detection of different gases in particular hydrogen ions or protons in a 3.5 kJ plasma focus device (PFD as uniquely observed by the unaided eyes). The panorama MS-PCID/MS-ECE image detection systems invented are novel with high potential for many applications in particular as applied to 4π panorama ion emission angular distribution image detection studies in PFD space, some results of which are presented and discussed.

Coincidence ion imaging with a fast frame camera

NASA Astrophysics Data System (ADS)

Lee, Suk Kyoung; Cudry, Fadia; Lin, Yun Fei; Lingenfelter, Steven; Winney, Alexander H.; Fan, Lin; Li, Wen

2014-12-01

A new time- and position-sensitive particle detection system based on a fast frame CMOS (complementary metal-oxide semiconductors) camera is developed for coincidence ion imaging. The system is composed of four major components: a conventional microchannel plate/phosphor screen ion imager, a fast frame CMOS camera, a single anode photomultiplier tube (PMT), and a high-speed digitizer. The system collects the positional information of ions from a fast frame camera through real-time centroiding while the arrival times are obtained from the timing signal of a PMT processed by a high-speed digitizer. Multi-hit capability is achieved by correlating the intensity of ion spots on each camera frame with the peak heights on the corresponding time-of-flight spectrum of a PMT. Efficient computer algorithms are developed to process camera frames and digitizer traces in real-time at 1 kHz laser repetition rate. We demonstrate the capability of this system by detecting a momentum-matched co-fragments pair (methyl and iodine cations) produced from strong field dissociative double ionization of methyl iodide.

Process for measuring degradation of sulfur hexafluoride in high voltage systems

DOEpatents

Sauers, Isidor

1986-01-01

This invention is a method of detecting the presence of toxic and corrosive by-products in high voltage systems produced by electrically induced degradation of SF.sub.6 insulating gas in the presence of certain impurities. It is an improvement over previous methods because it is extremely sensitive, detecting by-products present in parts per billion concentrations, and because the device employed is of a simple design and takes advantage of the by-products natural affinity for fluoride ions. The method employs an ion-molecule reaction cell in which negative ions of the by-products are produced by fluorine attachment. These ions are admitted to a negative ion mass spectrometer and identified by their spectra. This spectrometry technique is an improvement over conventional techniques because the negative ion peaks are strong and not obscured by a major ion spectra of the SF.sub.6 component as is the case in positive ion mass spectrometry.

Process for measuring degradation of sulfur hexafluoride in high voltage systems

DOEpatents

Sauers, I.

1985-04-23

This invention is a method of detecting the presence of toxic and corrosive by-products in high voltage systems produced by electrically induced degradation of SF/sub 6/ insulating gas in the presence of certain impurities. It is an improvement over previous methods because it is extremely sensitive, detecting by-products present in parts per billion concentrations, and because the device employed is of a simple design and takes advantage of the by-products natural affinity for fluoride ions. The method employs an ion-molecule reaction cell in which negative ions of the by-products are produced by fluorine attachment. These ions are admitted to a negative ion mass spectrometer and identified by their spectra. This spectrometry technique is an improvement over conventional techniques because the negative ion peaks are strong and not obscured by a major ion spectra of the SF/sub 6/ component as is the case in positive ion mass spectrometry.

Enhancement in sample collection for the detection of MDMA using a novel planar SPME (PSPME) device coupled to ion mobility spectrometry (IMS).

PubMed

Gura, Sigalit; Guerra-Diaz, Patricia; Lai, Hanh; Almirall, José R

2009-07-01

Trace detection of illicit drugs challenges the scientific community to develop improved sensitivity and selectivity in sampling and detection techniques. Ion mobility spectrometry (IMS) is one of the prominent trace detectors for illicit drugs and explosives, mostly due to its portability, high sensitivity and fast analysis. Current sampling methods for IMS rely on wiping suspected surfaces or withdrawing air through filters to collect particulates. These methods depend greatly on the particulates being bound onto surfaces or having sufficient vapour pressure to be airborne. Many of these compounds are not readily available in the headspace due to their low vapour pressure. This research presents a novel SPME device for enhanced air sampling and shows the use of optimized IMS by genetic algorithms to target volatile markers and/or odour signatures of illicit substances. The sampling method was based on unique static samplers, planar substrates coated with sol-gel polydimethyl siloxane (PDMS) nanoparticles, also known as planar solid-phase microextraction (PSPME). Due to its surface chemistry, high surface area and capacity, PSPME provides significant increases in sensitivity over conventional fibre SPME. The results show a 50-400 times increase in the detection capacity for piperonal, the odour signature of 3,4-methylenedioxymethamphetamine (MDMA). The PSPME-IMS technique was able to detect 600 ng of piperonal in a 30 s extraction from a quart-sized can containing 5 MDMA tablets, while detection using fibre SPME-IMS was not attainable. In a blind study of six cases suspected to contain varying amounts of MDMA in the tablets, PSPME-IMS successfully detected five positive cases and also produced no false positives or false negatives. One positive case had minimal amounts of MDMA resulting in a false negative response for fibre SPME-IMS.

Studies of metal ion binding by apo-metallothioneins attached onto preformed self-assembled monolayers using a highly sensitive surface plasmon resonance spectrometer

PubMed Central

Zhang, Yintang; Xu, Maotian; Wang, Yanju; Toledo, Freddy; Zhou, Feimeng

2007-01-01

The use of a flow-injection surface plasmon resonance (FI-SPR) spectrometer equipped with a bicell detector or a position-sensitive device for determining coordination of heavy metal ions (Cd2+ and Hg2+) by surface-confined apo-metallothionein (apo-MT) molecules is described. To facilitate the formation of a compact MT adsorbate layer with a uniform surface orientation, MT molecules were attached onto a preformed alkanethiol self-assembled monolayer. The method resorts to the generation of apo-MT at the surface by treating the MT-covered sensor chip with glycine–HCl and the measurement of the apo-MT conformation changes upon metal ion incorporation. Domain-specific metal ion binding processes by the apo-MT molecules were observed. Competitive replacement of one metal ion by another can be monitored in real time by FI-SPR. The tandem use of an immobilization scheme for forming a sub-monolayer of MT molecules at the sensor surface and the highly sensitive FI-SPR instrument affords a low concentration detection level. The detection level for Cd2+ (0.1 μM or 15 ppb) compares favorably with similar studies and the methodology complements to other well-established sensitive analytical techniques. The extent of metal incorporation by apo-MT molecules was also determined. PMID:18493298

High-field modulated ion-selective field-effect-transistor (FET) sensors with sensitivity higher than the ideal Nernst sensitivity.

PubMed

Chen, Yi-Ting; Sarangadharan, Indu; Sukesan, Revathi; Hseih, Ching-Yen; Lee, Geng-Yen; Chyi, Jen-Inn; Wang, Yu-Lin

2018-05-29

Lead ion selective membrane (Pb-ISM) coated AlGaN/GaN high electron mobility transistors (HEMT) was used to demonstrate a whole new methodology for ion-selective FET sensors, which can create ultra-high sensitivity (-36 mV/log [Pb 2+ ]) surpassing the limit of ideal sensitivity (-29.58 mV/log [Pb 2+ ]) in a typical Nernst equation for lead ion. The largely improved sensitivity has tremendously reduced the detection limit (10 -10  M) for several orders of magnitude of lead ion concentration compared to typical ion-selective electrode (ISE) (10 -7  M). The high sensitivity was obtained by creating a strong filed between the gate electrode and the HEMT channel. Systematical investigation was done by measuring different design of the sensor and gate bias, indicating ultra-high sensitivity and ultra-low detection limit obtained only in sufficiently strong field. Theoretical study in the sensitivity consistently agrees with the experimental finding and predicts the maximum and minimum sensitivity. The detection limit of our sensor is comparable to that of Inductively-Coupled-Plasma Mass Spectrum (ICP-MS), which also has detection limit near 10 -10  M.

Sensitive ionization of non-volatile analytes using protein solutions as spray liquid in desorption electrospray ionization mass spectrometry.

PubMed

Zhu, Zhiqiang; Han, Jing; Zhang, Yan; Zhou, Yafei; Xu, Ning; Zhang, Bo; Gu, Haiwei; Chen, Huanwen

2012-12-15

Desorption electrospray ionization (DESI) is the most popular ambient ionization technique for direct analysis of complex samples without sample pretreatment. However, for many applications, especially for trace analysis, it is of interest to improve the sensitivity of DESI-mass spectrometry (MS). In traditional DESI-MS, a mixture of methanol/water/acetic acid is usually used to generate the primary ions. In this article, dilute protein solutions were electrosprayed in the DESI method to create multiply charged primary ions for the desorption ionization of trace analytes on various surfaces (e.g., filter paper, glass, Al-foil) without any sample pretreatment. The analyte ions were then detected and structurally characterized using a LTQ XL mass spectrometer. Compared with the methanol/water/acetic acid (49:49:2, v/v/v) solution, protein solutions significantly increased the signal levels of non-volatile compounds such as benzoic acid, TNT, o-toluidine, peptide and insulin in either positive or negative ion detection mode. For all the analytes tested, the limits of detection (LODs) were reduced to about half of the original values which were obtained using traditional DESI. The results showed that the signal enhancement is highly correlated with the molecular weight of the proteins and the selected solid surfaces. The proposed DESI method is a universal strategy for rapid and sensitive detection of trace amounts of strongly bound and/or non-volatile analytes, including explosives, peptides, and proteins. The results indicate that the sensitivity of DESI can be further improved by selecting larger proteins and appropriate solid surfaces. Copyright © 2012 John Wiley & Sons, Ltd.

High-performance gas sensors with temperature measurement

PubMed Central

Zhang, Yong; Li, Shengtao; Zhang, Jingyuan; Pan, Zhigang; Min, Daomin; Li, Xin; Song, Xiaoping; Liu, Junhua

2013-01-01

There are a number of gas ionization sensors using carbon nanotubes as cathode or anode. Unfortunately, their applications are greatly limited by their multi-valued sensitivity, one output value corresponding to several measured concentration values. Here we describe a triple-electrode structure featuring two electric fields with opposite directions, which enable us to overcome the multi-valued sensitivity problem at 1 atm in a wide range of gas concentrations. We used a carbon nanotube array as the first electrode, and the two electric fields between the upper and the lower interelectrode gaps were designed to extract positive ions generated in the upper gap, hence significantly reduced positive ion bombardment on the nanotube electrode, which allowed us to maintain a high electric field near the nanotube tips, leading to a single-valued sensitivity and a long nanotube life. We have demonstrated detection of various gases and simultaneously monitoring temperature, and a potential for applications. PMID:23405281

Quaternary ammonium promoted ultra selective and sensitive fluorescence detection of fluoride ion in water and living cells.

PubMed

Li, Long; Ji, Yuzhuo; Tang, Xinjing

2014-10-21

Highly selective and sensitive fluorescent probes with a quaternary ammonium moiety have been rationally designed and developed for fast and sensitive fluorescence detection of fluoride ion (F(-) from NaF, not TBAF) in aqueous solution and living cells. With the sequestration effect of quaternary ammonium, the detection time was less than 2 min and the detection limit of fluoride ion was as low as 0.57 ppm that is among the lowest detection limits in aqueous solutions of many fluoride fluorescence probes in the literature.

Comparison of secondary ion intensity enhancement from polymers on silicon and silver substrates by using Au-TOF-SIMS

NASA Astrophysics Data System (ADS)

Kudo, M.; Aimoto, K.; Sunagawa, Y.; Kato, N.; Aoyagi, S.; Iida, S.; Sanada, N.

2008-12-01

The usefulness of the usage of cluster primary ion source together with an Ag substrate and detection of Ag cationized molecular ions was studied from the standpoint to realize high sensitivity TOF-SIMS analysis of organic materials. Although secondary ions from polymer thin films on a Si substrate can be detected in a higher sensitivity with Au 3+ cluster primary ion compared with Ga + ion bombardment, it was clearly observed that the secondary ion intensities from samples on an Ag substrate showed quite a different tendency from that on Si. When monoatomic primary ions, e.g., Au + and Ga +, were used for the measurement of the sample on an Ag substrate, [M+Ag] + ions (M corresponds to polyethylene glycol molecule) were detected in a high sensitivity. On the contrary, when Au 3+ was used, no intensity enhancement of [M+Ag] + ions was observed. The acceleration energy dependence of the detected secondary ions implies the different ionization mechanisms on the different substrates.

Microfabricated cylindrical ion trap

DOEpatents

Blain, Matthew G.

2005-03-22

A microscale cylindrical ion trap, having an inner radius of order one micron, can be fabricated using surface micromachining techniques and materials known to the integrated circuits manufacturing and microelectromechanical systems industries. Micromachining methods enable batch fabrication, reduced manufacturing costs, dimensional and positional precision, and monolithic integration of massive arrays of ion traps with microscale ion generation and detection devices. Massive arraying enables the microscale cylindrical ion trap to retain the resolution, sensitivity, and mass range advantages necessary for high chemical selectivity. The microscale CIT has a reduced ion mean free path, allowing operation at higher pressures with less expensive and less bulky vacuum pumping system, and with lower battery power than conventional- and miniature-sized ion traps. The reduced electrode voltage enables integration of the microscale cylindrical ion trap with on-chip integrated circuit-based rf operation and detection electronics (i.e., cell phone electronics). Therefore, the full performance advantages of microscale cylindrical ion traps can be realized in truly field portable, handheld microanalysis systems.

Microscope mode secondary ion mass spectrometry imaging with a Timepix detector.

PubMed

Kiss, Andras; Jungmann, Julia H; Smith, Donald F; Heeren, Ron M A

2013-01-01

In-vacuum active pixel detectors enable high sensitivity, highly parallel time- and space-resolved detection of ions from complex surfaces. For the first time, a Timepix detector assembly was combined with a secondary ion mass spectrometer for microscope mode secondary ion mass spectrometry (SIMS) imaging. Time resolved images from various benchmark samples demonstrate the imaging capabilities of the detector system. The main advantages of the active pixel detector are the higher signal-to-noise ratio and parallel acquisition of arrival time and position. Microscope mode SIMS imaging of biomolecules is demonstrated from tissue sections with the Timepix detector.

Modified graphene oxide sensors for ultra-sensitive detection of nitrate ions in water.

PubMed

Ren, Wen; Mura, Stefania; Irudayaraj, Joseph M K

2015-10-01

Nitrate ions is a very common contaminant in drinking water and has a significant impact on the environment, necessitating routine monitoring. Due to its chemical and physical properties, it is hard to directly detect nitrate ions with high sensitivity in a simple and inexpensive manner. Herein with amino group modified graphene oxide (GO) as a sensing element, we show a direct and ultra-sensitive method to detect nitrate ions, at a lowest detected concentration of 5 nM in river water samples, much lower than the reported methods based on absorption spectroscopy. Furthermore, unlike the reported strategies based on absorption spectroscopy wherein the nitrate concentration is determined by monitoring an increase in aggregation of gold nanoparticles (GNPs), our method evaluates the concentration of nitrate ions based on reduction in aggregation of GNPs for monitoring in real samples. To improve sensitivity, several optimizations were performed, including the assessment of the amount of modified GO required, concentration of GNPs and incubation time. The detection methodology was characterized by zeta potential, TEM and SEM. Our results indicate that an enrichment of modified GO with nitrate ions contributed to excellent sensitivity and the entire detection procedure could be completed within 75 min with only 20 μl of sample. This simple and rapid methodology was applied to monitor nitrate ions in real samples with excellent sensitivity and minimum pretreatment. The proposed approach paves the way for a novel means to detect anions in real samples and highlights the potential of GO based detection strategy for water quality monitoring. Copyright © 2015 Elsevier B.V. All rights reserved.

Coincidence ion imaging with a fast frame camera

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Suk Kyoung; Cudry, Fadia; Lin, Yun Fei

2014-12-15

A new time- and position-sensitive particle detection system based on a fast frame CMOS (complementary metal-oxide semiconductors) camera is developed for coincidence ion imaging. The system is composed of four major components: a conventional microchannel plate/phosphor screen ion imager, a fast frame CMOS camera, a single anode photomultiplier tube (PMT), and a high-speed digitizer. The system collects the positional information of ions from a fast frame camera through real-time centroiding while the arrival times are obtained from the timing signal of a PMT processed by a high-speed digitizer. Multi-hit capability is achieved by correlating the intensity of ion spots onmore » each camera frame with the peak heights on the corresponding time-of-flight spectrum of a PMT. Efficient computer algorithms are developed to process camera frames and digitizer traces in real-time at 1 kHz laser repetition rate. We demonstrate the capability of this system by detecting a momentum-matched co-fragments pair (methyl and iodine cations) produced from strong field dissociative double ionization of methyl iodide.« less

Evaluation and optimisation of indel detection workflows for ion torrent sequencing of the BRCA1 and BRCA2 genes.

PubMed

Yeo, Zhen Xuan; Wong, Joshua Chee Leong; Rozen, Steven G; Lee, Ann Siew Gek

2014-06-24

The Ion Torrent PGM is a popular benchtop sequencer that shows promise in replacing conventional Sanger sequencing as the gold standard for mutation detection. Despite the PGM's reported high accuracy in calling single nucleotide variations, it tends to generate many false positive calls in detecting insertions and deletions (indels), which may hinder its utility for clinical genetic testing. Recently, the proprietary analytical workflow for the Ion Torrent sequencer, Torrent Suite (TS), underwent a series of upgrades. We evaluated three major upgrades of TS by calling indels in the BRCA1 and BRCA2 genes. Our analysis revealed that false negative indels could be generated by TS under both default calling parameters and parameters adjusted for maximum sensitivity. However, indel calling with the same data using the open source variant callers, GATK and SAMtools showed that false negatives could be minimised with the use of appropriate bioinformatics analysis. Furthermore, we identified two variant calling measures, Quality-by-Depth (QD) and VARiation of the Width of gaps and inserts (VARW), which substantially reduced false positive indels, including non-homopolymer associated errors without compromising sensitivity. In our best case scenario that involved the TMAP aligner and SAMtools, we achieved 100% sensitivity, 99.99% specificity and 29% False Discovery Rate (FDR) in indel calling from all 23 samples, which is a good performance for mutation screening using PGM. New versions of TS, BWA and GATK have shown improvements in indel calling sensitivity and specificity over their older counterpart. However, the variant caller of TS exhibits a lower sensitivity than GATK and SAMtools. Our findings demonstrate that although indel calling from PGM sequences may appear to be noisy at first glance, proper computational indel calling analysis is able to maximize both the sensitivity and specificity at the single base level, paving the way for the usage of this technology for future clinical genetic testing.

Precision and sensitivity of the measurement of 15N enrichment in D-alanine from bacterial cell walls using positive/negative ion mass spectrometry

NASA Technical Reports Server (NTRS)

Tunlid, A.; Odham, G.; Findlay, R. H.; White, D. C.

1985-01-01

Sensitive detection of cellular components from specific groups of microbes can be utilized as 'signatures' in the examination of microbial consortia from soils, sediments or biofilms. Utilizing capillary gas chromatography/mass spectrometry and stereospecific derivatizing agents, D-alanine, a component localized in the prokaryotic (bacterial) cell wall, can be detected reproducibly. Enrichments of D-[15N]alanine determined in E. coli grown with [15N]ammonia can be determined with precision at 1.0 atom%. Chemical ionization with methane gas and the detection of negative ions (M - HF)- and (M - F or M + H - HF)- formed from the heptafluorobutyryl D-2 butanol ester of D-alanine allowed as little as 8 pg (90 fmol) to be detected reproducibly. This method can be utilized to define the metabolic activity in terms of 15N incorporation at the level of 10(3)-10(4) cells, as a function of the 15N-14N ratio.

Breakthrough in 4π ion emission mechanism understanding in plasma focus devices.

PubMed

Sohrabi, Mehdi; Zarinshad, Arefe; Habibi, Morteza

2016-12-12

Ion emission angular distribution mechanisms in plasma focus devices (PFD) have not yet been well developed and understood being due to the lack of an efficient wide-angle ion distribution image detection system to characterize a PFD space in detail. Present belief is that the acceleration of ions points from "anode top" upwards in forward direction within a small solid angle. A breakthrough is reported in this study, by mega-size position-sensitive polycarbonate ion image detection systems invented, on discovery of 4π ion emission from the "anode top" in a PFD space after plasma pinch instability and radial run-away of ions from the "anode cathodes array" during axial acceleration of plasma sheaths before the radial phase. These two ion emission source mechanisms behave respectively as a "Point Ion Source" and a "Line Ion Source" forming "Ion Cathode Shadows" on mega-size detectors. We believe that the inventions and discoveries made here will open new horizons for advanced ion emission studies towards better mechanisms understanding and in particular will promote efficient applications of PFDs in medicine, science and technology.

A microcantilever-based silver ion sensor using DNA-functionalized gold nanoparticles as a mass amplifier

NASA Astrophysics Data System (ADS)

You, Juneseok; Song, Yeongjin; Park, Chanho; Jang, Kuewhan; Na, Sungsoo

2017-06-01

Silver ions have been used to sterilize many products, however, it has recently been demonstrated that silver ions can be toxic. This toxicity has been studied over many years with the lethal concentration at 10 μM. Silver ions can accumulate through the food chain, causing serious health problems in many species. Hence, there is a need for a commercially available silver ion sensor, with high detection sensitivity. In this work, we develop an ultra-sensitive silver ion sensor platform, using cytosine based DNA and gold nanoparticles as the mass amplifier. We achieve a lower detection limit for silver ions of 10 pM; this detection limit is one million times lower than the toxic concentration. Using our sensor platform we examine highly selective characteristics of other typical ions in water from natural sources. Furthermore, our sensor platform is able to detect silver ions in a real practical sample of commercially available drinking water. Our sensor platform, which we have termed a ‘MAIS’ (mass amplifier ion sensor), with a simple detection procedure, high sensitivity, selectivity and real practical applicability has shown potential as an early toxicity assessment of silver ions in the environment.

Position-sensitive coincidence detection of nuclear reaction products at the Prague Van-de-Graaff accelerator

NASA Astrophysics Data System (ADS)

Granja, Carlos; Kraus, Vaclav; Pugatch, Valery; Kohout, Zdenek

2017-06-01

In low-energy nuclear reactions of astrophysical interest or fusion studies the spatial- and time-correlated detection of two and more reaction products can be a valuable tool in studies of reaction mechanisms, resolving reaction channels and measuring angular distributions of reaction products. For this purpose we constructed a configurable array of position-sensitive detectors based on the hybrid semiconductor pixel detector Timepix. Additional analog-signal electronics provide self-trigger together with extended multi-device control and synchronized readout electronics by a customized control and coincidence unit. The instrumentation, developed and used for detection of fission fragments in spontaneous and neutron induced fission as well as in charged particle detection in neutron induced reactions, is being implemented for low-energy light-ion induced nuclear reactions. Application and demonstration of the technique with two Timepix detectors on p+p elastic scattering at the Van-de-Graaff (VdG) accelerator in Prague is given.

Detection of positive and negative ions from a flowing atmospheric pressure afterglow using a Mattauch-Herzog mass spectrograph equipped with a Faraday-strip array detector.

PubMed

Schilling, Gregory D; Shelley, Jacob T; Barnes, James H; Sperline, Roger P; Denton, M Bonner; Barinaga, Charles J; Koppenaal, David W; Hieftje, Gary M

2010-01-01

An ambient desorption/ionization (ADI) source, known as the flowing atmospheric pressure afterglow (FAPA), has been coupled to a Mattauch-Herzog mass spectrograph (MHMS) equipped with a focal plane camera (FPC) array detector. The FAPA ionization source enables direct mass spectral analysis of solids, liquids, and gases through either positive or negative ionization modes. In either case, spectra are generally simple with dominant peaks being the molecular ions or protonated molecular ions. Use of the FAPA source with the MHMS allows the FPC detector to be characterized for the determination of molecular species, whereas previously only atomic mass spectrometry (MS) has been demonstrated. Furthermore, the FPC is shown to be sensitive to negative ions without the need to change any detector parameters. The analysis of solid, liquid, and gaseous samples through positive and negative ionization is demonstrated with detection limits (1-25 fmol/s, approximately 0.3-10 pg of analyte per mL of helium) surpassing those obtained with the FAPA source coupled to a time-of-flight mass analyzer. 2010 American Society for Mass Spectrometry. Published by Elsevier Inc. All rights reserved.

Compact multiwire proportional counters for the detection of fission fragments

NASA Astrophysics Data System (ADS)

Jhingan, Akhil; Sugathan, P.; Golda, K. S.; Singh, R. P.; Varughese, T.; Singh, Hardev; Behera, B. R.; Mandal, S. K.

2009-12-01

Two large area multistep position sensitive (two dimensional) multiwire proportional counters have been developed for experiments involving study of fission dynamics using general purpose scattering chamber facility at IUAC. Both detectors have an active area of 20×10 cm2 and provide position signals in horizontal (X) and vertical (Y) planes, timing signal for time of flight measurements and energy signal giving the differential energy loss in the active volume. The design features are optimized for the detection of low energy heavy ions at very low gas pressures. Special care was taken in setting up the readout electronics, constant fraction discriminators for position signals in particular, to get optimum position and timing resolutions along with high count rate handling capability of low energy heavy ions. A custom made charge sensitive preamplifier, having lower gain and shorter decay time, has been developed for extracting the differential energy loss signal. The position and time resolutions of the detectors were determined to be 1.1 mm full width at half maximum (FWHM) and 1.7 ns FWHM, respectively. The detector could handle heavy ion count rates exceeding 20 kHz without any breakdown. Time of flight signal in combination with differential energy loss signal gives a clean separation of fission fragments from projectile and target like particles. The timing and position signals of the detectors are used for fission coincidence measurements and subsequent extraction of their mass, angular, and total kinetic energy distributions. This article describes systematic study of these fission counters in terms of efficiency, time resolution, count rate handling capability, position resolution, and the readout electronics. The detector has been operated with both five electrode geometry and four electrode geometry, and a comparison has been made in their performances.

Rapid and Highly Sensitive Detection of Lead Ions in Drinking Water Based on a Strip Immunosensor

PubMed Central

Kuang, Hua; Xing, Changrui; Hao, Changlong; Liu, Liqiang; Wang, Libing; Xu, Chuanlai

2013-01-01

In this study, we have first developed a rapid and sensitive strip immunosensor based on two heterogeneously-sized gold nanoparticles (Au NPs) probes for the detection of trace lead ions in drinking water. The sensitivity was 4-fold higher than that of the conventional LFA under the optimized conditions. The visual limit of detection (LOD) of the amplified method for qualitative detection lead ions was 2 ng/mL and the LOD for semi-quantitative detection could go down to 0.19 ng/mL using a scanning reader. The method suffered from no interference from other metal ions and could be used to detect trace lead ions in drinking water without sample enrichment. The recovery of the test samples ranged from 96% to 103%. As the detection method could be accomplished within 15 min, this method could be used as a potential tool for preliminary monitoring of lead contamination in drinking water. PMID:23539028

A selective and sensitive method for quantitation of lysergic acid diethylamide (LSD) in whole blood by gas chromatography-ion trap tandem mass spectrometry.

PubMed

Libong, Danielle; Bouchonnet, Stéphane; Ricordel, Ivan

2003-01-01

A gas chromatography-ion trap tandem mass spectrometry (GC-ion trap MS-MS) method for detection and quantitation of LSD in whole blood is presented. The sample preparation process, including a solid-phase extraction step with Bond Elut cartridges, was performed with 2 mL of whole blood. Eight microliters of the purified extract was injected with a cold on-column injection method. Positive chemical ionization was performed using acetonitrile as reagent gas; LSD was detected in the MS-MS mode. The chromatograms obtained from blood extracts showed the great selectivity of the method. GC-MS quantitation was performed using lysergic acid methylpropylamide as the internal standard. The response of the MS was linear for concentrations ranging from 0.02 ng/mL (detection threshold) to 10.0 ng/mL. Several parameters such as the choice of the capillary column, the choice of the internal standard and that of the ionization mode (positive CI vs. EI) were rationalized. Decomposition pathways under both ionization modes were studied. Within-day and between-day stability were evaluated.

Time-resolved imaging of the MALDI linear-TOF ion cloud: direct visualization and exploitation of ion optical phenomena using a position- and time-sensitive detector.

PubMed

Ellis, Shane R; Soltwisch, Jens; Heeren, Ron M A

2014-05-01

In this study, we describe the implementation of a position- and time-sensitive detection system (Timepix detector) to directly visualize the spatial distributions of the matrix-assisted laser desorption ionization ion cloud in a linear-time-of-flight (MALDI linear-ToF) as it is projected onto the detector surface. These time-resolved images allow direct visualization of m/z-dependent ion focusing effects that occur within the ion source of the instrument. The influence of key parameters, namely extraction voltage (E(V)), pulsed-ion extraction (PIE) delay, and even the matrix-dependent initial ion velocity was investigated and were found to alter the focusing properties of the ion-optical system. Under certain conditions where the spatial focal plane coincides with the detector plane, so-called x-y space focusing could be observed (i.e., the focusing of the ion cloud to a small, well-defined spot on the detector). Such conditions allow for the stigmatic ion imaging of intact proteins for the first time on a commercial linear ToF-MS system. In combination with the ion-optical magnification of the system (~100×), a spatial resolving power of 11–16 μm with a pixel size of 550 nm was recorded within a laser spot diameter of ~125 μm. This study demonstrates both the diagnostic and analytical advantages offered by the Timepix detector in ToF-MS.

Ion mass spectrometer

NASA Technical Reports Server (NTRS)

Neugebauer, M. (Inventor); Clay, D. R.; Goldstein, B. E.; Goldstein, R.

1984-01-01

An ion mass spectrometer is described which detects and indicates the characteristics of ions received over a wide angle, and which indicates the mass to charge ratio, the energy, and the direction of each detected ion. The spectrometer includes a magnetic analyzer having a sector magnet that passes ions received over a wide angle, and an electrostatic analyzer positioned to receive ions passing through the magnetic analyzer. The electrostatic analyzer includes a two dimensional ion sensor at one wall of the analyzer chamber, that senses not only the lengthwise position of the detected ion to indicate its mass to charge ratio, but also detects the ion position along the width of the chamber to indicate the direction in which the ion was traveling.

Piezoelectric sensor for sensitive determination of metal ions based on the phosphate-modified dendrimer

NASA Astrophysics Data System (ADS)

Wang, S. H.; Shen, C. Y.; Lin, Y. M.; Du, J. C.

2016-08-01

Heavy metal ions arising from human activities are retained strongly in water; therefore public water supplies must be monitored regularly to ensure the timely detection of potential problems. A phosphate-modified dendrimer film was investigated on a quartz crystal microbalance (QCM) for sensing metal ions in water at room temperature in this study. The chemical structures and sensing properties were characterized by Fourier transform infrared spectroscopy and QCM measurement, respectively. This phosphate-modified dendrimer sensor can directly detect metal ions in aqueous solutions. This novel sensor was evaluated for its capacity to sense various metal ions. The sensor exhibited a higher sensitivity level and shorter response time to copper(II) ions than other sensors. The linear detection range of the prepared QCM based on the phosphate-modified dendrimer was 0.0001 ∼ 1 μM Cu(II) ions (R2 = 0.98). The detection properties, including sensitivity, response time, selectivity, reusability, maximum adsorption capacity, and adsorption equilibrium constants, were also investigated.

Coincidence electron/ion imaging with a fast frame camera

NASA Astrophysics Data System (ADS)

Li, Wen; Lee, Suk Kyoung; Lin, Yun Fei; Lingenfelter, Steven; Winney, Alexander; Fan, Lin

2015-05-01

A new time- and position- sensitive particle detection system based on a fast frame CMOS camera is developed for coincidence electron/ion imaging. The system is composed of three major components: a conventional microchannel plate (MCP)/phosphor screen electron/ion imager, a fast frame CMOS camera and a high-speed digitizer. The system collects the positional information of ions/electrons from a fast frame camera through real-time centroiding while the arrival times are obtained from the timing signal of MCPs processed by a high-speed digitizer. Multi-hit capability is achieved by correlating the intensity of electron/ion spots on each camera frame with the peak heights on the corresponding time-of-flight spectrum. Efficient computer algorithms are developed to process camera frames and digitizer traces in real-time at 1 kHz laser repetition rate. We demonstrate the capability of this system by detecting a momentum-matched co-fragments pair (methyl and iodine cations) produced from strong field dissociative double ionization of methyl iodide. We further show that a time resolution of 30 ps can be achieved when measuring electron TOF spectrum and this enables the new system to achieve a good energy resolution along the TOF axis.

Rapid and sensitive screening and characterization of phenolic acids, phthalides, saponins and isoflavonoids in Danggui Buxue Tang by rapid resolution liquid chromatography/diode-array detection coupled with time-of-flight mass spectrometry.

PubMed

Qi, Lian-Wen; Wen, Xiao-Dong; Cao, Jun; Li, Chang-Yin; Li, Ping; Yi, Ling; Wang, Yu-Xia; Cheng, Xiao-Lan; Ge, Xiao-Xiao

2008-08-01

A novel rapid resolution liquid chromatography (RRLC) method coupled with diode-array detection (DAD) and time-of-flight mass spectrometry (TOFMS) in both positive and negative modes has been developed for quick and sensitive identification of the major compounds in Danggui Buxue Tang (DBT) preparation. Significant advantages of the use of RRLC with 1.8-microm porous particles include the much higher speed of chromatographic separation and great enhancement in sensitivity, compared with the conventional high-performance liquid chromatography (HPLC). With dynamic adjustment of the key role as fragmentor voltage in TOFMS, an efficient transmission of the ions was achieved to obtain the best sensitivity for providing the molecular formula for each analyte, and abundant fragment ions for structural information. The structural characterization of the major compounds in DBT was elucidated with authentic standards by DAD-TOF/MS, including phenolic acids, phthalides, saponins and isoflavonoids. The targets were rapidly screened from the complicated DBT matrix using a narrow mass window of 0.01 Da to restructure extracted ion chromatograms. By accurate mass measurements within 3 ppm error for each molecular ion and subsequent fragment ions, ten phenolic acids and phthalides including three groups of isomers, thirteen major saponins with a 20,24-epoxy-9,19-cyclolanostane-3,6,16,25-tetrol skeleton, sixteen isoflavonoids, corresponding glycosides, malonylglycosides, and acetylglycosides were identified in DBT preparation. The appropriate fragmentation pathways for them were also proposed based on definite elemental composition of the fragment ions. Copyright (c) 2008 John Wiley & Sons, Ltd.

Dual mode ion mobility spectrometer and method for ion mobility spectrometry

DOEpatents

Scott, Jill R [Idaho Falls, ID; Dahl, David A [Idaho Falls, ID; Miller, Carla J [Idaho Falls, ID; Tremblay, Paul L [Idaho Falls, ID; McJunkin, Timothy R [Idaho Falls, ID

2007-08-21

Ion mobility spectrometer apparatus may include an ion interface that is operable to hold positive and negative ions and to simultaneously release positive and negative ions through respective positive and negative ion ports. A first drift chamber is operatively associated with the positive ion port of the ion interface and encloses an electric field therein. A first ion detector operatively associated with the first drift chamber detects positive ions from the first drift chamber. A second drift chamber is operatively associated with the negative ion port of the ion interface and encloses an electric field therein. A second ion detector operatively associated with the second drift chamber detects negative ions from said second drift chamber.

Advance in multi-hit detection and quantization in atom probe tomography.

PubMed

Da Costa, G; Wang, H; Duguay, S; Bostel, A; Blavette, D; Deconihout, B

2012-12-01

The preferential retention of high evaporation field chemical species at the sample surface in atom-probe tomography (e.g., boron in silicon or in metallic alloys) leads to correlated field evaporation and pronounced pile-up effects on the detector. The latter severely affects the reliability of concentration measurements of current 3D atom probes leading to an under-estimation of the concentrations of the high-field species. The multi-hit capabilities of the position-sensitive time-resolved detector is shown to play a key role. An innovative method based on Fourier space signal processing of signals supplied by an advance delay-line position-sensitive detector is shown to drastically improve the time resolving power of the detector and consequently its capability to detect multiple events. Results show that up to 30 ions on the same evaporation pulse can be detected and properly positioned. The major impact of this new method on the quantization of chemical composition in materials, particularly in highly-doped Si(B) samples is highlighted.

Multiple-channel detection of cellular activities by ion-sensitive transistors

NASA Astrophysics Data System (ADS)

Machida, Satoru; Shimada, Hideto; Motoyama, Yumi

2018-04-01

An ion-sensitive field-effect transistor to record cellular activities was demonstrated. This field-effect transistor (bio transistor) includes cultured cells on the gate insulator instead of gate electrode. The bio transistor converts a change in potential underneath the cells into variation of the drain current when ion channels open. The bio transistor has high detection sensitivity to even minute variations in potential utilizing a subthreshold swing region. To open ion channels, a reagent solution (acetylcholine) was added to a human-originating cell cultured on the bio transistor. The drain current was successfully decreased with the addition of acetylcholine. Moreover, we attempted to detect the opening of ion channels using a multiple-channel measurement circuit containing several bio transistors. As a consequence, the drain current distinctly decreased only after the addition of acetylcholine. We confirmed that this measurement system including bio transistors enables to observation of cellular activities sensitively and simultaneously.

Breakthrough in 4π ion emission mechanism understanding in plasma focus devices

PubMed Central

Sohrabi, Mehdi; Zarinshad, Arefe; Habibi, Morteza

2016-01-01

Ion emission angular distribution mechanisms in plasma focus devices (PFD) have not yet been well developed and understood being due to the lack of an efficient wide-angle ion distribution image detection system to characterize a PFD space in detail. Present belief is that the acceleration of ions points from “anode top” upwards in forward direction within a small solid angle. A breakthrough is reported in this study, by mega-size position-sensitive polycarbonate ion image detection systems invented, on discovery of 4π ion emission from the “anode top” in a PFD space after plasma pinch instability and radial run-away of ions from the “anode cathodes array” during axial acceleration of plasma sheaths before the radial phase. These two ion emission source mechanisms behave respectively as a “Point Ion Source” and a “Line Ion Source” forming “Ion Cathode Shadows” on mega-size detectors. We believe that the inventions and discoveries made here will open new horizons for advanced ion emission studies towards better mechanisms understanding and in particular will promote efficient applications of PFDs in medicine, science and technology. PMID:27941832

A flowing atmospheric pressure afterglow as an ion source coupled to a differential mobility analyzer for volatile organic compound detection.

PubMed

Bouza, Marcos; Orejas, Jaime; López-Vidal, Silvia; Pisonero, Jorge; Bordel, Nerea; Pereiro, Rosario; Sanz-Medel, Alfredo

2016-05-23

Atmospheric pressure glow discharges have been widely used in the last decade as ion sources in ambient mass spectrometry analyses. Here, an in-house flowing atmospheric pressure afterglow (FAPA) has been developed as an alternative ion source for differential mobility analysis (DMA). The discharge source parameters (inter-electrode distance, current and helium flow rate) determining the atmospheric plasma characteristics have been optimized in terms of DMA spectral simplicity with the highest achievable sensitivity while keeping an adequate plasma stability and so the FAPA working conditions finally selected were: 35 mA, 1 L min(-1) of He and an inter-electrode distance of 8 mm. Room temperature in the DMA proved to be adequate for the coupling and chemical analysis with the FAPA source. Positive and negative ions for different volatile organic compounds were tested and analysed by FAPA-DMA using a Faraday cup as a detector and proper operation in both modes was possible (without changes in FAPA operational parameters). The FAPA ionization source showed simpler ion mobility spectra with narrower peaks and a better, or similar, sensitivity than conventional UV-photoionization for DMA analysis in positive mode. Particularly, the negative mode proved to be a promising field of further research for the FAPA ion source coupled to ion mobility, clearly competitive with other more conventional plasmas such as corona discharge.

Detection of ionized gas molecules in air by graphene and carbon nanotube networks

NASA Astrophysics Data System (ADS)

Hao, Ji; Li, Bo; Yung, Hyun Young; Liu, Fangze; Hong, Sanghyung; Jung, Yung Joon; Kar, Swastik

The liquid phase ions sensing by graphene and carbon nanotube has been demonstrated in many publications due to the minimum gate voltage easily shift induced by ionic gating effect, but it is still unclear for vapor phase ions sensing. Here we want to report that the ionized gas molecules in air can be also very sensitively detected by graphene and carbon nanotube networks under very low applied voltage, which shows the very high charge to current amplification factor, the value can be up to 108 A/C, and the direction of current-change can be used to differentiate the positive and negative ions. In further, the field effect of graphene device induced by vapor phase ions was discussed. NSF ECCS 1202376, NSF ECCS CAREER 1351424 and NSF DMREF 1434824, a Northeastern University Provost's Tier-1 seed Grant for interdisciplinary research, Technology Innovation Program (10050481) from Ministry of Trade, Industry & Energy of Republic of Korea.

Liquid chromatography-electrospray mass spectrometry of beta-carotene and xanthophylls. Validation of the analytical method.

PubMed

Careri, M; Elviri, L; Mangia, A

1999-08-27

The investigation of beta-carotene and the xanthophylls beta-cryptoxanthin, lutein, zeaxanthin, canthaxanthin and astaxanthin using reversed-phase liquid chromatography-electrospray mass spectrometry interfaced with TurboIonspray (LC-TurboISP-MS) is described. Two narrow-bore C18 columns connected in series and an isocratic solvent system containing acetonitrile-methanol (0.1 M ammonium acetate)-dichloromethane at a flow-rate of 300 microl/min (without splitting) were used. Operating in the positive-ion mode over m/z 500-650, the effects on the formation of the molecular ion species or adduct ions and the MS detector response were investigated for carotenoids, varying the orifice plate voltage, the ring voltage and the ISP voltage. Both conventional ISP and TurboISP were performed; using the TurboISP-MS system, ionization efficiency increased with respect to ISP-MS, particularly at the highest temperature (500 degrees C). Good results were particularly obtained for beta-carotene, which was detectable at the low ng level, without the use of solution-phase oxidants. Using LC columns and acquiring in single-ion monitoring mode, detection limits were estimated to be in the 0.1-1 ng range; dynamic range was established between one- and two-orders of magnitude. Better sensitivity under positive-ion than negative-ion conditions was demonstrated.

On the effectiveness of ion range determination from in-beam PET data

NASA Astrophysics Data System (ADS)

Fiedler, Fine; Shakirin, Georgy; Skowron, Judith; Braess, Henning; Crespo, Paulo; Kunath, Daniela; Pawelke, Jörg; Pönisch, Falk; Enghardt, Wolfgang

2010-04-01

At present, in-beam positron emission tomography (PET) is the only method for in vivo and in situ range verification in ion therapy. At the GSI Helmholtzzentrum für Schwerionenforschung GmbH (GSI) Darmstadt, Germany, a unique in-beam PET installation has been operated from 1997 until the shut down of the carbon ion therapy facility in 2008. Therapeutic irradiation by means of 12C ion beams of more than 400 patients have been monitored. In this paper a first quantitative study on the accuracy of the in-beam PET method to detect range deviations between planned and applied treatment in clinically relevant situations using simulations based on clinical data is presented. Patient treatment plans were used for performing simulations of positron emitter distributions. For each patient a range difference of ± 6 mm in water was applied and compared to simulations without any changes. The comparisons were performed manually by six experienced evaluators for data of 81 patients. The number of patients required for the study was calculated using the outcome of a pilot study. The results indicate a sensitivity of (91 ± 3)% and a specificity of (96 ± 2)% for detecting an overrange, a reduced range is recognized with a sensitivity of (92 ± 3)% and a specificity of (96 ± 2)%. The positive and the negative predictive value of this method are 94% and 87%, respectively. The interobserver coefficient of variation is between 3 and 8%. The in-beam PET method demonstrated a high sensitivity and specificity for the detection of range deviations. As the range is a most indicative factor of deviations in the dose delivery, the promising results shown in this paper confirm the in-beam PET method as an appropriate tool for monitoring ion therapy.

Using gas chromatography with ion mobility spectrometry to resolve explosive compounds in the presence of interferents.

PubMed

Cook, Greg W; LaPuma, Peter T; Hook, Gary L; Eckenrode, Brian A

2010-11-01

Ion mobility spectrometry (IMS) is a valued field detection technology because of its speed and high sensitivity, but IMS cannot easily resolve analytes of interest within mixtures. Coupling gas chromatography (GC) to IMS adds a separation capability to resolve complex matrices. A GC-IONSCAN® operated in IMS and GC⁄ IMS modes was evaluated with combinations of five explosives and four interferents. In 100 explosive/interferent combinations, IMS yielded 21 false positives while GC⁄ IMS substantially reduced the occurrence of false positives to one. In addition, the results indicate that through redesign or modification of the preconcentrator there would be significant advantages to using GC⁄ IMS, such as enhancement of the linear dynamic range (LDR) in some situations. By balancing sensitivity with LDR, GC⁄ IMS could prove to be a very advantageous tool when addressing real world complex mixture situations.

Selective and sensitive optical chemosensor for detection of Ag(I) ions based on 2(4-hydroxy pent-3-en-2-ylideneamine) phenol in aqueous samples

NASA Astrophysics Data System (ADS)

Mirzaei, Mohammad; Saeed, Jaber

2011-11-01

A selective and sensitive chemosensor, based on the 2(4-hydroxy pent-3-en-2-ylideneamine) phenol (HPYAP) as chromophore, has been developed for colorimetric and visual detection of Ag(I) ions. HPYAP shows a considerable chromogenic behavior toward Ag(I) ions by changing the color of the solution from pale-yellow to very chromatic-yellow, which can be easily detected with the naked-eye. The chemosensor exhibited selective absorbance enhancement to Ag(I) ions in water samples over other metal ions at 438 nm, with a linear range of 0.4-500 μM ( r2 = 0.999) and a limit of detection 0.07 μM of Ag(I) ions with UV-vis spectrophotometer detection. The relative standard deviation (RSD) for 100 μM Ag(I) ions was 2.05% ( n = 7). The proposed method was applied for the determination Ag(I) ions in water and waste water samples.

Distance-of-Flight Mass Spectrometry: What, Why, and How?

NASA Astrophysics Data System (ADS)

Dennis, Elise A.; Gundlach-Graham, Alexander W.; Ray, Steven J.; Enke, Christie G.; Hieftje, Gary M.

2016-11-01

Distance-of-flight mass spectrometry (DOFMS) separates ions of different mass-to-charge ( m/ z) by the distance they travel in a given time after acceleration. Like time-of-flight mass spectrometry (TOFMS), separation and mass assignment are based on ion velocity. However, DOFMS is not a variant of TOFMS; different methods of ion focusing and detection are used. In DOFMS, ions are driven orthogonally, at the detection time, onto an array of detectors parallel to the flight path. Through the independent detection of each m/ z, DOFMS can provide both wider dynamic range and increased throughput for m/ z of interest compared with conventional TOFMS. The iso-mass focusing and detection of ions is achieved by constant-momentum acceleration (CMA) and a linear-field ion mirror. Improved energy focus (including turn-around) is achieved in DOFMS, but the initial spatial dispersion of ions remains unchanged upon detection. Therefore, the point-source nature of surface ionization techniques could put them at an advantage for DOFMS. To date, three types of position-sensitive detectors have been used for DOFMS: a microchannel plate with a phosphorescent screen, a focal plane camera, and an IonCCD array; advances in detector technology will likely improve DOFMS figures-of-merit. In addition, the combination of CMA with TOF detection has provided improved resolution and duty factor over a narrow m/ z range (compared with conventional, single-pass TOFMS). The unique characteristics of DOFMS can enable the intact collection of large biomolecules, clusters, and organisms. DOFMS might also play a key role in achieving the long-sought goal of simultaneous MS/MS.

Development of a Real-Time Resistance Measurement for Vibrio parahaemolyticus Detection by the Lecithin-Dependent Hemolysin Gene

PubMed Central

Xiang, Guiming; Pu, Xiaoyun; Jiang, Dongneng; Liu, Linlin; Liu, Chang; Liu, Xiaobo

2013-01-01

The marine bacterium Vibrio parahaemolyticus (V. parahaemolyticus) causes gastroenteritis in humans via the ingestion of raw or undercooked contaminated seafood, and early diagnosis and prompt treatment are important for the prevention of V. parahaemolyticus-related diseases. In this study, a real-time resistance measurement based on loop-mediated isothermal amplification (LAMP), electrochemical ion bonding (Crystal violet and Mg2+), real-time monitoring, and derivative analysis was developed. V. parahaemolyticus DNA was first amplified by LAMP, and the products (DNA and pyrophosphate) represented two types of negative ions that could combine with a positive dye (Crystal violet) and positive ions (Mg2+) to increase the resistance of the reaction liquid. This resistance was measured in real-time using a specially designed resistance electrode, thus permitting the quantitative detection of V. parahaemolyticus. The results were obtained in 1–2 hours, with a minimum bacterial density of 10 CFU.mL−1 and high levels of accuracy (97%), sensitivity (96.08%), and specificity (97.96%) when compared to cultivation methods. Therefore, this simple and rapid method has a potential application in the detection of V. parahaemolyticus on a gene chip or in point-of-care testing. PMID:23991096

Critical comparison of mass analyzers for forensic hair analysis by ambient ionization mass spectrometry.

PubMed

Duvivier, Wilco F; van Beek, Teris A; Nielen, Michel W F

2016-11-15

Recently, several direct and/or ambient mass spectrometry (MS) approaches have been suggested for drugs of abuse imaging in hair. The use of mass spectrometers with insufficient selectivity could result in false-positive measurements due to isobaric interferences. Different mass analyzers have been evaluated regarding their selectivity and sensitivity for the detection of Δ9-tetrahydrocannabinol (THC) from intact hair samples using direct analysis in real time (DART) ionization. Four different mass analyzers, namely (1) an orbitrap, (2) a quadrupole orbitrap, (3) a triple quadrupole, and (4) a quadrupole time-of-flight (QTOF), were evaluated. Selectivity and sensitivity were assessed by analyzing secondary THC standard dilutions on stainless steel mesh screens and blank hair samples, and by the analysis of authentic cannabis user hair samples. Additionally, separation of isobaric ions by use of travelling wave ion mobility (TWIM) was investigated. The use of a triple quadrupole instrument resulted in the highest sensitivity; however, transitions used for multiple reaction monitoring were only found to be specific when using high mass resolution product ion measurements. A mass resolution of at least 30,000 FWHM at m/z 315 was necessary to avoid overlap of THC with isobaric ions originating from the hair matrix. Even though selectivity was enhanced by use of TWIM, the QTOF instrument in resolution mode could not indisputably differentiate THC from endogenous isobaric ions in drug user hair samples. Only the high resolution of the (quadrupole) orbitrap instruments and the QTOF instrument in high-resolution mode distinguished THC in hair samples from endogenous isobaric interferences. As expected, enhanced selectivity compromises sensitivity and THC was only detectable in hair from heavy users. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Detection of heavy metal ions in contaminated water by surface plasmon resonance based optical fibre sensor using conducting polymer and chitosan.

PubMed

Verma, Roli; Gupta, Banshi D

2015-01-01

Optical fibre surface plasmon resonance (SPR) based sensor for the detection of heavy metal ions in the drinking water is designed. Silver (Ag) metal and indium tin oxide (ITO) are used for the fabrication of the SPR probe which is further modified with the coating of pyrrole and chitosan composite. The sensor works on the wavelength interrogation technique and is capable of detecting trace amounts of Cd(2+), Pb(2+), and Hg(2+) heavy metal ions in contaminated water. Four types of sensing probes are fabricated and characterised for heavy metal ions out of these pyrrole/chitosan/ITO/Ag coated probe is found to be highly sensitive among all other probes. Further, the cadmium ions bind strongly to the sensing surface than other ions and due to this the sensor is highly sensitive for Cd(2+) ions. The sensor's performance is best for the low concentrations of heavy metal ions and its sensitivity decreases with the increasing concentration of heavy metal ions. Copyright © 2014 Elsevier Ltd. All rights reserved.

The sensitivity of benzene cluster cation chemical ionization mass spectrometry to select biogenic terpenes

NASA Astrophysics Data System (ADS)

Lavi, Avi; Vermeuel, Michael P.; Novak, Gordon A.; Bertram, Timothy H.

2018-06-01

Benzene cluster cations are a sensitive and selective reagent ion for chemical ionization of select biogenic volatile organic compounds. We have previously reported the sensitivity of a field deployable chemical ionization time-of-flight mass spectrometer (CI-ToFMS), using benzene cluster cation ion chemistry, for detection of dimethyl sulfide, isoprene and α-pinene. Here, we present laboratory measurements of the sensitivity of the same instrument to a series of terpenes, including isoprene, α-pinene, β-pinene, D-limonene, ocimene, β-myrcene, farnesene, α-humulene, β-caryophyllene, and isolongifolene at atmospherically relevant mixing ratios (< 100 pptv). In addition, we determine the dependence of CI-ToFMS sensitivity on the reagent ion neutral delivery concentration and water vapor concentration. We show that isoprene is primarily detected as an adduct (C5H8 ṡ C6H6+) with a sensitivity ranging between 4 and 10 ncps ppt-1, which depends strongly on the reagent ion precursor concentration, de-clustering voltages, and specific humidity (SH). Monoterpenes are detected primarily as the molecular ion (C10H16+) with an average sensitivity, across the five measured compounds, of 14 ± 3 ncps ppt-1 for SH between 7 and 14 g kg-1, typical of the boreal forest during summer. Sesquiterpenes are detected primarily as the molecular ion (C15H24+) with an average sensitivity, across the four measured compounds, of 9.6 ± 2.3 ncps ppt-1, that is also independent of specific humidity. Comparable sensitivities across broad classes of terpenes (e.g., monoterpenes and sesquiterpenes), coupled to the limited dependence on specific humidity, suggest that benzene cluster cation CI-ToFMS is suitable for field studies of biosphere-atmosphere interactions.

Spatial and Time Coincidence Detection of the Decay Chain of Short-Lived Radioactive Nuclei

DOE Office of Scientific and Technical Information (OSTI.GOV)

Granja, Carlos; Jakubek, Jan; Platkevic, Michal

The quantum counting position sensitive pixel detector Timepix with per-pixel energy and time resolution enables to detect radioactive ions and register the consecutive decay chain by simultaneous position-and time-correlation. This spatial and timing coincidence technique in the same sensor is demonstrated by the registration of the decay chain {sup 8}He{yields}{sup {beta} 8}Li and {sup 8}Li{yields}{sup {beta}-} {sup 8}Be{yields}{alpha}+{alpha} and by the measurement of the {beta} decay half-lives. Radioactive ions, selectively obtained from the Lohengrin fission fragment spectrometer installed at the High Flux Reactor of the ILL Grenoble, are delivered to the Timepix silicon sensor where decays of the implanted ionsmore » and daughter nuclei are registered and visualized. We measure decay lifetimes in the range {>=}{mu}s with precision limited just by counting statistics.« less

Selective and sensitive detection of chromium(VI) in waters using electrospray ionization mass spectrometry.

PubMed

Weldy, Effie; Wolff, Chloe; Miao, Zhixin; Chen, Hao

2013-09-01

From 2000 through 2011, there were 14 criminal cases of violations of the Clean Water Act involving the discharge of chromium, a toxic heavy metal, into drinking and surface water sources. As chromium(VI), a potential carcinogen present in the environment, represents a significant safety concern, it is currently the subject of an EPA health risk assessment. Therefore, sensitive and selective detection of this species is highly desired. This study reports the analysis of chromium(VI) in water samples by electrospray ionization mass spectrometry (ESI-MS) following its reduction and complexation with ammonium pyrrolidinedithiocarbamate (APDC). The reduction and subsequent complexation produce a characteristic [Cr(III)O]-PDC complex which can be detected as a protonated ion of m/z 507 in the positive ion mode. The detection is selective to chromium(VI) under acidic pH, even in the presence of chromium(III) and other metal ions, providing high specificity. Different water samples were examined, including deionized, tap, and river waters, and sensitive detection was achieved. In the case of deionized water, quantification over the concentration range of 3.7 to 148ppb gave an excellent correlation coefficient of 0.9904 using the enhanced MS mode scan. Using the single-reaction monitoring (SRM) mode (monitoring the characteristic fragmentation of m/z 507 to m/z 360), the limit of detection (LOD) was found to be 0.25ppb. The LOD of chromium(VI) for both tap and river water samples was determined to be 2.0ppb. A preconcentration strategy using simple vacuum evaporation of the aqueous sample was shown to further improve the ESI signal by 15 fold. This method, with high sensitivity and selectivity, should provide a timely solution for the real-world analysis of toxic chromium(VI). Copyright © 2012 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Polyamidoamine dendrimers as sweeping agent and stationary phase for rapid and sensitive open-tubular capillary electrophoretic determination of heavy metal ions.

PubMed

Ge, Ying; Guo, Yujun; Qin, Weidong

2014-04-01

Polyamidoamine (PAMAM) dendrimer generation 2.5 was synthesized and evaluated as sweeping agent for in-column enrichment and as stationary phase for capillary electrochromatographic separation of heavy metal ions, viz., Pb(II), Cu(II), Hg(II), Zn(II) and Co(II), in a running buffer containing 4-(2-pyridylazo)resorcinol (PAR) as a chromogenic reagent. During experiment, a plug of aqueous PAMAM generation 2.5 solution was first introduced to the capillary, followed by electrokinetic injection of the heavy metal ions under a positive voltage. In this step, PAMAM acted as a sweeping agent, stacking the metal ions on the analyte/PAMAM boundary by forming metal ion-PAMAM complexes. The second preconcentration process occurred when PAR, a stronger ligand, moving toward the injection end under the electric field, reached and re-swept the metal ion-PAMAM zone, forming metal ion-PAR complexes. During separation, the neutral PAMAM moved toward the detector with the electroosmotic flow, dynamically coating the capillary wall, forming stationary phases that affected the separation of the metal ions. Due to the function of PAMAM, the detection sensitivity and resolution of the heavy metal ions improved significantly. Under the optimum conditions, the detection limits were 0.299, 0.184, 0.774, 0.182 and 0.047 μg/L for Pb(II), Cu(II), Hg(II), Zn(II) and Co(II), respectively. The method was successfully applied to the determination of heavy metals in snow, tap and rain water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

A tandem mass spectrometer for crossed-beam irradiation of mass-selected molecular systems by keV atomic ions

NASA Astrophysics Data System (ADS)

Schwob, Lucas; Lalande, Mathieu; Chesnel, Jean-Yves; Domaracka, Alicja; Huber, Bernd A.; Maclot, Sylvain; Poully, Jean-Christophe; Rangama, Jimmy; Rousseau, Patrick; Vizcaino, Violaine; Adoui, Lamri; Méry, Alain

2018-04-01

In the present paper, we describe a new home-built crossed-beam apparatus devoted to ion-induced ionization and fragmentation of isolated biologically relevant molecular systems. The biomolecular ions are produced by an electrospray ionization source, mass-over-charge selected, accumulated in a 3D ion trap, and then guided to the extraction region of an orthogonal time-of-flight mass spectrometer. Here, the target molecular ions interact with a keV atomic ion beam produced by an electron cyclotron resonance ion source. Cationic products from the collision are detected on a position sensitive detector and analyzed by time-of-flight mass spectrometry. A detailed description of the operation of the setup is given, and early results from irradiation of a protonated pentapeptide (leucine-enkephalin) by a 7 keV He+ ion beam are presented as a proof-of-principle.

Rapid detection and identification of N-acetyl-L-cysteine thioethers using constant neutral loss and theoretical multiple reaction monitoring combined with enhanced product-ion scans on a linear ion trap mass spectrometer.

PubMed

Scholz, Karoline; Dekant, Wolfgang; Völkel, Wolfgang; Pähler, Axel

2005-12-01

A sensitive and specific liquid chromatography-mass spectrometry (LC-MS) method based on the combination of constant neutral loss scans (CNL) with product ion scans was developed on a linear ion trap. The method is applicable for the detection and identification of analytes with identical chemical substructures (such as conjugates of xenobiotics formed in biological systems) which give common CNLs. A specific CNL was observed for thioethers of N-acetyl-L-cysteine (mercapturic acids, MA) by LC-MS/MS. MS and HPLC parameters were optimized with 16 MAs available as reference compounds. All of these provided a CNL of 129 Da in the negative-ion mode. To assess sensitivity, a multiple reaction monitoring (MRM) mode with 251 theoretical transitions using the CNL of 129 Da combined with a product ion scan (IDA thMRM) was compared with CNL combined with a product ion scan (IDA CNL). An information-dependent acquisition (IDA) uses a survey scan such as MRM (multiple reaction monitoring) to generate "informations" and starting a second acquisition experiment such as a product ion scan using these "informations." Th-MRM means calculated transitions and not transitions generated from an available standard in the tuning mode. The product ion spectra provide additional information on the chemical structure of the unknown analytes. All MA standards were spiked in low concentrations to rat urines and were detected with both methods with LODs ranging from 60 pmol/mL to 1.63 nmol/mL with IDA thMRM. The expected product ion spectra were observed in urine. Application of this screening method to biological samples indicated the presence of a number of MAs in urine of unexposed rats, and resulted in the identification of 1,4-dihydroxynonene mercapturic acid as one of these MAs by negative and positive product ion spectra. These results show that the developed methods have a high potential to serve as both a prescreen to detect unknown MAs and to identify these analytes in complex matrix.

Qualitative metabolome analysis of human cerebrospinal fluid by 13C-/12C-isotope dansylation labeling combined with liquid chromatography Fourier transform ion cyclotron resonance mass spectrometry.

PubMed

Guo, Kevin; Bamforth, Fiona; Li, Liang

2011-02-01

Metabolome analysis of human cerebrospinal fluid (CSF) is challenging because of low abundance of metabolites present in a small volume of sample. We describe and apply a sensitive isotope labeling LC-MS technique for qualitative analysis of the CSF metabolome. After a CSF sample is divided into two aliquots, they are labeled by (13)C-dansyl and (12)C-dansyl chloride, respectively. The differentially labeled aliquots are then mixed and subjected to LC-MS using Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS). Dansylation offers significant improvement in the performance of chromatography separation and detection sensitivity. Moreover, peaks detected in the mass spectra can be readily analyzed for ion pair recognition and database search based on accurate mass and/or retention time information. It is shown that about 14,000 features can be detected in a 25-min LC-FTICR MS run of a dansyl-labeled CSF sample, from which about 500 metabolites can be profiled. Results from four CSF samples are compared to gauge the detectability of metabolites by this method. About 261 metabolites are commonly detected in replicate runs of four samples. In total, 1132 unique metabolite ion pairs are detected and 347 pairs (31%) matched with at least one metabolite in the Human Metabolome Database. We also report a dansylation library of 220 standard compounds and, using this library, about 85 metabolites can be positively identified. Among them, 21 metabolites have never been reported to be associated with CSF. These results illustrate that the dansylation LC-FTICR MS method can be used to analyze the CSF metabolome in a more comprehensive manner. © American Society for Mass Spectrometry, 2011

Qualitative Metabolome Analysis of Human Cerebrospinal Fluid by 13C-/12C-Isotope Dansylation Labeling Combined with Liquid Chromatography Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

NASA Astrophysics Data System (ADS)

Guo, Kevin; Bamforth, Fiona; Li, Liang

2011-02-01

Metabolome analysis of human cerebrospinal fluid (CSF) is challenging because of low abundance of metabolites present in a small volume of sample. We describe and apply a sensitive isotope labeling LC-MS technique for qualitative analysis of the CSF metabolome. After a CSF sample is divided into two aliquots, they are labeled by 13C-dansyl and 12C-dansyl chloride, respectively. The differentially labeled aliquots are then mixed and subjected to LC-MS using Fourier-transform ion cyclotron resonance mass spectrometry (FTICR MS). Dansylation offers significant improvement in the performance of chromatography separation and detection sensitivity. Moreover, peaks detected in the mass spectra can be readily analyzed for ion pair recognition and database search based on accurate mass and/or retention time information. It is shown that about 14,000 features can be detected in a 25-min LC-FTICR MS run of a dansyl-labeled CSF sample, from which about 500 metabolites can be profiled. Results from four CSF samples are compared to gauge the detectability of metabolites by this method. About 261 metabolites are commonly detected in replicate runs of four samples. In total, 1132 unique metabolite ion pairs are detected and 347 pairs (31%) matched with at least one metabolite in the Human Metabolome Database. We also report a dansylation library of 220 standard compounds and, using this library, about 85 metabolites can be positively identified. Among them, 21 metabolites have never been reported to be associated with CSF. These results illustrate that the dansylation LC-FTICR MS method can be used to analyze the CSF metabolome in a more comprehensive manner.

Ion mobility spectrometric analysis of vaporous chemical warfare agents by the instrument with corona discharge ionization ammonia dopant ambient temperature operation.

PubMed

Satoh, Takafumi; Kishi, Shintaro; Nagashima, Hisayuki; Tachikawa, Masumi; Kanamori-Kataoka, Mieko; Nakagawa, Takao; Kitagawa, Nobuyoshi; Tokita, Kenichi; Yamamoto, Soichiro; Seto, Yasuo

2015-03-20

The ion mobility behavior of nineteen chemical warfare agents (7 nerve gases, 5 blister agents, 2 lachrymators, 2 blood agents, 3 choking agents) and related compounds including simulants (8 agents) and organic solvents (39) was comparably investigated by the ion mobility spectrometry instrument utilizing weak electric field linear drift tube with corona discharge ionization, ammonia doping, purified inner air drift flow circulation operated at ambient temperature and pressure. Three alkyl methylphosphonofluoridates, tabun, and four organophosphorus simulants gave the intense characteristic positive monomer-derived ion peaks and small dimer-derived ion peaks, and the later ion peaks were increased with the vapor concentrations. VX, RVX and tabun gave both characteristic positive monomer-derived ions and degradation product ions. Nitrogen mustards gave the intense characteristic positive ion peaks, and in addition distinctive negative ion peak appeared from HN3. Mustard gas, lewisite 1, o-chlorobenzylidenemalononitrile and 2-mercaptoethanol gave the characteristic negative ion peaks. Methylphosphonyl difluoride, 2-chloroacetophenone and 1,4-thioxane gave the characteristic ion peaks both in the positive and negative ion mode. 2-Chloroethylethylsulfide and allylisothiocyanate gave weak ion peaks. The marker ion peaks derived from two blood agents and three choking agents were very close to the reactant ion peak in negative ion mode and the respective reduced ion mobility was fluctuated. The reduced ion mobility of the CWA monomer-derived peaks were positively correlated with molecular masses among structurally similar agents such as G-type nerve gases and organophosphorus simulants; V-type nerve gases and nitrogen mustards. The slope values of the calibration plots of the peak heights of the characteristic marker ions versus the vapor concentrations are related to the detection sensitivity, and within chemical warfare agents examined the slope values for sarin, soman, tabun and nitrogen mustards were higher. Some CWA simulants and organic solvents gave the ion peaks eluting at the similar positions of the CWAs, resulting in false positive alarms. Copyright © 2015 Elsevier B.V. All rights reserved.

Relationships between structure, ionization profile and sensitivity of exogenous anabolic steroids under electrospray ionization and analysis in human urine using liquid chromatography-tandem mass spectrometry.

PubMed

Cha, Eunju; Kim, Sohee; Kim, Hee Won; Lee, Kang Mi; Kim, Ho Jun; Kwon, Oh-Seung; Lee, Jaeick

2016-04-01

The relationships between the ionization profile, sensitivity, and structures of 64 exogenous anabolic steroids (groups I-IV) was investigated under electrospray ionization (ESI) conditions. The target analytes were ionized as [M + H](+) or [M + H-nH2 O](+) in the positive mode, and these ions were used as precursor ions for selected reaction monitoring analysis. The collision energy and Q3 ions were optimized based on the sensitivity and selectivity. The limits of detection (LODs) were 0.05-20 ng/mL for the 64 steroids. The LODs for 38 compounds, 14 compounds and 12 compounds were in the range of 0.05-1, 2-5 and 10-20 ng/mL, respectively. Steroids including the conjugated keto-functional group at C3 showed good proton affinity and stability, and generated the [M + H](+) ion as the most abundant precursor ion. In addition, the LODs of steroids using the [M + H](+) ion as the precursor ion were mostly distributed at low concentrations. In contrast, steroids containing conjugated/unconjugated hydroxyl functional groups at C3 generated [M + H - H2 O](+) or [M + H - 2H2 O](+) ions, and these steroids showed relatively high LODs owing to poor stability and multiple ion formation. An LC-MS/MS method based on the present ionization profile was developed and validated for the determination of 78 steroids (groups I-V) in human urine. Copyright © 2015 John Wiley & Sons, Ltd.

A Single Serine Residue Determines Selectivity to Monovalent Metal Ions in Metalloregulators of the MerR Family

PubMed Central

Ibáñez, María M.

2015-01-01

ABSTRACT MerR metalloregulators alleviate toxicity caused by an excess of metal ions, such as copper, zinc, mercury, lead, cadmium, silver, or gold, by triggering the expression of specific efflux or detoxification systems upon metal detection. The sensor protein binds the inducer metal ion by using two conserved cysteine residues at the C-terminal metal-binding loop (MBL). Divalent metal ion sensors, such as MerR and ZntR, require a third cysteine residue, located at the beginning of the dimerization (α5) helix, for metal coordination, while monovalent metal ion sensors, such as CueR and GolS, have a serine residue at this position. This serine residue was proposed to provide hydrophobic and steric restrictions to privilege the binding of monovalent metal ions. Here we show that the presence of alanine at this position does not modify the activation pattern of monovalent metal sensors. In contrast, GolS or CueR mutant sensors with a substitution of cysteine for the serine residue respond to monovalent metal ions or Hg(II) with high sensitivities. Furthermore, in a mutant deleted of the Zn(II) exporter ZntA, they also trigger the expression of their target genes in response to either Zn(II), Cd(II), Pb(II), or Co(II). IMPORTANCE Specificity in a stressor's recognition is essential for mounting an appropriate response. MerR metalloregulators trigger the expression of specific resistance systems upon detection of heavy metal ions. Two groups of these metalloregulators can be distinguished, recognizing either +1 or +2 metal ions, depending on the presence of a conserved serine in the former or a cysteine in the latter. Here we demonstrate that the serine residue in monovalent metal ion sensors excludes divalent metal ion detection, as its replacement by cysteine renders a pan-metal ion sensor. Our results indicate that the spectrum of signals detected by these sensors is determined not only by the metal-binding ligand availability but also by the metal-binding cavity flexibility. PMID:25691529

Fourier transform ion cyclotron resonance mass spectrometry

NASA Astrophysics Data System (ADS)

Marshall, Alan G.

1998-06-01

As for Fourier transform infrared (FT-IR) interferometry and nuclear magnetic resonance (NMR) spectroscopy, the introduction of pulsed Fourier transform techniques revolutionized ion cyclotron resonance mass spectrometry: increased speed (factor of 10,000), increased sensitivity (factor of 100), increased mass resolution (factor of 10,000-an improvement not shared by the introduction of FT techniques to IR or NMR spectroscopy), increased mass range (factor of 500), and automated operation. FT-ICR mass spectrometry is the most versatile technique for unscrambling and quantifying ion-molecule reaction kinetics and equilibria in the absence of solvent (i.e., the gas phase). In addition, FT-ICR MS has the following analytically important features: speed (~1 second per spectrum); ultrahigh mass resolution and ultrahigh mass accuracy for analysis of mixtures and polymers; attomole sensitivity; MSn with one spectrometer, including two-dimensional FT/FT-ICR/MS; positive and/or negative ions; multiple ion sources (especially MALDI and electrospray); biomolecular molecular weight and sequencing; LC/MS; and single-molecule detection up to 108 Dalton. Here, some basic features and recent developments of FT-ICR mass spectrometry are reviewed, with applications ranging from crude oil to molecular biology.

A sensitive mass spectrometric method for hypothesis-driven detection of peptide post-translational modifications: multiple reaction monitoring-initiated detection and sequencing (MIDAS).

PubMed

Unwin, Richard D; Griffiths, John R; Whetton, Anthony D

2009-01-01

The application of a targeted mass spectrometric workflow to the sensitive identification of post-translational modifications is described. This protocol employs multiple reaction monitoring (MRM) to search for all putative peptides specifically modified in a target protein. Positive MRMs trigger an MS/MS experiment to confirm the nature and site of the modification. This approach, termed MIDAS (MRM-initiated detection and sequencing), is more sensitive than approaches using neutral loss scanning or precursor ion scanning methodologies, due to a more efficient use of duty cycle along with a decreased background signal associated with MRM. We describe the use of MIDAS for the identification of phosphorylation, with a typical experiment taking just a couple of hours from obtaining a peptide sample. With minor modifications, the MIDAS method can be applied to other protein modifications or unmodified peptides can be used as a MIDAS target.

Counting individual ions in the air by tagging them with particles

NASA Astrophysics Data System (ADS)

Gorbunov, B.

2017-07-01

The quantification of ultra-low concentrations of molecules and ions in gases is of fundamental and practical importance for science and technology, for example, the detection of explosives in airports or biomarkers in medical diagnostics. Often the Faraday cup is employed to transfer ion concentrations in an electric current that is then amplified and measured. One of the main challenges is to increase the sensitivity of detection. A novel concept has been developed that enables detection of individual ions in gases by tagging them with neutral nano-objects. The concentration of ionized molecules was measured and a detection limit of 5 cm-3 was observed. It is anticipated that this concept opens doors for advances in detection sensitivity for many applications including security, medical diagnostic, trace chemical analysis.

Identification and quantification of cardiac glycosides in blood and urine samples by HPLC/MS/MS.

PubMed

Guan, F; Ishii, A; Seno, H; Watanabe-Suzuki, K; Kumazawa, T; Suzuki, O

1999-09-15

Cardiac glycosides (CG) are of forensic importance because of their toxicity and the fact that very limited methods are available for identification of CG in biological samples. In this study, we have developed an identification and quantification method for digoxin, digitoxin, deslanoside, digoxigenin, and digitoxigenin by high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). CG formed abundant [M + NH4]+ ions and much less abundant [M + H]+ ions as observed with electrospray ionization (ESI) source and ammonium formate buffer. Under mild conditions for collision-induced dissociation (CID), each [M + NH4]+ ion fragmented to produce a dominant daughter ion, which was essential to the sensitive method of selected reaction monitoring (SRM) quantification of CG achieved in this study. SRM was compared with selected ion monitoring (SIM) regarding the effects of sample matrixes on the methodology. SRM produced lower detection limits with biological samples than SIM, while both methods produced equal detection limits with CG standards. On the basis of the HPLC/MS/MS results for CG, we have proposed some generalized points for conducting sensitive SRM measurements, in view of the property of analytes as well as instrumental conditions such as the type of HPLC/MS interface and CID parameters. Analytes of which the molecular ion can produce one abundant daughter ion with high yield under CID conditions may be sensitively measured by SRM. ESI is the most soft ionization source developed so far and can afford formation of the fragile molecular ions that are necessary for sensitive SRM detection. Mild CID conditions such as low collision energy and low pressure of collision gas favor production of an abundant daughter ion that is essential to sensitive SRM detection. This knowledge may provide some guidelines for conducting sensitive SRM measurements of very low concentrations of drugs or toxicants in biological samples.

An orientation analysis method for protein immobilized on quantum dot particles

NASA Astrophysics Data System (ADS)

Aoyagi, Satoka; Inoue, Masae

2009-11-01

The evaluation of orientation of biomolecules immobilized on nanodevices is crucial for the development of high performance devices. Such analysis requires ultra high sensitivity so as to be able to detect less than one molecular layer on a device. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) has sufficient sensitivity to evaluate the uppermost surface structure of a single molecular layer. The objective of this study is to develop an orientation analysis method for proteins immobilized on nanomaterials such as quantum dot particles, and to evaluate the orientation of streptavidin immobilized on quantum dot particles by means of TOF-SIMS. In order to detect fragment ions specific to the protein surface, a monoatomic primary ion source (Ga +) and a cluster ion source (Au 3+) were employed. Streptavidin-immobilized quantum dot particles were immobilized on aminosilanized ITO glass plates at amino groups by covalent bonding. The reference samples streptavidin directly immobilized on ITO plates were also prepared. All samples were dried with a freeze dryer before TOF-SIMS measurement. The positive secondary ion spectra of each sample were obtained using TOF-SIMS with Ga + and Au 3+, respectively, and then they were compared so as to characterize each sample and detect the surface structure of the streptavidin immobilized with the biotin-immobilized quantum dots. The chemical structures of the upper surface of the streptavidin molecules immobilized on the quantum dot particles were evaluated with TOF-SIMS spectra analysis. The indicated surface side of the streptavidin molecules immobilized on the quantum dots includes the biotin binding site.

Detecting negative ions on board small satellites

NASA Astrophysics Data System (ADS)

Lepri, S. T.; Raines, J. M.; Gilbert, J. A.; Cutler, J.; Panning, M.; Zurbuchen, T. H.

2017-04-01

Recent measurements near comets, planets, and their satellites have shown that heavy ions, energetic neutral atoms, molecular ions, and charged dust contain a wealth of information about the origin, evolution, and interaction of celestial bodies with their space environment. Using highly sensitive plasma instruments, positively charged heavy ions have been used to trace exospheric and surface composition of comets, planets, and satellites as well as the composition of interplanetary and interstellar dust. While positive ions dominate throughout the heliosphere, negative ions are also produced from surface interactions. In fact, laboratory experiments have shown that oxygen released from rocky surfaces is mostly negatively charged. Negative ions and negatively charged nanograins have been detected with plasma electron analyzers in several different environments (e.g., by Cassini and Rosetta), though more extensive studies have been challenging without instrumentation dedicated to negative ions. We discuss an adaptation of the Fast Imaging Plasma Spectrometer (FIPS) flown on MErcury Surface, Space ENvironment, GEochemistry and Ranging (MESSENGER) for the measurement of negatively charged particles. MESSENGER/FIPS successfully measured the plasma environment of Mercury from 2011 until 2015, when the mission ended, and has been used to map multiple ion species (H+ through Na+ and beyond) throughout Mercury's space environment. Modifications to the existing instrument design fits within a 3U CubeSat volume and would provide a low mass, low power instrument, ideal for future CubeSat or distributed sensor missions seeking, for the first time, to characterize the contribution of negative particles in the heliospheric plasmas near the planets, moons, comets, and other sources.

IBIC characterisation of novel detectors for single atom doping of quantum computer devices

NASA Astrophysics Data System (ADS)

Yang, Changyi; Jamieson, David N.; Pakes, Chris I.; George, Damien P.; Hearne, Sean M.; Dzurak, Andrew S.; Gauja, Eric; Stanley, F.; Clark, R. G.

2003-09-01

Single ion implantation and online detection is highly desirable for the emerging application, in which single 31P ions need to be inserted in prefabricated silicon cells to construct solid-state quantum bits (qubits). In order to fabricate qubit arrays, we have developed novel detectors that employ detector electrodes adjacent to the prefabricated cells that can detect single keV ion strikes appropriate for the fabrication of shallow phosphorus arrays. The method utilises a high purity silicon substrate with very high resistivity, a thin SiO 2 surface layer, nanometer masks for the lateral positioning single phosphorus implantation, biased electrodes applied to the surface of the silicon and sensitive electronics that can detect the charge transient from single keV ion strikes. A TCAD (Technology Computer Aided Design) software package was applied in the optimisation of the device design and simulation of the detector performance. Here we show the characterisation of these detectors using ion beam induced charge (IBIC) with a focused 2 MeV He ions in a nuclear microprobe. The IBIC imaging method in a nuclear microprobe allowed us to measure the dead-layer thickness of the detector structure (required to be very thin for successful detection of keV ions), and the spatial distribution of the charge collection efficiency around the entire region of the detector. We show that our detectors have near 100% charge collection efficiency for MeV ions, extremely thin dead-layer thickness (about 7 nm) and a wide active region extending laterally from the electrodes (10-20 μm) where qubit arrays can be constructed. We demonstrate that the device can be successfully applied in the detection of keV ionisation energy from single events of keV X-rays and keV 31P ions.

Ultra-sensitive and selective Hg{sup 2+} detection based on fluorescent carbon dots

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ruihua; Li, Haitao; Kong, Weiqian

2013-07-15

Graphical abstract: Fluorescent carbon dots were efficiently synthesized by one-step sodium hydroxide-assisted reflux method from PEG and demonstrated to show high selectivity toward Hg2+ ions detection. - Highlights: • FCDs were synthesized by one-step sodium hydroxide-assisted reflux method from PEG. • The FCDs emit blue photoluminescence and have upconversion fluorescent property. • The FCDs show ultra-sensitive detective ability for Hg{sup 2+} ions. - Abstract: Fluorescent carbon dots (FCDs) were efficiently synthesized by one-step sodium hydroxide-assisted reflux method from poly(ethylene glycol) (PEG). The obtained FCDs exhibit excellent water-solubility and high stability. Under the UV irradiation, the FCDs could emit bright bluemore » photoluminescence, and also they were found to show excellent up-conversion fluorescence. It was further demonstrated that such FCDs can serve as effective fluorescent sensing platform for Hg{sup 2+} ions detection with ultra-sensitivity and selectivity. The sensing system achieved a limit of detection as low as 1 fM, which is much lower than all the previous reported sensing systems for Hg{sup 2+} ions detection. This FCDs sensing system has been successfully applied for the analysis of Hg{sup 2+} ions in water samples from river, lake, and tap water, showing good practical feasibility.« less

Detection and identification of immobilized low-volatility organophosphates by desorption ionization mass spectrometry

NASA Astrophysics Data System (ADS)

Hagan, Nathan A.; Cornish, Timothy J.; Pilato, Robert S.; van Houten, Kelly A.; Antoine, Miquel D.; Lippa, Timothy P.; Becknell, Alan F.; Demirev, Plamen A.

2008-12-01

Two desorption ionization mass spectrometry (MS) techniques - ultraviolet laser desorption/ionization (LDI) and desorption electrospray ionization (DESI) - have been used to detect and identify low-volatility organophosphates when deposited on surfaces or loaded into the pore volume of porous inorganic or polymeric organic powders. The insecticides malathion and dicrotophos were chosen for this study as simulants of low vapor pressure chemical warfare agents which are inherently difficult to detect directly by traditional methods. Both liquid and powdered forms of either insecticide were readily detected by LDI or DESI MS. LDI MS was performed on a miniaturized home-built time-of-flight (TOF) mass spectrometer and a commercial TOF/TOF instrument. For DESI MS, a home-built ion source was interfaced to a commercial quadrupole ion trap. In LDI, intact molecular ion signatures could be acquired by using an appropriate cationizing agent and powder additive in positive ion mode. Tandem MS was used to confirm the identity of each analyte based on the observed characteristic fragmentation pattern. In DESI, less than 100 pg of the liquid insecticides spotted on clean surfaces were detected, while detection limits for the powder-loaded preparations were lower than 1 [mu]g. The effects of sample surface, salt additives, nanoparticle admixtures, and analyte solubility on the LDI and DESI MS sensitivity have been investigated as well.

Highly sensitive and selective detection of Al(III) ions in aqueous buffered solution with fluorescent peptide-based sensor.

PubMed

In, Byunggyu; Hwang, Gi Won; Lee, Keun-Hyeung

2016-09-15

A fluorescent sensor based on a tripeptide (SerGluGlu) with a dansyl fluorophore detected selectively Al(III) among 16 metal ions in aqueous buffered solutions without any organic cosolvent. The peptide-based sensor showed a highly sensitive turn on response to aluminium ion with high binding affinity (1.84×10(4)M(-1)) in aqueous buffered solutions. The detection limit (230nM, 5.98ppb) of the peptide-based sensor was much lower than the maximum allowable level (7.41μM) of aluminium ions in drinking water demanded by EPA. The binding mode of the peptide sensor with aluminium ions was characterized using ESI mass spectrometry, NMR titration, and pH titration experiments. Copyright © 2016 Elsevier Ltd. All rights reserved.

Single-atom detection of isotopes

DOEpatents

Meyer, Fred W.

2002-01-01

A method for performing accelerator mass spectrometry, includes producing a beam of positive ions having different multiple charges from a multicharged ion source; selecting positive ions having a charge state of from +2 to +4 to define a portion of the beam of positive ions; and scattering at least a portion of the portion of the beam of positive ions off a surface of a target to directly convert a portion of the positive ions in the portion of the beam of positive ions to negative ions.

Evaluation of ion-implanted-silicon detectors for use in intraoperative positron-sensitive probes.

PubMed

Raylman, R R; Wahl, R L

1996-11-01

The continuing development of probes for use with beta (positron and electron) emitting radionuclides may result in more complete excision of tracer-avid tumors. Perhaps one of the most promising radiopharmaceuticals for this task is 18F-labeled-Fluoro-2-Deoxy-D-Glucose (FDG). This positron-emitting agent has been demonstrated to be avidly and rapidly absorbed by many human cancers. We have investigated the use of ion-implanted-silicon detectors in intraoperative positron-sensitive surgical probes for use with FDG. These detectors possess very high positron detection efficiency, while the efficiency for 511 keV photon detection is low. The spatial resolution, as well as positron and annihilation photon detection sensitivity, of an ion-implanted-silicon detector used with 18F was measured at several energy thresholds. In addition, the ability of the device to detect the presence of relatively small amounts of FDG during surgery was evaluated by simulating a surgical field in which some tumor was left intact following lesion excision. The performance of the ion-implanted-silicon detector was compared to the operating characteristics of a positron-sensitive surgical probe which utilizes plastic scintillator. In all areas of performance the ion-implanted-silicon detector proved superior to the plastic scintillator-based probe. At an energy threshold of 14 keV positron sensitivity measured for the ion-implanted-silicon detector was 101.3 cps/kBq, photon sensitivity was 7.4 cps/kBq. In addition, spatial resolution was found to be relatively unaffected by the presence of distant sources of annihilation photon flux. Finally, the detector was demonstrated to be able to localize small amounts of FDG in a simulated tumor bed; indicating that this device has promise as a probe to aid in FDG-guided surgery.

Ion mobility analyzer - quadrupole mass spectrometer system design

NASA Astrophysics Data System (ADS)

Cuna, C.; Leuca, M.; Lupsa, N.; Mirel, V.; Bocos-Bintintan, V.; Cuna, Stela; Cosma, V.; Tusa, Florina

2009-08-01

Because of their extremely high sensitivity for chemicals with elevated electronegativity or high proton affinity the ion mobility analysers are ideal for the ultra-trace detection of toxic or explosive chemicals, most of these situated often at concentration levels of sub-ppb (parts-per-billion). Ion mobility spectrometers (IMS) can be used to identify illicit drugs or environmental pollutants. Since resolution of an IMS is relatively low, to achieve an accurate identification of target analyte it is recommended to couple the IMS with a quadrupole mass spectrometer (QMS) or a time of flight mass spectrometer, acquiring in this way confirmatory information. This coupling is made through a specific interface. In this paper, an experimental model of such a tandem instrument, IMS-QMS is described. Accomplishment of this general purpose will be done, overcoming a series of specific issues. This implies the solving, using innovative solutions, of a series of complex issues: ensuring the stability of the ions beam generated by ion source; transfer with a good efficiency of the ionic current from IMS analyser to QMS; and realization of a special electronic circuitry which will be able to detect both positive and negative ions.

Label-free signal-on aptasensor for sensitive electrochemical detection of arsenite.

PubMed

Cui, Lin; Wu, Jie; Ju, Huangxian

2016-05-15

A signal-on aptasensor was fabricated for highly sensitive and selective electrochemical detection of arsenite with a label-free Ars-3 aptamer self-assembled on a screen-printed carbon electrode (SPCE) via Au-S bond. The Ars-3 aptamer could adsorb cationic polydiallyldimethylammonium (PDDA) via electrostatic interaction to repel other cationic species. In the presence of arsenite, the change of Ars-3 conformation due to the formation of Ars-3/arsenite complex led to less adsorption of PDDA, and the complex could adsorb more positively charged [Ru(NH3)6](3+) as an electrochemically active indicator on the aptasensor surface, which produced a sensitive "turn-on" response. The target-induced structure switching could be used for sensitive detection of arsenite with a linear range from 0.2 nM to 100 nM and a detection limit down to 0.15 nM. Benefiting from Ars-3 aptamer, the proposed system exhibited excellent specificity against other heavy metal ions. The SPCE-based aptasensor exhibited the advantages of low cost and simple fabrication, providing potential application of arsenite detection in environment. Copyright © 2016 Elsevier B.V. All rights reserved.

Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

PubMed

Sklerov, J H; Kalasinsky, K S; Ehorn, C A

1999-10-01

A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were < 6% and < 13%, respectively. This procedure has been applied to quality-control specimens and LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

A Strategy for Sensitive, Large Scale Quantitative Metabolomics

PubMed Central

Liu, Xiaojing; Ser, Zheng; Cluntun, Ahmad A.; Mentch, Samantha J.; Locasale, Jason W.

2014-01-01

Metabolite profiling has been a valuable asset in the study of metabolism in health and disease. However, current platforms have different limiting factors, such as labor intensive sample preparations, low detection limits, slow scan speeds, intensive method optimization for each metabolite, and the inability to measure both positively and negatively charged ions in single experiments. Therefore, a novel metabolomics protocol could advance metabolomics studies. Amide-based hydrophilic chromatography enables polar metabolite analysis without any chemical derivatization. High resolution MS using the Q-Exactive (QE-MS) has improved ion optics, increased scan speeds (256 msec at resolution 70,000), and has the capability of carrying out positive/negative switching. Using a cold methanol extraction strategy, and coupling an amide column with QE-MS enables robust detection of 168 targeted polar metabolites and thousands of additional features simultaneously.  Data processing is carried out with commercially available software in a highly efficient way, and unknown features extracted from the mass spectra can be queried in databases. PMID:24894601

ICan: An Optimized Ion-Current-Based Quantification Procedure with Enhanced Quantitative Accuracy and Sensitivity in Biomarker Discovery

PubMed Central

2015-01-01

The rapidly expanding availability of high-resolution mass spectrometry has substantially enhanced the ion-current-based relative quantification techniques. Despite the increasing interest in ion-current-based methods, quantitative sensitivity, accuracy, and false discovery rate remain the major concerns; consequently, comprehensive evaluation and development in these regards are urgently needed. Here we describe an integrated, new procedure for data normalization and protein ratio estimation, termed ICan, for improved ion-current-based analysis of data generated by high-resolution mass spectrometry (MS). ICan achieved significantly better accuracy and precision, and lower false-positive rate for discovering altered proteins, over current popular pipelines. A spiked-in experiment was used to evaluate the performance of ICan to detect small changes. In this study E. coli extracts were spiked with moderate-abundance proteins from human plasma (MAP, enriched by IgY14-SuperMix procedure) at two different levels to set a small change of 1.5-fold. Forty-five (92%, with an average ratio of 1.71 ± 0.13) of 49 identified MAP protein (i.e., the true positives) and none of the reference proteins (1.0-fold) were determined as significantly altered proteins, with cutoff thresholds of ≥1.3-fold change and p ≤ 0.05. This is the first study to evaluate and prove competitive performance of the ion-current-based approach for assigning significance to proteins with small changes. By comparison, other methods showed remarkably inferior performance. ICan can be broadly applicable to reliable and sensitive proteomic survey of multiple biological samples with the use of high-resolution MS. Moreover, many key features evaluated and optimized here such as normalization, protein ratio determination, and statistical analyses are also valuable for data analysis by isotope-labeling methods. PMID:25285707

Coordination ability determined transition metal ions substitution of Tb in Tb-Asp fluorescent nanocrystals and a facile ions-detection approach.

PubMed

Duan, Jiazhi; Ma, Baojin; Liu, Feng; Zhang, Shan; Wang, Shicai; Kong, Ying; Du, Min; Han, Lin; Wang, Jianjun; Sang, Yuanhua; Liu, Hong

2018-04-26

Although the synthesis and fluorescent properties of lanthanide-amino acid complex nanostructures have been investigated extensively, limited studies have been reported on metal ions' substitution ability for the lanthanide ions in the complex and their effect on the fluorescent property. In this study, taking biocompatible Tb-aspartic acid (Tb-Asp) complex nanocrystals as a model, the substitution mechanism of metal ions, particularly transition metals, for Tb ions in Tb-Asp nanocrystals and the change in the fluorescent property of the Tb-Asp nanocrystals after substitution were systematically investigated. The experimental results illustrated that metal ions with higher electronegativity, higher valence, and smaller radius possess stronger ability for Tb ions' substitution in Tb-Asp nanocrystals. Based on the effect of substituting ions' concentration on the fluorescent property of Tb-Asp, a facile method for copper ions detection with high sensitivity was proposed by measuring the fluorescent intensity of Tb-Asp nanocrystals' suspensions containing different concentrations of copper ions. The good biocompatibility, great convenience of synthesis and sensitive detection ability make Tb-Asp nanocrystals a very low cost and effective material for metal ions detection, which also opens a new door for practical applications of metal-Asp coordinated nanocrystals.

Some Rare Earth Elements Analysis by Microwave Plasma Torch Coupled with the Linear Ion Trap Mass Spectrometry

PubMed Central

Xiong, Xiaohong; Jiang, Tao; Qi, Wenhao; Zuo, Jun; Yang, Meiling; Fei, Qiang; Xiao, Saijin; Yu, Aimin; Zhu, Zhiqiang; Chen, Huanwen

2015-01-01

A sensitive mass spectrometric analysis method based on the microwave plasma technique is developed for the fast detection of trace rare earth elements (REEs) in aqueous solution. The plasma was produced from a microwave plasma torch (MPT) under atmospheric pressure and was used as ambient ion source of a linear ion trap mass spectrometer (LTQ). Water samples were directly pneumatically nebulized to flow into the plasma through the central tube of MPT. For some REEs, the generated composite ions were detected in both positive and negative ion modes and further characterized in tandem mass spectrometry. Under the optimized conditions, the limit of detection (LOD) was at the level 0.1 ng/mL using MS2 procedure in negative mode. A single REE analysis can be completed within 2~3 minutes with the relative standard deviation ranging between 2.4% and 21.2% (six repeated measurements) for the 5 experimental runs. Moreover, the recovery rates of these REEs are between the range of 97.6%–122.1%. Two real samples have also been analyzed, including well and orange juice. These experimental data demonstrated that this method is a useful tool for the field analysis of REEs in water and can be used as an alternative supplement of ICP-MS. PMID:26421013

Simultaneous determination of asperosaponin VI and its active metabolite hederagenin in rat plasma by liquid chromatography-tandem mass spectrometry with positive/negative ion-switching electrospray ionization and its application in pharmacokinetic study.

PubMed

Zhu, He; Ding, Li; Shakya, Shailendra; Qi, Xiemin; Hu, Linlin; Yang, Xiaolin; Yang, Zhonglin

2011-11-15

A new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method operated in the positive/negative electrospray ionization (ESI) switching mode has been developed and validated for the simultaneous determination of asperosaponin VI and its active metabolite hederagenin in rat plasma. After addition of internal standards diazepam (for asperosaponin VI) and glycyrrhetic acid (for hederagenin), the plasma sample was deproteinized with acetonitrile, and separated on a reversed phase C18 column with a mobile phase of methanol (solvent A)-0.05% glacial acetic acid containing 10 mM ammonium acetate and 30 μM sodium acetate (solvent B) using gradient elution. The detection of target compounds was done in multiple reaction monitoring (MRM) mode using a tandem mass spectrometry equipped with positive/negative ion-switching ESI source. At the first segment, the MRM detection was operated in the positive ESI mode using the transitions of m/z 951.5 ([M+Na](+))→347.1 for asperosaponin VI and m/z 285.1 ([M+H](+))→193.1 for diazepam for 4 min, then switched to the negative ESI mode using the transitions of m/z 471.3 ([M-H](-))→471.3 for hederagenin and m/z 469.4 ([M-H](-))→425.4 for glycyrrhetic acid, respectively. The sodiated molecular ion [M+Na](+) at m/z 951.5 was selected as the precursor ion for asperosaponin VI, since it provided better sensitivity compared to the deprotonated and protonated molecular ions. Sodium acetate was added to the mobile phase to make sure that abundant amount of the sodiated molecular ion of asperosaponin VI could be produced, and more stable and intensive mass response of the product ion could be obtained. For the detection of hederagenin, since all of the mass responses of the fragment ions were very weak, the deprotonated molecular ion [M-H](-)m/z 471.3 was employed as both the precursor ion and the product ion. But the collision energy was still used for the MRM, in order to eliminate the influences induced by the interference substances from the rat plasma. The validated method was successfully applied to study the pharmacokinetics of asperosaponin VI and its active metabolite hederagenin in rat plasma after oral administration of asperosaponin VI at a dose of 90 mg/kg. Copyright © 2011 Elsevier B.V. All rights reserved.

New, high-efficiency ion trap mobility detection system for narcotics and explosives

NASA Astrophysics Data System (ADS)

McGann, William J.; Bradley, V.; Borsody, A.; Lepine, S.

1994-10-01

A new patented Ion Trap Mobility Spectrometer (ITMS) design is presented. Conventional IMS designs typically operate below 0.1% efficiency. This is due primarily to electric field driven, sample ion discharge on a shutter grid. Since 99.9% of the sample ions generated in the reaction region are lost in this discharge process, the sensitivity of conventional systems is limited. The new design provides greater detection efficiency than conventional designs through the use of an `ion trap' concept. The paper describes the plasma and sample ion dynamics in the reaction region of the new detector and discusses the advantages of utilizing a `field-free' space to generate sample ions with high efficiency. Fast electronic switching is described which is used to perturb the field-free space and pulse the sample ions into the drift region for separation and subsequent detection using pseudo real-time software for analysis and display of the data. Many applications for this new detector are now being considered including the detection of narcotics and explosives. Preliminary ion spectra, reduced mobility data and sensitivity data are presented for fifteen narcotics, including cocaine, THC and LSD are reported.

New high-efficiency ion-trap mobility detection system for narcotics

NASA Astrophysics Data System (ADS)

McGann, William J.

1997-02-01

A new patented Ion Trap Mobility Spectrometer design is presented. Conventional IMS designs typically operate below 0.1 percent efficiency. This is due primarily to electric field driven, sample ion discharge on a shutter grid. Since 99.9 percent of the sample ions generated in the reaction region are lost int his discharge process, the sensitivity of conventional systems is limited. The new design provides greater detection efficiency than conventional designs through the use of an 'ion trap' concept. The paper describes the plasma and sample ion dynamics in the reaction region of the new detector and discusses the advantages of utilizing a 'field-free' space to generate sample ions with high efficiency. Fast electronic switching is described which is used to perturb the field-free space and pulse the sample ions into the drift region for separation and subsequent detection using pseudo real-time software for analysis and display of the data. One application for this new detector is now being developed, a portable, hand-held system with switching capability for the detection of drugs and explosives. Preliminary ion spectra and sensitivity data are presented for cocaine and heroin using a hand sniffer configuration.

New high-efficiency ion trap mobility detection system for narcotics and explosives

NASA Astrophysics Data System (ADS)

McGann, William J.; Jenkins, Anthony; Ribiero, K.; Napoli, J.

1994-03-01

A new patented ion trap mobility spectrometer design is presented. Conventional IMS designs typically operate below 0.1% efficiency. This is due primarily to electrical-field-driven, sample ion discharge on a shutter grid. Since 99.9% of the sample ions generated in the reaction region are lost in this discharge process, the sensitivity of conventional systems is limited. The new design provides greater detection efficiency than conventional designs through the use of an `ion trap' concept. The paper describes the plasma and sample ion dynamics in the reaction region of the new detector and discusses the advantages of utilizing a `field-free' space to generate sample ions with high efficiency. Fast electronic switching is described which is used to perturb the field-free space and pulse the sample ions into the drift region for separation and subsequent detection using pseudo real-time software for analysis and display of the data. Many applications for this new detector are now being considered including the detection of narcotics and explosives. Preliminary ion spectra, reduced mobility data and sensitivity data are presented for fifteen narcotics, including cocaine, THC, and LSD are reported.

Highly sensitive heavy metal ion detection using AlQ3 microwire functionalized QCM

NASA Astrophysics Data System (ADS)

Can, Nursel; Aǧar, Meltem; Altındal, Ahmet

2016-03-01

Tris(8-hydroxyquinoline) aluminum (Alq3) microwires was successfully synthesized for the fabrication of Alq3 microwires-coated QCM sensors to detect the heavy metal ions in aqueous solution. AT-cut quartz crystal microbalance (QCM) of 10 MHz fundamental resonance frequency having gold electrodes were used as transducers. Typical measuring cycle consisted of repeated flow of target measurands through the flow cell and subsequent washing to return the baseline. The QCM results indicated that the Alq3 microwires exhibit excellent sensitivity, stability and short response-recovery time, which are much attractive for the development of portable and highly sensitive heavy metal ion sensors in water samples.

Highly Sensitive Aluminium(III) Ion Sensor Based on a Self-assembled Monolayer on a Gold Nanoparticles Modified Screen-printed Carbon Electrode.

PubMed

See, Wong Pooi; Heng, Lee Yook; Nathan, Sheila

2015-01-01

A new approach for the development of a highly sensitive aluminium(III) ion sensor via the preconcentration of aluminium(III) ion with a self-assembled monolayer on a gold nanoparticles modified screen-printed carbon electrode and current mediation by potassium ferricyanide redox behavior during aluminium(III) ion binding has been attempted. A monolayer of mercaptosuccinic acid served as an effective complexation ligand for the preconcentration of trace aluminium; this led to an enhancement of aluminium(III) ion capture and thus improved the sensitivity of the sensor with a detection limit of down to the ppb level. Under the optimum experimental conditions, the sensor exhibited a wide linear dynamic range from 0.041 to 12.4 μM. The lower detection limit of the developed sensor was 0.037 μM (8.90 ppb) using a 10 min preconcentration time. The sensor showed excellent selectivity towards aluminium(III) ion over other interference ions.

Electrochemical sensing of heavy metal ions with inorganic, organic and bio-materials.

PubMed

Cui, Lin; Wu, Jie; Ju, Huangxian

2015-01-15

As heavy metal ions severely harm human health, it is important to develop simple, sensitive and accurate methods for their detection in environment and food. Electrochemical detection featured with short analytical time, low power cost, high sensitivity and easy adaptability for in-situ measurement is one of the most developed methods. This review introduces briefly the recent achievements in electrochemical sensing of heavy metal ions with inorganic, organic and bio-materials modified electrodes. In particular, the unique properties of inorganic nanomaterials, organic small molecules or their polymers, enzymes and nucleic acids for detection of heavy metal ions are highlighted. By employing some representative examples, the design and sensing mechanisms of these electrodes are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Selective and Sensitive Detection of Heavy Metal Ions in 100% Aqueous Solution and Cells with a Fluorescence Chemosensor Based on Peptide Using Aggregation-Induced Emission.

PubMed

Neupane, Lok Nath; Oh, Eun-Taex; Park, Heon Joo; Lee, Keun-Hyeung

2016-03-15

A fluorescent peptidyl chemosensor for the detection of heavy metal ions in aqueous solution as well as in cells was synthesized on the basis of the peptide receptor for the metal ions using an aggregation-induced emission fluorophore. The peptidyl chemosensor (1) bearing tetraphenylethylene fluorophore showed an exclusively selective turn-on response to Hg(2+) among 16 metal ions in aqueous buffered solution containing NaCl. The peptidyl chemosensor complexed Hg(2+) ions and then aggregated in aqueous buffered solution, resulting in the significant enhancement (OFF-On) of emissions at around 470 nm. The fluorescent sensor showed a highly sensitive response to Hg(2+), and about 1.0 equiv of Hg(2+) was enough for the saturation of the emission intensity change. The detection limit (5.3 nM, R(2) = 0.99) of 1 for Hg(2+) ions was lower than the maximum allowable level of Hg(2+) in drinking water by EPA. Moreover, the peptidyl chemosensor penetrated live cells and detected intracellular Hg(2+) ions by the turn-on response.

Efficient ensemble system based on the copper binding motif for highly sensitive and selective detection of cyanide ions in 100% aqueous solutions by fluorescent and colorimetric changes.

PubMed

Jung, Kwan Ho; Lee, Keun-Hyeung

2015-09-15

A peptide-based ensemble for the detection of cyanide ions in 100% aqueous solutions was designed on the basis of the copper binding motif. 7-Nitro-2,1,3-benzoxadiazole-labeled tripeptide (NBD-SSH, NBD-SerSerHis) formed the ensemble with Cu(2+), leading to a change in the color of the solution from yellow to orange and a complete decrease of fluorescence emission. The ensemble (NBD-SSH-Cu(2+)) sensitively and selectively detected a low concentration of cyanide ions in 100% aqueous solutions by a colorimetric change as well as a fluorescent change. The addition of cyanide ions instantly removed Cu(2+) from the ensemble (NBD-SSH-Cu(2+)) in 100% aqueous solutions, resulting in a color change of the solution from orange to yellow and a "turn-on" fluorescent response. The detection limits for cyanide ions were lower than the maximum allowable level of cyanide ions in drinking water set by the World Health Organization. The peptide-based ensemble system is expected to be a potential and practical way for the detection of submicromolar concentrations of cyanide ions in 100% aqueous solutions.

Click chemistry-mediated cyclic cleavage of metal ion-dependent DNAzymes for amplified and colorimetric detection of human serum copper (II).

PubMed

Li, Daxiu; Xie, Jiaqing; Zhou, Wenjiao; Jiang, Bingying; Yuan, Ruo; Xiang, Yun

2017-11-01

The determination of the level of Cu 2+ plays important roles in disease diagnosis and environmental monitoring. By coupling Cu + -catalyzed click chemistry and metal ion-dependent DNAzyme cyclic amplification, we have developed a convenient and sensitive colorimetric sensing method for the detection of Cu 2+ in human serums. The target Cu 2+ can be reduced by ascorbate to form Cu + , which catalyzes the azide-alkyne cycloaddition between the azide- and alkyne-modified DNAs to form Mg 2+ -dependent DNAzymes. Subsequently, the Mg 2+ ions catalyze the cleavage of the hairpin DNA substrate sequences of the DNAzymes and trigger cyclic generation of a large number of free G-quadruplex sequences, which bind hemin to form the G-quadruplex/hemin artificial peroxidase to cause significant color transition of the sensing solution for sensitive colorimetric detection of Cu 2+ . This method shows a dynamic range of 5 to 500 nM and a detection limit of 2 nM for Cu 2+ detection. Besides, the level of Cu 2+ in human serums can also be determined by using this sensing approach. With the advantages of simplicity and high sensitivity, such sensing method thus holds great potential for on-site determination of Cu 2+ in different samples. Graphical abstract Sensitive colorimetric detection of copper (II) by coupling click chemistry with metal ion-dependentDNAzymes.

Detection of methamphetamine in the presence of nicotine using in situ chemical derivatization and ion mobility spectrometry.

PubMed

Ochoa, Mariela L; Harrington, Peter B

2004-02-15

The detection of methamphetamine in the presence of nicotine has been successfully accomplished using in situ chemical derivatization with propyl chloroformate as the derivatization reagent and ion mobility spectrometry (IMS). The rapid detection of methamphetamine is important for forensic scientists in order to establish a chain of evidence and link criminals to the crime scene. Nicotine is pervasive in clandestine drug laboratories from cigarette smoke residue. It has been demonstrated that nicotine obscures the methamphetamine peaks in ion mobility spectrometers due to their similar charge affinities and ion mobilities, which makes their detection a challenging task. As a consequence, false positive or negative responses may arise. In situ chemical derivatization poses as a sensitive, accurate, and reproducible alternative to remove the nicotine background when detecting nanogram amounts of methamphetamine. The derivatization agent was coated onto the sample disk, and the derivatization product corresponding to propyl methamphetamine carbamate was detected. In the present study, in situ chemical derivatization was demonstrated to be a feasible method to detect methamphetamine hydrochloride as the carbamate derivative, which was baseline-resolved from the nicotine peak. Alternating least squares (ALS) was used to model the datasets. A mixture containing both compounds revealed reduced mobilities of 1.61 cm(2)/V.s and 1.54 cm(2)/V.s for methamphetamine and nicotine, respectively. The reduced mobility of propyl methamphetamine carbamate was found at 1.35 cm(2)/V.s.

Highly Sensitive and Patchable Pressure Sensors Mimicking Ion-Channel-Engaged Sensory Organs.

PubMed

Chun, Kyoung-Yong; Son, Young Jun; Han, Chang-Soo

2016-04-26

Biological ion channels have led to much inspiration because of their unique and exquisite operational functions in living cells. Specifically, their extreme and dynamic sensing abilities can be realized by the combination of receptors and nanopores coupled together to construct an ion channel system. In the current study, we demonstrated that artificial ion channel pressure sensors inspired by nature for detecting pressure are highly sensitive and patchable. Our ion channel pressure sensors basically consisted of receptors and nanopore membranes, enabling dynamic current responses to external forces for multiple applications. The ion channel pressure sensors had a sensitivity of ∼5.6 kPa(-1) and a response time of ∼12 ms at a frequency of 1 Hz. The power consumption was recorded as less than a few μW. Moreover, a reliability test showed stability over 10 000 loading-unloading cycles. Additionally, linear regression was performed in terms of temperature, which showed no significant variations, and there were no significant current variations with humidity. The patchable ion channel pressure sensors were then used to detect blood pressure/pulse in humans, and different signals were clearly observed for each person. Additionally, modified ion channel pressure sensors detected complex motions including pressing and folding in a high-pressure range (10-20 kPa).

High sensitive detection of copper II ions using D-penicillamine-coated gold nanorods based on localized surface plasmon resonance.

PubMed

Hong, Yoochan; Jo, Seongjae; Park, Joohyung; Park, Jinsung; Yang, Jaemoon

2018-05-25

In this paper, we describe the development of a nanoplasmonic biosensor based on the localized surface plasmon resonance (LSPR) effect that enables a sensitive and selective recognition of copper II ions. First, we fabricated the nanoplasmonics as LSPR substrates using gold nanorods (GNR) and the nano-adsorption method. The LSPR sensitivity of the nanoplasmonics was evaluated using various solvents with different refractive indexes. Subsequently, D-penicillamine (DPA)-a chelating agent of copper II ions-was conjugated to the surface of the GNR. The limit of detection (LOD) for the DPA-conjugated nanoplasmonics was 100 pM. Furthermore, selectivity tests were conducted using various divalent cations, and sensitivity tests were conducted on the nanoplasmonics under blood-like environments. Finally, the developed nanoplasmonic biosensor based on GNR shows great potential for the effective recognition of copper II ions, even in human blood conditions.

Detection of reactive metabolites using isotope-labeled glutathione trapping and simultaneous neutral loss and precursor ion scanning with ultra-high-pressure liquid chromatography triple quadruple mass spectrometry.

PubMed

Huang, Ke; Huang, Lingyi; van Breemen, Richard B

2015-04-07

Metabolic activation of drugs to electrophilic species is responsible for over 60% of black box warnings and drug withdrawals from the market place in the United States. Reactive metabolite trapping using glutathione (GSH) and analysis using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) or HPLC with high resolution mass spectrometry (mass defect filtering) have enabled screening for metabolic activation to become routine during drug development. However, current MS-based approaches cannot detect all GSH conjugates present in complex mixtures, especially those present in extracts of botanical dietary supplements. To overcome these limitations, a fast triple quadrupole mass spectrometer-based approach was developed that can detect positively and negatively charged GSH conjugates in a single analysis without the need for advanced knowledge of the elemental compositions of potential conjugates and while avoiding false positives. This approach utilized UHPLC instead of HPLC to shorten separation time and enhance sensitivity, incorporated stable-isotope labeled GSH to avoid false positives, and used fast polarity switching electrospray MS/MS to detect GSH conjugates that form positive and/or negative ions. The general new method was then used to test the licorice dietary supplement Glycyrrhiza glabra, which was found to form multiple GSH conjugates upon metabolic activation. Among the GSH conjugates found in the licorice assay were conjugates with isoliquiritigenin and glabridin, which is an irreversible inhibitor of cytochrome P450 enzymes.

Application of Polypyrrole Multi-Walled Carbon Nanotube Composite Layer for Detection of Mercury, Lead and Iron Ions Using Surface Plasmon Resonance Technique

PubMed Central

Sadrolhosseini, Amir Reza; Noor, A. S. M.; Bahrami, Afarin; Lim, H. N.; Talib, Zainal Abidin; Mahdi, Mohd. Adzir

2014-01-01

Polypyrrole multi-walled carbon nanotube composite layers were used to modify the gold layer to measure heavy metal ions using the surface plasmon resonance technique. The new sensor was fabricated to detect trace amounts of mercury (Hg), lead (Pb), and iron (Fe) ions. In the present research, the sensitivity of a polypyrrole multi-walled carbon nanotube composite layer and a polypyrrole layer were compared. The application of polypyrrole multi-walled carbon nanotubes enhanced the sensitivity and accuracy of the sensor for detecting ions in an aqueous solution due to the binding of mercury, lead, and iron ions to the sensing layer. The Hg ion bonded to the sensing layer more strongly than did the Pb and Fe ions. The limitation of the sensor was calculated to be about 0.1 ppm, which produced an angle shift in the region of 0.3° to 0.6°. PMID:24733263

Rapid Trace Detection and Isomer Quantitation of Pesticide Residues via Matrix-Assisted Laser Desorption/Ionization Fourier Transform Ion Cyclotron Resonance Mass Spectrometry.

PubMed

Wu, Xinzhou; Li, Weifeng; Guo, Pengran; Zhang, Zhixiang; Xu, Hanhong

2018-04-18

Matrix-assisted laser desorption/ionization Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR-MS) has been applied for rapid, sensitive, undisputed, and quantitative detection of pesticide residues on fresh leaves with little sample pretreatment. Various pesticides (insecticides, bactericides, herbicides, and acaricides) are detected directly in the complex matrix with excellent limits of detection down to 4 μg/L. FTICR-MS could unambiguously identify pesticides with tiny mass differences (∼0.017 75 Da), thereby avoiding false-positive results. Remarkably, pesticide isomers can be totally discriminated by use of diagnostic fragments, and quantitative analysis of pesticide isomers is demonstrated. The present results expand the horizons of the MALDI-FTICR-MS platform in the reliable determination of pesticides, with integrated advantages of ultrahigh mass resolution and accuracy. This method provides growing evidence for the resultant detrimental effects of pesticides, expediting the identification and evaluation of innovative pesticides.

DEVELOPMENT OF A METHOD FOR THE OBSERVATION OF LIGHTNING IN PROTOPLANETARY DISKS USING ION LINES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Muranushi, Takayuki; Akiyama, Eiji; Inutsuka, Shu-ichiro

2015-12-20

In this paper, we propose observational methods for detecting lightning in protoplanetary disks. We do so by calculating the critical electric field strength in the lightning matrix gas (LMG), the parts of the disk where the electric field is strong enough to cause lightning. That electric field accelerates multiple positive ion species to characteristic terminal velocities. In this paper, we present three distinct discharge models with corresponding critical electric fields. We simulate the position–velocity diagrams and the integrated emission maps for the models. We calculate the measure-of-sensitivity values for detection of the models and for distinguishing between the models. Atmore » the distance of TW Hya (54 pc), LMG that occupies 2π in azimuth and has 25 AU < r < 50 AU is detectable at 1200σ to 4000σ. The lower limits of the radii of 5σ-detectable LMG clumps are between 1.6 AU and 5.3 AU, depending on the models.« less

Mass spectrometer characterization of halogen gases in air at atmospheric pressure.

PubMed

Ivey, Michelle M; Foster, Krishna L

2005-03-01

We have developed a new interface for a commercial ion trap mass spectrometer equipped with APCI capable of real-time measurements of gaseous compounds with limits of detection on the order of pptv. The new interface has been tested using the detection of Br2 and Cl2 over synthetic seawater ice at atmospheric pressure as a model system. A mechanical pump is used to draw gaseous mixtures through a glass manifold into the corona discharge area, where the molecules are ionized. Analysis of bromine and chlorine in dry air show that ion intensity is affected by the pumping rate and the position of the glass manifold. The mass spectrometer signals for Br2 are linear in the 0.1-10.6 ppbv range, and the estimated 3sigma detection limit is 20 pptv. The MS signals for Cl2 are linear in the 0.2-25 ppbv range, and the estimated 3sigma detection limit is 1 ppbv. This new interface advances the field of analytical chemistry by introducing a practical modification to a commercially available ion trap mass spectrometer that expands the available methods for performing highly specific and sensitive measurements of gases in air at atmospheric pressure.

Ion Fluxes in Giant Excised Cardiac Membrane Patches Detected and Quantified with Ion-selective Microelectrodes

PubMed Central

Kang, Tong Mook; Markin, Vladislav S.; Hilgemann, Donald W.

2003-01-01

We have used ion-selective electrodes (ISEs) to quantify ion fluxes across giant membrane patches by measuring and simulating ion gradients on both membrane sides. Experimental conditions are selected with low concentrations of the ions detected on the membrane side being monitored. For detection from the cytoplasmic (bath) side, the patch pipette is oscillated laterally in front of an ISE. For detection on the extracellular (pipette) side, ISEs are fabricated from flexible quartz capillary tubing (tip diameters, 2–3 microns), and an ISE is positioned carefully within the patch pipette with the tip at a controlled distance from the mouth of the patch pipette. Transport activity is then manipulated by solution changes on the cytoplasmic side. Ion fluxes can be quantified by simulating the ion gradients with appropriate diffusion models. For extracellular (intrapatch pipette) recordings, ion diffusion coefficients can be determined from the time courses of concentration changes. The sensitivity and utility of the methods are demonstrated with cardiac membrane patches by measuring (a) potassium fluxes via ion channels, valinomycin, and Na/K pumps; (b) calcium fluxes mediated by Na/Ca exchangers; (c) sodium fluxes mediated by gramicidin and Na/K pumps; and (d) proton fluxes mediated by an unknown electrogenic mechanism. The potassium flux-to-current ratio for the Na/K pump is approximately twice that determined for potassium channels and valinomycin, as expected for a 3Na/2K pump stoichiometery (i.e., 2K/charge moved). For valinomycin-mediated potassium currents and gramicidin-mediated sodium currents, the ion fluxes calculated from diffusion models are typically 10–15% smaller than expected from the membrane currents. As presently implemented, the ISE methods allow reliable detection of calcium and proton fluxes equivalent to monovalent cation currents <1 pA in magnitude, and they allow detection of sodium and potassium fluxes equivalent to <5 pA currents. The capability to monitor ion fluxes, independent of membrane currents, should facilitate studies of both electrogenic and electroneutral ion–coupled transporters in giant patches. PMID:12668735

Mass spectrometric characterization of a high-field asymmetric waveform ion mobility spectrometer

NASA Astrophysics Data System (ADS)

Purves, Randy W.; Guevremont, Roger; Day, Stephen; Pipich, Charles W.; Matyjaszczyk, Matthew S.

1998-12-01

Ion mobility spectrometry (IMS) has become an important method for the detection of many compounds because of its high sensitivity and amenability to miniaturization for field-portable monitoring; applications include detection of narcotics, explosives, and chemical warfare agents. High-field asymmetric waveform ion mobility spectrometry (FAIMS) differs from IMS in that the electric fields are applied using a high-frequency periodic asymmetric waveform, rather than a dc voltage. Furthermore, in FAIMS the compounds are separated by the difference in the mobility of ions at high electric field relative to low field, rather than by compound to compound differences in mobility at low electric field (IMS). We report here the first cylindrical-geometry-FAIMS interface with mass spectrometry (FAIMS-MS) and the MS identification of the peaks observed in a FAIMS compensation voltage (CV) spectrum. Using both an electrometer-based-FAIMS (FAIMS-E) and FAIMS-MS, several variables that affect the sensitivity of ion detection were examined for two (polarity reversed) asymmetric waveforms (modes 1 and 2) each of which yields a unique spectrum. An increase in the dispersion voltage (DV) was found to improve the sensitivity and separation observed in the FAIMS CV spectrum. This increase in sensitivity and the unexpected dissimilarity in modes 1 and 2 suggest that atmospheric pressure ion focusing is occurring in the FAIMS analyzer. The sensitivity and peak locations in the CV spectra were affected by temperature, gas flow rates, operating pressure, and analyte concentration.

Collection of ions

DOEpatents

Orr, Christopher Henry; Luff, Craig Janson; Dockray, Thomas; Macarthur, Duncan Whittemore; Bounds, John Alan; Koster, James E.

2001-01-01

The apparatus and method provide an improved technique for detecting ions as the area from which ions are attracted to a detector is increased, consequently increasing the number of ions detected. This is achieved by providing the outer electrodes of the detector connected to the electrical potential, together with alternate intermediate electrodes. The other intermediate electrodes and preferably the housing are grounded. The technique renders such detection techniques more sensitive and gives them a lower threshold at which they can function.

A catalytic beacon sensor for uranium with parts-per-trillion sensitivity and millionfold selectivity.

PubMed

Liu, Juewen; Brown, Andrea K; Meng, Xiangli; Cropek, Donald M; Istok, Jonathan D; Watson, David B; Lu, Yi

2007-02-13

Here, we report a catalytic beacon sensor for uranyl (UO2(2+)) based on an in vitro-selected UO2(2+)-specific DNAzyme. The sensor consists of a DNA enzyme strand with a 3' quencher and a DNA substrate with a ribonucleotide adenosine (rA) in the middle and a fluorophore and a quencher at the 5' and 3' ends, respectively. The presence of UO2(2+) causes catalytic cleavage of the DNA substrate strand at the rA position and release of the fluorophore and thus dramatic increase of fluorescence intensity. The sensor has a detection limit of 11 parts per trillion (45 pM), a dynamic range up to 400 nM, and selectivity of >1-million-fold over other metal ions. The most interfering metal ion, Th(IV), interacts with the fluorescein fluorophore, causing slightly enhanced fluorescence intensity, with an apparent dissociation constant of approximately 230 microM. This sensor rivals the most sensitive analytical instruments for uranium detection, and its application in detecting uranium in contaminated soil samples is also demonstrated. This work shows that simple, cost-effective, and portable metal sensors can be obtained with similar sensitivity and selectivity as much more expensive and sophisticated analytical instruments. Such a sensor will play an important role in environmental remediation of radionuclides such as uranium.

A catalytic beacon sensor for uranium with parts-per-trillion sensitivity and millionfold selectivity

PubMed Central

Liu, Juewen; Brown, Andrea K.; Meng, Xiangli; Cropek, Donald M.; Istok, Jonathan D.; Watson, David B.; Lu, Yi

2007-01-01

Here, we report a catalytic beacon sensor for uranyl (UO22+) based on an in vitro-selected UO22+-specific DNAzyme. The sensor consists of a DNA enzyme strand with a 3′ quencher and a DNA substrate with a ribonucleotide adenosine (rA) in the middle and a fluorophore and a quencher at the 5′ and 3′ ends, respectively. The presence of UO22+ causes catalytic cleavage of the DNA substrate strand at the rA position and release of the fluorophore and thus dramatic increase of fluorescence intensity. The sensor has a detection limit of 11 parts per trillion (45 pM), a dynamic range up to 400 nM, and selectivity of >1-million-fold over other metal ions. The most interfering metal ion, Th(IV), interacts with the fluorescein fluorophore, causing slightly enhanced fluorescence intensity, with an apparent dissociation constant of ≈230 μM. This sensor rivals the most sensitive analytical instruments for uranium detection, and its application in detecting uranium in contaminated soil samples is also demonstrated. This work shows that simple, cost-effective, and portable metal sensors can be obtained with similar sensitivity and selectivity as much more expensive and sophisticated analytical instruments. Such a sensor will play an important role in environmental remediation of radionuclides such as uranium. PMID:17284609

Sensitive and selective detection of Hg2+ and Cu2+ ions by fluorescent Ag nanoclusters synthesized via a hydrothermal method

NASA Astrophysics Data System (ADS)

Liu, Jing; Ren, Xiangling; Meng, Xianwei; Fang, Zheng; Tang, Fangqiong

2013-09-01

An easily prepared fluorescent Ag nanoclusters (Ag NCs) probe for the sensitive and selective detection of Hg2+ and Cu2+ ions was developed here. The Ag NCs were synthesized by using polymethacrylic acid sodium salt as a template via a convenient hydrothermal process. The as-prepared fluorescent Ag NCs were monodispersed, uniform and less than 2 nm in diameter, and can be quenched in the presence of mercury (Hg2+) or copper (Cu2+) ions. Excellent linear relationships existed between the quenching degree of the Ag NCs and the concentrations of Hg2+ or Cu2+ ions in the range of 10 nM to 20 μM or 10 nM to 30 μM, respectively. By using ethylenediaminetetraacetate (EDTA) as the masking agent of Cu2+, Hg2+ was exclusively detected in coexistence with Cu2+ with high sensitivity (LOD = 10 nM), which also provided a reusable detection method for Cu2+. Furthermore, the different quenching phenomena caused by the two metals ions such as changes in visible colour, shifts of UV absorbance peaks and changes in size of Ag NCs make it easy to distinguish between them. Therefore the easily synthesized fluorescent Ag NCs may have great potential as Hg2+ and Cu2+ ions sensors.An easily prepared fluorescent Ag nanoclusters (Ag NCs) probe for the sensitive and selective detection of Hg2+ and Cu2+ ions was developed here. The Ag NCs were synthesized by using polymethacrylic acid sodium salt as a template via a convenient hydrothermal process. The as-prepared fluorescent Ag NCs were monodispersed, uniform and less than 2 nm in diameter, and can be quenched in the presence of mercury (Hg2+) or copper (Cu2+) ions. Excellent linear relationships existed between the quenching degree of the Ag NCs and the concentrations of Hg2+ or Cu2+ ions in the range of 10 nM to 20 μM or 10 nM to 30 μM, respectively. By using ethylenediaminetetraacetate (EDTA) as the masking agent of Cu2+, Hg2+ was exclusively detected in coexistence with Cu2+ with high sensitivity (LOD = 10 nM), which also provided a reusable detection method for Cu2+. Furthermore, the different quenching phenomena caused by the two metals ions such as changes in visible colour, shifts of UV absorbance peaks and changes in size of Ag NCs make it easy to distinguish between them. Therefore the easily synthesized fluorescent Ag NCs may have great potential as Hg2+ and Cu2+ ions sensors. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr03329e

Choosing between atmospheric pressure chemical ionization and electrospray ionization interfaces for the HPLC/MS analysis of pesticides

USGS Publications Warehouse

Thurman, E.M.; Ferrer, I.; Barcelo, D.

2001-01-01

An evaluation of over 75 pesticides by high-performance liquid chromatography/mass spectrometry (HPLC/MS) clearly shows that different classes of pesticides are more sensitive using either atmospheric pressure chemical ionization (APCI) or electrospray ionization (ESI). For example, neutral and basic pesticides (phenylureas, triazines) are more sensitive using APCI (especially positive ion). While cationic and anionic herbicides (bipyridylium ions, sulfonic acids) are more sensitive using ESI (especially negative ion). These data are expressed graphically in a figure called an ionization-continuum diagram, which shows that protonation in the gas phase (proton affinity) and polarity in solution, expressed as proton addition or subtraction (pKa), is useful in selecting APCI or ESI. Furthermore, sodium adduct formation commonly occurs using positive ion ESI but not using positive ion APCI, which reflects the different mechanisms of ionization and strengthens the usefulness of the ionization-continuum diagram. The data also show that the concept of "wrong-way around" ESI (the sensitivity of acidic pesticides in an acidic mobile phase) is a useful modification of simple pKa theory for mobile-phase selection. Finally, this finding is used to enhance the chromatographic separation of oxanilic and sulfonic acid herbicides while maintaining good sensitivity in LC/MS using ESI negative.

Development of a targeted adductomic method for the determination of polycyclic aromatic hydrocarbon DNA adducts using online column-switching liquid chromatography/tandem mass spectrometry.

PubMed

Singh, Rajinder; Teichert, Friederike; Seidel, Albrecht; Roach, Jonathan; Cordell, Rebecca; Cheng, Mai-Kim; Frank, Heinrich; Steward, William P; Manson, Margaret M; Farmer, Peter B

2010-08-30

Human exposure to polycyclic aromatic hydrocarbons (PAHs) from sources such as industrial or urban air pollution, tobacco smoke and cooked food is not confined to a single compound, but instead to mixtures of different PAHs. The interaction of different PAHs may lead to additive, synergistic or antagonistic effects in terms of DNA adduct formation and carcinogenic activity resulting from changes in metabolic activation to reactive intermediates and DNA repair. The development of a targeted DNA adductomic approach using liquid chromatography/tandem mass spectrometry (LC/MS/MS) incorporating software-based peak picking and integration for the assessment of exposure to mixtures of PAHs is described. For method development PAH-modified DNA samples were obtained by reaction of the anti-dihydrodiol epoxide metabolites of benzo[a]pyrene, benzo[b]fluoranthene, dibenzo[a,l]pyrene (DB[a,l]P) and dibenz[a,h]anthracene with calf thymus DNA in vitro and enzymatically hydrolysed to 2'-deoxynucleosides. Positive LC/electrospray ionisation (ESI)-MS/MS collision-induced dissociation product ion spectra data showed that the majority of adducts displayed a common fragmentation for the neutral loss of 116 u (2'-deoxyribose) resulting in a major product ion derived from the adducted base. The exception was the DB[a,l]P dihydrodiol epoxide adduct of 2'-deoxyadenosine which resulted in major product ions derived from the PAH moiety being detected. Specific detection of mixtures of PAH-adducted 2'-deoxynucleosides was achieved using online column-switching LC/MS/MS in conjunction with selected reaction monitoring (SRM) of the [M+H](+) to [M+H-116](+) transition plus product ions derived from the PAH moiety for improved sensitivity of detection and a comparison was made to detection by constant neutral loss scanning. In conclusion, different PAH DNA adducts were detected by employing SRM [M+H-116](+) transitions or constant neutral loss scanning. However, for improved sensitivity of detection optimised SRM transitions relating to the PAH moiety product ions are required for certain PAH DNA adducts for the development of targeted DNA adductomic methods. 2010 John Wiley & Sons, Ltd.

Matching the laser wavelength to the absorption properties of matrices increases the ion yield in UV-MALDI mass spectrometry.

PubMed

Wiegelmann, Marcel; Soltwisch, Jens; Jaskolla, Thorsten W; Dreisewerd, Klaus

2013-09-01

A high analytical sensitivity in ultraviolet matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) is only achieved if the laser wavelength corresponds to a high optical absorption of the matrix. Laser fluence and the physicochemical properties of the compounds, e.g., the proton affinity, also influence analytical sensitivity significantly. In combination, these parameters determine the amount of material ejected per laser pulse and the ion yield, i.e., the fraction of ionized biomolecules. Here, we recorded peptide ion signal intensities as a function of these parameters. Three cinnamic acid matrices were investigated: α-cyano-4-hydroxycinnamic acid, α-cyano-4-chlorocinnamic acid, and α-cyano-2,4-difluorocinnamic acid. In addition, 2,5-dihydroxybenzoic acid was used in comparison experiments. Ion signal intensities "per laser shot" and integrated ion signal intensities were acquired over 900 consecutive laser pulses applied on distinct positions on the dried-droplet sample preparations. With respect to laser wavelength, the two standard MALDI wavelengths of 337/355 nm were investigated. Also, 305 or 320 nm was selected to account for the blue-shifted absorption profiles of the halogenated derivatives. Maximal peptide ion intensities were obtained if the laser wavelength fell within the peak of the absorption profile of the compound and for fluences two to three times the corresponding ion detection threshold. The results indicate ways for improving the analytical sensitivity in MALDI-MS, and in particular for MALDI-MS imaging applications where a limited amount of material is available per irradiated pixel.

A novel, highly sensitive, selective, reversible and turn-on chemi-sensor based on Schiff base for rapid detection of Cu(II)

NASA Astrophysics Data System (ADS)

Saleh, Sayed M.; Ali, Reham; Ali, Ibrahim A. I.

2017-08-01

In this work, a novel optical fluoro-chemisensor was designed and synthesized for copper (II) ions detection. The sensor film is created by embedded N,N-Bis(2-hydroxo-5-bromobenzyl)ethylenediamine in poly vinyl chloride (PVC) film in presence of dioctyl phthalate (DOP) as plasticizer. The receptor Schiff base reveals "off-on" mode with high selectivity, significant sensitivity to Cu(II) ions. The selectivity of optical sensor for Cu(II) ions is the result of chelation enhanced fluorescence (CHEF). The optimal conditions of pH and response time at which higher efficiency of sensor film is performed was found to be 6.8 and 2.48 min. The possible interference of other metal ions in solution was examined in presence of different types of metal ions. This film shows high selectivity and ultra-sensitivity with low detection limit LOD (1.1 × 10- 8 M). Thus, these considerable properties make it viable to monitor copper metal ions within very low concentration range (0-15 × 10- 6 M Cu(II)) and highly selective even in the presence of different types of metal ions. The sensor reversibility was achieved by utilizing EDTA solution with concentration of 0.1 M solution.

Theoretical investigation of low detection sensitivity for underivatized carbohydrates in ESI and MALDI.

PubMed

Chen, Jien-Lian; Lee, Chuping; Lu, I-Chung; Chien, Chia-Lung; Lee, Yuan-Tseh; Hu, Wei-Ping; Ni, Chi-Kung

2016-12-01

Electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI) mainly generate protonated ions from peptides and proteins but sodiated (or potassiated) ions from carbohydrates. The ion intensities of sodiated (or potassiated) carbohydrates generated by ESI and MALDI are generally lower than those of protonated peptides and proteins. Ab initio calculations and transition state theory were used to investigate the reasons for the low detection sensitivity for underivatized carbohydrates. We used glucose and cellobiose as examples and showed that the low detection sensitivity is partly attributable to the following factors. First, glucose exhibits a low proton affinity. Most protons generated by ESI or MALDI attach to water clusters and matrix molecules. Second, protonated glucose and cellobiose can easily undergo dehydration reactions. Third, the sodiation affinities of glucose and cellobiose are small. Some sodiated glucose and cellobiose dissociate into the sodium cations and neutral carbohydrates during ESI or MALDI process. The increase of detection sensitivity of carbohydrates in mass spectrometry by various methods can be rationalized according to these factors. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

A sensitive, selective and rapid determination of lead(II) ions in real-life samples using an electrochemically reduced graphene oxide-graphite reinforced carbon electrode.

PubMed

Hamsawahini, Kunashegaran; Sathishkumar, Palanivel; Ahamad, Rahmalan; Yusoff, Abdull Rahim Mohd

2015-11-01

In this study, a sensitive and cost-effective electrochemically reduced graphene oxide (ErGO) on graphite reinforced carbon (GRC) was developed for the detection of lead (Pb(II)) ions present in the real-life samples. A film of graphene oxide (GO) was drop-casted on GRC and their electrochemical properties were investigated using cyclic voltammetry (CV), amperometry and square wave voltammetry (SWV). Factors influencing the detection of Pb(II) ions, such as grades of GRC, constant applied cathodic potential (CACP), concentration of hydrochloric acid and drop-casting drying time were optimised. GO is irreversibly reduced in the range of -0.7 V to -1.6 V vs Ag/AgCl (3 M) in acidic condition. The results showed that the reduction behaviour of GO contributed to the high sensitivity of Pb(II) ions detection even at nanomolar level. The ErGO-GRC showed the detection limit of 0.5 nM and linear range of 3-15 nM in HCl (1 M). The developed electrode has potential to be a good candidate for the determination of Pb(II) ions in different aqueous system. The proposed method gives a good recovery rate of Pb(II) ions in real-life water samples such as tap water and river water. Copyright © 2015 Elsevier B.V. All rights reserved.

A B-TOF mass spectrometer for the analysis of ions with extreme high start-up energies.

PubMed

Lezius, M

2002-03-01

Weak magnetic deflection is combined with two acceleration stage time-of-flight mass spectrometry and subsequent position-sensitive ion detection. The experimental method, called B-TOF mass spectrometry, is described with respect to its theoretical background and some experimental results. It is demonstrated that the technique has distinct advantages over other approaches, with special respect to the identification and analysis of very highly energetic ions with an initially large energy broadening (up to 1 MeV) and with high charge states (up to 30+). Similar energetic targets are a common case in intense laser-matter interaction processes found during laser ablation, laser-cluster and laser-molecule interaction and fast particle and x-ray generation from laser-heated plasma. Copyright 2002 John Wiley & Sons, Ltd.

Negative corona discharge-ion mobility spectrometry as a detection system for low density extraction solvent-based dispersive liquid-liquid microextraction.

PubMed

Ebrahimi, Amir; Jafari, Mohammad T

2015-03-01

This paper deals with a method based on negative corona discharge ionization ion mobility spectrometry (NCD-IMS) for the analysis of ethion (as an organophosphorus pesticide). The negative ions such as O2(-) and NO(x)(-) were eliminated from the background spectrum to increase the instrument sensitivity. The method was used to specify the sample extracted via dispersive liquid-liquid microextraction (DLLME) based on low density extraction solvent. The ion mobility spectrum of ethion in the negative mode and the reduced mobility value for its ion peak are firstly reported and compared with those of the positive mode. In order to combine the low density solvent DLLME directly with NCD-IMS, cyclohexane was selected as the extraction solvent, helping us to have a direct injection up to 20 µL solution, without any signal interference. The method was exhaustively validated in terms of sensitivity, enrichment factor, relative recovery, and repeatability. The linear dynamic range of 0.2-100.0 µg L(-1), detection limit of 0.075 µg L(-1), and the relative standard deviation (RSD) of about 5% were obtained for the analysis of ethion through this method. The average recoveries were calculated about 68% and 92% for the grape juice and underground water, respectively. Finally, some real samples were analyzed and the feasibility of the proposed method was successfully verified by the efficient extraction of the analyte using DLLME before the analysis by NCD-IMS. Copyright © 2014 Elsevier B.V. All rights reserved.

Gold nanoparticle-sensitized quartz crystal microbalance sensor for rapid and highly selective determination of Cu(II) ions.

PubMed

Jin, Yulong; Huang, Yanyan; Liu, Guoquan; Zhao, Rui

2013-09-21

A novel quartz crystal microbalance (QCM) sensor for rapid, highly selective and sensitive detection of copper ions was developed. As a signal amplifier, gold nanoparticles (Au NPs) were self-assembled onto the surface of the sensor. A simple dip-and-dry method enabled the whole detection procedure to be accomplished within 20 min. High selectivity of the sensor towards copper ions is demonstrated by both individual and coexisting assays with interference ions. This gold nanoparticle mediated amplification allowed a detection limit down to 3.1 μM. Together with good repeatability and regeneration, the QCM sensor was also applied to the analysis of copper contamination in drinking water. This work provides a flexible method for fabricating QCM sensors for the analysis of important small molecules in environmental and biological samples.

New highly sensitive and selective fluorescent terbium complex for the detection of aluminium ions

NASA Astrophysics Data System (ADS)

Anwar, Zeinab M.; Ibrahim, Ibrahim A.; Kamel, Rasha M.; Abdel-Salam, Enas T.; El-Asfoury, Mahmoud H.

2018-02-01

A highly sensitive and selective spectrofluorimetric method has been developed for the rapid determination of aluminium ions. The method is based on the fluorescence enhancement of Tb complex with 3,4-dimetyl-thieno[2,3 b] thiophene-2,5-dicarboxylic acid (LN) after addition trace amount of aluminium ions. The fluorescence of the probe is monitored at the characteristic an emission wavelength of Tb3+ at 545 nm with excitation at 300 nm. Optimum detection was obtained in DMSO-H2O (2:8, v/v) and at pH 6.0 using MOPSO buffer. Under the optimum conditions linear calibration curves were obtained from 0.5 μ mol L-1 to 20 μ mol L-1 with detection limit of 0.1 μ mol L-1. Effect of interference of other ions was studied.

A reversible metal ion fueled DNA three-way junction molecular device for "turn-on and -off" fluorescence detection of mercury ions (II) and biothiols respectively with high selectivity and sensitivity.

PubMed

Ma, Long; Wu, Guanrong; Li, Yufeng; Qin, Ping; Meng, Lingpei; Liu, Haiyan; Li, Yuyin; Diao, Aipo

2015-11-21

We constructed a reversible molecular device in the nanoscale based on a DNA three-way junction (3WJ) fueled by Hg(2+) binding and sequestration. It is highly responsive to external stimuli, which brings about optically detectable global structural changes. Such a DNA device can serve as a novel "turn-on and -off" fluorescent sensor for Hg(2+) and biothiol detection with high selectivity and sensitivity.

Charged Particle Detection: Potential of Love Wave Acoustic Devices

NASA Astrophysics Data System (ADS)

Pedrick, Michael; Tittmann, Bernhard

2006-03-01

An investigation of the dependence of film density on group and phase velocities in a Love Wave Device shows potential for acoustic-based charged particle detection (CPD). Exposure of an ion sensitive photoresist to charged particles causes localized changes in density through either scission or cross-linking. A theoretical model was developed to study ion fluence effects on Love Wave sensitivity based on: ion energy, effective density changes, layer thickness and mode selection. The model is based on a Poly(Methyl Methacralate) (PMMA) film deposited on a Quartz substrate. The effect of Helium ion fluence on the properties of PMMA has previously been studied. These guidelines were used as an initial basis for the prediction of helium ion detection in a PMMA layer. Procedures for experimental characterization of ion effects on the material properties of PMMA are reviewed. Techniques for experimental validation of the predicted velocity shifts are discussed. A Love Wave Device for CPD could potentially provide a cost-effective alternative to semiconductor or photo-based counterparts. The potential for monitoring ion implantation effects on material properties is also discussed.

Versatile, high-sensitivity faraday cup array for ion implanters

DOEpatents

Musket, Ronald G.; Patterson, Robert G.

2003-01-01

An improved Faraday cup array for determining the dose of ions delivered to a substrate during ion implantation and for monitoring the uniformity of the dose delivered to the substrate. The improved Faraday cup array incorporates a variable size ion beam aperture by changing only an insertable plate that defines the aperture without changing the position of the Faraday cups which are positioned for the operation of the largest ion beam aperture. The design enables the dose sensitivity range, typically 10.sup.11 -10.sup.18 ions/cm.sup.2 to be extended to below 10.sup.6 ions/cm.sup.2. The insertable plate/aperture arrangement is structurally simple and enables scaling to aperture areas between <1 cm.sup.2 and >750 cm.sup.2, and enables ultra-high vacuum (UHV) applications by incorporation of UHV-compatible materials.

A self-amplified transistor immunosensor under dual gate operation: highly sensitive detection of hepatitis B surface antigen

NASA Astrophysics Data System (ADS)

Lee, I.-K.; Jeun, M.; Jang, H.-J.; Cho, W.-J.; Lee, K. H.

2015-10-01

Ion-sensitive field-effect transistors (ISFETs), although they have attracted considerable attention as effective immunosensors, have still not been adopted for practical applications owing to several problems: (1) the poor sensitivity caused by the short Debye screening length in media with high ion concentration, (2) time-consuming preconditioning processes for achieving the highly-diluted media, and (3) the low durability caused by undesirable ions such as sodium chloride in the media. Here, we propose a highly sensitive immunosensor based on a self-amplified transistor under dual gate operation (immuno-DG ISFET) for the detection of hepatitis B surface antigen. To address the challenges in current ISFET-based immunosensors, we have enhanced the sensitivity of an immunosensor by precisely tailoring the nanostructure of the transistor. In the pH sensing test, the immuno-DG ISFET showed superior sensitivity (2085.53 mV per pH) to both standard ISFET under single gate operation (58.88 mV per pH) and DG ISFET with a non-tailored transistor (381.14 mV per pH). Moreover, concerning the detection of hepatitis B surface antigens (HBsAg) using the immuno-DG ISFET, we have successfully detected trace amounts of HBsAg (22.5 fg mL-1) in a non-diluted 1× PBS medium with a high sensitivity of 690 mV. Our results demonstrate that the proposed immuno-DG ISFET can be a biosensor platform for practical use in the diagnosis of various diseases.Ion-sensitive field-effect transistors (ISFETs), although they have attracted considerable attention as effective immunosensors, have still not been adopted for practical applications owing to several problems: (1) the poor sensitivity caused by the short Debye screening length in media with high ion concentration, (2) time-consuming preconditioning processes for achieving the highly-diluted media, and (3) the low durability caused by undesirable ions such as sodium chloride in the media. Here, we propose a highly sensitive immunosensor based on a self-amplified transistor under dual gate operation (immuno-DG ISFET) for the detection of hepatitis B surface antigen. To address the challenges in current ISFET-based immunosensors, we have enhanced the sensitivity of an immunosensor by precisely tailoring the nanostructure of the transistor. In the pH sensing test, the immuno-DG ISFET showed superior sensitivity (2085.53 mV per pH) to both standard ISFET under single gate operation (58.88 mV per pH) and DG ISFET with a non-tailored transistor (381.14 mV per pH). Moreover, concerning the detection of hepatitis B surface antigens (HBsAg) using the immuno-DG ISFET, we have successfully detected trace amounts of HBsAg (22.5 fg mL-1) in a non-diluted 1× PBS medium with a high sensitivity of 690 mV. Our results demonstrate that the proposed immuno-DG ISFET can be a biosensor platform for practical use in the diagnosis of various diseases. Electronic supplementary information (ESI) available: Material preparation, surface functionalization and anti-HBsAg immobilization. See DOI: 10.1039/c5nr03146j

MRI biosensor for lead detection based on the DNAzyme-induced catalytic reaction.

PubMed

Xu, Liguang; Yin, Honghong; Ma, Wei; Wang, Libing; Kuang, Hua; Xu, Chuanlai

2013-11-21

A MRI biosensor for sensitive and specific detection of lead ions (Pb(2+)) was developed based on DNAzyme-induced cleavage of magnetic nanoparticles (MNPs). A low limit of detection (LOD) of 0.05 ng mL(-1) was obtained. This biosensor has the potential to serve as a general platform for the detection of heavy metal ions.

A mass spectrometer based explosives trace detector

NASA Astrophysics Data System (ADS)

Vilkov, Andrey; Jorabchi, Kaveh; Hanold, Karl; Syage, Jack A.

2011-05-01

In this paper we describe the application of mass spectrometry (MS) to the detection of trace explosives. We begin by reviewing the issue of explosives trace detection (ETD) and describe the method of mass spectrometry (MS) as an alternative to existing technologies. Effective security screening devices must be accurate (high detection and low false positive rate), fast and cost effective (upfront and operating costs). Ion mobility spectrometry (IMS) is the most commonly deployed method for ETD devices. Its advantages are compact size and relatively low price. For applications requiring a handheld detector, IMS is an excellent choice. For applications that are more stationary (e.g., checkpoint and alternatives to IMS are available. MS is recognized for its superior performance with regard to sensitivity and specificity, which translate to lower false negative and false positive rates. In almost all applications outside of security where accurate chemical analysis is needed, MS is usually the method of choice and is often referred to as the gold standard for chemical analysis. There are many review articles and proceedings that describe detection technologies for explosives. 1,2,3,4 Here we compare MS and IMS and identify the strengths and weaknesses of each method. - Mass spectrometry (MS): MS offers high levels of sensitivity and specificity compared to other technologies for chemical detection. Its traditional disadvantages have been high cost and complexity. Over the last few years, however, the economics have greatly improved and MS is now capable of routine and automated operation. Here we compare MS and IMS and identify the strengths and weaknesses of each method. - Ion mobility spectrometry (IMS): 5 MS-ETD Screening System IMS is similar in concept to MS except that the ions are dispersed by gas-phase viscosity and not by molecular weight. The main advantage of IMS is that it does not use a vacuum system, which greatly reduces the size, cost, and complexity relative to MS. However, the trade-off is that the measurement accuracy is considerably less than MS. This is especially true for complex samples or when screening for a large number of target compounds simultaneously.

Development of a sensitive setup for laser spectroscopy studies of very exotic calcium isotopes

NASA Astrophysics Data System (ADS)

Garcia Ruiz, R. F.; Gorges, C.; Bissell, M.; Blaum, K.; Gins, W.; Heylen, H.; Koenig, K.; Kaufmann, S.; Kowalska, M.; Krämer, J.; Lievens, P.; Malbrunot-Ettenauer, S.; Neugart, R.; Neyens, G.; Nörtershäuser, W.; Yordanov, D. T.; Yang, X. F.

2017-04-01

An experimental setup for sensitive high-resolution measurements of hyperfine structure spectra of exotic calcium isotopes has been developed and commissioned at the COLLAPS beam line at ISOLDE, CERN. The technique is based on the radioactive detection of decaying isotopes after optical pumping and state selective neutralization (ROC) (Vermeeren et al 1992 Phys. Rev. Lett. 68 1679). The improvements and developments necessary to extend the applicability of the experimental technique to calcium isotopes produced at rates as low as few ions s-1 are discussed. Numerical calculations of laser-ion interaction and ion-beam simulations were explored to obtain the optimum performance of the experimental setup. Among the implemented features are a multi-step optical pumping region for sensitive measurements of isotopes with hyperfine splitting, a high-voltage platform for adequate control of low-energy ion beams and simultaneous β-detection of neutralized and remaining ions. The commissioning of the experimental setup, and the first online results on neutron-rich calcium isotopes are presented.

Label-free liquid crystal biosensor based on specific oligonucleotide probes for heavy metal ions.

PubMed

Yang, Shengyuan; Wu, Chao; Tan, Hui; Wu, Yan; Liao, Shuzhen; Wu, Zhaoyang; Shen, Guoli; Yu, Ruqin

2013-01-02

In this study, to enhance the capability of metal ions disturbing the orientation of liquid crystals (LCs), we designed a new label-free LC biosensor for the highly selective and sensitive detection of heavy metal ions. This strategy makes use of the target-induced DNA conformational change to enhance the disruption of target molecules for the orientation of LC leading to an amplified optical signal. The Hg(2+) ion, which possesses a unique property to bind specifically to two DNA thymine (T) bases, is used as a model heavy metal ion. In the presence of Hg(2+), the specific oligonucleotide probes form a conformational reorganization of the oligonucleotide probes from hairpin structure to duplex-like complexes. The duplex-like complexes are then bound on the triethoxysilylbutyraldehyde/N,N-dimethyl-N-octadecyl (3-aminopropyl) trimethoxysilyl chloride (TEA/DMOAP)-coated substrate modified with capture probes, which can greatly distort the orientational profile of LC, making the optical image of LC cell birefringent as a result. The optical signal of LC sensor has a visible change at the Hg(2+) concentration of low to 0.1 nM, showing good detection sensitivity. The cost-effective LC sensing method can translate the concentration signal of heavy metal ions in solution into the presence of DNA duplexes and is expected to be a sensitive detection platform for heavy metal ions and other small molecule monitors.

A pixel detector system for laser-accelerated ion detection

NASA Astrophysics Data System (ADS)

Reinhardt, S.; Draxinger, W.; Schreiber, J.; Assmann, W.

2013-03-01

Laser ion acceleration is an unique acceleration process that creates ultra-short ion pulses of high intensity ( > 107 ions/cm2/ns), which makes online detection an ambitious task. Non-electronic detectors such as radio-chromic films (RCF), imaging plates (IP) or nuclear track detectors (e.g. CR39) are broadly used at present. Only offline information on ion pulse intensity and position are available by these detectors, as minutes to hours of processing time are required after their exposure. With increasing pulse repetition rate of the laser system, there is a growing need for detection of laser accelerated ions in real-time. Therefore, we have investigated a commercial pixel detector system for online detection of laser-accelerated proton pulses. The CMOS imager RadEye1 was chosen, which is based on a photodiode array, 512 × 1024 pixels with 48 μm pixel pitch, thus offering a large sensitive area of approximately 25 × 50 mm2. First detection tests were accomplished at the conventional electrostatic 14 MV Tandem accelerator in Munich as well as Atlas laser accelerator. Detector response measurements at the conventional accelerator have been accomplished in a proton beam in dc (15 MeV) and pulsed (20 MeV) irradiation mode, the latter providing comparable particle flux as under laser acceleration conditions. Radiation hardness of the device was studied using protons (20 MeV) and C-ions (77 MeV), additionally. The detector system shows a linear response up to a maximum pulse flux of about 107 protons/cm2/ns. Single particle detection is possible in a low flux beam (104 protons/cm2/s) for all investigated energies. The radiation hardness has shown to give reasonable lifetime for an application at the laser accelerator. The results from the irradiation at a conventional accelerator are confirmed by a cross-calibration with CR39 in a laser-accelerated proton beam at the MPQ Atlas Laser in Garching, showing no problems of detector operation in presence of electro-magnetic pulse (EMP). The calibrated detector system was finally used for online detection of laser-accelerated proton and carbon ions at the Astra-Gemini laser.

Highly sensitive oligothiophene-phenylamine-based dual-functional fluorescence "turn-on" sensor for rapid and simultaneous detection of Al3+ and Fe3+ in environment and food samples.

PubMed

Guo, Zongrang; Niu, Qingfen; Li, Tianduo

2018-07-05

Developing low-cost and efficient sensors for rapid, selective and sensitive detection of the transition metal ions in environmental and food science is very important. In this study, a novel dual-functional fluorescent "turn-on" sensor 3TP based on oligothiophene-phenylamine Schiff base has been synthesized for discrimination and simultaneous detection of both Al 3+ and Fe 3+ ions with high selectivity and anti-interference over other metal ions. Sensor 3TP displayed a very fast fluorescence-enhanced response towards Al 3+ and Fe 3+ ions with low detection limits (0.177μM for Al 3+ and 0.172μM for Fe 3+ ) and wide pH response range (4.0-12.0). The Al 3+ /Fe 3+ sensing mechanisms were investigated by fluorescence experiments, 1 H NMR titrations, FT-IR and ESI-MS spectra. Importantly, sensor 3TP was served as an efficient solid material for the highly sensitive and selective detection of Fe 3+ on TLC plates. Moreover, the sensor 3TP has been successfully used to detect trace Al 3+ and Fe 3+ in environment and food samples with satisfactory results and good recoveries, revealing a convenient, reliable and accurate method for Al 3+ and Fe 3+ analysis in real samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Highly sensitive oligothiophene-phenylamine-based dual-functional fluorescence "turn-on" sensor for rapid and simultaneous detection of Al3+ and Fe3+ in environment and food samples

NASA Astrophysics Data System (ADS)

Guo, Zongrang; Niu, Qingfen; Li, Tianduo

2018-07-01

Developing low-cost and efficient sensors for rapid, selective and sensitive detection of the transition metal ions in environmental and food science is very important. In this study, a novel dual-functional fluorescent "turn-on" sensor 3TP based on oligothiophene-phenylamine Schiff base has been synthesized for discrimination and simultaneous detection of both Al3+ and Fe3+ ions with high selectivity and anti-interference over other metal ions. Sensor 3TP displayed a very fast fluorescence-enhanced response towards Al3+ and Fe3+ ions with low detection limits (0.177 μM for Al3+ and 0.172 μM for Fe3+) and wide pH response range (4.0-12.0). The Al3+/Fe3+ sensing mechanisms were investigated by fluorescence experiments, 1H NMR titrations, FT-IR and ESI-MS spectra. Importantly, sensor 3TP was served as an efficient solid material for the highly sensitive and selective detection of Fe3+ on TLC plates. Moreover, the sensor 3TP has been successfully used to detect trace Al3+ and Fe3+ in environment and food samples with satisfactory results and good recoveries, revealing a convenient, reliable and accurate method for Al3+ and Fe3+ analysis in real samples.

Development of slew-rate-limited time-over-threshold (ToT) ASIC for a multi-channel silicon-based ion detector

NASA Astrophysics Data System (ADS)

Uenomachi, M.; Orita, T.; Shimazoe, K.; Takahashi, H.; Ikeda, H.; Tsujita, K.; Sekiba, D.

2018-01-01

High-resolution Elastic Recoil Detection Analysis (HERDA), which consists of a 90o sector magnetic spectrometer and a position-sensitive detector (PSD), is a method of quantitative hydrogen analysis. In order to increase sensitivity, a HERDA system using a multi-channel silicon-based ion detector has been developed. Here, as a parallel and fast readout circuit from a multi-channel silicon-based ion detector, a slew-rate-limited time-over-threshold (ToT) application-specific integrated circuit (ASIC) was designed, and a new slew-rate-limited ToT method is proposed. The designed ASIC has 48 channels and each channel consists of a preamplifier, a slew-rate-limited shaping amplifier, which makes ToT response linear, and a comparator. The measured equivalent noise charges (ENCs) of the preamplifier, the shaper, and the ToT on no detector capacitance were 253±21, 343±46, and 560±56 electrons RMS, respectively. The spectra from a 241Am source measured using a slew-rate-limited ToT ASIC are also reported.

Highly selective and sensitive coumarin-triazole-based fluorometric 'turn-off' sensor for detection of Pb2+ ions.

PubMed

Shaily; Kumar, Ajay; Parveen, Iram; Ahmed, Naseem

2018-06-01

Exposure to even very low concentrations of Pb 2+ is known to cause cardiovascular, neurological, developmental, and reproductive disorders, and affects children in particular more severely. Consequently, much effort has been dedicated to the development of colorimetric and fluorescent sensors that can selectively detect Pb 2+ ions. Here, we describe the development of a triazole-based fluorescent sensor L5 for Pb 2+ ion detection. The fluorescence intensity of chemosensor L5 was selectively quenched by Pb 2+ ions and a clear color change from colorless to yellow could be observed by the naked eye. Chemosensor L5 exhibited high sensitivity and selectivity towards Pb 2+ ions in phosphate-buffered solution [20 mM, 1:9 DMSO/H 2 O (v/v), pH 8.0] with a 1:1 binding stoichiometry, a detection limit of 1.9 nM and a 6.76 × 10 6  M -1 binding constant. Additionally, low-cost and easy-to-prepare test strips impregnated with chemosensor L5 were also produced for efficient of Pb 2+ detection and proved the practical use of this test. Copyright © 2018 John Wiley & Sons, Ltd.

Strain detection in crystalline heterostructures using bidimensional blocking patterns of channelled particles

NASA Astrophysics Data System (ADS)

Redondo-Cubero, A.; David-Bosne, E.; Wahl, U.; Miranda, P.; da Silva, M. R.; Correia, J. G.; Lorenz, K.

2018-03-01

Strain is a critical parameter affecting the growth and the performance of many semiconductor systems but, at the same time, the accurate determination of strain profiles in heterostructures can be challenging, especially at the nanoscale. Ion channelling/blocking is a powerful technique for the detection of the strain state of thin films, normally carried out through angular scans with conventional particle detectors. Here we report the novel application of position sensitive detectors for the evaluation of the strain in a series of AlInN/GaN heterostructures with different compositions and thicknesses. The tetragonal strain is varied from compressive to tensile and analysed through bidimensional blocking patterns. The results demonstrate that strain can be correctly quantified when compared to Monte Carlo channelling simulations, which are essential because of the presence of ion steering effects at the interface between the layer and the substrate. Despite this physical limitation caused by ion steering, our results show that full bidimensional patterns can be applied to detect fingerprints and enhance the accuracy for most critical cases, in which the angular shift associated to the lattice distortion is below the critical angle for channelling.

True ion pick (TIPick): a denoising and peak picking algorithm to extract ion signals from liquid chromatography/mass spectrometry data.

PubMed

Ho, Tsung-Jung; Kuo, Ching-Hua; Wang, San-Yuan; Chen, Guan-Yuan; Tseng, Yufeng J

2013-02-01

Liquid Chromatography-Time of Flight Mass Spectrometry has become an important technique for toxicological screening and metabolomics. We describe TIPick a novel algorithm that accurately and sensitively detects target compounds in biological samples. TIPick comprises two main steps: background subtraction and peak picking. By subtracting a blank chromatogram, TIPick eliminates chemical signals of blank injections and reduces false positive results. TIPick detects peaks by calculating the S(CC(INI)) values of extracted ion chromatograms (EICs) without considering peak shapes, and it is able to detect tailing and fronting peaks. TIPick also uses duplicate injections to enhance the signals of the peaks and thus improve the peak detection power. Commonly seen split peaks caused by either saturation of the mass spectrometer detector or a mathematical background subtraction algorithm can be resolved by adjusting the mass error tolerance of the EICs and by comparing the EICs before and after background subtraction. The performance of TIPick was tested in a data set containing 297 standard mixtures; the recall, precision and F-score were 0.99, 0.97 and 0.98, respectively. TIPick was successfully used to construct and analyze the NTU MetaCore metabolomics chemical standards library, and it was applied for toxicological screening and metabolomics studies. Copyright © 2013 John Wiley & Sons, Ltd.

Acquisition of electrical signals using commercial electronic components for detection system of Lead ion in distilled water

NASA Astrophysics Data System (ADS)

Pujiyanto; Yasin, M.; Rusydi, F.

2018-03-01

Development of lead ion detection systems is expected to have an advantage in terms of simplicity of the device and easy for concentration analysis of a lead ion with very high performance. One important part of lead ion detection systems are electrical signal acquisition parts. The electrical signal acquisition part uses the main electronic components: non inverting op-amplifier, instrumentation amplifier, multiplier circuit and logarithmic amplifier. Here will be shown the performance of lead ion detection systems when the existing electrical signal processors use commercial electronic components. The results that can be drawn from this experimental were the lead ion sensor that has been developed can be used to detect lead ions with a sensitivity of 10.48 mV/ppm with the linearity 97.11% and had a measurement range of 0.1 ppm to 80 ppm.

In-situ measurement of smoke particles in the wintertime polar mesosphere between 80 and 85 km altitude

NASA Astrophysics Data System (ADS)

Amyx, K.; Sternovsky, Z.; Knappmiller, S.; Robertson, S.; Horanyi, M.; Gumbel, J.

2008-01-01

The MAGIC sounding rocket, launched in January 2005 into the polar mesosphere, carried two detectors for charged aerosol particles. The detectors are graphite patch collectors mounted flush with the skin of the payload and are connected to sensitive electrometers. The measured signal is the net current deposited on the detectors by heavy aerosol particles. The collection of electrons and ions is prevented by magnetic shielding and a small positive bias, respectively. Both instruments detected a layer of heavy aerosol particles between 80 and 85 km with a number density approximately 103 cm-3. Aerodynamic flow simulations imply that the collected particles are larger than ˜1 nm in radius. The particles are detected as a net positive charge deposited on the graphite collectors. It is suggested that the measured positive polarity is due to the electrification of the smoke particles upon impact on the graphite collectors.

Electrochemical and density functional theory investigation on the differential behaviors of core-ring structured NiCo2O4 nanoplatelets toward heavy metal ions.

PubMed

Liao, Jianjun; Zhang, Junping; Wang, Cai-Zhuang; Lin, Shiwei

2018-08-31

In order to further improve the electroanalytical performance toward heavy metal ions, core-ring structured NiCo 2 O 4 nanoplatelets were used to modify glass carbon electrode (GCE) for the determination of heavy metal ions in water. Owing to the high surface area of NiCo 2 O 4 nanoplatelets, the Pb(II) sensitivity increased by a factor of 1.70, and the detection limit decreased by a factor of 2.64 as compared to solid NiCo 2 O 4 nanoparticles modified GCE. Interestingly, NiCo 2 O 4 nanoplatelets showed different sensitivities toward heavy metal ions with the same valence states, following the order Pb(II) > Cd(II) > Hg(II) > Cu(II). To better and scientifically understand the difference in sensitivity, adsorption and desorption abilities were integrated into account. Density functional theory calculations verified that the adsorption capability of NiCo 2 O 4 toward Pb(II) was strongest among all heavy metal ions, thereby resulting in the largest sensitivity. Further desorption current measurements indicated the large desorption barrier of Cu(II) was another important factor leading to its lowest sensitivity. Finally, the applicability of the proposed method was demonstrated by the detection of heavy metal ions in real seawater. Copyright © 2018 Elsevier B.V. All rights reserved.

High sensitive detection of copper II ions using D-penicillamine-coated gold nanorods based on localized surface plasmon resonance

NASA Astrophysics Data System (ADS)

Hong, Yoochan; Jo, Seongjae; Park, Joohyung; Park, Jinsung; Yang, Jaemoon

2018-05-01

In this paper, we describe the development of a nanoplasmonic biosensor based on the localized surface plasmon resonance (LSPR) effect that enables a sensitive and selective recognition of copper II ions. First, we fabricated the nanoplasmonics as LSPR substrates using gold nanorods (GNR) and the nano-adsorption method. The LSPR sensitivity of the nanoplasmonics was evaluated using various solvents with different refractive indexes. Subsequently, D-penicillamine (DPA)—a chelating agent of copper II ions—was conjugated to the surface of the GNR. The limit of detection (LOD) for the DPA-conjugated nanoplasmonics was 100 pM. Furthermore, selectivity tests were conducted using various divalent cations, and sensitivity tests were conducted on the nanoplasmonics under blood-like environments. Finally, the developed nanoplasmonic biosensor based on GNR shows great potential for the effective recognition of copper II ions, even in human blood conditions.

Simultaneous Automatic Electrochemical Detection of Zinc, Cadmium, Copper and Lead Ions in Environmental Samples Using a Thin-Film Mercury Electrode and an Artificial Neural Network

PubMed Central

Kudr, Jiri; Nguyen, Hoai Viet; Gumulec, Jaromir; Nejdl, Lukas; Blazkova, Iva; Ruttkay-Nedecky, Branislav; Hynek, David; Kynicky, Jindrich; Adam, Vojtech; Kizek, Rene

2015-01-01

In this study a device for automatic electrochemical analysis was designed. A three electrodes detection system was attached to a positioning device, which enabled us to move the electrode system from one well to another of a microtitre plate. Disposable carbon tip electrodes were used for Cd(II), Cu(II) and Pb(II) ion quantification, while Zn(II) did not give signal in this electrode configuration. In order to detect all mentioned heavy metals simultaneously, thin-film mercury electrodes (TFME) were fabricated by electrodeposition of mercury on the surface of carbon tips. In comparison with bare electrodes the TMFEs had lower detection limits and better sensitivity. In addition to pure aqueous heavy metal solutions, the assay was also performed on mineralized rock samples, artificial blood plasma samples and samples of chicken embryo organs treated with cadmium. An artificial neural network was created to evaluate the concentrations of the mentioned heavy metals correctly in mixture samples and an excellent fit was observed (R2 = 0.9933). PMID:25558996

Sensitive detection of mercury and copper ions by fluorescent DNA/Ag nanoclusters in guanine-rich DNA hybridization

NASA Astrophysics Data System (ADS)

Peng, Jun; Ling, Jian; Zhang, Xiu-Qing; Bai, Hui-Ping; Zheng, Liyan; Cao, Qiu-E.; Ding, Zhong-Tao

2015-02-01

In this work, we designed a new fluorescent oligonucleotides-stabilized silver nanoclusters (DNA/AgNCs) probe for sensitive detection of mercury and copper ions. This probe contains two tailored DNA sequence. One is a signal probe contains a cytosine-rich sequence template for AgNCs synthesis and link sequence at both ends. The other is a guanine-rich sequence for signal enhancement and link sequence complementary to the link sequence of the signal probe. After hybridization, the fluorescence of hybridized double-strand DNA/AgNCs is 200-fold enhanced based on the fluorescence enhancement effect of DNA/AgNCs in proximity of guanine-rich DNA sequence. The double-strand DNA/AgNCs probe is brighter and stable than that of single-strand DNA/AgNCs, and more importantly, can be used as novel fluorescent probes for detecting mercury and copper ions. Mercury and copper ions in the range of 6.0-160.0 and 6-240 nM, can be linearly detected with the detection limits of 2.1 and 3.4 nM, respectively. Our results indicated that the analytical parameters of the method for mercury and copper ions detection are much better than which using a single-strand DNA/AgNCs.

Extractive electrospray ionization mass spectrometry toward in situ analysis without sample pretreatment.

PubMed

Li, Ming; Hu, Bin; Li, Jianqiang; Chen, Rong; Zhang, Xie; Chen, Huanwen

2009-09-15

A homemade novel nanoextractive electrospray ionization (nanoEESI) source has been characterized for in situ mass spectrometric analysis of ambient samples without sample pretreatment. The primary ions generated using a nanospray emitter interact with the neutral sample plume created by manually nebulizing liquid samples, allowing production of the analyte ions in the spatial cross section of the nanoEESI source. The performance of nanoEESI is experimentally investigated by coupling the nanoEESI source to a commercial LTQ mass spectrometer for rapid analysis of various ambient samples using positive/negative ion detection modes. Compounds of interest in actual samples such as aerosol drug preparations, beverages, milk suspensions, farmland water, and groundwater were unambiguously detected using tandem nanoEESI ion trap mass spectrometry. The limit of detection was low picogram per milliliter levels for the compounds tested. Acceptable relative standard deviation (RSD) values (5-10%) were obtained for direct measurement of analytes in complex matrixes, providing linear dynamic signal responses using manual sample introduction. A single sample analysis was completed within 1.2 s. Requiring no sheath gas for either primary ion production or neutral sample introduction, the nanoEESI has advantages including readiness for miniaturization and integration, simple maintenance, easy operation, and low cost. The experimental data demonstrate that the nanoEESI is a promising tool for high-throughput, sensitive, quantitative, in situ analysis of ambient complex samples, showing potential applications for in situ analysis in multiple disciplines including but not limited to pharmaceutical analysis, food quality control, pesticides residue detection, and homeland security.

Ultra-sensitive and selective detection of mercury ion (Hg2+) using free-standing silicon nanowire sensors

NASA Astrophysics Data System (ADS)

Jin, Yan; Gao, Anran; Jin, Qinghui; Li, Tie; Wang, Yuelin; Zhao, Jianlong

2018-04-01

In this paper, ultra-sensitive and highly selective Hg2+ detection in aqueous solutions was studied by free-standing silicon nanowire (SiNW) sensors. The all-around surface of SiNW arrays was functionalized with (3-Mercaptopropyl)trimethoxysilane serving as Hg2+ sensitive layer. Due to effective electrostatic control provided by the free-standing structure, a detection limit as low as 1 ppt was obtained. A linear relationship (R 2 = 0.9838) between log(CHg2+ ) and a device current change from 1 ppt to 5 ppm was observed. Furthermore, the developed SiNW sensor exhibited great selectivity for Hg2+ over other heavy metal ions, including Cd2+. Given the extraordinary ability for real-time Hg2+ detection, the small size and low cost of the SiNW device, it is expected to be a potential candidate in field detection of environmentally toxic mercury.

A very sensitive ion collection device for plasma-laser characterization.

PubMed

Cavallaro, S; Torrisi, L; Cutroneo, M; Amato, A; Sarta, F; Wen, L

2012-06-01

In this paper a very sensitive ion collection device, for diagnostic of laser ablated-target plasma, is described. It allows for reducing down to few microvolts the signal threshold at digital scope input. A standard ion collector is coupled to a transimpedance amplifier, specially designed, which increases data acquisition sensitivity by a gain ≈1100 and does not introduce any significant distortion of input signal. By time integration of current intensity, an amount of charge as small as 2.7 × 10(-2) pC can be detected for photopeak events.

Two in one: making electron and ion measurements using a single MCP in future top hat instruments.

NASA Astrophysics Data System (ADS)

Bedington, Robert; Saito, Yoshifumi

To allow for the reduced use of spacecraft resources in future missions, we are developing techniques to enable both electrons and ions to be measured in a single top hat instrument. Top hat energy analyser instruments typically analyse charged particles from a few eV to a few tens keV. They consist of an electrostatic, energy-analyser section and a detector. MCPs (micro-channel plates) are the most commonly used detectors, because of their high sensitivity and strong heritage in space instrumentation. To detect the lowest energies of charged particles, a pre-accelerating bias potential is applied to the front surface of the MCP, however this voltage cannot be altered quickly without drastically affecting the detector response. Any instrument that detects both electrons and ions, will therefore typically use two detectors (with fixed voltages)—one for electrons, one for ions, and will often use two separate energy analysers. Significant resource savings are available however if just a single MCP can be used. This can be achieved by having incoming ions (and optionally incoming electrons also) impact a secondary electron emitting material, and thus release secondary electrons to be detected by a positively biased (electron-detecting) MCP. Unlike MCPs, the electrostatic, energy-analyser sections are able to have their voltages cycled extremely rapidly, so that they can be made to sample electrons and then ions in quick succession with minimal design changes required. Two secondary electron conversion methods are being investigated: ultra-thin carbon foils, and dynodes. Using carbon foils in front of the MCPs, incoming ions can be detected by the secondary electrons they release, while incoming electrons pass straight through them. Using dynodes all incoming particles can be converted to secondary electrons before detection. The challenges include finding materials with uniform electron emission responses for the desired energies and particles, managing electric fields and scattered primary electrons. Experiments pertaining to this research will be discussed. These investigations are being pursued as prototype developments for the SCOPE mission for use on the EISA (Electron & Ion Spectrum Analyzer) instrument.

Highly sensitive determination of cadmium and lead using a low-cost electrochemical flow-through cell based on a carbon paste electrode.

PubMed

Wonsawat, Wanida; Dungchai, Wijitar; Motomizu, Shoji; Chuanuwatanakul, Suchada; Chailapakul, Orawon

2012-01-01

A low-cost thin-layer electrochemical flow-through cell based on a carbon paste electrode (CPE), was constructed for the highly sensitive determination of cadmium(II) (Cd(2+)) and lead(II) (Pb(2+)) ions. The sensitivity of the proposed cell for Cd(2+) and Pb(2+) ion detection was improved by using the smallest channel height without the need for any complicated electrode modification. Under the optimum conditions, the detection limits of Cd(2+) and Pb(2+) ions (0.08 and 0.07 µg dm(-3), respectively) were 13.8- and 11.4-fold lower than that of a commercial flow cell (1.1 and 0.8 µg dm(-3), respectively). Moreover, the percentage recoveries of Cd(2+) and Pb(2+) for the in-house designed thin-layer flow cell were higher than those for the commercially available cell in all tested water samples, and within the acceptable range. The proposed flow cell is promising as an inexpensive and alternative one for the highly sensitive monitoring of heavy metal ions. 2012 © The Japan Society for Analytical Chemistry

Quadrant anode image sensor

NASA Technical Reports Server (NTRS)

Lampton, M.; Malina, R. F.

1976-01-01

A position-sensitive event-counting electronic readout system for microchannel plates (MCPs) is described that offers the advantages of high spatial resolution and fast time resolution. The technique relies upon a four-quadrant electron-collecting anode located behind the output face of the microchannel plate, so that the electron cloud from each detected event is partly intercepted by each of the four quadrants. The relative amounts of charge collected by each quadrant depend on event position, permitting each event to be localized with two ratio circuits. A prototype quadrant anode system for ion, electron, and extreme ultraviolet imaging is described. The spatial resolution achieved, about 10 microns, allows individual MCP channels to be distinguished.

Sensitivity and selectivity of switchable reagent ion soft chemical ionization mass spectrometry for the detection of picric acid.

PubMed

Agarwal, Bishu; González-Méndez, Ramón; Lanza, Matteo; Sulzer, Philipp; Märk, Tilmann D; Thomas, Neil; Mayhew, Chris A

2014-09-18

We have investigated the reactions of NO(+), H3O(+), O2(+), and Kr(+) with picric acid (2,4,6 trinitrophenol, C6H3N3O7, PiA) using a time-of-flight mass spectrometer with a switchable reagent ion source. NO(+) forms a simple adduct ion PiA·NO(+), while H3O(+) reacts with PiA via nondissociative proton transfer to form PiAH(+). In contrast, both O2(+) and Kr(+) react with PiA by nondissociative charge transfer to produce PiA(+). For Kr(+), we also observe dissociation of PiA, producing NO2(+) with a branching percentage of approximately 40%. For the reagent ions H3O(+) and O2(+) (and operating the drift tube with normal laboratory air), we find that the intensities of the PiAH(+) and PiA(+) ions both exhibit a peak at a given drift-tube voltage (which is humidity dependent). This unusual behavior implies a peak in the detection sensitivity of PiA as a function of the drift-tube voltage (and hence E/N). Aided by electronic-structure calculations and our previous studies of trinitrotoluene and trinitrobenzene, we provide a possible explanation for the observed peak in the detection sensitivity of PiA.

Hg2+-reactive double hydrophilic block copolymer assemblies as novel multifunctional fluorescent probes with improved performance.

PubMed

Hu, Jinming; Li, Changhua; Liu, Shiyong

2010-01-19

We report on novel type of responsive double hydrophilic block copolymer (DHBC)-based multifunctional chemosensors to Hg(2+) ions, pH, and temperatures and investigate the effects of thermo-induced micellization on the detection sensitivity. Well-defined DHBCs bearing rhodamine B-based Hg(2+)-reactive moieties (RhBHA) in the thermo-responsive block, poly(ethylene oxide)-b-poly(N-isopropylacrylamide-co-RhBHA) (PEO-b-P(NIPAM-co-RhBHA)), were synthesized via reversible addition-fragmentation chain transfer (RAFT) polymerization. Nonfluorescent RhBHA moieties are subjected to selective ring-opening reaction upon addition of Hg(2+) ions or lowering solution pH, producing highly fluorescent acyclic species. Thus, at room temperature PEO-b-P(NIPAM-co-RhBHA) DHBCs can serve as water-soluble multifunctional and efficient fluorescent chemosensors to Hg(2+) ions and pH. Upon heating above the lower critical solution temperature (approximately 36 degrees C) of the PNIPAM block, they self-assemble into micelles possessing P(NIPAM-co-RhBHA) cores and well-solvated PEO coronas, which were fully characterized by dynamic and static laser light scattering. It was found that the detection sensitivity to Hg(2+) ions and pH could be dramatically improved at elevated temperatures due to fluorescence enhancement of RhBHA residues in the acyclic form, which were embedded within hydrophobic cores of thermo-induced micellar aggregates. This work represents a proof-of-concept example of responsive DHBC-based multifunctional fluorescent chemosensors for the highly efficient detection of Hg(2+) ions, pH, and temperatures with tunable detection sensitivity. Compared to reaction-based small molecule Hg(2+) probes in previous literature reports, the integration of stimuli-responsive block copolymers with well-developed small molecule-based selective sensing moieties in the current study are expected to exhibit preferred advantages including enhanced detection sensitivity, water dispersibility, biocompatibility, facile incorporation into devices, and the ability of further functionalization for targeted imaging and detection.

Optical tweezers for the measurement of binding forces: system description and application for the study of E. coli adhesion

NASA Astrophysics Data System (ADS)

Fallman, Erik G.; Schedin, Staffan; Andersson, Magnus J.; Jass, Jana; Axner, Ove

2003-06-01

Optical tweezers together with a position sensitive detection system allows measurements of forces in the pN range between micro-sized biological objects. A prototype force measurement system has been constructed around in inverted microscope with an argon-ion pumped Ti:sapphire laser as light source for optical trapping. A trapped particle in the focus of the high numerical aperture microscope-objective behaves like an omni-directional mechanical spring if an external force displaces it. The displacement from the equilibrium position is a measure of the exerted force. For position detection of the trapped particle (polystyrene beads), a He-Ne laser beam is focused a small distance below the trapping focus. An image of the bead appears as a distinct spot in the far field, monitored by a photosensitive detector. The position data is converted to a force measurement by a calibration procedure. The system has been used for measuring the binding forces between E-coli bacterial adhesin and their receptor sugars.

Real-time fluorescence assay of alkaline phosphatase in living cells using boron-doped graphene quantum dots as fluorophores.

PubMed

Chen, Li; Yang, Guancao; Wu, Ping; Cai, Chenxin

2017-10-15

This work reports a convenient and real-time assay of alkaline phosphatase (ALP) in living cells based on a fluorescence quench-recovery process at a physiological pH using the boron-doped graphene quantum dots (BGQDs) as fluorophore. The fluorescence of BGQDs is found to be effectively quenched by Ce 3+ ions because of the coordination of Ce 3+ ions with the carboxyl group of BGQDs. Upon addition of adenosine triphosphate (ATP) into the system, the quenched fluorescence can be recovered by the ALP-positive expressed cells (such as MCF-7 cells) due to the removal of Ce 3+ ions from BGQDs surface by phosphate ions, which are generated from ATP under catalytic hydrolysis of ALP that expressed in cells. The extent of fluorescence signal recovery depends on the level of ALP in cells, which establishes the basis of ALP assay in living cells. This approach can also be used for specific discrimination of the ALP expression levels in different type of cells and thus sensitive detection of those ALP-positive expressed cells (for example MCF-7 cells) at a very low abundance (10±5 cells mL -1 ). The advantages of this approach are that it has high sensitivity because of the significant suppression of the background due to the Ce 3+ ion quenching the fluorescence of BGQDs, and has the ability of avoiding false signals arising from the nonspecific adsorption of non-target proteins because it operates via a fluorescence quench-recovery process. In addition, it can be extended to other enzyme systems, such as ATP-related kinases. Copyright © 2017 Elsevier B.V. All rights reserved.

Coupling corona discharge for ambient extractive ionization mass spectrometry.

PubMed

Hu, Bin; Zhang, Xinglei; Li, Ming; Peng, Xuejiao; Han, Jing; Yang, Shuiping; Ouyang, Yongzhong; Chen, Huanwen

2011-12-07

Unlike the extractive electrospray ionization (EESI) technique described elsewhere, a corona discharge instead of electrospray ionization has been utilized to charge a neutral solvent spray under ambient conditions for the generation of highly charged microdroplets, which impact a neutral sample plume for the extractive ionization of the analytes in raw samples without any sample pretreatment. Using the positive ion mode, molecular radical cations were easily generated for the detection of non-polar compounds (e.g., benzene, cyclohexane, etc.), while protonated molecular ions of polar compounds (e.g., acetonitrile, acetic ether) were readily produced for the detection. By dispensing the matrix in a relatively large space, this method tolerates highly complex matrices. For a given sample such as lily fragrances, more compounds were detected by the method established here than the EESI technique. An acceptable relative standard deviation (RSD 8.9%, n = 11) was obtained for the direct measurement of explosives (10 ppb) in waste water samples. The experimental data demonstrate that this method could simultaneously detect both polar and non-polar analytes with high sensitivity, showing promising applications for the rapid detection of a wide variety of compounds present in complex matrices.

Visual and sensitive fluorescent sensing for ultratrace mercury ions by perovskite quantum dots.

PubMed

Lu, Li-Qiang; Tan, Tian; Tian, Xi-Ke; Li, Yong; Deng, Pan

2017-09-15

Mercury ions sensing is an important issue for human health and environmental safety. A novel fluorescence nanosensor was designed for rapid visual detection of ultratrace mercury ions (Hg 2+ ) by using CH 3 NH 3 PbBr 3 perovskite quantum dots (QDs) based on the surface ion-exchange mechanism. The synthesized CH 3 NH 3 PbBr 3 QDs can emitt intense green fluorescence with high quantum yield of 50.28%, and can be applied for Hg 2+ sensing with the detection limit of 0.124 nM (24.87 ppt) in the range of 0 nM-100 nM. Furthermore, the interfering metal ions have no any influence on the fluorescence intensity of QDs, showing the perovskite QDs possess the high selectivity and sensitivity for Hg 2+ detection. The sensing mechanism of perovskite QDs for Hg 2+ is has also been investigated by XPS, EDX studies, showing Pb 2+ on the surface of perovskite QDs has been partially replaced by Hg 2+ . Spot plate test shows that the perovskite QDs can also be used for visual detection of Hg 2+ . Our research indicated the perovskite QDs are promising candidates for the visual fluorescence detection of environmental micropollutants. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of portable mass spectrometer with electron cyclotron resonance ion source for detection of chemical warfare agents in air.

PubMed

Urabe, Tatsuya; Takahashi, Kazuya; Kitagawa, Michiko; Sato, Takafumi; Kondo, Tomohide; Enomoto, Shuichi; Kidera, Masanori; Seto, Yasuo

2014-01-01

A portable mass spectrometer with an electron cyclotron resonance ion source (miniECRIS-MS) was developed. It was used for in situ monitoring of trace amounts of chemical warfare agents (CWAs) in atmospheric air. Instrumental construction and parameters were optimized to realize a fast response, high sensitivity, and a small body size. Three types of CWAs, i.e., phosgene, mustard gas, and hydrogen cyanide were examined to check if the mass spectrometer was able to detect characteristic elements and atomic groups. From the results, it was found that CWAs were effectively ionized in the miniECRIS-MS, and their specific signals could be discerned over the background signals of air. In phosgene, the signals of the 35Cl+ and 37Cl+ ions were clearly observed with high dose-response relationships in the parts-per-billion level, which could lead to the quantitative on-site analysis of CWAs. A parts-per-million level of mustard gas, which was far lower than its lethal dosage (LCt50), was successfully detected with a high signal-stability of the plasma ion source. It was also found that the chemical forms of CWAs ionized in the plasma, i.e., monoatomic ions, fragment ions, and molecular ions, could be detected, thereby enabling the effective identification of the target CWAs. Despite the disadvantages associated with miniaturization, the overall performance (sensitivity and response time) of the miniECRIS-MS in detecting CWAs exceeded those of sector-type ECRIS-MS, showing its potential for on-site detection in the future. Copyright © 2013 Elsevier B.V. All rights reserved.

pH responsive label-assisted click chemistry triggered sensitivity amplification for ultrasensitive electrochemical detection of carbohydrate antigen 24-2.

PubMed

Zheng, Yun; Zhao, Lihua; Ma, Zhanfang

2018-05-15

Sensitivity amplification strategy by implementing click chemistry in the construction of biosensing interface can efficiently improve the performance of immunosensor. Herein, we developed a sandwich-type amperometric immunosensor for ultrasensitive detection of carbohydrate antigen 24-2 (CA 242) based on pH responsive label-assisted click chemistry triggered sensitivity amplification strategy. The sensitivity of amperometric immunosensor relies on the current response differences (ΔI) caused by per unit concentration target analyte. The pH responsive Cu 2+ -loaded polydopamine (CuPDA) particles conjugated with detection antibodies were employed as labels, which can release Cu(II) ions by regulating pH. In the presence of ascorbic acid (reductant), Cu(II) ions were reduced to Cu(I) ions. Azide-functionalized double-stranded DNA (dsDNA) as signal enhancer was immobilized on the substrate through Cu + -catalyzed azide/alkyne cycloaddition reaction. With the help of the click reaction, the ΔI caused by target was elevated prominently, resulting in sensitivity amplification of the immunosensor. Under optimal condition, the proposed immunosensor exhibited excellent performance with linear range from 0.0001 to 100 U mL -1 and ultralow detection limit of 20.74 μU mL -1 . This work successfully combines click chemistry with pH-responsive labels in sandwich-type amperometric immunosensor, providing a promising sensitivity amplification strategy to construct immunosensing platform for analysis of other tumor marker. Copyright © 2018 Elsevier B.V. All rights reserved.

Use of recombinantly produced 15N3-labelled nicotianamine for fast and sensitive stable isotope dilution ultra-performance liquid chromatography/electrospray ionization time-of-flight mass spectrometry.

PubMed

Schmidt, Holger; Böttcher, Christoph; Trampczynska, Aleksandra; Clemens, Stephan

2011-01-01

Nicotianamine (NA) is an important metal chelator, implicated in the intra- and intercellular trafficking of several transition metal ions in plants. To decipher its roles in physiological processes such as micronutrient acquisition, distribution or storage, fast and sensitive analytical techniques for quantification of this non-proteinogenic amino acid will be required. The use of a recombinant Schizosaccharomyces pombe strain expressing a nicotianamine synthase (NAS) gene allowed for the production of [(15)N(3)]-NA, which was enriched from cell extracts through cation exchange and used for stable isotope dilution analysis of NA. Such an approach should be widely applicable to important bioanalytes that are difficult to synthesize. The analytical procedure comprises mild aqueous extraction and rapid Fmoc derivatization, followed by fast separation using ultra-performance liquid chromatography (UPLC) and sensitive detection by positive ion electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) with a chromatographic cycle time of only 8 min. Derivatization was optimized with respect to incubation time and species suitable for quantification. The limit of detection was 0.14 to 0.23 pmol in biological matrices with the response being linear up to 42 pmol. Recovery rates were between 83% and 104% in various biological matrices including fission yeast cells, fungal mycelium, plant leaves and roots.

Postage stamp-sized array sensor for the sensitive screening test of heavy-metal ions.

PubMed

Zhang, Yu; Li, Xiao; Li, Hui; Song, Ming; Feng, Liang; Guan, Yafeng

2014-10-07

The sensitive determination of heavy-metal ions has been widely investigated in recent years due to their threat to the environment and to human health. Among various analytical detection techniques, inexpensive colorimetric testing papers/strips play a very important role. The limitation, however, is also clear: the sensitivity is usually low and the selectivity is poor. In this work, we have developed a postage stamp-sized array sensor composed of nine commercially available heterocyclic azo indicators. Combining filtration-based enrichment with an array of technologies-based pattern-recognition, we have obtained the discrimination capability for seven heavy-metal ions (Hg(2+), Pb(2+), Ag(+), Ni(2+), Cu(2+), Zn(2+), and Co(2+)) at their Chinese wastewater discharge standard concentrations. The allowable detection level of Hg(2+) was down to 0.05 mg L(-1). The heavy-metal ions screening test was readily achieved using a standard chemometric approach. And the array sensor applied well in real water samples.

An optical MEMS accelerometer fabricated using double-sided deep reactive ion etching on silicon-on-insulator wafer

NASA Astrophysics Data System (ADS)

Teo, Adrian J. T.; Li, Holden; Tan, Say Hwa; Yoon, Yong-Jin

2017-06-01

Optical MEMS devices provide fast detection, electromagnetic resilience and high sensitivity. Using this technology, an optical gratings based accelerometer design concept was developed for seismic motion detection purposes that provides miniaturization, high manufacturability, low costs and high sensitivity. Detailed in-house fabrication procedures of a double-sided deep reactive ion etching (DRIE) on a silicon-on-insulator (SOI) wafer for a micro opto electro mechanical system (MOEMS) device are presented and discussed. Experimental results obtained show that the conceptual device successfully captured motion similar to a commercial accelerometer with an average sensitivity of 13.6 mV G-1, and a highest recorded sensitivity of 44.1 mV G-1. A noise level of 13.5 mV was detected due to experimental setup limitations. This is the first MOEMS accelerometer developed using double-sided DRIE on SOI wafer for the application of seismic motion detection, and is a breakthrough technology platform to open up options for lower cost MOEMS devices.

Design and development of amperometric biosensor for the detection of lead and mercury ions in water matrix-a permeability approach.

PubMed

Gumpu, Manju Bhargavi; Krishnan, Uma Maheswari; Rayappan, John Bosco Balaguru

2017-07-01

Intake of water contaminated with lead (Pb 2+ ) and mercury (Hg 2+ ) ions leads to various toxic effects and health issues. In this context, an amperometric urease inhibition-based biosensor was developed to detect Pb 2+ and Hg 2+ ions in water matrix. The modified Pt/CeO 2 /urease electrode was fabricated by immobilizing CeO 2 nanoparticles and urease using a semi-permeable adsorption layer of nafion. With urea as a substrate, urease catalytic activity was examined through cyclic voltammetry. Further, maximum amperometric inhibitive response of the modified Pt/CeO 2 /urease electrode was observed in the presence of Pb 2+ and Hg 2+ ions due to the urease inhibition at specific potentials of -0.03 and 0 V, respectively. The developed sensor exhibited a detection limit of 0.019 ± 0.001 μM with a sensitivity of 89.2 × 10 -3  μA μM -1 for Pb 2+ ions. A detection limit of 0.018 ± 0.003 with a sensitivity of 94.1 × 10 -3  μA μM -1 was achieved in detecting Hg 2+ ions. The developed biosensor showed a fast response time (<1 s) with a linear range of 0.5-2.2 and 0.02-0.8 μM for Pb 2+ and Hg 2+ ions, respectively. The modified electrode offered a good stability for 20 days with a good repeatability and reproducibility. The developed sensor was used to detect Pb 2+ and Hg 2+ ions contaminating Cauvery river water and the observed results were in good co-ordination with atomic absorption spectroscopic data.

Chloride ions in the pore of glycine and GABA channels shape the time course and voltage dependence of agonist currents

PubMed Central

Moroni, Mirko; Biro, Istvan; Giugliano, Michele; Vijayan, Ranjit; Biggin, Philip C.; Beato, Marco; Sivilotti, Lucia G.

2011-01-01

In the vertebrate CNS, fast synaptic inhibition is mediated by GABA and glycine receptors. We recently reported that the time course of these synaptic currents is slower when intracellular chloride is high. Here we extend these findings to measure the effects of both extracellular and intracellular chloride on the deactivation of glycine and GABA currents at both negative and positive holding potentials. Currents were elicited by fast agonist application to outside-out patches from HEK293 cells expressing rat glycine or GABA receptors. The slowing effect of high extracellular chloride on current decay was detectable only in low intracellular chloride (4 mM). Our main finding is that glycine and GABA receptors “sense” chloride concentrations because of interactions between the M2 pore-lining domain and the permeating ions. This hypothesis is supported by the observation that the sensitivity of channel gating to intracellular chloride is abolished if the channel is engineered to become cation-selective, or if positive charges in the external pore vestibule are eliminated by mutagenesis. The appropriate interaction between permeating ions and channel pore is also necessary to maintain the channel voltage sensitivity of gating, which prolongs current decay at depolarized potentials. Voltage-dependence is abolished by the same mutations that suppress the effect of intracellular chloride and also by replacing chloride with another permeant ion, thiocyanate. These observations suggest that permeant chloride affects gating by a foot-in-the-door effect, binding to a channel site with asymmetrical access from the intracellular and extracellular sides of the membrane. PMID:21976494

Highly sensitive and selective analysis of urinary steroids by comprehensive two-dimensional gas chromatography combined with positive chemical ionization quadrupole mass spectrometry

PubMed Central

Zhang, Ying; Tobias, Herbert J.; Brenna, J. Thomas

2014-01-01

Comprehensive two dimensional gas chromatography (GC×GC) provides greater separation space than conventional GC. Because of fast peak elution, a time of flight mass spectrometer (TOFMS) is the usual structure-specific detector of choice. The quantitative capabilities of a novel GC×GC fast quadrupole MS were investigated with electron ionization (EI), and CH4 or NH3 positive chemical ionization (PCI) for analysis of endogenous urinary steroids targeted in anti-doping tests. Average precisions for steroid quantitative analysis from replicate urine extractions were 6% (RSD) for EI and 8% for PCI-NH3. The average limits of detection (LOD) calculated by quantification ions for 12 target steroids spiked into steroid-free urine matrix (SFUM) were 2.6 ng mL−1 for EI, 1.3 ng mL−1 for PCI-CH4, and 0.3 ng mL−1 for PCI-NH3, all in mass scanning mode. The measured limits of quantification (LOQ) with full mass scan GC×GC-qMS were comparable with the LOQ values measured by one-dimensional GC-MS in single ion monitoring (SIM) mode. PCI-NH3 yields fewer fragments and greater (pseudo)molecular ion abundances than EI or PCI-CH4. These data show a benchtop GC×GC-qMS system has the sensitivity, specificity, and resolution to analyze urinary steroids at normal urine concentrations, and that PCI-NH3, not currently available on most GC×GC-TOFMS instruments, is of particular value for generation of structure-specific ions. PMID:22606686

Remote Sensing of Icy Galilean Moon Surface and Atmospheric Composition Using Low Energy (1 eV-4 keV) Neutral Atom Imaging

NASA Technical Reports Server (NTRS)

Collier, M. R.; Sittler, E.; Chornay, D.; Cooper, J. F.; Coplan, M.; Johnson, R. E.

2004-01-01

We describe a low energy neutral atom imager suitable for composition measurements Europa and other icy Galilean moons in the Jovian magnetosphere. This instrument employs conversion surface technology and is sensitive to either neutrals converted to negative ions, neutrals converted to positive ions and the positive ions themselves depending on the power supply. On a mission such as the Jupiter Icy Moons Orbiter (JIMO), two back-to-back sensors would be flown with separate power supplies fitted to the neutral atom and iodneutral atom sides. This will allow both remote imaging of 1 eV < E < 4 keV neutrals from icy moon surfaces and atmospheres, and in situ measurements of ions at similar energies in the moon ionospheres and Jovian magnetospheric plasma. The instrument provides composition measurements of the neutrals and ions that enter the spectrometer with a mass resolution dependent on the time-of-flight subsystem and capable of resolving molecules. The lower energy neutrals, up to tens of eV, arise from atoms and molecules sputtered off the moon surfaces and out of the moon atmospheres by impacts of more energetic (keV to MeV) ions from the magnetosphere. Direct Simulation Monte Carlo (DSMC) models are used to convert measured neutral abundances to compositional distributions of primary and trace species in the sputtered surfaces and atmospheres. The escaping neutrals can also be detected as ions after photo- or plasma-ionization and pickup. Higher energy, keV neutrals come from charge exchange of magnetospheric ions in the moon atmospheres and provide information on atmospheric structure. At the jovicentric orbits of the icy moons the presence of toroidal gas clouds, as detected at Europa's orbit, provide M e r opportunities to analyze both the composition of neutrals and ions originating from the moon surfaces, and the characteristics of magnetospheric ions interacting with neutral cloud material. Charge exchange of low energy ions near the moons, and directional distributions of the resultant neutrals, allow indirect global mapping of magnetic field structures around the moons. Temporal variation of the magnetic structures can be linked to induced magnetic fields associated with subsurface oceans.

Colorimetric determination of Al(III) based on the aggregation of gold nanoparticles functionalized with novel 4-benzoyl pyrazolone derivative

NASA Astrophysics Data System (ADS)

Abubaker, Mariam; Ngah, Che Wan Zanariah Che Wan; Ahmad, Musa; Kuswandi, Bambang

2018-06-01

A sensitive and selective colorimetric method has been developed for detection of Al3+ ion using 4-benzoyl pyrazolone-functionalized gold nanoparticles (BMPBP-AuNPs) as novel colorimetric probes. The BMPBP-AuNPs were characterized by UV-visible spectrometry and transmission electron microscopy (TEM). It was found that the addition of the Al3+ ions led to a rapid aggregation of the BMPBP-AuNPs, which changed the color of the mixture from red to blue. Furthermore, there was a shift in the characteristic surface plasmon resonance (SPR) peak from 524 to 650 nm of BMPBP-AuNPs, which confirmed that a good linear relation (R2 = 0.9935) was present between the absorption ratio of 524 and 650 nm. Also, the assay detected the Al3+ ion concentrations in the linear range 0-12 ppm with the detection limit is 0.05 ppm. Finally, the synthesized BMPBP-AuNPs were successfully used as a colorimetric sensor for the selective and sensitive detection of the Al3+ ions in water samples.

Sensitive and selective detection of Cu(II) ion: A new effective 1,8-naphthalimide-based fluorescence 'turn off' sensor.

PubMed

Huang, Guozhen; Li, Chuang; Han, Xintong; Aderinto, Stephen Opeyemi; Shen, Kesheng; Mao, Shanshan; Wu, Huilu

2018-06-01

The present study reports the development of a new 1,8-naphthalimide-based fluorescent sensor V for monitoring Cu(II) ions. The sensor exhibited pH independence over a wide pH range 2.52-9.58, and indicated its possible use for monitoring Cu(II) ions in a competitive pH medium. The sensor also showed high selectivity and sensitivity towards the Cu(II) ions over other competitive metal ions in DMSO-HEPES buffer (v/v, 1:1; pH 7.4) with a fluorescence 'turn off' mode of 79.79% observed. A Job plot indicated the formation of a 1:1 binding mode of the sensor with Cu(II) ions. The association constant and detection limit were 1.14 × 10 6  M -1 and 4.67 × 10 -8 M, respectively. The fluorescence spectrum of the sensor was quenched due to the powerful paramagnetic nature of the Cu(II) ions. Potential application of this sensor was also demonstrated when determining Cu(II) ion levels in two different water samples. Copyright © 2018 John Wiley & Sons, Ltd.

Simulating the bio nanoelectronic interface

NASA Astrophysics Data System (ADS)

Millar, Campbell; Roy, Scott; Brown, Andrew R.; Asenov, Asen

2007-05-01

As the size of conventional nano-CMOS devices continues to shrink, they are beginning to approach the size of biologically relevant macromolecules such as ion channels. This, in concert with the increasing understanding of the behaviour of proteins in vivo, creates the potential for a revolution in the sensing, measurement and interaction with biological systems. In this paper we will demonstrate the theoretical possibility of directly coupling a nanoscale MOSFET with a model ion channel protein. This will potentially allow a much better understanding of the behaviour of biologically relevant molecules, since the measurement of the motion of charged particles can reveal a substantial amount of information about protein structure-function relationships. We can use the MOSFET's innate sensitivity to stray charge to detect the positions of single ions and, thus, better explore the dynamics of ion conduction in channel proteins. In addition, we also demonstrate that the MOSFET can be 'tuned' to sense current flow through channel proteins, thus providing, for the first time, a direct solid state/biological interface at the atomic level.

Development of an ion mobility spectrometer with UV ionization source to detect ketones and BTX

NASA Astrophysics Data System (ADS)

Ni, Kai; Guo, Jingran; Ou, Guangli; Lei, Yu; Wang, Xiaohao

2014-11-01

Ion mobility spectrometry (IMS) is an attractive material analysis technology for developing a miniaturized volatile organic compounds (VOCs) on-site monitoring sensor. Having simple instrumentation, IMS is especially suitable when portability and sensitivity are required. In this work, we designed an ion mobility spectrometer with UV ionization. The geometric parameters of the UV-IMS were optimized based on a numerical simulation. The simulation results demonstrated that the drift electric field in the drift region was approximately homogenous and in the reaction region had an ion focusing effect, which could improve the sensitivity and resolving power of the IMS. The UV-IMS has been constructed and used to detect VOCs, such as acetone, benzene, toluene and m-xylene (BTX). The resolution of these substance measured from the UV-IMS in the atmospheric conditions are about 30 and the limit of detection (LOD) is low to ppmv. The ion mobility module and electric circuit are integrated in a main PCB, which can facilitate mass production and miniaturization. The present UV-IMS is expected to become a tool of choice for the on-site monitoring for VOCs.

Stripping analysis of nanomolar perchlorate in drinking water with a voltammetric ion-selective electrode based on thin-layer liquid membrane.

PubMed

Kim, Yushin; Amemiya, Shigeru

2008-08-01

A highly sensitive analytical method is required for the assessment of nanomolar perchlorate contamination in drinking water as an emerging environmental problem. We developed the novel approach based on a voltammetric ion-selective electrode to enable the electrochemical detection of "redox-inactive" perchlorate at a nanomolar level without its electrolysis. The perchlorate-selective electrode is based on the submicrometer-thick plasticized poly(vinyl chloride) membrane spin-coated on the poly(3-octylthiophene)-modified gold electrode. The liquid membrane serves as the first thin-layer cell for ion-transfer stripping voltammetry to give low detection limits of 0.2-0.5 nM perchlorate in deionized water, commercial bottled water, and tap water under a rotating electrode configuration. The detection limits are not only much lower than the action limit (approximately 246 nM) set by the U.S. Environmental Protection Agency but also are comparable to the detection limits of the most sensitive analytical methods for detecting perchlorate, that is, ion chromatography coupled with a suppressed conductivity detector (0.55 nM) or electrospray ionization mass spectrometry (0.20-0.25 nM). The mass transfer of perchlorate in the thin-layer liquid membrane and aqueous sample as well as its transfer at the interface between the two phases were studied experimentally and theoretically to achieve the low detection limits. The advantages of ion-transfer stripping voltammetry with a thin-layer liquid membrane against traditional ion-selective potentiometry are demonstrated in terms of a detection limit, a response time, and selectivity.

Pulsed Multiple Reaction Monitoring Approach to Enhancing Sensitivity of a Tandem Quadrupole Mass Spectrometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Belov, Mikhail E.; Prasad, Satendra; Prior, David C.

2011-02-23

Liquid chromatography (LC)-triple quadrupole mass spectrometers operating in a Multiple Reaction Monitoring (MRM) mode are increasingly used for quantitative analysis of low abundance analytes in highly complex biochemical matrices. After development and selection of optimum MRM transition, sensitivity and data quality limitations are largely related to mass spectral peak interferences from sample or matrix constituents and statistical limitations at low number of ions reaching the detector. Herein, we report a new approach to enhancing MRM sensitivity by converting the continuous stream of ions from the ion source into a pulsed ion beam through the use of an Ion Funnel Trapmore » (IFT). Evaluation of the pulsed MRM approach was performed with a tryptic digest of Shewanella oneidensis strain MR-1 spiked with several reference peptides. The sensitivity improvement observed with the IFT coupled to the triple quadrupole instrument is based on several unique features. First, ion accumulation in the radio frequency (RF) ion trap facilitates improved droplet desolvation, which is manifested in the reduced background ion noise at the detector. Second, signal amplitude for a given transition is enhanced because of an order-of-magnitude increase in the ion charge density per unit time compared to a continuous mode of operation. Third, signal detection at the full duty cycle is obtained, as the trap use eliminates dead times between transitions, which are inevitable with continuous ion streams. In comparison with the conventional approach, the pulsed MRM signals showed up to 5-fold enhanced peak amplitude and 2-3 fold reduced chemical background, resulting in an improvement in the limit of detection (LOD) by a factor of ~ 4 to ~ 8.« less

Improvement in ionization efficiency of direct analysis in real time-mass spectrometry (DART-MS) by corona discharge.

PubMed

Sekimoto, Kanako; Sakakura, Motoshi; Kawamukai, Takatomo; Hike, Hiroshi; Shiota, Teruhisa; Usui, Fumihiko; Bando, Yasuhiko; Takayama, Mitsuo

2016-08-02

Herein it is shown that a combination of direct analysis in real time (DART) with a corona discharge system consisting of only a needle electrode easily improves DART ionization efficiency. Positive and negative DC corona discharges led to a formation of abundant excited helium atoms as well as the reactant ions H3O(+)(H2O)n and O2˙(-) in the DART analyte ionization area. These phenomena resulted in an increase in the absolute intensities of (de)protonated analytes by a factor of 2-20 over conventional DART. The other analyte ions detected in this corona-DART system (i.e., molecular ions, fragment ions, oxygenated (de)protonated analytes, dehydrogenated deprotonated analytes, and negative ion adducts) were quite similar to those obtained from DART alone. This indicates a lack of side reactions due to the corona discharge. The change in the relative intensities of individual analyte-related ions due to the combination of a corona discharge system with DART suggests that there is no effect of the abundant excited helium in the analyte ionization area on the fragmentation processes or enhancement of oxidation due to hydroxyl radicals HO˙. Furthermore, it was found that the corona-DART combination can be applied to the highly sensitive analysis of n-alkanes, in which the alkanes are ionized as positive ions via hydride abstraction and oxidation, independent of the type of alkane or the mass spectrometer used.

Surface plasmon resonance sensing detection of mercury and lead ions based on conducting polymer composite.

PubMed

Abdi, Mahnaz M; Abdullah, Luqman Chuah; Sadrolhosseini, Amir R; Mat Yunus, Wan Mahmood; Moksin, Mohd Maarof; Tahir, Paridah Md

2011-01-01

A new sensing area for a sensor based on surface plasmon resonance (SPR) was fabricated to detect trace amounts of mercury and lead ions. The gold surface used for SPR measurements were modified with polypyrrole-chitosan (PPy-CHI) conducting polymer composite. The polymer layer was deposited on the gold surface by electrodeposition. This optical sensor was used for monitoring toxic metal ions with and without sensitivity enhancement by chitosan in water samples. The higher amounts of resonance angle unit (ΔRU) were obtained for PPy-CHI film due to a specific binding of chitosan with Pb(2+) and Hg(2+) ions. The Pb(2+) ion bind to the polymer films most strongly, and the sensor was more sensitive to Pb(2+) compared to Hg(2+). The concentrations of ions in the parts per million range produced the changes in the SPR angle minimum in the region of 0.03 to 0.07. Data analysis was done by Matlab software using Fresnel formula for multilayer system.

Strategy to improve the quantitative LC-MS analysis of molecular ions resistant to gas-phase collision induced dissociation: application to disulfide-rich cyclic peptides.

PubMed

Ciccimaro, Eugene; Ranasinghe, Asoka; D'Arienzo, Celia; Xu, Carrie; Onorato, Joelle; Drexler, Dieter M; Josephs, Jonathan L; Poss, Michael; Olah, Timothy

2014-12-02

Due to observed collision induced dissociation (CID) fragmentation inefficiency, developing sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) assays for CID resistant compounds is especially challenging. As an alternative to traditional LC-MS/MS, we present here a methodology that preserves the intact analyte ion for quantification by selectively filtering ions while reducing chemical noise. Utilizing a quadrupole-Orbitrap MS, the target ion is selectively isolated while interfering matrix components undergo MS/MS fragmentation by CID, allowing noise-free detection of the analyte's surviving molecular ion. In this manner, CID affords additional selectivity during high resolution accurate mass analysis by elimination of isobaric interferences, a fundamentally different concept than the traditional approach of monitoring a target analyte's unique fragment following CID. This survivor-selected ion monitoring (survivor-SIM) approach has allowed sensitive and specific detection of disulfide-rich cyclic peptides extracted from plasma.

An innovative diagnostic technology for the codon mutation C580Y in kelch13 of Plasmodium falciparum with MinION nanopore sequencer.

PubMed

Imai, Kazuo; Tarumoto, Norihito; Runtuwene, Lucky Ronald; Sakai, Jun; Hayashida, Kyoko; Eshita, Yuki; Maeda, Ryuichiro; Tuda, Josef; Ohno, Hideaki; Murakami, Takashi; Maesaki, Shigefumi; Suzuki, Yutaka; Yamagishi, Junya; Maeda, Takuya

2018-05-29

The recent spread of artemisinin (ART)-resistant Plasmodium falciparum represents an emerging global threat to public health. In Southeast Asia, the C580Y mutation of kelch13 (k13) is the dominant mutation of ART-resistant P. falciparum. Therefore, a simple method for the detection of C580Y mutation is urgently needed to enable widespread routine surveillance in the field. The aim of this study is to develop a new diagnostic procedure for the C580Y mutation using loop-mediated isothermal amplification (LAMP) combined with the MinION nanopore sequencer. A LAMP assay for the k13 gene of P. falciparum to detect the C580Y mutation was successfully developed. The detection limit of this procedure was 10 copies of the reference plasmid harboring the k13 gene within 60 min. Thereafter, amplicon sequencing of the LAMP products using the MinION nanopore sequencer was performed to clarify the nucleotide sequences of the gene. The C580Y mutation was identified based on the sequence data collected from MinION reads 30 min after the start of sequencing. Further, clinical evaluation of the LAMP assay in 34 human blood samples collected from patients with P. falciparum malaria in Indonesia revealed a positive detection rate of 100%. All LAMP amplicons of up to 12 specimens were simultaneously sequenced using MinION. The results of sequencing were consistent with those of the conventional PCR and Sanger sequencing protocol. All procedures from DNA extraction to variant calling were completed within 3 h. The C580Y mutation was not found among these 34 P. falciparum isolates in Indonesia. An innovative method combining LAMP and MinION will enable simple, rapid, and high-sensitivity detection of the C580Y mutation of P. falciparum, even in resource-limited situations in developing countries.

Peptides Labeled with Pyridinium Salts for Sensitive Detection and Sequencing by Electrospray Tandem Mass Spectrometry

NASA Astrophysics Data System (ADS)

Waliczek, Mateusz; Kijewska, Monika; Rudowska, Magdalena; Setner, Bartosz; Stefanowicz, Piotr; Szewczuk, Zbigniew

2016-11-01

Mass spectrometric analysis of trace amounts of peptides may be problematic due to the insufficient ionization efficiency resulting in limited sensitivity. One of the possible ways to overcome this problem is the application of ionization enhancers. Herein we developed new ionization markers based on 2,4,6-triphenylpyridinium and 2,4,6-trimethylpyridinium salts. Using of inexpensive and commercially available pyrylium salt allows selective derivatization of primary amino groups, especially those sterically unhindered, such as ɛ-amino group of lysine. The 2,4,6-triphenylpyridinium modified peptides generate in MS/MS experiments an abundant protonated 2,4,6-triphenylpyridinium ion. This fragment is a promising reporter ion for the multiple reactions monitoring (MRM) analysis. In addition, the fixed positive charge of the pyridinium group enhances the ionization efficiency. Other advantages of the proposed ionization enhancers are the simplicity of derivatization of peptides and the possibility of convenient incorporation of isotopic labels into derivatized peptides.

A fluorescent nanosensor based on graphene quantum dots-aptamer probe and graphene oxide platform for detection of lead (II) ion.

PubMed

Qian, Zhao Sheng; Shan, Xiao Yue; Chai, Lu Jing; Chen, Jian Rong; Feng, Hui

2015-06-15

The sensitive detection of heavy metal ions in the organism and aquatic ecosystem using nanosensors based on environment friendly and biocompatible materials still remains a challenge. A fluorescent turn-on nanosensor for lead (II) detection based on biocompatible graphene quantum dots and graphene oxide by employment of Pb(2+)-induced G-quadruplex formation was reported. Graphene quantum dots with high quantum yield, good biocompatibility were prepared and served as the fluorophore of Pb(2+) probe. Fluorescence turn-off of graphene quantum dots is easily achieved through efficient photoinduced electron transfer between graphene quantum dots and graphene oxide, and subsequent fluorescence turn-on process is due to the formation of G-quadraplex aptamer-Pb(2+) complex triggered by the addition of Pb(2+). This nanosensor can distinguish Pb(2+) ion from other ions with high sensitivity and good reproducibility. The detection method based on this nanosensor possesses a fast response time of one minute, a broad linear span of up to 400.0 nM and ultralow detection limit of 0.6 nM. Copyright © 2015 Elsevier B.V. All rights reserved.

Release of Gd-ions from peralkaline borosilicate glass in pure water for neutrino detection in Water-Cherenkov Detectors

NASA Astrophysics Data System (ADS)

Dongol, R.; Sundaram, S. K.

2017-09-01

The addition of Gadolinium (Gd)-based salt, specially GdCl3, in the Water Cherenkov Detectors (WCDs) enhances the sensitivity to neutrino detection. However, the unwanted Cl-based byproducts, significantly reduces the transparency of water and sensitivity of WCDs. An alternative method, to introduce Gd-ions in the WCDs, is through Gd-release from a custom designed Gd-doped glass, when in contact with water. This can potentially eliminate the use of Gd-based salts and byproducts. In this work, we report the Gd-ions release for a Gd-doped peralkaline (Na/Al > 1) borosilicate glass, which closely represents photomultiplier tube (PMT) glass composition used in WCDs. The purpose of the paper is to show that the Gd-ion release from a custom designed glass in the form of beads or powders is feasible and could be used as a controlled Gd-source in future WCDs to enhance neutrino detection. In addition, we present our results of Gd-solubility in the base glass composition.

A Robust Luminescent Tb(III)-MOF with Lewis Basic Pyridyl Sites for the Highly Sensitive Detection of Metal Ions and Small Molecules.

PubMed

Zhao, Jun; Wang, Ye-Nan; Dong, Wen-Wen; Wu, Ya-Pan; Li, Dong-Sheng; Zhang, Qi-Chun

2016-04-04

A new luminescent terbium-metal-organic framework [Tb3(L)2(HCOO)(H2O)5]·DMF·4H2O (1) (H4L = 4,4'-(pyridine-3,5-diyl)diisophthalic acid) has been successfully assembled by Tb(3+) ions and an undeveloped pyridyl-tetracarboxylate. Compound 1 exhibits a 3D porous (3,8)-connected (4.5(2))2(4(2).5(12).6(6).7(5).8(3)) topological framework with fascinating 1D open hydrophilic channels decorated by uncoordinated Lewis basic pyridyl nitrogen atoms. In particular, the Tb-MOF (1) can detect Cu(2+) ions with high selectivity and sensitivity, and its luminescence is nearly entirely quenched in N,N-dimethylformamide (DMF) solution and biological system. In addition, 1 still has high detection for the trace content of nitromethane with 70 ppm, which suggests that 1 is a promising example of dual functional materials with sensing copper ions and nitromethane.

Human perception of electric fields and ion currents associated with high-voltage DC transmission lines.

PubMed

Blondin, J P; Nguyen, D H; Sbeghen, J; Goulet, D; Cardinal, C; Maruvada, P S; Plante, M; Bailey, W H

1996-01-01

The objective of this study was to assess the ability of humans to detect the presence of DC electric field and ion currents. An exposure chamber simulating conditions present in the vicinity of high-voltage DC (HVDC) lines was designed and built for this purpose. In these experiments, the facility was used to expose observers to DC electric fields up to 50 kV/m and ion current densities up to 120 nA/m2. Forty-eight volunteers (25 women and 23 men) between the ages of 18 and 57 years served as observers. Perception of DC fields was examined by using two psychophysical methods: an adaptive staircase procedure and a rating method derived from signal-detection theory. Subjects completed three different series of observations by using each of these methods; one was conducted without ion currents, and the other two involved various combinations of electric fields and ion currents. Overall, subjects were significantly more likely to detect DC fields as the intensity increased. Observers were able to detect the presence of DC fields alone, but only at high intensities; the average threshold was 45 kV/m. Except in the most sensitive individuals, ion current densities up to 60 nA/m2 did not significantly facilitate the detection of DC fields. However, higher ion current densities were associated with a substantial lowering of sensory thresholds in a large majority of observers. Data analysis also revealed large variations in perceptual thresholds among observers. Normative data indicating DC field and ion current intensities that can be detected by 50% of all observers are provided. In addition, for the most sensitive observers, several other detection proportions were derived from the distribution of individual detection capabilities. These data can form the basis for environmental guidelines relating to the design of HVDC lines.

Electrochemical detection of Hg (II) ions using EDTA-PANI/SWNTs nanocomposite modified SS electrode

NASA Astrophysics Data System (ADS)

Deshmukh, M. A.; Patil, H. K.; Shirsat, M. D.; Ramanavicius, A.

2017-05-01

Detection of Hg (II) ions using EDTA modified polyaniline (PANI) and single walled carbon nanotubes (SWNTs) nanocomposite (PANI/SWNTs) was performed electrochemically via cyclic voltammetry (CV) technique. Dodecyl benzene sulphonic next step, PANI/SWNTs nanocomposite was modified acid sodium salt (DBSA) was used as a surfactant during this synthesis to get uniform suspension SWNTs. In the by EDTA solution containing crosslinking agent 1-ethyl-3(3-(dimethylamino) propyl) - carbodiimide (EDC) utilizing dip coating technique. The sensitivity of EDTA modified PANI/SWNTs nanocomposite towards Hg (II) ions was investigated. Differential pulse voltammetry (DPV) technique was applied for the electrochemical detection of Hg (II) ions.

A new detector for mass spectrometry: direct detection of low energy ions using a multi-pixel photon counter.

PubMed

Wilman, Edward S; Gardiner, Sara H; Nomerotski, Andrei; Turchetta, Renato; Brouard, Mark; Vallance, Claire

2012-01-01

A new type of ion detector for mass spectrometry and general detection of low energy ions is presented. The detector consists of a scintillator optically coupled to a single-photon avalanche photodiode (SPAD) array. A prototype sensor has been constructed from a LYSO (Lu(1.8)Y(0.2)SiO(5)(Ce)) scintillator crystal coupled to a commercial SPAD array detector. As proof of concept, the detector is used to record the time-of-flight mass spectra of butanone and carbon disulphide, and the dependence of detection sensitivity on the ion kinetic energy is characterised.

The Thermal Ion Dynamics Experiment and Plasma Source Instrument

NASA Technical Reports Server (NTRS)

Moore, T. E.; Chappell, C. R.; Chandler, M. O.; Fields, S. A.; Pollock, C. J.; Reasoner, D. L.; Young, D. T.; Burch, J. L.; Eaker, N.; Waite, J. H., Jr.;

Development and characterization of high-resolution neutron pixel detectors based on Timepix read-out chips

NASA Astrophysics Data System (ADS)

Krejci, F.; Zemlicka, J.; Jakubek, J.; Dudak, J.; Vavrik, D.; Köster, U.; Atkins, D.; Kaestner, A.; Soltes, J.; Viererbl, L.; Vacik, J.; Tomandl, I.

2016-12-01

Using a suitable isotope such as 6Li and 10B semiconductor hybrid pixel detectors can be successfully adapted for position sensitive detection of thermal and cold neutrons via conversion into energetic light ions. The adapted devices then typically provides spatial resolution at the level comparable to the pixel pitch (55 μm) and sensitive area of about few cm2. In this contribution, we describe further progress in neutron imaging performance based on the development of a large-area hybrid pixel detector providing practically continuous neutron sensitive area of 71 × 57 mm2. The measurements characterising the detector performance at the cold neutron imaging instrument ICON at PSI and high-flux imaging beam-line Neutrograph at ILL are presented. At both facilities, high-resolution high-contrast neutron radiography with the newly developed detector has been successfully applied for objects which imaging were previously difficult with hybrid pixel technology (such as various composite materials, objects of cultural heritage etc.). Further, a significant improvement in the spatial resolution of neutron radiography with hybrid semiconductor pixel detector based on the fast read-out Timepix-based detector is presented. The system is equipped with a thin planar 6LiF convertor operated effectively in the event-by-event mode enabling position sensitive detection with spatial resolution better than 10 μm.

DNA as Sensors and Imaging Agents for Metal Ions

PubMed Central

Xiang, Yu

2014-01-01

Increasing interests in detecting metal ions in many chemical and biomedical fields have created demands for developing sensors and imaging agents for metal ions with high sensitivity and selectivity. This review covers recent progress in DNA-based sensors and imaging agents for metal ions. Through both combinatorial selection and rational design, a number of metal ion-dependent DNAzymes and metal ion-binding DNA structures that can selectively recognize specific metal ions have been obtained. By attaching these DNA molecules with signal reporters such as fluorophores, chromophores, electrochemical tags, and Raman tags, a number of DNA-based sensors for both diamagnetic and paramagnetic metal ions have been developed for fluorescent, colorimetric, electrochemical, and surface Raman detections. These sensors are highly sensitive (with detection limit down to 11 ppt) and selective (with selectivity up to millions-fold) toward specific metal ions. In addition, through further development to simplify the operation, such as the use of “dipstick tests”, portable fluorometers, computer-readable discs, and widely available glucose meters, these sensors have been applied for on-site and real-time environmental monitoring and point-of-care medical diagnostics. The use of these sensors for in situ cellular imaging has also been reported. The generality of the combinatorial selection to obtain DNAzymes for almost any metal ion in any oxidation state, and the ease of modification of the DNA with different signal reporters make DNA an emerging and promising class of molecules for metal ion sensing and imaging in many fields of applications. PMID:24359450

Linear electronic field time-of-flight ion mass spectrometers

DOEpatents

Funsten, Herbert O.

2010-08-24

Time-of-flight mass spectrometer comprising a first drift region and a second drift region enclosed within an evacuation chamber; a means of introducing an analyte of interest into the first drift region; a pulsed ionization source which produces molecular ions from said analyte of interest; a first foil positioned between the first drift region and the second drift region, which dissociates said molecular ions into constituent atomic ions and emits secondary electrons; an electrode which produces secondary electrons upon contact with a constituent atomic ion in second drift region; a stop detector comprising a first ion detection region and a second ion detection region; and a timing means connected to the pulsed ionization source, to the first ion detection region, and to the second ion detection region.

A novel Laser Ion Mobility Spectrometer

NASA Astrophysics Data System (ADS)

Göbel, J.; Kessler, M.; Langmeier, A.

2009-05-01

IMS is a well know technology within the range of security based applications. Its main advantages lie in the simplicity of measurement, along with a fast and sensitive detection method. Contemporary technology often fails due to interference substances, in conjunction with saturation effects and a low dynamic detection range. High throughput facilities, such as airports, require the analysis of many samples at low detection limits within a very short timeframe. High detection reliability is a requirement for safe and secure operation. In our present work we developed a laser based ion-mobility-sensor which shows several advantages over known IMS sensor technology. The goal of our research was to increase the sensitivity compared to the range of 63Ni based instruments. This was achieved with an optimised geometric drift tube design and a pulsed UV laser system at an efficient intensity. In this intensity range multi-photon ionisation is possible, which leads to higher selectivity in the ion-formation process itself. After high speed capturing of detection samples, a custom designed pattern recognition software toolbox provides reliable auto-detection capability with a learning algorithm and a graphical user interface.

Relating to monitoring ion sources

DOEpatents

Orr, Christopher Henry; Luff, Craig Janson; Dockray, Thomas; Macarthur, Duncan Whittemore; Bounds, John Alan

2002-01-01

The apparatus and method provide techniques for monitoring the position on alpha contamination in or on items or locations. The technique is particularly applicable to pipes, conduits and other locations to which access is difficult. The technique uses indirect monitoring of alpha emissions by detecting ions generated by the alpha emissions. The medium containing the ions is moved in a controlled manner frog in proximity with the item or location to the detecting unit and the signals achieved over time are used to generate alpha source position information.

Plasma-laser ion discrimination by TOF technique applied to coupled SiC detectors.

NASA Astrophysics Data System (ADS)

Cavallaro, Salvatore

2018-01-01

The rate estimation of nuclear reactions induced in high intensity laser-target interaction (≥1016 W/cm2), is strongly depending on the neutron detection efficiency and ion charge discrimination, according to particles involved in exit open-channels. Ion discrimination is basically performed by means of analysis of pits observed on track detector, which is critically dependent on calibration and/or fast TOF devices based on SiC and diamond detectors. Last setup is used to determine the ion energy and to obtain a rough estimation of yields. However, for each TOF interval, the dependence of yield from the energy deposited in the detector sensitive region, introduces a distortion in the ion spectra. Moreover, if two ion species are present in the same spectrum, the discrimination of their contribution is not attainable. In this paper a new method is described which allows to discriminate the contribution of two ion species in the wide energy range of nuclear reactions induced in laser-target interactions. The method is based on charge response of two TOF-SiC detectors, of suitable thicknesses, placed in adjacent positions. In presence of two ion species, the response of the detectors, associated with different energy losses, can determine the ion specific contribution to each TOF interval.

Sputtering erosion in ion and plasma thrusters

NASA Technical Reports Server (NTRS)

Ray, Pradosh K.

1995-01-01

An experimental set-up to measure low-energy (below 1 keV) sputtering of materials is described. The materials to be bombarded represent ion thruster components as well as insulators used in the stationary plasma thruster. The sputtering takes place in a 9 inch diameter spherical vacuum chamber. Ions of argon, krypton and xenon are used to bombard the target materials. The sputtered neutral atoms are detected by a secondary neutral mass spectrometer (SNMS). Samples of copper, nickel, aluminum, silver and molybdenum are being sputtered initially to calibrate the spectrometer. The base pressure of the chamber is approximately 2 x 10(exp -9) Torr. the primary ion beam is generated by an ion gun which is capable of delivering ion currents in the range of 20 to 500 nA. The ion beam can be focused to a size approximately 1 mm in diameter. The mass spectrometer is positioned 10 mm from the target and at 90 deg angle to the primary ion beam direction. The ion beam impinges on the target at 45 deg. For sputtering of insulators, charge neutralization is performed by flooding the sample with electrons generated from an electron gun. Preliminary sputtering results, methods of calculating the instrument response function of the spectrometer and the relative sensitivity factors of the sputtered elements will be discussed.

Atmospheric pressure chemical ionization of explosives using alternating current corona discharge ion source.

PubMed

Usmanov, D T; Chen, L C; Yu, Z; Yamabe, S; Sakaki, S; Hiraoka, K

2015-04-01

The high-sensitive detection of explosives is of great importance for social security and safety. In this work, the ion source for atmospheric pressure chemical ionization/mass spectrometry using alternating current corona discharge was newly designed for the analysis of explosives. An electromolded fine capillary with 115 µm inner diameter and 12 mm long was used for the inlet of the mass spectrometer. The flow rate of air through this capillary was 41 ml/min. Stable corona discharge could be maintained with the position of the discharge needle tip as close as 1 mm to the inlet capillary without causing the arc discharge. Explosives dissolved in 0.5 µl methanol were injected to the ion source. The limits of detection for five explosives with 50 pg or lower were achieved. In the ion/molecule reactions of trinitrotoluene (TNT), the discharge products of NOx (-) (x = 2,3), O3 and HNO3 originating from plasma-excited air were suggested to contribute to the formation of [TNT - H](-) (m/z 226), [TNT - NO](-) (m/z 197) and [TNT - NO + HNO3 ](-) (m/z 260), respectively. Formation processes of these ions were traced by density functional theory calculations. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Determination of ambroxol in human plasma using LC-MS/MS.

PubMed

Kim, Hohyun; Yoo, Jeong-Yeon; Han, Sang Beom; Lee, Hee Joo; Lee, Kyung Ryul

2003-06-01

A sensitive and selective liquid chromatographic method coupled with tandem mass spectrometry (LC-MS/MS) was developed for the quantification of ambroxol in human plasma. Domperidone was used as internal standard, with plasma samples extracted using diethyl ether under basic condition. A centrifuged upper layer was then evaporated and reconstituted with 200 microl methanol. The reconstituted samples were injected into a C(18) XTerra MS column (2.1 x 30 mm) with 3.5 microm particle size. The analytical column lasted for at least 600 injections. The mobile phase was composed of 20 mM ammonium acetate in 90% acetonitrile (pH 8.8), with flow rate at 250 microl/min. The mass spectrometer was operated in positive ion mode using turbo electrospray ionization. Nitrogen was used as the nebulizer, curtain, collision, and auxiliary gases. Using MS/MS with multiple reaction monitoring (MRM) mode, ambroxol was detected without severe interferences from plasma matrix. Ambroxol produced a protonated precursor ion ([M+H](+)) at m/z 379 and a corresponding product ion at m/z 264. And internal standard (domperidone) produced a protonated precursor ion ([M+H](+)) at m/z 426 and a corresponding product ion at m/z 174. Detection of ambroxol in human plasma was accurate and precise, with quantification limit at 0.2 ng/ml. This method has been successfully applied to a study of ambroxol in human specimens.

Potentiometric Detection of Pathogens

DTIC Science & Technology

2012-01-01

nanosize organic electrode (conducting polymer top-layer) surface. This approach has then been changed to the gate modification in ion sensitive field...electrode (conducting polymer top-layer) surface. This approach has then been changed to the gate modification in ion sensitive field effect transistors, in...the conducting polymer top-layer, which makes the devices very functional and competitive. Secondly, the device development is discussed and finally

Sensing the heat with TRPM3.

PubMed

Vriens, Joris; Voets, Thomas

2018-05-01

Heat sensation, the ability to detect warm and noxious temperatures, is an ancient and indispensable sensory process. Noxious temperatures can have detrimental effects on the physiology and integrity of cells, and therefore, the detection of environmental hot temperatures is absolutely crucial for survival. Temperature-sensitive ion channels, which conduct ions in a highly temperature-dependent manner, have been put forward as molecular thermometers expressed at the endings of sensory neurons. In particular, several temperature-sensitive members of the transient receptor potential (TRP) superfamily of ion channels have been identified, and a multitude of in vivo studies have shown that the capsaicin-sensitive TRPV1 channel plays a key role as a noxious heat sensor. However, Trpv1-deficient mice display a residual heat sensitivity suggesting the existence of additional heat sensor(s). In this chapter, we provide evidence for the role of the non-selective calcium-permeable TRPM3 ion channel as an additional heat sensor that acts independently of TRPV1, and give an update of the modulation of this channel by various molecular mechanisms. Finally, we compare antagonists of TRPM3 to specific blockers of TRPV1 as potential analgesic drugs to treat pathological pain.

Ion sensors based on novel fiber organic electrochemical transistors for lead ion detection.

PubMed

Wang, Yuedan; Zhou, Zhou; Qing, Xing; Zhong, Weibing; Liu, Qiongzhen; Wang, Wenwen; Li, Mufang; Liu, Ke; Wang, Dong

2016-08-01

Fiber organic electrochemical transistors (FECTs) based on polypyrrole and nanofibers have been prepared for the first time. FECTs exhibited excellent electrical performances, on/off ratios up to 10(4) and low applied voltages below 2 V. The ion sensitivity behavior of the fiber organic electrochemical transistors was investigated. It exhibited that the transfer curve of FECTs shifted to lower gate voltage with increasing cations concentration, the sensitivity reached to 446 μA/dec in the 10(-5)-10(-2) M Pb(2+) concentration range. The ion selective properties of the FECTs have also been systematically studied for the detection of potassium, calcium, aluminum, and lead ions. The devices with different cations showed great difference in response curves. It was suitable for selectively monitoring Pb(2+) with respect to other cations. The results indicated FECTs were very effective for electrochemical sensing of lead ion, which opened a promising perspective for wearable electronics in healthcare and biological application. Graphical Abstract The schematic diagram of fiber organic electrochemical transistors based on polypyrrole and nanofibers for ion sensing.

CdS quantum dots as fluorescence probes for the sensitive and selective detection of highly reactive HSe- ions in aqueous solution.

PubMed

Wu, Chuan-Liu; Zhao, Yi-Bing

2007-06-01

Water-soluble cadmium sulfide (CdS) quantum dots (QDs) capped by mercaptoacetic acid were synthesized by aqueous-phase arrested precipitation, and characterized by transmission electron microscopy, spectrofluorometry, and UV-Vis spectrophotometry. The prepared luminescent water-soluble CdS QDs were evaluated as fluorescence probes for the detection of highly reactive hydrogen selenide ions (HSe(-) ions). The quenching of the fluorescence emission of CdS QDs with the addition of HSe(-) ions is due to the elimination of the S(2-) vacancies which are luminescence centers. Quantitative analysis based on chemical interaction between HSe(-) ions and the surface of CdS QDs is very simple, easy to develop, and has demonstrated very high sensitivity and selectivity features. The effect of foreign ions (common anions and biologically relevant cations) on the fluorescence of the CdS QDs was examined to evaluate the selectivity. Only Cu(2+) and S(2-) ions exhibit significant effects on the fluorescence of CdS QDs. With the developed method, we are able to determine the concentration of HSe(-) ions in the range from 0.10 to 4.80 micromol L(-1), and the limit of detection is 0.087 micromol L(-1). The proposed method was successfully applied to monitor the obtained HSe(-) ions from the reaction of glutathione with selenite. To the best of our knowledge, this is the first report on fluorescence analysis of HSe(-) ions in aqueous solution.

SU-G-BRB-03: Assessing the Sensitivity and False Positive Rate of the Integrated Quality Monitor (IQM) Large Area Ion Chamber to MLC Positioning Errors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boehnke, E McKenzie; DeMarco, J; Steers, J

2016-06-15

Purpose: To examine both the IQM’s sensitivity and false positive rate to varying MLC errors. By balancing these two characteristics, an optimal tolerance value can be derived. Methods: An un-modified SBRT Liver IMRT plan containing 7 fields was randomly selected as a representative clinical case. The active MLC positions for all fields were perturbed randomly from a square distribution of varying width (±1mm to ±5mm). These unmodified and modified plans were measured multiple times each by the IQM (a large area ion chamber mounted to a TrueBeam linac head). Measurements were analyzed relative to the initial, unmodified measurement. IQM readingsmore » are analyzed as a function of control points. In order to examine sensitivity to errors along a field’s delivery, each measured field was divided into 5 groups of control points, and the maximum error in each group was recorded. Since the plans have known errors, we compared how well the IQM is able to differentiate between unmodified and error plans. ROC curves and logistic regression were used to analyze this, independent of thresholds. Results: A likelihood-ratio Chi-square test showed that the IQM could significantly predict whether a plan had MLC errors, with the exception of the beginning and ending control points. Upon further examination, we determined there was ramp-up occurring at the beginning of delivery. Once the linac AFC was tuned, the subsequent measurements (relative to a new baseline) showed significant (p <0.005) abilities to predict MLC errors. Using the area under the curve, we show the IQM’s ability to detect errors increases with increasing MLC error (Spearman’s Rho=0.8056, p<0.0001). The optimal IQM count thresholds from the ROC curves are ±3%, ±2%, and ±7% for the beginning, middle 3, and end segments, respectively. Conclusion: The IQM has proven to be able to detect not only MLC errors, but also differences in beam tuning (ramp-up). Partially supported by the Susan Scott Foundation.« less

An aqueous fluorescent sensor for Pb2+ based on phenothiazine-polyamide.

PubMed

Xie, Yadian; Li, Han; Liu, Xingliang; Wang, Zhaoqian; Lv, Haitang; Cao, Jianfang; Zhang, Chao; Jia, Qiangqiang; Han, Aixia

2018-04-30

A sensitive and selective fluorescent sensor for Pb 2+ ion based on phenothiazine-polyamide was built (named sensor PP). Due to introducing of four diethanolamine groups to polyamide, this sensor was totally water soluble. PP could detect Pb 2+ ion within 1 min in the presence of other metal ions in aqueous solution, the detect limit was 9.11 × 10 -8  M. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid, quantitative and sensitive immunochromatographic assay based on stripping voltammetric detection of a metal ion label

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, Fang; Wang, Kaihua; Lin, Yuehe

2005-10-10

A novel, sensitive immunochromatographic electrochemical biosensor (IEB) which combines an immunochromatographic strip technique with an electrochemical detection technique is demonstrated. The IEB takes advantages of the speed and low-cost of the conventional immunochromatographic test kits and high-sensitivity of stripping voltammetry. Bismuth ions (Bi3+) have been coupled with the antibody through the bifunctional chelating agent diethylenetriamine pentaacetic acid (DTPA). After immunoreactions, Bi3+ was released and quantified by anodic stripping voltammetry at a built-in single-use screen-printed electrode. As an example for the applications of such novel device, the detection of human chorionic gonadotronphin (HCG) in a specimen was performed. This biosensor providesmore » a more user-friendly, rapid, clinically accurate, and less expensive immunoassay for such analysis in specimens than currently available test kits.« less

Ultrasensitive Detection of Cu2+ Using a Microcantilever Sensor Modified with L-Cysteine Self-Assembled Monolayer.

PubMed

Xu, Xiaohe; Zhang, Na; Brown, Gilbert M; Thundat, Thomas G; Ji, Hai-Feng

2017-10-01

A microcantilever was modified with a self-assembled monolayer (SAM) of L-cysteine for the sensitively and selectively response to Cu(II) ions in aqueous solution. The microcantilever undergoes bending due to sorption of Cu(II) ions. The interaction of Cu(II) ions with the L-cysteine on the cantilever is diffusion controlled and does not follow a simple Langmuir adsorption model. A concentration of 10 -10  M Cu(II) was detected in a fluid cell using this technology. Other cations, such as Ni 2+ , Zn 2+ , Pb 2+ , Cd 2+ , Ca 2+ , K + , and Na + , did not respond with a significant deflection, indicating that this L-cysteine-modified cantilever responded selectively and sensitively to Cu(II).

Ruthenium Nanoparticles Mediated Electrocatalytic Reduction of UO22+ Ions for Its Rapid and Sensitive Detection in Natural Waters.

PubMed

Gupta, Ruma; Sundararajan, Mahesh; Gamare, Jayashree S

2017-08-01

Reduction of UO 2 2+ ions to U 4+ ions is difficult due to involvement of two axially bonded oxygen atoms, and often requires a catalyst to lower the activation barrier. The noble metal nanoparticles (NPs) exhibit high electrocatalytic activity, and could be employed for the sensitive and rapid quantifications of U0 2 2+ ions in the aqueous matrix. Therefore, the Pd, Ru, and Rh NPs decorated glassy carbon electrode were examined for their efficacy toward electrocatalytic reduction of UO 2 2+ ions and observed that Ru NPs mediate efficiently the electro-reduction of UO 2 2+ ions. The mechanism of the electroreduction of UO 2 2+ by the RuNPs/GC was studied using density functional theory calculations which pointed different approach of 5f metal ions electroreduction unlike 4p metal ions such as As(III). RuNP decorated on the glassy carbon would be hydrated, which in turn assist to adsorb the uranyl sulfates through hydrogen bonding thus facilitated electro-reduction. Differential pulse voltammetric (DPV) technique, was used for rapid and sensitive quantification of UO 2 2+ ions. The RuNPs/GC based DPV technique could be used to determine the concentration of uranyl in a few minutes with a detection limit of 1.95 ppb. The RuNPs/GC based DPV was evaluated for its analytical performance using seawater as well lake water and groundwater spiked with known amounts of UO 2 2+ .

Improving the Sensitivity of Mass Spectrometer using a High-Pressure Electrodynamic Ion Funnel Interface

PubMed Central

Ibrahim, Yehia; Tang, Keqi; Tolmachev, Aleksey V.; Shvartsburg, Alexandre A.

2006-01-01

We report on a new electrodynamic ion funnel that operates at a pressure of 30 Torr with no loss of ion transmission. The enhanced performance compared to previous ion funnel designs optimized for pressures of <5 Torr was achieved by reducing the ion funnel capacitance and increasing the RF drive frequency (1.7 MHz) and amplitude (100-170 V peak-to-peak). No degradation of ion transmission was observed for pressures from 2 - 30 Torr. The ability to operate at higher pressure enabled a new tandem ion funnel mass spectrometer (MS) interface design that can accommodate a greater gas load. When combined with a multicapillary inlet, the interface provided more efficient introduction of ions, resulting in a significant enhancement in MS sensitivity and detection limits. PMID:16839773

Development of a plug-type IMS-MS instrument and its applications in resolving problems existing in in-situ detection of illicit drugs and explosives by IMS.

PubMed

Du, Zhenxia; Sun, Tangqiang; Zhao, Jianan; Wang, Di; Zhang, Zhongxia; Yu, Wenlian

2018-07-01

Ion mobility spectrometry (IMS) which acts as a rapid analysis technique is widely used in the field detection of illicit drugs and explosives. Due to limited separation abilities of the pint-sized IMS challenges and problems still exist regarding high false positive and false negative responses due to the interference of the matrix. In addition, the gas-phase ion chemistry and special phenomena in the IMS spectra, such one substance showing two peaks, were not identified unambiguously. In order to explain or resolve these questions, in this paper, an ion mobility spectrometry was coupled to a mass spectrometry (IMS-MS). A commercial IMS is embedded in a custom-built ion chamber shell was attached to the mass spectrometer. The faraday plate of IMS was fabricated with a hole for the ions to passing through to the mass spectrometer. The ion transmission efficiency of IMS-MS was optimized by optimizing the various parameters, especially the distance between the faraday plate and the cone of mass spectrum. This design keeps the integrity of the two original instruments and the mass spectrometry still works with multimode ionization source (i.e., IMS-MS, ESI-MS, APCI-MS modes). The illicit drugs and explosive samples were analyzed by the IMS-MS with 63 Ni source. The results showed that the IMS-MS is of high sensitivity. The ionization mechanism of the illicit drug and explosive samples with 63 Ni source were systematically studied. In addition, the interferent which interfered the detection of cocaine was identified as dibutyl phthalate (DBP) by this platform. The reason why the acetone solution of amphetamine showed two peaks was explained. Copyright © 2018 Elsevier B.V. All rights reserved.

Indirect photometric detection of boron cluster anions electrophoretically separated in methanol.

PubMed

Vítová, Lada; Fojt, Lukáš; Vespalec, Radim

2014-04-18

3,5-Dinitrobenzoate and picrate are light absorbing anions pertinent to indirect photometric detection of boron cluster anions in buffered methanolic background electrolytes (BGEs). Tris(hydroxymethyl)aminomethane and morpholine have been used as buffering bases, which eliminated baseline steps, and minimized the baseline noise. In methanolic BGEs, mobilities of boron cluster anions depend on both ionic constituents of the BGE buffer. This dependence can be explained by ion pair interaction of detected anions with BGE cations, which are not bonded into ion pairs with the BGE anions. The former ion pair interaction decreases sensitivity of the indirect photometric detection. Copyright © 2014 Elsevier B.V. All rights reserved.

4-(2-Pyridylazo)-resorcinol Functionalized Thermosensitive Ionic Microgels for Optical Detection of Heavy Metal Ions at Nanomolar Level.

PubMed

Zhou, Xianjing; Nie, Jingjing; Du, Binyang

2015-10-07

4-(2-Pyridylazo)-resorcinol (PAR) functionalized thermosensitive ionic microgels (PAR-MG) were synthesized by a one-pot quaternization method. The PAR-MG microgels were spherical in shape with radius of ca. 166.0 nm and narrow size distribution and exhibited thermo-sensitivity in aqueous solution. The PAR-MG microgels could optically detect trace heavy metal ions, such as Cu(2+), Mn(2+), Pb(2+), Zn(2+), and Ni(2+), in aqueous solutions with high selectivity and sensitivity. The PAR-MG microgel suspensions exhibited characteristic color with the presence of various trace heavy metal ions, which could be visually distinguished by naked eyes. The limit of colorimetric detection (DL) was determined to be 38 nM for Cu(2+) at pH 3, 12 nM for Cu(2+) at pH 7, and 14, 79, 20, and 21 nM for Mn(2+), Pb(2+), Zn(2+), and Ni(2+), respectively, at pH 11, which was lower than (or close to) the United States Environmental Protection Agency standard for the safety limit of these heavy metal ions in drinking water. The mechanism of detection was attributed to the chelation between the nitrogen atoms and o-hydroxyl groups of PAR within the microgels and heavy metal ions.

Performance evaluation of a miniature magnetic sector mass spectrometer onboard a satellite in space.

PubMed

Guo, Meiru; Li, Detian; Cheng, Yongjun; Wang, Yongjun; Sun, Wenjun; Pei, Xiaoqiang; Dong, Meng; Sheng, Xuemin; Zhao, Lan; Li, Yanwu

2018-04-01

With the rapid development of space technology in China, it is urgent to use mass spectrometer to detect the space environment. In this work, a space miniature magnetic sector mass spectrometer is evaluated, which consists of three subsystems: (1) physical unit, (2) electric control unit, (3) and high voltage power. It has 90° magnetic sector-field analyzer with double trajectory, in which a trajectory measurement range is from 1 to 12 amu, the other range is from 6 to 90 amu.The mass spectrometer has two work models, one is used to measure space neutral gas when the filament of mass spectrometer ion source turned on, the other is used to measure space charged ions when the filament turned off. The absolute resolution of this device is less than 1 amu, the minimum detectable ion current is about 10 -13  A, and the sensitivity is 10 -6  A/Pa (N 2 ). Its overall size is 170 mm × 165 mm × 170 mm, its weight is 4.5 kg, and its power consumption is 18 W. A series of environmental adaptability tests, including high and low temperature cycle, shock, vibration, thermal vacuum cycle, were carried out on the ground before launching, and sensitivity and peak position were also calibrated on the ground. In November 2012, the mass spectrometer was carried by an experimental satellite to 499 km sun synchronization and is still working right now. It successfully detected the atmosphere compositions both in the satellite orbit and gas-emitted from satellite, including O, He, 12 CO 2 , 13 CO 2 , H 2 , N 2 , O 2 , H 2 O, and so on.

Sensitive naked eye detection and quantification assay for nitrite by a fluorescence probe in various water resources

NASA Astrophysics Data System (ADS)

Zhang, Fengyuan; Zhu, Xinyue; Jiao, Zhijuan; Liu, Xiaoyan; Zhang, Haixia

2018-07-01

An uncontrolled increase of nitrite concentration in groundwater, rivers and lakes is a growing threat to public health and environment. It is important to monitor the nitrite levels in water and clinical diagnosis. Herein, we developed a switch-off fluorescence probe (PyI) for the sensitive detection of nitrite ions in the aqueous media. This probe selectively recognizes nitrite ions through a distinct visual color change from colorless to pink with a detection limit of 0.1 μM. This method has been successfully applied to the determination of nitrites in tap water, lake water and Yellow River water with recoveries in the range of 94.8%-105.4%.

[Preparation of 1-(2-naphthyl) -3-methyl-5-pyrazolone as pre-column derivatization reagent for the determination of saccharides using high performance liquid chromatography-mass spectrometry].

PubMed

Sun, Zhiwei; Liu, Lingjun; Hu, Baojun; Sheng, Xiao; Wang, Xiaoyan; Suo, Yourui; You, Jinmao

2008-03-01

Eight saccharides were derivatized using 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) as pre-column derivatizing reagent, and separated on a reversed-phase Hypersil ODS 2 column (4.6 mm x 200 mm, 5 microm), by high performance liquid chromatography (HPLC) in conjunction with a gradient elution, detected by a diode array detector (DAD), and identified by electrospray ionization-mass spectrometry (ESI-MS) in positive ion mode. NMP reacted with reductive saccharides easily in the presence of 17% ammonia water at 70 degrees C. All linear correlation coefficients for saccharide derivatives were over 0.998 5. The detection limits (at signal-to-noise of 3:1) were 0.58 - 1.1 pmol for saccharide derivatives. The characteristic fragment ions, especially m/z 473, from the cleavage of NMP-labeled saccharides exhibited high regularity for the identification of the composition of saccharide mixture. The established method is sensitive and repeatable for the determination of saccharides.

Detection of Ketones by a Novel Technology: Dipolar Proton Transfer Reaction Mass Spectrometry (DP-PTR-MS)

NASA Astrophysics Data System (ADS)

Pan, Yue; Zhang, Qiangling; Zhou, Wenzhao; Zou, Xue; Wang, Hongmei; Huang, Chaoqun; Shen, Chengyin; Chu, Yannan

2017-05-01

Proton transfer reaction mass spectrometry (PTR-MS) has played an important role in the field of real-time monitoring of trace volatile organic compounds (VOCs) due to its advantages such as low limit of detection (LOD) and fast time response. Recently, a new technology of proton extraction reaction mass spectrometry (PER-MS) with negative ions OH- as the reagent ions has also been presented, which can be applied to the detection of VOCs and even inorganic compounds. In this work, we combined the functions of PTR-MS and PER-MS in one instrument, thereby developing a novel technology called dipolar proton transfer reaction mass spectrometry (DP-PTR-MS). The selection of PTR-MS mode and PER-MS mode was achieved in DP-PTR-MS using only water vapor in the ion source and switching the polarity. In this experiment, ketones (denoted by M) were selected as analytes. The ketone (molecular weight denoted by m) was ionized as protonated ketone [M + H]+ [mass-to-charge ratio ( m/z) m + 1] in PTR-MS mode and deprotonated ketone [M - H]- ( m/z m - 1) in PER-MS mode. By comparing the m/z value of the product ions in the two modes, the molecular weight of the ketone can be positively identified as m. Results showed that whether it is a single ketone sample or a mixed sample of eight kinds of ketones, the molecular weights can be detected with DP-PTR-MS. The newly developed DP-PTR-MS not only maintains the original advantages of PTR-MS and PER-MS in sensitive and rapid detection of ketones, but also can estimate molecular weight of ketones.

The Remote Detection of Alpha-Radioactive Nucleus Decay

NASA Astrophysics Data System (ADS)

Gurkovskiy, Boris; Miroshnichenko, Vladimir; Onishchenko, Evgeny; Simakov, Andrey; Streil, Thomas

Results of the new device design for the alpha-radiation remote detection are presented. Negative ions from the alpha particle tracks are detected by the discharge wire counter opened to air. Ion clusters being transferred from the particle tracks to the detector volume by an air flux. The detector works in a counting mode that provides sharp selectivity and accuracy of measurements. The basic parameters of the device are: detecting distance -0.5 m; measurement time -30 s; the square sensitivity -0.05 Bq/cm2.

A Metal-Polydopamine Framework (MPDA) as an Effective Fluorescent Quencher for Highly Sensitive Detection of Hg (II) And Ag (I) ions Through Exonuclease III Activity.

PubMed

Ravikumar, Ayyanu; Panneerselvam, Perumal; Morad, Norhashimah

2018-05-24

In this paper, we propose a metal-polydopamine framework (MPDA) with specific molecular probe which appears to be the most promising approach to a strong fluorescence quencher. The MPDA framework quenching ability towards various organic fluorophore such as aminoethylcomarin acetate (AMCA), 6-carboxyfluorescein (FAM), carboxyteramethylrhodamine (TAMRA) and Cy5 are used to establish a fluorescent biosensor that can selectively recognize Hg2+ and Ag+ ion. The fluorescent quenching efficiency was sufficient to achieve more than 96%. The MPDA framework also exhibits different affinities with ssDNA and dsDNA. In addition, the FAM labelled ssDNA was adsorbed onto MPDA framework, based on their interaction with the complex formed between MPDA frameworks/ssDNA taken as a sensing platform. By taking advantage of this sensor highly sensitive and selective determination of Hg2+and Ag+ ions is achieved through Exonuclease III signal amplification activity. The detection limits of Hg2+and Ag+ achieved to be 1.2 pM and 34 pM respectively, were compared to co-existing metal ions and GO based sensors. Furthermore, the potential applications of this study establish the highly sensitive fluorescence detection targets in environmental and biological fields.

Rapid synthesis of N, S co-doped carbon dots and their application for Fe3+ ion detection

NASA Astrophysics Data System (ADS)

Zhang, Jian; Wang, Junbin; Fu, Jinping; Fu, Xucheng; Gan, Wei; Hao, Hequn

2018-02-01

In this study, nitrogen and sulfur co-doped carbon dots (NSCDs) were fabricated by microwave-assisted one-pot synthesis using vitamin C and thiourea as precursors. The as-prepared NSCDs demonstrated excellent properties, including aqueous dispensability, strong fluorescence emission, excellent environmental stability, high selectivity, and sensitivity toward Fe3+ ions. The NSCD-based material can be used as a "turn off" fluorescent probe for detecting Fe3+ ions at a low detection limit (4.2 nM). In addition, the "turn off" and "turn on" of NSCD fluorescent probe could be modulated by adding Fe3+ and EDTA, indicating weak interaction between the Fe3+ ions and NSCDs.

Simultaneous determination of water-soluble vitamins in selected food matrices by liquid chromatography/electrospray ionization tandem mass spectrometry.

PubMed

Gentili, Alessandra; Caretti, Fulvia; D'Ascenzo, Giuseppe; Marchese, Stefano; Perret, Daniela; Di Corcia, Daniele; Rocca, Lucia Mainero

2008-07-01

A rapid, simple and sensitive method based on liquid chromatography/tandem mass spectrometry (LC/MS/MS) with an electrospray ionization (ESI) source for the simultaneous analysis of fourteen water-soluble vitamins (B1, B2, two B3 vitamers, B5, five B6 vitamers, B8, B9, B12 and C) in various food matrices, i.e. maize flour, green and golden kiwi and tomato pulp, is presented here. Analytes were separated by ion-suppression reversed-phase liquid chromatography in less than 10 min and detected in positive ion mode. Sensitivity and specificity of this method allowed two important results to be achieved: (i) limits of detection of the analytes at ng g(-1) levels (except for vitamin C); (ii) development of a rapid sample treatment that minimizes analyte exposition to light, air and heat, eliminating any step of extract concentration. Analyte recovery depended on the type of matrix. In particular, recovery of the analytes in maize flour was > or =70%, with the exception of vitamin C, pyridoxal-5'-phosphate and vitamin B9 (ca 40%); with tomato pulp, recovery was > or =64%, except for vitamin C (41%); with kiwi, recovery was > or =73%, except for nicotinamide (ca. 30%).

Using ion chromatography to monitor haloacetic acids in drinking water: a review of current technologies.

PubMed

Paull, Brett; Barron, Leon

2004-08-13

A review of the application of ion chromatography to the determination of haloacetic acids in drinking water is given. As it requires no sample derivatisation, ion chromatography in its various modes, such as ion-exchange, ion-interaction and ion-exclusion chromatography, is increasingly being investigated as a simpler alternative to gas chromatographic methods for the determination of polar disinfection by-products (DBPs) in drinking waters. Detection limits quoted for the regulated haloacetic acids (HAA5), are commonly in the mid to low microg/L range, however, in most cases analyte preconcentration is still necessary for detection at concentrations commonly found in actual drinking water samples. The coupling of ion chromatography to electrospray mass spectrometry provides a potential future direction, with improved sensitivity and selectivity compared to conductivity based detection, however associated cost and complexity for routine analysis is currently relatively high.

High sensitivity field asymmetric ion mobility spectrometer

NASA Astrophysics Data System (ADS)

Chavarria, Mario A.; Matheoud, Alessandro V.; Marmillod, Philippe; Liu, Youjiang; Kong, Deyi; Brugger, Jürgen; Boero, Giovanni

2017-03-01

A high sensitivity field asymmetric ion mobility spectrometer (FAIMS) was designed, fabricated, and tested. The main components of the system are a 10.6 eV UV photoionization source, an ion filter driven by a high voltage/high frequency n-MOS inverter circuit, and a low noise ion detector. The ion filter electronics are capable to generate square waveforms with peak-to-peak voltages up to 1000 V at frequencies up to 1 MHz with adjustable duty cycles. The ion detector current amplifier has a gain up to 1012 V/A with an effective equivalent input noise level down to about 1 fA/Hz1/2 during operation with the ion filter at the maximum voltage and frequency. The FAIMS system was characterized by detecting different standard chemical compounds. Additionally, we investigated the use of a synchronous modulation/demodulation technique to improve the signal-to-noise ratio in FAIMS measurements. In particular, we implemented the modulation of the compensation voltage with the synchronous demodulation of the ion current. The analysis of the measurements at low concentration levels led to an extrapolated limit of detection for acetone of 10 ppt with an averaging time of 1 s.

Simultaneous analysis of strychnine and brucine and their major metabolites by liquid chromatography-electrospray ion trap mass spectrometry.

PubMed

Chen, Xueguo; Lai, Yongquan; Cai, Zongwei

2012-04-01

A liquid chromatography-electrospray ionization-ion trap mass spectrometry (LC-ESI-ITMS) method was developed for the simultaneous analysis of strychnine, brucine and their major metabolites. Strychnine and brucine were individually incubated with rat liver S9 fraction. The incubation samples were pooled together and analyzed with LC-ESI-ITMS in positive ion and full-scan detection mode. The calibration curves of strychnine and brucine in rat liver showed good linearity in ranges of 0.020 to 8.0 µg/mL for strychnine and 0.020 to 8.5 µg/mL for brucine. The limits of detections were both 0.008 µg/mL and the recoveries were 88.3 and 83.2% for strychnine and brucine, respectively. Two metabolites were identified as strychnine N-oxide and brucine N-oxide by comparing the molecular mass, retention time, full-scan mass spectra, tandem MS and MS(3) spectra with those of strychnine and brucine. The developed method provided high sensitivity and selectivity for the determination of poisonous alkaloids and their major metabolites and can be applied in the determination of samples in forensic and clinically toxicological cases.

Reversal electron attachment ionizer for detection of trace species

NASA Technical Reports Server (NTRS)

Bernius, Mark T. (Inventor); Chutjian, Ara (Inventor)

1990-01-01

An in-line reversal electron, high-current ionizer capable of focusing a beam of electrons to a reversal region and executing a reversal of said electrons, such that the electrons possess zero kinetic energy at the point of reversal, may be used to produce both negative and positive ions. A sample gas is introduced at the point of electron reversal for low energy electron-(sample gas) molecule attachment with high efficiency. The attachment process produces negative ions from the sample gas, which includes species present in trace (minute) amounts. These ions are extracted efficiently and directed to a mass analyzer where they may be detected and identified. The generation and detection of positive ions is accomplished in a similar fashion with minimal adjustment to potentials applied to the apparatus.

Reversal electron attachment ionizer for detection of trace species

NASA Technical Reports Server (NTRS)

Bernius, Mark T. (Inventor); Chutjian, Ara (Inventor)

1989-01-01

An in-line reversal electron, high-current ionizer capable of focusing a beam of electrons to a reversal region and executing a reversal of the electrons, such that the electrons possess zero kinetic energy at the point of reversal, may be used to produce both negative and positive ions. A sample gas is introduced at the point of electron reversal for low energy electron-(sample gas) molecule attachment with high efficiency. The attachment process produces negative ions from the sample gas, which includes species present in trace (minute) amounts. These ions are extracted efficiently and directed to a mass analyzer where they may be detected and identified. The generation and detection of positive ions is accomplished in a similar fashion with minimal adjustment to potentials applied to the apparatus.

Hydrogen sulfide measurement using sulfide dibimane: critical evaluation with electrospray ion trap mass spectrometry

PubMed Central

Shen, Xinggui; Chakraborty, Sourav; Dugas, Tammy R; Kevil, Christopher G

2015-01-01

Accurate measurement of hydrogen sulfide bioavailability remains a technical challenge due to numerous issues involving sample processing, detection methods used, and actual biochemical products measured. Our group and others have reported that reverse phase HPLC detection of sulfide dibimane (SDB) product from the reaction of H2S/HS− with monobromobimane allows for analytical detection of hydrogen sulfide bioavailability in free and other biochemical forms. However, it remains unclear whether possible interfering contaminants may contribute to HPLC SDB peak readings that may result in inaccurate measurements of bioavailable sulfide. In this study, we critically compared hydrogen sulfide dependent SDB detection using reverse phase HPLC (RP-HPLC) versus quantitative SRM electrospray ionization mass spectrometry (ESI/MS) to obtain greater clarity into the validity of the reverse phase HPLC method for analytical measurement of hydrogen sulfide. Using an LCQ-deca ion-trap mass spectrometer, SDB was identified by ESI/MS positive ion mode, and quantified by selected reaction monitoring (SRM) using hydrocortisone as an internal standard. Collision induced dissociation (CID) parameters were optimized at MS2 level for SDB and hydrocortisone. ESI/MS detection of SDB standard was found to be a log order more sensitive than RP-HPLC with a lower limit of 0.25 nM. Direct comparison of tissue and plasma SDB levels using RP-HPLC and ESI/MS methods revealed comparable sulfide levels in plasma, aorta, heart, lung and brain. Together, these data confirm the use of SDB as valid indicator of H2S bioavailability and highlights differences between analytical detection methods. PMID:24932544

DOE Office of Scientific and Technical Information (OSTI.GOV)

Burrows, T.A.; Thoma, P.J.

Two types of ion-mobility detectors were evaluated in both laboratory and field tests. Laboratory test results show that these detectors are highly sensitive to dynamite and pistol powder and have good false-alarm agent rejection. Field tests of these two detectors revealed that they would detect dynamite and Ball-C-Propellent in free air. However, neither of the ion-mobility detectors would detect these explosives if the explosives were concealed.

In situ electro-polymerization of nitrogen doped carbon dots and their application in an electrochemiluminescence biosensor for the detection of intracellular lead ions.

PubMed

Xiong, Chengyi; Liang, Wenbin; Wang, Haijun; Zheng, Yingning; Zhuo, Ying; Chai, Yaqin; Yuan, Ruo

2016-04-25

Here, a novel sensitive electrochemiluminescence (ECL) biosensor using N doped carbon dots (N-CDs) in situ electro-polymerized onto a glassy carbon electrode (GCE) as luminophores, and Pd-Au hexoctahedrons (Pd@Au HOHs) as enhancers, was developed for the detection of intracellular lead ions (Pb(2+)).

On-site Rapid Detection of Trace Non-volatile Inorganic Explosives by Stand-alone Ion Mobility Spectrometry via Acid-enhanced Evaporization

PubMed Central

Peng, Liying; Hua, Lei; Wang, Weiguo; Zhou, Qinghua; Li, Haiyang

2014-01-01

New techniques for the field detection of inorganic improvised explosive devices (IEDs) are urgently developed. Although ion mobility spectrometry (IMS) has been proved to be the most effective method for screening organic explosives, it still faces a major challenge to detect inorganic explosives owing to their low volatilities. Herein, we proposed a strategy for detecting trace inorganic explosives by thermal desorption ion mobility spectrometry (TD-IMS) with sample-to-sample analysis time less than 5 s based on in-situ acidification on the sampling swabs. The responses for typical oxidizers in inorganic explosives, such as KNO3, KClO3 and KClO4 were at least enhanced by a factor of 3000 and their limits of detection were found to be subnanogram. The common organic explosives and their mixtures with inorganic oxidizers were detected, indicating that the acidification process did not affect the detection of organic explosives. Moreover, the typical inorganic explosives such as black powders, firecrackers and match head could be sensitively detected as well. These results demonstrated that this method could be easily employed in the current deployed IMS for on-site sensitive detection of either inorganic explosives or organic ones. PMID:25318960

Detection of volatile compounds emitted by Pseudomonas aeruginosa using selected ion flow tube mass spectrometry.

PubMed

Carroll, Will; Lenney, Warren; Wang, Tianshu; Spanel, Patrik; Alcock, Alice; Smith, David

2005-05-01

Pseudomonas aeruginosa (PA) is associated with a distinctive smell produced by a combination of volatile compounds (VCs). Selected ion flow tube mass spectrometry (SIFT-MS) provides a novel and rapid methodology for rapid, accurate detection of trace quantities (parts per billion; ppb) of VCs in air. We studied the VCs produced by different isolates of PA cultures in vitro from patients with cystic fibrosis. Twenty-one patients with cystic fibrosis provided sputum and cough swab samples for culture. These were used to inoculate blood agar (BA) and Pseudomonas-selective media (PSM). These plates were incubated for 48 hr at 37 degrees C inside sealed plastic bags. The air surrounding the samples after 48 hr (headspace) was analyzed using SIFT-MS. PA growth was commonly associated with the production of significant quantities of VCs, notably hydrogen cyanide gas (HCN). This was detectable in the headspace of 15/22 of PA-positive samples. In contrast, it was only seen in the headspace of 1/13 control samples (6 sterile plates and 7 plates with only mixed upper respiratory tract flora). The concentration of HCN was significantly higher above PA-positive samples than above other bacterial growth (P < 0.01), and in our study, levels of HCN greater than 100 ppb were a sensitive (68%) and highly specific (100%) biomarker of PA. SIFT-MS can detect a range of VCs from PA in vitro. HCN may be a specific indicator of PA infection in vivo, and offers promise as a biomarker for noninvasive detection of PA infection by breath analysis. Copyright 2005 Wiley-Liss, Inc

Beam production of a laser ion source with a rotating hollow cylinder target for low energy positive and negative ions

NASA Astrophysics Data System (ADS)

Saquilayan, G. Q.; Wada, M.

2017-08-01

A laser ion source that utilizes a hollow cylinder target is being developed for the production of positive and negative ions. Continuous operation of the laser ion source is possible through the design of a rotating target. Ion extraction through a grounded circular aperture was tested for positive and negative ions up to 1 kV. Time-of-flight measurements for the mass separation of ions were made by placing a Faraday cup at locations 0 and 15 mm from the beam extraction axis. Signals corresponding to slow and massive ions were detected with mass at least 380 amu. Investigation on the beam profile suggests a geometrical optimization of the beam forming system is necessary.

Sodium Chloride Crystal-Induced SERS Platform for Controlled Highly Sensitive Detection of Illicit Drugs.

PubMed

Yu, Borong; Li, Pan; Zhou, Binbin; Tang, Xianghu; Li, Shaofei; Yang, Liangbao

2018-04-03

A sodium chloride crystal-driven spontaneous 'hot spot' structure was demonstrated as a SERS-active platform, to get reproducible SERS signals, and eliminate the need for mapping large areas, in comparison with solution phase testing. During the process of solvent evaporation, the crystals produced induced silver aggregates to assemble around themselves. The micro-scale crystals can also act as a template to obtain an optical position, such that the assembled hot area is conveniently located during SERS measurements. More importantly, the chloride ions added in colloids can also replace the citrate and on the surface of the silver sol, and further decrease the background interference. High quality SERS spectra from heroin, methamphetamine (MAMP), and cocaine have been obtained on the crystal-driven hot spot structure with high sensitivity and credible reproducibility. This approach can not only bring the nanoparticles to form plasmonic hot spots in a controlled way, and thus provide high sensitivity, but also potentially be explored as an active substrate for label-free detection of other illicit drugs or additives. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Chloride ion transport and overexpression of TMEM16A in a guinea-pig asthma model.

PubMed

Kondo, M; Tsuji, M; Hara, K; Arimura, K; Yagi, O; Tagaya, E; Takeyama, K; Tamaoki, J

2017-06-01

TMEM16A, a Ca-activated Cl channel, regulates various physiological functions such as mucin secretion. However, the role of TMEM16A in hyper-secretion in asthma is not fully understood. The aim of this study is to evaluate Cl ion transport via TMEM16A and determine the localization of TMEM16A in a guinea-pig asthma model. Guinea-pigs were sensitized with ovalbumin (OVA) i.p. on Days 1 and 8. On Day 22, we assessed OVA challenge-induced Cl ion transport in the sensitized tracheas ex vivo in an Ussing chamber, compared with the non-sensitized tracheas. We then examined the effect of T16Ainh-A01, a TMEM16A inhibitor, on the increase in Cl ion transport. The tracheal epithelium was immunostained with an anti-TMEM16A antibody. Epithelial cells from guinea-pig tracheas were cultured at the air-liquid interface in the presence of IL-13 for in vitro study. We studied the effect of TMEM16A inhibitors on Ca-dependent agonist, uridine triphosphate (UTP)-induced increases in Cl ion transport in the cultured cells. The cells were immunostained with an anti-TMEM16A antibody, an anti-MUC5AC antibody and an anti-α-tubulin antibody. OVA challenge induced an increase in short circuit current within 1 min in the OVA-sensitized tracheas but not in the non-sensitized tracheas, which was inhibited by pretreatment of T16Ainh-A01. Sensitized tracheas showed goblet cell metaplasia with more positive TMEM16A immunostaining, particularly in the apical portion compared with the non-sensitized tracheas. The in vitro UTP-induced increase in Cl ion transport was strongly inhibited by pretreatment with T16Ainh-A01, benzbromarone, and niflumic acid. TMEM16A was positively immunostained at the apical portion and in the MUC5AC-positive area in IL-13-induced goblet cell metaplasia. Antigen challenge and Ca-dependent agonist treatment increased Cl ion transport via the overexpression of TMEM16A in goblet cell metaplasia in a guinea-pig asthma model. TMEM16A inhibitors may be useful for the treatment of hyper-secretion in asthma. © 2017 John Wiley & Sons Ltd.

Mastering analytical challenges for the characterization of pentacyclic triterpene mono- and diesters of Calendula officinalis flowers by non-aqueous C30 HPLC and hyphenation with APCI-QTOF-MS.

PubMed

Nicolaus, Christoph; Sievers-Engler, Adrian; Murillo, Renato; D'Ambrosio, Michele; Lämmerhofer, Michael; Merfort, Irmgard

2016-01-25

Pentacyclic triterpene mono- and diesters have been isolated from Calendula officinalis flowers. GC-MS, APCI-Exactive Orbitrap HR-MS and NMR allowed to identify the triterpene skeleton in various samples (different triterpene mixtures from Calendula n-hexane extract). NMR provided evidence that triterpene diesters are present in the samples as well. However, the corresponding quasi-molecular ions could not be detected by APCI-Exactive Orbitrap HR-MS. Instability of triterpene diesters and loss of a fatty acid residue, respectively, in the ion-source made their MS detection challenging. Thus, a set of new APCI-QTOF-MS methods (using the TripleTOF 5600+ mass spectrometer) were developed which made it eventually possible to solve this problem and confirm the diester structures by MS via quasi-molecular ion [M+H](+) detection. Direct infusion APCI-QTOF MS experiments in MS/MS high sensitivity scan mode with low collision energy and multi-channel averaging acquisition (MCA) allowed the detection of quasi-molecular ions of triterpene diesters for the first time and unequivocally confirmed the presence of faradiol 3,16-dimyristate and -dipalmitate, as well as the corresponding mixed diesters faradiol 3-myristate,16-palmitate and faradiol 3-palmitate,16-myristate. Preferential loss of the fatty acid in 16-position made it possible to distinguish the mixed diesters by MS/MS spectra. Their chromatographic separations turned out to be challenging due to their bulkiness and extended molecular dimensions. However, separation could be achieved by an uncommon non-aqueous RPLC mode with an in-house synthesized C30 phase. Finally, two (U)HPLC-APCI-QTOF-MS methods with C18- and C30-based non-aqueous RPLC provided suitable, sensitive assays to monitor the presence of monoesters and diesters of various triterpenes (faradiol, maniladiol, arnidiol, arnitriol A and lupane-3β,16β,20-triol esters) in the n-hexane extract of C. officinalis with high mass resolution and good mass accuracy. Copyright © 2015 Elsevier B.V. All rights reserved.

A new dual-channel optical signal probe for Cu2+ detection based on morin and boric acid.

PubMed

Wang, Peng; Yuan, Bin Fang; Li, Nian Bing; Luo, Hong Qun

2014-01-01

In this work we utilized the common analytical reagent morin to develop a new a dual-channel, cost-effective, and sensitive method for determination of Cu(2+). It is found that morin is only weakly fluorescent by itself, but forms highly fluorescent complexes with boric acid. Moreover, the fluorescence of complexes of morin with boric acid is quenched linearly by Cu(2+) in a certain concentration range. Under optimum conditions, the fluorescence quenching efficiency was linearly proportional to the concentration of cupric ions in the range of 0.5-25 μM with high sensitivity, and the detection limit for Cu(2+) was 0.38 μM. The linear range was 1-25 μM determined by spectrophotometry, and the detection limit for cupric ions was 0.8 μM. Furthermore, the mechanism of sensitive fluorescence quenching response of morin to Cu(2+) is discussed.

Highly sensitive strategy for Hg2+ detection in environmental water samples using long lifetime fluorescence quantum dots and gold nanoparticles.

PubMed

Huang, Dawei; Niu, Chenggang; Ruan, Min; Wang, Xiaoyu; Zeng, Guangming; Deng, Canhui

2013-05-07

The authors herein described a time-gated fluorescence resonance energy transfer (TGFRET) sensing strategy employing water-soluble long lifetime fluorescence quantum dots and gold nanoparticles to detect trace Hg(2+) ions in aqueous solution. The water-soluble long lifetime fluorescence quantum dots and gold nanoparticles were functionalized by two complementary ssDNA, except for four deliberately designed T-T mismatches. The quantum dot acted as the energy-transfer donor, and the gold nanoparticle acted as the energy-transfer acceptor. When Hg(2+) ions were present in the aqueous solution, DNA hybridization will occur because of the formation of T-Hg(2+)-T complexes. As a result, the quantum dots and gold nanoparticles are brought into close proximity, which made the energy transfer occur from quantum dots to gold nanoparticles, leading to the fluorescence intensity of quantum dots to decrease obviously. The decrement fluorescence intensity is proportional to the concentration of Hg(2+) ions. Under the optimum conditions, the sensing system exhibits the same liner range from 1 × 10(-9) to 1 × 10(-8) M for Hg(2+) ions, with the detection limits of 0.49 nM in buffer and 0.87 nM in tap water samples. This sensor was also used to detect Hg(2+) ions from samples of tap water, river water, and lake water spiked with Hg(2+) ions, and the results showed good agreement with the found values determined by an atomic fluorescence spectrometer. In comparison to some reported colorimetric and fluorescent sensors, the proposed method displays the advantage of higher sensitivity. The TGFRET sensor also exhibits excellent selectivity and can provide promising potential for Hg(2+) ion detection.

Application of Ni-63 photo and corona discharge ionization for the analysis of chemical warfare agents and toxic wastes

NASA Technical Reports Server (NTRS)

Stach, J.; Adler, J.; Brodacki, M.; Doring, H.-R.

1995-01-01

Over the past decade, advances in instrumental design and refinements in the understanding of ion molecule reactions at atmospheric pressure enabled the application of Ion Mobility Spectrometry (IMS) as a simple inexpensive and sensitive analytical method for the detection of organic trace compounds. Positive and negative gas-phase ions for ion mobility spectrometry have been produced by a variety of methods, including photo-ionization, laser multi photon ionization, surface ionization, corona discharge ionization. The most common ion source used in ion mobility spectrometry is a radioactive Ni-63 foil which is favored due to simplicity, stability, convenience, and high selectivity. If reactant ions like (H2O(n)H)(+) or (H2O(n)O2)(-) dominate in the reaction region, nearly all kinds of compounds with a given proton or electron affinity; are ionized. However, the radioactivity of the Ni-63 foil is one disadvantage of this ion source that stimulates the development and application of other ionization techniques. In this paper, we report analyses of old chemical warfare agents and toxic wastes using Bruker RAID ion mobility spectrometers. Due to the modular construction of the measuring cell, the spectrometers can be equipped with different ion sources. The combined use of Ni-63, photo- and corona discharge ionization allows the identification of different classes of chemical compounds and yields in most cases comparable results.

The molecular basis for water taste in Drosophila

PubMed Central

Cameron, Peter; Hiroi, Makoto; Ngai, John; Scott, Kristin

2010-01-01

The detection of water and the regulation of water intake are essential for animals to maintain proper osmotic homeostasis1. Drosophila and other insects have gustatory sensory neurons that mediate the recognition of external water sources2-4, but little is known about the underlying molecular mechanism for water taste detection. Here, we identify a member of the Degenerin/Epithelial Sodium Channel family5, ppk28, as an osmosensitive ion channel that mediates the cellular and behavioral response to water. We use molecular, cellular, calcium imaging and electrophysiological approaches to show that ppk28 is expressed in water-sensing neurons and loss of ppk28 abolishes water sensitivity. Moreover, ectopic expression of ppk28 confers water sensitivity to bitter-sensing gustatory neurons in the fly and sensitivity to hypo-osmotic solutions when expressed in heterologous cells. These studies link an osmosensitive ion channel to water taste detection and drinking behavior, providing the framework for examining the molecular basis for water detection in other animals. PMID:20364123

Improvement of ion chromatography with ultraviolet photometric detection and comparison with conductivity detection for the determination of serum cations.

PubMed

Shintani, H

1985-05-31

Studies were made of the analytical conditions required for indirect photometric ion chromatography using ultraviolet photometric detection (UV method) for the determination of serum cations following a previously developed serum pre-treatment. The sensitivities of the conductivity detection (CD) and UV methods and the amounts of serum cations determined by both methods were compared. Attempts to improve the sensitivity of the conventional UV method are reported. It was found that the mobile phase previously reported by Small and Miller showed no quantitative response when more than 4 mM copper(II) sulphate pentahydrate was used. As a result, there was no significant difference in the amounts of serum cations shown by the CD and UV methods. However, by adding 0.5-5 mM cobalt(II) sulphate heptahydrate, nickel(II) sulphate hexahydrate, zinc(II) sulphate heptahydrate or cobalt(II) diammonium sulphate hexahydrate to 0.5-1.5 mM copper(II) sulphate pentahydrate, higher sensitivity and a quantitative response were attained.

Highly Sensitive and Selective Uranium Detection in Natural Water Systems Using a Luminescent Mesoporous Metal-Organic Framework Equipped with Abundant Lewis Basic Sites: A Combined Batch, X-ray Absorption Spectroscopy, and First Principles Simulation Investigation.

PubMed

Liu, Wei; Dai, Xing; Bai, Zhuanling; Wang, Yanlong; Yang, Zaixing; Zhang, Linjuan; Xu, Lin; Chen, Lanhua; Li, Yuxiang; Gui, Daxiang; Diwu, Juan; Wang, Jianqiang; Zhou, Ruhong; Chai, Zhifang; Wang, Shuao

2017-04-04

Uranium is not only a strategic resource for the nuclear industry but also a global contaminant with high toxicity. Although several strategies have been established for detecting uranyl ions in water, searching for new uranium sensor material with great sensitivity, selectivity, and stability remains a challenge. We introduce here a hydrolytically stable mesoporous terbium(III)-based MOF material compound 1, whose channels are as large as 27 Å × 23 Å and are equipped with abundant exposed Lewis basic sites, the luminescence intensity of which can be efficiently and selectively quenched by uranyl ions. The detection limit in deionized water reaches 0.9 μg/L, far below the maximum contamination standard of 30 μg/L in drinking water defined by the United States Environmental Protection Agency, making compound 1 currently the only MOF material that can achieve this goal. More importantly, this material exhibits great capability in detecting uranyl ions in natural water systems such as lake water and seawater with pH being adjusted to 4, where huge excesses of competing ions are present. The uranyl detection limits in Dushu Lake water and in seawater were calculated to be 14.0 and 3.5 μg/L, respectively. This great detection capability originates from the selective binding of uranyl ions onto the Lewis basic sites of the MOF material, as demonstrated by synchrotron radiation extended X-ray adsorption fine structure, X-ray adsorption near edge structure, and first principles calculations, further leading to an effective energy transfer between the uranyl ions and the MOF skeleton.

Proton transfer mass spectrometry at 11 hPa with a circular glow discharge: Sensitivities and applications

NASA Astrophysics Data System (ADS)

Hanson, D. R.; Koppes, M.; Stoffers, A.; Harsdorf, R.; Edelen, K.

2009-04-01

The design and testing of a circular glow discharge ion source on a custom built proton transfer mass spectrometer are described. Also, issues important for quantitative measurements of volatile organic compounds using this instrument were investigated. Detailed calibration procedures based on gravimetry are presented, and representative outdoor air data are shown. Calibrations yield a good sensitivity, up to a few Hz/pptv for some compounds, and the detection limit (S/N = 3) is ~100 pptv or better for methanol, acetaldehyde and acetone (5 s sampling time with a 5 s zero). Detection limits are much lower for most other compounds due to high sensitivity and low background. For ions with m/z > ~90 the background signals are very low and species that appear efficiently at these m/z can be detected at the 10 pptv level in a few seconds. Ion breakup processes for alcohols show that a major product ion of mono-functional alcohols is at 57 u, presumably C4H9+. Oxalic acid is an interesting case in that a major product ion appears on an even mass, 46 u, presumably CO2H2+. The circular glow discharge source is easy to construct and deploy in proton transfer mass spectrometry studies at ~11 hPa. Continuous use of the system over time periods of many days and stable operation over time periods of months to years between disassembly and cleaning demonstrates its robustness.

Microscopy outperformed in a comparison of five methods for detecting Trichomonas vaginalis in symptomatic women.

PubMed

Nathan, B; Appiah, J; Saunders, P; Heron, D; Nichols, T; Brum, R; Alexander, S; Baraitser, P; Ison, C

2015-03-01

In the UK, despite its low sensitivity, wet mount microscopy is often the only method of detecting Trichomonas vaginalis infection. A study was conducted in symptomatic women to compare the performance of five methods for detecting T. vaginalis: an in-house polymerase chain reaction (PCR); Aptima T. vaginalis kit; OSOM ®Trichomonas Rapid Test; culture and microscopy. Symptomatic women underwent routine testing; microscopy and further swabs were taken for molecular testing, OSOM and culture. A true positive was defined as a sample that was positive for T. vaginalis by two or more different methods. Two hundred and forty-six women were recruited: 24 patients were positive for T. vaginalis by two or more different methods. Of these 24 patients, 21 patients were detected by real-time PCR (sensitivity 88%); 22 patients were detected by the Aptima T. vaginalis kit (sensitivity 92%); 22 patients were detected by OSOM (sensitivity 92%); nine were detected by wet mount microscopy (sensitivity 38%); and 21 were detected by culture (sensitivity 88%). Two patients were positive by just one method and were not considered true positives. All the other detection methods had a sensitivity to detect T. vaginalis that was significantly greater than wet mount microscopy, highlighting the number of cases that are routinely missed even in symptomatic women if microscopy is the only diagnostic method available. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

Direct large volume injection ultra-high performance liquid chromatography-tandem mass spectrometry determination of artificial sweeteners sucralose and acesulfame in well water.

PubMed

Wu, Minghuo; Qian, Yichao; Boyd, Jessica M; Hrudey, Steve E; Le, X Chris; Li, Xing-Fang

2014-09-12

Acesulfame (ACE) and sucralose (SUC) have become recognized as ideal domestic wastewater contamination indicators. Liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) analysis is commonly used; however, the sensitivity of SUC is more than two orders of magnitude lower than that of ACE, limiting the routine monitoring of SUC. To address this issue, we examined the ESI behavior of both ACE and SUC under various conditions. ACE is ionic in aqueous solution and efficiently produces simple [M-H](-) ions, but SUC produces multiple adduct ions, limiting its sensitivity. The formic acid (FA) adducts of SUC [M+HCOO](-) are sensitively and reproducibly generated under the LC-MS conditions. When [M+HCOO](-) is used as the precursor ion for SUC detection, the sensitivity increases approximately 20-fold compared to when [M-H](-) is the precursor ion. To further improve the limit of detection (LOD), we integrated the large volume injection approach (500μL injection) with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), which reduced the method detection limit (MDL) to 0.2ng/L for ACE and 5ng/L for SUC. To demonstrate the applicability of this method, we analyzed 100 well water samples collected in Alberta. ACE was detected in 24 wells at concentrations of 1-1534ng/L and SUC in 8 wells at concentrations of 65-541ng/L. These results suggest that wastewater is the most likely source of ACE and SUC impacts in these wells, suggesting the need for monitoring the quality of domestic well water. Copyright © 2014 Elsevier B.V. All rights reserved.

Field ion spectrometry: a new technology for cocaine and heroin detection

NASA Astrophysics Data System (ADS)

Carnahan, Byron L.; Day, Stephen; Kouznetsov, Viktor; Tarassov, Alexandre

1997-02-01

Field ion spectrometry, also known as transverse field compensation ion mobility spectrometry, is a new technique for trace gas analysis that can be applied to the detection of cocaine and heroin. Its principle is based on filtering ion species according to the functional dependence of their mobilities with electric field strength. Field ion spectrometry eliminates the gating electrodes needed in conventional IMS to pulse ions into the spectrometer; instead, ions are injected in to the spectrometer and reach the detector continuously, resulting in improved sensitivity. The technique enables analyses that are difficult with conventional constant field strength ion mobility spectrometers. We have shown that a filed ion spectrometer can selectively detect the vapors from cocaine and heroin emitted from both their base and hydrochloride forms. The estimated volumetric limits of detection are in the low pptv range, based on testing with standardized drug vapor generation systems. The spectrometer can detect cocaine base in the vapor phase, at concentrations well below its estimated 100 pptv vapor pressure equivalent at 20 degrees C. This paper describes the underlying principles of field ion spectrometry in relation to narcotic drug detection, and recent results obtained for cocaine and heroin. The work has been sponsored in part by the United States Advanced Research Projects Agency under contract DAAB10-95C-0004, for the DOD Counterdrug Technology Development Program.

A Sensitivity Enhanced MWCNT/PDMS Tactile Sensor Using Micropillars and Low Energy Ar⁺ Ion Beam Treatment.

PubMed

Azkar Ul Hasan, Syed; Jung, Youngdo; Kim, Seonggi; Jung, Cho-Long; Oh, Sunjong; Kim, Junhee; Lim, Hyuneui

2016-01-12

High sensitive flexible and wearable devices which can detect delicate touches have attracted considerable attentions from researchers for various promising applications. This research was aimed at enhancing the sensitivity of a MWCNT/PDMS piezoresistive tactile sensor through modification of its surface texture in the form of micropillars on MWCNT/PDMS film and subsequent low energy Ar⁺ ion beam treatment of the micropillars. The introduction of straight micropillars on the MWCNT/PDMS surface increased the sensitivity under gentle touch. Low energy ion beam treatment was performed to induce a stiff layer on the exposed surface of the micropillar structured MWCNT/PDMS film. The low energy ion bombardment stabilized the electrical properties of the MWCNT/PDMS surface and tuned the curvature of micropillars according to the treatment conditions. The straight micropillars which were treated by Ar⁺ ion with an incident angle of 0° demonstrated the enhanced sensitivity under normal pressure and the curved micropillars which were treated with Ar⁺ ion with an incident angle of 60° differentiated the direction of an applied shear pressure. The ion beam treatment on micropillar structured MWCNT/PDMS tactile sensors can thus be applied to reliable sensing under gentle touch with directional discrimination.

Radiation microscope for SEE testing using GeV ions.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Doyle, Barney Lee; Knapp, James Arthur; Rossi, Paolo

2009-09-01

Radiation Effects Microscopy is an extremely useful technique in failure analysis of electronic parts used in radiation environment. It also provides much needed support for development of radiation hard components used in spacecraft and nuclear weapons. As the IC manufacturing technology progresses, more and more overlayers are used; therefore, the sensitive region of the part is getting farther and farther from the surface. The thickness of these overlayers is so large today that the traditional microbeams, which are used for REM are unable to reach the sensitive regions. As a result, higher ion beam energies have to be used (>more » GeV), which are available only at cyclotrons. Since it is extremely complicated to focus these GeV ion beams, a new method has to be developed to perform REM at cyclotrons. We developed a new technique, Ion Photon Emission Microscopy, where instead of focusing the ion beam we use secondary photons emitted from a fluorescence layer on top of the devices being tested to determine the position of the ion hit. By recording this position information in coincidence with an SEE signal we will be able to indentify radiation sensitive regions of modern electronic parts, which will increase the efficiency of radiation hard circuits.« less

Single-ion quantum lock-in amplifier.

PubMed

Kotler, Shlomi; Akerman, Nitzan; Glickman, Yinnon; Keselman, Anna; Ozeri, Roee

2011-05-05

Quantum metrology uses tools from quantum information science to improve measurement signal-to-noise ratios. The challenge is to increase sensitivity while reducing susceptibility to noise, tasks that are often in conflict. Lock-in measurement is a detection scheme designed to overcome this difficulty by spectrally separating signal from noise. Here we report on the implementation of a quantum analogue to the classical lock-in amplifier. All the lock-in operations--modulation, detection and mixing--are performed through the application of non-commuting quantum operators to the electronic spin state of a single, trapped Sr(+) ion. We significantly increase its sensitivity to external fields while extending phase coherence by three orders of magnitude, to more than one second. Using this technique, we measure frequency shifts with a sensitivity of 0.42 Hz Hz(-1/2) (corresponding to a magnetic field measurement sensitivity of 15 pT Hz(-1/2)), obtaining an uncertainty of less than 10 mHz (350 fT) after 3,720 seconds of averaging. These sensitivities are limited by quantum projection noise and improve on other single-spin probe technologies by two orders of magnitude. Our reported sensitivity is sufficient for the measurement of parity non-conservation, as well as the detection of the magnetic field of a single electronic spin one micrometre from an ion detector with nanometre resolution. As a first application, we perform light shift spectroscopy of a narrow optical quadrupole transition. Finally, we emphasize that the quantum lock-in technique is generic and can potentially enhance the sensitivity of any quantum sensor. ©2011 Macmillan Publishers Limited. All rights reserved

Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

PubMed

Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

2009-05-15

A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were <11.2%. Aflatoxins were detected at <10 ng/g in several commercial food samples.

Magnetic separation of heavy metal ions and evaluation based on surface-enhanced Raman spectroscopy: copper(II) ions as a case study.

PubMed

Yan, Xue; Zhang, Xue-Jiao; Yuan, Ya-Xian; Han, San-Yang; Xu, Min-Min; Gu, Ren'ao; Yao, Jian-Lin

2013-11-01

A new approach was developed for the magnetic separation of copper(II) ions with easy operation and high efficiency. p-Mercaptobenzoic acid served as the modified tag of Fe2O3@Au nanoparticles both for the chelation ligand and Raman reporter. Through the chelation between the copper(II) ions and carboxyl groups on the gold shell, the Fe2O3@Au nanoparticles aggregated to form networks that were enriched and separated from the solution by a magnet. A significant decrease in the concentration of copper(II) ions in the supernatant solution was observed. An extremely sensitive method based on surface-enhanced Raman spectroscopy was employed to detect free copper(II) ions that remained after the magnetic separation, and thus to evaluate the separation efficiency. The results indicated the intensities of the surface-enhanced Raman spectroscopy bands from p-mercaptobenzoic acid were dependent on the concentration of copper(II) ions, and the concentration was decreased by several orders of magnitude after the magnetic separation. The present protocol effectively decreased the total amount of heavy metal ions in the solution. This approach opens a potential application in the magnetic separation and highly sensitive detection of heavy metal ions. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Study for online range monitoring with the interaction vertex imaging method.

PubMed

Finck, Ch; Karakaya, Y; Reithinger, V; Rescigno, R; Baudot, J; Constanzo, J; Juliani, D; Krimmer, J; Rinaldi, I; Rousseau, M; Testa, E; Vanstalle, M; Ray, C

2017-11-21

Ion beam therapy enables a highly accurate dose conformation delivery to the tumor due to the finite range of charged ions in matter (i.e. Bragg peak (BP)). Consequently, the dose profile is very sensitive to patients anatomical changes as well as minor mispositioning, and so it requires improved dose control techniques. Proton interaction vertex imaging (IVI) could offer an online range control in carbon ion therapy. In this paper, a statistical method was used to study the sensitivity of the IVI technique on experimental data obtained from the Heidelberg Ion-Beam Therapy Center. The vertices of secondary protons were reconstructed with pixelized silicon detectors. The statistical study used the [Formula: see text] test of the reconstructed vertex distributions for a given displacement of the BP position as a function of the impinging carbon ions. Different phantom configurations were used with or without bone equivalent tissue and air inserts. The inflection points in the fall-off region of the longitudinal vertex distribution were computed using different methods, while the relation with the BP position was established. In the present setup, the resolution of the BP position was about 4-5 mm in the homogeneous phantom under clinical conditions (10 6 incident carbon ions). Our results show that the IVI method could therefore monitor the BP position with a promising resolution in clinical conditions.

Study for online range monitoring with the interaction vertex imaging method

NASA Astrophysics Data System (ADS)

Finck, Ch; Karakaya, Y.; Reithinger, V.; Rescigno, R.; Baudot, J.; Constanzo, J.; Juliani, D.; Krimmer, J.; Rinaldi, I.; Rousseau, M.; Testa, E.; Vanstalle, M.; Ray, C.

2017-12-01

Ion beam therapy enables a highly accurate dose conformation delivery to the tumor due to the finite range of charged ions in matter (i.e. Bragg peak (BP)). Consequently, the dose profile is very sensitive to patients anatomical changes as well as minor mispositioning, and so it requires improved dose control techniques. Proton interaction vertex imaging (IVI) could offer an online range control in carbon ion therapy. In this paper, a statistical method was used to study the sensitivity of the IVI technique on experimental data obtained from the Heidelberg Ion-Beam Therapy Center. The vertices of secondary protons were reconstructed with pixelized silicon detectors. The statistical study used the χ2 test of the reconstructed vertex distributions for a given displacement of the BP position as a function of the impinging carbon ions. Different phantom configurations were used with or without bone equivalent tissue and air inserts. The inflection points in the fall-off region of the longitudinal vertex distribution were computed using different methods, while the relation with the BP position was established. In the present setup, the resolution of the BP position was about 4-5 mm in the homogeneous phantom under clinical conditions (106 incident carbon ions). Our results show that the IVI method could therefore monitor the BP position with a promising resolution in clinical conditions.

Exploring Molecular Complexity of the Diffuse and Translucent Gas and PhotoDissociation Regions

NASA Astrophysics Data System (ADS)

McCarthy, Michael

This proposal requests funds to continue a laboratory program in close coordination with radio astronomical observations dedicated to the study of highly reactive polyatomic molecular ions in low density regions and photo-dissociation regions (PDRs). In doing so, the proposed studies will advance our understanding of the chemistry beyond light ions that have been observed so successfully in these regions with Herschel and recently extended with SOFIA, and thereby critically address a significant but unresolved question in molecular astronomy: Are larger molecules formed in a bottom-up or top-down chemistry? The rotational spectra of most new molecular ions will be detected in the laboratory in a resonant microwave cavity, followed either by microwave/millimeterwave double resonance or millimeter/THz absorption to better characterize their spectrum in bands covered by the heterodyne receivers HIFI on Herschel and GREAT on SOFIA. In collaboration with radioastronomer colleagues, we will search for the new ions in the published survey of the PDR region of the Orion Bar and archival data of other PDRs observed with the IRAM 30 m telescope; retrieve and analyze archival data from Herschel; and undertake searches for some of the new ions in PDRs and low density regions with SOFIA. This work will also have a strong bearing on proposed Early Release Science (ERS) observations of dense PDRs with the James Webb Space Telescope (JWST). The laboratory effort will build on previous work on molecular ions , specifically detection of the rotational spectra of a number of positive ions of astronomical interest such as H2NCO+, CCCH+, the cis- and trans isomers of HOSO+, HNCOH+, and H2CC(H)CNH+. We will focus our efforts on positive ions derived from closed-shell neutral molecules, radicals, and carbenes whose rotational spectra have been observed in our laboratory, and nearly all of which have also been identified in galactic molecular clouds. Examples of the ions we seek include polyatomic ions such as CN+, HCCCN+, HNCO+, c-C3H2+, etc. Collaborations with leading theoretical groups to accurately predict spectroscopic constants of the new ions will enhance the proposed laboratory investigations. Instrumental refinement will also be undertaken with particular emphasis on construction of a new cryogenically cooled ( 6 K) buffer gas cell. This ultra-sensitive instrument will possess a system temperature that is nearly 50 times lower than our most sensitive cavity spectrometer, and one close to the fundamental limit set by modern technology, thereby greatly enhancing our ability to detect elusive molecular ions that are produced in very low steady state concentrations. The essential capabilities of this instrument have already been demonstrated in collaborative investigations. Our laboratory program is well aligned with NASA's overall mission, because we seek to understand the role of the chemical bond on a cosmic scale and to provide a firm chemical foundation by which more complicated questions of biological origins can be addressed. The work here also provides much basic information to aid subsequent astronomical searches, particularly in the infrared. Finally, our research program is an excellent vehicle for integrating research and education. It provides exposure to quite diverse areas of science in a setting which encourages student initiative and independent investigation.

Ion-Sensitive Field-Effect Transistor for Biological Sensing

PubMed Central

Lee, Chang-Soo; Kim, Sang Kyu; Kim, Moonil

2009-01-01

In recent years there has been great progress in applying FET-type biosensors for highly sensitive biological detection. Among them, the ISFET (ion-sensitive field-effect transistor) is one of the most intriguing approaches in electrical biosensing technology. Here, we review some of the main advances in this field over the past few years, explore its application prospects, and discuss the main issues, approaches, and challenges, with the aim of stimulating a broader interest in developing ISFET-based biosensors and extending their applications for reliable and sensitive analysis of various biomolecules such as DNA, proteins, enzymes, and cells. PMID:22423205

Barium Tagging n Solid Xenon for nEXO Neutrinoless Double Beta Decay

NASA Astrophysics Data System (ADS)

Walton, Tim; Chambers, Chris; Craycraft, Adam; Fairbank, William; nEXO Collaboration

2015-04-01

nEXO is a next-generation experiment designed to search for neutrinoless double beta decay of the isotope Xe136 in a liquid xenon time projection chamber. Positive observation of this decay would determine the nature of the neutrino to be a Majorana particle. Since the daughter of this decay is barium (Ba136), detecting the presence of Ba136 at a decay site (called ``barium tagging'') would provide strong rejection of backgrounds in the search for this decay. This would involve detecting a single barium ion from within a macroscopic volume of liquid xenon. This technique may be available for a second phase of the nEXO detector and sensitivity beyond the inverted hierarchy to neutrino oscillations. Several methods of barium tagging are being explored by the nEXO collaboration, but here we present a method of trapping the barium ion/atom (it may neutralize) in solid xenon (SXe) at the end of a cold probe, and then detecting the ion/atom by its fluorescence in the SXe. Our group at CSU has been studying the fluorescence of Ba in SXe by laser excitation, in order to ultimately detect a single Ba +/Ba in a SXe sample. We present studies of fluorescence signals, as well as recent results on imaging small numbers of Ba atoms in SXe, in a focused laser region. This work is supported by grants from the National Science Foundation and the Department of Energy.

Colorimetric detection of trace copper ions based on catalytic leaching of silver-coated gold nanoparticles.

PubMed

Lou, Tingting; Chen, Lingxin; Chen, Zhaopeng; Wang, Yunqing; Chen, Ling; Li, Jinhua

2011-11-01

A colorimetric, label-free, and nonaggregation-based silver coated gold nanoparticles (Ag/Au NPs) probe has been developed for detection of trace Cu(2+) in aqueous solution, based on the fact that Cu(2+) can accelerate the leaching rate of Ag/Au NPs by thiosulfate (S(2)O(3)(2-)). The leaching of Ag/Au NPs would lead to dramatic decrease in the surface plasmon resonance (SPR) absorption as the size of Ag/Au NPs decreased. This colorimetric strategy based on size-dependence of nanoparticles during their leaching process provided a highly sensitive (1.0 nM) and selective detection toward Cu(2+), with a wide linear detection range (5-800 nM) over nearly 3 orders of magnitude. The cost-effective probe allows rapid and sensitive detection of trace Cu(2+) ions in water samples, indicating its potential applicability for the determination of copper in real samples.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Markovic, M; Stathakis, S; Jurkovic, I

Purpose The aim for the study was to compare intrinsic characteristics of the nine detectors and evaluate their performance in non-equilibrium radiation dosimetry. Methods The intrinsic characteristics of the nine detectors that were evaluated are based on the composition and size of the active volume, operating voltage, initial recombination of the collected charge, temperature, the effective cross section of the detectors. The shortterm stability and collection efficiency has been investigated. The minimum radiation detection sensitivity and detectors leakage current has been measured. The sensitivity to changes in energy spectrum as well as change in incident beam angles were measured anmore » analyzed. Results The short-term stability of the measurements within every detector showed consistency in the measured values with the highest value of the standard deviation of the mean not exceeding 0.5%. Air ion chamber detectors showed minimum sensitivity to change in incident beam angles while diode detectors underestimated measurements up to 16%. Comparing the slope of the tangents for detector’s sensitivity curve, diode detectors illustrate more sensitivity to change in photon spectrum than ion chamber detectors. The change in radiation detection sensitivity with increase in dose delivered has been observed for semiconductor detectors with maximum deviation 0.01% for doses between 1 Gy and 10 Gy. Leakage current has been mainly influenced by bias voltage (ion chamber detectors) and room light intensity (diode detectors). With dose per pulse varying from 1.47E−4 to 5.1E−4 Gy/pulse the maximum change in collection efficiency was 1.4% for the air ion chambers up to 8% for liquid filled ion chamber. Conclusion Broad range of measurements performed showed all the detectors susceptible to some limitations and while they are suitable for use in broad scope of applications, careful selection has to be made for particular range of measurements.« less

Advances in ultrasensitive mass spectrometry of organic molecules.

PubMed

Kandiah, Mathivathani; Urban, Pawel L

2013-06-21

Ultrasensitive mass spectrometric analysis of organic molecules is important for various branches of chemistry, and other fields including physics, earth and environmental sciences, archaeology, biomedicine, and materials science. It finds applications--as an enabling tool--in systems biology, biological imaging, clinical analysis, and forensics. Although there are a number of technical obstacles associated with the analysis of samples by mass spectrometry at ultratrace level (for example analyte losses during sample preparation, insufficient sensitivity, ion suppression), several noteworthy developments have been made over the years. They include: sensitive ion sources, loss-free interfaces, ion optics components, efficient mass analyzers and detectors, as well as "smart" sample preparation strategies. Some of the mass spectrometric methods published to date can achieve sensitivity which is by several orders of magnitude higher than that of alternative approaches. Femto- and attomole level limits of detection are nowadays common, while zepto- and yoctomole level limits of detection have also been reported. We envision that the ultrasensitive mass spectrometric assays will soon contribute to new discoveries in bioscience and other areas.

Simultaneous determination of eight major steroids from Polyporus umbellatus by high-performance liquid chromatography coupled with mass spectrometry detections.

PubMed

Zhao, Ying-yong; Cheng, Xian-long; Zhang, Yongmin; Zhao, Ye; Lin, Rui-chao; Sun, Wen-ji

2010-02-01

Polyporus umbellatus is a widely used diuretic herbal medicine. In this study, a high-performance liquid chromatography coupled with atmospheric pressure chemical ionization-mass spectrometric detection (HPLC-APCI-MS) method was developed for qualitative and quantitative analysis of steroids, as well as for the quality control of Polyporus umbellatus. The selectivity, reproducibility and sensitivity were compared with HPLC with photodiode array detection and evaporative light scattering detection (ELSD). Selective ion monitoring in positive mode was used for qualitative and quantitative analysis of eight major components and beta-ecdysterone was used as the internal standard. Limits of detection and quantification fell in the ranges 7-21 and 18-63 ng/mL for the eight analytes with an injection of 10 microL samples, and all calibration curves showed good linear regression (r(2) > 0.9919) within the test range. The quantitative results demonstrated that samples from different localities showed different qualities. Advantages, in comparison with conventional HPLC-diode array detection and HPLC-ELSD, are that reliable identification of target compounds could be achieved by accurate mass measurements along with characteristic retention time, and the great enhancement in selectivity and sensitivity allows identification and quantification of low levels of constituents in complex Polyporus umbellatus matrixes. (c) 2009 John Wiley & Sons, Ltd.

Analysis of model Titan atmospheric components using ion mobility spectrometry

NASA Technical Reports Server (NTRS)

Kojiro, D. R.; Cohen, M. J.; Wernlund, R. F.; Stimac, R. M.; Humphry, D. E.; Takeuchi, N.

1991-01-01

The Gas Chromatograph-Ion Mobility Spectrometer (GC-IMS) was proposed as an analytical technique for the analysis of Titan's atmosphere during the Cassini Mission. The IMS is an atmospheric pressure, chemical detector that produces an identifying spectrum of each chemical species measured. When the IMS is combined with a GC as a GC-IMS, the GC is used to separate the sample into its individual components, or perhaps small groups of components. The IMS is then used to detect, quantify, and identify each sample component. Conventional IMS detection and identification of sample components depends upon a source of energetic radiation, such as beta radiation, which ionizes the atmospheric pressure host gas. This primary ionization initiates a sequence of ion-molecule reactions leading to the formation of sufficiently energetic positive or negative ions, which in turn ionize most constituents in the sample. In conventional IMS, this reaction sequence is dominated by the water cluster ion. However, many of the light hydrocarbons expected in Titan's atmosphere cannot be analyzed by IMS using this mechanism at the concentrations expected. Research at NASA Ames and PCP Inc., has demonstrated IMS analysis of expected Titan atmospheric components, including saturated aliphatic hydrocarbons, using two alternate sample ionizations mechanisms. The sensitivity of the IMS to hydrocarbons such as propane and butane was increased by several orders of magnitude. Both ultra dry (waterless) IMS sample ionization and metastable ionization were successfully used to analyze a model Titan atmospheric gas mixture.

Potassium permanganate-glutaraldehyde chemiluminescence system catalyzed by gold nanoprisms toward selective determination of fluoride.

PubMed

Abolhasani, Jafar; Hassanzadeh, Javad; Ghorbani-Kalhor, Ebrahim

2016-02-01

Gold and silver nanoparticles (NPs) are shown to exert a positive effect on the chemiluminescence (CL) reaction of permanganate aldehydes. Interestingly, between various shapes examined, Au nanoprisms have the highest beneficial effect. This effect is even more notable in the presence of sodium dodecyl sulfate (SDS) surfactant. UV-vis spectra and transmission electron microscopy were used to characterize the NP shapes and sizes. Furthermore, it was observed that iron(III) ions can slightly increase CL emission of this system. This intensification is very effective in the presence of fluoride ions (F(-)). These observations form the basis of the method for the high sensitive determination of F(-) in the 6-1200 nmol L(-1) concentration range, with a detection limit of 2.1 nmol L(-1). The proposed method has good precision and was satisfactorily used in the selective determination of low concentrations of fluoride ion in real samples. Copyright © 2015 John Wiley & Sons, Ltd.

Ultrasensitive and highly selective detection of Cu2 + ions based on a new carbazole-Schiff

NASA Astrophysics Data System (ADS)

Yin, Jun; Bing, Qijing; Wang, Lin; Wang, Guang

2018-01-01

A new chemosensor for Cu2 + based on Schiff base with high sensitivity and selectivity was designed and synthesized. The fluorescence intensity of the chemosensor in CH3CN solution was enhanced 160-fold after the addition of 10 equiv. Cu2 + over other metal ions. In addition, it also facilitates colorimetric detection for Cu2 + in CH3CN solution. The chemosensor displayed low detection limit and fast response time to Cu2 +.

Ion spectrometric detection technologies for ultra-traces of explosives: a review.

PubMed

Mäkinen, Marko; Nousiainen, Marjaana; Sillanpää, Mika

2011-01-01

In recent years, explosive materials have been widely employed for various military applications and civilian conflicts; their use for hostile purposes has increased considerably. The detection of different kind of explosive agents has become crucially important for protection of human lives, infrastructures, and properties. Moreover, both the environmental aspects such as the risk of soil and water contamination and health risks related to the release of explosive particles need to be taken into account. For these reasons, there is a growing need to develop analyzing methods which are faster and more sensitive for detecting explosives. The detection techniques of the explosive materials should ideally serve fast real-time analysis in high accuracy and resolution from a minimal quantity of explosive without involving complicated sample preparation. The performance of the in-field analysis of extremely hazardous material has to be user-friendly and safe for operators. The two closely related ion spectrometric methods used in explosive analyses include mass spectrometry (MS) and ion mobility spectrometry (IMS). The four requirements-speed, selectivity, sensitivity, and sampling-are fulfilled with both of these methods. Copyright © 2011 Wiley Periodicals, Inc.

A Simple, Cost-Effective Sensor for Detecting Lead Ions in Water Using Under-Potential Deposited Bismuth Sub-Layer with Differential Pulse Voltammetry (DPV)

PubMed Central

Dai, Yifan; Liu, Chung Chiun

2017-01-01

This research has developed a simple to use, cost effective sensor system for the detection of lead ions in tap water. An under-potential deposited bismuth sub-layer on a thin gold film based electrochemical sensor was designed, manufactured, and evaluated. Differential pulse voltammetry (DPV) measurement technique was employed in this detection. Tap water from the Cleveland, OH, USA regional water district was the test medium. Concentrations of lead ion in the range of 8 × 10−7 M to 5 × 10−4 M were evaluated, showing a good sensitivity over this concentration range. The calibration curve for the DPV measurements of lead ions in tap water showed excellent reproducibility with R2 value of 0.970. This DPV detection system required 3–6 min to complete the detection measurement. A longer measurement time of 6 min was used for the lower lead ion concentration. The selectivity of this lead ion sensor was very good, and Fe III, Cu II, Ni II, and Mg II at a concentration level of 5 × 10−4 M did not interfere with the lead ion measurement. PMID:28441356

UPLC-MS/MS determination of ephedrine, methylephedrine, amygdalin and glycyrrhizic acid in Beagle plasma and its application to a pharmacokinetic study after oral administration of Ma Huang Tang.

PubMed

Yan, Tianhua; Fu, Qiang; Wang, Jing; Ma, Shiping

2015-02-01

An ultra performance liquid chromatography-mass spectrometric (UPLC-MS) method was developed to investigate the pharmacokinetic properties of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid after oral gavage of Ma Huang Tang (MHT) in Beagles. Beagle plasma samples were pretreated using liquid-liquid extraction, and chromatographic separation was performed on a C18 column using a linear gradient of water-formic acid mixture (0.1%). The pharmacokinetic parameters of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid from MHT in Beagles were quantitatively determined by UPLC with tandem mass detector. The qualitative detection of the four compounds was accomplished by selected ion monitoring in negative/positive ion modes electrospray ionization-mass spectrometry (ESI-MS). Detection was based on multiple reaction monitoring with the precursor-to-product ion transitions m/z 166.096-116.983 (ephedrine), m/z 179.034-146.087 (methylephedrine), m/z 456.351-323.074 (amygdalin), and m/z 821.606-351.062 (glycyrrhizic acid). The selectivity, sensitivity, linearity, accuracy, precision, extraction recovery, ion suppression, and stability were within the acceptable ranges. The method described was successfully applied to reveal the pharmacokinetic properties of ephedrine, methylephedrine, amygdalin, and glycyrrhizic acid after oral gavage of MHT in Beagles. Copyright © 2014 John Wiley & Sons, Ltd.

Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

USGS Publications Warehouse

Ferrer, I.; Furlong, E.T.

2002-01-01

Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

Low picomolar, instrument-free visual detection of mercury and silver ions using low-cost programmable nanoprobes

PubMed Central

Rana, Muhit; Balcioglu, Mustafa; Robertson, Neil M.; Hizir, Mustafa Salih; Yumak, Sumeyra

2017-01-01

The EPA's recommended maximum allowable level of inorganic mercury in drinking water is 2 ppb (10 nM). To our knowledge, the most sensitive colorimetric mercury sensor reported to date has a limit of detection (LOD) of 800 pM. Here, we report an instrument-free and highly practical colorimetric methodology, which enables detection of as low as 2 ppt (10 pM) of mercury and/or silver ions with the naked eye using a gold nanoprobe. Synthesis of the nanoprobe costs less than $1.42, which is enough to perform 200 tests in a microplate; less than a penny for each test. We have demonstrated the detection of inorganic mercury from water, soil and urine samples. The assay takes about four hours and the color change is observed within minutes after the addition of the last required element of the assay. The nanoprobe is highly programmable which allows for the detection of mercury and/or silver ions separately or simultaneously by changing only a single parameter of the assay. This highly sensitive approach for the visual detection relies on the combination of the signal amplification features of the hybridization chain reaction with the plasmonic properties of the gold nanoparticles. Considering that heavy metal ion contamination of natural resources is a major challenge and routine environmental monitoring is needed, yet time-consuming, this colorimetric approach may be instrumental for on-site heavy metal ion detection. Since the color transition can be measured in a variety of formats including using the naked eye, a simple UV-Vis spectrophotometer, or recording using mobile phone apps for future directions, our cost-efficient assay and method have the potential to be translated into the field. PMID:28451261

Studying ion exchange in solution and at biological membranes by FCS.

PubMed

Widengren, Jerker

2013-01-01

By FCS, a wide range of processes can be studied, covering time ranges from subnanoseconds to seconds. In principle, any process at equilibrium conditions can be measured, which reflects itself by a change in the detected fluorescence intensity. In this review, it is described how FCS and variants thereof can be used to monitor ion exchange, in solution and along biological membranes. Analyzing fluorescence fluctuations of ion-sensitive fluorophores by FCS offers selective advantages over other techniques for measuring local ion concentrations, and, in particular, for studying exchange kinetics of ions on a very local scale. This opens for several areas of application. The FCS approach was used to investigate fundamental aspects of proton exchange at and along biological membranes. The protonation relaxation rate, as measured by FCS for a pH-sensitive dye, can also provide information about local accessibility/interaction of a particular labeling site and conformational states of biomolecules, in a similar fashion as in a fluorescence quenching experiment. The same FCS concept can also be applied to ion exchange studies using other ion-sensitive fluorophores, and by use of dyes sensitive to other ambient conditions the concept can be extended also beyond ion exchange studies. Copyright © 2013 Elsevier Inc. All rights reserved.

Morphological control of gold nanorods via thermally driven bi-surfactant growth and application for detection of heavy metal ions.

PubMed

Huang, Hao; Li, Huiyi; Wang, Huaiyu; Li, Jia; Li, Penghui; Chen, Qidan; Chen, Yue; Chu, Paul K; Li, Bo; Yu, Xuefeng

2018-05-22

We report a modified synthesis route of colloidal gold nanorods (AuNRs) by combining the thermal re-shaping treatment and bi-surfactant modification using hexadecyltrimethylammonium bromide (CTAB) and sodium oleate (NaOL). Aspect ratios down to 1.3 ± 0.1 can be achieved in addition to good monodispersity, uniformity, and chemical stability of the materials. Furthermore, without needing post-treatment, metal ions directly interact with the AuNRs efficiently, allowing rapid and sensitive colorimetric detection of heavy metal ions such as Pb²⁺ and Cu²⁺ with a low concentration down to 2.5 μM. The detection performance in terms of selectivity, sensitivity and stability is systematically evaluated. The AuNRs with tunable aspect ratios as well as chemical stability have potential in surface-plasmon-based applications such as biochemical sensing, biochemical imaging, medical diagnostics, and cancer therapy. © 2018 IOP Publishing Ltd.

Application of hybrid SiO2-coated CdTe nanocrystals for sensitive sensing of Cu2+ and Ag+ ions.

PubMed

Cao, Yongqiang; Zhang, Aiyu; Ma, Qian; Liu, Ning; Yang, Ping

2013-01-01

A new ion sensor based on hybrid SiO2 -coated CdTe nanocrystals (NCs) was prepared and applied for sensitive sensing of Cu(2+) and Ag(+) for the selective quenching of photoluminescence (PL) of NCs in the presence of ions. As shown by ion detection experiments conducted in pure water rather than buffer solution, PL responses of NCs were linearly proportional to concentrations of Cu(2+) and Ag(+) ions < 3 and 7 uM, respectively. Much lower detection limits of 42.37 nM for Cu(2+) and 39.40 nM for Ag(+) were also observed. In addition, the NC quenching mechanism was discussed in terms of the characterization of static and transient optical spectra. The transfer and trapping of photoinduced charges in NCs by surface energy levels of CuS and Ag2 S clusters as well as surface defects generated by the exchange of Cu(2+) and Ag(+) ions with Cd(2+) ion in NCs, resulted in PL quenching and other optical spectra changes, including steady-state absorption and transient PL spectra. It is our hope that these results will be helpful in the future preparation of new ion sensors. Copyright © 2012 John Wiley & Sons, Ltd.

Electro-thermal vaporization direct analysis in real time-mass spectrometry for water contaminant analysis during space missions.

PubMed

Dwivedi, Prabha; Gazda, Daniel B; Keelor, Joel D; Limero, Thomas F; Wallace, William T; Macatangay, Ariel V; Fernández, Facundo M

2013-10-15

The development of a direct analysis in real time-mass spectrometry (DART-MS) method and first prototype vaporizer for the detection of low molecular weight (∼30-100 Da) contaminants representative of those detected in water samples from the International Space Station is reported. A temperature-programmable, electro-thermal vaporizer (ETV) was designed, constructed, and evaluated as a sampling interface for DART-MS. The ETV facilitates analysis of water samples with minimum user intervention while maximizing analytical sensitivity and sample throughput. The integrated DART-ETV-MS methodology was evaluated in both positive and negative ion modes to (1) determine experimental conditions suitable for coupling DART with ETV as a sample inlet and ionization platform for time-of-flight MS, (2) to identify analyte response ions, (3) to determine the detection limit and dynamic range for target analyte measurement, and (4) to determine the reproducibility of measurements made with the method when using manual sample introduction into the vaporizer. Nitrogen was used as the DART working gas, and the target analytes chosen for the study were ethyl acetate, acetone, acetaldehyde, ethanol, ethylene glycol, dimethylsilanediol, formaldehyde, isopropanol, methanol, methylethyl ketone, methylsulfone, propylene glycol, and trimethylsilanol.

Simultaneous determination of cadmium, lead and mercury ions at trace level by magnetic solid phase extraction with Fe@Ag@Dimercaptobenzene coupled to high performance liquid chromatography.

PubMed

Zhou, Qingxiang; Lei, Man; Liu, Yongli; Wu, Yalin; Yuan, Yongyong

2017-12-01

Pollution resulted from heavy metal ions have absorbed much attention, and it is of great importance to develop sensitive and simultaneous determination method for them with common technologies without highly sensitive instruments. We prepared a new and functional core-shell magnetic nano-material, Fe@Ag@dimercaptobenzene (Fe@Ag@DMB), by a one-step method with sodium borohydride as the reducing agent and transmission electron microscopy (TEM) and energy dispersive spectrometer (EDS) were used for characterisation. The mercapto functional groups on the newly synthesised magnetic nanoparticles could interact with Cd 2+ , Pb 2+ , and Hg 2+ ions in water samples and then efficient extraction for Cd 2+ , Pb 2+ , and Hg 2+ ions was achieved. DDTC-Na solution was a good elutent for elution of these ions from Fe@Ag@DMB nanoparticles. Based on these, a sensitive method was developed for simultaneous preconcentration and determination of the aforementioned ions using magnetic Fe@Ag@DMB nanoparticles as the magnetic solid phase extraction adsorbent prior to high performance liquid chromatography coupled with variable wavelength detection. Under the optimal conditions, the detection limits of the three metal ions were in the range of 0.011-0.031μgL -1 , and precisions were below 2.37% (n=6). The proposed method was evaluated with real water samples, and excellent spiked recoveries achieved indicated that the developed method would be a promising tool for monitoring these heavy metal ions in water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Cavity-Enhanced Spectroscopy of Molecular Ions in the Mid-Infrared with Up-Conversion Detection and Brewster-Plate Spoilers

NASA Astrophysics Data System (ADS)

Markus, Charles R.; McCollum, Jefferson E.; Hodges, James Neil; Perry, Adam J.; McCall, Benjamin J.

2017-06-01

Molecular ions are challenging to study with conventional spectroscopic methods. Laboratory discharges produce ions in trace quantities which can be obscured by the abundant neutral molecules present. The technique Noise Immune Cavity Enhanced Optical Heterodyne Velocity Modulation Spectroscopy (NICE-OHVMS) overcomes these challenges by combining the ion-neutral discrimination of velocity modulation spectroscopy with the sensitivity of Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectroscopy (NICE-OHMS), and has been able to determine transition frequencies of molecular ions in the mid-infrared (mid-IR) with sub-MHz uncertainties when calibrated with an optical frequency comb. However, the extent of these studies was limited by the presence of fringes due to parasitic etalons and the speed and noise characteristics of mid-IR detectors. Recently, we have overcome these limitations by implementing up-conversion detection and dithered optics. We performed up-conversion using periodically poled lithium niobate to convert light from the mid-IR to the visible to be within the coverage of sensitive and fast silicon detectors while maintaining our heterodyne and velocity modulation signals. The parasitic etalons were removed by rapidly rotating CaF_2 windows with galvanometers, which is known as a Brewster-plate spoiler, which averaged out the fringes in detection. Together, these improved the sensitivity by more than an order of magnitude and have enabled extended spectroscopic surveys of molecular ions in the mid-IR. J. N. Hodges, A. J. Perry, P. A. Jenkins II, B. M. Siller, and B. J. McCall, J. Chem. Phys. (2013), 139, 164201. C. R. Webster, J. Opt. Soc. Am. B (1985), 2, 1464. C. R. Markus, A. J. Perry, J. N. Hodges, and B. J. McCall, Opt. Express (2017), 25, 3709-3721.

Highly sensitive and selective liquid crystal optical sensor for detection of ammonia.

PubMed

Niu, Xiaofang; Zhong, Yuanbo; Chen, Rui; Wang, Fei; Luo, Dan

2017-06-12

Ammonia detection technologies are very important in environment monitoring. However, most existing technologies are complex and expensive, which limit the useful range of real-time application. Here, we propose a highly sensitive and selective optical sensor for detection of ammonia (NH 3 ) based on liquid crystals (LCs). This optical sensor is realized through the competitive binding between ammonia and liquid crystals on chitosan-Cu 2+ that decorated on glass substrate. We achieve a broad detection range of ammonia from 50 ppm to 1250 ppm, with a low detection limit of 16.6 ppm. This sensor is low-cost, simple, fast, and highly sensitive and selective for detection of ammonia. The proposal LC sensing method can be a sensitive detection platform for other molecule monitors such as proteins, DNAs and other heavy metal ions by modifying sensing molecules.

Highly selective visual monitoring of hazardous fluoride ion in aqueous media using thiobarbituric-capped gold nanoparticles.

PubMed

Boken, Jyoti; Thatai, Sheenam; Khurana, Parul; Prasad, Surendra; Kumar, Dinesh

2015-01-01

The rapid, selective and sensitive measurement and monitoring of hazardous materials as analytes are the central themes in the development of any successful analytical technique. With this aim, we have synthesized the thiobarbituric-capped gold nanoparticles (TBA-capped Au NPs) involving chemical reduction of HAuCl4 using 2-thiobarbituric acid (TBA) as a reducing and capping agent. The morphology of the TBA-capped Au NPs was confirmed using transmission electron microscope images. For the first time this article reports that the developed TAB-capped Au NPs displays selective, ultrafast and sensitive colorimetric detection of fluoride ion in aqueous samples. The detection of fluoride ion was confirmed by the disappearance of the localized surface plasmon resonance (LSPR) band at 554 nm using UV-vis spectroscopy. The interaction of F(-) with TBA-capped Au NPs in aqueous solution has also been confirmed by Raman and FTIR spectroscopy. One of the most exciting accomplishments is the visual detection limit for fluoride ion has been found to be 10 mM at commonly acceptable water pH range 7-8. The whole detection procedure takes not more than 40s with excellent selectivity providing sample throughput of more than 60 per hour. Copyright © 2014 Elsevier B.V. All rights reserved.

Simultaneous Analysis of Monovalent Anions and Cations with a Sub-Microliter Dead-Volume Flow-Through Potentiometric Detector for Ion Chromatography

PubMed Central

Dumanli, Rukiye; Attar, Azade; Erci, Vildan; Isildak, Ibrahim

2016-01-01

A microliter dead-volume flow-through cell as a potentiometric detector is described in this article for sensitive, selective and simultaneous detection of common monovalent anions and cations in single column ion chromatography for the first time. The detection cell consisted of less selective anion- and cation-selective composite membrane electrodes together with a solid-state composite matrix reference electrode. The simultaneous separation and sensitive detection of sodium (Na+), potassium (K+), ammonium (NH4+), chloride (Cl−) and nitrate (NO3−) in a single run was achieved by using 98% 1.5 mM MgSO4 and 2% acetonitrile eluent with a mixed-bed ion-exchange separation column without suppressor column system. The separation and simultaneous detection of the anions and cations were completed in 6 min at the eluent flow-rate of 0.8 mL/min. Detection limits, at S/N = 3, were ranged from 0.2 to 1.0 µM for the anions and 0.3 to 3.0 µM for the cations, respectively. The developed method was successfully applied to the simultaneous determination of monovalent anions and cations in several environmental and biological samples. PMID:26786906

Colorimetric Detection of Mercury(II) Ion in Aqueous Solution Using Silver Nanoparticles.

PubMed

Firdaus, M Lutfi; Fitriani, Ikka; Wyantuti, Santhy; Hartati, Yeni W; Khaydarov, Renat; McAlister, Jason A; Obata, Hajime; Gamo, Toshitaka

2017-01-01

Novel green-chemistry synthesis of silver nanoparticles (AgNPs) is introduced as a low-cost, rapid and easy-to-use analytical method for mercury ion detection. Aqueous fruit extract of water apple (Syzygium aqueum) was used for the first time as bioreductant to synthesize stable AgNPs. The prepared AgNPs have a yellowish-brown color with a surface plasmon resonance peak at 420 nm. The addition of Hg(II) ions then changes the AgNPs color to colorless. The color change was in proportion to the concentration of Hg(II) ions. The presence of other metal ions in the system was also evaluated. The proposed method shows good selectivity and sensitivity towards Hg(II) ions. Using UV-visible spectrophotometry, the detection limit of the developed method was 8.5 × 10 -7 M. The proposed method has been successfully applied for determination of Hg(II) ions in tap and lake water samples with precision better than 5%.

Infrared laser dissociation of single megadalton polymer ions in a gated electrostatic ion trap: the added value of statistical analysis of individual events.

PubMed

Halim, Mohammad A; Clavier, Christian; Dagany, Xavier; Kerleroux, Michel; Dugourd, Philippe; Dunbar, Robert C; Antoine, Rodolphe

2018-05-07

In this study, we report the unimolecular dissociation mechanism of megadalton SO 3 -containing poly(2-acrylamido-2-methyl-1-propanesulfonic acid) (PAMPS) polymer cations and anions with the aid of infrared multiphoton dissociation coupled to charge detection ion trap mass spectrometry. A gated electrostatic ion trap ("Benner trap") is used to store and detect single gaseous polymer ions generated by positive and negative polarity in an electrospray ionization source. The trapped ions are then fragmented due to the sequential absorption of multiple infrared photons produced from a continuous-wave CO 2 laser. Several fragmentation pathways having distinct signatures are observed. Highly charged parent ions characteristically adopt a distinctive "stair-case" pattern (assigned to the "fission" process) whereas low charge species take on a "funnel like" shape (assigned to the "evaporation" process). Also, the log-log plot of the dissociation rate constants as a function of laser intensity between PAMPS positive and negative ions is significantly different.

Limits to Sensitivity in Laser Enhanced Ionization.

ERIC Educational Resources Information Center

Travis, J. C.

1982-01-01

Laser enhanced ionization (LEI) occurs when a tunable dye laser is used to excite a specific atomic population in a flame. Explores the origin of LEI's high sensitivity and identifies possible avenues to higher sensitivity by describing instrument used and experimental procedures and discussing ion formation/detection. (Author/JN)

Selective detection of Co2+ by fluorescent nano probe: Diagnostic approach for analysis of environmental samples and biological activities

NASA Astrophysics Data System (ADS)

Mahajan, Prasad G.; Dige, Nilam C.; Desai, Netaji K.; Patil, Shivajirao R.; Kondalkar, Vijay V.; Hong, Seong-Karp; Lee, Ki Hwan

2018-06-01

Nowadays scientist over the world are engaging to put forth improved methods to detect metal ion in an aqueous medium based on fluorescence studies. A simple, selective and sensitive method was proposed for detection of Co2+ ion using fluorescent organic nanoparticles. We synthesized a fluorescent small molecule viz. 4,4‧-{benzene-1,4-diylbis-[(Z)methylylidenenitrilo]}dibenzoic acid (BMBA) to explore its suitability as sensor for Co2+ ion and biocompatibility in form of nanoparticles. Fluorescence nanoparticles (BMBANPs) prepared by simple reprecipitation method. Aggregation induced enhanced emission of BMBANPs exhibits the narrower particle size of 68 nm and sphere shape morphology. The selective fluorescence quenching was observed by addition of Co2+ and does not affected by presence of other coexisting ion solutions. The photo-physical properties, viz. UV-absorption, fluorescence emission, and lifetime measurements are in support of ligand-metal interaction followed by static fluorescence quenching phenomenon in emission of BMBANPs. Finally, we develop a simple analytical method for selective and sensitive determination of Co2+ ion in environmental samples. The cell culture E. coli, Bacillus sps., and M. tuberculosis H37RV strain in the vicinity of BMBANPs indicates virtuous anti-bacterial and anti-tuberculosis activity which is of additional novel application shown by prepared nanoparticles.

Precise Determination of the Lyman-1 Transition Energy in Hydrogen-like Gold Ions with Microcalorimeters

NASA Astrophysics Data System (ADS)

Kraft-Bermuth, S.; Andrianov, V.; Bleile, A.; Echler, A.; Egelhof, P.; Grabitz, P.; Kilbourne, C.; Kiselev, O.; McCammon, D.; Scholz, P.

2014-09-01

The precise determination of the transition energy of the Lyman-1 line in hydrogen-like heavy ions provides a sensitive test of quantum electrodynamics in very strong Coulomb fields. We report the determination of the Lyman-1 transition energy of gold ions (Au) with microcalorimeters at the experimental storage ring at GSI. X-rays produced by the interaction of 125 MeV/u Au ions with an internal argon gas-jet target were detected. The detector array consisted of 14 pixels with silicon thermistors and Sn absorbers, for which an energy resolution of 50 eV for an X-ray energy of 59.5 keV was obtained in the laboratory. The Lyman-1 transition energy was determined for each pixel in the laboratory frame, then transformed into the emitter frame and averaged. A Dy-159 source was used for energy calibration. The absolute positions of the detector pixels, which are needed for an accurate correction of the Doppler shift, were determined by topographic measurements and by scanning a collimated Am-241 source across the cryostat window. The energy of the Lyman-1 line in the emitter frame is eV, in good agreement with theoretical predictions. The systematic error is dominated by the uncertainty in the position of the cryostat relative to the interaction region of beam and target.

Linker-assisted immunoassay and liquid chromatography/mass spectrometry for the analysis of glyphosate

USGS Publications Warehouse

Lee, E.A.; Zimmerman, L.R.; Bhullar, B.S.; Thurman, E.M.

2002-01-01

A novel, sensitive, linker-assisted enzyme-linked immunosorbent assay (L'ELISA) was compared to on-line solidphase extraction (SPE) with high-performance liquid chromatography/mass spectrometry (HPLC/MS) for the analysis of glyphosate in surface water and groundwater samples. The L'ELISA used succinic anhydride to derivatize glyphosate, which mimics the epitotic attachment of glyphosate to horseradish peroxidase hapten. Thus, L'ELISA recognized the derivatized glyphosate more effectively (detection limit of 0.1 μg/L) and with increased sensitivity (10-100 times) over conventional ELISA and showed the potential for other applications. The precision and accuracy of L'ELISA then was compared with on-line SPE/HPLC/MS, which detected glyphosate and its degradate derivatized with 9-fluorenylmethyl chloroformate using negative-ion electrospray (detection limit 0.1 μg/L, relative standard deviation ±15%). Derivatization efficiency and matrix effects were minimized by adding an isotope-labeled glyphosate (2-13C15N). The accuracy of L'ELISA gave a false positive rate of 18% between 0.1 and 1.0 μg/L and a false positive rate of only 1% above 1.0 μg/L. The relative standard deviation was ±20%. The correlation of L'ELISA and HPLC/MS for 66 surface water and groundwater samples was 0.97 with a slope of 1.28, with many detections of glyphosate and its degradate in surface water but not in groundwater.

Development of a cyclic voltammetry method for the detection of Clostridium novyi in black disease.

PubMed

Liu, L L; Jiang, D N; Xiang, G M; Liu, C; Yu, J C; Pu, X Y

2014-03-17

Black disease is an acute disease of sheep and cattle. The pathogen is the obligate anaerobe, Clostridium novyi. Due to difficulties of anaerobic culturing in the country or disaster sites, a simple, rapid, and sensitive method is required. In this study, an electrochemical method, the cyclic voltammetry method, basing on loop-mediated isothermal amplification (LAMP), electrochemical ion bonding (positive dye, methylene blue), was introduced. DNA extracted from C. novyi specimens was amplified through the LAMP reaction. Then the products combined were with methylene blue, which lead to a reduction in the oxidation peak current (ipA) and the reduction peak current (ipC) of the cyclic voltammetry. The changes of ipA/ipC were real-time measured by special designed electrode, so the DNA was quantitatively detected. The results displayed that this electrochemical detection of C. novyi could be completed in 1-2 h with the lowest bacterial concentration of 10(2) colony forming units/mL, and high accuracy (96.5%), sensitivity (96%), and specificity (97%) compared to polymerase chain reation. The cyclic voltammetry method was a simple and fast method, with high sensitivity and high specificity, and has great potential to be a usable molecular tool for fast diagnosis of Black disease.

The effect of pre-evaporation on ion distributions in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Liu, Shulan; Beauchemin, Diane

2006-02-01

The connecting tube (2 or 5-mm i. d., 11-cm long) between the spray chamber and the torch was heated (to 400 °C) to investigate the effect of pre-evaporation on the distribution of ions in inductively coupled plasma mass spectrometry (ICP-MS). Axial and radial profiles of analyte ions (Al +, V +, Cr +, Ni +, Zn +, Mn +, Zn +, As +, Se +, Mo +, Cd +, Sb +, La +, Pb +) in 1% HNO 3 as well as some polyatomic ions (LaO +, ArO +, ArN +, CO 2+) were simultaneously obtained on a time-of-flight ICP-MS instrument. Upon heating the connecting tube, the optimal axial position of all elements shifted closer to the load coil. Without the heated tube, 3.5 mm was the compromise axial position for multielemental analysis, which was optimal for 6 analytes. With the heated tube, this position became 1.5 mm, which was then optimal for 9 of the 14 analytes. Furthermore, the radial profiles, which were wide with a plateau in their middle without heating, became significantly narrower and Gaussian-like with a heated tube. This narrowing, which was most important for the 5-mm tube, slightly (by a factor of two at the most) yet significantly (at the 95% confidence level) improved the sensitivity of all elements but Mn upon optimisation of the axial position for compromise multi-element analysis. Furthermore, a concurrent decrease in the standard deviation of the blank was significant at the 95% confidence level for 9 of the 14 analytes. For most of the analytes, this translated into a two-fold to up to an order of magnitude improvement in detection limit, which is commensurate with a reduction of noise resulting from the smaller droplets entering the plasma after traversing the pre-evaporation tube.

Simultaneous and confirmative detection of multi-residues of β₂-agonists and β-blockers in urine using LC-MS/MS/MS coupled with β-receptor molecular imprinted polymer SPE clean-up.

PubMed

Fan, S; Zou, J H; Miao, H; Zhao, Y F; Chen, H J; Zhao, R; Wu, Y N

2013-01-01

A liquid chromatography-linear ion-trap spectrometry (LC-MS³) method using β-receptor molecular-imprinted polymer (MIP) solid-phase extraction (SPE) as clean-up was developed to determine simultaneously and confirmatively residues of 25 β₂-agonists and 21 β-blockers in urine samples. Urine samples were subjected to enzymatic hydrolysis by β-glucoronidase/arylsulphatase, and then extracted with perchloric acid. Sample clean-up was performed using β-receptor MIP SPE. A Supelco Ascentis® express Rp-Amide column was used to separate the analytes, and MS³ detection used an electrospray ionisation source in positive-ion mode. Recovery studies were carried out using blank urine samples fortified with the 46 analytes at the levels of 0.5, 1.0 and 2.0 μg l⁻¹. Recoveries were obtained ranging from 60.1% to 109.9% with relative standard deviations (RSDs, n = 7) from 0.5% to 19.4%. The limits of detection (LODs) and limits of quantitation (LOQs) of the 46 analytes in urine were 0.02-0.18 and 0.05-0.60 μg l⁻¹, respectively. As a result of the selective clean-up by MIP SPE and MS³ detection of the target drugs, the sensitivity and accuracy of the present method was high enough for monitoring β₂-agonist and β-blocker residues in urine samples. Satisfactory results were obtained in the process of the determination of positive urine samples.

Sensitive naked eye detection and quantification assay for nitrite by a fluorescence probe in various water resources.

PubMed

Zhang, Fengyuan; Zhu, Xinyue; Jiao, Zhijuan; Liu, Xiaoyan; Zhang, Haixia

2018-07-05

An uncontrolled increase of nitrite concentration in groundwater, rivers and lakes is a growing threat to public health and environment. It is important to monitor the nitrite levels in water and clinical diagnosis. Herein, we developed a switch-off fluorescence probe (PyI) for the sensitive detection of nitrite ions in the aqueous media. This probe selectively recognizes nitrite ions through a distinct visual color change from colorless to pink with a detection limit of 0.1 μM. This method has been successfully applied to the determination of nitrites in tap water, lake water and Yellow River water with recoveries in the range of 94.8%-105.4%. Copyright © 2018 Elsevier B.V. All rights reserved.

Ultrasensitive quantum dot fluorescence quenching assay for selective detection of mercury ions in drinking water.

PubMed

Ke, Jun; Li, Xinyong; Zhao, Qidong; Hou, Yang; Chen, Junhong

2014-07-09

Mercury is one of the most acutely toxic substances at trace level to human health and living thing. Developing a rapid, cheap and water soluble metal sensor for detecting mercury ions at ppb level remains a challenge. Herein, a metal sensor consisting of MPA coated Mn doped ZnSe/ZnS colloidal nanoparticles was utilized to ultrasensitively and selectively detect Hg(2+) ions with a low detection limit (0.1 nM) over a dynamic range from 0 to 20 nM. According to strong interaction between thiol(s) and mercury ions, mercaptopropionic acid (MPA) was used as a highly unique acceptor for mercury ions in the as-obtained ultrasensitive sensor. In the presence of mercury ions, colloidal nanoparticles rapidly agglomerated due to changes of surface chemical properties, which results in severe quenching of fluorescent intensity. Meanwhile, we find that the original ligands are separated from the surface of colloidal nanoparticles involving strongly chelation between mercury ion and thiol(s) proved by controlled IR analysis. The result shows that the QD-based metal ions sensor possesses satisfactory precision, high sensitivity and selectivity, and could be applied for the quantification analysis of real samples.

A novel and simple fluorescence probe for detecting main group magnesium ion in HeLa cells and Arabidopsis.

PubMed

Yu, Tingting; Sun, Ping; Hu, Yijie; Ji, Yinggang; Zhou, Hongping; Zhang, Baowei; Tian, Yupeng; Wu, Jieying

2016-12-15

A simple-molecule fluorescence probe L has been designed, synthesized and characterized, which shows high selectivity and sensitivity for the main group magnesium ion through fluorescence "turn-on" response in ethanol solution, and no interference from calcium ion in particular. Detection limit of probe L is 1.47×10(-6) M and the rapid response could reach about 15-20s. The recognition mechanism has been established by fluorescence spectra, (1)H NMR study. Moreover, probe L presents a great photostability, low toxicity and cellular permeability, then we have carried out fluorescent bio-imaging of the probe L for magnesium ions in HeLa cells, which showed that probe L could be utilized to detect the intracellular magnesium ion. Furthermore, it is successfully used as a magnesium ion developer in plant tissues, which shows that it not only can be well tracking the transport of magnesium ion but also make a corresponding fluorescence response to different concentrations magnesium ion. These results would make this probe a great potential application for detecting Mg(2+) in biological system. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultrasensitive Quantum Dot Fluorescence quenching Assay for Selective Detection of Mercury Ions in Drinking Water

PubMed Central

Ke, Jun; Li, Xinyong; Zhao, Qidong; Hou, Yang; Chen, Junhong

2014-01-01

Mercury is one of the most acutely toxic substances at trace level to human health and living thing. Developing a rapid, cheap and water soluble metal sensor for detecting mercury ions at ppb level remains a challenge. Herein, a metal sensor consisting of MPA coated Mn doped ZnSe/ZnS colloidal nanoparticles was utilized to ultrasensitively and selectively detect Hg2+ ions with a low detection limit (0.1 nM) over a dynamic range from 0 to 20 nM. According to strong interaction between thiol(s) and mercury ions, mercaptopropionic acid (MPA) was used as a highly unique acceptor for mercury ions in the as-obtained ultrasensitive sensor. In the presence of mercury ions, colloidal nanoparticles rapidly agglomerated due to changes of surface chemical properties, which results in severe quenching of fluorescent intensity. Meanwhile, we find that the original ligands are separated from the surface of colloidal nanoparticles involving strongly chelation between mercury ion and thiol(s) proved by controlled IR analysis. The result shows that the QD-based metal ions sensor possesses satisfactory precision, high sensitivity and selectivity, and could be applied for the quantification analysis of real samples. PMID:25005836

SRAM As An Array Of Energetic-Ion Detectors

NASA Technical Reports Server (NTRS)

Buehler, Martin G.; Blaes, Brent R.; Lieneweg, Udo; Nixon, Robert H.

1993-01-01

Static random-access memory (SRAM) designed for use as array of energetic-ion detectors. Exploits well-known tendency of incident energetic ions to cause bit flips in cells of electronic memories. Design of ion-detector SRAM involves modifications of standard SRAM design to increase sensitivity to ions. Device fabricated by use of conventional complementary metal oxide/semiconductor (CMOS) processes. Potential uses include gas densimetry, position sensing, and measurement of cosmic-ray spectrum.

Photosensitivity enhancement of PLZT ceramics by positive ion implantation

DOEpatents

Land, Cecil E.; Peercy, Paul S.

1983-01-01

The photosensitivity of lead lanthanum zirconate titanate (PLZT) ceramic material used in high resolution, high contrast, and non-volatile photoferroelectric image storage and display devices is enhanced significantly by positive ion implantation of the PLZT near its surface. Implanted ions include H.sup.+, He.sup.+, Ne.sup.+, Ar.sup.+, as well as chemically reactive ions from Fe, Cr, and Al. The positive ion implantation advantageously serves to shift the absorption characteristics of the PLZT material from near-UV light to visible light. As a result, photosensitivity enhancement is such that the positive ion implanted PLZT plate is sensitive even to sunlight and conventional room lighting, such as fluorescent and incandescent light sources. The method disclosed includes exposing the PLZT plate to the positive ions at sufficient density, from 1.times.10.sup.12 to 1.times.10.sup.17, and with sufficient energy, from 100 to 500 KeV, to provide photosensitivity enhancement. The PLZT material may have a lanthanum content ranging from 5 to 10%, a lead zirconate content of 62 to 70 mole %, and a lead titanate content of 38 to 30%. The ions are implanted at a depth of 0.1 to 2 microns below the surface of the PLZT plate.

A targeted strategy to identify untargeted metabolites from in vitro to in vivo: Rapid and sensitive metabolites profiling of licorice in rats using ultra-high performance liquid chromatography coupled with triple quadrupole-linear ion trap mass spectrometry.

PubMed

Huang, Meilin; Cheng, Zhongzhe; Wang, Lu; Feng, Yulin; Huang, Jiangeng; Du, Zhifeng; Jiang, Hongliang

2018-05-29

It is challenging to conduct in vivo metabolic study for traditional Chinese medicines (TCMs) because of complex components, unpredictable metabolic pathways and low metabolite concentrations. Herein, we proposed a sensitive strategy to characterize TCM metabolites in vivo at an orally clinical dose using ultra-high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (UHPLC-QTRAP-MS). Firstly, the metabolism of individual compounds in rat liver microsomes was studied to obtain the metabolic pathways and fragmentation patterns. The untargeted metabolites in vitro were detected by multiple ion monitoring-enhanced product ion (EPI) and neutral loss-EPI scans. Subsequently, a sensitive multiple reaction monitoring-EPI method was developed according to the in vitro results and predicted metabolites to profile the in vivo metabolites. Licorice as a model herb was used to evaluate and validate our strategy. A clinical dose of licorice water extract was orally administered to rats, then a total of 45 metabolites in urine, 21 metabolites in feces and 35 metabolites in plasma were detected. Among them, 18 minor metabolites have not been reported previously and 6 minor metabolites were first detected in vivo. Several isomeric metabolites were well separated and differentiated in our strategy. These results suggested that this new strategy could be widely used for the detection and characterization of in vivo metabolites of TCMs. Copyright © 2018. Published by Elsevier B.V.

Microbeam mapping of single event latchups and single event upsets in CMOS SRAMs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barak, J.; Adler, E.; Fischer, B.E.

1998-06-01

The first simultaneous microbeam mapping of single event upset (SEU) and latchup (SEL) in the CMOS RAM HM65162 is presented. The authors found that the shapes of the sensitive areas depend on V{sub DD}, on the ions being used and on the site on the chip being hit by the ion. In particular, they found SEL sensitive sites close to the main power supply lines between the memory-bit-arrays by detecting the accompanying current surge. All these SELs were also accompanied by bit-flips elsewhere in the memory (which they call indirect SEUs in contrast to the well known SEUs induced inmore » the hit memory cell only). When identical SEL sensitive sites were hit farther away from the supply lines only indirect SEL sensitive sites could be detected. They interpret these events as latent latchups in contrast to the classical ones detected by their induced current surge. These latent SELs were probably decoupled from the main supply lines by the high resistivity of the local supply lines.« less

Copper Ion Detection in Drinking Water via a Fabric Nanocomposite Sensor

NASA Astrophysics Data System (ADS)

Yu, Guoqiang

Excessive Cu(II) ions in drinking water are always a big threat to people's health. In this work, we developed a flexible amperometric sensor by a simple dip-coating method, which was able to rapidly, sensitively, and selectively detect the Cu(II) ions in the range of 0.65 to 39 ppm in real time. The prepared Cu(II) sensor consisted of three layers that were electrospun nylon-6 nanofibers, multiwalled carbon nanotubes (MWCNTs), and 2,2':5',2''-terthiophene molecules, respectively. When a voltage was applied to the Cu(II) sensor, the current was obviously impeded in the presence of Cu(II) ions. Interfering metal ions, including Cd(II), Fe(II), Pb(II), Hg(II), and Ag(I) ions, had almost no influence on the responsiveness of the Cu(II) sensor.

Apparatus and method for the simultaneous detection of neutrons and ionizing electromagnetic radiation

DOEpatents

Bell, Zane W.

2000-01-01

A sensor for simultaneously detecting neutrons and ionizing electromagnetic radiation comprising: a sensor for the detection of gamma radiation, the sensor defining a sensing head; the sensor further defining an output end in communication with the sensing head; and an exterior neutron-sensitive material configured to form around the sensing head; wherein the neutron-sensitive material, subsequent to the capture of the neutron, fissions into an alpha-particle and a .sup.7 Li ion that is in a first excited state in a majority of the fissions, the first excited state decaying via the emission of a single gamma ray at 478 keV which can in turn be detected by the sensing head; and wherein the sensing head can also detect the ionizing electromagnetic radiation from an incident radiation field without significant interference from the neutron-sensitive material. A method for simultaneously detecting neutrons and ionizing electromagnetic radiation comprising the steps of: providing a gamma ray sensitive detector comprising a sensing head and an output end; conforming an exterior neutron-sensitive material configured to form around the sensing head of the detector; capturing neutrons by the sensing head causing the neutron-sensitive material to fission into an alpha-particle and a .sup.7 Li ion that is in a first excited state in a majority of the fissions, the state decaying via the emission of a single gamma ray at 478 keV; sensing gamma rays entering the detector through the neutron-sensitive material; and producing an output through a readout device coupled to the output end; wherein the detector provides an output which is proportional to the energy of the absorbed ionizing electromagnetic radiation.

Fluorescence-based ion-sensing with colloidal particles.

PubMed

Ashraf, Sumaira; Carrillo-Carrion, Carolina; Zhang, Qian; Soliman, Mahmoud G; Hartmann, Raimo; Pelaz, Beatriz; Del Pino, Pablo; Parak, Wolfgang J

2014-10-01

Particle-based fluorescence sensors for the quantification of specific ions can be made by coupling ion-sensitive fluorophores to carrier particles, or by using intrinsically fluorescent particles whose fluorescence properties depend on the concentration of the ions. Despite the advantages of such particle-based sensors for the quantitative detection of ions, such as the possibility to tune the surface chemistry and thus entry portal of the sensor particles to cells, they have also some associated problems. Problems involve for example crosstalk of the ion-sensitive fluorescence read-out with pH, or spectral overlap of the emission spectra of different fluorescent particles in multiplexing formats. Here the benefits of using particle-based fluorescence sensors, their limitations and strategies to overcome these limitations will be described and exemplified with selected examples. Copyright © 2014 Elsevier Ltd. All rights reserved.

L-cysteine protected copper nanoparticles as colorimetric sensor for mercuric ions.

PubMed

Soomro, Razium A; Nafady, Ayman; Sirajuddin; Memon, Najma; Sherazi, Tufail H; Kalwar, Nazar H

2014-12-01

This report demonstrates a novel, simple and efficient protocol for the synthesis of copper nanoparticles in aqueous solution using L-cysteine as capping or protecting agent. UV-visible (UV-vis) spectroscopy was employed to monitor the LSPR band of L-cysteine functionalized copper nanoparticles (Cyst-Cu NPs) based on optimizing various reaction parameters. Fourier Transform Infrared (FTIR) spectroscopy provided information about the surface interaction between L-cysteine and Cu NPs. Transmission Electron Microscopy (TEM) confirmed the formation of fine spherical, uniformly distributed Cyst-Cu NPs with average size of 34 ± 2.1 nm. X-ray diffractometry (XRD) illustrated the formation of pure metallic phase crystalline Cyst-Cu NPs. As prepared Cyst-Cu NPs were tested as colorimetric sensor for determining mercuric (Hg(2+)) ions in an aqueous system. Cyst-Cu NPs demonstrated very sensitive and selective colorimetric detection of Hg(2+) ions in the range of 0.5 × 10(-6)-3.5 × 10(-6) mol L(-1) based on decrease in LSPR intensity as monitored by a UV-vis spectrophotometer. The developed sensor is simple, economic compared to those based on precious metal nanoparticles and sensitive to detect Hg(2+) ions with detection limit down to 4.3 × 10(-8) mol L(-1). The sensor developed in this work has a high potential for rapid and on-site detection of Hg(2+) ions. The sensor was successfully applied for assessment of Hg(2+) ions in real water samples collected from various locations of the Sindh River. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of polyphosphates in fish and shrimps tissues by two different ion chromatography methods: implications on false-negative and -positive findings.

PubMed

Kaufmann, A; Maden, K; Leisser, W; Matera, M; Gude, T

2005-11-01

Inorganic polyphosphates (di-, tri- and higher polyphosphates) can be used to treat fish, fish fillets and shrimps in order to improve their water-binding capacity. The practical relevance of this treatment is a significant gain of weight caused by the retention/uptake of water and natural juice into the fish tissues. This practice is legal; however, the use of phosphates has to be declared. The routine control testing of fish for the presence of polyphosphates, produced some results that were difficult to explain. One of the two analytical methods used determined low diphosphate concentrations in a number of untreated samples, while the other ion chromatography (IC) method did not detect them. This initiated a number of investigations: results showed that polyphosphates in fish and shrimps tissue undergo a rapid enzymatic degradation, producing the ubiquitous orthophosphate. This led to the conclusion that sensitive analytical methods are required in order to detect previous polyphosphate treatment of a sample. The polyphosphate concentrations detected by one of the analytical methods could not be explained by the degradation of endogenous high-energy nucleotides like ATP into diphosphate, but by a coeluting compound. Further investigations by LC-MS-MS proved that the substance responsible for the observed peak was inosine monophsosphate (IMP) and not as thought the inorganic diphosphate. The method producing the false-positive result was modified and both methods were ultimately able to detect polyphosphates well separated from natural nucleotides. Polyphosphates could no longer be detected (<0.5 mg kg-1) after modification of the analytical methodology. The relevance of these findings lies in the fact that similar analytical methods are employed in various control laboratories, which might lead to false interpretation of measurements.

Highly selectively monitoring heavy and transition metal ions by a fluorescent sensor based on dipeptide.

PubMed

Neupane, Lok Nath; Thirupathi, Ponnaboina; Jang, Sujung; Jang, Min Jung; Kim, Jung Hwa; Lee, Keun-Hyeung

2011-09-15

Fluorescent sensor (DMH) based on dipeptide was efficiently synthesized in solid phase synthesis. The dipeptide sensor shows sensitive response to Ag(I), Hg(II), and Cu(II) among 14 metal ions in 100% aqueous solution. The fluorescent sensor differentiates three heavy metal ions by response type; turn on response to Ag(I), ratiometric response to Hg(II), and turn off detection of Cu(II). The detection limits of the sensor for Ag(I) and Cu(II) were much lower than the EPA's drinking water maximum contaminant levels (MCL). Specially, DMH penetrated live cells and detected intracellular Ag(+) by turn on response. We described the fluorescent change, binding affinity, detection limit for the metal ions. The study of a heavy metal-responsive sensor based on dipeptide demonstrates its potential utility in the environment field. Copyright © 2011 Elsevier B.V. All rights reserved.

Terpyridine derivatives as "turn-on" fluorescence chemosensors for the selective and sensitive detection of Zn2+ ions in solution and in live cells.

PubMed

Mandal, Tripti; Hossain, Anowar; Dhara, Anamika; Al Masum, Abdulla; Konar, Saugata; Manna, Saikat Kumar; Seth, Saikat Kumar; Pathak, Sudipta; Mukhopadhyay, Subrata

2018-06-20

A terpyridine based compound L1 was designed and synthesized as an "off-on" chemosensor for the detection of Zn2+. Chemosensor L1 showed excellent selectivity and sensitivity toward Zn2+ by exhibiting a large fluorescence enhancement (∼51-fold) at 370 nm whereas other competitive metal ions did not show any noticeable change in the emission spectra of chemosensor L1. The chemosensor (L1) was shown to detect Zn2+ ions down to 9.76 μM at pH 7.4. However, chemosensor L1 binds Zn2+ in a 1 : 2 ratio (receptor : metal) with an association constant of 1.85 × 104 (R2 = 0.993) and this 1 : 2 stoichiometric fashion is established on the basis of a Job plot and mass spectroscopy. DFT/TD-DFT calculations were carried out to understand the binding nature, coordination features and electronic properties of L1 and the L1-2Zn2+ complex. In addition, this "turn-on" fluorescence probe was effectively used to image intracellular Zn2+ ions in cultured MDA-MB-468 cells.

Highly sensitive and selective fluoride detection in water through fluorophore release from a metal-organic framework

PubMed Central

Hinterholzinger, Florian M.; Rühle, Bastian; Wuttke, Stefan; Karaghiosoff, Konstantin; Bein, Thomas

2013-01-01

The detection, differentiation and visualization of compounds such as gases, liquids or ions are key challenges for the design of selective optical chemosensors. Optical chemical sensors employ a transduction mechanism that converts a specific analyte recognition event into an optical signal. Here we report a novel concept for fluoride ion sensing where a porous crystalline framework serves as a host for a fluorescent reporter molecule. The detection is based on the decomposition of the host scaffold which induces the release of the fluorescent dye molecule. Specifically, the hybrid composite of the metal-organic framework NH2-MIL-101(Al) and fluorescein acting as reporter shows an exceptional turn-on fluorescence in aqueous fluoride-containing solutions. Using this novel strategy, the optical detection of fluoride is extremely sensitive and highly selective in the presence of many other anions. PMID:24008779

Artemisinin-Luminol Chemiluminescence for Forensic Bloodstain Detection Using a Smart Phone as a Detector.

PubMed

Gao, Wenyue; Wang, Chao; Muzyka, Kateryna; Kitte, Shimeles Addisu; Li, Jianping; Zhang, Wei; Xu, Guobao

2017-06-06

Forensic luminol chemiluminescence test is one of the most sensitive and popular methods for the determination of latent bloodstains. It mainly uses hydrogen peroxide or sodium perborate as coreactants. The easy decomposition of hydrogen peroxide and sodium perborate in the presence of many ions significantly affects the selectivity. Artemisinin is a natural peroxide that is quite stable in the presence of common ions. In the present study, artemisinin has been exploited for the forensic bloodstain chemiluminescence detection for the first time. Using smart phone as cost-effective portable detector, the visual detection of bloodstains has been achieved with a dilution factor of blood up to 100 000. Moreover, this system shows excellent selectivity against many common species. It can well differentiate bloodstains from other stains, such as coffee, brown sugar, and black tea. Both favorable sensitivity and selectivity makes the present method promising in forensic detection.

Integrating a DNA Strand Displacement Reaction with a Whispering Gallery Mode Sensor for Label-Free Mercury (II) Ion Detection.

PubMed

Wu, Fengchi; Wu, Yuqiang; Niu, Zhongwei; Vollmer, Frank

2016-07-29

Mercury is an extremely toxic chemical pollutant of our environment. It has attracted the world's attention due to its high mobility and the ease with which it accumulates in organisms. Sensitive devices and methods specific for detecting mercury ions are, hence, in great need. Here, we have integrated a DNA strand displacement reaction with a whispering gallery mode (WGM) sensor for demonstrating the detection of Hg(2+) ions. Our approach relies on the displacement of a DNA hairpin structure, which forms after the binding of mercury ions to an aptamer DNA sequence. The strand displacement reaction of the DNA aptamer provides highly specific and quantitative means for determining the mercury ion concentration on a label-free WGM sensor platform. Our approach also shows the possibility for manipulating the kinetics of a strand displacement reaction with specific ionic species.

Integrating a DNA Strand Displacement Reaction with a Whispering Gallery Mode Sensor for Label-Free Mercury (II) Ion Detection

PubMed Central

Wu, Fengchi; Wu, Yuqiang; Niu, Zhongwei; Vollmer, Frank

2016-01-01

Mercury is an extremely toxic chemical pollutant of our environment. It has attracted the world’s attention due to its high mobility and the ease with which it accumulates in organisms. Sensitive devices and methods specific for detecting mercury ions are, hence, in great need. Here, we have integrated a DNA strand displacement reaction with a whispering gallery mode (WGM) sensor for demonstrating the detection of Hg2+ ions. Our approach relies on the displacement of a DNA hairpin structure, which forms after the binding of mercury ions to an aptamer DNA sequence. The strand displacement reaction of the DNA aptamer provides highly specific and quantitative means for determining the mercury ion concentration on a label-free WGM sensor platform. Our approach also shows the possibility for manipulating the kinetics of a strand displacement reaction with specific ionic species. PMID:27483277

Atmospheric pressure chemical ionization studies of non-polar isomeric hydrocarbons using ion mobility spectrometry and mass spectrometry with different ionization techniques

NASA Technical Reports Server (NTRS)

Borsdorf, H.; Nazarov, E. G.; Eiceman, G. A.

2002-01-01

The ionization pathways were determined for sets of isomeric non-polar hydrocarbons (structural isomers, cis/trans isomers) using ion mobility spectrometry and mass spectrometry with different techniques of atmospheric pressure chemical ionization to assess the influence of structural features on ion formation. Depending on the structural features, different ions were observed using mass spectrometry. Unsaturated hydrocarbons formed mostly [M - 1]+ and [(M - 1)2H]+ ions while mainly [M - 3]+ and [(M - 3)H2O]+ ions were found for saturated cis/trans isomers using photoionization and 63Ni ionization. These ionization methods and corona discharge ionization were used for ion mobility measurements of these compounds. Different ions were detected for compounds with different structural features. 63Ni ionization and photoionization provide comparable ions for every set of isomers. The product ions formed can be clearly attributed to the structures identified. However, differences in relative abundance of product ions were found. Although corona discharge ionization permits the most sensitive detection of non-polar hydrocarbons, the spectra detected are complex and differ from those obtained with 63Ni ionization and photoionization. c. 2002 American Society for Mass Spectrometry.

Carbon nanoparticle for highly sensitive and selective fluorescent detection of mercury(II) ion in aqueous solution.

PubMed

Li, Hailong; Zhai, Junfeng; Tian, Jingqi; Luo, Yonglan; Sun, Xuping

2011-08-15

In this article, carbon nanoparticles (CNPs) were used as a novel fluorescent sensing platform for highly sensitive and selective Hg(2+) detection. To the best of our knowledge, this is the first example of CNPs obtained from candle soot used in this type of sensor. The general concept used in this approach is based on that adsorption of the fluorescently labeled single-stranded DNA (ssDNA) probe by CNP via π-π stacking interactions between DNA bases and CNP leads to substantial dye fluorescence quenching; however, in the presence of Hg(2+), T-Hg(2+)-T induced hairpin structure does not adsorb on CNP and thus retains the dye fluorescence. A detection limit as low as 10nM was achieved. The present CNP-based biosensor for Hg(2+) detection exhibits remarkable specificity against other possible metal ions. Furthermore, superior selectivity performance was observed when Hg(2+) detection was carried out in the presence of a large amount of other interference ions. Finally, in order to evaluate its potential practical application, Hg(2+) detection was conducted with the use of lake water other than pure buffer and it is believed that it holds great promise for real sample analysis upon further development. Copyright © 2011 Elsevier B.V. All rights reserved.

Paired emitter-detector diode detection with dual wavelength monitoring for enhanced sensitivity to transition metals in ion chromatography with post-column reaction.

PubMed

O' Toole, Martina; Barron, Leon; Shepherd, Roderick; Paull, Brett; Nesterenko, Pavel; Diamond, Dermot

2009-01-01

The combination of post-column derivatisation and visible detection are regularly employed in ion chromatography (IC) to detect poorly absorbing species. Although this mode is often highly sensitive, one disadvantage is the increase in repeating baseline artifacts associated with out-of-sync pumping systems. The work presented here will demonstrate the use of a second generation design paired emitter-detector diode (PEDD-II) detection mode offering enhanced sensitivity to transition metals in IC by markedly reducing this problem and also by improving signal noise. First generation designs demonstrated the use of a single integrated PEDD detector cell as a simple, small (15 x 5 mm), highly sensitive, low cost photometric detector for the detection of metals in IC. The basic principle of this detection mode lies in the employment of two linear light emitting diodes (LEDs), one operating in normal mode as a light source and the other in reverse bias serving as a light detector. The second generation PEDD-II design showed increased sensitivity for Mn(II)- and Co(II)-2-(pyridylazo)resorcinol (PAR) complexes as a result of two simultaneously acquiring detection cells--one analytical PEDD cell and one reference PEDD cell. Therefore, the PEDD-II employs two wavelengths whereby one monitors the analyte reaction product and the second monitors a wavelength close to the isosbestic point. The optimum LED wavelength to be used for the analytical cell was investigated to maximise peak response. The fabrication process for both the analytical and reference PEDD cells was validated by determining the reproducibility of detectors within a batch. The reproducibility and sensitivity of the PEDD-II detector was then investigated using signals obtained from both intra- and inter-day chromatograms.

QCM-nanomagnetic beads biosensor for lead ion detection.

PubMed

Zhang, Qingli; Cui, Haixia; Xiong, Xingliang; Chen, Jun; Wang, Ying; Shen, Jia; Luo, Yiting; Chen, Longcong

2018-01-15

As lead poses a serious threat to humans even in small amounts, all kinds of lead detection sensors with high sensitivity and selectivity are being constantly improved and put forward. In this report, a novel, simple and label-free quartz crystal microbalance (QCM) biosensor is proposed for detecting lead ions (Pb 2+ ). The biosensor takes full advantage of the high specificity of GR-5 DNAzyme to Pb 2+ and the high sensitivity of QCM. In particular, nanomagnetic beads (NMBs) are used as a novel and effective mean of signal amplification in the biosensor because of their mass and their ability to enhance the inductive effect, which are very beneficial for both higher sensitivity and a lower detection limit. In practice, GR-5 DNAzyme, innovatively combined with NMBs, was modified on the gold electrode of the QCM through gold-sulfur self-assembly. When the electrode was exposed to Pb 2+ solution, DNAzyme was severed into two parts at the RNA site (rA), along with the release of NMBs, which caused a great increase in frequency shift of the QCM electrode. Finally, a perfect linear correlation between the logarithm of Pb 2+ concentration and the change in frequency was obtained from 1 pM to 50 nM, with a detection limit as low as 0.3 pM. Moreover, the biosensor shows both an average recovery of 97 ± 6% in a drinking water sample and an excellent specificity for Pb 2+ compared with other metal ions.

Use of high-performance liquid chromatography with diode array detection coupled to electrospray-Qq-time-of-flight mass spectrometry for the direct characterization of the phenolic fraction in organic commercial juices.

PubMed

Rodríguez-Medina, I C; Segura-Carretero, A; Fernández-Gutiérrez, A

2009-06-05

We have developed a direct method for the qualitative analysis of polyphenols in commercial organic fruit juices. The juices were diluted with water (50/50), filtered and directly injected. The analysis of phenolic compounds was carried out by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to photodiode array detection (DAD) and electrospray ionisation-Qq-time-of-flight mass spectrometry (ESI-Qq-TOF-MS). A unique gradient program has been optimized for the separation of several phenolic classes and the analysis time was only 5 min. The fruit juice samples were successfully analysed in positive and negative ionisation modes. In positive mode the anthocyanins were identified whereas the vast majority of polyphenols were identified using the negative ionisation mode. The sensitivity, together with mass accuracy and true isotopic pattern of the Qq-TOF-MS, allowed the identification of the phenolic compounds. Moreover, the advantage of the proposed method is the combined search of MS and MS/MS spectra, which improves the identification of compounds considerably, reducing ambiguities and false positive hits. Therefore the total fragmentation of the compound ion leading to the aglycone ion or other fragments was corroborated by MS-MS. The method was successfully employed to characterize diverse phenolic families in commercially available organic juices from four different fruits and consequently could be used in the future for the quantification purposes to compare different content of polyphenols in juices.

Method and apparatus for detection of charge on ions and particles

DOEpatents

Fuerstenau, Stephen Douglas; Soli, George Arthur

2002-01-01

The present invention provides a tessellated array detector with charge collecting plate (or cup) electrode pixels and amplifying circuitry integrated into each pixel making it sensitive to external electrostatic charge; a micro collector/amplifier pixel design possessing a small capacitance to ensure a high charge to voltage signal conversion for low noise/high sensitivity operation; a micro-fabricated array of such pixels to create a useful macroscopic target area for ion and charged particle collection.

Bennett ion mass spectrometers on the Pioneer Venus Bus and Orbiter

NASA Technical Reports Server (NTRS)

Taylor, H. A., Jr.; Brinton, H. C.; Wagner, T. C. G.; Blackwell, B. H.; Cordier, G. R.

1980-01-01

Identical Bennett radio-frequency ion mass spectrometer instruments on the Pioneer Venus Bus and Orbiter have provided the first in-situ measurements of the detailed composition of the planet's ionosphere. The sensitivity, resolution, and dynamic range are sufficient to provide measurements of the solar-wind-induced bow-shock, the ionopause, and highly structured distributions of up to 16 thermal ion species within the ionosphere. The use of adaptive scan and detection circuits and servo-controlled logic for ion mass and energy analysis permits detection of ion concentrations as low as 5 ions/cu cm and ion flow velocities as large as 9 km/sec for O(+). A variety of commandable modes provides ion sampling rates ranging from 0.1 to 1.6 sec between measurements of a single constituent. A lightweight sensor and electronics housing are features of a compact instrument package.

Analysis of cocaine and three of its metabolites in hair by gas chromatography-mass spectrometry using ion-trap detection for CI/MS/MS.

PubMed

Cognard, Emmanuelle; Rudaz, Serge; Bouchonnet, Stéphane; Staub, Christian

2005-11-05

A sensitive GC/CI/MS/MS method was developed for the simultaneous determination of cocaine (COC), anhydroecgonine methylester (cocaine pyrolysis product, AEME), ecgonine methylester (cocaine enzymatic hydrolysis product, EME) and cocaethylene (cocaine with ethanol trans-esterification product, COET) in human hair samples. After acid hydrolysis, hair samples were extracted with an automated solid phase extraction (SPE). The analysis of cocaine and its three metabolites was performed using an ion-trap spectrometer in positive chemical ionization with isobutane as gas reagent. The procedure was validated. Weighted linear regression was found appropriate in a concentration range of 0.10-5.00 ng/mg for AEME, 0.05-5.00 ng/mg for COC, EME and COET. The limit of detection was estimated at 0.005 ng/mg for COC and COET, at 0.025 ng/mg for EME, and at 0.050 ng/mg for AEME. Method performance was evaluated in terms of trueness and precision using quality control (QC) samples over the investigated ranges. Method selectivity and robustness were also demonstrated.

Determination of chlorpyrifos and its metabolites in cells and culture media by liquid chromatography-electrospray ionization tandem mass spectrometry.

PubMed

Yang, Xiangkun; Wu, Xian; Brown, Kyle A; Le, Thao; Stice, Steven L; Bartlett, Michael G

2017-09-15

A sensitive method to simultaneously quantitate chlorpyrifos, chlorpyrifos oxon and the detoxified product 3,5,6-trichloro-2-pyridinol (TCP) was developed using either liquid-liquid extraction for culture media samples, or protein precipitation for cell samples. Multiple reaction monitoring in positive ion mode was applied for the detection of chlorpyrifos and chlorpyrifos oxon, and selected ion recording in negative mode was applied to detect TCP. The method provided linear ranges from 5 to 500, 0.2-20 and 20-2000ng/mL for media samples and from 0.5-50, 0.02-2 and 2-200ng/million cells for CPF, CPO and TCP, respectively. The method was validated using selectivity, linearity, precision, accuracy, recovery, stability and dilution tests. All relative standard deviations (RSDs) and relative errors (REs) for QC samples were within 15% (except for LLOQ, within 20%). This method has been successfully applied to study the neurotoxicity and metabolism of chlorpyrifos in a human neuronal model. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrasensitive photoelectrochemical aptasensor for lead ion detection based on sensitization effect of CdTe QDs on MoS2-CdS:Mn nanocomposites by the formation of G-quadruplex structure.

PubMed

Shi, Jian-Jun; Zhu, Jing-Chun; Zhao, Ming; Wang, Yan; Yang, Ping; He, Jie

2018-06-01

An ultrasensitive photoelectrochemical (PEC) aptasensor for lead ion (Pb 2+ ) detection was fabricated based on MoS 2 -CdS:Mn nanocomposites and sensitization effect of CdTe quantum dots (QDs). MoS 2 -CdS:Mn modified electrode was used as the PEC matrix for the immobilization of probe DNA (pDNA) labeled with CdTe QDs. Target DNA (tDNA) were hybridized with pDNA to made the QDs locate away from the electrode surface by the rod-like double helix. The detection of Pb 2+ was based on the conformational change of the pDNA to G-quadruplex structure in the presence of Pb 2+ , which made the labeled QDs move close to the electrode surface, leading to the generation of sensitization effect and evident increase of the photocurrent intensity. The linear range was 50 fM to 100 nM with a detection limit of 16.7 fM. The recoveries of the determination of Pb 2+ in real samples were in the range of 102.5-108.0%. This proposed PEC aptasensor provides a new sensing strategy for various heavy metal ions at ultralow levels. Copyright © 2018 Elsevier B.V. All rights reserved.

A novel fluorescent probe (dtpa-bis(cytosine)) for detection of Eu(III) in rare earth metal ions

NASA Astrophysics Data System (ADS)

Yang, Fan; Ren, Peipei; Liu, Guanhong; Song, Youtao; Bu, Naishun; Wang, Jun

2018-03-01

In this paper, a novel fluorescent probe, dtpa-bis(cytosine), was designed and synthesized for detecting europium (Eu3 +) ion. Upon addition of Eu3 + ions into the dtpa-bis(cytosine) solution, the fluorescence intensity can strongly be enhanced. Conversely, adding other rare earth metal ions, such as Y3 +, Ce3 +, Pr3 +, Nd3 +, Sm3 +, Gd3 +, Tb3 +, Dy3 +, Ho3 +, Er3 +, Yb3 + and Lu3 +, into dtpa-bis(cytosine) solution, the fluorescence intensity is decreased slightly. Some parameters affecting the fluorescence intensity of dtpa-bis(cytosine) solution in the presence of Eu3 + ions were investigated, including solution pH value, Eu3 + ion concentration and interfering substances. The detection mechanism of Eu3 + ion using dtpa-bis(cytosine) as fluorescent probe was proposed. Under optimum conditions, the fluorescence emission intensities of EuIII-dtpa-bis(cytosine) at 375 nm in the concentration range of 0.50 × 10- 5 mol • L- 1-5.00 × 10- 5 mol • L- 1 of Eu3 + ion display a better linear relationship. The limit of detection (LOD) was determined as 8.65 × 10- 7 mol • L- 1 and the corresponding correlation coefficient (R2) of the linear equation is 0.9807. It is wished that the proposed method could be applied for sensitively and selectively detecting Eu3 + ion.

Integrated multi-ISE arrays with improved sensitivity, accuracy and precision

NASA Astrophysics Data System (ADS)

Wang, Chunling; Yuan, Hongyan; Duan, Zhijuan; Xiao, Dan

2017-03-01

Increasing use of ion-selective electrodes (ISEs) in the biological and environmental fields has generated demand for high-sensitivity ISEs. However, improving the sensitivities of ISEs remains a challenge because of the limit of the Nernstian slope (59.2/n mV). Here, we present a universal ion detection method using an electronic integrated multi-electrode system (EIMES) that bypasses the Nernstian slope limit of 59.2/n mV, thereby enabling substantial enhancement of the sensitivity of ISEs. The results reveal that the response slope is greatly increased from 57.2 to 1711.3 mV, 57.3 to 564.7 mV and 57.7 to 576.2 mV by electronic integrated 30 Cl- electrodes, 10 F- electrodes and 10 glass pH electrodes, respectively. Thus, a tiny change in the ion concentration can be monitored, and correspondingly, the accuracy and precision are substantially improved. The EIMES is suited for all types of potentiometric sensors and may pave the way for monitoring of various ions with high accuracy and precision because of its high sensitivity.

Carbon Dots and 9AA as a Binary Matrix for the Detection of Small Molecules by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Chen, Yongli; Gao, Dan; Bai, Hangrui; Liu, Hongxia; Lin, Shuo; Jiang, Yuyang

2016-07-01

Application of matrix-assisted laser-desorption/ionization mass spectrometry (MALDI MS) to analyze small molecules have some limitations, due to the inhomogeneous analyte/matrix co-crystallization and interference of matrix-related peaks in low m/z region. In this work, carbon dots (CDs) were for the first time applied as a binary matrix with 9-Aminoacridine (9AA) in MALDI MS for small molecules analysis. By 9AA/CDs assisted desorption/ionization (D/I) process, a wide range of small molecules, including nucleosides, amino acids, oligosaccharides, peptides, and anticancer drugs with a higher sensitivity were demonstrated in the positive ion mode. A detection limit down to 5 fmol was achieved for cytidine. 9AA/CDs matrix also exhibited excellent reproducibility compared with 9AA matrix. Moreover, by exploring the ionization mechanism of the matrix, the influence factors might be attributed to the four parts: (1) the strong UV absorption of 9AA/CDs due to their π-conjugated network; (2) the carboxyl groups modified on the CDs surface act as protonation sites for proton transfer in positive ion mode; (3) the thin layer crystal of 9AA/CDs could reach a high surface temperature more easily and lower transfer energy for LDI MS; (4) CDs could serve as a matrix additive to suppress 9AA ionization. Furthermore, this matrix was allowed for the analysis of glucose as well as nucleosides in human urine, and the level of cytidine was quantified with a linear range of 0.05-5 mM (R2 > 0.99). Therefore, the 9AA/CDs matrix was proven to be an effective MALDI matrix for the analysis of small molecules with improved sensitivity and reproducibility. This work provides an alternative solution for small molecules detection that can be further used in complex samples analysis.

Cadmium sulfide nanocluster-based electrochemical stripping detection of DNA hybridization.

PubMed

Zhu, Ningning; Zhang, Aiping; He, Pingang; Fang, Yuzhi

2003-03-01

A novel, sensitive electrochemical DNA hybridization detection assay, using cadmium sulfide (CdS) nanoclusters as the oligonucleotide labeling tag, is described. The assay relies on the hybridization of the target DNA with the CdS nanocluster oligonucleotide DNA probe, followed by the dissolution of the CdS nanoclusters anchored on the hybrids and the indirect determination of the dissolved cadmium ions by sensitive anodic stripping voltammetry (ASV) at a mercury-coated glassy carbon electrode (GCE). The results showed that only a complementary sequence could form a double-stranded dsDNA-CdS with the DNA probe and give an obvious electrochemical response. A three-base mismatch sequence and non-complementary sequence had negligible response. The combination of the large number of cadmium ions released from each dsDNA hybrid with the remarkable sensitivity of the electrochemical stripping analysis for cadmium at mercury-film GCE allows detection at levels as low as 0.2 pmol L(-1) of the complementary sequence of DNA.

Detection and Site Localization of Phosphorylcholine-Modified Peptides by NanoLC-ESI-MS/MS Using Precursor Ion Scanning and Multiple Reaction Monitoring Experiments

NASA Astrophysics Data System (ADS)

Timm, Thomas; Lenz, Christof; Merkel, Dietrich; Sadiffo, Christian; Grabitzki, Julia; Klein, Jochen; Lochnit, Guenter

2015-03-01

Phosphorylcholine (PC)-modified biomolecules like lipopolysaccharides, glycosphingolipids, and (glyco)proteins are widespread, highly relevant antigens of parasites, since this small hapten shows potent immunomodulatory capacity, which allows the establishment of long-lasting infections of the host. Especially for PC-modified proteins, structural data is rare because of the zwitterionic nature of the PC substituent, resulting in low sensitivities and unusual but characteristic fragmentation patterns. We have developed a targeted mass spectrometric approach using hybrid triple quadrupole/linear ion trap (QTRAP) mass spectrometry coupled to nanoflow chromatography for the sensitive detection of PC-modified peptides from complex proteolytic digests, and the localization of the PC-modification within the peptide backbone. In a first step, proteolytic digests are screened using precursor ion scanning for the marker ions of choline ( m/z 104.1) and phosphorylcholine ( m/z 184.1) to establish the presence of PC-modified peptides. Potential PC-modified precursors are then subjected to a second analysis using multiple reaction monitoring (MRM)-triggered product ion spectra for the identification and site localization of the modified peptides. The approach was first established using synthetic PC-modified synthetic peptides and PC-modified model digests. Following the optimization of key parameters, we then successfully applied the method to the detection of PC-peptides in the background of a proteolytic digest of a whole proteome. This methodological invention will greatly facilitate the detection of PC-substituted biomolecules and their structural analysis.

Cadmium Sulphide-Reduced Graphene Oxide-Modified Photoelectrode-Based Photoelectrochemical Sensing Platform for Copper(II) Ions

PubMed Central

Ibrahim, I; Lim, H. N; Huang, N. M; Pandikumar, A

2016-01-01

A photoelectrochemical (PEC) sensor with excellent sensitivity and detection toward copper (II) ions (Cu2+) was developed using a cadmium sulphide-reduced graphene oxide (CdS-rGO) nanocomposite on an indium tin oxide (ITO) surface, with triethanolamine (TEA) used as the sacrificial electron donor. The CdS nanoparticles were initially synthesized via the aerosol-assisted chemical vapor deposition (AACVD) method using cadmium acetate and thiourea as the precursors to Cd2+ and S2-, respectively. Graphene oxide (GO) was then dip-coated onto the CdS electrode and sintered under an argon gas flow (50 mL/min) for the reduction process. The nanostructured CdS was adhered securely to the ITO by a continuous network of rGO that also acted as an avenue to intensify the transfer of electrons from the conduction band of CdS. The photoelectrochemical results indicated that the ITO/CdS-rGO photoelectrode could facilitate broad UV-visible light absorption, which would lead to a higher and steady-state photocurrent response in the presence of TEA in 0.1 M KCl. The photocurrent decreased with an increase in the concentration of Cu2+ ions. The photoelectrode response for Cu2+ ion detection had a linear range of 0.5–120 μM, with a limit of detection (LoD) of 16 nM. The proposed PEC sensor displayed ultra-sensitivity and good selectivity toward Cu2+ ion detection. PMID:27176635

Hydrothermal growth of CuO nanoleaf structures, and their mercuric ion detection application.

PubMed

Ibupoto, Z H; Khun, K; Willander, M

2014-09-01

Mercury is the hazardous heavy metal ion for the environment and the human being therefore its determination is very important and herein we describe the development of mercury ion sensor on the CuO nanoleaf like nanostructures using cetyltrimethylammonium bromide (CTAB) surfactant as template for the growth by hydrothermal growth method. Scanning electron microscopy and X-ray diffraction study has shown high density and good crystal quality of the fabricated CuO nanostructures respectively. The presented mercury ion sensor has detected the wide range of 1.0 x 10(-7) to 1.0 x 10(-1) M mercury ion concentrations with an acceptable Nernstian behaviour and a sensitivity of 30.1 ± 0.6 mV/decade. The proposed mercury ion sensor exhibited low detection limit of 1.0 x 10(-8) M and also a fast response time of less than 5 s. In addition, the presented mercury ion sensor has shown an excellent repeatability, reproducibility, stability and selectivity. Moreover, the mercury ion selective electrode based on CuO nanoleaves was tested as an indicator electrode in the potentiometric titration.

Investigating the causes of low detectability of pesticides in fruits and vegetables analysed by high-performance liquid chromatography - Time-of-flight.

PubMed

Muehlwald, S; Buchner, N; Kroh, L W

2018-03-23

Because of the high number of possible pesticide residues and their chemical complexity, it is necessary to develop methods which cover a broad range of pesticides. In this work, a qualitative multi-screening method for pesticides was developed by use of HPLC-ESI-Q-TOF. 110 pesticides were chosen for the creation of a personal compound database and library (PCDL). The MassHunter Qualitative Analysis software from Agilent Technologies was used to identify the analytes. The software parameter settings were optimised to produce a low number of false positive as well as false negative results. The method was validated for 78 selected pesticides. However, the validation criteria were not fulfilled for 45 analytes. Due to this result, investigations were started to elucidate reasons for the low detectability. It could be demonstrated that the three main causes of the signal suppression were the co-eluting matrix (matrix effect), the low sensitivity of the analyte in standard solution and the fragmentation of the analyte in the ion source (in-source collision-induced dissociation). In this paper different examples are discussed showing that the impact of these three causes is different for each analyte. For example, it is possible that an analyte with low signal intensity and an intense fragmentation in the ion source is detectable in a difficult matrix, whereas an analyte with a high sensitivity and a low fragmentation is not detectable in a simple matrix. Additionally, it could be shown that in-source fragments are a helpful tool for an unambiguous identification. Copyright © 2018 Elsevier B.V. All rights reserved.

Detection and Spatial Mapping of Mercury Contamination in Water Samples Using a Smart-Phone

PubMed Central

2014-01-01

Detection of environmental contamination such as trace-level toxic heavy metal ions mostly relies on bulky and costly analytical instruments. However, a considerable global need exists for portable, rapid, specific, sensitive, and cost-effective detection techniques that can be used in resource-limited and field settings. Here we introduce a smart-phone-based hand-held platform that allows the quantification of mercury(II) ions in water samples with parts per billion (ppb) level of sensitivity. For this task, we created an integrated opto-mechanical attachment to the built-in camera module of a smart-phone to digitally quantify mercury concentration using a plasmonic gold nanoparticle (Au NP) and aptamer based colorimetric transmission assay that is implemented in disposable test tubes. With this smart-phone attachment that weighs <40 g, we quantified mercury(II) ion concentration in water samples by using a two-color ratiometric method employing light-emitting diodes (LEDs) at 523 and 625 nm, where a custom-developed smart application was utilized to process each acquired transmission image on the same phone to achieve a limit of detection of ∼3.5 ppb. Using this smart-phone-based detection platform, we generated a mercury contamination map by measuring water samples at over 50 locations in California (USA), taken from city tap water sources, rivers, lakes, and beaches. With its cost-effective design, field-portability, and wireless data connectivity, this sensitive and specific heavy metal detection platform running on cellphones could be rather useful for distributed sensing, tracking, and sharing of water contamination information as a function of both space and time. PMID:24437470

Selective and sensitized spectrophotometric determination of trace amounts of Ni(II) ion using α-benzyl dioxime in surfactant media

NASA Astrophysics Data System (ADS)

Ghaedi, Mehrorang

2007-02-01

Highly sensitive and interference-free sensitized spectrophotometric method for the determination of Ni(II) ions is described. The method is based on the reaction between Ni(II) ion and benzyl dioxime in micellar media in the presence of sodium dodecyl sulfate (SDS). The absorbance is linear from 0.1 up to 25.0 μg mL -1 in aqueous solution with repeatability (RSD) of 1.0% at a concentration of 1 μg mL -1 and a detection limit of 0.12 ng mL -1 and molar absorption coefficient of 68,600 L mol -1 cm -1. The influence of reaction variables including type and amount of surfactant, pH, and amount of ligand and complexation time and the effect of interfering ions are investigated. The proposed procedure was applied to the determination of trace amounts of Ni(II) ion in tap water, river water, chocolate and vegetable without separation or organic solvent extraction.

Molecular wake shield gas analyzer

NASA Technical Reports Server (NTRS)

Hoffman, J. H.

1980-01-01

Techniques for measuring and characterizing the ultrahigh vacuum in the wake of an orbiting spacecraft are studied. A high sensitivity mass spectrometer that contains a double mass analyzer consisting of an open source miniature magnetic sector field neutral gas analyzer and an identical ion analyzer is proposed. These are configured to detect and identify gas and ion species of hydrogen, helium, nitrogen, oxygen, nitric oxide, and carbon dioxide and any other gas or ion species in the 1 to 46 amu mass range. This range covers the normal atmospheric constituents. The sensitivity of the instrument is sufficient to measure ambient gases and ion with a particle density of the order of one per cc. A chemical pump, or getter, is mounted near the entrance aperture of the neutral gas analyzer which integrates the absorption of ambient gases for a selectable period of time for subsequent release and analysis. The sensitivity is realizable for all but rare gases using this technique.

A colorimetric and fluorogenic probe for bisulfite using benzopyrylium as the recognition unit.

PubMed

Zhang, Yun; Zhang, Xiangwen; Yang, Xiao-Feng; Zhang, Juan

2017-11-01

A coumarin-benzopyrylium (CB) platform has been developed for the colorimetric and fluorogenic detection of bisulfite. The proposed probe utilizes coumarin as the fluorophore and positively charged benzopyrylium as the reaction site. The method employs the nucleophilic addition of bisulfite to the benzopyrylium moiety of CB to inactivate the electron-deficient oxonium ion. The driving force for photo-induced electron transfer is considerably diminished, thereby promoting the emission intensity of the coumarin fluorophore. The fluorescence intensity at 510 nm is linear with bisulfite concentration over a range of 0.2-7.5 μM with a detection limit of 42 nM (3δ). CB shows a rapid response (within 30 s) and high selectivity and sensitivity for bisulfite. Preliminary studies show that CB has great potential for bisulfite detection in real samples and in living cells. Copyright © 2017 John Wiley & Sons, Ltd.

Non-invasive screening for Alzheimer's disease by sensing salivary sugar using Drosophila cells expressing gustatory receptor (Gr5a) immobilized on an extended gate ion-sensitive field-effect transistor (EG-ISFET) biosensor.

PubMed

Lau, Hui-Chong; Lee, In-Kyu; Ko, Pan-Woo; Lee, Ho-Won; Huh, Jeung-Soo; Cho, Won-Ju; Lim, Jeong-Ok

2015-01-01

Body fluids are often used as specimens for medical diagnosis. With the advent of advanced analytical techniques in biotechnology, the diagnostic potential of saliva has been the focus of many studies. We recently reported the presence of excess salivary sugars, in patients with Alzheimer's disease (AD). In the present study, we developed a highly sensitive, cell-based biosensor to detect trehalose levels in patient saliva. The developed biosensor relies on the overexpression of sugar sensitive gustatory receptors (Gr5a) in Drosophila cells to detect the salivary trehalose. The cell-based biosensor was built on the foundation of an improved extended gate ion-sensitive field-effect transistor (EG-ISFET). Using an EG-ISFET, instead of a traditional ion-sensitive field-effect transistor (ISFET), resulted in an increase in the sensitivity and reliability of detection. The biosensor was designed with the gate terminals segregated from the conventional ISFET device. This design allows the construction of an independent reference and sensing region for simultaneous and accurate measurements of samples from controls and patients respectively. To investigate the efficacy of the cell-based biosensor for AD screening, we collected 20 saliva samples from each of the following groups: participants diagnosed with AD, participants diagnosed with Parkinson's disease (PD), and a control group composed of healthy individuals. We then studied the response generated from the interaction of the salivary trehalose of the saliva samples and the Gr5a in the immobilized cells on an EG-ISFET sensor. The cell-based biosensor significantly distinguished salivary sugar, trehalose of the AD group from the PD and control groups. Based on these findings, we propose that salivary trehalose, might be a potential biomarker for AD and could be detected using our cell-based EG-ISFET biosensor. The cell-based EG-ISFET biosensor provides a sensitive and direct approach for salivary sugar detection and may be used in the future as a screening method for AD.

Characterization of multilayer Thick-GEM geometries as 10B converters aiming thermal neutron detection

NASA Astrophysics Data System (ADS)

Natal da Luz, H.; Souza, F. A.; Moralles, M.; Carlin, N.; Oliveira, R. A. N.; Bregant, M.; Suaide, A. A. P.; Chubaci, J. F. D.; Matsuoka, M.; Silva, T. F.; Moro, M. V.; Rodrigues, C. L.; Munhoz, M. G.

2018-02-01

Boron-based thermal neutron detectors have recently regained some attention from the instrumentation community as a strong alternative to helium-3 detectors. From the existing concepts exploiting boron layers in position sensitive detectors, the Cascade [1] is the one that takes full advantage of the 2D capabilities of gaseous detectors, with the position resolution not limited by the architecture of the detector. In this work, a proposal for the Cascade detector, based on Thick-GEMs is presented, together with some preliminary studies of the suitable pitch that optimizes the neutron conversion efficiency, while keeping the collection efficiency intact. The characterization of Thick-GEM prototypes produced in Brazil with hole pitch from 0.75 to 3 mm shows that these devices already present a stable performance at low gains, also resulting in fair energy resolution, when cascaded with a standard KaptonTM 50 µm GEM. Results of the first attempts of boron film depositions with Ion Beam Assisted Deposition and characterization by Ion Beam Analysis are also presented.

Sensor apparatus using an electrochemical cell

DOEpatents

Thakur, Mrinal

2002-01-01

A novel technology for sensing mechanical quantities such as force, stress, strain, pressure and acceleration has been invented. This technology is based on a change in the electrochemically generated voltage (electromotive force) with application of force, stress, strain, pressure or acceleration. The change in the voltage is due to a change in the internal resistance of the electrochemical cell with a change in the relative position or orientation of the electrodes (anode and cathode) in the cell. The signal to be detected (e.g. force, stress, strain, pressure or acceleration) is applied to one of the electrodes to cause a change in the relative position or orientation between the electrodes. Various materials, solid, semisolid, gel, paste or liquid can be utilized as the electrolyte. The electrolyte must be an ion conductor. The examples of solid electrolytes include specific polymer conductors, polymer composites, ion conducting glasses and ceramics. The electrodes are made of conductors such as metals with dissimilar electronegativities. Significantly enhanced sensitivities, up to three orders of magnitude higher than that of comparable commercial sensors, are obtained. The materials are substantially less expensive than commercially used materials for mechanical sensors.

Carbon nanotubes and graphene modified screen-printed carbon electrodes as sensitive sensors for the determination of phytochelatins in plants using liquid chromatography with amperometric detection.

PubMed

Dago, Àngela; Navarro, Javier; Ariño, Cristina; Díaz-Cruz, José Manuel; Esteban, Miquel

2015-08-28

Nanomaterials are of great interest for the development of electrochemical sensors. Multi-walled carbon nanotubes and graphene were used to modify the working electrode surface of different screen-printed carbon electrodes (SPCE) with the aim of improving the sensitivity of the SPCE and comparing it with the conventional glassy carbon electrode. To assay the usability of these sensors, a HPLC methodology with amperometric detection was developed to analyze several phytochelatins in plants of Hordeum vulgare and Glycine max treated with Hg(II) or Cd(II) giving detection limits in the low μmolL(-1) range. Phytochelatins are low molecular weight peptides with the general structure γ-(Glu-Cys)n-Gly (n=2-5) which are synthesized in plants in the presence of heavy metal ions. These compounds can chelate heavy metal ions by the formation of complexes which, are transported to the vacuoles, where the toxicity is not threatening. For this reason phytochelatins are essential in the detoxification of heavy metal ions in plants. The developed HPLC method uses a mobile phase of 1% of formic acid in water with KNO3 or NaCl (pH=2.00) and 1% of formic acid in acetonitrile. Electrochemical detection at different carbon-based electrodes was used. Among the sensors tested, the conventional glassy carbon electrode offers the best sensitivity although modification improves the sensitivity of the SPCE. Glutathione and several isoforms of phytochelatin two were found in plant extracts of both studied species. Copyright © 2015 Elsevier B.V. All rights reserved.

Liquid crystal based optical platform for the detection of Pb2+ ions using NiFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Zehra, Saman; Gul, Iftikhar Hussain; Hussain, Zakir

2018-06-01

A simple, sensitive, selective and real time detection protocol was developed for Pb2+ ions in water using liquid crystals (LCs). In this method, NiFe2O4 nanoparticles were synthesized using chemical co-precipitation method. Crystallite size, morphological, functional groups and magnetization studies were confirmed using X-ray diffraction, Scanning Electron Microscopy, and Fourier transform infrared spectroscopy techniques, respectively. The nanoparticles were mono dispersed with average particle size of 20 ± 2 nm. The surfactant stabilized magnetic nanoparticles were incubated in liquid crystal based sensor system for the detection of Pb+2 ions. The bright to dark transition of LC was observed through optical microscope. When this system was further immersed with a solution containing Pb2+ ions, it caused homeotropic to planar orientation of LC. This interaction is attributed to the presence of abundant hydroxyl groups in such as M-OH, Fe-OH on the surface of spinel ferrites nanoparticles. These groups interact with metal ions at aqueous interface, causing disruption in LCs orientation giving bright texture. This sensor showed higher selectivity towards Pb2+ ions. The detection limit was estimated to be 100 ppb. The cheap and effective protocol reported here should make promising development of LC based sensor for lead ion detection.

Photoinduced Electron Transfer Based Ion Sensing within an Optical Fiber

PubMed Central

Englich, Florian V.; Foo, Tze Cheung; Richardson, Andrew C.; Ebendorff-Heidepriem, Heike; Sumby, Christopher J.; Monro, Tanya M.

2011-01-01

We combine suspended-core microstructured optical fibers with the photoinduced electron transfer (PET) effect to demonstrate a new type of fluorescent optical fiber-dip sensing platform for small volume ion detection. A sensor design based on a simple model PET-fluoroionophore system and small core microstructured optical fiber capable of detecting sodium ions is demonstrated. The performance of the dip sensor operating in a high sodium concentration regime (925 ppm Na+) and for lower sodium concentration environments (18.4 ppm Na+) is explored and future approaches to improving the sensor’s signal stability, sensitivity and selectivity are discussed. PMID:22163712

Chemometric studies for the characterization and differentiation of microorganisms using in situ derivatization and thermal desorption ion mobility spectrometry.

PubMed

Ochoa, Mariela L; Harrington, Peter B

2005-02-01

Whole-cell bacteria were characterized and differentiated by thermal desorption ion mobility spectrometry and chemometric modeling. Principal component analysis was used to evaluate the differences in the ion mobility spectra of whole-cell bacteria and the fatty acid methyl esters (FAMEs) generated in situ after derivatization of the bacterial lipids. Alternating least squares served to extract bacterial peaks from the complex ion mobility spectra of intact microorganisms and, therefore, facilitated the characterization of bacterial strains, species, and Gram type. In situ thermal hydrolysis/methylation with tetramethylammonium hydroxide was necessary for the differentiation of Escherichia coli strains, which otherwise could not be distinguished by spectra acquired with the ITEMISER ion mobility spectrometer. The addition of the methylating agent had no effect on Gram-positive bacteria, and therefore, they could not be differentiated by genera. The classification of E. coli strains was possible by analysis of the IMS spectra from the FAMEs generated in situ. By using the fuzzy multivariate rule-building expert system and cross-validation, a correct classification rate of 96% (22 out of 23 spectra) was obtained. Chemometric modeling on bacterial ion mobility spectra coupled to thermal hydrolysis/methylation proved a simple, rapid (2 min/sample), inexpensive, and sensitive technique to characterize and differentiate intact microorganisms. The ITEMISER ion mobility spectrometer could detect as few as 4 x 10(6) cells/sample.

Calorimetric low temperature detectors for low-energetic heavy ions and their application in accelerator mass spectrometry

NASA Astrophysics Data System (ADS)

Kraft-Bermuth, S.; Andrianov, V. A.; Bleile, A.; Echler, A.; Egelhof, P.; Kiseleva, A.; Kiselev, O.; Meier, H. J.; Meier, J. P.; Shrivastava, A.; Weber, M.; Golser, R.; Kutschera, W.; Priller, A.; Steier, P.; Vockenhuber, C.

2009-10-01

The energy-sensitive detection of heavy ions with calorimetric low temperature detectors was investigated in the energy range of E =0.1-1 MeV/amu, commonly used for accelerator mass spectrometry (AMS). The detectors used consist of sapphire absorbers and superconducting aluminum transition edge thermometers operated at T ˜1.5 K. They were irradiated with various ion beams (C13,A197u,U238) provided by the VERA tandem accelerator in Vienna, Austria. The relative energy resolution obtained was ΔE /E=(5-9)×10-3, even for the heaviest ions such as U238. In addition, no evidence for a pulse height defect was observed. This performance allowed for the first time to apply a calorimetric low temperature detector in an AMS experiment. The aim was to precisely determine the isotope ratio of U236/U238 for several samples of natural uranium, U236 being known as a sensitive monitor for neutron fluxes. Replacing a conventionally used detection system at VERA by the calorimetric detector enabled to substantially reduce background from neighboring isotopes and to increase the detection efficiency. Due to the high sensitivity achieved, a value of U236/U238=6.1×10-12 could be obtained, representing the smallest U236/U238 ratio measured at the time. In addition, we contributed to establishing an improved material standard of U236/U238, which can be used as a reference for future AMS measurements.

Detection of lead(II) ions with a DNAzyme and isothermal strand displacement signal amplification.

PubMed

Li, Wenying; Yang, Yue; Chen, Jian; Zhang, Qingfeng; Wang, Yan; Wang, Fangyuan; Yu, Cong

2014-03-15

A DNAzyme based method for the sensitive and selective quantification of lead(II) ions has been developed. A DNAzyme that requires Pb(2+) for activation was selected. An RNA containing DNA substrate was cleaved by the DNAzyme in the presence of Pb(2+). The 2',3'-cyclic phosphate of the cleaved 5'-part of the substrate was efficiently removed by Exonuclease III. The remaining part of the single stranded DNA (9 or 13 base long) was subsequently used as the primer for the strand displacement amplification reaction (SDAR). The method is highly sensitive, 200 pM lead(II) could be easily detected. A number of interference ions were tested, and the sensor showed good selectivity. Underground water samples were also tested, which demonstrated the feasibility of the current approach for real sample applications. It is feasible that our method could be used for DNAzyme or aptazyme based new sensing method developments for the quantification of other target analytes with high sensitivity and selectivity. © 2013 Elsevier B.V. All rights reserved.

Fabrication of an electrochemical sensor based on spiropyran for sensitive and selective detection of fluoride ion.

PubMed

Tao, Jia; Zhao, Peng; Li, Yinhui; Zhao, Wenjie; Xiao, Yue; Yang, Ronghua

2016-04-28

In the past decades, numerous electrochemical sensors based on exogenous electroactive substance have been reported. Due to non-specific interaction between the redox mediator and the target, the instability caused by false signal may not be avoided. To address this issue, in this paper, a new electrochemical sensor based on spiropyran skeleton, namely SPOSi, was designed for specific electrochemical response to fluoride ions (F(-)). The breakage of Si-O induced by F(-) based on the specific nucleophilic substitution reaction between F(-) and silica would directly produce a hydroquinone structure for electrochemical signal generation. To improve the sensitivity, SPOSi probe was assembled on the single-walled carbon nanotubes (SWCNTs) modified glassy carbon electrode (GCE) through the π-π conjugating interaction. This electrode was successfully applied to monitor F(-) with a detection limit of 8.3 × 10(-8) M. Compared with the conventional F(-) ion selected electrode (ISE) which utilized noncovalent interaction, this method displays higher stability and a comparable sensitivity in the urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Radiation sensitive devices and systems for detection of radioactive materials and related methods

DOEpatents

Kotter, Dale K

2014-12-02

Radiation sensitive devices include a substrate comprising a radiation sensitive material and a plurality of resonance elements coupled to the substrate. Each resonance element is configured to resonate responsive to non-ionizing incident radiation. Systems for detecting radiation from a special nuclear material include a radiation sensitive device and a sensor located remotely from the radiation sensitive device and configured to measure an output signal from the radiation sensitive device. In such systems, the radiation sensitive device includes a radiation sensitive material and a plurality of resonance elements positioned on the radiation sensitive material. Methods for detecting a presence of a special nuclear material include positioning a radiation sensitive device in a location where special nuclear materials are to be detected and remotely interrogating the radiation sensitive device with a sensor.

Detection of trace heavy metal ions in water by nanostructured porous Si biosensors.

PubMed

Shtenberg, Giorgi; Massad-Ivanir, Naama; Segal, Ester

2015-07-07

A generic biosensing platform, based on nanostructured porous Si (PSi), Fabry-Pérot thin films, for label-free monitoring of heavy metal ions in aqueous solutions by enzymatic activity inhibition, is described. First, we show a general detection assay by immobilizing horseradish peroxidase (HRP) within the oxidized PSi nanostructure and monitor its catalytic activity in real time by reflective interferometric Fourier transform spectroscopy. Optical studies reveal the high specificity and sensitivity of the HRP-immobilized PSi towards three metal ions (Ag(+) > Pb(2+) > Cu(2+)), with a detection limit range of 60-120 ppb. Next, we demonstrate the concept of specific detection of Cu(2+) ions (as a model heavy metal) by immobilizing Laccase, a multi-copper oxidase, within the oxidized PSi. The resulting biosensor allows for specific detection and quantification of copper ions in real water samples by monitoring the Laccase relative activity. The optical biosensing results are found to be in excellent agreement with those obtained by the gold standard analytical technique (ICP-AES) for all water samples. The main advantage of the presented biosensing concept is the ability to detect heavy metal ions at environmentally relevant concentrations using a simple and portable experimental setup, while the specific biosensor design can be tailored by varying the enzyme type.

Using fluorometry and ion-sensitive microelectrodes to study the functional expression of heterologously-expressed ion channels and transporters in Xenopus oocytes

PubMed Central

Musa-Aziz, Raif; Boron, Walter F.; Parker, Mark D.

2010-01-01

The Xenopus laevis oocyte is a model system for the electrophysiological study of exogenous ion transporters. Three main reasons make the oocyte suitable for this purpose: (a) it has a large cell size (~1 mm diameter), (b) it has an established capacity to produce—from microinjected mRNAs or cRNAs—exogenous ion transporters with close-to-physiological post-translational modifications and actions, and (c) its membranes contain endogenous ion-transport activities which are usually smaller in magnitude than the activities of exogenously-expressed ion transporters. The expression of ion-transporters as green-fluorescent-protein fusions allows the fluorometric assay of transporter yield in living oocytes. Monitoring of transporter-mediated movement of ions such as Cl−, H+ (and hence base equivalents like OH−1 and HCO3−), K+, and Na+ is achieved by positioning the tips of ion-sensitive microelectrodes inside the oocyte and/or at the surface of the oocyte plasma membrane. The use of ion-sensitive electrodes is critical for studying net ion-movements mediated by electroneutral transporters. The combined use of fluorometry and electrophysiology expedites transporter study by allowing measurement of transporter yield prior to electrophysiological study and correlation of relative transporter yield with transport rates. PMID:20051266

Sensitive screening of abused drugs in dried blood samples using ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry.

PubMed

Chepyala, Divyabharathi; Tsai, I-Lin; Liao, Hsiao-Wei; Chen, Guan-Yuan; Chao, Hsi-Chun; Kuo, Ching-Hua

2017-03-31

An increased rate of drug abuse is a major social problem worldwide. The dried blood spot (DBS) sampling technique offers many advantages over using urine or whole blood sampling techniques. This study developed a simple and efficient ultra-high-performance liquid chromatography-ion booster-quadrupole time-of-flight mass spectrometry (UHPLC-IB-QTOF-MS) method for the analysis of abused drugs and their metabolites using DBS. Fifty-seven compounds covering the most commonly abused drugs, including amphetamines, opioids, cocaine, benzodiazepines, barbiturates, and many other new and emerging abused drugs, were selected as the target analytes of this study. An 80% acetonitrile solvent with a 5-min extraction by Geno grinder was used for sample extraction. A Poroshell column was used to provide efficient separation, and under optimal conditions, the analytical times were 15 and 5min in positive and negative ionization modes, respectively. Ionization parameters of both electrospray ionization source and ion booster (IB) source containing an extra heated zone were optimized to achieve the best ionization efficiency of the investigated abused drugs. In spite of their structural diversity, most of the abused drugs showed an enhanced mass response with the high temperature ionization from an extra heated zone of IB source. Compared to electrospray ionization, the ion booster (IB) greatly improved the detection sensitivity for 86% of the analytes by 1.5-14-fold and allowed the developed method to detect trace amounts of compounds on the DBS cards. The validation results showed that the coefficients of variation of intra-day and inter-day precision in terms of the signal intensity were lower than 19.65%. The extraction recovery of all analytes was between 67.21 and 115.14%. The limits of detection of all analytes were between 0.2 and 35.7ngmL -1 . The stability study indicated that 7% of compounds showed poor stability (below 50%) on the DBS cards after 6 months of storage at room temperature and -80°C. The reported method provides a new direction for abused drug screening using DBS. Copyright © 2017 Elsevier B.V. All rights reserved.

A Signature of Spatial Correlations between rare earth ions and single-wall nanotubes wrapped with DNA in their mixed solution

NASA Astrophysics Data System (ADS)

Ignatova, Tetyana; Rotkin, Slava V.

2012-02-01

We propose that the fluorescence resonance energy transfer (FRET) between the rare earth ions (REI) and single-wall nanotubes (SWNT) can be used to measure their Coulomb correlation in solution. As a calibration experiment the FRET between two different REIs, being the energy donor and the acceptor, in their mixed solution has been used. From the photoluminescence decay time we were able to extract the characteristic distance between unlike REIs. Our study revealed negative correlation (the repulsion) for Tb-Eu solution. In the case of the solution containing the REI and the SWNTs wrapped with DNA we observed a significant positive correlation (the attraction and the complex formation). The data is in a good agreement with the theoretical estimates and allows to propose REIs and their FRET as a sensitive tool for detecting kinetics of interaction of SWNTs in aqueous solutions.

Experimental validation of the dual positive and negative ion beam acceleration in the plasma propulsion with electronegative gases thruster

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rafalskyi, Dmytro, E-mail: dmytro.rafalskyi@lpp.polytechnique.fr; Popelier, Lara; Aanesland, Ane

The PEGASES (Plasma Propulsion with Electronegative Gases) thruster is a gridded ion thruster, where both positive and negative ions are accelerated to generate thrust. In this way, additional downstream neutralization by electrons is redundant. To achieve this, the thruster accelerates alternately positive and negative ions from an ion-ion plasma where the electron density is three orders of magnitude lower than the ion densities. This paper presents a first experimental study of the alternate acceleration in PEGASES, where SF{sub 6} is used as the working gas. Various electrostatic probes are used to investigate the source plasma potential and the energy, composition,more » and current of the extracted beams. We show here that the plasma potential control in such system is key parameter defining success of ion extraction and is sensitive to both parasitic electron current paths in the source region and deposition of sulphur containing dielectric films on the grids. In addition, large oscillations in the ion-ion plasma potential are found in the negative ion extraction phase. The oscillation occurs when the primary plasma approaches the grounded parts of the main core via sub-millimetres technological inputs. By controlling and suppressing the various undesired effects, we achieve perfect ion-ion plasma potential control with stable oscillation-free operation in the range of the available acceleration voltages (±350 V). The measured positive and negative ion currents in the beam are about 10 mA for each component at RF power of 100 W and non-optimized extraction system. Two different energy analyzers with and without magnetic electron suppression system are used to measure and compare the negative and positive ion and electron fluxes formed by the thruster. It is found that at alternate ion-ion extraction the positive and negative ion energy peaks are similar in areas and symmetrical in position with +/− ion energy corresponding to the amplitude of the applied acceleration voltage.« less

Observation of Iron Specific Interaction with a Charge Neutral Phospholipid

NASA Astrophysics Data System (ADS)

Wang, Wenjie; Zhang, Honghu; Feng, Shuren; San Emeterio, Josue; Kuzmenko, Ivan; Nilsen-Hamilton, Marit; Mallapragada, Surya; Vaknin, David

2015-03-01

Using surface sensitive X-ray scattering and spectroscopic techniques we show that phosphatidyl choline (PC) head groups attract positively charged iron ions and complexes even at pH values that are lower than 3. DPPC (1,2-dipalmitoyl-sn-glycero-3-phosphocholine) is a zwitterionic lipid typically used as a model system for cell membranes. Within a large pH range (3 -11), it carries a negative charge on the phosphate group and a positive charge on the quaternary ammonium cation, thus appears charge neutral. Further lowering the pH, i.e. adding a proton to the phosphate group, results in a positively charged headgroup. Surprisingly, we detect significant enrichment of iron at the interface of the DPPC monolayer and the aqueous subphase with the pH maintained at 3 or even lower. With a supposedly charge neutral or even positive surface, the observation of surface bound, charge positive iron ions or iron hydroxides is counter-intuitive and suggests iron-specific interaction with the phospholipid headgroup, which is not governed by electrostatic interaction. The effect of the integration of Mms6, a membrane protein that promotes the formation of magnetic nanocrystals, into the DPPC monolayer will also be discussed. Research supported by the U.S. Department of Energy under Contract No. DE-AC02-07CH11358 and DE-AC02-06CH11357.

Optical transitions in highly charged californium ions with high sensitivity to variation of the fine-structure constant.

PubMed

Berengut, J C; Dzuba, V A; Flambaum, V V; Ong, A

2012-08-17

We study electronic transitions in highly charged Cf ions that are within the frequency range of optical lasers and have very high sensitivity to potential variations in the fine-structure constant, α. The transitions are in the optical range despite the large ionization energies because they lie on the level crossing of the 5f and 6p valence orbitals in the thallium isoelectronic sequence. Cf(16+) is a particularly rich ion, having several narrow lines with properties that minimize certain systematic effects. Cf(16+) has very large nuclear charge and large ionization energy, resulting in the largest α sensitivity seen in atomic systems. The lines include positive and negative shifters.

High-resolution high-sensitivity elemental imaging by secondary ion mass spectrometry: from traditional 2D and 3D imaging to correlative microscopy

NASA Astrophysics Data System (ADS)

Wirtz, T.; Philipp, P.; Audinot, J.-N.; Dowsett, D.; Eswara, S.

2015-10-01

Secondary ion mass spectrometry (SIMS) constitutes an extremely sensitive technique for imaging surfaces in 2D and 3D. Apart from its excellent sensitivity and high lateral resolution (50 nm on state-of-the-art SIMS instruments), advantages of SIMS include high dynamic range and the ability to differentiate between isotopes. This paper first reviews the underlying principles of SIMS as well as the performance and applications of 2D and 3D SIMS elemental imaging. The prospects for further improving the capabilities of SIMS imaging are discussed. The lateral resolution in SIMS imaging when using the microprobe mode is limited by (i) the ion probe size, which is dependent on the brightness of the primary ion source, the quality of the optics of the primary ion column and the electric fields in the near sample region used to extract secondary ions; (ii) the sensitivity of the analysis as a reasonable secondary ion signal, which must be detected from very tiny voxel sizes and thus from a very limited number of sputtered atoms; and (iii) the physical dimensions of the collision cascade determining the origin of the sputtered ions with respect to the impact site of the incident primary ion probe. One interesting prospect is the use of SIMS-based correlative microscopy. In this approach SIMS is combined with various high-resolution microscopy techniques, so that elemental/chemical information at the highest sensitivity can be obtained with SIMS, while excellent spatial resolution is provided by overlaying the SIMS images with high-resolution images obtained by these microscopy techniques. Examples of this approach are given by presenting in situ combinations of SIMS with transmission electron microscopy (TEM), helium ion microscopy (HIM) and scanning probe microscopy (SPM).

Quantitative determination of flavonoids by column high-performance liquid chromatography with mass spectrometry and ultraviolet absorption detection in Artemisia afra and comparative studies with various species of Artemisia plants.

PubMed

Avula, Bharathi; Wang, Yan-Hong; Smillie, Troy J; Mabusela, Wilfred; Vincent, Leszek; Weitz, Frans; Khan, Ikhlas A

2009-01-01

A simple and specific analytical method for the quantitative determination of flavonoids from the aerial parts of the Artemisia afra plant samples was developed. By column high-performance liquid chromatography (HPLC) with UV absorption and mass spectrometry (MS) detection, separation was achieved on a reversed-phase octadecylsilyl (C18) column with water, methanol, and acetonitrile, all containing 0.1% acetic acid, as the mobile phase. These methods were used to analyze various species of Artemisia plant samples. The wavelength used for quantification of flavonoids with the diode array detector was 335 nm. The limits of detection (LOD) by HPLC/MS were found to be 7.5, 7.5, 10, 2.0, and 2.0 ng/mL; and by LC-UV the LODs were 500, 500, 500, 300, and 300 ng/mL for apigenin, chrysoeriol, tamarixetin, acacetin, and genkwanin, respectively. The HPLC/MS method was found to be 50-150 times more sensitive than the HPLC-UV method. HPLC/MS coupled with an electrospray ionization interface is described for the identification and quantification of flavonoids in various plant samples. This method involved the use of the [M+H]+ ions of the compounds at mass-to-charge ratio of 1.0606, 301.0712, 317.0661, 285.0763, and 285.0763 (calculated mass), respectively, in the positive ion mode with extractive ion monitoring.

Quasi-dynamic mode of nanomembranes for time-of-flight mass spectrometry of proteins.

PubMed

Park, Jonghoo; Kim, Hyunseok; Blick, Robert H

2012-04-21

Mechanical resonators realized on the nano-scale by now offer applications in mass-sensing of biomolecules with extraordinary sensitivity. The general idea is that perfect mechanical biosensors should be of extremely small size to achieve zeptogram sensitivity in weighing single molecules similar to a balance. However, the small scale and long response time of weighing biomolecules with a cantilever restrict their usefulness as a high-throughput method. Commercial mass spectrometry (MS) such as electro-spray ionization (ESI)-MS and matrix-assisted laser desorption/ionization (MALDI)-time of flight (TOF)-MS are the gold standards to which nanomechanical resonators have to live up to. These two methods rely on the ionization and acceleration of biomolecules and the following ion detection after a mass selection step, such as time-of-flight (TOF). Hence, the spectrum is typically represented in m/z, i.e. the mass to ionization charge ratio. Here, we describe the feasibility and mass range of detection of a new mechanical approach for ion detection in time-of-flight mass spectrometry, the principle of which is that the impinging ion packets excite mechanical oscillations in a silicon nitride nanomembrane. These mechanical oscillations are henceforth detected via field emission of electrons from the nanomembrane. Ion detection is demonstrated in MALDI-TOF analysis over a broad range with angiotensin, bovine serum albumin (BSA), and an equimolar protein mixture of insulin, BSA, and immunoglobulin G (IgG). We find an unprecedented mass range of operation of the nanomembrane detector.

ISFET pH Sensitivity: Counter-Ions Play a Key Role.

PubMed

Parizi, Kokab B; Xu, Xiaoqing; Pal, Ashish; Hu, Xiaolin; Wong, H S Philip

2017-02-02

The Field Effect sensors are broadly used for detecting various target analytes in chemical and biological solutions. We report the conditions under which the pH sensitivity of an Ion Sensitive Field Effect transistor (ISFET) sensor can be significantly enhanced. Our theory and simulations show that by using pH buffer solutions containing counter-ions that are beyond a specific size, the sensor shows significantly higher sensitivity which can exceed the Nernst limit. We validate the theory by measuring the pH response of an extended gate ISFET pH sensor. The consistency and reproducibility of the measurement results have been recorded in hysteresis free and stable operations. Different conditions have been tested to confirm the accuracy and validity of our experiment results such as using different solutions, various oxide dielectrics as the sensing layer and off-the-shelf versus IC fabricated transistors as the basis of the ISFET sensor.

ISFET pH Sensitivity: Counter-Ions Play a Key Role

PubMed Central

Parizi, Kokab B.; Xu, Xiaoqing; Pal, Ashish; Hu, Xiaolin; Wong, H. S. Philip

2017-01-01

The Field Effect sensors are broadly used for detecting various target analytes in chemical and biological solutions. We report the conditions under which the pH sensitivity of an Ion Sensitive Field Effect transistor (ISFET) sensor can be significantly enhanced. Our theory and simulations show that by using pH buffer solutions containing counter-ions that are beyond a specific size, the sensor shows significantly higher sensitivity which can exceed the Nernst limit. We validate the theory by measuring the pH response of an extended gate ISFET pH sensor. The consistency and reproducibility of the measurement results have been recorded in hysteresis free and stable operations. Different conditions have been tested to confirm the accuracy and validity of our experiment results such as using different solutions, various oxide dielectrics as the sensing layer and off-the-shelf versus IC fabricated transistors as the basis of the ISFET sensor. PMID:28150700

Enzyme-assisted cycling amplification and DNA-templated in-situ deposition of silver nanoparticles for the sensitive electrochemical detection of Hg(2.).

PubMed

Xie, Hua; Wang, Qin; Chai, Yaqin; Yuan, Yali; Yuan, Ruo

2016-12-15

In this work, a label-free electrochemical biosensor was developed for sensitive and selective detection of mercury (II) ions (Hg(2+)) based on in-situ deposition of silver nanoparticles (AgNPs) on terminal deoxynucleotidyl transferase (TdT) extended ssDNA for signal output and nicking endonuclease for cycling amplification. In the presence of target Hg(2+), the T-rich DNA (HP1) could partly fold into duplex-like structure (termed as output DNA) via T-Hg(2+)-T base pairs and thus exposed its sticky end. The sticky end of output DNA could then hybridize with 3'-PO4 terminated capture DNA (HP2) on electrode surface to form output DNA-HP2 hybridization complex with the sequence 5'-CCTCAGC-3'/3'-GGAGTCG-5' (the sequence could be recognized by nicking endonuclease Nt. BbvCI). With the introduction of Nt. BbvCI, output DNA existed in hybridization complex was released from electrode and participated in the next hybridization process, accompanying with the cleave of HP2 to expose substantial 3'-OH group, which could be extended into a long ssDNA nanotail with the aid of TdT and deoxyadenosine triphosphate (dATP). Since the long negatively charged ssDNA nanotail absorbed the positively charged silver ions on the DNA skeleton, the metallic silver could be in-situ deposited on electrode surface for electrochemical signal output upon addition of reduction regent sodium borohydride. Under optimal conditions, the developed electrochemical biosensor presented a good response to Hg(2+) with a detection limit of 3 pM (S/N=3). Furthermore, the biosensor exhibited good reproducibility and high selectivity towards other interfering ions. The proposed sensing system also showed a promising potential application in real sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Watson, Thomas B.

The Particle-into-Liquid Sampler (PILS) is an aqueous-solution-based online technique for determining bulk chemical composition of ambient aerosol particles. As shown in Figure 1, the instrument consists of two units, briefly described below: 1. An aerosol extraction unit where particles are passed through a growth chamber saturated with water vapor, liquid droplets are grown, and the resulting liquid collected and transferred to the detection system. 2. The detection system that includes ion chromatographs (IC) or a total organic carbon detector (TOC). Ion chromatography is performed using two Metrohm ICs—one for positive ions and one for negative ions—with conductivity detectors. The TOCmore » is detected using a GE TOC analyzer. The instrument can be run in either the ion detection mode or the TOC mode.« less

Oligonucleotide-functionalized gold nanoparticles-enhanced QCM-D sensor for mercury(II) ions with high sensitivity and tunable dynamic range.

PubMed

Chen, Qiang; Wu, Xiaojie; Wang, Dingzhong; Tang, Wei; Li, Na; Liu, Feng

2011-06-21

A quartz crystal microbalance with dissipation monitoring (QCM-D) sensor was developed for highly sensitive and specific detection of mercury(II) ions (Hg(2+)) with a tunable dynamic range, using oligonucleotide-functionalized gold nanoparticles (GNPs) for both frequency and dissipation amplification. The fabrication of the sensor employed a 'sandwich-type' strategy, and formation of T-Hg(2+)-T structures in linker DNA reduced the hybridization of the GNPs-tagged DNA on the gold electrode, which could be used as the molecular switch for Hg(2+) sensing. This QCM-D mercury sensor showed a linear response of 10-200 nM, with detection limits of 4 nM and 7 nM for frequency and dissipation measurements, respectively. Moreover, the dynamic range of the sensor could be tuned by simply altering the concentration of linker DNA without designing new sensors in the cases where detection of Hg(2+) at different levels is required. This sensor afforded excellent selectivity toward Hg(2+) compared with other potential coexisting metal ions. The feasibility of the sensor was demonstrated by analyzing Hg(2+)-spiked tap- and lake-water samples with satisfactory recoveries. The proposed approach extended the application of the QCM-D system in metal ions sensing, and could be adopted for the detection of other analytes when complemented with the use of functional DNA structures.

NAIM and site-specific functional group modification analysis of RNase P RNA: magnesium dependent structure within the conserved P1-P4 multihelix junction contributes to catalysis.

PubMed

Kaye, Nicholas M; Christian, Eric L; Harris, Michael E

2002-04-09

The tRNA processing endonuclease ribonuclease P contains an essential and highly conserved RNA molecule (RNase P RNA) that is the catalytic subunit of the enzyme. To identify and characterize functional groups involved in RNase P RNA catalysis, we applied self-cleaving ribozyme-substrate conjugates, on the basis of the RNase P RNA from Escherichia coli, in nucleotide analogue interference mapping (NAIM) and site-specific modification experiments. At high monovalent ion concentrations (3 M) that facilitate protein-independent substrate binding, we find that the ribozyme is largely insensitive to analogue substitution and that concentrations of Mg2+ (1.25 mM) well below that necessary for optimal catalytic rate (>100 mM) are required to produce interference effects because of modification of nucleotide bases. An examination of the pH dependence of the reaction rate at 1.25 mM Mg2+ indicates that the increased sensitivity to analogue interference is not due to a change in the rate-limiting step. The nucleotide positions detected by NAIM under these conditions are located exclusively in the catalytic domain, consistent with the proposed global structure of the ribozyme, and predominantly occur within the highly conserved P1-P4 multihelix junction. Several sensitive positions in J3/4 and J2/4 are proximal to a previously identified site of divalent metal ion binding in the P1-P4 element. Kinetic analysis of ribozymes with site-specific N7-deazaadenosine and deazaguanosine modifications in J3/4 was, in general, consistent with the interference results and also permitted the analysis of sites not accessible by NAIM. These results show that, in this region only, modification of the N7 positions of A62, A65, and A66 resulted in measurable effects on reaction rate and modification at each position displayed distinct sensitivities to Mg2+ concentration. These results reveal a restricted subset of individual functional groups within the catalytic domain that are particularly important for substrate cleavage and demonstrate a close association between catalytic function and metal ion-dependent structure in the highly conserved P1-P4 multihelix junction.

Three-dimensional activated graphene network-sulfonate-terminated polymer nanocomposite as a new electrode material for the sensitive determination of dopamine and heavy metal ions.

PubMed

Yuan, Xiaoyan; Zhang, Yijia; Yang, Lu; Deng, Wenfang; Tan, Yueming; Ma, Ming; Xie, Qingji

2015-03-07

We report here that three-dimensional activated graphene networks (3DAGNs) are a better matrix to prepare graphene-polymer nanocomposites for sensitive electroanalysis than two-dimensional graphene nanosheets (2DGNs). 3DAGNs were synthesized in advance by the direct carbonization and simultaneous chemical activation of a cobalt ion-impregnated D113-type ion exchange resin, which showed an interconnected network structure and a large specific surface area. Then, the 3DAGN-sulfonate-terminated polymer (STP) nanocomposite was prepared via the in situ chemical co-polymerization of m-aminobenzene sulfonic acid and aniline in the presence of 3DAGNs. The 3DAGN-STP nanocomposite can adsorb dopamine (DA) and heavy metal ions, which was confirmed by quartz crystal microbalance studies. The 3DAGN-STP modified glassy carbon electrode (GCE) was used for the electrochemical detection of DA in the presence of ascorbic acid and uric acid, with a linear response range of 0.1-32 μM and a limit of detection of 10 nM. In addition, differential pulse voltammetry was used for the simultaneous determination of Cd(2+) and Pb(2+) at the 3DAGN-STP/GCE further modified with a bismuth film, exhibiting linear response ranges of 1-70 μg L(-1) for Cd(2+) and 1-80 μg L(-1) for Pb(2+) with limits of detection of 0.1 μg L(-1) for Cd(2+) and 0.2 μg L(-1) for Pb(2+). Because the 3DAGN-STP can integrate the advantages of 3DAGNs with STPs, the 3DAGN-STP/GCE was more sensitive than the bare GCE, 3DAGN/GCE, and 2DGN-STP/GCE for the determination of DA and heavy metal ions.

Investigations of negative and positive cesium ion species

NASA Technical Reports Server (NTRS)

Chanin, L. M.

1978-01-01

A direct test is provided of the hypothesis of negative ion creation at the anode or collector of a diode operating under conditions simulating a cesium thermionic converter. The experimental technique involves using direct ion sampling through the collector electrode with mass analysis using a quadrupole mass analyzer. Similar measurements are undertaken on positive ions extracted through the emitter electrode. Measurements were made on a variety of gases including pure cesium, helium-cesium mixtures and cesium-hydrogen as well as cesium-xenon mixtures. The gas additive was used primarily to aid in understanding the negative ion formation processes. Measurements were conducted using emitter (cathode) temperatures up to about 1000 F. The major negative ion identified through the collector was Cs(-) with minor negative ion peaks tentatively identified as H(-), H2(-), H3(-), He(-) and a mass 66. Positive ions detected were believed to be Cs(+), Cs2(+) and Cs3(+).

Using Metal Complex Ion-Molecule Reactions in a Miniature Rectilinear Ion Trap Mass Spectrometer to Detect Chemical Warfare Agents

NASA Astrophysics Data System (ADS)

Graichen, Adam M.; Vachet, Richard W.

2013-06-01

The gas-phase reactions of a series of coordinatively unsaturated [Ni(L)n]y+ complexes, where L is a nitrogen-containing ligand, with chemical warfare agent (CWA) simulants in a miniature rectilinear ion trap mass spectrometer were investigated as part of a new approach to detect CWAs. Results show that upon entering the vacuum system via a poly(dimethylsiloxane) (PDMS) membrane introduction, low concentrations of several CWA simulants, including dipropyl sulfide (simulant for mustard gas), acetonitrile (simulant for the nerve agent tabun), and diethyl phosphite (simulant for nerve agents sarin, soman, tabun, and VX), can react with metal complex ions generated by electrospray ionization (ESI), thereby providing a sensitive means of detecting these compounds. The [Ni(L)n]2+ complexes are found to be particularly reactive with the simulants of mustard gas and tabun, allowing their detection at low parts-per-billion (ppb) levels. These detection limits are well below reported exposure limits for these CWAs, which indicates the applicability of this new approach, and are about two orders of magnitude lower than electron ionization detection limits on the same mass spectrometer. The use of coordinatively unsaturated metal complexes as reagent ions offers the possibility of further tuning the ion-molecule chemistry so that desired compounds can be detected selectively or at even lower concentrations.

Small-scale structure of O2(+) and proton hydrates in a Noctilucent Cloud and polar mesospheric summer echo of August 9/10 1991 above Kiruna

NASA Technical Reports Server (NTRS)

Balsiger, F.; Kopp, E.; Friedrich, M.; Torkar, K. M.; Walchli, U.

1993-01-01

A novel mass spectrometer designed to measure simultaneously positive ion composition in the mesosphere, was successfully launched during the NLC-91 project. Instruments supporting the mass spectrometer were a probed to measure both electrons and positive ions as well as a wave propagation experiment. The location of the Noctilucent Clouds (NLC) was determined by a particle impact sensor to detect secondary electrons and ions from the impact of NLC particle. The density of proton hydrates and of the related total ions is depleted in the NLC region at 83 km. An improved detection limit of 5 x 10(exp 4)/cu m for positive ions and improved height resolution revealed for the first time large gradients in the O2(+), H(+)(H2O)2 and H(+)(H2O)6 densities within a small height range of the order of 50 m. Such gradients at the altitude of NLC and Polar Mesospheric Summer Echoes (PMSE) are associated with strong variability of mesospheric water vapor, temperature and neutral air density.

A new pH-sensitive rectifying potassium channel in mitochondria from the embryonic rat hippocampus.

PubMed

Kajma, Anna; Szewczyk, Adam

2012-10-01

Patch-clamp single-channel studies on mitochondria isolated from embryonic rat hippocampus revealed the presence of two different potassium ion channels: a large-conductance (288±4pS) calcium-activated potassium channel and second potassium channel with outwardly rectifying activity under symmetric conditions (150/150mM KCl). At positive voltages, this channel displayed a conductance of 67.84pS and a strong voltage dependence at holding potentials from -80mV to +80mV. The open probability was higher at positive than at negative voltages. Patch-clamp studies at the mitoplast-attached mode showed that the channel was not sensitive to activators and inhibitors of mitochondrial potassium channels but was regulated by pH. Moreover, we demonstrated that the channel activity was not affected by the application of lidocaine, an inhibitor of two-pore domain potassium channels, or by tertiapin, an inhibitor of inwardly rectifying potassium channels. In summary, based on the single-channel recordings, we characterised for the first time mitochondrial pH-sensitive ion channel that is selective for cations, permeable to potassium ions, displays voltage sensitivity and does not correspond to any previously described potassium ion channels in the inner mitochondrial membrane. This article is part of a Special Issue entitled: 17th European Bioenergetics Conference (EBEC 2012). Copyright © 2012 Elsevier B.V. All rights reserved.

SU-D-BRB-02: Investigations of Secondary Ion Distributions in Carbon Ion Therapy Using the Timepix Detector.

PubMed

Gwosch, K; Hartmann, B; Jakubek, J; Granja, C; Soukup, P; Jaekel, O; Martisikova, M

2012-06-01

Due to the high conformity of carbon ion therapy, unpredictable changes in the patient's geometry or deviations from the planned beam properties can result in changes of the dose distribution. PET has been used successfully to monitor the actual dose distribution in the patient. However, it suffers from biological washout processes and low detection efficiency. The purpose of this contribution is to investigate the potential of beam monitoring by detection of prompt secondary ions emerging from a homogeneous phantom, simulating a patient's head. Measurements were performed at the Heidelberg Ion-Beam Therapy Center (Germany) using a carbon ion pencil beam irradiated on a cylindrical PMMA phantom (16cm diameter). For registration of the secondary ions, the Timepix detector was used. This pixelated silicon detector allows position-resolved measurements of individual ions (256×256 pixels, 55μm pitch). To track the secondary ions we used several parallel detectors (3D voxel detector). For monitoring of the beam in the phantom, we analyzed the directional distribution of the registered ions. This distribution shows a clear dependence on the initial beam energy, width and position. Detectable were range differences of 1.7mm, as well as vertical and horizontal shifts of the beam position by 1mm. To estimate the clinical potential of this method, we measured the yield of secondary ions emerging from the phantom for a beam energy of 226MeV/u. The differential distribution of secondary ions as a function of the angle from the beam axis for angles between 0 and 90° will be presented. In this setup the total yield in the forward hemisphere was found to be in the order of 10 -1 secondary ions per primary carbon ion. The presented measurements show that tracking of secondary ions provides a promising method for non-invasive monitoring of ion beam parameters for clinical relevant carbon ion fluences. Research with the pixel detectors was carried out in frame of the Medipix Collaboration. © 2012 American Association of Physicists in Medicine.

Highly sensitive determination of iron (III) ion based on phenanthroline probe: Surface-enhanced Raman spectroscopy methods

NASA Astrophysics Data System (ADS)

Chen, Lei; Ma, Ning; Park, Yeonju; Jin, Sila; Hwang, Hoon; Jiang, Dayu; Jung, Young Mee

2018-05-01

In this paper, we introduced Raman spectroscopy techniques that were based on the traditional Fe3 + determination method with phenanthroline as a probe. Interestingly, surface-enhanced Raman spectroscopy (SERS)-based approach exhibited excellent sensitivities to phenanthroline. Different detection mechanisms were observed for the RR and SERS techniques, in which the RR intensity increased with increasing Fe3 + concentration due to the observation of the RR effect of the phenanthroline-Fe2 + complex, whereas the SERS intensity increased with decreasing Fe3 + concentration due to the observation of the SERS effect of the uncomplexed phenanthroline. More importantly, the determination sensitivity was substantially improved in the presence of a SERS-active substrate, giving a detection limit as low as 0.001 μg/mL, which is 20 times lower than the limit of the UV-vis and RR methods. Furthermore, the proposed SERS method was free from other ions interference and can be used quality and sensitivity for the determination of the city tap water.

LC-ESI-MS/MS on an ion trap for the determination of LSD, iso-LSD, nor-LSD and 2-oxo-3-hydroxy-LSD in blood, urine and vitreous humor.

PubMed

Favretto, Donata; Frison, Giampietro; Maietti, Sergio; Ferrara, Santo Davide

2007-07-01

A method has been developed for the simultaneous determination of lysergic acid diethylamide (LSD), its epimer iso-LSD, and its main metabolites nor-LSD and 2-oxo-3-hydroxy LSD in blood, urine, and, for the first time, vitreous humor samples. The method is based on liquid/liquid extraction and liquid chromatography-multiple mass spectrometry detection in an ion trap mass spectrometer, in positive ion electrospray ionization conditions. Five microliter of sample are injected and analysis time is 12 min. The method is specific, selective and sensitive, and achieves limits of quantification of 20 pg/ml for both LSD and nor-LSD in blood, urine, and vitreous humor. No significant interfering substance or ion suppression was identified for LSD, iso-LSD, and nor-LSD. The interassay reproducibilities for LSD at 20 pg/ml and 2 ng/ml in urine were 8.3 and 5.6%, respectively. Within-run precision using control samples at 20 pg/ml and 2 ng/ml was 6.9 and 3.9%. Mean recoveries of two concentrations spiked into drug free samples were in the range 60-107% in blood, 50-105% in urine, and 65-105% in vitreous humor. The method was successfully applied to the forensic determination of postmortem LSD levels in the biological fluids of a multi drug abuser; for the first time, LSD could be detected in vitreous humor.

Synthesis of a ratiometric fluorescent peptide sensor for the highly selective detection of Cd2+.

PubMed

Li, Yan; Li, Lianzhi; Pu, Xuewei; Ma, Guolin; Wang, Erqiong; Kong, Jinming; Liu, Zhipeng; Liu, Yangzhong

2012-06-15

A novel ratiometric fluorescent peptidyl chemosensor (Dansyl-Cys-Pro-Gly-Cys-Trp-NH(2), D-P5) for metal ions detection has been synthesized via Fmoc solid-phase peptide synthesis. The chemosensor exhibited a high selectivity for Cd(2+) over other metal ions including competitive transition and Group I and II metal ions in neutral pH. The fluorescence emission intensity of D-P5 was significantly enhanced in the presence of Cd(2+) by fluorescent resonance energy transfer (FRET) and chelation enhanced fluorescence (CHEF) effects. The binding stoichiometry, detection limit, binding affinity, reversibility and pH sensitivity of the sensor for Cd(2+) were investigated. Copyright © 2012 Elsevier Ltd. All rights reserved.

A reversible fluorescence "off-on-off" sensor for sequential detection of aluminum and acetate/fluoride ions.

PubMed

Gupta, Vinod Kumar; Mergu, Naveen; Kumawat, Lokesh Kumar; Singh, Ashok Kumar

2015-11-01

A new rhodamine functionalized fluorogenic Schiff base CS was synthesized and its colorimetric and fluorescence responses toward various metal ions were explored. The sensor exhibited highly selective and sensitive colorimetric and "off-on" fluorescence response towards Al(3+) in the presence of other competing metal ions. These spectral changes are large enough in the visible region of the spectrum and thus enable naked-eye detection. Studies proved that the formation of CS-Al(3+) complex is fully reversible and can sense to AcO(-)/F(-) via dissociation. The results revealed that the sensor provides fluorescence "off-on-off" strategy for the sequential detection of Al(3+) and AcO(-)/F(-). Copyright © 2015 Elsevier B.V. All rights reserved.

Highly selective "turn-on" fluorescent and colorimetric sensing of fluoride ion using 2-(2-hydroxyphenyl)-2,3-dihydroquinolin-4(1H)-one based on excited-state proton transfer.

PubMed

Kanagaraj, Kuppusamy; Pitchumani, Kasi

2014-01-01

A simple, highly selective and sensitive colorimetric system for the detection of fluoride ion in an aqueous medium has been developed using 2-(2-hydroxyphenyl)-2,3-dihydroquinolin-4(1H)-one. This system allows selective "turn-on" fluorescence detection of fluoride ion, which is found to be dependent upon guest basicity. An excited-state proton transfer is proposed to be the signaling mechanism, which is rationalized by DFT and TD-DFT calculations. The present sensor can also be applied to detect fluoride levels in real water samples. Copyright © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Novel Microwave-Induced Plasma Ionization Source for Ion Mobility Spectrometry

NASA Astrophysics Data System (ADS)

Dai, Jianxiong; Zhao, Zhongjun; Liang, Gaoling; Duan, Yixiang

2017-03-01

This work demonstrates the application of a novel microwave induced plasma ionization (MIPI) source to ion mobility spectrometry (IMS). The MIPI source, called Surfatron, is composed of a copper cavity and a hollow quartz discharge tube. The ion mobility spectrum of synthetics air has a main peak with reduced mobility of 2.14 cm2V-1s-1 for positive ion mode and 2.29 cm2V-1s-1 for negative ion mode. The relative standard deviations (RSD) are 0.7% and 1.2% for positive and negative ion mode, respectively. The total ion current measured was more than 3.5 nA, which is much higher than that of the conventional 63Ni source. This indicates that a better signal-to-noise ratio (SNR) can be acquired from the MIPI source. The SNR was 110 in the analysis of 500 pptv methyl tert-butyl ether (MTBE), resulting in the limit of detection (SNR = 3) of 14 pptv. The linear range covers close to 2.5 orders of magnitude in the detection of triethylamine with a concentration range from 500 pptv to 80 ppbv. Finally, this new MIPI-IMS was used to detect some volatile organic compounds, which demonstrated that the MIPI-IMS has great potential in monitoring pollutants in air.

Chemical enhancement of surface deposition

DOEpatents

Patch, Keith D.; Morgan, Dean T.

1997-07-29

A method and apparatus for increasing the deposition of ions onto a surface, such as the adsorption of uranium ions on the detecting surface of a radionuclide detector. The method includes the step of exposing the surface to a complexing agent, such as a phosphate ion solution, which has an affinity for the dissolved species to be deposited on the surface. This provides, for example, enhanced sensitivity of the radionuclide detector.

Single molecule fluorescence imaging as a technique for barium tagging in neutrinoless double beta decay

NASA Astrophysics Data System (ADS)

Jones, B. J. P.; McDonald, A. D.; Nygren, D. R.

2016-12-01

Background rejection is key to success for future neutrinoless double beta decay experiments. To achieve sensitivity to effective Majorana lifetimes of ~ 1028 years, backgrounds must be controlled to better than 0.1 count per ton per year, beyond the reach of any present technology. In this paper we propose a new method to identify the birth of the barium daughter ion in the neutrinoless double beta decay of 136Xe. The method adapts Single Molecule Fluorescent Imaging, a technique from biochemistry research with demonstrated single ion sensitivity. We explore possible SMFI dyes suitable for the problem of barium ion detection in high pressure xenon gas, and develop a fiber-coupled sensing system with which we can detect the presence of bulk Ba++ ions remotely. We show that our sensor produces signal-to-background ratios as high as 85 in response to Ba++ ions when operated in aqueous solution. We then describe the next stage of this R&D program, which will be to demonstrate chelation and fluorescence in xenon gas. If a successful barium ion tag can be developed using SMFI adapted for high pressure xenon gas detectors, the first essentially zero background, ton-scale neutrinoless double beta decay technology could be realized.

Effect of capping agent on selectivity and sensitivity of CdTe quantum dots optical sensor for detection of mercury ions

NASA Astrophysics Data System (ADS)

Labeb, Mohmed; Sakr, Abdel-Hamed; Soliman, Moataz; Abdel-Fettah, Tarek M.; Ebrahim, Shaker

2018-05-01

Cadmium telluride (CdTe) quantum dots (QDs) were prepared from an aqueous solution containing CdCl2 and Te precursor in the presence of thioglycolic acid (TGA) or L-cysteine as capping agents. Two optical sensors have been developed for Hg2+ ions with very low concentration in the range of nanomolar (nM) or picomolar (pM) depending on the type of capping agents and based on photoluminescence (PL) quenching of CdTe QDs. It was observed that low concentrations of Hg2+ ions quench the fluorescence spectra of CdTe QDs and TGA capped CdTe QDs exhibited a linear response to Hg2+ ions in the concentration range from 1.25 to 10 nM. Moreover, it was found that L-cysteine capped CdTe QDs optical sensor with a sensitivity of 6 × 109 M-1, exhibited a linear coefficient of 0.99 and showed a detection limit of 2.7 pM in range from 5 to 25 pM of Hg2+ ions was achieved. In contrast to the significant response that was observed for Hg2+, a weak signal response was noted upon the addition of other metal ions indicating an excellent selectivity of CdTe QDs towards Hg2+.

Breaking through the false coincidence barrier in electron–ion coincidence experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Osborn, David L.; Hayden, Carl C.; Hemberger, Patrick

Photoelectron Photoion Coincidence (PEPICO) spectroscopy holds the promise of a universal, isomer-selective, and sensitive analytical technique for time-resolved quantitative analysis of bimolecular chemical reactions. Unfortunately, its low dynamic range of ~10 3 has largely precluded its use for this purpose, where a dynamic range of at least 10 5 is generally required. This limitation is due to the false coincidence background common to all coincidence experiments, especially at high count rates. Electron/ion pairs emanating from separate ionization events but arriving within the ion time of flight (TOF) range of interest constitute the false coincidence background. Although this background has uniformmore » intensity at every m/z value, the Poisson scatter in the false coincidence background obscures small signals. In this paper, temporal ion deflection coupled with a position-sensitive ion detector enables suppression of the false coincidence background, increasing the dynamic range in the PEPICO TOF mass spectrum by 2–3 orders of magnitude. The ions experience a time-dependent electric deflection field at a well-defined fraction of their time of flight. This deflection defines an m/z- and ionization-time dependent ion impact position for true coincidences, whereas false coincidences appear randomly outside this region and can be efficiently suppressed. When cold argon clusters are ionized, false coincidence suppression allows us to observe species up to Ar 9 +, whereas Ar 4 + is the largest observable cluster under traditional operation. As a result, this advance provides mass-selected photoelectron spectra for fast, high sensitivity quantitative analysis of reacting systems.« less

Breaking through the false coincidence barrier in electron–ion coincidence experiments

DOE PAGES

Osborn, David L.; Hayden, Carl C.; Hemberger, Patrick; ...

2016-10-31

Photoelectron Photoion Coincidence (PEPICO) spectroscopy holds the promise of a universal, isomer-selective, and sensitive analytical technique for time-resolved quantitative analysis of bimolecular chemical reactions. Unfortunately, its low dynamic range of ~10 3 has largely precluded its use for this purpose, where a dynamic range of at least 10 5 is generally required. This limitation is due to the false coincidence background common to all coincidence experiments, especially at high count rates. Electron/ion pairs emanating from separate ionization events but arriving within the ion time of flight (TOF) range of interest constitute the false coincidence background. Although this background has uniformmore » intensity at every m/z value, the Poisson scatter in the false coincidence background obscures small signals. In this paper, temporal ion deflection coupled with a position-sensitive ion detector enables suppression of the false coincidence background, increasing the dynamic range in the PEPICO TOF mass spectrum by 2–3 orders of magnitude. The ions experience a time-dependent electric deflection field at a well-defined fraction of their time of flight. This deflection defines an m/z- and ionization-time dependent ion impact position for true coincidences, whereas false coincidences appear randomly outside this region and can be efficiently suppressed. When cold argon clusters are ionized, false coincidence suppression allows us to observe species up to Ar 9 +, whereas Ar 4 + is the largest observable cluster under traditional operation. As a result, this advance provides mass-selected photoelectron spectra for fast, high sensitivity quantitative analysis of reacting systems.« less

A novel fluorescent probe (dtpa-bis(cytosine)) for detection of Eu(III) in rare earth metal ions.

PubMed

Yang, Fan; Ren, Peipei; Liu, Guanhong; Song, Youtao; Bu, Naishun; Wang, Jun

2018-03-15

In this paper, a novel fluorescent probe, dtpa-bis(cytosine), was designed and synthesized for detecting europium (Eu 3+ ) ion. Upon addition of Eu 3+ ions into the dtpa-bis(cytosine) solution, the fluorescence intensity can strongly be enhanced. Conversely, adding other rare earth metal ions, such as Y 3+ , Ce 3+ , Pr 3+ , Nd 3+ , Sm 3+ , Gd 3+ , Tb 3+ , Dy 3+ , Ho 3+ , Er 3+ , Yb 3+ and Lu 3+ , into dtpa-bis(cytosine) solution, the fluorescence intensity is decreased slightly. Some parameters affecting the fluorescence intensity of dtpa-bis(cytosine) solution in the presence of Eu 3+ ions were investigated, including solution pH value, Eu 3+ ion concentration and interfering substances. The detection mechanism of Eu 3+ ion using dtpa-bis(cytosine) as fluorescent probe was proposed. Under optimum conditions, the fluorescence emission intensities of Eu III -dtpa-bis(cytosine) at 375nm in the concentration range of 0.50×10 -5 mol∙L -1 -5.00×10 -5 mol∙L -1 of Eu 3+ ion display a better linear relationship. The limit of detection (LOD) was determined as 8.65×10 -7 mol∙L -1 and the corresponding correlation coefficient (R 2 ) of the linear equation is 0.9807. It is wished that the proposed method could be applied for sensitively and selectively detecting Eu 3+ ion. Copyright © 2017 Elsevier B.V. All rights reserved.

Highly charged ion secondary ion mass spectroscopy

DOEpatents

Hamza, Alex V.; Schenkel, Thomas; Barnes, Alan V.; Schneider, Dieter H.

2001-01-01

A secondary ion mass spectrometer using slow, highly charged ions produced in an electron beam ion trap permits ultra-sensitive surface analysis and high spatial resolution simultaneously. The spectrometer comprises an ion source producing a primary ion beam of highly charged ions that are directed at a target surface, a mass analyzer, and a microchannel plate detector of secondary ions that are sputtered from the target surface after interaction with the primary beam. The unusually high secondary ion yield permits the use of coincidence counting, in which the secondary ion stops are detected in coincidence with a particular secondary ion. The association of specific molecular species can be correlated. The unique multiple secondary nature of the highly charged ion interaction enables this new analytical technique.

Ultrasensitive detection of target analyte-induced aggregation of gold nanoparticles using laser-induced nanoparticle Rayleigh scattering.

PubMed

Lin, Jia-Hui; Tseng, Wei-Lung

2015-01-01

Detection of salt- and analyte-induced aggregation of gold nanoparticles (AuNPs) mostly relies on costly and bulky analytical instruments. To response this drawback, a portable, miniaturized, sensitive, and cost-effective detection technique is urgently required for rapid field detection and monitoring of target analyte via the use of AuNP-based sensor. This study combined a miniaturized spectrometer with a 532-nm laser to develop a laser-induced Rayleigh scattering technique, allowing the sensitive and selective detection of Rayleigh scattering from the aggregated AuNPs. Three AuNP-based sensing systems, including salt-, thiol- and metal ion-induced aggregation of the AuNPs, were performed to examine the sensitivity of laser-induced Rayleigh scattering technique. Salt-, thiol-, and metal ion-promoted NP aggregation were exemplified by the use of aptamer-adsorbed, fluorosurfactant-stabilized, and gallic acid-capped AuNPs for probing K(+), S-adenosylhomocysteine hydrolase-induced hydrolysis of S-adenosylhomocysteine, and Pb(2+), in sequence. Compared to the reported methods for monitoring the aggregated AuNPs, the proposed system provided distinct advantages of sensitivity. Laser-induced Rayleigh scattering technique was improved to be convenient, cheap, and portable by replacing a diode laser and a miniaturized spectrometer with a laser pointer and a smart-phone. Using this smart-phone-based detection platform, we can determine whether or not the Pb(2+) concentration exceed the maximum allowable level of Pb(2+) in drinking water. Copyright © 2014 Elsevier B.V. All rights reserved.

A SERS biosensor with magnetic substrate CoFe2O4@Ag for sensitive detection of Hg2+

NASA Astrophysics Data System (ADS)

Yang, Xia; He, Yi; Wang, Xueling; Yuan, Ruo

2017-09-01

Mercuric ion (Hg2+) is one toxic metal ion existed in aquatic ecosystems which would seriously damage human central nervous system and other organs. So developing an approach to sensitively detect Hg2+ in our living environment is urgent and important. In this work, a novel surface enhancement Raman spectrum(SERS) sensor is fabricated for high selective and ultrasensitive detection of Hg2+ in aqueous solution, based on a stable thymine-Hg2+-thymine (T-Hg2+-T) structure and the π-π interaction between single-stranded DNA (ssDNA) and single walled carbon nanotubes (SWCNTs). Herein, SWCNTs act as Raman labels to produce characteristic Raman peaks which can be a beacon to quantitative detect Hg2+. In the presence of Hg2+, the ssDNA can capture Hg2+ forming T-Hg2+-T structure, which makes SWCNTs leave the hot spots of the SERS-based biosensor. With this design, the Raman intensity of SWCNTs decreased with the increasing concentration of Hg2+. At the same time, CoFe2O4@Ag as active SERS substrates can effectively enhance sensitivity and uniformity of the biosensor through aggregation by magnet. Under optimal conditions, this proposed biosensor can detect Hg2+ at a range from 1 pM to 100 nM with a detection limit of 0.84 pM. With the advantages of good sensitivity, selectivity, simplicity and rapidity, the biosensor is potentially suitable for monitoring of Hg2+ in environmental applications.

Single-ion adsorption and switching in carbon nanotubes

DOE PAGES

Bushmaker, Adam W.; Oklejas, Vanessa; Walker, Don; ...

2016-01-25

Single-ion detection has, for many years, been the domain of large devices such as the Geiger counter, and studies on interactions of ionized gasses with materials have been limited to large systems. To date, there have been no reports on single gaseous ion interaction with microelectronic devices, and single neutral atom detection techniques have shown only small, barely detectable responses. Here we report the observation of single gaseous ion adsorption on individual carbon nanotubes (CNTs), which, because of the severely restricted one-dimensional current path, experience discrete, quantized resistance increases of over two orders of magnitude. Only positive ions cause changes,more » by the mechanism of ion potentialinduced carrier depletion, which is supported by density functional and Landauer transport theory. Lastly, our observations reveal a new single-ion/CNT heterostructure with novel electronic properties, and demonstrate that as electronics are ultimately scaled towards the one-dimensional limit, atomic-scale effects become increasingly important.« less

Plasma Ion Sources for Atmospheric Pressure Ionization Mass Spectrometry.

NASA Astrophysics Data System (ADS)

Zhao, Jian-Guo

1994-01-01

Atmospheric pressure ionization (API) sources using direct-current (DC) and radio-frequency (RF) plasma have been developed in this thesis work. These ion sources can provide stable discharge currents of ~ 1 mA, 2-3 orders of magnitude larger than that of the corona discharge, a widely used API source. The plasmas can be generated and maintained in 1 atm of various buffer gases by applying -500 to -1000 V (DC plasma) or 1-15 W with a frequency of 165 kHz (RF plasma) on the needle electrode. These ion sources have been used with liquid injection to detect various organic compounds of pharmaceutical, biotechnological and environmental interest. Key features of these ion sources include soft ionization with the protonated molecule as the largest peak, and superb sensitivity with detection limits in the low picogram or femtomole range and a linear dynamic range over ~4 orders of magnitude. The RF plasma has advantages over the DC plasma in its ability to operate in various buffer gases and to produce a more stable plasma. Factors influencing the performance of the ion sources have been studied, including RF power level, liquid flow rate, chamber temperature, solvent composition, and voltage affecting the collision induced dissociation (CID). Ionization of hydrocarbons by the RF plasma API source was also studied. Soft ionization is generally produced. To obtain high sensitivity, the ion source must be very dry and the needle-to-orifice distance must be small. Nitric oxide was used to enhance the sensitivity. The RF plasma source was then used for the analysis of hydrocarbons in auto emissions. Comparisons between the corona discharge and the RF plasma have been made in terms of discharge current, ion residence time, and the ion source model. The RF plasma source provides larger linear dynamic range and higher sensitivity than the corona discharge, due to its much larger discharge current. The RF plasma was also observed to provide longer ion residence times and was not limited by space-charge effect as in the corona source.

Silicon chip integrated photonic sensors for biological and chemical sensing

NASA Astrophysics Data System (ADS)

Chakravarty, Swapnajit; Zou, Yi; Yan, Hai; Tang, Naimei; Chen, Ray T.

2016-03-01

We experimentally demonstrate applications of photonic crystal waveguide based devices for on-chip optical absorption spectroscopy for the detection of chemical warfare simulant, triethylphosphate as well as applications with photonic crystal microcavity devices in the detection of biomarkers for pancreatic cancer in patient serum and cadmium metal ions in heavy metal pollution sensing. At mid-infrared wavelengths, we experimentally demonstrate the higher sensitivity of photonic crystal based structures compared to other nanophotonic devices such as strip and slot waveguides with detection down to 10ppm triethylphosphate. We also detected 5ppb (parts per billion) of cadmium metal ions in water at near-infrared wavelengths using established techniques for the detection of specific probe-target biomarker conjugation chemistries.

Hand-Held Devices Detect Explosives and Chemical Agents

NASA Technical Reports Server (NTRS)

2010-01-01

Ion Applications Inc., of West Palm Beach, Florida, partnered with Ames Research Center through Small Business Innovation Research (SBIR) agreements to develop a miniature version ion mobility spectrometer (IMS). While NASA was interested in the instrument for detecting chemicals during exploration of distant planets, moons, and comets, the company has incorporated the technology into a commercial hand-held IMS device for use by the military and other public safety organizations. Capable of detecting and identifying molecules with part-per-billion sensitivity, the technology now provides soldiers with portable explosives and chemical warfare agent detection. The device is also being adapted for detecting drugs and is employed in industrial processes such as semiconductor manufacturing.

Determination of fluspirilene in human plasma by liquid chromatography-tandem mass spectrometry with electrospray ionisation.

PubMed

Swart, K J; Sutherland, F C; van Essen, G H; Hundt, H K; Hundt, A F

1998-12-18

An ultra-sensitive method for the determination of fluspirilene in plasma was established, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. The samples were extracted with hexane/isoamyl alcohol, separated on a Phenomenex Luna C18 5 mu 150 x 2.1 mm column with a mobile phase consisting of methanol-water-acetic acid (600:400:1) at a flow-rate of 0.3 ml/min. Detection was achieved by a Finnigan Matt mass spectrometer (LCQ) at unit resolution in full scan mode scanning the product ion spectrum from m/z 130-500 and monitoring the transition of the protonated molecular ion at m/z 476.2, to the sum of the largest product ions m/z 371, 342 and 274 (MS-MS). Electrospray ionisation was used for ion production. The mean recovery for fluspirilene was 90% with a lower limit of quantification of 21.50 pg/ml using 1 ml plasma for extraction. This is the first chromatographic method described for the determination of fluspirilene in plasma that is accurate and sensitive enough to be used in pharmacokinetic studies.

Colloidal GdVO4:Eu3+@SiO2 nanocrystals for highly selective and sensitive detection of Cu2+ ions

NASA Astrophysics Data System (ADS)

Liang, Yanjie; Noh, Hyeon Mi; Park, Sung Heum; Choi, Byung Chun; Jeong, Jung Hyun

2018-03-01

Nowadays, in view of health and safety demands, the controlled design of selective and sensitive sensors for Cu2+ detection is of considerable importance. Therefore, we construct herein core-shell colloidal GdVO4:Eu3+@SiO2 nanocrystals (NCs) as optical sensor for the detection of Cu2+, which were synthesized by a facile hydrothermal reaction and encapsulated with a uniform layer of ultrathin silica through a sol-gel strategy. The NCs present strong red emission due to energy transfer from VO43- groups to Eu3+ when exciting with ultraviolet (UV) light. This intense red emission from Eu3+ could be selectively quenched in the presence of Cu2+ in comparison to other metal ions and the limit of detection is as low as 80 nM in aqueous solution. It is revealed that the spectral overlap between the emission band of NCs and the absorption of Cu2+ accounts for this intriguing luminescence behavior. The detection ability is highly reversible by the addition of ethylenediaminetetraacetic acid (EDTA) with the recovery of almost 100% of the original luminescence. The luminescence quenching and recovery processes can be performed repeatedly with good sensing ability. These remarkable performances allow the colloidal GdVO4:Eu3+@SiO2 NCs a promising fluorescence chemosensor for detecting Cu2+ ions in aqueous solution.

Computational simulation of biomolecules transport with multi-physics near microchannel surface for development of biomolecules-detection devices.

PubMed

Suzuki, Yuma; Shimizu, Tetsuhide; Yang, Ming

2017-01-01

The quantitative evaluation of the biomolecules transport with multi-physics in nano/micro scale is demanded in order to optimize the design of microfluidics device for the biomolecules detection with high detection sensitivity and rapid diagnosis. This paper aimed to investigate the effectivity of the computational simulation using the numerical model of the biomolecules transport with multi-physics near a microchannel surface on the development of biomolecules-detection devices. The biomolecules transport with fluid drag force, electric double layer (EDL) force, and van der Waals force was modeled by Newtonian Equation of motion. The model validity was verified in the influence of ion strength and flow velocity on biomolecules distribution near the surface compared with experimental results of previous studies. The influence of acting forces on its distribution near the surface was investigated by the simulation. The trend of its distribution to ion strength and flow velocity was agreement with the experimental result by the combination of all acting forces. Furthermore, EDL force dominantly influenced its distribution near its surface compared with fluid drag force except for the case of high velocity and low ion strength. The knowledges from the simulation might be useful for the design of biomolecules-detection devices and the simulation can be expected to be applied on its development as the design tool for high detection sensitivity and rapid diagnosis in the future.

Fluorescence spectroscopy of trapped molecular ions

NASA Astrophysics Data System (ADS)

Wright, Kenneth Charles

This thesis describes the development of a unique instrument capable of detecting fluorescence emission from large gas phase molecular ions trapped in a three-dimensional quadrupole ion trap. The hypothesis that has formed the basis of this work is the belief that fluorescence spectroscopy can be combined with ion trap mass spectrometry to probe the structure of gas phase molecular ions. The ion trap provides a rarefied environment where fluorescence experiments can be conducted without interference from solvent molecules or impurities. Although fluorescence was not detected during preliminary experiments, two significant experimental challenges associated with detecting the gas phase fluorescence of ions were discovered. First, gas phase ions were vulnerable to photodissociation and low laser powers were necessary to avoid photodissociation. Since fluorescence emission is directly proportional to laser intensity, a lower laser power limits the fluorescence signal. Second, the fluorescence emission was not significantly Stokes shifted from the excitation. The lack of Stokes shift meant the small fluorescence signal must be detected in the presence of a large amount of background scatter generated by the excitation. Initially, this background was seven orders of magnitude higher than the analytical signal ultimately detected. A specially designed fiber optic probe was inserted between the electrodes of the ion trap to stop light scattered off the outside surfaces of the trap from reaching the detector. The inside surfaces of the ion trap were coated black to further reduce the amount of scattered light collected. These innovations helped reduced the background by six orders of magnitude and fluorescence emission from rhodamine-6G was detected. Pulse counting experiments were used to optimize fluorescence detection. The effects of trapping level, laser power, and irradiation time were investigated and optimized. The instrument developed in this work not only allows for the detection of fluorescent photons, but the sensitivity is high enough for the light to be dispersed and an emission spectrum recorded. The emission spectra of rhodamine-6G and 5-carboxyrhodamine-6G ions reported in this thesis represent the first spectra recorded from large molecular ions confined in a quadrupole ion trap. Finally, anti-Stokes fluorescence from rhodamine-6G was also detected.

Photosensitivity enhancement of PLZT ceramics by positive ion implantation

DOEpatents

Peercy, P.S.; Land, C.E.

1980-06-13

The photosensitivity of lead lanthanum zirconate titanate (PLZT) ceramic material used in high resolution, high contrast, and non-volatile photoferroelectric image storage and display devices is enhanced significantly by positive ion implantation of the PLZT near its surface. Ions that are implanted include H/sup +/, He/sup +/, Ar/sup +/, and a preferred co-implant of Ar/sup +/ and Ne/sup +/. The positive ion implantation advantageously serves to shift the band gap energy threshold of the PLZT material from near-uv light to visible blue light. As a result, photosensitivity enhancement is such that the positive ion implanted PLZT plate is sensitive even to sunlight and conventional room lighting, such as fluorescent and incandescent light sources. The method disclosed includes exposing the PLZT plate to these positive ions of sufficient density and with sufficient energy to provide an image. The PLZT material may have a lanthanum content ranging from 5 to 10%; a lead zirconate content ranging from 62 to 70 mole %; and a lead titanate content ranging from 38 to 30%. The region of ion implantation is in a range from 0.1 to 2 microns below the surface of the PLZT plate. Density of ions is in the range from 1 x 10/sup 12/ to 1 x 10/sup 17/ ions/cm/sup 2/ and having an energy in the range from 100 to 500 keV.

First signal from a broadband cryogenic preamplifier cooled by circulating liquid nitrogen in a 7 T Fourier transform ion cyclotron resonance mass spectrometer.

PubMed

Choi, Myoung Choul; Lee, Jeong Min; Lee, Se Gyu; Choi, Sang Hwan; Choi, Yeon Suk; Lee, Kyung Jae; Kim, SeungYong; Kim, Hyun Sik; Stahl, Stefan

2012-12-18

Despite the outstanding performance of Fourier transform ion cyclotron/mass spectrometry (FTICR/MS), the complexity of the cellular proteome or natural compounds presents considerable challenges. Sensitivity is a key performance parameter of a FTICR mass spectrometer. By improving this parameter, the dynamic range of the instrument can be increased to improve the detection signal of low-abundance compounds or fragment ion peaks. In order to improve sensitivity, a cryogenic detection system was developed by the KBSI (Korean Basic Science Institute) in collaboration with Stahl-Electronics (Mettenheim, Germany). A simple, efficient liquid circulation cooling system was designed and a cryogenic preamplifier implemented inside a FTICR mass spectrometer. This cooling system circulates a cryoliquid from a Dewar to the "liquid circulation unit" through a CF flange to cool a copper block and a cryopreamplifier; the cooling medium is subsequently exhausted into the air. The cryopreamplifier can be operated over a very wide temperature range, from room temperature to low temperature environments (4.2 K). First, ion signals detected by the cryopreamplifier using a circulating liquid nitrogen cooling system were observed and showed a signal-to-noise ratio (S/N) about 130% better than that obtained at room temperature.

Iron oxide nanomatrix facilitating metal ionization in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Obena, Rofeamor P; Lin, Po-Chiao; Lu, Ying-Wei; Li, I-Che; del Mundo, Florian; Arco, Susan dR; Nuesca, Guillermo M; Lin, Chung-Chen; Chen, Yu-Ju

2011-12-15

The significance and epidemiological effects of metals to life necessitate the development of direct, efficient, and rapid method of analysis. Taking advantage of its simple, fast, and high-throughput features, we present a novel approach to metal ion detection by matrix-functionalized magnetic nanoparticle (matrix@MNP)-assisted MALDI-MS. Utilizing 21 biologically and environmentally relevant metal ion solutions, the performance of core and matrix@MNP against conventional matrixes in MALDI-MS and laser desorption ionization (LDI) MS were systemically tested to evaluate the versatility of matrix@MNP as ionization element. The matrix@MNPs provided 20- to >100-fold enhancement on detection sensitivity of metal ions and unambiguous identification through characteristic isotope patterns and accurate mass (<5 ppm), which may be attributed to its multifunctional role as metal chelator, preconcentrator, absorber, and reservoir of energy. Together with the comparison on the ionization behaviors of various metals having different ionization potentials (IP), we formulated a metal ionization mechanism model, alluding to the role of exciton pooling in matrix@MNP-assisted MALDI-MS. Moreover, the detection of Cu in spiked tap water demonstrated the practicability of this new approach as an efficient and direct alternative tool for fast, sensitive, and accurate determination of trace metal ions in real samples.

Sensitive fluorescence detection of mercury(ii) in aqueous solution by the fluorescence quenching effect of MoS2 with DNA functionalized carbon dots.

PubMed

Srinivasan, K; Subramanian, K; Murugan, K; Dinakaran, K

2016-10-24

A rapid and sensitive fluorescent sensor based on the MoS 2 nanosheet/DNA/carbon dot nanoassembly has been developed towards the detection of mercury(ii) present in environmental samples. Bio-carbon dots (CDs) having strong fluorescence maxima at 451 nm were synthesized via one-step treatment with honey under low temperature carbonization. These CDs were nearly spherical with good size distribution and excellent monodispersity, and the average sizes of CD were around 2-4 nm as evidenced from transmission electron microscopy. The conjugation of DNA strands on the surface of the carbon dots provided an efficient fluorescent probe. The fluorescence of the MoS 2 nanosheet/DNA/carbon dot nanoassembly enhanced gradually with the increase in the concentration of Hg 2+ ions and the detection limit was found to be 1.02 nM. Furthermore, the fluorescence intensity was found to be linear with the concentration of Hg 2+ ions in the range from 0 to 10 nM and their respective coefficient of determination was found to be 0.93676 and 0.98178. The present MoS 2 nanosheet/DNA/carbon dot nanoassembly is highly selective toward Hg 2+ ions over a wide range of metal ions tested.

Selectivity improvement of positive photoionization ion mobility spectrometry for rapid detection of organophosphorus pesticides by switching dopant concentration.

PubMed

Zhou, Qinghua; Li, Jia; Wang, Bin; Wang, Shuang; Li, Haiyang; Chen, Jinyuan

2018-01-01

Ion mobility spectrometry (IMS) opened a potential avenue for the rapid detection of organophosphorus pesticides (OPPs), though an improved selectivity of stand-alone IMS was still in high demand. In this study, a stand-alone positive photoionization ion mobility spectrometry (PP-IMS) apparatus was constructed for the rapid detection of OPPs with acetone as dopant. The photoionization of acetone molecules was induced by the ultraviolet irradiation to produce the reactant ions (Ac) 2 H + , which were employed to ionize the OPPs including fenthion, imidan, phosphamidon, dursban, dimethoate and isocarbophos via the proton transfer reaction. Due to the difference in proton affinity, the tested OPPs exhibited the different dopant-dependent manners. Based on this observation, the switching of dopant concentration was implemented to improve the selectivity of PP-IMS for OPPs detection. For instance, a mixture of fenthion, dursban and dimethoate was tested. By switching the concentration of doped acetone from 0.07 to 2.33 to 19.94mgL -1 , the ion peaks of fenthion and dursban were inhibited in succession, achieving the selective detection of dimethoate at last. In addition, another mixture of imidan and phosphamidon was initially detected by PP-IMS with a dose of 0.07mgL -1 acetone, indicating that their ion peaks were severely overlapped; when the concentration of doped acetone was switched to 19.94mgL -1 , the inhibition of imidan signals promised the accurate identification of phosphamidon in mixture. Finally, the PP-IMS in combination of switching dopant concentration was applied to detect the mixed fenthion, dursban and dimethoate in Chinese cabbage, demonstrating the applicability of proposed method to real samples. Copyright © 2017. Published by Elsevier B.V.

Multifunctional Nanomaterials Utilizing Hybridization Chain Reaction for Molecular Diagnostics and Bioanalytical Applications

NASA Astrophysics Data System (ADS)

Rana, Md. Muhit

DNA nanotechnology has shown great promise in molecular diagnostic, bioanalytical and biomedical applications. The great challenge of detecting target analytes, biomarkers and small molecules, in molecular diagnostics is low yield sensitivity. To address this challenge, different nanomaterials have been used for a long time and to date there is no such cost-effective bioanalytical technique which can detect these target biomarkers (DNA, RNA, circulating DNA/miRNA) or environmental heavy metal ions (Hg2+ and Ag+) in a cost-effective and efficient manner. Herein, we initially discuss two possible bioanalytical detection methods- a) colorimetric and b) fluorometric assays which are very popular nowadays due to their distinctive spectroscopic properties. Finally, we report the promising colorimetric assay using a novel DNA based amplification strategy know as hybridization chain reaction (HCR) for potential application in the visual detection of low copies of biomarkers (miRNAs as little as 20 femtomole in an RNA pool and cell extracts in seven different combinations and Ebola virus DNA as low as 400 attomoles in liquid biopsy mimics in sixteen different combinations), environmental and biological heavy metal ions (mercury and silver concentrations as low as 10 pM in water, soil and urine samples) and also successfully applied to a molecular logic gate operation to distinguish OR and AND logic gates. No results showed any false-positive or false-negative information. On the other hand, we also discuss the future possibilities of HCR amplification technology, which is very promising for fluorometric bioanalysis. The HCR based nanoprobe technology has numerous remarkable advantages over other methods. It is re-programmable, simple, inexpensive, easy to assemble and operate and can be performed with visual and spectroscopic read-outs upon recognition of the target analytes. This rapid, specific and sensitive approach for biomarkers and heavy metal ion detection generates an on-site signal while eliminating the use of sophisticated high-maintenance instrumentation. We demonstrate that this state-of-the-art technology and methodology can potentially serve as an alternative approach to detect novel disease biomarkers, small molecules and inorganic compounds. This approach can be combined with the current existing methods for real-time point-of-care molecular diagnostics and is significant for preclinical or clinical studies.

Ultrananocrystalline Diamond Membranes for Detection of High-Mass Proteins

NASA Astrophysics Data System (ADS)

Kim, H.; Park, J.; Aksamija, Z.; Arbulu, M.; Blick, R. H.

2016-12-01

Mechanical resonators realized on the nanoscale by now offer applications in mass sensing of biomolecules with extraordinary sensitivity. The general idea is that perfect mechanical mass sensors should be of extremely small size to achieve zepto- or yoctogram sensitivity in weighing single molecules similar to a classical scale. However, the small effective size and long response time for weighing biomolecules with a cantilever restricts their usefulness as a high-throughput method. Commercial mass spectrometry (MS), on the other hand, such as electrospray ionization and matrix-assisted laser desorption and ionization (MALDI) time of flight (TOF) and their charge-amplifying detectors are the gold standards to which nanomechanical resonators have to live up to. These two methods rely on the ionization and acceleration of biomolecules and the following ion detection after a mass selection step, such as TOF. The principle we describe here for ion detection is based on the conversion of kinetic energy of the biomolecules into thermal excitation of chemical vapor deposition diamond nanomembranes via phonons followed by phonon-mediated detection via field emission of thermally emitted electrons. We fabricate ultrathin diamond membranes with large lateral dimensions for MALDI TOF MS of high-mass proteins. These diamond membranes are realized by straightforward etching methods based on semiconductor processing. With a minimal thickness of 100 nm and cross sections of up to 400 ×400 μ m2 , the membranes offer extreme aspect ratios. Ion detection is demonstrated in MALDI TOF analysis over a broad range from insulin to albumin. The resulting data in detection show much enhanced resolution as compared to existing detectors, which can offer better sensitivity and overall performance in resolving protein masses.

Automatic detection of ECG cable interchange by analyzing both morphology and interlead relations.

PubMed

Han, Chengzong; Gregg, Richard E; Feild, Dirk Q; Babaeizadeh, Saeed

2014-01-01

ECG cable interchange can generate erroneous diagnoses. For algorithms detecting ECG cable interchange, high specificity is required to maintain a low total false positive rate because the prevalence of interchange is low. In this study, we propose and evaluate an improved algorithm for automatic detection and classification of ECG cable interchange. The algorithm was developed by using both ECG morphology information and redundancy information. ECG morphology features included QRS-T and P-wave amplitude, frontal axis and clockwise vector loop rotation. The redundancy features were derived based on the EASI™ lead system transformation. The classification was implemented using linear support vector machine. The development database came from multiple sources including both normal subjects and cardiac patients. An independent database was used to test the algorithm performance. Common cable interchanges were simulated by swapping either limb cables or precordial cables. For the whole validation database, the overall sensitivity and specificity for detecting precordial cable interchange were 56.5% and 99.9%, and the sensitivity and specificity for detecting limb cable interchange (excluding left arm-left leg interchange) were 93.8% and 99.9%. Defining precordial cable interchange or limb cable interchange as a single positive event, the total false positive rate was 0.7%. When the algorithm was designed for higher sensitivity, the sensitivity for detecting precordial cable interchange increased to 74.6% and the total false positive rate increased to 2.7%, while the sensitivity for detecting limb cable interchange was maintained at 93.8%. The low total false positive rate was maintained at 0.6% for the more abnormal subset of the validation database including only hypertrophy and infarction patients. The proposed algorithm can detect and classify ECG cable interchanges with high specificity and low total false positive rate, at the cost of decreased sensitivity for certain precordial cable interchanges. The algorithm could also be configured for higher sensitivity for different applications where a lower specificity can be tolerated. Copyright © 2014 Elsevier Inc. All rights reserved.

Source Apportionment of PM2.5 Mass and Optical Attenuation Over an Ecologically Sensitive Zone in Central India by Positive Matrix Factorization

NASA Astrophysics Data System (ADS)

Nirmalkar, J.; Raman, R. S.

2016-12-01

Ambient PM2.5 samples (N=366) were collected over an ecologically sensitive zone (Van Vihar National Park) in Bhopal, Central India for two years (01 January, 2012 to 31 December, 2013). Samples were collected using three co-located Mini-Vol® samplers on Teflon, Nylon, and Quartz filter substrates. The aerosol was then chemically characterized for water-soluble inorganic ions, elements, and carbon fractions (elemental carbon and organic carbon) using ion chromatography, ED-XRF, and thermal-optical EC/OC analyzer, respectively. The optical attenuation (at 370 nm and 800 nm) of PM2.5 aerosols was also determined by optical transmissometry (OT-21). The application of Positive matrix factorization (PMF) to a combination of PM2.5 mass, its ions, elements, carbon fractions, and optical attenuation and its outcomes will be discussed.

An ultra-sensitive Au nanoparticles functionalized DNA biosensor for electrochemical sensing of mercury ions.

PubMed

Zhang, Yanyan; Zhang, Cong; Ma, Rui; Du, Xin; Dong, Wenhao; Chen, Yuan; Chen, Qiang

2017-06-01

The present work describes an effective strategy to fabricate a highly sensitive and selective DNA-biosensor for the determination of mercury ions (Hg 2+ ). The DNA 1 was modified onto the surface of Au electrode by the interaction between sulfydryl group and Au electrode. DNA probe is complementary with DNA 1. In the presence of Hg 2+ , the electrochemical signal increases owing to that Hg 2+ -mediated thymine bases induce the conformation of DNA probe to change from line to hairpin and less DNA probes adsorb into DNA 1. Taking advantage of its reduction property, methylene blue is considered as the signal indicating molecule. For improving the sensitivity of the biosensor, Au nanoparticles (Au NPs) modified reporter DNA 3 is used to adsorb DNA 1. Electrochemical behaviors of the biosensor were evaluated by electrochemical impedance spectroscopy and cyclic voltammetry. Several important parameters which could affect the property of the biosensor were studied and optimized. Under the optimal conditions, the biosensor exhibits wide linear range, high sensitivity and low detection limit. Besides, it displays superior selectivity and excellent stability. The biosensor was also applied for water sample detection with satisfactory result. The novel strategy of fabricating biosensor provides a potential platform for fabricating a variety of metal ions biosensors. Copyright © 2017 Elsevier B.V. All rights reserved.

A Multifunctional Bimetallic Molecular Device for Ultrasensitive Detection, Naked-Eye Recognition, and Elimination of Cyanide Ions.

PubMed

Chow, Cheuk-Fai; Ho, Pui-Yu; Wong, Wing-Leung; Gong, Cheng-Bin

2015-09-07

A new bimetallic Fe(II) -Cu(II) complex was synthesized, characterized, and applied as a selective and sensitive sensor for cyanide detection in water. This complex is the first multifunctional device that can simultaneously detect cyanide ions in real water samples, amplify the colorimetric signal upon detection for naked-eye recognition at the parts-per-million (ppb) level, and convert the toxic cyanide ion into the much safer cyanate ion in situ. The mechanism of the bimetallic complex for high-selectivity recognition and signaling toward cyanide ions was investigated through a series of binding kinetics of the complex with different analytes, including CN(-) , SO4 (2-) , HCO3 (-) , HPO4 (2-) , N3 (-) , CH3 COO(-) , NCS(-) , NO3 (-) , and Cl(-) ions. In addition, the use of the indicator/catalyst displacement assay (ICDA) is demonstrated in the present system in which one metal center acts as a receptor and inhibitor and is bridged to another metal center that is responsible for signal transduction and catalysis, thus showing a versatile approach to the design of new multifunctional devices. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Composites Based on Conducting Polymers and Carbon Nanomaterials for Heavy Metal Ion Sensing (Review).

PubMed

Deshmukh, Megha A; Shirsat, Mahendra D; Ramanaviciene, Almira; Ramanavicius, Arunas

2018-07-04

Current review signifies recent trends and challenges in the development of electrochemical sensors based on organic conducting polymers (OCPs), carbon nanotubes (CNTs) and their composites for the determination of trace heavy metal ions in water are reviewed. OCPs and CNTs have some suitable properties, such as good electrical, mechanical, chemical and structural properties as well as environmental stability, etc. However, some of these materials still have significant limitations toward selective and sensitive detection of trace heavy metal ions. To overcome the limitations of these individual materials, OCPs/CNTs composites were developed. Application of OCPs/CNTs composite and their novel properties for the adsorption and detection of heavy metal ions outlined and discussed in this review.

Multi-mode acquisition (MMA): An MS/MS acquisition strategy for maximizing selectivity, specificity and sensitivity of DIA product ion spectra.

PubMed

Williams, Brad J; Ciavarini, Steve J; Devlin, Curt; Cohn, Steven M; Xie, Rong; Vissers, Johannes P C; Martin, LeRoy B; Caswell, Allen; Langridge, James I; Geromanos, Scott J

2016-08-01

In proteomics studies, it is generally accepted that depth of coverage and dynamic range is limited in data-directed acquisitions. The serial nature of the method limits both sensitivity and the number of precursor ions that can be sampled. To that end, a number of data-independent acquisition (DIA) strategies have been introduced with these methods, for the most part, immune to the sampling issue; nevertheless, some do have other limitations with respect to sensitivity. The major limitation with DIA approaches is interference, i.e., MS/MS spectra are highly chimeric and often incapable of being identified using conventional database search engines. Utilizing each available dimension of separation prior to ion detection, we present a new multi-mode acquisition (MMA) strategy multiplexing both narrowband and wideband DIA acquisitions in a single analytical workflow. The iterative nature of the MMA workflow limits the adverse effects of interference with minimal loss in sensitivity. Qualitative identification can be performed by selected ion chromatograms or conventional database search strategies. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Single ion hit detection set-up for the Zagreb ion microprobe

NASA Astrophysics Data System (ADS)

Smith, R. W.; Karlušić, M.; Jakšić, M.

2012-04-01

Irradiation of materials by heavy ions accelerated in MV tandem accelerators may lead to the production of latent ion tracks in many insulators and semiconductors. If irradiation is performed in a high resolution microprobe facility, ion tracks can be ordered by submicrometer positioning precision. However, full control of the ion track positioning can only be achieved by a reliable ion hit detection system that should provide a trigger signal irrespectively of the type and thickness of the material being irradiated. The most useful process that can be utilised for this purpose is emission of secondary electrons from the sample surface that follows the ion impact. The status report of the set-up presented here is based on the use of a channel electron multiplier (CEM) detector mounted on an interchangable sample holder that is inserted into the chamber in a close geometry along with the sample to be irradiated. The set-up has been tested at the Zagreb ion microprobe for different ions and energies, as well as different geometrical arrangements. For energies of heavy ions below 1 MeV/amu, results show that efficient (100%) control of ion impact can be achieved only for ions heavier than silicon. The successful use of the set-up is demonstrated by production of ordered single ion tracks in a polycarbonate film and by monitoring fluence during ion microbeam patterning of Foturan glass.

Modern Directions for Potentiometric Sensors

PubMed Central

Bakker, Eric; Chumbimuni-Torres, Karin

2009-01-01

This paper gives an overview of the newest developments of polymeric membrane ion-selective electrodes. A short essence of the underlying theory is given, emphasizing how the electromotive force may be used to assess binding constants of the ionophore, and how the selectivity and detection limit are related to the underlying membrane processes. The recent developments in lowering the detection limits of ISEs are described, including recent approaches of developing all solid state ISEs, and breakthroughs in detecting ultra-small quantities of ions at low concentrations. These developments have paved the way to use potentiometric sensors as in ultra-sensitive affinity bioanalysis in conjunction with nanoparticle labels. Recent results establish that potentiometry compares favorably to electrochemical stripping analysis. Other new developments with ion-selective electrodes are also described, including the concept of backside calibration potentiometry, controlled current coulometry, pulsed chronopotentiometry, and localized flash titration with ion-selective membranes to design sensors for the direct detection of total acidity without net sample perturbation. These developments have further opened the field for exciting new possibilities and applications. PMID:19890473

Ion mobility spectrometer using frequency-domain separation

DOEpatents

Martin, Stephen J.; Butler, Michael A.; Frye, Gregory C.; Schubert, W. Kent

1998-01-01

An apparatus and method is provided for separating and analyzing chemical species in an ion mobility spectrometer using a frequency-domain technique wherein the ions generated from the chemical species are selectively transported through an ion flow channel having a moving electrical potential therein. The moving electrical potential allows the ions to be selected according to ion mobility, with certain of the ions being transported to an ion detector and other of the ions being effectively discriminated against. The apparatus and method have applications for sensitive chemical detection and analysis for monitoring of exhaust gases, hazardous waste sites, industrial processes, aerospace systems, non-proliferation, and treaty verification. The apparatus can be formed as a microelectromechanical device (i.e. a micromachine).

Determination of hexabromocyclododecane by flowing atmospheric pressure afterglow mass spectrometry.

PubMed

Smoluch, Marek; Silberring, Jerzy; Reszke, Edward; Kuc, Joanna; Grochowalski, Adam

2014-10-01

The first application of a flowing atmospheric-pressure afterglow ion source for mass spectrometry (FAPA-MS) for the chemical characterization and determination of hexabromocyclododecane (HBCD) is presented. The samples of technical HBCD and expanded polystyrene foam (EPS) containing HBCD as a flame retardant were prepared by dissolving the appropriate solids in dichloromethane. The ionization of HBCD was achieved with a prototype FAPA source. The ions were detected in the negative-ion mode. The ions corresponding to a deprotonated HBCD species (m/z 640.7) as well as chlorine (m/z 676.8), nitrite (m/z 687.8) and nitric (m/z 703.8) adducts were observed in the spectra. The observed isotope pattern is characteristic for a compound containing six bromine atoms. This technique is an effective approach to detect HBCD, which is efficiently ionized in a liquid phase, resulting in high detection efficiency and sensitivity. Copyright © 2014 Elsevier B.V. All rights reserved.

Nickel-Cobalt Oxide Decorated Three-Dimensional Graphene as an Enzyme Mimic for Glucose and Calcium Detection.

PubMed

Wu, Meiyan; Meng, Shangjun; Wang, Qian; Si, Weili; Huang, Wei; Dong, Xiaochen

2015-09-30

Glucose and calcium ion play key roles in human bodies. The needlelike NiCo2O4 nanostructures are in situ deposited on three-dimensional graphene foam (3DGF) by a facile hydrothermal procedure. The structure and morphology of the hierarchical NiCo2O4/3DGF are characterized by scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. With the self-standing NiCo2O4/3DGF as electrochemical electrode, it can realize the high-sensitivity detections for glucose and calcium ion. The limit of detection can reach 0.38 and 4.45 μM, respectively. In addition, the electrochemical electrode presents excellent selectivity for glucose and calcium ion. This study demonstrates that NiCo2O4/3DGF is a unique and promising material for practical application in both glucose and calcium ion sensing.

Optimized separation and determination of methyl sulfone metabolites of polychlorinated biphenyls (PCBs) and p,p'-DDE in biota samples.

PubMed

Chu, Shaogang; Covaci, Adrian; Haraguchi, Koichi; Schepens, Paul

2002-12-01

An optimised method is described for the determination of 27 methyl sulfone polychlorobiphenyls (PCBs) and DDE in biota samples. Initially, the samples were extracted by hot Soxhlet and the methyl sulfones were separated by liquid/liquid extraction with concentrated sulfuric acid and back-extracted with hexane. The parameters of the back-extraction were studied and it was found that for a quantitative extraction of the methyl sulfones from the concentrated acid layer, a 50% dilution with cold water should be done. The hexane layer containing the methyl sulfones was further cleaned-up on basic silica (33% KOH) and Florisil. After concentration, the extract was analysed by gas chromatography-mass spectrometry (GC-MS) with electron capture negative ionisation (ECNI) in selected ion monitoring mode (SIM). It was shown that, for methyl sulfones, the ion formation was dependent on the chlorine substitution, position of the MeSO2-group and the ion source temperature. If the ion source temperature was higher than 200 degrees C, [M-CH3]- was the predominant ion for most methyl sulfones. Therefore, for increased sensitivity, quantitation of most congeners was done using [M-CH3]- ions instead of the molecular ion as used in previously reported methods. The method was validated for the determination of 26 tri- to hepta- 3- and 4-substituted MeSO2-PCBs and 3-MeSO2-DDE in animal and human tissues. Good sensitivity and selectivity of the method were obtained. Limits of detection (LODs) ranged from 0.06 to 0.10 ng g(-1) lipid weight. Average recoveries of individual congeners from vegetable oil spiked with individual standards (3.33 ng g(-1)) ranged from 73 to 112% with a mean value of 89%. The coefficients of variation ranged from 5.2 to 12.2%, which is within the acceptable range for environmental analyses.

Amperometric Sensor for Detection of Chloride Ions.

PubMed

Trnkova, Libuse; Adam, Vojtech; Hubalek, Jaromir; Babula, Petr; Kizek, Rene

2008-09-15

Chloride ion sensing is important in many fields such as clinical diagnosis, environmental monitoring and industrial applications. We have measured chloride ions at a carbon paste electrode (CPE) and at a CPE modified with solid AgNO₃, a solution of AgNO₃ and/or solid silver particles. Detection limits (3 S/N) for chloride ions were 100 μM, 100 μM and 10 μM for solid AgNO₃, solution of AgNO₃ and/or solid silver particles, respectively. The CPE modified with silver particles is the most sensitive to the presence chloride ions. After that we approached to the miniaturization of the whole electrochemical instrument. Measurements were carried out on miniaturized instrument consisting of a potentiostat with dimensions 35 × 166 × 125 mm, screen printed electrodes, a peristaltic pump and a PC with control software. Under the most suitable experimental conditions (Britton-Robinson buffer, pH 1.8 and working electrode potential 550 mV) we estimated the limit of detection (3 S/N) as 500 nM.

Sensing Using Rare-Earth-Doped Upconversion Nanoparticles

PubMed Central

Hao, Shuwei; Chen, Guanying; Yang, Chunhui

2013-01-01

Optical sensing plays an important role in theranostics due to its capability to detect hint biochemical entities or molecular targets as well as to precisely monitor specific fundamental psychological processes. Rare-earth (RE) doped upconversion nanoparticles (UCNPs) are promising for these endeavors due to their unique frequency converting capability; they emit efficient and sharp visible or ultraviolet (UV) luminescence via use of ladder-like energy levels of RE ions when excited at near infrared (NIR) light that are silent to tissues. These features allow not only a high penetration depth in biological tissues but also a high detection sensitivity. Indeed, the energy transfer between UCNPs and biomolecular or chemical indicators provide opportunities for high-sensitive bio- and chemical-sensing. A temperature-sensitive change of the intensity ratio between two close UC bands promises them for use in temperature mapping of a single living cell. In this work, we review recent investigations on using UCNPs for the detection of biomolecules (avidin, ATP, etc.), ions (cyanide, mecury, etc.), small gas molecules (oxygen, carbon dioxide, ammonia, etc.), as well as for in vitro temperature sensing. We also briefly summarize chemical methods in synthesizing UCNPs of high efficiency that are important for the detection limit. PMID:23650480

Amplicon-based semiconductor sequencing of human exomes: performance evaluation and optimization strategies.

PubMed

Damiati, E; Borsani, G; Giacopuzzi, Edoardo

2016-05-01

The Ion Proton platform allows to perform whole exome sequencing (WES) at low cost, providing rapid turnaround time and great flexibility. Products for WES on Ion Proton system include the AmpliSeq Exome kit and the recently introduced HiQ sequencing chemistry. Here, we used gold standard variants from GIAB consortium to assess the performances in variants identification, characterize the erroneous calls and develop a filtering strategy to reduce false positives. The AmpliSeq Exome kit captures a large fraction of bases (>94 %) in human CDS, ClinVar genes and ACMG genes, but with 2,041 (7 %), 449 (13 %) and 11 (19 %) genes not fully represented, respectively. Overall, 515 protein coding genes contain hard-to-sequence regions, including 90 genes from ClinVar. Performance in variants detection was maximum at mean coverage >120×, while at 90× and 70× we measured a loss of variants of 3.2 and 4.5 %, respectively. WES using HiQ chemistry showed ~71/97.5 % sensitivity, ~37/2 % FDR and ~0.66/0.98 F1 score for indels and SNPs, respectively. The proposed low, medium or high-stringency filters reduced the amount of false positives by 10.2, 21.2 and 40.4 % for indels and 21.2, 41.9 and 68.2 % for SNP, respectively. Amplicon-based WES on Ion Proton platform using HiQ chemistry emerged as a competitive approach, with improved accuracy in variants identification. False-positive variants remain an issue for the Ion Torrent technology, but our filtering strategy can be applied to reduce erroneous variants.

Optimization of a low noise detection circuit for probing the structure of damage cascades with IBIC

DOE PAGES

Auden, Elizabeth C.; Doyle, Barney L.; Bielejec, Edward; ...

2015-06-18

Optimal detector / pre-amplifier combinations have been identified for the use of light ion IBIC (ion beam induced charge) to probe the physical structure of electrically active defects in damage cascades caused by heavy ion implantation. The ideal detector must have a sufficiently thin dead layer that incident ions will produce the majority of damage cascades in the depletion region of the detector rather than the dead layer. Detector and circuit noise must be low enough to detect the implantation of a single heavy ion as well as the decrease in the light ion IBIC signal caused by Shockley-Read-Hall recombinationmore » when the beam scans regions of the detector damaged by the heavy ion. The IBIC signals from three detectors irradiated with 750 keV He⁺ ions are measured with commercial and bespoke charge sensitive pre-amplifiers to identify the combination with the lowest noise.« less

Comparison of Sanger and next generation sequencing performance for genotyping Cryptosporidium isolates at the 18S rRNA and actin loci.

PubMed

Paparini, Andrea; Gofton, Alexander; Yang, Rongchang; White, Nicole; Bunce, Michael; Ryan, Una M

2015-01-01

Cryptosporidium is an important enteric pathogen that infects a wide range of humans and animals. Rapid and reliable detection and characterisation methods are essential for understanding the transmission dynamics of the parasite. Sanger sequencing, and high-throughput sequencing (HTS) on an Ion Torrent platform, were compared with each other for their sensitivity and accuracy in detecting and characterising 25 Cryptosporidium-positive human and animal faecal samples. Ion Torrent reads (n = 123,857) were obtained at both 18S rRNA and actin loci for 21 of the 25 samples. Of these, one isolate at the actin locus (Cattle 05) and three at the 18S rRNA locus (HTS 10, HTS 11 and HTS 12), suffered PCR drop-out (i.e. PCR failures) when using fusion-tagged PCR. Sanger sequences were obtained for both loci for 23 of the 25 samples and showed good agreement with Ion Torrent-based genotyping. Two samples both from pythons (SK 02 and SK 05) produced mixed 18S and actin chromatograms by Sanger sequencing but were clearly identified by Ion Torrent sequencing as C. muris. One isolate (SK 03) was typed as C. muris by Sanger sequencing but was identified as a mixed C. muris and C. tyzzeri infection by HTS. 18S rRNA Type B sequences were identified in 4/6 C. parvum isolates when deep sequenced but were undetected in Sanger sequencing. Sanger was cheaper than Ion Torrent when sequencing a small numbers of samples, but when larger numbers of samples are considered (n = 60), the costs were comparative. Fusion-tagged amplicon based approaches are a powerful way of approaching mixtures, the only draw-back being the loss of PCR efficiency on low-template samples when using primers coupled to MID tags and adaptors. Taken together these data show that HTS has excellent potential for revealing the "true" composition of species/types in a Cryptosporidium infection, but that HTS workflows need to be carefully developed to ensure sensitivity, accuracy and contamination are controlled. Copyright © 2015 Elsevier Inc. All rights reserved.

Mercury-modulated supramolecular assembly of a hexaphenylbenzene derivative for selective detection of picric acid.

PubMed

Bhalla, Vandana; Kaur, Sharanjeet; Vij, Varun; Kumar, Manoj

2013-05-06

Spherical aggregates of hexaphenylbenzene derivative 5 undergo metal-induced modulation to form nanorods in the presence of Hg(2+) ions, which exhibit selective and sensitive response toward picric acid (PA) with a detection limit of 6.87 ppb.

A new high selective and sensitive turn-on fluorescent and ratiometric absorption chemosensor for Cu2+ based on benzimidazole in aqueous solution and its application in live cell.

PubMed

Bing, Qijing; Wang, Lin; Li, Donglin; Wang, Guang

2018-09-05

A new benzimidazole base turn-on fluorescent and ratiometric absorption chemosensor (L) bearing bidentate ligand for detection of Cu 2+ was designed and synthesized. Fluorescence and UV-vis spectra studies demonstrated that L can detect Cu 2+ ions in aqueous solution using fluorescence enhancement and ratiometric absorption sensing over a wide pH range. Both fluorescent and ratiometric absorption sensing of L for Cu 2+ possessed high selectivity and sensitivity over other competitive metal ions and had low detection limit. Job's plot, mass spectra and DFT calculation indicated the sensing mechanism is the complex formation between L and Cu 2+ with 1:2 stoichiometry. Fluorescence images of HepG2 in the absence and presence of Cu 2+ displayed L had cell permeability and detection ability for Cu 2+ in live cells. Copyright © 2018 Elsevier B.V. All rights reserved.

Comparison of ion chromatographic methods based on conductivity detection, post-column-reaction and on-line-coupling IC-ICP-MS for the determination of bromate.

PubMed

Schminke, G; Seubert, A

2000-02-01

An established method for the determination of the disinfection by-product bromate is ion chromatography (IC). This paper presents a comparison of three IC methods based on either conductivity detection (IC-CD), a post-column-reaction (IC-PCR-VIS) or the on-line-coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS). Main characteristics of the methods such as method detection limits (MDL), time of analysis and sample pretreatment are compared and applicability for routine analysis is critically discussed. The most sensitive and rugged method is IC-ICP-MS, followed by IC-PCR-VIS. The photometric detection is subject to a minor interference in real world samples, presumably caused by carbonate. The lowest sensitivity is shown by the IC-CD method as slowest method compared, which, in addition, requires a sample pretreatment. The highest amount of information is delivered by IC-PCR-VIS, which allows the simultaneous determination of the seven standard anions and bromate.

Total hydrocarbon analysis by ion mobility spectrometry

NASA Technical Reports Server (NTRS)

Cross, John H.; Limero, Thomas F.; James, John T.

1994-01-01

Astronauts must be alerted quickly to chemical leaks that compromise their health and the success of their missions. An ideal leak detector would be equally sensitive to all compounds that might constitute a hazard and insensitive to nontoxic compounds. No ideal sensor exists; thus, selection of a methodology is a series of compromises. The commonly used methods are either insensitive at the low exposure levels set by OSHA, NASA, and other organizations or are selectively insensitive to important classes of chemicals such as Freons. After extensive study and experience, the Toxicology Group at JSC has selected ion mobility spectrometry (IMS) for development into a broad range, sensitive detector. In addition to the sensing method, signal processing is important leak detection because a background signal can be expected at all times. The leak-detecting instrument must be programmed to discriminate between authentic leaks and background fluctuations caused by routine operations. The results of an evaluation of the prototype THA is presented in terms related to spacecraft operations. The evaluation included determination of instrumental parameters such as stability and response times. We also included responses to some common components of spacecraft atmospheres in pure form and in binary and ternary mixtures. The output of the four algorithms to the mixtures was found to be noticeably different. These responses are compared on the basis of their utility for signaling a chemical leak. As a means of evaluating its resistance to a falsely positive response, the THA was challenged with carbon dioxide and methane, compounds whose concentrations normally increase in spacecraft air during human habitation. The instrument showed virtually no response to these interferences. Although the prototype THA is designed for space flight, this detector is expected to be useful for field screening at chemical waste dumps and other environmentally sensitive locations.

Time-resolved determination of Fe(II) ions using cysteine-bridged Mn-doped ZnS quantum dots as a phosphorimetric probe.

PubMed

Jing, Wenjie; Lu, Yuexiang; Wang, Feiyang; He, Liuying; Sun, Jingwei; Liu, Yueying

2018-05-12

A time-resolved phosphorescence (TRP) is applied to the highly sensitive determination of Fe(II) ions. The method is based on the use of a phosphorescent probe consisting of cysteine-bridged Mn-doped ZnS quantum dots (Mn/ZnS QDs). The presence of cysteine enhances the phosphorescence of the QDs and also increases the efficiency of quenching caused by Fe(II) ions. This results in strongly improved selectivity for Fe(II). The linear response is obtained in the concentration range of 50-1000 nM with a 19 nM detection limit. Phosphorescence is recorded at excitation/emission peaks of 301/602 nm. The interference of short-lived fluorescent and scattering background from the biological fluids is eliminated by using the TRP mode with a delay time of 200 μs. The determination of Fe(II) in human serum samples spiked at a 150 nM level gave a 92.4% recovery when using the TRP mode, but only 52.4% when using steady-state phosphorescence. This demonstrates that this probe along with TRP detection enables highly sensitive and accurate determination of Fe(II) in serum. Graphical abstract Schematic of a novel phosphorescent method for the detection of Fe 2+ ions based on cysteine-bridged Mn-doped ZnS quantum dots. The sensitivity of this assay greatly increases due to the addition of cysteine. Interferences by short-lived auto-fluorescence and the scattering light from the biological fluids is eliminated by using time-resolved phosphorescence mode.

A tandem time–of–flight spectrometer for negative–ion/positive–ion coincidence measurements with soft x-ray excitation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stråhlman, Christian, E-mail: Christian.Strahlman@maxlab.lu.se; Sankari, Rami; Nyholm, Ralf

2016-01-15

We present a newly constructed spectrometer for negative–ion/positive–ion coincidence spectroscopy of gaseous samples. The instrument consists of two time–of–flight ion spectrometers and a magnetic momentum filter for deflection of electrons. The instrument can measure double and triple coincidences between mass–resolved negative and positive ions with high detection efficiency. First results include identification of several negative–ion/positive–ion coincidence channels following inner-shell photoexcitation of sulfur hexafluoride (SF{sub 6})

Chemical enhancement of surface deposition

DOEpatents

Patch, K.D.; Morgan, D.T.

1997-07-29

A method and apparatus are disclosed for increasing the deposition of ions onto a surface, such as the adsorption of uranium ions on the detecting surface of a radionuclide detector. The method includes the step of exposing the surface to a complexing agent, such as a phosphate ion solution, which has an affinity for the dissolved species to be deposited on the surface. This provides, for example, enhanced sensitivity of the radionuclide detector. 16 figs.

Detection of nitro-based and peroxide-based explosives by fast polarity-switchable ion mobility spectrometer with ion focusing in vicinity of Faraday detector.

PubMed

Zhou, Qinghua; Peng, Liying; Jiang, Dandan; Wang, Xin; Wang, Haiyan; Li, Haiyang

2015-05-29

Ion mobility spectrometer (IMS) has been widely deployed for on-site detection of explosives. The common nitro-based explosives are usually detected by negative IMS while the emerging peroxide-based explosives are better detected by positive IMS. In this study, a fast polarity-switchable IMS was constructed to detect these two explosive species in a single measurement. As the large traditional Faraday detector would cause a trailing reactant ion peak (RIP), a Faraday detector with ion focusing in vicinity was developed by reducing the detector radius to 3.3 mm and increasing the voltage difference between aperture grid and its front guard ring to 591 V, which could remove trailing peaks from RIP without loss of signal intensity. This fast polarity-switchable IMS with ion focusing in vicinity of Faraday detector was employed to detect a mixture of 10 ng 2,4,6-trinitrotoluene (TNT) and 50 ng hexamethylene triperoxide diamine (HMTD) by polarity-switching, and the result suggested that [TNT-H](-) and [HMTD+H](+) could be detected in a single measurement. Furthermore, the removal of trailing peaks from RIP by the Faraday detector with ion focusing in vicinity also promised the accurate identification of KClO4, KNO3 and S in common inorganic explosives, whose product ion peaks were fairly adjacent to RIP.

Electrospray ionization of uranyl-citrate complexes

NASA Astrophysics Data System (ADS)

Somogyi, Árpád; Pasilis, Sofie P.; Pemberton, Jeanne E.

2007-09-01

Results presented here demonstrate the usefulness of electrospray ionization and gas-phase ion-molecule reactions to predict structural and electronic differences in complex inorganic ions. Electrospray ionization of uranyl citrate solutions generates positively and negatively charged ions that participate in further ion-molecule reactions in 3D ion trap and FT-ICR mass analyzers. Most ions observed are derived from the major solution uranyl-citrate complexes and involve species of {(UO2)2Cit2}2-, (UO2)3Cit2, and {(UO2)3Cit3}3-, where Cit indicates the citrate trianion, C6H5O73-. In a 3D ion trap operated at relatively high pressure, complex adducts containing solvent molecules, alkali and ammonium cations, and nitrate or chloride anions are dominant, and proton/alkali cation (Na+, K+) exchange is observed for up to six exchangeable protons in an excess of alkali cations. Adduct formation in a FT-ICR cell that is operated at lower pressures is less dominant, and direct detection of positive and negative ions of the major solution complexes is possible. Multiply charged ions are also detected, suggesting the presence of uranium in different oxidation states. Changes in uranium oxidation state are detected by He-CID and SORI-CID fragmentation, and certain fragments undergo association reactions in trapping analyzers, forming "exotic" species such as [(UO2)4O3]-, [(UO2)4O4]-, and [(UO2)4O5]-. Ion-molecule reactions with D2O in the FT-ICR cell indicate substantial differences in H/D exchange rate and D2O accommodation for different ion structures and charge states. Most notably, the positively charged ions [H2(UO2)2Cit2(H)]+ and [(UO2)2(Cit)]+ accommodate two and three D2O molecules, respectively, which reflects well the structural differences, i.e., tighter uranyl-citrate coordination in the former ion than in the latter. The corresponding negatively charged ions accommodate zero or two D2O molecules, which can be rationalized using suggested solution phase structures and charge state distributions.

Using MASHA+TIMEPIX Setup for Registration Beta Decay Isotopes Produced in Heavy Ion Induced Reactions

NASA Astrophysics Data System (ADS)

Rodin, A. M.; Belozerov, A. V.; Chernysheva, E. V.; Dmitriev, S. N.; Gulyaev, A. V.; Gulyaeva, A. V.; Itkis, M. G.; Novoselov, A. S.; Oganessian, Yu. Ts.; Salamatin, V. S.; Stepantsov, S. V.; Vedeneev, V. Yu.; Yukhimchuk, S. A.; Krupa, L.; Granja, C.; Pospisil, S.; Kliman, J.; Motycak, S.; Sivacek, I.

2015-06-01

Radon and mercury isotopes were produced in multi nucleon transfer (48Ca + 232Th) and complete fusion (48Ca + naturalNd) reactions, respectively. The isotopes with given masses were detected using two detectors: a multi-strip detector of the well-type (made in CANBERRA) and a position-sensitive quantum counting hybrid pixel detector of the TIMEPIX type. The isotopes implanted into the detectors then emit alpha- and betaparticles until reaching the long lived isotopes. The position of the isotopes, the tracks, the time and energy of beta-particles were measured and analyzed. A new software for the particle recognition and data analysis of experimental results was developed and used. It was shown that MASHA+ TIMEPIX setup is a powerful instrument for investigation of neutron-rich isotopes far from stability limits.

Long-term sub second-response monitoring of gaseous ammonia in ambient air by positive inhaling ion mobility spectrometry.

PubMed

Huang, Wei; Wang, Weiguo; Chen, Chuang; Li, Mei; Peng, Liying; Li, Hang; Liu, Jiwei; Hou, Keyong; Li, Haiyang

2017-12-01

A real-time dynamic measurements of ammonia (NH 3 ) is crucial for understanding the atmospheric nucleation process. A novel method was developed for on line monitoring at the sub-second time scale for the gaseous ammonia in ambient air for months, based on a positive inhaling ion mobility spectrometry (IMS) with a 63 Ni ion source. The selective detection of NH 3 was achieved using a high resolution IMS with an optimization of the drift tube temperature above 150°C. This method improved the peak-to-peak resolution significantly, thus avoided the interferences of the adjacent peaks to the quantitative analysis of NH 3 . The time resolution of the IMS was less than 0.1s at a data averaging of 10 times. The limit of detection (LOD) achieved at sub-ppb level while a linear response of peak intensity versus concentration of NH 3 in the range of 10-60ppb and 60-400ppb were obtained. The relative standard deviations (RSD), the confidence level and the errors were 1.06%, 95% and ± 0.21ppb by measuring 100ppb NH 3 for 100 times. The effect of ambient humidity could be greatly reduced by using the drift temperature of over 150°C. At last, the application of measuring the NH 3 concentration evolutions of Dalian city was performed from June 19 to December 3 in 2015. The results illustrated a potential method of using IMS for a real-time measuring atmospheric NH 3 at an unprecedented accuracy and sensitivity with long-term stability. Copyright © 2017 Elsevier B.V. All rights reserved.

Arbitrary amplitude ion-acoustic solitary waves in electronegative plasmas with electrons featuring Tsallis distribution

NASA Astrophysics Data System (ADS)

Ghebache, Siham; Tribeche, Mouloud

2017-10-01

The problem of arbitrary amplitude ion-acoustic solitary waves (IASWs), which accompany electronegative plasmas having positive ions, negative ions, and nonextensive electrons is addressed. The energy integral equation with a new Sagdeev potential is analyzed to examine the existence regions of the IASWs. Different types of electronegative plasmas inspired from the experimental studies of Ichiki et al. (2001) are discussed. Our results show that in such plasmas IASWs, the amplitude and nature of which depend sensitively on the mass and density ratio of the positive and negative ions as well as the q-nonextensive parameter, can exist. Interestingly, one finds that our plasma model supports the coexistence of smooth rarefactive and spiky compressive IASWs. Our results complement and provide new insights on previously published findings on this problem.

Ion mobility spectrometry for food quality and safety.

PubMed

Vautz, W; Zimmermann, D; Hartmann, M; Baumbach, J I; Nolte, J; Jung, J

2006-11-01

Ion mobility spectrometry is known to be a fast and sensitive technique for the detection of trace substances, and it is increasingly in demand not only for protection against explosives and chemical warfare agents, but also for new applications in medical diagnosis or process control. Generally, a gas phase sample is ionized by help of ultraviolet light, ss-radiation or partial discharges. The ions move in a weak electrical field towards a detector. During their drift they collide with a drift gas flowing in the opposite direction and, therefore, are slowed down depending on their size, shape and charge. As a result, different ions reach the detector at different drift times, which are characteristic for the ions considered. The number of ions reaching the detector are a measure of the concentration of the analyte. The method enables the identification and quantification of analytes with high sensitivity (ng l(-1) range). The selectivity can even be increased - as necessary for the analyses of complex mixtures - using pre-separation techniques such as gas chromatography or multi-capillary columns. No pre-concentration of the sample is necessary. Those characteristics of the method are preserved even in air with up to a 100% relative humidity rate. The suitability of the method for application in the field of food quality and safety - including storage, process and quality control as well as the characterization of food stuffs - was investigated in recent years for a number of representative examples, which are summarized in the following, including new studies as well: (1) the detection of metabolites from bacteria for the identification and control of their growth; (2) process control in food production - beer fermentation being an example; (3) the detection of the metabolites of mould for process control during cheese production, for quality control of raw materials or for the control of storage conditions; (4) the quality control of packaging materials during the production of polymeric materials; and (5) the characterization of products - wine being an example. The challenges of such applications were operation in humid air, fast on-line analyses of complex mixtures, high sensitivity - detection limits have to be, for example, in the range of the odour limits - and, in some cases, the necessity of mobile instrumentation. It can be shown that ion mobility spectrometry is optimally capable of fulfilling those challenges for many applications.

9,10-Phenanthrenequinone as a mass-tagging reagent for ultra-sensitive liquid chromatography-tandem mass spectrometry assay of aliphatic aldehydes in human serum.

PubMed

El-Maghrabey, Mahmoud; Kishikawa, Naoya; Kuroda, Naotaka

2016-09-02

9,10-Phenanthrenequinone (PQ) was successfully used as a new mass-tagging reagent for sensitive labeling of aliphatic aldehydes (C3-C10) prior liquid chromatography-electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS). This reagent could overcome the drawbacks of previous amine or hydrazine-based reagents, such as lower sensitivity, formation of two stereoisomeric reaction products for each single analyte, need for longer derivatization time, and poor reactivity with aliphatic aldehydes. The PQ-aldehyde derivatives exhibited intense [M+H](+) and a common product ion with ESI in the positive-ion mode. The derivatives were monitored at the transition of [M+H](+)→m/z 231.9 with detection limits from 4.0 to 100 pM (signal to noise ratio=3). 3-Phenylpropanal was used as an internal standard (IS) and the separation of the eight aldehydes and IS was achieved in less than 10min employing gradient elution with methanol and ammonium formate buffer (20mM, pH 4.0). The method employed salting out liquid-liquid extraction for aliphatic aldehydes form serum for the first time with excellent recoveries (92.6-110.8%). The developed method was validated and applied for quantification of the target aldehydes in serum of healthy volunteers (n=14). Copyright © 2016 Elsevier B.V. All rights reserved.

Glutathione-Capped Gold Nanoparticles-Based Photoacoustic Sensor for Label-Free Detection of Lead Ions

NASA Astrophysics Data System (ADS)

Shi, R.; Liu, X.-J.; Ying, Y.

2017-07-01

The photoacoustic signal generated by laser-induced nanobubbles (PA-LINB) proved to be a sensitive tool to monitor the aggregation of gold nanoparticles. Here, a simple and label-free photoacoustic method for the rapid detection of Pb2+ in the aqueous phase was developed. Due to the high affinity of Pb2+ ions to glutathione, the presence of Pb2+ led to the aggregation of glutathione-conjugated gold nanoparticles (GSH-GNPs). Hence, by measuring the variation of the PA-LINB signal after the aggregation of GSH-GNPs, Pb2+ can be quantified. A low detection limit for Pb2+ (42 nM) and a wide linear working range ( 42-1000 nM) were achieved. Furthermore, the proposed method showed good selectivity against other metal ions.

Naphthaldimine-based simple glucose derivative as a highly selective sensor for colorimetric detection of Cu2+ ion in aqueous media

NASA Astrophysics Data System (ADS)

Dolai, Bholanath; Bhaumik, Atanu; Pramanik, Nabakumar; Ghosh, Kalyan Sundar; Atta, Ananta Kumar

2018-07-01

Naphthaldimine-based glucose derivatives 1 and 3 have been designed, synthesized and characterized. In aqueous media, glucose derivative 1, exhibited high selectivity and sensitivity towards Cu2+ ion in comparison with various cations and anions. In presence of Cu2+, sensor 1 has provided significant naked-eye detectable color change. The formation of 1-Cu2+ complex has been analyzed by UV-vis spectroscopy, 1H NMR titration experiments, mass spectrometry and DFT (density functional theory) calculations. Limit of detection of 1 as a colorimetric sensor for Cu2+ ion is found to be 0.23 μM, much lower than recommended value of World Health Organization (WHO), which makes to Cu2+ sensor 1 more effective and useful.

Using fluorescence measurement of zinc ions liberated from ZnS nanoparticle labels in bioassay for Escherichia coli O157:H7

NASA Astrophysics Data System (ADS)

Cowles, Chad L.; Zhu, Xiaoshan; Pai, Chi-Yun

2011-10-01

In this study, an alternative approach using ZnS nanoparticle biolabels as fluorescence signal transducers is reported for the immunoassay of E. coli O157:H7 in tap water samples. Instead of measuring the fluorescence of ZnS nanoparticles in the assay, the fluorescence signal is generated through the binding of zinc ions released from nanoparticle labels with zinc-ion sensitive fluorescence indicator Fluozin-3. In the assay, ZnS nanoparticles around 50 nm in diameter were synthesized, bioconjugated, and applied for the detection of E. coli O157:H7. The assay shows a detection range over two orders of magnitude and a detection limit around 1000 colony-forming units (cfu) of E. coli O157:H7.

Multiresponsive polysiloxane bearing spiropyran: synthesis and sensing of pH and metal ions of different valence

NASA Astrophysics Data System (ADS)

Li, Hongqi; Zheng, Tao; Zhao, Yong; Xu, Zhenxiang; Dai, Xuhang; Shao, Zhiyu

2018-03-01

A spiropyran-appended polysiloxane (SP-Si) was synthesized and characterized. The pH-responsive behavior of SP-Si was investigated. It was found that with the decrease of the pH of SP-Si solution the intensity of the absorption peak at 440 nm increased and the color of SP-Si solution turned from colorless to yellow gradually. The polymer serves as chemosensor for colorimetric detection of Ag+ and Fe3+ ions. Addition of Ag+ and Fe3+ ions to SP-Si solution induced color change from colorless to brown and earthy yellow, respectively. Sensing of Ag+ ions by SP-Si was not affected by common competitive metal ions except Hg2+ ions. Based on the transformation from colorless SP-Si solution with negligible absorption at 440 nm to brown SP-Si/Ag+ showing extremely strong absorption at 440 nm by addition of Ag+ ions and subsequent transformation from brown to colorless SP-Si/Ag+/Hg2+ with relatively weak absorption at 440 nm after addition of 1 equivalent of Hg2+ ions, SP-Si/Ag+ system serves as a dual colorimetric and spectroscopic probe for highly selective and sensitive detection of Hg2+ ions. The selective detection of Fe3+ ions by SP-Si is not interfered by common competitive metal ions including Na+, K+, Li+, Hg2+, Ni2+, Fe2+, Zn2+, Co2+, Sr2+, Cu2+, Al3+, Ce3+ and Cr3+. The detection limit of Ag+ and Fe3+ ions is 1.45 × 10-6 M and 3.52 × 10-6 M, respectively.

Depth enhancement of ion sensitized data

DOEpatents

Lamartine, Bruce C.

2001-01-01

A process of fabricating a durable data storage medium is disclosed, the durable data storage medium capable of storing, digital or alphanumeric characters as well as graphical shapes or characters. Additionally, a durable data storage medium including a substrate having etched characters therein is disclosed, the substrate characterized as containing detectable residual amounts of ions used in the preparation process.

Sensitive detection of n-alkanes using a mixed ionization mode proton-transfer-reaction mass spectrometer

NASA Astrophysics Data System (ADS)

Amador-Muñoz, Omar; Misztal, Pawel K.; Weber, Robin; Worton, David R.; Zhang, Haofei; Drozd, Greg; Goldstein, Allen H.

2016-11-01

Proton-transfer-reaction mass spectrometry (PTR-MS) is a technique that is widely used to detect volatile organic compounds (VOCs) with proton affinities higher than water. However, n-alkanes generally have a lower proton affinity than water and therefore proton transfer (PT) by reaction with H3O+ is not an effective mechanism for their detection. In this study, we developed a method using a conventional PTR-MS to detect n-alkanes by optimizing ion source and drift tube conditions to vary the relative amounts of different primary ions (H3O+, O2+, NO+) in the reaction chamber (drift tube). There are very few studies on O2+ detection of alkanes and the mixed mode has never been proposed before. We determined the optimum conditions and the resulting reaction mechanisms, allowing detection of n-alkanes from n-pentane to n-tridecane. These compounds are mostly emitted by evaporative/combustion process from fossil fuel use. The charge transfer (CT) mechanism observed with O2+ was the main reaction channel for n-heptane and longer n-alkanes, while for n-pentane and n-hexane the main reaction channel was hydride abstraction (HA). Maximum sensitivities were obtained at low E / N ratios (83 Td), low water flow (2 sccm) and high O2+ / NO+ ratios (Uso = 180 V). Isotopic 13C contribution was taken into account by subtracting fractions of the preceding 12C ion signal based on the number of carbon atoms and the natural abundance of 13C (i.e., 5.6 % for n-pentane and 14.5 % for n-tridecane). After accounting for isotopic distributions, we found that PT cannot be observed for n-alkanes smaller than n-decane. Instead, protonated water clusters of n-alkanes (M ṡ H3O+) species were observed with higher abundance using lower O2+ and higher water cluster fractions. M ṡ H3O+ species are probably the source for the M + H+ species observed from n-decane to n-tridecane. Normalized sensitivities to O2+ or to the sum of O2++ NO+ were determined to be a good metric with which to compare sensitivities for n-alkane detection between experiments. Double hydride abstraction was observed from the reaction with O2+. Sensitivity to CT increased with carbon chain length from n-pentane to n-dodecane, sensitivity to HA increased from n-heptane to n-dodecane and sensitivity to PT increased from n-decane to n-tridecane. Sensitivity to CT exponentially decreased with molecular ionization energy, which is inversely related to the carbon chain length. We introduce a calibrated fragmentation algorithm as a method to determine the concentrations of n-alkanes and demonstrate its effectiveness using a custom n-alkane mixture and a much more complex oil example representing perhaps the most difficult mixture available for application of the method. We define optimum conditions for using the mixed ionization mode to measure n-alkanes in conventional PTR-MS instruments regardless of whether they are equipped with switchable reagent ion (SRI) capabilities.

Dual-Emission SG7@MOF Sensor via SC-SC Transformation: Enhancing the Formation of Excimer Emission and the Range and Sensitivity of Detection.

PubMed

Fu, Hong-Ru; Wu, Xiao-Xia; Ma, Lu-Fang; Wang, Fei; Zhang, Jian

2018-05-30

In this study, a water stable metal-organic framework FIR-53 is applied as a single-crystal container for anion exchange. The exceptional chemical stability and low crystallographic symmetry of FIR-53 makes it possible to determine anionic guests. Through ion exchange and single-crystal to single-crystal (SC-SC) transformation, 8-hydroxypyrene-1,3,6-trisulfonate (SG7, solvent green 7, ion form as SG7 3- ) is introduced into the pores of FIR-53 to obtain SG7@FIR-53. Because of the spatial confinement and partition effect, SG7@FIR-53 shows the bright exciter emission of SG7 ions. Interestingly, the composite SG7@FIR-53 exhibits a sensitive fluorescence quenching response against Cr 2 O 7 2- and MnO 4 - in aqueous solution. Especially, the detection limit toward MnO 4 - is as low as 0.12 ppb, which is the smallest value to date. Moreover, the prepared SG7@FIR-53 film also displays a broad response to nitro explosives in vapor/aqueous phase. Compared with the results of FIR-53, the range and sensitivity were greatly improved.

Highly Sensitive and Selective In-Situ SERS Detection of Pb(2+), Hg(2+), and Cd(2+) Using Nanoporous Membrane Functionalized with CNTs.

PubMed

Shaban, Mohamed; Galaly, A R

2016-05-04

Porous Anodic Alumina (PAA) membrane was functionalized with CoFe2O4 nanoparticles and used as a substrate for the growing of very long helical-structured Carbon Nanotubes (CNTs) with a diameter less than 20 nm. The structures and morphologies of the fabricated nanostructures were characterized by field emission- scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), and Raman spectroscopy. By uploading the CNTs on PAA, the characteristic Raman peaks of CNTs and PAA showed 4 and 3 times enhancement, respectively, which leads to more sensitive Surface-Enhanced Raman Spectroscopy (SERS) substrates. For comparison, PAA and CNTs/PAA arrays were used as SERS substrates for the detection of Hg(2+), Cd(2+), and Pb(2+). The proposed sensor demonstrated high sensitivity and selectivity between these heavy metal ions. CNTs/PAA sensor showed excellent selectivity toward Pb(2+) over other metal ions, where the enhancement factor is decreased from ~17 for Pb(2+) to ~12 for Hg(2+) and to ~4 for Cd(2+). Therefore, the proposed CNTs/PAA sensor can be used as a powerful tool for the determination of heavy metal ions in aqueous solutions.

Highly Sensitive and Selective In-Situ SERS Detection of Pb2+, Hg2+, and Cd2+ Using Nanoporous Membrane Functionalized with CNTs

PubMed Central

Shaban, Mohamed; Galaly, A. R.

2016-01-01

Porous Anodic Alumina (PAA) membrane was functionalized with CoFe2O4 nanoparticles and used as a substrate for the growing of very long helical-structured Carbon Nanotubes (CNTs) with a diameter less than 20 nm. The structures and morphologies of the fabricated nanostructures were characterized by field emission- scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), and Raman spectroscopy. By uploading the CNTs on PAA, the characteristic Raman peaks of CNTs and PAA showed 4 and 3 times enhancement, respectively, which leads to more sensitive Surface-Enhanced Raman Spectroscopy (SERS) substrates. For comparison, PAA and CNTs/PAA arrays were used as SERS substrates for the detection of Hg2+, Cd2+, and Pb2+. The proposed sensor demonstrated high sensitivity and selectivity between these heavy metal ions. CNTs/PAA sensor showed excellent selectivity toward Pb2+ over other metal ions, where the enhancement factor is decreased from ~17 for Pb2+ to ~12 for Hg2+ and to ~4 for Cd2+. Therefore, the proposed CNTs/PAA sensor can be used as a powerful tool for the determination of heavy metal ions in aqueous solutions. PMID:27143512

RAPID DETECTION OF ALGAL TOXINS - PHASE I

EPA Science Inventory

The proposed program will demonstrate the ability of a detector based on measuring the conductance of nicotinic acetylcholine receptor (nAChR) ion channels to detect and quantify anatoxin-a contamination in drinking water systems.  The nAChR is extremely sensitive to the p...

Cluster secondary ion mass spectrometry microscope mode mass spectrometry imaging.

PubMed

Kiss, András; Smith, Donald F; Jungmann, Julia H; Heeren, Ron M A

2013-12-30

Microscope mode imaging for secondary ion mass spectrometry is a technique with the promise of simultaneous high spatial resolution and high-speed imaging of biomolecules from complex surfaces. Technological developments such as new position-sensitive detectors, in combination with polyatomic primary ion sources, are required to exploit the full potential of microscope mode mass spectrometry imaging, i.e. to efficiently push the limits of ultra-high spatial resolution, sample throughput and sensitivity. In this work, a C60 primary source was combined with a commercial mass microscope for microscope mode secondary ion mass spectrometry imaging. The detector setup is a pixelated detector from the Medipix/Timepix family with high-voltage post-acceleration capabilities. The system's mass spectral and imaging performance is tested with various benchmark samples and thin tissue sections. The high secondary ion yield (with respect to 'traditional' monatomic primary ion sources) of the C60 primary ion source and the increased sensitivity of the high voltage detector setup improve microscope mode secondary ion mass spectrometry imaging. The analysis time and the signal-to-noise ratio are improved compared with other microscope mode imaging systems, all at high spatial resolution. We have demonstrated the unique capabilities of a C60 ion microscope with a Timepix detector for high spatial resolution microscope mode secondary ion mass spectrometry imaging. Copyright © 2013 John Wiley & Sons, Ltd.

A sensitive fluorescent sensor for quantification of alpha-fetoprotein based on immunosorbent assay and click chemistry.

PubMed

Xie, Qunfang; Weng, Xiuhua; Lu, Lijun; Lin, Zhenyu; Xu, Xiongwei; Fu, Caili

2016-03-15

A novel fluoresencent immunosensor for determination of cancer biomarkers such as alpha-fetoprotein (AFP) was designed by utilizing both the high specificity of antigen-antibody sandwich structure and the high sensitivity of the click chemistry based fluorescence detection. Instead of an enzyme or fluorophore, the CuO nanoparticles are labeled on the detection antibody, which was not susceptible to the change of the external environments. The CuO nanoparticles which were modified on the sandwich structure can be dissolved to produce Cu(2+) ions with the help of HCl and then the Cu(2+) ions were reduced by sodium ascorbate to produce Cu(+) ions which triggered the Cu(+) catalyzed alkyne-azide cycloaddition (CuAAC) reaction between the weak fluorescent compound (3-azido-7-hydroxycoumarin) and propargyl alcohol to form a strong fluorescent compound. A good linear relationship was observed between the fluorescence increase factor of the system and the concentration of AFP in the range of 0.025-5.0 ng/mL with a detection limit of 12 pg/mL (S/N=3). The proposed fluorescent sensor had been applied to detect AFP in the human serum samples and gave satisfactory results. Copyright © 2015 Elsevier B.V. All rights reserved.

Pyrogen tests of infusions, blood anticoagulant solutions, plastic materials and rubber products.

PubMed

Pintér, J; Zsdánszky, C; Györffy, G

1977-01-01

The methods of the pyrogen test in rabbit as adopted by the authors are presented. The test includes positive and negative controls. The conditions of using the same rabbits on two consecutive days are discussed. Methods of sampling of sterile infusions and the preparation for pyrogen test of anticoagulant solutions containing citrate, phosphate and/or edetate ions are presented. The necessity of pyrogen control of distilled water is stressed. Attention is called on the importance of testing for pyrogenicity of the plastic materials and the rubber-wares to be applied during the production of anticoagulant solutions and infusions. A pyrogen test highly sensitive for detecting traces of detergent is applied for washed glassware. It is emphasized that sensitive pyrogen tests are indispensable not only when new derivatives are being introduced, but also during routine control, because occasional changes in the manufacturer's technology may sometimes be demonstrable in this way.

Ultra-sensitive suspended atomically thin-layered black phosphorus mercury sensors.

PubMed

Li, Peng; Zhang, Dongzhi; Jiang, Chuanxing; Zong, Xiaoqi; Cao, Yuhua

2017-12-15

The extraordinary properties of black phosphorus (BP) make it a promising candidate for next-generation transistor chemical sensors. However, BP films reported so far are supported on substrate, and substrate scattering drastically deteriorates its electrical properties. Consequentially, the potential sensing capability of intrinsic BP is highly underestimated and its sensing mechanism is masked. Additionally, the optimum sensing regime of BP remains unexplored. This article is the first demonstration of suspended BP sensor operated in subthreshold regime. BP exhibited significant enhancement of sensitivity for ultra-low-concentration mercury detection in the absence of substrate, and the sensitivity reached maximum in subthreshold regime. Without substrate scattering, the suspended BP device demonstrated 10 times lower 1/f noise which contributed to better signal-to-noise ratio. Therefore, rapid label-free trace detection of Hg 2+ was achieved with detection limit of 0.01 ppb, lower than the world health organization (WHO) tolerance level (1 ppb). The time constant for ion detection extracted was 3s. Additionally, experimental results revealed that good stability, repeatability, and selectivity were achieved. BP sensors also demonstrated the ability of detecting mercury ions in environment water samples. The underling sensing mechanism of intrinsic BP was ascribed to the carrier density variation resulted from surface charge gating effect, so suspended BP in subthreshold regime with optimum gating effect demonstrated the best sensitivity. Our results show the prominent advantages of intrinsic BP as a sensing material. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

An Ultrastable Europium(III)-Organic Framework with the Capacity of Discriminating Fe2+/Fe3+ Ions in Various Solutions.

PubMed

Wen, Guo-Xuan; Wu, Ya-Pan; Dong, Wen-Wen; Zhao, Jun; Li, Dong-Sheng; Zhang, Jian

2016-10-05

An ultrastable luminescent europium-organic framework, {[Eu(L)(H 2 O) 2 ]·NMP·H 2 O} n (CTGU-2; NMP = N-methyl-2-pyrrolidone), can first detect Fe 2+ /Fe 3+ cations in different medium systems with high selectivity and sensitivity, and it also exhibits high sensitivity for Cr 2 O 7 2- anion and acetone with a wide linear range and a low detection limit.

Mass spectrometric characterization of tamoxifene metabolites in human urine utilizing different scan parameters on liquid chromatography/tandem mass spectrometry.

PubMed

Mazzarino, Monica; de la Torre, Xavier; Di Santo, Roberto; Fiacco, Ilaria; Rosi, Federica; Botrè, Francesco

2010-03-01

Different liquid chromatographic/tandem mass spectrometric (LC/MS/MS) scanning techniques were considered for the characterization of tamoxifene metabolites in human urine for anti-doping purpose. Five different LC/MS/MS scanning methods based on precursor ion scan (precursor ion scan of m/z 166, 152 and 129) and neutral loss scan (neutral loss of 72 Da and 58 Da) in positive ion mode were assessed to recognize common ions or common losses of tamoxifene metabolites. The applicability of these methods was checked first by infusion and then by the injection of solution of a mixture of reference standards of four tamoxifene metabolites available in our laboratory. The data obtained by the analyses of the mixture of the reference standards showed that the five methods used exhibited satisfactory results for all tamoxifene metabolites considered at a concentration level of 100 ng/mL, whereas the analysis of blank urine samples spiked with the same tamoxifene metabolites at the same concentration showed that the neutral loss scan of 58 Da lacked sufficient specificity and sensitivity. The limit of detection in urine of the compounds studied was in the concentration range 10-100 ng/mL, depending on the compound structure and on the selected product ion. The suitability of these approaches was checked by the analysis of urine samples collected after the administration of a single dose of 20 mg of tamoxifene. Six metabolites were detected: 4-hydroxytamoxifene, 3,4-dihydroxytamoxifene, 3-hydroxy-4-methoxytamoxifene, N-demethyl-4-hydroxytamoxifene, tamoxifene-N-oxide and N-demethyl-3-hydroxy-4-methoxytamoxifene, which is in conformity to our previous work using a time-of-flight (TOF) mass spectrometer in full scan acquisition mode. Copyright (c) 2010 John Wiley & Sons, Ltd.

Atmospheric pressure photoionization mass spectrometry as a tool for the investigation of the hydrolysis reaction mechanisms of phosphite antioxidants

NASA Astrophysics Data System (ADS)

Papanastasiou, M.; McMahon, A. W.; Allen, N. S.; Johnson, B. W.; Keck-Antoine, K.; Santos, L.; Neumann, M. G.

2008-08-01

The hydrolysis reaction mechanism of phosphite antioxidants is investigated by liquid chromatography-mass spectrometry (LC/MS). The phosphites were chosen because they differed in chemical structure and phosphorus content. Dopant assisted-atmospheric pressure photoionization (DA-APPI) is chosen as the ion source for the ionization of the compounds. In our previous work, DA-APPI was shown to offer an attractive alternative to atmospheric pressure chemical ionization (APCI) since it provided background-ion free mass spectra and higher sensitivity [M. Papanastasiou, et al., Polymer Degradation and Stability 91 (11) (2006) 2675-2682]. In positive ion mode, the molecules are generally detected in their protonated form. In negative ion mode, the phosphites are unstable and only fragment ions are observed; these however, are characteristic of each phosphite and may be used for the identification of the analytes in complex mixtures. The analytes under investigation are exposed to accelerated humid ageing conditions and their hydrolytic pathway and stability is investigated. Different substituents around the phosphorus atom are shown to have a significant effect on the stability of the phosphites, with phenol substituents producing very hydrolytically stable structures. Alkanox P24 and PEP-36 follow a similar hydrolytic pathway via the scission of the first and then the second POphenol bonds, eventually leading to the formation of phenol, phosphorous acid and pentaerythritol as end products. HP-10 exhibits a rather different structure and the products detected suggest scission of either the POhydrocarbon or one of the POphenol bonds. A phenomenon similar to that of autocatalysis is observed for all phosphites and is attributed to the formation of dialkyl phosphites as intermediate products.

Constraining the sensitivity of iodide adduct chemical ionization mass spectrometry to multifunctional organic molecules using the collision limit and thermodynamic stability of iodide ion adducts

DOE PAGES

Lopez-Hilfiker, Felipe D.; Iyer, Siddarth; Mohr, Claudia; ...

2016-04-06

The sensitivity of a chemical ionization mass spectrometer (ions formed per number density of analytes) is fundamentally limited by the collision frequency between reagent ions and analytes, known as the collision limit, the ion–molecule reaction time, and the transmission efficiency of product ions to the detector. We use the response of a time-of-flight chemical ionization mass spectrometer (ToF-CIMS) to N 2O 5, known to react with iodide at the collision limit, to constrain the combined effects of ion–molecule reaction time, which is strongly influenced by mixing and ion losses in the ion–molecule reaction drift tube. A mass spectrometric voltage scanningmore » procedure elucidates the relative binding energies of the ion adducts, which influence the transmission efficiency of molecular ions through the electric fields within the vacuum chamber. Together, this information provides a critical constraint on the sensitivity of a ToF-CIMS towards a wide suite of routinely detected multifunctional organic molecules for which no calibration standards exist. Lastly, we describe the scanning procedure and collision limit determination, and we show results from the application of these constraints to the measurement of organic aerosol composition at two different field locations.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Watson, Thomas B.

The Proton Transfer Reaction Mass Spectrometer (PTRMS) measures gas-phase compounds in ambient air and headspace samples before using chemical ionization to produce positively charged molecules, which are detected with a time-of-flight (TOF) mass spectrometer. This ionization method uses a gentle proton transfer reaction method between the molecule of interest and protonated water, or hydronium ion (H 3O +), to produce limited fragmentation of the parent molecule. The ions produced are primarily positively charged with the mass of the parent ion, plus an additional proton. Ion concentration is determined by adding the number of ions counted at the molecular ion’s mass-to-chargemore » ratio to the number of air molecules in the reaction chamber, which can be identified according to the pressure levels in the reaction chamber. The PTRMS allows many volatile organic compounds in ambient air to be detected at levels from 10–100 parts per trillion by volume (pptv). The response time is 1 to 10 seconds.« less

Polymer-based lanthanide luminescent sensor for detection of the hydrolysis product of the nerve agent Soman in water.

PubMed

Jenkins, A L; Uy, O M; Murray, G M

1999-01-15

The techniques of molecular imprinting and sensitized lanthanide luminescence have been combined to create the basis for a sensor that can selectively measure the hydrolysis product of the nerve agent Soman in water. The sensor functions by selectively and reversibly binding the phosphonate hydrolysis product of this agent to a functionality-imprinted copolymer possessing a coordinatively bound luminescent lanthanide ion, Eu3+. Instrumental support for this device is designed to monitor the appearance of a narrow luminescence band in the 610-nm region of the Eu3+ spectrum that results when the analyte is coordinated to the copolymer. The ligand field shifted luminescence was excited using 1 mW of the 465.8-nm line of an argon ion laser and monitored via an optical fiber using a miniature spectrometer. For this configuration, the limit of detection for the hydrolysis product is 7 parts per trillion (ppt) in solution with a linear range from 10 ppt to 10 ppm. Chemical and spectroscopic selectivities have been combined to reduce the likelihood of false positive analyses. Chemically analogous organophosphorus pesticides tested against the sensor have been shown to not interfere with determination.

BODIPY-based fluorometric sensor array for the highly sensitive identification of heavy-metal ions.

PubMed

Niu, Li-Ya; Li, Hui; Feng, Liang; Guan, Ying-Shi; Chen, Yu-Zhe; Duan, Chun-Feng; Wu, Li-Zhu; Guan, Ya-Feng; Tung, Chen-Ho; Yang, Qing-Zheng

2013-05-02

A BODIPY(4,4-difluoro-4-bora-3a,4a-diaza-s-indacene)-based fluorometric sensor array has been developed for the highly sensitive detection of eight heavy-metal ions at micromolar concentration. The di-2-picolyamine (DPA) derivatives combine high affinities for a variety of heavy-metal ions with the capacity to perturb the fluorescence properties of BODIPY, making them perfectly suitable for the design of fluorometric sensor arrays for heavy-metal ions. 12 cross-reactive BODIPY fluorescent indicators provide facile identification of the heavy-metal ions using a standard chemometric approach (hierarchical clustering analysis); no misclassifications were found over 45 trials. Clear differentiation among heavy-metal ions as a function of concentration was also achieved, even down to 10(-7)M. A semi-quantitative interpolation of the heavy-metal concentration is obtained by comparing the total Euclidean distance of the measurement with a set of known concentrations in the library. Copyright © 2013 Elsevier B.V. All rights reserved.

Selective ion accumulation in an ICP/ITMS using a filtered noise field

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eiden, G.C.; Barinaga, C.J.; Koppenaal, D.W.

1995-12-31

Selective accumulation of ions in an ion trap mass spectrometer (ITMS) has been characterized using both single frequency and broadband resonant excitation. The goal of this work is to enhance selective accumulation of ions from plasmas and other external ion sources. The charge capacity of the ITMS is 10{sup 6} to 10{sup 7} ions, although the mass spectrum is distorted at much lower space charge. Detection of trace ions necessitates selective detection schemes such as selective trapping or optical detection. The authors report results of selective trapping studies for Sr, Y, and Zr solutions (100 ppb Y and 1 ppbmore » each Sr, Zr). {open_quotes}Background{close_quotes} ions in mass channels adjacent to the channel of interest is a worst case situation with respect to selective ejection and abundance sensitivity. Real samples will often have matrix ion m/z values much further removed from the m/z of the ions of interest. Thus, the authors also give results for a multielement solution. Ions from an inductively coupled plasma ion source are endcap injected into the ITMS. Broadband waveforms were generated by an HST-1000 (Teledyne MEC) instrument, using the filtered noise field (FNF) method. The experiment is controlled by the ITMS electronics and ICMS software. The sequence of experimental events is: ion injection at q{sub z} = 0.4 (typical), collisionally cool ions, set trapping potential for resonant excitation (q{sub z} = 0.2 to 0.6), analysis rf ramp.« less

Direct real-time detection of vapors from explosive compounds.

PubMed

Ewing, Robert G; Clowers, Brian H; Atkinson, David A

2013-11-19

The real-time detection of vapors from low volatility explosives including PETN, tetryl, RDX, and nitroglycerine along with various compositions containing these substances was demonstrated. This was accomplished with an atmospheric flow tube (AFT) using a nonradioactive ionization source coupled to a mass spectrometer. Direct vapor detection was accomplished in less than 5 s at ambient temperature without sample preconcentration. The several seconds of residence time of analytes in the AFT provided a significant opportunity for reactant ions to interact with analyte vapors to achieve ionization. This extended reaction time, combined with the selective ionization using the nitrate reactant ions (NO3(-) and NO3(-)·HNO3), enabled highly sensitive explosives detection from explosive vapors present in ambient laboratory air. Observed signals from diluted explosive vapors indicated detection limits below 10 ppqv using selected ion monitoring (SIM) of the explosive-nitrate adduct at m/z 349, 378, 284, and 289 for tetryl, PETN, RDX, and NG, respectively. Also provided is a demonstration of the vapor detection from 10 different energetic formulations sampled in ambient laboratory air, including double base propellants, plastic explosives, and commercial blasting explosives using SIM for the NG, PETN, and RDX product ions.

Dissociative Recombination of Molecular Ions for Astrochemistry

NASA Astrophysics Data System (ADS)

Novotny, Oldrich; Becker, A.; Buhr, H.; Fleischmann, Andreas; Gamer, Lisa; Geppert, W.; Krantz, C.; Kreckel, H.; Schwalm, D.; Spruck, K.; Wolf, A.; Savin, Daniel Wolf

2014-06-01

Dissociative recombination (DR) of molecular ions is a key chemical process in the cold interstellar medium (ISM). DR affects the composition, charge state, and energy balance of such environments. Astrochemical models of the ISM require reliable total DR cross sections as well as knowledge of the chemical composition of the neutral DR products. We have systematically measured DR for many astrophysically relevant molecular ions utilizing the TSR storage ring at the Max-Planck-Institute for Nuclear Physics (MPIK) in Heidelberg, Germany. We used the merged ion-electron beam technique combined with an energy- and position-sensitive imaging detector and are able to study DR down to plasma temperatures as low as 10 K. The DR count rate is used to obtain an absolute merged beams DR rate coefficient from which we can derive a thermal rate coefficient needed for plasma models. Additionally we determine the masses of the DR products by measuring their kinetic energy in the laboratory reference frame. This allows us to assign particular DR fragmentation channels and to obtain their branching ratios. All this information is particularly important for understanding DR of heteronuclear polyatomic ions. We will present DR results for several ions recently investigated at TSR. A new Cryogenic Storage Ring (CSR) is currently being commissioned at MPIK. With the chamber cooled down to ~10 K and a base pressure better than 10-13 mbar, this setup will allow internal cooling of the stored ions down to their rotational ground states, thus opening a new era in DR experiments. New technological challenges arise due to the ultracold, ultra-high vacuum environment of the CSR and thus the detection techniques used at TSR cannot be easily transferred to CSR. We will present new approaches for DR fragment detection in cryogenic environment. This work is supported in part by NASA and the NSF.

Ion mobility spectrometer using frequency-domain separation

DOEpatents

Martin, S.J.; Butler, M.A.; Frye, G.C.; Schubert, W.K.

1998-08-04

An apparatus and method are provided for separating and analyzing chemical species in an ion mobility spectrometer using a frequency-domain technique wherein the ions generated from the chemical species are selectively transported through an ion flow channel having a moving electrical potential therein. The moving electrical potential allows the ions to be selected according to ion mobility, with certain of the ions being transported to an ion detector and other of the ions being effectively discriminated against. The apparatus and method have applications for sensitive chemical detection and analysis for monitoring of exhaust gases, hazardous waste sites, industrial processes, aerospace systems, non-proliferation, and treaty verification. The apparatus can be formed as a microelectromechanical device (i.e. a micromachine). 6 figs.

Structural characterization by both positive and negative electrospray ion trap mass spectrometry of oligogalacturonates purified by high-performance anion-exchange chromatography.

PubMed

Quéméner, Bernard; Désiré, Cédric; Debrauwer, Laurent; Rathahao, Estelle

2003-01-17

The off-line coupling of high-performance anion-exchange chromatography to electrospray ion trap mass spectrometry (ESI-IT-MS) is described. Two sets of isocratic conditions were optimised for the semi-preparative purification of oligogalacturonates of degree of polymerisation from 4 to 6 by monitoring eluates with either pulsed amperometric detection or evaporative light scattering detection in the presence of an online Dionex Carbohydrate Membrane Desalter (CMD). In these conditions, purified oligogalacturonate solutions were suitable, without further desalting steps, for infusion ESI-IT-MS experiments. This paper provides some interesting features of positive and negative ESI-IT-multiple MS (MSn) of these acidic oligosaccharides. The spectra acquired in both ion modes show characteristic fragments resulting from glycosidic bond and cross-ring cleavages. Under negative ionization conditions, the fragmentation of the singly-charged [M-H]- ions, as well as the Ci-, and Zi-, fragment ions through sequential MSn experiments, was always dominated by product ions from C- and Z-type glycosidic cleavages. All spectra also displayed 0.2 A-type cross-ring cleavage ions which carry linkage information. Collision-induced dissociation (CID) spectra of sodium-cationized species obtained under positive ionization conditions were more complex. Successive MSn experiments also led to the 0.2 A-type cross-ring cleavage ions observed together with B- and Y-type ions. The presence of the 0.2 A ion series was related to Mr 60 (C2H4O2) losses. Combined with the absence of the Mr 30 (CH2O) and the Mr 90 (C3H6O3) ions, these ions were indicative of 1-4 type glycosidic linkage.

Measurement and Simulation of First-Orbit Fast-Ion D-Alpha Emission and the Application to Fast-Ion Loss Detection in the DIII-D Tokamak

NASA Astrophysics Data System (ADS)

Bolte, Nathan; Heidbrink, W. W.; Pace, D. C.; van Zeeland, M. A.; Chen, X.

2015-11-01

A new fast-ion diagnostic method uses passive emission of D-alpha radiation to determine fast-ion losses quantitatively. The passive fast-ion D-alpha simulation (P-FIDAsim) forward models the Doppler-shifted spectra of first-orbit fast ions that charge exchange with edge neutrals. Simulated spectra are up to 80 % correlated with experimental spectra. Calibrated spectra are used to estimate the 2D neutral density profile by inverting simulated spectra. The inferred neutral density shows the expected increase toward each x-point and an average value of 8 × 10 9 cm-3 at the plasma boundary and 1 × 10 11 cm-3 near the wall. Measuring and simulating first-orbit spectra effectively ``calibrates'' the system, allowing for the quantification of more general fast-ion losses. Sawtooth crashes are estimated to eject 1.2 % of the fast-ion inventory, in good agreement with a 1.7 % loss estimate made by TRANSP. Sightlines sensitive to passing ions observe larger sawtooth losses than sightlines sensitive to trapped ions. Supported by US DOE under SC-G903402, DE-FC02-04ER54698.

Fluorescent and colorimetric ion probes based on conjugated oligopyrroles.

PubMed

Ding, Yubin; Tang, Yunyu; Zhu, Weihong; Xie, Yongshu

2015-03-07

Metal ions and anions play important roles in many industrial and biochemical processes, and thus it is highly desired to detect them in the relevant systems. Small organic molecule based sensors for selective and sensitive detection of target ions show the advantages of low cost, high sensitivity and convenient implementation. In this area, pyrrole has incomparable advantages. It can be easily incorporated into linear and macrocyclic conjugated structures such as dipyrrins, porphyrins, and N-confused porphyrins, which may utilize the imino N and amino NH moieties for binding metal ions and anions, respectively. In this tutorial review, we focus on representative examples to describe the design, syntheses, sensing mechanisms, and applications of the conjugated oligopyrroles. These compounds could be used as colorimetric or fluorescent ion probes, with the advantages of vivid colour and fluorescence changes, easy structural modification and functionalization, and tunable emission wavelengths. Compared with normal porphyrins, simple di- and tripyrrins, as well as some porphyrinoids are more suitable for designing fluorescence "turn-on" metal probes, because they may exhibit flexible confirmations, and metal coordination will improve the rigidity, resulting in vivid fluorescence enhancement. It is noteworthy that the oligopyrrolic moieties may simultaneously act as the binding unit as well as the reporting moiety, which simplifies the design and syntheses of the probes.

Detection of immunocytological markers in photomicroscopic images

NASA Astrophysics Data System (ADS)

Friedrich, David; zur Jacobsmühlen, Joschka; Braunschweig, Till; Bell, André; Chaisaowong, Kraisorn; Knüchel-Clarke, Ruth; Aach, Til

2012-03-01

Early detection of cervical cancer can be achieved through visual analysis of cell anomalies. The established PAP smear achieves a sensitivity of 50-90%, most false negative results are caused by mistakes in the preparation of the specimen or reader variability in the subjective, visual investigation. Since cervical cancer is caused by human papillomavirus (HPV), the detection of HPV-infected cells opens new perspectives for screening of precancerous abnormalities. Immunocytochemical preparation marks HPV-positive cells in brush smears of the cervix with high sensitivity and specificity. The goal of this work is the automated detection of all marker-positive cells in microscopic images of a sample slide stained with an immunocytochemical marker. A color separation technique is used to estimate the concentrations of the immunocytochemical marker stain as well as of the counterstain used to color the nuclei. Segmentation methods based on Otsu's threshold selection method and Mean Shift are adapted to the task of segmenting marker-positive cells and their nuclei. The best detection performance of single marker-positive cells was achieved with the adapted thresholding method with a sensitivity of 95.9%. The contours differed by a modified Hausdorff Distance (MHD) of 2.8 μm. Nuclei of single marker positive cells were detected with a sensitivity of 95.9% and MHD = 1.02 μm.

A Colorimetric and Fluorescent Probe for the Detection of Cu2+ in a Complete Aqueous Solution.

PubMed

Xu, Jing; Wang, Zuokai; Liu, Caiyun; Xu, Zhenghe; Zhu, Baocun; Wang, Ning; Wang, Kun; Wang, Jiangting

2018-01-01

The fluorescent probe has become an important method for the detection of heavy metal ions. In the present work, a new and simple fluorescent probe, Cu-P, for detecting copper ion (Cu 2+ ) was designed and synthesized. The probe has shown high sensitivity and selectivity toward Cu 2+ . The detection limit was 13 nM (based on the 3σ/slope). A significant color change from yellow to pink was observed; thus, the probe Cu-P could serve as a "naked-eye" indicator for Cu 2+ . Furthermore, the proposed probe was used to detect Cu 2+ in real water and soil extract samples, with the result being satisfactory. Therefore, our proposed probe would provide a promising method for the detection of Cu 2+ in the environment.

Detection of heavy-metal ions using liquid crystal droplet patterns modulated by interaction between negatively charged carboxylate and heavy-metal cations.

PubMed

Han, Gyeo-Re; Jang, Chang-Hyun

2014-10-01

Herein, we demonstrated a simple, sensitive, and rapid label-free detection method for heavy-metal (HM) ions using liquid crystal (LC) droplet patterns on a solid surface. Stearic-acid-doped LC droplet patterns were spontaneously generated on an n-octyltrichlorosilane (OTS)-treated glass substrate by evaporating a solution of the nematic LC, 4-cyano-4'-pentylbiphenyl (5CB), dissolved in heptane. The optical appearance of the droplet patterns was a dark crossed texture when in contact with air, which represents the homeotropic orientation of the LC. This was caused by the steric interaction between the LC molecules and the alkyl chains of the OTS-treated surface. The dark crossed appearance of the acid-doped LC patterns was maintained after the addition of phosphate buffered saline (PBS) solution (pH 8.1 at 25°C). The deprotonated stearic-acid molecules self-assembled through the LC/aqueous interface, thereby supporting the homeotropic anchoring of 5CB. However, the optical image of the acid-doped LC droplet patterns incubated with PBS containing HM ions appeared bright, indicating a planar orientation of 5CB at the aqueous/LC droplet interface. This dark to bright transition of the LC patterns was caused by HM ions attached to the deprotonated carboxylate moiety, followed by the sequential interruption of the self-assembly of the stearic acid at the LC/aqueous interface. The results showed that the acid-doped LC pattern system not only enabled the highly sensitive detection of HM ions at a sub-nanomolar concentration but it also facilitated rapid detection (<10 min) with simple procedures. Copyright © 2014 Elsevier B.V. All rights reserved.

Motional studies of one and two laser-cooled trapped ions for electric-field sensing applications

NASA Astrophysics Data System (ADS)

Domínguez, F.; Gutiérrez, M. J.; Arrazola, I.; Berrocal, J.; Cornejo, J. M.; Del Pozo, J. J.; Rica, R. A.; Schmidt, S.; Solano, E.; Rodríguez, D.

2018-03-01

We have studied the dynamics of one and two laser-cooled trapped ?Ca? ions by applying electric fields of different nature along the axial direction of the trap, namely, driving the motion with a harmonic dipolar field, or with white noise. These two types of driving induce distinct motional states of the axial modes: a coherent oscillation with the dipolar field, or an enhanced Brownian motion due to an additional contribution to the heating rate from the electric noise. In both scenarios, the sensitivity of an isolated ion and a laser-cooled two-ion crystal has been evaluated and compared. The analysis and understanding of this dynamics is important towards the implementation of a novel Penning trap mass-spectroscopy technique based on optical detection, aiming at improving precision and sensitivity.

Enhancement in sensitivity of copper sulfide thin film ammonia gas sensor: Effect of swift heavy ion irradiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sagade, Abhay Abhimanyu; Sharma, Ramphal; Department of Chemistry, Hanyang University, Sungdong-Ku, Haengdang-dong 17, Seoul 133-791

2009-02-15

The studies are carried out on the effect of swift heavy ion (SHI) irradiation on surface morphology and electrical properties of copper sulfide (Cu{sub x}S) thin films with three different chemical compositions (x values). The irradiation experiments have been carried out on Cu{sub x}S films with x=1.4, 1.8, and 2 by 100 MeV gold heavy ions at room temperature. These as-deposited and irradiated thin films have been used to detect ammonia gas at room temperature (300 K). The SHI irradiation treatment on x=1.4 and 1.8 copper sulfide films enhances the sensitivity of the gas sensor. The results are discussed consideringmore » high electronic energy deposition by 100 MeV gold heavy ions in a matrix of copper sulfide.« less

Nonfaradaic nanoporous electrochemistry for conductometry at high electrolyte concentration.

PubMed

Bae, Je Hyun; Kang, Chung Mu; Choi, Hyoungseon; Kim, Beom Jin; Jang, Woohyuk; Lim, Sung Yul; Kim, Hee Chan; Chung, Taek Dong

2015-02-17

Nanoporous electrified surfaces create a unique nonfaradaic electrochemical behavior that is sensitively influenced by pore size, morphology, ionic strength, and electric field modulation. Here, we report the contributions of ion concentration and applied ac frequency to the electrode impedance through an electrical double layer overlap and ion transport along the nanopores. Nanoporous Pt with uniform pore size and geometry (L2-ePt) responded more sensitively to conductivity changes in aqueous solutions than Pt black with poor uniformity despite similar real surface areas and enabled the previously difficult quantitative conductometry measurements at high electrolyte concentrations. The nanopores of L2-ePt were more effective in reducing the electrode impedance and exhibited superior linear responses to not only flat Pt but also Pt black, leading to successful conductometric detection in ion chromatography without ion suppressors and at high ionic strengths.

Ultrahigh-performance liquid chromatography/electrospray ionization linear ion trap Orbitrap mass spectrometry of antioxidants (amines and phenols) applied in lubricant engineering.

PubMed

Kassler, Alexander; Pittenauer, Ernst; Doerr, Nicole; Allmaier, Guenter

2014-01-15

For the qualification and quantification of antioxidants (aromatic amines and sterically hindered phenols), most of them applied as lubricant additives, two ultrahigh-performance liquid chromatography (UHPLC) electrospray ionization mass spectrometric methods applying the positive and negative ion mode have been developed for lubricant design and engineering thus allowing e.g. the study of the degradation of lubricants. Based on the different chemical properties of the two groups of antioxidants, two methods offering a fast separation (10 min) without prior derivatization were developed. In order to reach these requirements, UHPLC was coupled with an LTQ Orbitrap hybrid tandem mass spectrometer with positive and negative ion electrospray ionization for simultaneous detection of spectra from UHPLC-high-resolution (HR)-MS (full scan mode) and UHPLC-low-resolution linear ion trap MS(2) (LITMS(2)), which we term UHPLC/HRMS-LITMS(2). All 20 analytes investigated could be qualified by an UHPLC/HRMS-LITMS(2) approach consisting of simultaneous UHPLC/HRMS (elemental composition) and UHPLC/LITMS(2) (diagnostic product ions) according to EC guidelines. Quantification was based on an UHPLC/LITMS(2) approach due to increased sensitivity and selectivity compared to UHPLC/HRMS. Absolute quantification was only feasible for seven analytes with well-specified purity of references whereas relative quantification was obtainable for another nine antioxidants. All of them showed good standard deviation and repeatability. The combined methods allow qualitative and quantitative determination of a wide variety of different antioxidants including aminic/phenolic compounds applied in lubricant engineering. These data show that the developed methods will be versatile tools for further research on identification and characterization of the thermo-oxidative degradation products of antioxidants in lubricants. Copyright © 2013 John Wiley & Sons, Ltd.

Mass spectrometer calibration of Cosmic Dust Analyzer

NASA Astrophysics Data System (ADS)

Ahrens, Thomas J.; Gupta, Satish C.; Jyoti, G.; Beauchamp, J. L.

2003-02-01

The time-of-flight (TOF) mass spectrometer (MS) of the Cosmic Dust Analyzer (CDA) instrument aboard the Cassini spacecraft is expected to be placed in orbit about Saturn to sample submicrometer-diameter ring particles and impact ejecta from Saturn's satellites. The CDA measures a mass spectrum of each particle that impacts the chemical analyzer sector of the instrument. Particles impact a Rh target plate at velocities of 1-100 km/s and produce some 10-8 to 10-5 times the particle mass of positive valence, single-charged ions. These are analyzed via a TOF MS. Initial tests employed a pulsed N2 laser acting on samples of kamacite, pyrrhotite, serpentine, olivine, and Murchison meteorite induced bursts of ions which were detected with a microchannel plate and a charge sensitive amplifier (CSA). Pulses from the N2 laser (1011 W/cm2) are assumed to simulate particle impact. Using aluminum alloy as a test sample, each pulse produces a charge of ~4.6 pC (mostly Al+1), whereas irradiation of a stainless steel target produces a ~2.8 pC (Fe+1) charge. Thus the present system yields ~10-5% of the laser energy in resulting ions. A CSA signal indicates that at the position of the microchannel plate, the ion detector geometry is such that some 5% of the laser-induced ions are collected in the CDA geometry. Employing a multichannel plate detector in this MS yields for Al-Mg-Cu alloy and kamacite targets well-defined peaks at 24 (Mg+1), 27(Al+1), and 64 (Cu+1) and 56 (Fe+1), 58 (Ni+1), and 60 (Ni+1) dalton, respectively.

A carbon dot-based "off-on" fluorescent probe for highly selective and sensitive detection of phytic acid.

PubMed

Gao, Zhao; Wang, Libing; Su, Rongxin; Huang, Renliang; Qi, Wei; He, Zhimin

2015-08-15

We herein report a facile, one-step pyrolysis synthesis of photoluminescent carbon dots (CDs) using citric acid as the carbon source and lysine as the surface passivation reagent. The as-prepared CDs show narrow size distribution, excellent blue fluorescence and good photo-stability and water dispersivity. The fluorescence of the CDs was found to be effectively quenched by ferric (Fe(III)) ions with high selectivity via a photo-induced electron transfer (PET) process. Upon addition of phytic acid (PA) to the CDs/Fe(III) complex dispersion, the fluorescence of the CDs was significantly recovered, arising from the release of Fe(III) ions from the CDs/Fe(III) complex because PA has a higher affinity for Fe(III) ions compared to CDs. Furthermore, we developed an "off-on" fluorescence assay method for the detection of phytic acid using CDs/Fe(III) as a fluorescent probe. This probe enables the selective detection of PA with a linear range of 0.68-18.69 μM and a limit of detection (signal-to-noise ratio is 3) of 0.36 μM. The assay method demonstrates high selectivity, repeatability, stability and recovery ratio in the detection of the standard and real PA samples. We believe that the facile operation, low-cost, high sensitivity and selectivity render this CD-based "off-on" fluorescent probe an ideal sensing platform for the detection of PA. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of Solvent and Ion Source Pressure on the Analysis of Anabolic Steroids by Low Pressure Photoionization Mass Spectrometry.

PubMed

Liu, Chengyuan; Zhu, Yanan; Yang, Jiuzhong; Zhao, Wan; Lu, Deen; Pan, Yang

2017-04-01

Solvent and ion source pressure were two important factors relating to the photon induced ion-molecule reactions in low pressure photoionization (LPPI). In this work, four anabolic steroids were analyzed by LPPI mass spectrometry. Both the ion species present and their relative abundances could be controlled by switching the solvent and adjusting the ion source pressure. Whereas M •+ , MH + , [M - H 2 O] + , and solvent adducts were observed in positive LPPI, [M - H] - and various oxidation products were abundant in negative LPPI. Changing the solvent greatly affected formation of the ion species in both positive and negative ion modes. The ion intensities of the solvent adduct and oxygen adduct were selectively enhanced when the ion source pressure was elevated from 68 to 800 Pa. The limit of detection could be decreased by increasing the ion source pressure. Graphical Abstract ᅟ.

Effects of Solvent and Ion Source Pressure on the Analysis of Anabolic Steroids by Low Pressure Photoionization Mass Spectrometry

NASA Astrophysics Data System (ADS)

Liu, Chengyuan; Zhu, Yanan; Yang, Jiuzhong; Zhao, Wan; Lu, Deen; Pan, Yang

2017-04-01

Solvent and ion source pressure were two important factors relating to the photon induced ion-molecule reactions in low pressure photoionization (LPPI). In this work, four anabolic steroids were analyzed by LPPI mass spectrometry. Both the ion species present and their relative abundances could be controlled by switching the solvent and adjusting the ion source pressure. Whereas M•+, MH+, [M - H2O]+, and solvent adducts were observed in positive LPPI, [M - H]- and various oxidation products were abundant in negative LPPI. Changing the solvent greatly affected formation of the ion species in both positive and negative ion modes. The ion intensities of the solvent adduct and oxygen adduct were selectively enhanced when the ion source pressure was elevated from 68 to 800 Pa. The limit of detection could be decreased by increasing the ion source pressure.

Imaging radiation detector with gain

DOEpatents

Morris, C.L.; Idzorek, G.C.; Atencio, L.G.

1982-07-21

A radiation imaging device which has application in x-ray imaging. The device can be utilized in CAT scanners and other devices which require high sensitivity and low x-ray fluxes. The device utilizes cumulative multiplication of charge carriers on the anode plane and the collection of positive ion charges to image the radiation intensity on the cathode plane. Parallel and orthogonal cathode wire arrays are disclosed as well as a two-dimensional grid pattern for collecting the positive ions on the cathode.

Imaging radiation detector with gain

DOEpatents

Morris, Christopher L.; Idzorek, George C.; Atencio, Leroy G.

1984-01-01

A radiation imaging device which has application in x-ray imaging. The device can be utilized in CAT scanners and other devices which require high sensitivity and low x-ray fluxes. The device utilizes cumulative multiplication of charge carriers on the anode plane and the collection of positive ion charges to image the radiation intensity on the cathode plane. Parallel and orthogonal cathode wire arrays are disclosed as well as a two-dimensional grid pattern for collecting the positive ions on the cathode.

Beam-centroid tracking instrument for ion thrusters

NASA Astrophysics Data System (ADS)

Pollard, J. E.

1995-03-01

Thrust vector stability for an electrostatic ion engine can be measured with improved sensitivity and time resolution by the method described here. Four double-wire Langmuir probes, aligned in the form of a cross, are placed in the exhaust plume and are translated by a motorized positioning system to balance the currents collected along two orthogonal axes. The thrust vector position is thereby measured with an angular resolution of less than 0.01 deg and a response time of less than 5 sec.

Colorimetric anion sensors based on positional effect of nitro group for recognition of biologically relevant anions in organic and aqueous medium, insight real-life application and DFT studies

NASA Astrophysics Data System (ADS)

Singh, Archana; Sahoo, Suban K.; Trivedi, Darshak R.

2018-01-01

A new six colorimetric receptors A1-A6 were designed and synthesized, characterized by typical common spectroscopic techniques like FT-IR, UV-Visible, 1H NMR, 13C NMR and ESI-MS. The receptor A1 and A2 exhibit a significant naked-eye response towards F- and AcO- ions in DMSO. Due to presences of the NO2 group at para and ortho position with extended π-conjugation of naphthyl group carrying sbnd OH as a binding site. Compared to receptor A2, A1 is extremely capable of detecting F- and AcO- ions present in the form of sodium salts in an aqueous medium. This is owed to the occurrence of sbnd NO2 group at para position induced in increasing the acidity of sbnd OH proton. Consequently, it easily gets deprotonated in aqueous media. The detection limit of receptor A1 was turned out to be 0.40 and 0.35 ppm for F- and AcO- ions which is beneath WHO permission level (1.0 ppm). Receptor A1 shows a solitary property of solvatochromism in different aprotic solvents in presence of AcO- ion. Receptor A1 depicts high selectivity towards AcO- ion in DMSO: HEPES buffer (9:1, v/v). Receptor A1 proved itself for real life application by detecting anion in solution and solid state. The binding mechanism of receptor A1 with AcO- and F- ions was monitored from 1HNMR titration and DFT study.

An improved experimental scheme for simultaneous measurement of high-resolution zero electron kinetic energy (ZEKE) photoelectron and threshold photoion (MATI) spectra

NASA Astrophysics Data System (ADS)

Michels, François; Mazzoni, Federico; Becucci, Maurizio; Müller-Dethlefs, Klaus

2017-10-01

An improved detection scheme is presented for threshold ionization spectroscopy with simultaneous recording of the Zero Electron Kinetic Energy (ZEKE) and Mass Analysed Threshold Ionisation (MATI) signals. The objective is to obtain accurate dissociation energies for larger molecular clusters by simultaneously detecting the fragment and parent ion MATI signals with identical transmission. The scheme preserves an optimal ZEKE spectral resolution together with excellent separation of the spontaneous ion and MATI signals in the time-of-flight mass spectrum. The resulting improvement in sensitivity will allow for the determination of dissociation energies in clusters with substantial mass difference between parent and daughter ions.

Multianalyte biosensor based on pH-sensitive ZnO electrolyte–insulator–semiconductor structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haur Kao, Chyuan; Chun Liu, Che; Ueng, Herng-Yih

2014-05-14

Multianalyte electrolyte–insulator–semiconductor (EIS) sensors with a ZnO sensing membrane annealed on silicon substrate for use in pH sensing were fabricated. Material analyses were conducted using X-ray diffraction and atomic force microscopy to identify optimal treatment conditions. Sensing performance for various ions of Na{sup +}, K{sup +}, urea, and glucose was also tested. Results indicate that an EIS sensor with a ZnO membrane annealed at 600 °C exhibited good performance with high sensitivity and a low drift rate compared with all other reported ZnO-based pH sensors. Furthermore, based on well-established pH sensing properties, pH-ion-sensitive field-effect transistor sensors have also been developed formore » use in detecting urea and glucose ions. ZnO-based EIS sensors show promise for future industrial biosensing applications.« less

Ratiometric fluorescent nanosensor based on carbon dots for the detection of mercury ion

NASA Astrophysics Data System (ADS)

Ma, Yusha; Mei, Jing; Bai, Jianliang; Chen, Xu; Ren, Lili

2018-05-01

A novel ratiometric fluorescent nanosensor based on carbon dots has been synthesized via bonding rhodamine B hydrazide to the carbon dots surface by an amide reaction. The ratiometric fluorescent nanosensor showed only a single blue fluorescence emission around 450 nm. While, as mercury ion was added, due to the open-ring of rhodamine moiety bonded on the CDs surface, the orange emission of the open-ring rhodamine would increase obviously according to the concentration of mercury ion, resulting in the distinguishable dual emissions at 450 nm and 575 nm under a single 360 excitation wavelength. Meanwhile, the ratiometric fluorescent nanosensor based on carbon dots we prepared is more sensitive to qualitative and semi-quantitative detection of mercury ion in the range of 0–100 μM, because fluorescence changes gradually from blue to orange emission under 365 nm lamp with the increasing of mercury ion in the tested solution.

Low sensitivity of anion gap to detect clinically significant lactic acidosis in the emergency department.

PubMed

Xu, Q; HowlettClyne, S; Fuezery, A; Cembrowski, G S

2017-12-01

Lactic acidosis represents the pathologic accumulation of lactate and hydrogen ions. It is important to efficiently diagnose lactic acidosis as delayed treatment will lead to poor patient outcomes. As plasma lactate levels may not be rapidly available, some physicians may use elevated anion gaps to test for the need to measure lactate. All Edmonton metropolitan hospitals have Radiometer blood gas/electrolyte instruments in the ED or close by. As lactate is measured for each set of electrolytes, we were able to determine the effectiveness of a screening anion gap for lactic acidosis. Two years of emergency department lactates and electrolytes from Edmonton's 5 metropolitan hospitals were analyzed. We determined the sensitivity, specificity and positive predictive value of detecting an elevated lactate, defined as ≥2.5mmol/L or ≥4mmol/L. Depending on the elevated anion gap cut-off and the definition of elevated lactate, between 40-80% of elevated lactates are missed. In general, the positive predictive value approaches 40% for AGs ≥12mmol/L and 60% for AGs ≥16mmol/L. Anion gap is an inadequate marker of lactic acidosis. We recommend that lactate be done with each set of electrolytes and/or blood gases. In this way lactic acidosis will not be missed. Copyright © 2017. Published by Elsevier Inc.

Coexistence of negative and positive polarity electrostatic solitary waves in ultradense relativistic negative-ion-beam permeated plasmas

NASA Astrophysics Data System (ADS)

Elkamash, I. S.; Kourakis, I.

2018-05-01

The criteria for occurrence and the dynamical features of electrostatic solitary waves in a homogeneous, unmagnetized ultradense plasma penetrated by a negative ion beam are investigated, relying on a quantum hydrodynamic model. The ionic components are modeled as inertial fluids, while the relativistic electrons obey Fermi-Dirac statistics. A new set of exact analytical conditions for localized solitary pulses to exist is obtained, in terms of plasma density. The algebraic analysis reveals that these depend sensitively on the negative ion beam characteristics, that is, the beam velocity and density. Particular attention is paid to the simultaneous occurrence of positive and negative potential pulses, identified by their respective distinct ambipolar electric field structure forms. It is shown that the coexistence of positive and negative potential pulses occurs in a certain interval of parameter values, where the ion beam inertia becomes significant.

A novel surface-enhanced Raman scattering nanosensor for detecting multiple heavy metal ions based on 2-mercaptoisonicotinic acid functionalized gold nanoparticles.

PubMed

Tan, Enzhong; Yin, Penggang; Lang, Xiufeng; Zhang, Hongyan; Guo, Lin

2012-11-01

A novel, effective and simple surface-enhanced Raman scattering (SERS) nanosensor for selectively and sensitively detecting heavy metal ions in aqueous solution has been developed in the form of 2-mercaptoisonicotinic acid (2 MNA)-modified gold nanoparticles (AuNPs). Multiple heavy metal ions can be identified and quantified by using relative peak intensity ratios of selected vibrational bands in the SERS spectra of 2 MNA. Especially, concentration of Hg(2+) and Pb(2+) ions are determined by comparing the intensity ratios of the bands 1160/1230 cm(-1) for Hg(2+) and 861/815 cm(-1) (or 815/1392 cm(-1)) for Pb(2+), with detection limits of 3.4×10(-8) and 1.0×10(-7)M, respectively. 2 MNA-AuNPs sensors show a high selectivity for Hg(2+) without masking reagent, and they can also be highly selective for Pb(2+) when using sodium thiosulphate and l-cysteine as masking reagents. These results demonstrate that these 2 MNA-AuNPs nanosensors are promising candidates for in situ heavy metal ions detection and quantification, maybe even inside living cells. Copyright © 2012 Elsevier B.V. All rights reserved.

Nanoscale detection of bacteriophage triggered ion cascade (Invited Paper)

NASA Astrophysics Data System (ADS)

Dobozi-King, Maria; Seo, Sungkyu; Kim, Jong U.; Cheng, Mosong; Kish, Laszlo B.; Young, Ryland

2005-05-01

In an era of potential bioterrorism and pandemics of antibiotic-resistant microbes, bacterial contaminations of food and water supplies is a major concern. There is an urgent need for the rapid, inexpensive and specific identification of bacteria under field conditions. Here we describe a method that combines the specificity and avidity of bacteriophages with fluctuation analysis of electrical noise. The method is based on the massive, transitory ion leakage that occurs at the moment of phage DNA injection into the host cell. The ion fluxes require only that the cells be physiologically viable (i.e., have energized membranes) and can occur within seconds after mixing the cells with sufficient concentrations of phage particles. To detect these fluxes, we have constructed a nano-well, a lateral, micron-size capacitor of titanium electrodes with gap size of 150 nm, and used it to measure the electrical field fluctuations in microliter (mm3) samples containing phage and bacteria. In mixtures where the analyte bacteria were sensitive to the phage, large stochastic waves with various time and amplitude scales were observed, with power spectra of approximately 1/f2 shape over at 1 - 10 Hz. Development of this SEPTIC (SEnsing of Phage-Triggered Ion Cascades) technology could provide rapid detection and identification of live, pathogenic bacteria on the scale of minutes, with unparalleled specificity. The method has a potential ultimate sensitivity of 1 bacterium/microliter (1 bacterium/mm3).

Dual-peak electrogenerated chemiluminescence of carbon dots for iron ions detection.

PubMed

Zhang, Pengjia; Xue, Zhenjie; Luo, Dan; Yu, Wei; Guo, Zhihui; Wang, Tie

2014-06-17

Carbon dots (CDs) have rigorously been investigated on their unique fluorescent properties but rarely their electrogenerated chemiluminescence (ECL) behavior. We are here to report a dual-peak ECL system of CDs, one at -2.84 V (ECL-1) and the other at -1.71 V (ECL-2) during the cyclic sweep between -3.0 and 3.0 V at scan rate of 0.2 V s(-1) in 0.1 M tetrabutyl ammonium bromide (TBAB) ethanol solution, which is more efficiency to distinguish metallic ions than single-peak ECL. The electron transfer reaction between individual electrochemically reduced nanocrystal species and coreactants led to ECL-1, in which the electron injected to the conduction band of CDs in the cathodic process. Ion annihilation reactions induced direct formation of exciplexes that produced another ECL signal, ECL-2. ECL-1 showed higher sensitivity to the surrounding environment than ECL-2 and thus was used for ECL detection of metallic ions. Herein, we can serve as an internal standard method to detect iron ions. A linear relationship of the intensity ratio R of ECL-1 and ECL-2 to iron ions was observed in the concentration extending from 5 × 10(-6) to 8 × 10(-5) M with a detection limit of 7 × 10(-7) M.

Wavelet method for CT colonography computer-aided polyp detection.

PubMed

Li, Jiang; Van Uitert, Robert; Yao, Jianhua; Petrick, Nicholas; Franaszek, Marek; Huang, Adam; Summers, Ronald M

2008-08-01

Computed tomographic colonography (CTC) computer aided detection (CAD) is a new method to detect colon polyps. Colonic polyps are abnormal growths that may become cancerous. Detection and removal of colonic polyps, particularly larger ones, has been shown to reduce the incidence of colorectal cancer. While high sensitivities and low false positive rates are consistently achieved for the detection of polyps sized 1 cm or larger, lower sensitivities and higher false positive rates occur when the goal of CAD is to identify "medium"-sized polyps, 6-9 mm in diameter. Such medium-sized polyps may be important for clinical patient management. We have developed a wavelet-based postprocessor to reduce false positives for this polyp size range. We applied the wavelet-based postprocessor to CTC CAD findings from 44 patients in whom 45 polyps with sizes of 6-9 mm were found at segmentally unblinded optical colonoscopy and visible on retrospective review of the CT colonography images. Prior to the application of the wavelet-based postprocessor, the CTC CAD system detected 33 of the polyps (sensitivity 73.33%) with 12.4 false positives per patient, a sensitivity comparable to that of expert radiologists. Fourfold cross validation with 5000 bootstraps showed that the wavelet-based postprocessor could reduce the false positives by 56.61% (p <0.001), to 5.38 per patient (95% confidence interval [4.41, 6.34]), without significant sensitivity degradation (32/45, 71.11%, 95% confidence interval [66.39%, 75.74%], p=0.1713). We conclude that this wavelet-based postprocessor can substantially reduce the false positive rate of our CTC CAD for this important polyp size range.

Colorimetric assay of copper ions based on the inhibition of peroxidase-like activity of MoS2 nanosheets

NASA Astrophysics Data System (ADS)

Chen, Huan; Li, Zhihong; Liu, Xueting; Zhong, Jianhai; Lin, Tianran; Guo, Liangqia; Fu, Fengfu

2017-10-01

The peroxidase-like catalytic activity of MoS2 nanomaterials has been utilized for colorimetric bioassays and medical diagnostics. However, the application of peroxidase-like catalytic activity of MoS2 nanomaterials in environmental analysis was seldom explored. Herein, copper ions were found to inhibit the peroxidase-like catalytic activity of MoS2 nanosheets, which can catalyze the oxidation of 3, 3‧, 5, 5‧-tetramethylbenzidine by H2O2 to produce a colorimetric product. Based on this finding, a simple sensitive colorimetric method for the detection of copper ions was developed. In the presence of copper ions, the absorbance and color of the solution decreased with the increasing concentration of copper ions. The color of the solution can be used to semi-quantitative on-site assay of copper ions by naked eyes. A linear relationship between the absorbance and the concentration of copper ions was observed in the range of 0.4-4.0 μmol L- 1 with a detection limit of 92 nmol L- 1, which was much lower than the maximum contaminant level of copper in drinking water legislated by the Environmental Protection Agency of USA and the World Health Organization. The method was applied to detect copper ions in environmental water samples with satisfactory results.

Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry.

PubMed

Kaufmann, Anton; Widmer, Mirjam; Maden, Kathryn; Butcher, Patrick; Walker, Stephan

2018-03-05

A reversed-phase ion-pairing chromatographic method was developed for the detection and quantification of inorganic and organic anionic food additives. A single-stage high-resolution mass spectrometer (orbitrap ion trap, Orbitrap) was used to detect the accurate masses of the unfragmented analyte ions. The developed ion-pairing chromatography method was based on a dibutylamine/hexafluoro-2-propanol buffer. Dibutylamine can be charged to serve as a chromatographic ion-pairing agent. This ensures sufficient retention of inorganic and organic anions. Yet, unlike quaternary amines, it can be de-charged in the electrospray to prevent the formation of neutral analyte ion-pairing agent adducts. This process is significantly facilitated by the added hexafluoro-2-propanol. This approach permits the sensitive detection and quantification of additives like nitrate and mono-, di-, and triphosphate as well as citric acid, a number of artificial sweeteners like cyclamate and aspartame, flavor enhancers like glutamate, and preservatives like sorbic acid. This is a major advantage, since the currently used analytical methods as utilized in food safety laboratories are only capable in monitoring a few compounds or a particular category of food additives. Graphical abstract Deptotonation of ion pair agent in the electrospray interface.

Rapid and sensitive approach to simultaneous detection of genomes of hepatitis A, B, C, D and E viruses.

PubMed

Kodani, Maja; Mixson-Hayden, Tonya; Drobeniuc, Jan; Kamili, Saleem

2014-10-01

Five viruses have been etiologically associated with viral hepatitis. Nucleic acid testing (NAT) remains the gold standard for diagnosis of viremic stages of infection. NAT methodologies have been developed for all hepatitis viruses; however, a NAT-based assay that can simultaneously detect all five viruses is not available. We designed TaqMan card-based assays for detection of HAV RNA, HBV DNA, HCV RNA, HDV RNA and HEV RNA. The performances of individual assays were evaluated on TaqMan Array Cards (TAC) for detecting five viral genomes simultaneously. Sensitivity and specificity were determined by testing 329 NAT-tested clinical specimens. All NAT-positive samples for HCV (n = 32), HDV (n = 28) and HEV (n = 14) were also found positive in TAC (sensitivity, 100%). Forty-three of 46 HAV-NAT positive samples were also positive in TAC (sensitivity, 94%), while 36 of 39 HBV-NAT positive samples were positive (sensitivity, 92%). No false-positives were detected for HBV (n = 32), HCV (n = 36), HDV (n = 30), and HEV (n = 31) NAT-negative samples (specificity 100%), while 38 of 41 HAV-NAT negative samples were negative by TAC (specificity 93%). TAC assay was concordant with corresponding individual NATs for hepatitis A-E viral genomes and can be used for their detection simultaneously. The TAC assay has potential for use in hepatitis surveillance, for screening of donor specimens and in outbreak situations. Wider availability of TAC-ready assays may allow for customized assays, for improving acute jaundice surveillance and for other purposes for which there is need to identify multiple pathogens rapidly. Published by Elsevier B.V.

Fast detection of narcotics by single photon ionization mass spectrometry and laser ion mobility spectrometry

NASA Astrophysics Data System (ADS)

Laudien, Robert; Schultze, Rainer; Wieser, Jochen

2010-10-01

In this contribution two analytical devices for the fast detection of security-relevant substances like narcotics and explosives are presented. One system is based on an ion trap mass spectrometer (ITMS) with single photon ionization (SPI). This soft ionization technique, unlike electron impact ionization (EI), reduces unwanted fragment ions in the mass spectra allowing the clear determination of characteristic (usually molecular) ions. Their enrichment in the ion trap and identification by tandem MS investigations (MS/MS) enables the detection of the target substances in complex matrices at low concentrations without time-consuming sample preparation. For SPI an electron beam pumped excimer light source of own fabrication (E-Lux) is used. The SPI-ITMS system was characterized by the analytical study of different drugs like cannabis, heroin, cocaine, amphetamines, and some precursors. Additionally, it was successfully tested on-site in a closed illegal drug laboratory, where low quantities of MDMA could be directly detected in samples from floors, walls and lab equipments. The second analytical system is based on an ion mobility (IM) spectrometer with resonant multiphoton ionization (REMPI). With the frequency quadrupled Nd:YAG laser (266 nm), used for ionization, a selective and sensitive detection of aromatic compounds is possible. By application of suited aromatic dopants, in addition, also non-aromatic polar compounds are accessible by ion molecule reactions like proton transfer or complex formation. Selected drug precursors could be successfully detected with this device as well, qualifying it to a lower-priced alternative or useful supplement of the SPI-ITMS system for security analysis.

Partially reduced graphene oxide based FRET on fiber optic interferometer for biochemical detection

NASA Astrophysics Data System (ADS)

Yao, B. C.; Wu, Y.; Yu, C. B.; He, J. R.; Rao, Y. J.; Gong, Y.; Chen, Y. F.; Li, Y. R.

2017-04-01

An all-fiber graphene oxide (GO) based 'FRET on Fiber' concept is proposed and applied in biochemical detections. This method is of both good selectivity and high sensitivity, with detection limits of 1.2 nM, 1.3 μM and 1 pM, for metal ion, dopamine and single-stranded DNA (ssDNA), respectively.

Fracto-emission from the peeling of pressure sensitive adhesives

NASA Technical Reports Server (NTRS)

Dickinson, J. T.; Shen, X. A.; Jensen, L. C.

1985-01-01

The electron emission, positive ion emission, photon emission, and long wavelength electromagnetic radiation accompanying the peeling of pressure sensitive adhesives in vacuum are examined. These results are interpreted in terms of a previously presented model involving fracture-induced microdischarges which excite the fracture surfaces by particle bombardment.

Detection of Micrococcus luteus biofilm formation in microfluidic environments by pH measurement using an ion-sensitive field-effect transistor.

PubMed

Matsuura, Koji; Asano, Yuka; Yamada, Akira; Naruse, Keiji

2013-02-18

Biofilm formation in microfluidic channels is difficult to detect because sampling volumes are too small for conventional turbidity measurements. To detect biofilm formation, we used an ion-sensitive field-effect transistor (ISFET) measurement system to measure pH changes in small volumes of bacterial suspension. Cells of Micrococcus luteus (M. luteus) were cultured in polystyrene (PS) microtubes and polymethylmethacrylate (PMMA)-based microfluidic channels laminated with polyvinylidene chloride. In microtubes, concentrations of bacteria and pH in the suspension were analyzed by measuring turbidity and using an ISFET sensor, respectively. In microfluidic channels containing 20 μL of bacterial suspension, we measured pH changes using the ISFET sensor and monitored biofilm formation using a microscope. We detected acidification and alkalinization phases of M. luteus from the ISFET sensor signals in both microtubes and microfluidic channels. In the alkalinization phase, after 2 day culture, dense biofilm formation was observed at the bottom of the microfluidic channels. In this study, we used an ISFET sensor to detect biofilm formation in clinical and industrial microfluidic environments by detecting alkalinization of the culture medium. 

Position sensitive radioactivity detection for gas and liquid chromatography

DOEpatents

Cochran, Joseph L.; McCarthy, John F.; Palumbo, Anthony V.; Phelps, Tommy J.

2001-01-01

A method and apparatus are provided for the position sensitive detection of radioactivity in a fluid stream, particularly in the effluent fluid stream from a gas or liquid chromatographic instrument. The invention represents a significant advance in efficiency and cost reduction compared with current efforts.

A new fluorescent probe for distinguishing Zn2+ and Cd2+ with high sensitivity and selectivity.

PubMed

Tan, Yiqun; Gao, Junkuo; Yu, Jiancan; Wang, Ziqi; Cui, Yuanjing; Yang, Yu; Qian, Guodong

2013-08-28

A new fluorescence probe for distinguishing Zn(2+) and Cd(2+) is designed and synthesized. For the first time to our knowledge, this probe can recognize similar metal ions by coherently utilizing intramolecular charge transfer (ICT) and different electronic affinities of various metal ions, instead of by selective coordination alone, which may be interfered with and lose its selectivity easily in a complicated environment, providing a distinct recognition even by the naked eye for Zn(2+) and Cd(2+) with the sensitivity at the ppb level. This design strategy may initiate a straightforward approach for the selective detection of various metal ions with similar chemical properties in extensive applications such as environmental, industrial, and bio-science.

Positive and negative ion outflow at Rhea as observed by Cassini

NASA Astrophysics Data System (ADS)

Desai, Ravindra; Jones, Geraint; Regoli, Leonardo; Cowee, Misa; Coates, Andrew; Kataria, Dhiren

2017-04-01

Rhea is Saturn's largest icy moon and hosts an ethereal oxygen and carbon-dioxide atmosphere as was detected when Cassini observed positive and negative pickup ions outflowing from the moon and an extended neutral exosphere. These pickup ions can form current systems which, with the resulting jxB force, act to slow-down the incident magneto-plasma and cause field-line draping. As well as impacting the plasma interaction, the composition and density of picked up ions provide key diagnostics of the moon's sputter-induced atmosphere and surface. During the first Cassini-Rhea encounter (R1), the Cassini Plasma Spectrometer (CAPS) observed positively and negatively charged pickup ions before and after passing through the moon's plasma wake respectively, in agreement with their anticipated cycloidal trajectories. On the subsequent more distant wake encounter (R1.5) however, only positively charged pickup ions were observed, indicating high loss rates of the negative ions in Saturn's magnetosphere. Here, using an updated model of Cassini's Electron Spectrometer response function, we are able to estimate the outward flux of negatively charged pickup ions, the first time such a plasma population has been constrained. Using test-particle simulations we trace both the positive and negative particles back to Rhea's exobase to better understand their production and loss processes and the implications for Rhea's sputter-induced exosphere. We also look to examine whether the calculated ion densities could generate ion cyclotron wave activity.

Improving low-level plasma protein mass spectrometry-based detection for candidate biomarker discovery and validation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Page, Jason S.; Kelly, Ryan T.; Camp, David G.

2008-09-01

Methods. To improve the detection of low abundance protein candidate biomarker discovery and validation, particularly in complex biological fluids such as blood plasma, increased sensitivity is desired using mass spectrometry (MS)-based instrumentation. A key current limitation on the sensitivity of electrospray ionization (ESI) MS is due to the fact that many sample molecules in solution are never ionized, and the vast majority of the ions that are created are lost during transmission from atmospheric pressure to the low pressure region of the mass analyzer. Two key technologies, multi-nanoelectrospray emitters and the electrodynamic ion funnel have recently been developed and refinedmore » at Pacific Northwest National Laboratory (PNNL) to greatly improve the ionization and transmission efficiency of ESI MS based analyses. Multi-emitter based ESI enables the flow from a single source (typically a liquid chromatography [LC] column) to be divided among an array of emitters (Figure 1). The flow rate delivered to each emitter is thus reduced, allowing the well-documented benefits of nanoelectrospray 1 for both sensitivity and quantitation to be realized for higher flow rate separations. To complement the increased ionization efficiency afforded by multi-ESI, tandem electrodynamic ion funnels have also been developed at PNNL, and shown to greatly improve ion transmission efficiency in the ion source interface.2, 3 These technologies have been integrated into a triple quadrupole mass spectrometer for multiple reaction monitoring (MRM) of probable biomarker candidates in blood plasma and show promise for the identification of new species even at low level concentrations.« less

Determination of parts per trillion levels of organophosphorus pesticides in groundwater by automated on-line liquid-solid extraction followed by liquid chromatography/atmospheric pressure chemical ionization mass spectrometry using positive and negative ion modes of operation.

PubMed

Lacorte, S; Barceló, D

1996-08-01

Liquid chromatography/atmospheric pressure chemical ionization mass spectrometry with positive and negative ion modes of operations was used for the trace determination of several organophosphorus pesticides, (E)- and (Z)-mevinphos, dichlorvos, azinphos-methyl, azinphosethyl, parathion-methyl, parathion-ethyl, malathion, fenitrothion, fenthion, chlorfenvinphos, and diazinon, in groundwater. This method required only 100 mL of water, and it was combined with a prior automated online liquid-solid extraction step using an OSP-2 autosampler containing C18 cartridges. The limit of quantitation (LOQ) varied between 5 and 37 ng/L in positive ion (PI) mode. Under negative ion (NI) mode of operation, only the parathion group (both parathions and fenitrothion) had a better sensitivity as compared to that in PI mode, with a LOQ of 5-15 ng/L, whereas the rest of pesticides had 2-4 times higher LOQs as compared to those in PI mode. Selected ion monitoring of the group-specific fragment of the organophosphorus pesticides, e.g., [(CH3O)2PO2]- or the [M + H]+ ions, under NI or PI mode, respectively, was used. Sample cone voltage varied from 10 to 130 V. This parameter influenced the transmission and fragmentation of quasi-molecular ions, and it was optimized to achieve identification capabilities with the highest sensitivity. At 20 V, good fragmentation was obtained for most of the studied analytes. The system was used for the certification of a groundwater sample spiked at the nanograms per liter level with organophosphorus pesticides provided by Aquachek.

Heralded ions via ionization coincidence

NASA Astrophysics Data System (ADS)

McCulloch, A. J.; Speirs, R. W.; Wissenberg, S. H.; Tielen, R. P. M.; Sparkes, B. M.; Scholten, R. E.

2018-04-01

We demonstrate a method for the deterministic production of single ions by exploiting the correlation between an electron and associated ion following ionization. Coincident detection and feedback in combination with Coulomb-driven particle selection allows for high-fidelity heralding of ions at a high repetition rate. Extension of the scheme beyond time-correlated feedback to position- and momentum-correlated feedback will provide a general and powerful means to optimize the ion beam brightness for the development of next-generation focused ion beam technologies.

Argon direct analysis in real time mass spectrometry in conjunction with makeup solvents: a method for analysis of labile compounds.

PubMed

Yang, Hongmei; Wan, Debin; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

2013-02-05

Helium direct analysis in real time (He-DART) mass spectrometry (MS) analysis of labile compounds usually tends to be challenging because of the occurrence of prominent fragmentation, which obscures the assigning of an ion to an independent species or merely a fragment in a mixture. In the present work, argon DART (Ar-DART) MS in conjunction with makeup solvents has been demonstrated to analyze a variety of labile compounds including nucleosides, alkaloids, glucose, and other small molecules. The results presented here confirm that Ar-DART can generate significantly less energetic ions than conventional He-DART and is able to produce the intact molecular ions with little or no fragmentation in both positive and negative ion modes. Adding a makeup solvent (absolute ethyl alcohol, methanol, fluorobenzene, or acetone) to the argon gas stream at the exit of the DART ion source can result in 1-2 orders of magnitude increase in detection signals. The sensitivity attainable by Ar-DART was found to be comparable to that by He-DART. The investigation of influence of solvents improves our understanding of the fundamental desorption and ionization processes in DART. The practical application of this rapid and high throughput method is demonstrated by the successful analysis of a natural product (Crude Kusnezoff Monkshood) extract, demonstrating the great potential in mixture research.

Using contemporary liquid chromatography theory and technology to improve capillary gradient ion-exchange separations.

PubMed

Wouters, Bert; Broeckhoven, Ken; Wouters, Sam; Bruggink, Cees; Agroskin, Yury; Pohl, Christopher A; Eeltink, Sebastiaan

2014-11-28

The gradient-performance limits of capillary ion chromatography have been assessed at maximum system pressure (34.5 MPa) using capillary columns packed with 4.1 μm macroporous anion-exchange particles coated with 65 nm positively-charged nanobeads. In analogy to the van-Deemter curve, the gradient performance was assessed applying different flow rates, while decreasing the gradient time inversely proportional to the increase in flow rate in order to maintain the same retention properties. The gradient kinetic-performance limits were determined at maximum system pressure, applying tG/t0=5, 10, and 20. In addition, the effect of retention on peak width was assessed in gradient mode for mono-, di-, and trivalent inorganic anions. The peak width of late-eluting ions can be significantly reduced by using concave gradient, resulting in better detection sensitivity. A signal enhancement factor of 8 was measured for a late-eluting ion when applying a concave instead of a linear gradient. For the analysis of a complex anion mixture, a coupled column with a total length of 1.05 m was operated at the kinetic-performance limit applying a linear 250 min gradient (tG/t0=10). The peak capacity varied between 200 and 380 depending on analyte retention, and hence on charge and size of the ion. Copyright © 2014 Elsevier B.V. All rights reserved.

Ultra-high-mass mass spectrometry with charge discrimination using cryogenic detectors

DOEpatents

Frank, Matthias; Mears, Carl A.; Labov, Simon E.; Benner, W. Henry

1999-01-01

An ultra-high-mass time-of-flight mass spectrometer using a cryogenic particle detector as an ion detector with charge discriminating capabilities. Cryogenic detectors have the potential for significantly improving the performance and sensitivity of time-of-flight mass spectrometers, and compared to ion multipliers they exhibit superior sensitivity for high-mass, slow-moving macromolecular ions and can be used as "stop" detectors in time-of-flight applications. In addition, their energy resolving capability can be used to measure the charge state of the ions. Charge discrimination is very valuable in all time-of-flight mass spectrometers. Using a cryogenically-cooled Nb-Al.sub.2 O.sub.3 -Nb superconductor-insulator-superconductor (SIS) tunnel junction (STJ) detector operating at 1.3 K as an ion detector in a time-of-flight mass spectrometer for large biomolecules it was found that the STJ detector has charge discrimination capabilities. Since the cryogenic STJ detector responds to ion energy and does not rely on secondary electron production, as in the conventionally used microchannel plate (MCP) detectors, the cryogenic detector therefore detects large molecular ions with a velocity-independent efficiency approaching 100%.

Development of a reverse transcription-loop-mediated isothermal amplification (RT-LAMP) system for a highly sensitive detection of enterovirus in the stool samples of acute flaccid paralysis cases.

PubMed

Arita, Minetaro; Ling, Hua; Yan, Dongmei; Nishimura, Yorihiro; Yoshida, Hiromu; Wakita, Takaji; Shimizu, Hiroyuki

2009-12-16

In the global eradication program for poliomyelitis, the laboratory diagnosis plays a critical role by isolating poliovirus (PV) from the stool samples of acute flaccid paralysis (AFP) cases. In this study, we developed a reverse transcription-loop-mediated isothermal amplification (RT-LAMP) system for a rapid and highly sensitive detection of enterovirus including PV to identify stool samples positive for enterovirus including PV. A primer set was designed for RT-LAMP to detect enterovirus preferably those with PV-like 5'NTRs of the viral genome. The sensitivity of RT-LAMP system was evaluated with prototype strains of enterovirus. Detection of enterovirus from stool extracts was examined by using RT-LAMP system. We detected at least 400 copies of the viral genomes of PV(Sabin) strains within 90 min by RT-LAMP with the primer set. This RT-LAMP system showed a preference for Human enterovirus species C (HEV-C) strains including PV, but exhibited less sensitivity to the prototype strains of HEV-A and HEV-B (detection limits of 7,400 to 28,000 copies). Stool extracts, from which PV, HEV-C, or HEV-A was isolated in the cell culture system, were mostly positive by RT-LAMP method (positive rates of 15/16 (= 94%), 13/14 (= 93%), and 4/4 (= 100%), respectively). The positive rate of this RT-LAMP system for stool extracts from which HEV-B was isolated was lower than that of HEV-C (positive rate of 11/21 (= 52%)). In the stool samples, which were negative for enterovirus isolation by the cell culture system, we found that two samples were positive for RT-LAMP (positive rates of 2/38 (= 5.3%)). In these samples, enterovirus 96 was identified by sequence analysis utilizing a seminested PCR system. RT-LAMP system developed in this study showed a high sensitivity comparable to that of the cell culture system for the detection of PV, HEV-A, and HEV-C, but less sensitivity to HEV-B. This RT-LAMP system would be useful for the direct detection of enterovirus from the stool extracts.

Human salivary glucose analysis by high-performance ion-exchange chromatography and pulsed amperometric detection.

PubMed

Gough, H; Luke, G A; Beeley, J A; Geddes, D A

1996-02-01

The aim of this project was to develop an analytical procedure with the required level of sensitivity for the determination of glucose concentrations in small volumes of unstimulated fasting whole saliva. The technique involves high-performance ion-exchange chromatography at high pH and pulsed amperometric detection. It has a high level of reproducibility, a sensitivity as low as 0.1 mumol/l and requires only 50 microliters samples (sensitivity = 0.002 pmol). Inhibition of glucose metabolism, by procedures such as collection into 0.1% (w/v) sodium fluoride, was shown to be essential if accurate results are to be obtained. Collection on to ice followed by storage at -20 degrees C was shown to be unsuitable and resulted in glucose loss by degradation. There were inter- and intraindividual variations in the glucose concentration in unstimulated mixed saliva (range; 0.02-0.4 mmol/l). The procedure can be used for the analysis of other salivary carbohydrates and for monitoring the clearance of dietary carbohydrates from the mouth.

Note: Low temperature superconductor superconducting quantum interference device system with wide pickup coil for detecting small metallic particles

NASA Astrophysics Data System (ADS)

Kandori, Akihiko; Ogata, Kuniomi; Kawabata, Ryuzo; Tanimoto, Sayaka; Seki, Yusuke

2012-07-01

A one-channel low temperature superconductor superconducting quantum interference device system comprising a second-order axial gradiometer with a sensing area of 10 mm × 190 mm was developed. The gradiometer was mounted in a liquid-helium dewar (450-mm diameter; 975-mm length), with a gap of 12 mm between the pickup coil and the dewar-tail surface. The magnetic field sensitivity was measured to be 16 fT/Hz1/2 in the white noise regime above 2 Hz. The system was used to measure stainless steel particles of different sizes passing through the sensing area. A 100-μm diameter SUS304 particle was readily detected passing at different positions underneath the large pickup coil by measuring its 1.3-pT magnetic field. Thus, the system was shown to be applicable to quality control of lamination sheet products such as lithium ion batteries.

Potentiometric determination of trypsin using a polymeric membrane polycation-sensitive electrode based on current-controlled reagent delivery.

PubMed

Chen, Yan; Ding, Jiawang; Qin, Wei

2012-12-01

A potentiometric biosensor for the determination of trypsin is described based on current-controlled reagent delivery. A polymeric membrane protamine-sensitive electrode with dinonylnaphthalene sulfonate as cation exchanger is used for in situ generation of protamine. Diffusion of protamine across the polymeric membrane can be controlled precisely by applying an external current. The hydrolysis catalyzed with trypsin in sample solution decreases the concentration of free protamine released at the sample-membrane interface and facilitates the stripping of protamine out of the membrane surface via the ion-exchange process with sodium ions from the sample solution, thus decreasing the membrane potential, by which the protease can be sensed potentiometrically. The influences of anodic current amplitude, current pulse duration and protamine concentration in the inner filling solution on the membrane potential response have been studied. Under optimum conditions, the proposed protamine-sensitive electrode is useful for continuous and reversible detection of trypsin over the concentration range of 0.5-5UmL(-1) with a detection limit of 0.3UmL(-1). The proposed detection strategy provides a rapid and reagentless way for the detection of protease activities and offers great potential in the homogeneous immunoassays using proteases as labels. Copyright © 2012 Elsevier B.V. All rights reserved.

Highly selective rhodamine-based fluorescence turn-on chemosensor for Al3+ ion

NASA Astrophysics Data System (ADS)

Manjunath, Rangasamy; Kannan, Palaninathan

2018-05-01

A new rhodamine-based colorimetric and fluorescent turn-on chemosensor (L) has been designed and synthesized for selective and sensitive detection of Al3+ ion. The sensing behavior toward metal ion was investigated by UV/Vis and fluorescence spectroscopy. Upon addition of Al3+ ion to solution of L provided a visual color change as well as significantly fluorescent enhancement, while other metal ions including Na+, Mg2+, K+, Mn2+, Fe3+, Ni2+, Cu2+, Zn2+, Pb2+, Cd2+ and Hg2+ ions fails to generate a distinct color and spectral changes, the distinct color change and rapid switch-on fluorescence also provide naked eye detection for Al3+ ion. The mechanism involved equilibrium between non-fluorescent spirocyclic form and highly fluorescent ring open form process was utilized and 1:2 stoichiometry for L-Al3+ complex formed with an association constant of 1.42 × 103 M-1. Moreover, chemosensor L was applied for living cell imaging and confirmed that can be used as a fluorescent probe for monitoring Al3+ ion in living cells.

Development of analytically capable time-of-flight mass spectrometer with continuous ion introduction

NASA Astrophysics Data System (ADS)

Hárs, György; Dobos, Gábor

2010-03-01

The present article describes the results and findings explored in the course of the development of the analytically capable prototype of continuous time-of-flight (CTOF) mass spectrometer. Currently marketed pulsed TOF (PTOF) instruments use ion introduction with a 10 ns or so pulse width, followed by a waiting period roughly 100 μs. Accordingly, the sample is under excitation in 10-4 part of the total measuring time. This very low duty cycle severely limits the sensitivity of the PTOF method. A possible approach to deal with this problem is to use linear sinusoidal dual modulation technique (CTOF) as described in this article. This way the sensitivity of the method is increased, due to the 50% duty cycle of the excitation. All other types of TOF spectrometer use secondary electron multiplier (SEM) for detection, which unfortunately discriminates in amplification in favor of the lighter ions. This discrimination effect is especially undesirable in a mass spectrometric method, which targets high mass range. In CTOF method, SEM is replaced with Faraday cup detector, thus eliminating the mass discrimination effect. Omitting SEM is made possible by the high ion intensity and the very slow ion detection with some hundred hertz detection bandwidth. The electrometer electronics of the Faraday cup detector operates with amplification 1010 V/A. The primary ion beam is highly monoenergetic due to the construction of the ion gun, which made possible to omit any electrostatic mirror configuration for bunching the ions. The measurement is controlled by a personal computer and the intelligent signal generator Type Tabor WW 2571, which uses the direct digital synthesis technique for making arbitrary wave forms. The data are collected by a Labjack interface board, and the fast Fourier transformation is performed by the software. Noble gas mixture has been used to test the analytical capabilities of the prototype setup. Measurement presented proves the results of the mathematical calculations as well as the future potentiality for use in chemical analysis of gaseous mixtures.

Poly(acrylic acid)-templated silver nanoclusters as a platform for dual fluorometric turn-on and colorimetric detection of mercury (II) ions.

PubMed

Tao, Yu; Lin, Youhui; Huang, Zhenzhen; Ren, Jinsong; Qu, Xiaogang

2012-01-15

An easy prepared fluorescence turn-on and colorimetric dual channel probe was developed for rapid assay of Hg(2+) ions with high sensitivity and selectivity by using poly(acrylic acid)-templated silver nanoclusters (PAA-AgNCs). The PAA-AgNCs exhibited weak fluorescence, while upon the addition of Hg(2+) ions, AgNCs gives a dramatic increase in fluorescence as a result of the changes of the AgNCs states. The detection limit was estimated to be 2 nM, which is much lower than the Hg(2+) detection requirement for drinking water of U.S. Environmental Protection Agency, and the turn-on sensing mode offers additional advantage to efficiently reduce background noise. Also, a colorimetric assay of Hg(2+) ions can be realized due to the observed absorbance changes of the AgNCs. More importantly, the method was successfully applied to the determination of Hg(2+) ions in real water samples, which suggests our proposed method has a great potential of application in environmental monitoring. Copyright © 2011 Elsevier B.V. All rights reserved.

Making Shock Waves in Microfluidics: The Physics and Applications of Isotachophoresis

NASA Astrophysics Data System (ADS)

Santiago, Juan

2007-11-01

Microfluidics lies at the interfaces between engineering, chemistry, and biology, and aims to develop chemical laboratories on a chip. An important technique is on-chip capillary electrophoresis which has been applied to a wide range of chemical and biochemical assay applications over the last decade. Perhaps the best way of improving the sensitivity of on-chip electrophoresis is to integrate an online sample preconcentration method. At Stanford, we are developing methods to concentrate ions into small volumes using a method called isotachophoresis (ITP). In ITP, sample ions are injected between the high mobility co-ions of a leading electrolyte (LE) and the low mobility co-ions of a trailing electrolyte (TE). Upon application of an electric field, the disparate ion mobilities of the LE and TE cause sample species to segregate and focus into a series of narrow self-sharpening zones which migrate at equal velocity (hence ``isotacho''). ITP-type processes have been studied and used for more than 60 years, and yet there remain significant challenges in the robust modeling of these transport processes and the creation of widely applicable assays. We use ITP to create sample ion concentration ``shock waves'' in microchannels. These concentration waves can be integrated with on-chip electrophoresis for high sensitivity assays, and novel modes of operation. The talk will summarize the basic physics of ITP, experimental studies of ITP, models of ITP, and the development of novel ITP-assays with unprecedented sensitivity and new functionality. For example, using leading-to-sample ion concentration ratios of 10^15 and local electric fields of ˜4 kV/cm, we can achieve order one micron wide ITP zones. We can achieve million fold preconcentration in 120 s and can detect 100 attomolar sample concentrations (to our knowledge the highest demonstrated sensitivity for an electrophoresis-related assay). We have also developed a method that uses ITP to separate, indirectly detect, and identify the electrophoretic mobilities of unlabeled (non-fluorescent) analytes using surrogate fluorescent molecules. Our goal is the development of novel on-chip ITP assays which expand the design space of microfluidic devices.

Improved Spectroscopy of Molecular Ions in the Mid-Infrared with Up-Conversion Detection

NASA Astrophysics Data System (ADS)

Markus, Charles R.; Perry, Adam J.; Hodges, James N.; McCall, Benjamin J.

2016-06-01

Heterodyne detection, velocity modulation, and cavity enhancement are useful tools for observing rovibrational transitions of important molecular ions. We have utilized these methods to investigate a number of molecular ions, such as H_3^+, CH_5^+, HeH^+, and OH^+. In the past, parasitic etalons and the lack of fast and sensitive detectors in the mid-infrared have limited the number of transitions we could measure with MHz-level precision. Recently, we have significantly reduced the amplitude of unwanted interference fringes with a Brewster-plate spoiler. We have also developed a detection scheme which up-converts the mid-infrared light with difference frequency generation which allows the use of a faster and more sensitive avalanche photodetector. The higher detection bandwidth allows for optimized heterodyne detection at higher modulation frequencies. The overall gain in signal-to-noise from both improvements will enable extensive high-precision line lists of molecular ions and searches for previously unobserved transitions. K.N. Crabtree, J.N. Hodges, B.M. Siller, A.J. Perry, J.E. Kelly, P.A. Jenkins II, and B.J. McCall, Chem. Phys. Lett. 551 (2012) 1-6. A.J. Perry, J.N. Hodges, C.R. Markus, G.S. Kocheril, and B.J. McCall, J. Mol. Spec. 317 (2015) 71-73. J.N. Hodges, A.J. Perry, P.A. Jenkins II, B.M. Siller, and B.J. McCall, J. Chem. Phys. 139 (2013) 164291. A.J. Perry, J.N. Hodges, C.R. Markus, G.S. Kocheril, and B.J. McCall. 2014, J. Chem. Phys. 141, 101101 C.R. Markus, J.N. Hodges, A.J. Perry, G.S. Kocheril, H.S.P. Muller, and B.J. McCall, Astrophys. J. 817 (2016) 138.

Numerical Model of the Plasma Sheath Generated by the Plasma Source Instrument Aboard the Polar Satellite

NASA Technical Reports Server (NTRS)

Leung, Wing C.; Singh, Nagendra; Moore, Thomas E.; Craven, Paul D.

2000-01-01

The plasma sheath generated by the operation of the Plasma Source Instrument (PSI) aboard the POLAR satellite is studied by using a 3-dimensional Particle-In-Cell (PIC) code. When the satellite passes through the region of low density plasma, the satellite charges to positive potentials as high as 4050Volts due to the photoelectrons emission. In such a case, ambient core ions cannot accurately be measured or detected. The goal of the onboard PSI is to reduce the floating potential of the satellite to a sufficiently low value so that the ions in the polar wind become detectable. When the PSI is operated, an ion-rich Xenon plasma is ejected from the satellite, such that the floating potential of the satellite is reduced and is maintained at about 2Volts. Accordingly, in our 3-dimensional PIC simulation, we considered that the potential of the satellite is 2Volts as a fixed bias. Considering the relatively high density of the Xenon plasma in the sheath (approx. 10 - 10(exp 3)/cc), the ambient plasma of low density (less than 1/cc) is neglected. In the simulations, the electric fields and plasma dynamics are calculated self-consistently. We found that an "Apple" shape positive potential sheath forms surrounding the satellite. In the region near the PSI emission, a high positive potential hill develops. Near the Thermal Ion Detection Experiment (TIDE) detector away from the PSI, the potentials are sufficiently low for the ambient polar wind ions to reach it. In the simulations, it takes about a hundred electron gyroperiods for the sheath to reach a quasi-steady state. This time is approximately the time taken by the heavy Xe(+) ions to expand up to about one average Larmor radius of electrons from the satellite surface. Using the steady state sheath, we performed trajectory calculations to characterize the detector response to a highly supersonic polar wind flow. The detected ions' velocity distribution shows significant deviations from a shifted Maxwellian in the ambient polar wind population. The deviations are caused by the effects of electric fields on the ions' motion as they traverse the sheath.

Characterization of Downstream Ion Energy Distributions From a High Current Hollow Cathode in a Ring Cusp Discharge Chamber

NASA Technical Reports Server (NTRS)

Foster, John E.; Patterson, Michael J.

2003-01-01

The presence of energetic ions produced by a hollow cathodes operating at high emission currents (greater than 10 Angstroms) has been documented in the literature. As part of an ongoing effort to uncover the underlying physics of the formation of these ions, ion efflux from a high current hollow cathode operating in an ion thruster discharge chamber was investigated. Using a spherical sector electrostatic energy analyzer located downstream of the discharge cathode, the ion energy distribution over a 0 to 60 eV energy range was measured. The sensitivity of the ion energy distribution function to zenith angle was also assessed at 3 different positions: 0, 15, and 25 degrees. The measurements suggest that the majority of the ion current at the measuring point falls into the analyzer with an energy approximately equal to the discharge voltage. The ion distribution, however, was found to be quite broad. The high energy tail of the distribution function tended to grow with increasing discharge current. Sensitivity of the profiles to flow rate at fixed discharge current was also investigated. A simple model is presented that provides a potential mechanism for the production of ions with energies above the discharge voltage.

Analysis of phenolic choline esters from seeds of Arabidopsis thaliana and Brassica napus by capillary liquid chromatography/electrospray- tandem mass spectrometry.

PubMed

Böttcher, Christoph; von Roepenack-Lahaye, Edda; Schmidt, Jürgen; Clemens, Stephan; Scheel, Dierk

2009-04-01

Total phenolic choline ester fractions prepared from seeds of Arabidopsis thaliana and Brassica napus were analyzed by capillary LC/ESI-QTOF-MS and direct infusion ESI-FTICR-MS. In addition to the dominating sinapoylcholine, 30 phenolic choline esters could be identified based on accurate mass measurements, interpretation of collision-induced dissociation (CID) mass spectra, and synthesis of selected representatives. The compounds identified so far include substituted hydroxycinnamoyl- and hydroxybenzoylcholines, respective monohexosides as well as oxidative coupling products of phenolic choline esters and monolignols. Phenolic choline esters are well separable by reversed-phase liquid chromatography and sensitively detectable using electrospray ionization mass spectrometry in positive ion mode. CID mass spectra obtained from molecular ions facilitate the characterization of both the type and substitution pattern of such compounds. Therefore, LC/ESI-MS/MS represents a valuable tool for comprehensive qualitative and quantitative analysis of this compound class. Copyright (c) 2009 John Wiley & Sons, Ltd.

Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

PubMed

Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

2017-04-15

A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ultrasensitive sliver nanorods array SERS sensor for mercury ions.

PubMed

Song, Chunyuan; Yang, Boyue; Zhu, Yu; Yang, Yanjun; Wang, Lianhui

2017-01-15

With years of outrageous mercury emissions, there is an urgent need to develop convenient and sensitive methods for detecting mercury ions in response to increasingly serious mercury pollution in water. In the present work, a portable, ultrasensitive SERS sensor is proposed and utilized for detecting trace mercury ions in water. The SERS sensor is prepared on an excellent sliver nanorods array SERS substrate by immobilizing T-component oligonucleotide probes labeled with dye on the 3'-end and -SH on the 5'-end. The SERS sensor responses to the specific chemical bonding between thymine and mercury ions, which causes the previous flexible single strand of oligonucleotide probe changing into rigid and upright double chain structure. Such change in the structure drives the dyes far away from the excellent SERS substrate and results in a SERS signal attenuation of the dye. Therefore, by monitoring the decay of SERS signal of the dye, mercury ions in water can be detected qualitatively and quantitatively. The experimental results indicate that the proposed optimal SERS sensor owns a linear response with wide detecting range from 1pM to 1μM, and a detection limit of 0.16pM is obtained. In addition, the SERS sensor demonstrates good specificity for Hg 2+ , which can accurately identify trace mercury ions from a mixture of ten kinds of other ions. The SERS sensor has been further executed to analyze the trace mercury ions in tap water and lake water respectively, and good recovery rates are obtained for sensing both kinds of water. With its high selectivity and good portability, the ultrasensitive SERS sensor is expected to be a promising candidate for discriminating mercury ions in the fields of environmental monitoring and food safety. Copyright © 2016 Elsevier B.V. All rights reserved.

Assessing the sensitivity of benzene cluster cation chemical ionization mass spectrometry toward a wide array of biogenic volatile organic compounds

NASA Astrophysics Data System (ADS)

Lavi, Avi; Vermeuel, Michael; Novak, Gordon; Bertram, Timothy

2017-04-01

Chemical ionization mass spectrometry is a real-time, sensitive and selective measurement technique for the detection of volatile organic compounds (VOCs). The benefits of CIMS technology make it highly suitable for field measurements that requires fast (10Hz and higher) response rates, such as the study of surface-atmosphere exchange processes by the eddy covariance method. The use of benzene cluster cations as a regent ion was previously demonstrated as a sensitive and selective method for the detection of select biogenic VOCs (e.g. isoprene, monoterpenes and sesquiterpenes) [Kim et al., 2016; Leibrock and Huey, 2000]. Quantitative analysis of atmospheric trace gases necessitates calibration for each analyte as a function of atmospheric conditions. We describe a custom designed calibration system, based on liquid evaporation, for determination of the sensitivity of the benzene-CIMS to a wide range of organic compounds at atmospherically relevant mixing ratios (<200 ppt). We report on the effect of atmospheric water vapor and oxygen concentrations on instrument response for isoprene and a wide range of monoterpenes and sesquiterpenes. To gain mechanistic insight into the ion-molecule reactions and the role of water vapor and oxygen, we compare our measured sensitivities with a computational analysis of the charge distribution between the analyte, reagent ion and water molecules in the gas phase. These parameters provide insight on the ionization mechanism and provide parameters for quantification of organic molecules measured during field campaigns. References Kim, M. J., M. C. Zoerb, N. R. Campbell, K. J. Zimmermann, B. W. Blomquist, B. J. Huebert, and T. H. Bertram (2016), Revisiting benzene cluster cations for the chemical ionization of dimethyl sulfide and select volatile organic compounds, Atmos Meas Tech, 9(4), 1473-1484, doi:10.5194/amt-9-1473-2016. Leibrock, E., and L. G. Huey (2000), Ion chemistry for the detection of isoprene and other volatile organic compounds in ambient air, Geophys Res Lett, 27(12), 1719-1722, doi:Doi 10.1029/1999gl010804.