"Reagentless" flow injection determination of ammonia and urea using membrane separation and solid phase basification

NASA Technical Reports Server (NTRS)

Akse, J. R.; Thompson, J. O.; Sauer, R. L.; Atwater, J. E.

1998-01-01

Flow injection analysis instrumentation and methodology for the determination of ammonia and ammonium ions in an aqueous solution are described. Using in-line solid phase basification beds containing crystalline media. the speciation of ammoniacal nitrogen is shifted toward the un-ionized form. which diffuses in the gas phase across a hydrophobic microporous hollow fiber membrane into a pure-water-containing analytical stream. The two streams flow in a countercurrent configuration on opposite sides of the membrane. The neutral pH of the analytical stream promotes the formation of ammonium cations, which are detected using specific conductance. The methodology provides a lower limit of detection of 10 microgram/L and a dynamic concentration range spanning three orders of magnitude using a 315-microliters sample injection volume. Using immobilized urease to enzymatically promote the hydrolysis of urea to produce ammonia and carbon dioxide, the technique has been extended to the determination of urea.

Analytical methods for the assessment of endocrine disrupting chemical exposure during human fetal and lactation stages: a review.

PubMed

Jiménez-Díaz, I; Vela-Soria, F; Rodríguez-Gómez, R; Zafra-Gómez, A; Ballesteros, O; Navalón, A

2015-09-10

In the present work, a review of the analytical methods developed in the last 15 years for the determination of endocrine disrupting chemicals (EDCs) in human samples related with children, including placenta, cord blood, amniotic fluid, maternal blood, maternal urine and breast milk, is proposed. Children are highly vulnerable to toxic chemicals in the environment. Among these environmental contaminants to which children are at risk of exposure are EDCs -substances able to alter the normal hormone function of wildlife and humans-. The work focuses mainly on sample preparation and instrumental techniques used for the detection and quantification of the analytes. The sample preparation techniques include, not only liquid-liquid extraction (LLE) and solid-phase extraction (SPE), but also modern microextraction techniques such as extraction with molecular imprinted polymers (MIPs), stir-bar sorptive extraction (SBSE), hollow-fiber liquid-phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME), matrix solid phase dispersion (MSPD) or ultrasound-assisted extraction (UAE), which are becoming alternatives in the analysis of human samples. Most studies focus on minimizing the number of steps and using the lowest solvent amounts in the sample treatment. The usual instrumental techniques employed include liquid chromatography (LC), gas chromatography (GC) mainly coupled to tandem mass spectrometry. Multiresidue methods are being developed for the determination of several families of EDCs with one extraction step and limited sample preparation. Copyright © 2015 Elsevier B.V. All rights reserved.

SOLID3: a multiplex antibody microarray-based optical sensor instrument for in situ life detection in planetary exploration.

PubMed

Parro, Víctor; de Diego-Castilla, Graciela; Rodríguez-Manfredi, José A; Rivas, Luis A; Blanco-López, Yolanda; Sebastián, Eduardo; Romeral, Julio; Compostizo, Carlos; Herrero, Pedro L; García-Marín, Adolfo; Moreno-Paz, Mercedes; García-Villadangos, Miriam; Cruz-Gil, Patricia; Peinado, Verónica; Martín-Soler, Javier; Pérez-Mercader, Juan; Gómez-Elvira, Javier

2011-01-01

The search for unequivocal signs of life on other planetary bodies is one of the major challenges for astrobiology. The failure to detect organic molecules on the surface of Mars by measuring volatile compounds after sample heating, together with the new knowledge of martian soil chemistry, has prompted the astrobiological community to develop new methods and technologies. Based on protein microarray technology, we have designed and built a series of instruments called SOLID (for "Signs Of LIfe Detector") for automatic in situ detection and identification of substances or analytes from liquid and solid samples (soil, sediments, or powder). Here, we present the SOLID3 instrument, which is able to perform both sandwich and competitive immunoassays and consists of two separate functional units: a Sample Preparation Unit (SPU) for 10 different extractions by ultrasonication and a Sample Analysis Unit (SAU) for fluorescent immunoassays. The SAU consists of five different flow cells, with an antibody microarray in each one (2000 spots). It is also equipped with an exclusive optical package and a charge-coupled device (CCD) for fluorescent detection. We demonstrated the performance of SOLID3 in the detection of a broad range of molecular-sized compounds, which range from peptides and proteins to whole cells and spores, with sensitivities at 1-2 ppb (ng mL⁻¹) for biomolecules and 10⁴ to 10³ spores per milliliter. We report its application in the detection of acidophilic microorganisms in the Río Tinto Mars analogue and report the absence of substantial negative effects on the immunoassay in the presence of 50 mM perchlorate (20 times higher than that found at the Phoenix landing site). Our SOLID instrument concept is an excellent option with which to detect biomolecules because it avoids the high-temperature treatments that may destroy organic matter in the presence of martian oxidants.

Performance of the MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission

NASA Astrophysics Data System (ADS)

Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Grand, Noël; Freissinet, Caroline; Danell, Ryan; van Ameron, Friso; Arevalo, Ricardo; Brinckerhoff, William; Raulin, François; Mahaffy, Paul; Goesmann, Fred

2015-04-01

The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquir-ing samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis gas chromatograph (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide in-formation on elemental and molecular makeup, po-larity, chirality and isotopic patterns of analyte spe-cies. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatography-mass spec-trometry (GC-MS) mode of operation. Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

Chemical imaging of drug delivery systems with structured surfaces-a combined analytical approach of confocal raman microscopy and optical profilometry.

PubMed

Kann, Birthe; Windbergs, Maike

2013-04-01

Confocal Raman microscopy is an analytical technique with a steadily increasing impact in the field of pharmaceutics as the instrumental setup allows for nondestructive visualization of component distribution within drug delivery systems. Here, the attention is mainly focused on classic solid carrier systems like tablets, pellets, or extrudates. Due to the opacity of these systems, Raman analysis is restricted either to exterior surfaces or cross sections. As Raman spectra are only recorded from one focal plane at a time, the sample is usually altered to create a smooth and even surface. However, this manipulation can lead to misinterpretation of the analytical results. Here, we present a trendsetting approach to overcome these analytical pitfalls with a combination of confocal Raman microscopy and optical profilometry. By acquiring a topography profile of the sample area of interest prior to Raman spectroscopy, the profile height information allowed to level the focal plane to the sample surface for each spectrum acquisition. We first demonstrated the basic principle of this complementary approach in a case study using a tilted silica wafer. In a second step, we successfully adapted the two techniques to investigate an extrudate and a lyophilisate as two exemplary solid drug carrier systems. Component distribution analysis with the novel analytical approach was neither hampered by the curvature of the cylindrical extrudate nor the highly structured surface of the lyophilisate. Therefore, the combined analytical approach bears a great potential to be implemented in diversified fields of pharmaceutical sciences.

Comparison of laser ablation and dried solution aerosol as sampling systems in inductively coupled plasma mass spectrometry.

PubMed

Coedo, A G; Padilla, I; Dorado, M T

2004-12-01

This paper describes a study designed to determine the possibility of using a dried aerosol solution for calibration in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The relative sensitivities of tested materials mobilized by laser ablation and by aqueous nebulization were established, and the experimentally determined relative sensitivity factors (RSFs) were used in conjunction with aqueous calibration for the analysis of solid steel samples. To such a purpose a set of CRM carbon steel samples (SS-451/1 to SS-460/1) were sampled into an ICP-MS instrument by solution nebulization using a microconcentric nebulizer with membrane desolvating (D-MCN) and by laser ablation (LA). Both systems were applied with the same ICP-MS operating parameters and the analyte signals were compared. The RSF (desolvated aerosol response/ablated solid response) values were close to 1 for the analytes Cr, Ni, Co, V, and W, about 1.3 for Mo, and 1.7 for As, P, and Mn. Complementary tests were carried out using CRM SS-455/1 as a solid standard for one-point calibration, applying LAMTRACE software for data reduction and quantification. The analytical results are in good agreement with the certified values in all cases, showing that the applicability of dried aerosol solutions is a good alternative calibration system for laser ablation sampling.

State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

PubMed

Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

2016-01-28

Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

High-sensitivity ESCA instrument

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

Davies, R.D.; Herglotz, H.K.; Lee, J.D.

1973-01-01

A new electron spectroscopy for chemical analysis (ESCA) instrument has been developed to provide high sensitivity and efficient operation for laboratory analysis of composition and chemical bonding in very thin surface layers of solid samples. High sensitivity is achieved by means of the high-intensity, efficient x-ray source described by Davies and Herglotz at the 1968 Denver X-Ray Conference, in combination with the new electron energy analyzer described by Lee at the 1972 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. A sample chamber designed to provide for rapid introduction and replacement of samples has adequate facilities for various sample treatmentsmore » and conditiouing followed immediately by ESCA analysis of the sample. Examples of application are presented, demonstrating the sensitivity and resolution achievable with this instrument. Its usefulness in trace surface analysis is shown and some chemical shifts'' measured by the instrument are compared with those obtained by x-ray spectroscopy. (auth)« less

A comprehensive program to develop correlations for physical properties of kraft black liquor. Final report

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

Fricke, A.L.; Zaman, A.A.; Stoy, M.O.

A wide variety of experimental techniques have been used in this work, and many of these have been developed completely or improved significantly in the course of the research done during this program. Therefore, it is appropriate to describe these techniques in detail as a reference for future workers so that the techniques can be used in future work with little additional effort or so that the results reported from this program can be compared better with future results from other work. In many cases, the techniques described are for specific analytical instruments. It is recognized that these may bemore » superseded by future developments and improvements in instrumentation if a complete description of techniques used successfully in the past on other instrumentation is available. The total pulping and liquor preparation research work performed included chip and white liquor preparation, digestion, pulp washing, liquor and wash recovery, liquor sampling, weak liquor concentration in two steps to about 45--50% solids with an intermediate soap skimming at about 140F and 27--30% solids, determination of pulp yield and Kappa number, determination of total liquor solids, and a check on the total material balance for pulping. All other research was performed either on a sample of the weak black liquor (the combined black liquor and washes from the digester) or on the skimmed liquor that had been concentrated.« less

Quantitative analysis of flavanones from citrus fruits by using mesoporous molecular sieve-based miniaturized solid phase extraction coupled to ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

PubMed

Cao, Wan; Ye, Li-Hong; Cao, Jun; Xu, Jing-Jing; Peng, Li-Qing; Zhu, Qiong-Yao; Zhang, Qian-Yun; Hu, Shuai-Shuai

2015-08-07

An analytical procedure based on miniaturized solid phase extraction (SPE) and ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was developed and validated for determination of six flavanones in Citrus fruits. The mesoporous molecular sieve SBA-15 as a solid sorbent was characterised by Fourier transform-infrared spectroscopy and scanning electron microscopy. Additionally, compared with reported extraction techniques, the mesoporous SBA-15 based SPE method possessed the advantages of shorter analysis time and higher sensitivity. Furthermore, considering the different nature of the tested compounds, all of the parameters, including the SBA-15 amount, solution pH, elution solvent, and the sorbent type, were investigated in detail. Under the optimum condition, the instrumental detection and quantitation limits calculated were less than 4.26 and 14.29ngmL(-1), respectively. The recoveries obtained for all the analytes were ranging from 89.22% to 103.46%. The experimental results suggested that SBA-15 was a promising material for the purification and enrichment of target flavanones from complex citrus fruit samples. Copyright © 2015 Elsevier B.V. All rights reserved.

The space shuttle payload planning working groups. Volume 8: Earth and ocean physics

NASA Technical Reports Server (NTRS)

1973-01-01

The findings and recommendations of the Earth and Ocean Physics working group of the space shuttle payload planning activity are presented. The requirements for the space shuttle mission are defined as: (1) precision measurement for earth and ocean physics experiments, (2) development and demonstration of new and improved sensors and analytical techniques, (3) acquisition of surface truth data for evaluation of new measurement techniques, (4) conduct of critical experiments to validate geophysical phenomena and instrumental results, and (5) development and validation of analytical/experimental models for global ocean dynamics and solid earth dynamics/earthquake prediction. Tables of data are presented to show the flight schedule estimated costs, and the mission model.

MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

NASA Astrophysics Data System (ADS)

Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

2015-10-01

The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

NASA Technical Reports Server (NTRS)

Panda, Binayak

2009-01-01

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Study on bending behaviour of nickel–titanium rotary endodontic instruments by analytical and numerical analyses

PubMed Central

Tsao, C C; Liou, J U; Wen, P H; Peng, C C; Liu, T S

2013-01-01

Aim To develop analytical models and analyse the stress distribution and flexibility of nickel–titanium (NiTi) instruments subject to bending forces. Methodology The analytical method was used to analyse the behaviours of NiTi instruments under bending forces. Two NiTi instruments (RaCe and Mani NRT) with different cross-sections and geometries were considered. Analytical results were derived using Euler–Bernoulli nonlinear differential equations that took into account the screw pitch variation of these NiTi instruments. In addition, the nonlinear deformation analysis based on the analytical model and the finite element nonlinear analysis was carried out. Numerical results are obtained by carrying out a finite element method. Results According to analytical results, the maximum curvature of the instrument occurs near the instrument tip. Results of the finite element analysis revealed that the position of maximum von Mises stress was near the instrument tip. Therefore, the proposed analytical model can be used to predict the position of maximum curvature in the instrument where fracture may occur. Finally, results of analytical and numerical models were compatible. Conclusion The proposed analytical model was validated by numerical results in analysing bending deformation of NiTi instruments. The analytical model is useful in the design and analysis of instruments. The proposed theoretical model is effective in studying the flexibility of NiTi instruments. Compared with the finite element method, the analytical model can deal conveniently and effectively with the subject of bending behaviour of rotary NiTi endodontic instruments. PMID:23173762

Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

PubMed

da Silva, Alessandra Furtado; Borges, Daniel L G; Lepri, Fábio Grandis; Welz, Bernhard; Curtius, Adilson J; Heitmann, Uwe

2005-08-01

This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 degrees C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 degrees C and atomization at 1500 degrees C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g(-1), calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6-1.2 mg were analyzed.

A microfabricated, low dark current a-Se detector for measurement of microplasma optical emission in the UV for possible use on-site

NASA Astrophysics Data System (ADS)

Abbaszadeh, Shiva; Karim, Karim S.; Karanassios, Vassili

2013-05-01

Traditionally, samples are collected on-site (i.e., in the field) and are shipped to a lab for chemical analysis. An alternative is offered by using portable chemical analysis instruments that can be used on-site (i.e., in the field). Many analytical measurements by optical emission spectrometry require use of light-sources and of spectral lines that are in the Ultra-Violet (UV, ~200 nm - 400 nm wavelength) region of the spectrum. For such measurements, a portable, battery-operated, fiber-optic spectrometer equipped with an un-cooled, linear, solid-state detector may be used. To take full advantage of the advanced measurement capabilities offered by state-of-the-art solid-state detectors, cooling of the detector is required. But cooling and other thermal management hamper portability and use on-site because they add size and weight and they increase electrical power requirements. To address these considerations, an alternative was implemented, as described here. Specifically, a microfabricated solid-state detector for measurement of UV photons will be described. Unlike solid-state detectors developed on crystalline Silicon, this miniaturized and low-cost detector utilizes amorphous Selenium (a-Se) as its photosensitive material. Due to its low dark current, this detector does not require cooling, thus it is better suited for portable use and for chemical measurements on-site. In this paper, a microplasma will be used as a light-source of UV photons for the a-Se detector. For example, spectra acquired using a microplasma as a light-source will be compared with those obtained with a portable, fiber-optic spectrometer equipped with a Si-based 2080-element detector. And, analytical performance obtained by introducing ng-amounts of analytes into the microplasma will be described.

Analysis of Volatile Fragrance and Flavor Compounds by Headspace Solid Phase Microextraction and GC-MS: An Undergraduate Instrumental Analysis Experiment

NASA Astrophysics Data System (ADS)

Galipo, Randolph C.; Canhoto, Alfredo J.; Walla, Michael D.; Morgan, Stephen L.

1999-02-01

A senior-level undergraduate laboratory experiment that demonstrates the use of solid-phase microextraction (SPME) and capillary gas chromatography-mass spectrometry (GC-MS) was developed for the identification of volatile compounds in consumer products. SPME minimizes sample preparation and concentrates volatile analytes in a solvent-free manner. Volatile flavor and fragrance compounds were extracted by SPME from the headspace of vials containing shampoos, chewing gums, and perfumes and analyzed by GC-MS. Headspace SPME was shown to be more sensitive than conventional headspace analysis of similar samples performed with an airtight syringe. Analysis times were less than 30 min, allowing multiple analyses to be performed in a typical laboratory class period.

Analytical techniques and instrumentation: A compilation. [analytical instrumentation, materials performance, and systems analysis

NASA Technical Reports Server (NTRS)

1974-01-01

Technical information is presented covering the areas of: (1) analytical instrumentation useful in the analysis of physical phenomena; (2) analytical techniques used to determine the performance of materials; and (3) systems and component analyses for design and quality control.

Analytical techniques for steroid estrogens in water samples - A review.

PubMed

Fang, Ting Yien; Praveena, Sarva Mangala; deBurbure, Claire; Aris, Ahmad Zaharin; Ismail, Sharifah Norkhadijah Syed; Rasdi, Irniza

2016-12-01

In recent years, environmental concerns over ultra-trace levels of steroid estrogens concentrations in water samples have increased because of their adverse effects on human and animal life. Special attention to the analytical techniques used to quantify steroid estrogens in water samples is therefore increasingly important. The objective of this review was to present an overview of both instrumental and non-instrumental analytical techniques available for the determination of steroid estrogens in water samples, evidencing their respective potential advantages and limitations using the Need, Approach, Benefit, and Competition (NABC) approach. The analytical techniques highlighted in this review were instrumental and non-instrumental analytical techniques namely gas chromatography mass spectrometry (GC-MS), liquid chromatography mass spectrometry (LC-MS), enzyme-linked immuno sorbent assay (ELISA), radio immuno assay (RIA), yeast estrogen screen (YES) assay, and human breast cancer cell line proliferation (E-screen) assay. The complexity of water samples and their low estrogenic concentrations necessitates the use of highly sensitive instrumental analytical techniques (GC-MS and LC-MS) and non-instrumental analytical techniques (ELISA, RIA, YES assay and E-screen assay) to quantify steroid estrogens. Both instrumental and non-instrumental analytical techniques have their own advantages and limitations. However, the non-instrumental ELISA analytical techniques, thanks to its lower detection limit and simplicity, its rapidity and cost-effectiveness, currently appears to be the most reliable for determining steroid estrogens in water samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Integrated Results from Analysis of the Rocknest Aeolian Deposit by the Curiosity Rover

NASA Technical Reports Server (NTRS)

Leshin, L. A.; Grotzinger, J. P.; Blake, D. F.; Edgett, K. S.; Gellert, R.; Mahaffy, P. R.; Malin, M. C.; Wiens, R. C.; Treiman, A. H.; Ming, D. W.;

Two-step Laser Time-of-Flight Mass Spectrometry to Elucidate Organic Diversity in Planetary Surface Materials.

NASA Technical Reports Server (NTRS)

Getty, Stephanie A.; Brinckerhoff, William B.; Cornish, Timothy; Li, Xiang; Floyd, Melissa; Arevalo, Ricardo Jr.; Cook, Jamie Elsila; Callahan, Michael P.

2013-01-01

Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) holds promise to be a low-mass, compact in situ analytical capability for future landed missions to planetary surfaces. The ability to analyze a solid sample for both mineralogical and preserved organic content with laser ionization could be compelling as part of a scientific mission pay-load that must be prepared for unanticipated discoveries. Targeted missions for this instrument capability include Mars, Europa, Enceladus, and small icy bodies, such as asteroids and comets.

Scoping study to expedite development of a field deployable and portable instrument for UF6 enrichment assay

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

Chan, George; Valentine, John D.; Russo, Richard E.

The primary objective of the present study is to identity the most promising, viable technologies that are likely to culminate in an expedited development of the next-generation, field-deployable instrument for providing rapid, accurate, and precise enrichment assay of uranium hexafluoride (UF6). UF6 is typically involved, and is arguably the most important uranium compound, in uranium enrichment processes. As the first line of defense against proliferation, accurate analytical techniques to determine the uranium isotopic distribution in UF6 are critical for materials verification, accounting, and safeguards at enrichment plants. As nuclear fuel cycle technology becomes more prevalent around the world, international nuclearmore » safeguards and interest in UF6 enrichment assay has been growing. At present, laboratory-based mass spectrometry (MS), which offers the highest attainable analytical accuracy and precision, is the technique of choice for the analysis of stable and long-lived isotopes. Currently, the International Atomic Energy Agency (IAEA) monitors the production of enriched UF6 at declared facilities by collecting a small amount (between 1 to 10 g) of gaseous UF6 into a sample bottle, which is then shipped under chain of custody to a central laboratory (IAEA’s Nuclear Materials Analysis Laboratory) for high-precision isotopic assay by MS. The logistics are cumbersome and new shipping regulations are making it more difficult to transport UF6. Furthermore, the analysis is costly, and results are not available for some time after sample collection. Hence, the IAEA is challenged to develop effective safeguards approaches at enrichment plants. In-field isotopic analysis of UF6 has the potential to substantially reduce the time, logistics and expense of sample handling. However, current laboratory-based MS techniques require too much infrastructure and operator expertise for field deployment and operation. As outlined in the IAEA Department of Safeguards Long-Term R&D Plan, 2012–2023, one of the IAEA long-term R&D needs is to “develop tools and techniques to enable timely, potentially real-time, detection of HEU (Highly Enriched Uranium) production in LEU (Lowly Enriched Uranium) enrichment facilities” (Milestone 5.2). Because it is common that the next generation of analytical instruments is driven by technologies that are either currently available or just now emerging, one reasonable and practical approach to project the next generation of chemical instrumentation is to track the recent trends and to extrapolate them. This study adopted a similar approach, and an extensive literature review on existing and emerging technologies for UF6 enrichment assay was performed. The competitive advantages and current limitations of different analytical techniques for in-field UF6 enrichment assay were then compared, and the main gaps between needs and capabilities for their field use were examined. Subsequently, based on these results, technologies for the next-generation field-deployable instrument for UF6 enrichment assay were recommended. The study was organized in a way that a suite of assessment metric was first identified. Criteria used in this evaluation are presented in Section 1 of this report, and the most important ones are described briefly in the next few paragraphs. Because one driving force for in-field UF6 enrichment assay is related to the demanding transportation regulation for gaseous UF6, Section 2 contains a review of solid sorbents that convert and immobilized gaseous UF6 to a solid state, which is regarded as more transportation friendly and is less regulated. Furthermore, candidate solid sorbents, which show promise in mating with existing and emerging assay technologies, also factor into technology recommendations. Extensive literature reviews on existing and emerging technologies for UF6 enrichment assay, covering their scientific principles, instrument options, and current limitations are detailed in Sections 3 and 4, respectively. In Section 5, the technological gaps as well as start-of-the-art and commercial off-the-shelf components that can be adopted to expedite the development of a fieldable or portable UF6 enrichment-assay instrument are identified and discussed. Finally, based on the results of the review, requirements and recommendations for developing the next-generation field-deployable instrument for UF6 enrichment assay are presented in Section 6.« less

A review on development of solid phase microextraction fibers by sol-gel methods and their applications.

PubMed

Kumar, Ashwini; Gaurav; Malik, Ashok Kumar; Tewary, Dhananjay Kumar; Singh, Baldev

2008-03-03

Solid phase microextraction (SPME) is an innovative, solvent free technology that is fast, economical and versatile. SPME is a fiber coated with a liquid (polymer), a solid (sorbent) or a combination of both. The fiber coating takes up the compounds from the sample by absorption in the case of liquid coatings or adsorption in the case of solid coatings. The SPME fiber is then transferred with the help of a syringe like device into the analytical instrument for desorption and analysis of the target analytes. The sol-gel process provides a versatile method to prepare size, shape and charge selective materials of high purity and homogeneity by means of preparation techniques different from the traditional ones, for the chemical analysis. This review is on the current state of the art and future trends in the developments of solid phase microextraction (SPME) fibers using sol-gel method. To achieve more selective determination of different compound classes, the variety of different coating material for SPME fibers has increased. Further developments in SPME as a highly efficient extraction technique, will greatly depend on new breakthroughs in the area of new coating material developments for the SPME fibers. In sol-gel approach, appropriate sol-gel precursors and other building blocks can be selected to create a stationary phase with desired structural and surface properties. This approach is efficient in integrating the advantageous properties of organic and inorganic material systems and thereby increasing and improving the extraction selectivity of the produced amalgam organic-inorganic stationary phases. This review is mainly focused on recent advanced developments in the design, synthesis, characterisation, properties and application of sol-gel in preparation of coatings for the SPME fibers.

Development of multiclass methods for drug residues in eggs: hydrophilic solid-phase extraction cleanup and liquid chromatography/tandem mass spectrometry analysis of tetracycline, fluoroquinolone, sulfonamide, and beta-lactam residues.

PubMed

Heller, David N; Nochetto, Cristina B; Rummel, Nathan G; Thomas, Michael H

2006-07-26

A method was developed for detection of a variety of polar drug residues in eggs via liquid chromatography/tandem mass spectrometry (LC/MS/MS) with electrospray ionization (ESI). A total of twenty-nine target analytes from four drug classes-sulfonamides, tetracyclines, fluoroquinolones, and beta-lactams-were extracted from eggs using a hydrophilic-lipophilic balance polymer solid-phase extraction (SPE) cartridge. The extraction technique was developed for use at a target concentration of 100 ng/mL (ppb), and it was applied to eggs containing incurred residues from dosed laying hens. The ESI source was tuned using a single, generic set of tuning parameters, and analytes were separated with a phenyl-bonded silica cartridge column using an LC gradient. In a related study, residues of beta-lactam drugs were not found by LC/MS/MS in eggs from hens dosed orally with beta-lactam drugs. LC/MS/MS performance was evaluated on two generations of ion trap mass spectrometers, and key operational parameters were identified for each instrument. The ion trap acquisition methods could be set up for screening (a single product ion) or confirmation (multiple product ions). The lower limit of detection for screening purposes was 10-50 ppb (sulfonamides), 10-20 ppb (fluoroquinolones), and 10-50 ppb (tetracyclines), depending on the drug, instrument, and acquisition method. Development of this method demonstrates the feasibility of generic SPE, LC, and MS conditions for multiclass LC/MS residue screening.

Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

PubMed

Hertzog, Gabriel I; Soares, Karina L; Caldas, Sergiane S; Primel, Ednei G

2015-06-01

A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g(-1). The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.

Towards a green analytical laboratory: microextraction techniques as a useful tool for the monitoring of polluted soils

NASA Astrophysics Data System (ADS)

Lopez-Garcia, Ignacio; Viñas, Pilar; Campillo, Natalia; Hernandez Cordoba, Manuel; Perez Sirvent, Carmen

2016-04-01

Microextraction techniques are a valuable tool at the analytical laboratory since they allow sensitive measurements of pollutants to be carried out by means of easily available instrumentation. There is a large number of such procedures involving miniaturized liquid-liquid or liquid-solid extractions with the common denominator of using very low amounts (only a few microliters) or even none of organic solvents. Since minimal amounts of reagents are involved, and the generation of residues is consequently minimized, the approach falls within the concept of Green Analytical Chemistry. This general methodology is useful both for inorganic and organic pollutants. Thus, low amounts of metallic ions can be measured without the need of using ICP-MS since this instrument can be replaced by a simple AAS spectrometer which is commonly present in any laboratory and involves low acquisition and maintenance costs. When dealing with organic pollutants, the microextracts obtained can be introduced into liquid or gas chromatographs equipped with common detectors and there is no need for the most sophisticated and expensive mass spectrometers. This communication reports an overview of the advantages of such a methodology, and gives examples for the determination of some particular contaminants in soil and water samples The authors are grateful to the Comunidad Autonóma de la Región de Murcia , Spain (Fundación Séneca, 19888/GERM/15) for financial support

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Panda, Binayak; Gorti, Sridhar

2013-01-01

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

ExoMars Raman laser spectrometer for Exomars

NASA Astrophysics Data System (ADS)

Rull, F.; Sansano, A.; Díaz, E.; Canora, C. P.; Moral, A. G.; Tato, C.; Colombo, M.; Belenguer, T.; Fernández, M.; Manfredi, J. A. R.; Canchal, R.; Dávila, B.; Jiménez, A.; Gallego, P.; Ibarmia, S.; Prieto, J. A. R.; Santiago, A.; Pla, J.; Ramos, G.; Díaz, C.; González, C.

2011-10-01

The Raman Laser Spectrometer (RLS) is one of the Pasteur Payload instruments, within the ESA's Aurora Exploration Programme, ExoMars mission. ExoMars 2018 main Scientific objective is "Searching for evidence of past and present life on Mars". Raman Spectroscopy is used to analyze the vibrational modes of a substance either in the solid, liquid or gas state. It relies on the inelastic scattering (Raman Scattering) of monochromatic light produced by atoms and molecules. The radiation-matter interaction results in the energy of the exciting photons to be shifted up or down. The shift in energy appears as a spectral distribution and therefore provides an unique fingerprint by which the substances can be identified and structurally analyzed. The RLS is being developed by an European Consortium composed by Spanish, French, German and UK partners. It will perform Raman spectroscopy on crushed powdered samples inside the Rover's Analytical Laboratory Drawer. Instrument performances are being evaluated by means of simulation tools and development of an instrument prototype.

Parallel, confocal, and complete spectrum imager for fluorescent detection of high-density microarray

NASA Astrophysics Data System (ADS)

Bogdanov, Valery L.; Boyce-Jacino, Michael

1999-05-01

Confined arrays of biochemical probes deposited on a solid support surface (analytical microarray or 'chip') provide an opportunity to analysis multiple reactions simultaneously. Microarrays are increasingly used in genetics, medicine and environment scanning as research and analytical instruments. A power of microarray technology comes from its parallelism which grows with array miniaturization, minimization of reagent volume per reaction site and reaction multiplexing. An optical detector of microarray signals should combine high sensitivity, spatial and spectral resolution. Additionally, low-cost and a high processing rate are needed to transfer microarray technology into biomedical practice. We designed an imager that provides confocal and complete spectrum detection of entire fluorescently-labeled microarray in parallel. Imager uses microlens array, non-slit spectral decomposer, and high- sensitive detector (cooled CCD). Two imaging channels provide a simultaneous detection of localization, integrated and spectral intensities for each reaction site in microarray. A dimensional matching between microarray and imager's optics eliminates all in moving parts in instrumentation, enabling highly informative, fast and low-cost microarray detection. We report theory of confocal hyperspectral imaging with microlenses array and experimental data for implementation of developed imager to detect fluorescently labeled microarray with a density approximately 103 sites per cm2.

Quantitation of fumonisin B1 and B2 in feed using FMOC pre-column derivatization with HPLC and fluorescence detection.

PubMed

Smith, Lori L; Francis, Kyle A; Johnson, Joseph T; Gaskill, Cynthia L

2017-11-01

Pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) was determined to be effective for quantitation of fumonisins B 1 and B 2 in feed. Liquid-solid extraction, clean-up using immunoaffinity solid phase extraction chromatography, and FMOC-derivatization preceded analysis by reverse phase HPLC with fluorescence. Instrument response was unchanged in the presence of matrix, indicating no need to use matrix-matched calibrants. Furthermore, high method recoveries indicated calibrants do not need to undergo clean-up to account for analyte loss. Established method features include linear instrument response from 0.04-2.5µg/mL and stable derivatized calibrants over 7days. Fortified cornmeal method recoveries from 0.1-30.0μg/g were determined for FB 1 (75.1%-109%) and FB 2 (96.0%-115.2%). Inter-assay precision ranged from 1.0%-16.7%. Method accuracy was further confirmed using certified reference material. Inter-laboratory comparison with naturally-contaminated field corn demonstrated equivalent results with conventional derivatization. These results indicate FMOC derivatization is a suitable alternative for fumonisins B 1 and B 2 quantitation in corn-based feeds. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evaluation of the Effect of Exhausts from Liquid and Solid Rockets on Ozone Layer

NASA Astrophysics Data System (ADS)

Yamagiwa, Yoshiki; Ishimaki, Tetsuya

This paper reports the analytical results of the influences of solid rocket and liquid rocket exhausts on ozone layer. It is worried about that the exhausts from solid propellant rockets cause the ozone depletion in the ozone layer. Some researchers try to develop the analytical model of ozone depletion by rocket exhausts to understand its physical phenomena and to find the effective design of rocket to minimize its effect. However, these models do not include the exhausts from liquid rocket although there are many cases to use solid rocket boosters with a liquid rocket at the same time in practical situations. We constructed combined analytical model include the solid rocket exhausts and liquid rocket exhausts to analyze their effects. From the analytical results, we find that the exhausts from liquid rocket suppress the ozone depletion by solid rocket exhausts.

Multiplexed Colorimetric Solid-Phase Extraction

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Fritz, James S.; Porter, Marc D.

2009-01-01

Multiplexed colorimetric solid-phase extraction (MC-SPE) is an extension of colorimetric solid-phase extraction (C-SPE) an analytical platform that combines colorimetric reagents, solid phase extraction, and diffuse reflectance spectroscopy to quantify trace analytes in water. In CSPE, analytes are extracted and complexed on the surface of an extraction membrane impregnated with a colorimetric reagent. The analytes are then quantified directly on the membrane surface using a handheld diffuse reflectance spectrophotometer. Importantly, the use of solid-phase extraction membranes as the matrix for impregnation of the colorimetric reagents creates a concentration factor that enables the detection of low concentrations of analytes in small sample volumes. In extending C-SPE to a multiplexed format, a filter holder that incorporates discrete analysis channels and a jig that facilitates the concurrent operation of multiple sample syringes have been designed, enabling the simultaneous determination of multiple analytes. Separate, single analyte membranes, placed in a readout cartridge create unique, analyte-specific addresses at the exit of each channel. Following sample exposure, the diffuse reflectance spectrum of each address is collected serially and the Kubelka-Munk function is used to quantify each water quality parameter via calibration curves. In a demonstration, MC-SPE was used to measure the pH of a sample and quantitate Ag(I) and Ni(II).

Promoting Active Learning by Practicing the "Self-Assembly" of Model Analytical Instruments

ERIC Educational Resources Information Center

Algar, W. Russ; Krull, Ulrich J.

2010-01-01

In our upper-year instrumental analytical chemistry course, we have developed "cut-and-paste" exercises where students "build" models of analytical instruments from individual schematic images of components. These exercises encourage active learning by students. Instead of trying to memorize diagrams, students are required to think deeply about…

Determination of hydrazine in drinking water: Development and multivariate optimization of a rapid and simple solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry protocol.

PubMed

Gionfriddo, Emanuela; Naccarato, Attilio; Sindona, Giovanni; Tagarelli, Antonio

2014-07-04

In this work, the capabilities of solid phase microextraction were exploited in a fully optimized SPME-GC-QqQ-MS analytical approach for hydrazine assay. A rapid and easy method was obtained by a simple derivatization reaction with propyl chloroformate and pyridine carried out directly in water samples, followed by automated SPME analysis in the same vial without further sample handling. The affinity of the different derivatized compounds obtained towards five commercially available SPME coatings was evaluated, in order to achieve the best extraction efficiency. GC analyses were carried out using a GC-QqQ-MS instrument in selected reaction monitoring (SRM) acquisition mode which has allowed the achievement of high specificity by selecting appropriate precursor-product ion couples improving the capability in analyte identification. The multivariate approach of experimental design was crucial in order to optimize derivatization reaction, SPME process and tandem mass spectrometry parameters. Accuracy of the proposed protocol, tested at 60, 200 and 800 ng L(-1), provided satisfactory values (114.2%, 83.6% and 98.6%, respectively), whereas precision (RSD%) at the same concentration levels were of 10.9%, 7.9% and 7.7% respectively. Limit of detection and quantification of 4.4 and 8.3 ng L(-1) were obtained. The reliable application of the proposed protocol to real drinking water samples confirmed its capability to be used as analytical tool for routine analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

A Comparison of Analytical and Data Preprocessing Methods for Spectral Fingerprinting

PubMed Central

LUTHRIA, DEVANAND L.; MUKHOPADHYAY, SUDARSAN; LIN, LONG-ZE; HARNLY, JAMES M.

2013-01-01

Spectral fingerprinting, as a method of discriminating between plant cultivars and growing treatments for a common set of broccoli samples, was compared for six analytical instruments. Spectra were acquired for finely powdered solid samples using Fourier transform infrared (FT-IR) and Fourier transform near-infrared (NIR) spectrometry. Spectra were also acquired for unfractionated aqueous methanol extracts of the powders using molecular absorption in the ultraviolet (UV) and visible (VIS) regions and mass spectrometry with negative (MS−) and positive (MS+) ionization. The spectra were analyzed using nested one-way analysis of variance (ANOVA) and principal component analysis (PCA) to statistically evaluate the quality of discrimination. All six methods showed statistically significant differences between the cultivars and treatments. The significance of the statistical tests was improved by the judicious selection of spectral regions (IR and NIR), masses (MS+ and MS−), and derivatives (IR, NIR, UV, and VIS). PMID:21352644

Merging Old and New: An Instrumentation-Based Introductory Analytical Laboratory

ERIC Educational Resources Information Center

Jensen, Mark B.

2015-01-01

An instrumentation-based laboratory curriculum combining traditional unknown analyses with student-designed projects has been developed for an introductory analytical chemistry course. In the first half of the course, students develop laboratory skills and instrumental proficiency by rotating through six different instruments performing…

Detecting a wide range of environmental contaminants in human blood samples--combining QuEChERS with LC-MS and GC-MS methods.

PubMed

Plassmann, Merle M; Schmidt, Magdalena; Brack, Werner; Krauss, Martin

2015-09-01

Exposure to environmental pollution and consumer products may result in an uptake of chemicals into human tissues. Several studies have reported the presence of diverse environmental contaminants in human blood samples. However, previously developed multi-target methods for the analysis of human blood include a fairly limited amount of compounds stemming from one or two related compound groups. Thus, the sample preparation method QuEChERS (quick easy cheap effective rugged and safe) was tested for the extraction of 64 analytes covering a broad compound domain followed by detection using liquid and gas chromatography coupled to mass spectrometry (LC- and GC-MS). Forty-seven analytes showed absolute recoveries above 70% in the first QuEChERS step, being a simple liquid-liquid extraction (LLE) using acetonitrile and salt. The second QuEChERS step, being a dispersive solid phase extraction, did not result in an overall improvement of recoveries or removal of background signals. Using solely the LLE step, eight analytes could subsequently be detected in human blood samples from the German Environmental Specimen Bank. Using a LC-multiple reaction monitoring (MRM) method with a triple quadrupole instrument, better recoveries were achieved than with an older LC-high-resolution (HR) MS full scan orbitrap instrument, which required a higher concentration factor of the extracts. However, the application of HRMS full scan methods could be used for the detection of additional compounds retrospectively.

Microfabricated field calibration assembly for analytical instruments

DOEpatents

Robinson, Alex L [Albuquerque, NM; Manginell, Ronald P [Albuquerque, NM; Moorman, Matthew W [Albuquerque, NM; Rodacy, Philip J [Albuquerque, NM; Simonson, Robert J [Cedar Crest, NM

2011-03-29

A microfabricated field calibration assembly for use in calibrating analytical instruments and sensor systems. The assembly comprises a circuit board comprising one or more resistively heatable microbridge elements, an interface device that enables addressable heating of the microbridge elements, and, in some embodiments, a means for positioning the circuit board within an inlet structure of an analytical instrument or sensor system.

Development and application of GC-MS method for monitoring of long-term exposure to the pesticide cypermethrin.

PubMed

Kavvalakis, Matthaios P; Tzatzarakis, Manolis N; Alegakis, Athanasios K; Vynias, Dionysios; Tsakalof, Andreas K; Tsatsakis, Aristidis M

2014-06-01

Cypermethrin (CPMN) is a synthetic pyrethroid used as an insecticide in large-scale commercial agricultural applications as well as for domestic purposes. In the present study a gas chromatography-mass spectrometry (GC-MS) based method was developed and validated for the quantitation of CPMN metabolites, 3-phenoxybenzoic acid (3-PBA) and cis- and trans- 3-(2,2-dichlorovinyl)-2,2-dimethyl-1-cyclopropane (cis- and trans- Cl2 CA). The developed method was applied for the monitoring of CPMN metabolites in hair of laboratory animals (rabbits) intentionally exposed per os to CPMN at 40 (low dose) and 80 (high dose) mg/kg weight/day for 16 weeks. The analytical method comprises three main steps: isolation of analytes from hair, analytes derivatization, and subsequent instrumental analysis by GC-MS. The limits of detection ensured by the method are 4.0, 3.9 and 1.0 pg/mg hair for cis-Cl2 CA, trans-Cl2 CA and 3-PBA, respectively. The instrument responce is linear (r(2)  > 0.99) in the investigated concentrations range from 25 to 1000 pg/mg. With and between-run precision as well as accuracy were estimated and found satisfactory. Analytes were efficiently isolated by solid-liquid extraction from hair with recoveries greater than 84.8% for cis-Cl2 CA, 87.2% for trans-Cl2 CA and 96.4% for 3-PBA. Rabbit's hair showed increasing levels for all metabolites (metabolites accumulation in a time and dose dependent manner) over time and in a dose-dependent manner. The developed experimental procedure could be used for biomonitoring of population exposure to CPMN. Copyright © 2014 John Wiley & Sons, Ltd.

Analytical solution for the transient wave propagation of a buried cylindrical P-wave line source in a semi-infinite elastic medium with a fluid surface layer

NASA Astrophysics Data System (ADS)

Shan, Zhendong; Ling, Daosheng

2018-02-01

This article develops an analytical solution for the transient wave propagation of a cylindrical P-wave line source in a semi-infinite elastic solid with a fluid layer. The analytical solution is presented in a simple closed form in which each term represents a transient physical wave. The Scholte equation is derived, through which the Scholte wave velocity can be determined. The Scholte wave is the wave that propagates along the interface between the fluid and solid. To develop the analytical solution, the wave fields in the fluid and solid are defined, their analytical solutions in the Laplace domain are derived using the boundary and interface conditions, and the solutions are then decomposed into series form according to the power series expansion method. Each item of the series solution has a clear physical meaning and represents a transient wave path. Finally, by applying Cagniard's method and the convolution theorem, the analytical solutions are transformed into the time domain. Numerical examples are provided to illustrate some interesting features in the fluid layer, the interface and the semi-infinite solid. When the P-wave velocity in the fluid is higher than that in the solid, two head waves in the solid, one head wave in the fluid and a Scholte wave at the interface are observed for the cylindrical P-wave line source.

Applicability of UV laser-induced solid-state fluorescence spectroscopy for characterization of solid dosage forms.

PubMed

Woltmann, Eva; Meyer, Hans; Weigel, Diana; Pritzke, Heinz; Posch, Tjorben N; Kler, Pablo A; Schürmann, Klaus; Roscher, Jörg; Huhn, Carolin

2014-10-01

High production output of solid pharmaceutical formulations requires fast methods to ensure their quality. Likewise, fast analytical procedures are required in forensic sciences, for example at customs, to substantiate an initial suspicion. We here present the design and the optimization of an instrumental setup for rapid and non-invasive characterization of tablets by laser-induced fluorescence spectroscopy (with a UV-laser (λ ex = 266 nm) as excitation source) in reflection geometry. The setup was first validated with regard to repeatability, bleaching phenomena, and sensitivity. The effect on the spectra by the physical and chemical properties of the samples, e.g. their hardness, homogeneity, chemical composition, and granule grain size of the uncompressed material, using a series of tablets, manufactured in accordance with design of experiments, was investigated. Investigation of tablets with regard to homogeneity, especially, is extremely important in pharmaceutical production processes. We demonstrate that multiplicative scatter correction is an appropriate tool for data preprocessing of fluorescence spectra. Tablets with different physical and chemical characteristics can be discriminated well from their fluorescence spectra by subjecting the results to principal component analysis.

Pre-concentration technique for reduction in "Analytical instrument requirement and analysis"

NASA Astrophysics Data System (ADS)

Pal, Sangita; Singha, Mousumi; Meena, Sher Singh

2018-04-01

Availability of analytical instruments for a methodical detection of known and unknown effluents imposes a serious hindrance in qualification and quantification. Several analytical instruments such as Elemental analyzer, ICP-MS, ICP-AES, EDXRF, ion chromatography, Electro-analytical instruments which are not only expensive but also time consuming, required maintenance, damaged essential parts replacement which are of serious concern. Move over for field study and instant detection installation of these instruments are not convenient to each and every place. Therefore, technique such as pre-concentration of metal ions especially for lean stream elaborated and justified. Chelation/sequestration is the key of immobilization technique which is simple, user friendly, most effective, least expensive, time efficient; easy to carry (10g - 20g vial) to experimental field/site has been demonstrated.

A high-throughput solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for rapid determination of trace heavy metals in natural water.

PubMed

Shih, Tsung-Ting; Hsieh, Cheng-Chuan; Luo, Yu-Ting; Su, Yi-An; Chen, Ping-Hung; Chuang, Yu-Chen; Sun, Yuh-Chang

2016-04-15

Herein, a hyphenated system combining a high-throughput solid-phase extraction (htSPE) microchip with inductively coupled plasma-mass spectrometry (ICP-MS) for rapid determination of trace heavy metals was developed. Rather than performing multiple analyses in parallel for the enhancement of analytical throughput, we improved the processing speed for individual samples by increasing the operation flow rate during SPE procedures. To this end, an innovative device combining a micromixer and a multi-channeled extraction unit was designed. Furthermore, a programmable valve manifold was used to interface the developed microchip and ICP-MS instrumentation in order to fully automate the system, leading to a dramatic reduction in operation time and human error. Under the optimized operation conditions for the established system, detection limits of 1.64-42.54 ng L(-1) for the analyte ions were achieved. Validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Each analysis could be readily accomplished within just 186 s using the established system. This represents, to the best of our knowledge, an unprecedented speed for the analysis of trace heavy metal ions. Copyright © 2016 Elsevier B.V. All rights reserved.

Life in Solid Ice on Earth and Other Planetary Bodies

NASA Astrophysics Data System (ADS)

Price, P. Buford

2004-06-01

Theory and direct observation indicate that micro-organisms exist in liquid veins in ice and permafrost, provided the temperature is above the eutectic for H_2O and soluble impurities present. Microbes can exist and metabolize in glacial ice and permafrost on Earth, Mars, and Europa. One can search directly (with fluorescence microscopy at liquid veins in Vostok ice core samples) or with a biologging instrument (for microbial fluorescence in a borehole in terrestrial or martian permafrost or ice). The viability lifetime against DNA destruction of bacterial spores can be measured with analytical techniques that identify calcium dipicolinate, which is unique to spores.

Utilizing global data to estimate analytical performance on the Sigma scale: A global comparative analysis of methods, instruments, and manufacturers through external quality assurance and proficiency testing programs.

PubMed

Westgard, Sten A

2016-06-01

To assess the analytical performance of instruments and methods through external quality assessment and proficiency testing data on the Sigma scale. A representative report from five different EQA/PT programs around the world (2 US, 1 Canadian, 1 UK, and 1 Australasian) was accessed. The instrument group standard deviations were used as surrogate estimates of instrument imprecision. Performance specifications from the US CLIA proficiency testing criteria were used to establish a common quality goal. Then Sigma-metrics were calculated to grade the analytical performance. Different methods have different Sigma-metrics for each analyte reviewed. Summary Sigma-metrics estimate the percentage of the chemistry analytes that are expected to perform above Five Sigma, which is where optimized QC design can be implemented. The range of performance varies from 37% to 88%, exhibiting significant differentiation between instruments and manufacturers. Median Sigmas for the different manufacturers in three analytes (albumin, glucose, sodium) showed significant differentiation. Chemistry tests are not commodities. Quality varies significantly from manufacturer to manufacturer, instrument to instrument, and method to method. The Sigma-assessments from multiple EQA/PT programs provide more insight into the performance of methods and instruments than any single program by itself. It is possible to produce a ranking of performance by manufacturer, instrument and individual method. Laboratories seeking optimal instrumentation would do well to consult this data as part of their decision-making process. To confirm that these assessments are stable and reliable, a longer term study should be conducted that examines more results over a longer time period. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Measuring solids concentration in stormwater runoff: comparison of analytical methods.

PubMed

Clark, Shirley E; Siu, Christina Y S

2008-01-15

Stormwater suspended solids typically are quantified using one of two methods: aliquot/subsample analysis (total suspended solids [TSS]) or whole-sample analysis (suspended solids concentration [SSC]). Interproject comparisons are difficult because of inconsistencies in the methods and in their application. To address this concern, the suspended solids content has been measured using both methodologies in many current projects, but the question remains about how to compare these values with historical water-quality data where the analytical methodology is unknown. This research was undertaken to determine the effect of analytical methodology on the relationship between these two methods of determination of the suspended solids concentration, including the effect of aliquot selection/collection method and of particle size distribution (PSD). The results showed that SSC was best able to represent the known sample concentration and that the results were independent of the sample's PSD. Correlations between the results and the known sample concentration could be established for TSS samples, but they were highly dependent on the sample's PSD and on the aliquot collection technique. These results emphasize the need to report not only the analytical method but also the particle size information on the solids in stormwater runoff.

Planetary Protection Plan for an Antibody based instrument proposed for Mars2020

NASA Astrophysics Data System (ADS)

Smith, Heather; Parro, Víctor

The Signs Of Life Detector (SOLID) instrument is a high TRL level instrument proposed for the Mars 2020 instrument suite. In this presentation we describe the planetary protection instrument plan as if the instrument is classified as a life detection instrument compliant with Category IV(b) planetary protection mission requirements, NASA, ESA, and COSPAR policy. SOLID uses antibodies as a method for detecting organic and biomolecular components in soils. Due to the sensitive detection method, the scientific integrity of the instrument exceeds the planetary protection requirements. The instrument will be assembled and integrated in an ISO level 8 cleanroom or better (ISO 4 for the sample read out and fluidics components). Microbial reduction methods and assays employed are as follows: Wipe the outside and inside of the instrument with a mixture of isopropyl alcohol (70%) and water. Cell cultures will be the standard assay to determine enumeration of “viable” spores and other rapid assays such as LAL and ATP bioluminescence as secondary assays to verify the interior of the instrument is microbe free. SOLID’s design factors for contamination control include the following features: SOLID has the capability to heat the catchment tray to pyrolyze any Earth hitchhikers. There will also be an “air gap” of cm maintained between the sample acquisition device and the funnel inlet. This will prevent forward contamination of the sample collection device and reverse contamination of the detection unit. To mitigate false positives, SOLID will include anti-bodies for potential contaminants from organisms most commonly found in clean rooms. If selected for the Mars 2020 Rover, SOLID would be the first life detection instrument based on biomolecules sent by NASA, as such the planetary protection plan will set a precedence for future life detection instruments carrying biomolecules to other planetary bodies.

Comparison of different mesoporous silicas for off-line solid phase extraction of 17β-estradiol from waters and its determination by HPLC-DAD.

PubMed

Gañán, Judith; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

2013-09-15

Functionalized (SBA-C₁₈ and SM-C₁₈) and non-functionalized (SBA-15 and SM) mesoporous silicas were then examined as sorbents for solid-phase extraction of 17β-estradiol in aqueous media. Experiments were run in order to test critical factors affecting the procedure extraction efficiency, including the type of sorbent, the analyte concentration, the solvent and volume used for elution and the sample volume. Among the prepared materials, SBA-C₁₈ had the highest adsorption affinity towards 17β-estradiol and under optimized conditions (200mg of sorbent, 150 mL of water sample, elution with 3 × 2 mL of methanol) this sorbent proved good extraction capacity and elution efficiency for this hormone from aqueous media (recovery near 100%). To evaluate the analytical applicability of the proposed method, it was applied to the determination of 17β-estradiol in drinking water by high performance liquid chromatography with a photodiode array detector. Calibration curves were shown to be linear between 1.25 and 100 mg L(-1)with correlation coefficients ≥0.999 (n=5) for 17β-estradiol. The instrumental detection and quantitation limits calculated were 0.38 and 1.25 mg L(-1), respectively. The relative standard deviation obtained values were ≤3% and the mean recoveries obtained were of 82%. The results suggest that SBA-C18 is a promising material for the off-line solid phase extraction of 17β-estradiol from waters. Copyright © 2013 Elsevier B.V. All rights reserved.

Analytical improvements of hybrid LC-MS/MS techniques for the efficient evaluation of emerging contaminants in river waters: a case study of the Henares River (Madrid, Spain).

PubMed

Pérez-Parada, Andrés; Gómez-Ramos, María del Mar; Martínez Bueno, María Jesús; Uclés, Samanta; Uclés, Ana; Fernández-Alba, Amadeo R

2012-02-01

Instrumental capabilities and software tools of modern hybrid mass spectrometry (MS) instruments such as high-resolution mass spectrometry (HRMS), quadrupole time-of-flight (QTOF), and quadrupole linear ion trap (QLIT) were experimentally investigated for the study of emerging contaminants in Henares River water samples. Automated screening and confirmatory capabilities of QTOF working in full-scan MS and tandem MS (MS/MS) were explored when dealing with real samples. Investigations on the effect of sensitivity and resolution power influence on mass accuracy were studied for the correct assignment of the amoxicillin transformation product 5(R) amoxicillin-diketopiperazine-2',5' as an example of a nontarget compound. On the other hand, a comparison of quantitative and qualitative strategies based on direct injection analysis and off-line solid-phase extraction sample treatment were assayed using two different QLIT instruments for a selected group of emerging contaminants when operating in selected reaction monitoring (SRM) and information-dependent acquisition (IDA) modes. Software-aided screening usually needs a further confirmatory step. Resolving power and MS/MS feature of QTOF showed to confirm/reject most findings in river water, although sensitivity-related limitations are usually found. Superior sensitivity of modern QLIT-MS/MS offered the possibility of direct injection analysis for proper quantitative study of a variety of contaminants, while it simultaneously reduced the matrix effect and increased the reliability of the results. Confirmation of ethylamphetamine, which lacks on a second SRM transition, was accomplished by using the IDA feature. Hybrid MS instruments equipped with high resolution and high sensitivity contributes to enlarge the scope of targeted analytes in river waters. However, in the tested instruments, there is a margin of improvement principally in required sensitivity and data treatment software tools devoted to reliable confirmation and improved automated data processing.

Instrumentation '79.

ERIC Educational Resources Information Center

Chemical and Engineering News, 1979

1979-01-01

Surveys the state of commerical development of analytical instrumentation as reflected by the Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. Includes optical spectroscopy, liquid chromatography, magnetic spectrometers, and x-ray. (Author/MA)

Analytical Chemistry in Russia.

PubMed

Zolotov, Yuri

2016-09-06

Research in Russian analytical chemistry (AC) is carried out on a significant scale, and the analytical service solves practical tasks of geological survey, environmental protection, medicine, industry, agriculture, etc. The education system trains highly skilled professionals in AC. The development and especially manufacturing of analytical instruments should be improved; in spite of this, there are several good domestic instruments and other satisfy some requirements. Russian AC has rather good historical roots.

Space debris, asteroids and satellite orbits; Proceedings of the Fourth and Thirteenth Workshops, Graz, Austria, June 25-July 7, 1984

NASA Technical Reports Server (NTRS)

Kessler, D. J.; Gruen, E.; Sehnal, L.

1985-01-01

The workshops covered a variety of topics relevant to the identification, characterization and monitoring of near-earth solar system debris. Attention was given to man-made and naturally occurring microparticles, their hazards to present and future spacecraft, and ground- and space-based techniques for tracking both large and small debris. The studies are extended to solid fuel particulates in circular space. Asteroid rendezvous missions are discussed, including propulsion and instrumentation options, the possibility of encountering asteroids during Hohman transfer flights to Venus and/or Mars, and the benefits of multiple encounters by one spacecraft. Finally, equipment and analytical models for generating precise satellite orbits are reviewed.

Raman Laser Spectrometer for 2020 ExoMars

NASA Astrophysics Data System (ADS)

Moral, Andoni G.; Pérez, Carlos; INTA, University of Valladolid, INSA, Leicester University, IRAP, RAL, OHB

2016-10-01

The Raman Laser Spectrometer (RLS) is one of the Pasteur Payload instruments, within the ESA's Aurora Exploration Programme, ExoMars mission.ExoMars 2020 main scientific objective is "Searching for evidence of past and present life on Mars".Raman Spectroscopy is used to analyze the vibrational modes of a substance either in the solid, liquid or gas state. It relies on the inelastic scattering (Raman Scattering) of monochromatic light produced by atoms and molecules. The radiation-matter interaction results in the energy of the exciting photons to be shifted up or down. The shift in energy appears as a spectral distribution and therefore provides an unique fingerprint by which the substances can be identified and structurally analyzed.The RLS is being developed by an European Consortium composed by Spanish, UK, French and German partners. It will perform Raman spectroscopy on crushed powdered samples, obtained from 2 meters depth under Mars surface, inside the Rover's Analytical Laboratory Drawer.After a wide campaign for evaluating Instrument performances by means of simulation tools and development of an instrument prototype, Instrument Structural and Thermal Model was successfully delivered on February 2015, and the Engineering and Qualification Model has been manufactured and is expected to be delivered by November 2016, after a testing campaign developed during Q2 & Q3 of 2016.A summary of main Instrument performances obtained during the last months, achieving high levels of spectral resolution and accuracy in the obtained spectra.

Organoarsenicals in poultry litter: detection, fate, and toxicity.

PubMed

P Mangalgiri, Kiranmayi; Adak, Asok; Blaney, Lee

2015-02-01

Arsenic contamination in groundwater has endangered the health and safety of millions of people around the world. One less studied mechanism for arsenic introduction into the environment is the use of organoarsenicals in animal feed. Four organoarsenicals are commonly employed as feed additives: arsanilic acid, carbarsone, nitarsone, and roxarsone. Organoarsenicals are composed of a phenylarsonic acid molecule with substituted functional groups. This review documents the use of organoarsenicals in the poultry industry, reports analytical methods available for quantifying organic arsenic, discusses the fate and transport of organoarsenicals in environmental systems, and identifies toxicological concerns associated with these chemicals. In reviewing the literature on organoarsenicals, several research needs were highlighted: advanced analytical instrumentation that allows for identification and quantification of organoarsenical degradation products; a greater research emphasis on arsanilic acid, carbarsone, and nitarsone; identification of degradation pathways, products, and kinetics; and testing/development of agricultural wastewater and solid treatment technologies for organoarsenical-laden waste. Copyright © 2014 Elsevier Ltd. All rights reserved.

Comparison between 2 methods of solid-liquid extraction for the production of Cinchona calisaya elixir: an experimental kinetics and numerical modeling approach.

PubMed

Naviglio, Daniele; Formato, Andrea; Gallo, Monica

2014-09-01

The purpose of this study is to compare the extraction process for the production of China elixir starting from the same vegetable mixture, as performed by conventional maceration or a cyclically pressurized extraction process (rapid solid-liquid dynamic extraction) using the Naviglio Extractor. Dry residue was used as a marker for the kinetics of the extraction process because it was proportional to the amount of active principles extracted and, therefore, to their total concentration in the solution. UV spectra of the hydroalcoholic extracts allowed for the identification of the predominant chemical species in the extracts, while the organoleptic tests carried out on the final product provided an indication of the acceptance of the beverage and highlighted features that were not detectable by instrumental analytical techniques. In addition, a numerical simulation of the process has been performed, obtaining useful information about the timing of the process (time history) as well as its mathematical description. © 2014 Institute of Food Technologists®

Recent Advances in On-Line Methods Based on Extraction for Speciation Analysis of Chromium in Environmental Matrices.

PubMed

Trzonkowska, Laura; Leśniewska, Barbara; Godlewska-Żyłkiewicz, Beata

2016-07-03

The biological activity of Cr(III) and Cr(VI) species, their chemical behavior, and toxic effects are dissimilar. The speciation analysis of Cr(III) and Cr(VI) in environmental matrices is then of great importance and much research has been devoted to this area. This review presents recent developments in on-line speciation analysis of chromium in such samples. Flow systems have proved to be excellent tools for automation of sample pretreatment, separation/preconcentration of chromium species, and their detection by various instrumental techniques. Analytical strategies used in chromium speciation analysis discussed in this review are divided into categories based on selective extraction/separation of chromium species on solid sorbents and liquid-liquid extraction of chromium species. The most popular strategy is that based on solid-phase extraction. Therefore, this review shows the potential of novel materials designed and used for selective binding of chromium species. The progress in miniaturization of measurement systems is also presented.

Data Acquisition Programming (LabVIEW): An Aid to Teaching Instrumental Analytical Chemistry.

ERIC Educational Resources Information Center

Gostowski, Rudy

A course was developed at Austin Peay State University (Tennessee) which offered an opportunity for hands-on experience with the essential components of modern analytical instruments. The course aimed to provide college students with the skills necessary to construct a simple model instrument, including the design and fabrication of electronic…

Normal incidence X-ray mirror for chemical microanalysis

DOEpatents

Carr, Martin J.; Romig, Jr., Alton D.

1990-01-01

A non-planar, focusing mirror, to be utilized in both electron column instruments and micro-x-ray fluorescence instruments for performing chemical microanalysis on a sample, comprises a concave, generally spherical base substrate and a predetermined number of alternating layers of high atomic number material and low atomic number material contiguously formed on the base substrate. The thickness of each layer is an integral multiple of the wavelength being reflected and may vary non-uniformly according to a predetermined design. The chemical analytical instruments in which the mirror is used also include a predetermined energy source for directing energy onto the sample and a detector for receiving and detecting the x-rays emitted from the sample; the non-planar mirror is located between the sample and detector and collects the x-rays emitted from the sample at a large solid angle and focuses the collected x-rays to the sample. For electron column instruments, the wavelengths of interest lie above 1.5 nm, while for x-ray fluorescence instruments, the range of interest is below 0.2 nm. Also, x-ray fluorescence instruments include an additional non-planar focusing mirror, formed in the same manner as the previously described m The invention described herein was made in the performance of work under contract with the Department of Energy, Contract No. DE-AC04-76DP00789, and the United States Government has rights in the invention pursuant to this contract.

Instrumental effects on the temperature and density derived from the light ion mass spectrometer

NASA Technical Reports Server (NTRS)

Craven, P. D.; Reasoner, D. L.

1983-01-01

An expression for the flux into a retarding potential analyzer (RPA) is derived which takes into account the instrumental effect of a dependence on energy of the solid angle of the acceptance cone. A second instrumental effect of a limited bandpass is briefly discussed. Using the (LIMS) instrument on SCATHA, it is shown that temperatures and densities derived without considering the effect of the solid angle dependence on energy will be too low, dramatically so for E(t) E(1), where E(1) is the e folding distance of the solid angle dependence and E(t) is the thermal energy of the plasma. For E(t) E(1), there is effectively no impact on the derived temperatures and densities if the solid angle effect is ignored.

[Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry].

PubMed

Wang, Jincheng; Xiong, Li; Zhang, Haijun; Chen, Jiping

2011-12-01

A simple method based on solid phase extraction (SPE) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of octylphenol (OP), nonylphenol (NP), octylphenol ethoxylates (OPEOs) and nonylphenol ethoxylates (NPEOs) in brine. The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges. The complete separation among OP, NP, OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase. The determination was achieved using HPLC-MS with electrospray ionization (ESI) in selected ion monitoring mode. The results showed that the average recoveries of target compounds were 59.6% - 104.4% and the corresponding relative standard deviations (RSDs, n = 3) were 1.0% - 13.5%. The instrumental limits of detection for the compounds were 0.08 - 3 microg/L. This method was applied to the analysis of the samples of seawater near Dalian coast. The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.

Chemical Detection and Identification Techniques for Exobiology Flight Experiments

NASA Technical Reports Server (NTRS)

Kojiro, Daniel R.; Sheverev, Valery A.; Khromov, Nikolai A.

2002-01-01

Exobiology flight experiments require highly sensitive instrumentation for in situ analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical Instrumentation to detect and identify all species present. The minimal resources available onboard for such missions mandate that the instruments provide maximum analytical capabilities with minimal requirements of volume, weight and consumables. Advances in technology may be achieved by increasing the amount of information acquired by a given technique with greater analytical capabilities and miniaturization of proven terrestrial technology. We describe here methods to develop analytical instruments for the detection and identification of a wide range of chemical species using Gas Chromatography. These efforts to expand the analytical capabilities of GC technology are focused on the development of detectors for the GC which provide sample identification independent of the GC retention time data. A novel new approach employs Penning Ionization Electron Spectroscopy (PIES).

Solid Lubrication Fundamentals and Applications. Chapter 2

NASA Technical Reports Server (NTRS)

Miyoshi, Kazuhisa

1998-01-01

This chapter describes powerful analytical techniques capable of sampling tribological surfaces and solid-film lubricants. Some of these techniques may also be used to determine the locus of failure in a bonded structure or coated substrate; such information is important when seeking improved adhesion between a solid-film lubricant and a substrate and when seeking improved performance and long life expectancy of solid lubricants. Many examples are given here and through-out the book on the nature and character of solid surfaces and their significance in lubrication, friction, and wear. The analytical techniques used include the late spectroscopic methods.

Detection of Organic Constituents Including Chloromethylpropene in the Analyses of the ROCKNEST Drift by Sample Analysis at Mars (SAM)

NASA Technical Reports Server (NTRS)

Eigenbrode, J. L.; Glavin, D.; Coll, P.; Summons, R. E.; Mahaffy, P.; Archer, D.; Brunner, A.; Conrad, P.; Freissinet, C.; Martin, M.;

The SOLID (Signs Of LIfe Detector) instrument concept: an antibody microarray-based biosensor for life detection in astrobiology

NASA Astrophysics Data System (ADS)

Parro, V.; Rivas, L. A.; Rodríguez-Manfredi, J. A.; Blanco, Y.; de Diego-Castilla, G.; Cruz-Gil, P.; Moreno-Paz, M.; García-Villadangos, M.; Compostizo, C.; Herrero, P. L.

2009-04-01

Immunosensors have been extensively used since many years for environmental monitoring. Different technological platforms allow new biosensor designs and implementations. We have reported (Rivas et al., 2008) a shotgun approach for antibody production for biomarker detection in astrobiology and environmental monitoring, the production of 150 new polyclonal antibodies against microbial strains and environmental extracts, and the construction and validation of an antibody microarray (LDCHIP200, for "Life Detector Chip") containing 200 different antibodies. We have successfully used the LDCHIP200 for the detection of biological polymers in extreme environments in different parts of the world (e.g., a deep South African mine, Antarctica's Dry valleys, Yellowstone, Iceland, and Rio Tinto). Clustering analysis associated similar immunopatterns to samples from apparently very different environments, indicating that they indeed share similar universal biomarkers. A redundancy in the number of antibodies against different target biomarkers apart of revealing the presence of certain biomolecules, it renders a sample-specific immuno-profile, an "immnuno-fingerprint", which may constitute by itself an indirect biosignature. We will present a case study of immunoprofiling different iron-sulfur as well as phylosilicates rich samples along the Rio Tinto river banks. Based on protein microarray technology, we designed and built the concept instrument called SOLID (for "Signs Of LIfe Detector"; Parro et al., 2005; 2008a, b; http://cab.inta.es/solid) for automatic in situ analysis of soil samples and molecular biomarkers detection. A field prototype, SOLID2, was successfully tested for the analysis of grinded core samples during the 2005 "MARTE" campaign of a Mars drilling simulation experiment by a sandwich microarray immunoassay (Parro et al., 2008b). We will show the new version of the instrument (SOLID3) which is able to perform both sandwich and competitive immunoassays. SOLID3 consists of two separate functional units: a Sample Preparation Unit (SPU), for ten different extractions by ultrasonication, and a Sample Analysis Unit (SAU), for fluorescent immunoassays. The SAU consists of ten different flow cells each of one allocate one antibody microarray (up to 2000 spots), and is equipped with an unique designed optical package for fluorescent detection. We demonstrate the performance of SOLID3 for the detection of a broad range of molecular size compounds, from the amino acid size, peptides, proteins, to whole cells and spores, with sensitivities at the ppb level. References Parro, V., et al., 2005. Planetary and Space Science 53: 729-737. Parro, V., et al., 2008a. Space Science Reviews 135: 293-311 Parro, V., et al., 2008b. Astrobiology 8:987-99 Rivas, L. A., et al., 2008. Analytical Chemistry 80: 7970-7979

Analytical techniques for characterization of cyclodextrin complexes in the solid state: A review.

PubMed

Mura, Paola

2015-09-10

Cyclodextrins are cyclic oligosaccharides able to form inclusion complexes with a variety of hydrophobic guest molecules, positively modifying their physicochemical properties. A thorough analytical characterization of cyclodextrin complexes is of fundamental importance to provide an adequate support in selection of the most suitable cyclodextrin for each guest molecule, and also in view of possible future patenting and marketing of drug-cyclodextrin formulations. The demonstration of the actual formation of a drug-cyclodextrin inclusion complex in solution does not guarantee its existence also in the solid state. Moreover, the technique used to prepare the solid complex can strongly influence the properties of the final product. Therefore, an appropriate characterization of the drug-cyclodextrin solid systems obtained has also a key role in driving in the choice of the most effective preparation method, able to maximize host-guest interactions. The analytical characterization of drug-cyclodextrin solid systems and the assessment of the actual inclusion complex formation is not a simple task and involves the combined use of several analytical techniques, whose results have to be evaluated together. The objective of the present review is to present a general prospect of the principal analytical techniques which can be employed for a suitable characterization of drug-cyclodextrin systems in the solid state, evidencing their respective potential advantages and limits. The applications of each examined technique are described and discussed by pertinent examples from literature. Copyright © 2015 Elsevier B.V. All rights reserved.

A miniaturised laser ablation/ionisation analyser for investigation of elemental/isotopic composition with the sub-ppm detection sensitivity

NASA Astrophysics Data System (ADS)

Tulej, M.; Riedo, A.; Meyer, S.; Iakovleva, M.; Neuland, M.; Wurz, P.

2012-04-01

Detailed knowledge of the elemental and isotopic composition of solar system objects imposes critical constraints on models describing the origin of our solar system and can provide insight to chemical and physical processes taking place during the planetary evolution. So far, the investigation of chemical composition of planetary surfaces could be conducted almost exclusively by remotely controlled spectroscopic instruments from orbiting spacecraft, landers or rovers. With some exceptions, the sensitivity of these techniques is, however, limited and often only abundant elements can be investigated. Nevertheless, the spectroscopic techniques proved to be successful for global chemical mapping of entire planetary objects such as the Moon, Mars and asteroids. A combined afford of the measurements from orbit, landers and rovers can also yield the determination of local mineralogy. New instruments including Laser Induced Breakdown Spectroscopy (LIBS) and Laser Ablation/Ionisation Mass Spectrometer (LIMS), have been recently included for several landed missions. LIBS is thought to improve flexibility of the investigations and offers a well localised chemical probing from distances up to 10-13 m. Since LIMS is a mass spectrometric technique it allows for very sensitive measurements of elements and isotopes. We will demonstrate the results of the current performance tests obtained by application of a miniaturised laser ablation/ionisation mass spectrometer, a LIMS instrument, developed in Bern for the chemical analysis of solids. So far, the only LIMS instrument on a spacecraft is the LAZMA instrument. This spectrometer was a part of the payload for PHOBOS-GRUNT mission and is also currently selected for LUNA-RESURCE and LUNA-GLOB missions to the lunar south poles (Managadze et al., 2011). Our LIMS instrument has the dimensions of 120 x Ø60 mm and with a weight of about 1.5 kg (all electronics included), it is the lightest mass analyser designed for in situ chemical analysis of solid materials on the planetary surfaces (Rohner et al., 2003). Initial laboratory tests that were conducted with an IR laser radiation for the ablation, atomisation and ionisation of the material, indicated a high performance of the instrument in terms of sensitivity, dynamic range and mass resolution (Tulej et al., 2011). After some technical improvements and implementation of a computer-controlled performance optimiser we have achieved further improvements of both, the instrumental sensitivity down to sub-ppm level and reproducibility of the measurements. We will demonstrate the potential of the mass analyser to perform the quantitative elemental analysis of solids with a spatial (vertical, lateral) resolution commensurate with typical grain sizes, and its capabilities for investigation of isotopic patterns with accuracy and precision comparable to that of large analytical laboratory instruments, e.g., TIMS, SIMS, LA-ICP-MS. The results can be of considerable interest for in situ dating or investigation of other fine isotopic fractionation effects including studies of bio-markers.

Sample Analysis at Mars Instrument Simulator

NASA Technical Reports Server (NTRS)

Benna, Mehdi; Nolan, Tom

2013-01-01

The Sample Analysis at Mars Instrument Simulator (SAMSIM) is a numerical model dedicated to plan and validate operations of the Sample Analysis at Mars (SAM) instrument on the surface of Mars. The SAM instrument suite, currently operating on the Mars Science Laboratory (MSL), is an analytical laboratory designed to investigate the chemical and isotopic composition of the atmosphere and volatiles extracted from solid samples. SAMSIM was developed using Matlab and Simulink libraries of MathWorks Inc. to provide MSL mission planners with accurate predictions of the instrument electrical, thermal, mechanical, and fluid responses to scripted commands. This tool is a first example of a multi-purpose, full-scale numerical modeling of a flight instrument with the purpose of supplementing or even eliminating entirely the need for a hardware engineer model during instrument development and operation. SAMSIM simulates the complex interactions that occur between the instrument Command and Data Handling unit (C&DH) and all subsystems during the execution of experiment sequences. A typical SAM experiment takes many hours to complete and involves hundreds of components. During the simulation, the electrical, mechanical, thermal, and gas dynamics states of each hardware component are accurately modeled and propagated within the simulation environment at faster than real time. This allows the simulation, in just a few minutes, of experiment sequences that takes many hours to execute on the real instrument. The SAMSIM model is divided into five distinct but interacting modules: software, mechanical, thermal, gas flow, and electrical modules. The software module simulates the instrument C&DH by executing a customized version of the instrument flight software in a Matlab environment. The inputs and outputs to this synthetic C&DH are mapped to virtual sensors and command lines that mimic in their structure and connectivity the layout of the instrument harnesses. This module executes, and thus validates, complex command scripts prior to their up-linking to the SAM instrument. As an output, this module generates synthetic data and message logs at a rate that is similar to the actual instrument.

Analytical Electrochemistry: Theory and Instrumentation of Dynamic Techniques.

ERIC Educational Resources Information Center

Johnson, Dennis C.

1980-01-01

Emphasizes trends in the development of six topics concerning analytical electrochemistry, including books and reviews (34 references cited), mass transfer (59), charge transfer (25), surface effects (33), homogeneous reactions (21), and instrumentation (31). (CS)

[Survey of analytical works for drugs at emergency and critical care centers with high-performance instruments provided by the Ministry of Health and Welfare (at present: Ministry of Health, Labour, and Welfare) in fiscal 1998--continuation of survey with 2008 survey results as point of reference].

PubMed

Saito, Takeshi; Tominaga, Aya; Nozawa, Mayu; Unei, Hiroko; Hatano, Yayoi; Fujita, Yuji; Iseki, Ken; Hori, Yasushi

2013-09-01

In a 2008 survey of the 73 emergency and critical care centers around the nation that were equipped with the drug and chemical analytical instrument provided by the Ministry of Welfare (currently the Ministry of Health, Labour, and Welfare) in 1998, 36 of those facilities were using the analytical instruments. Of these 36 facilities, a follow-up survey of the 17 facilities that recorded 50 or analyses per year. Responses were gained from 16 of the facilities and we learned that of those, 14 facilities (87.5%) were conducting analyses using the instrument. There was a positive mutual correlation between the annual number of cases of the 14 facilities conducting analyses with the instrument and the number of work hours. Depending on the instrument in use, average analytical instrument parts and maintenance expenses were roughly three million yen and consumables required a maximum three million yen for analysis of 51-200 cases per year. From this, we calculate that such expenses can be covered under the allowed budget for advanced emergency and critical care centers of 5,000 NHI points (1 point = 10 yen). We found there were few facilities using the instrument for all 15 of the toxic substances recommended for testing by the Japanese Society for Clinical Toxicology. There tended to be no use of the analytical instrument for compounds with no toxicology cases. However, flexible responses were noted at each facility in relation to frequently analyzed compounds. It is thought that a reevaluation of compounds subject to analysis is required.

Assessment of economic instruments for countries with low municipal waste management performance: An approach based on the analytic hierarchy process.

PubMed

Kling, Maximilian; Seyring, Nicole; Tzanova, Polia

2016-09-01

Economic instruments provide significant potential for countries with low municipal waste management performance in decreasing landfill rates and increasing recycling rates for municipal waste. In this research, strengths and weaknesses of landfill tax, pay-as-you-throw charging systems, deposit-refund systems and extended producer responsibility schemes are compared, focusing on conditions in countries with low waste management performance. In order to prioritise instruments for implementation in these countries, the analytic hierarchy process is applied using results of a literature review as input for the comparison. The assessment reveals that pay-as-you-throw is the most preferable instrument when utility-related criteria are regarded (wb = 0.35; analytic hierarchy process distributive mode; absolute comparison) mainly owing to its waste prevention effect, closely followed by landfill tax (wb = 0.32). Deposit-refund systems (wb = 0.17) and extended producer responsibility (wb = 0.16) rank third and fourth, with marginal differences owing to their similar nature. When cost-related criteria are additionally included in the comparison, landfill tax seems to provide the highest utility-cost ratio. Data from literature concerning cost (contrary to utility-related criteria) is currently not sufficiently available for a robust ranking according to the utility-cost ratio. In general, the analytic hierarchy process is seen as a suitable method for assessing economic instruments in waste management. Independent from the chosen analytic hierarchy process mode, results provide valuable indications for policy-makers on the application of economic instruments, as well as on their specific strengths and weaknesses. Nevertheless, the instruments need to be put in the country-specific context along with the results of this analytic hierarchy process application before practical decisions are made. © The Author(s) 2016.

Development of a pressurized liquid extraction-solid-phase extraction followed by liquid chromatography-electrospray ionization tandem mass spectrometry method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soil.

PubMed

Villagrasa, M; Guillamón, M; Navarro, A; Eljarrat, E; Barceló, D

2008-02-01

A new analytical method for the quantitative determination of benzoxazolinones and their degradation products in agricultural soils based on the use of pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) and then instrumental determination using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS) is described. Using this method, the characterization, separation and quantitative detection of a mixture of two benzoxazolinones, benzoxazolin-2-one (BOA) and 6-methoxybenzoxazolin-2-one (MBOA) and their degradation products, 2-aminophenol (APH), N-(2-hydroxyphenyl)malonamic acid (HMPMA), 2-amino-3-H-phenoxazin-3-one (APO), 9-methoxy-2-amino-3-H-phenoxazin-3-one (AMPO), 2-acetylamino-3-H-phenoxazin-3-one (AAPO) and 2-acetylamino-9-methoxy-2-amino-3-H-phenoxazin-3-one (AAMPO) was achieved. The complete LC-ESI-MS-MS precursor-product ion fragmentation pathways for the degradation products of benzoxazolinones are described for the first time. Quantitative analysis was done in the multiple reaction mode using two specific combinations of precursor-product ion transitions for each compound. The optimized method was quality assessed by the measure of parameter as recovery, linearity, sensitivity, repeatability and reproducibility. Recoveries of the analytes ranged from 53 to 123%. The developed method offered improvements to the sensitivity as compared with our previously LC-MS method, with detection limits down to 2.4-21 ng/g of dry weight. This achievement allows us to identify and quantify for the first time degradation products of benzoxazolinones in real agricultural soil samples. Analytes were found in the range of 20.6-149 ng/g dry weight.

Continuous low-level aquatic monitoring (CLAM) samplers for pesticide contaminant screening in urban runoff: Analytical approach and a field test case.

PubMed

Ensminger, Michael P; Vasquez, Martice; Tsai, Hsing-Ju; Mohammed, Sarah; Van Scoy, A; Goodell, Korena; Cho, Gail; Goh, Kean S

2017-10-01

Monitoring of surface waters for organic contaminants is costly. Grab water sampling often results in non-detects for organic contaminants due to missing a pulse event or analytical instrumentation limitations with a small sample size. Continuous Low-Level Aquatic Monitoring (CLAM) samplers (C.I.Agent ® Solutions) continually extract and concentrate organic contaminants in surface water onto a solid phase extraction disk. Utilizing CLAM samplers, we developed a broad spectrum analytical screen for monitoring organic contaminants in urban runoff. An intermediate polarity solid phase, hydrophobic/lipophilic balance (HLB), was chosen as the sorbent for the CLAM to target a broad range of compounds. Eighteen urban-use pesticides and pesticide degradates were targeted for analysis by LC/MS/MS, with recoveries between 59 and 135% in laboratory studies. In field studies, CLAM samplers were deployed at discrete time points from February 2015 to March 2016. Half of the targeted chemicals were detected with reporting limits up to 90 times lower than routine 1-L grab samples with good precision between field replicates. In a final deployment, CLAM samplers were compared to 1-L water samples. In this side-by-side comparison, imidacloprid, fipronil, and three fipronil degradates were detected by the CLAM sampler but only imidacloprid and fipronil sulfone were detected in the water samples. However, concentrations of fipronil sulfone and imidacloprid were significantly lower with the CLAM and a transient spike of diuron was not detected. Although the CLAM sampler has limitations, it can be a powerful tool for development of more focused and informed monitoring efforts based on pre-identified targets in the field. Copyright © 2017 Elsevier Ltd. All rights reserved.

Comparative evaluation of liquid-liquid extraction, solid-phase extraction and solid-phase microextraction for the gas chromatography-mass spectrometry determination of multiclass priority organic contaminants in wastewater.

PubMed

Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

2013-12-15

The European Water Framework Directive (WFD) 2000/60/EC establishes guidelines to control the pollution of surface water by sorting out a list of priority substances that involves a significant risk to or via the aquatic systems. In this article, the analytical performance of three different sample preparation methodologies for the GC-MS/MS determination of multiclass organic contaminants-including priority comprounds from the WFD-in wastewater samples using gas chromatography-mass spectrometry was evaluated. The methodologies tested were: (a) liquid-liquid extraction (LLE) with n-hexane; (b) solid-phase extraction (SPE) with C18 cartridges and elution with ethyl acetate:dichloromethane (1:1 (v/v)), and (c) headspace solid-phase microextraction (HS-SPME) using two different fibers: polyacrylate and polydimethylsiloxane/carboxen/divinilbenzene. Identification and confirmation of the selected 57 compounds included in the study (comprising polycyclic aromatic hydrocarbons (PAHs), pesticides and other contaminants) were accomplished using gas chromatography tandem mass spectrometry (GC-MS/MS) with a triple quadrupole instrument operated in the multiple reaction monitoring (MRM) mode. Three MS/MS transitions were selected for unambiguous confirmation of the target chemicals. The different advantages and pitfalls of each method were discussed. In the case of both LLE and SPE procedures, the method was validated at two different concentration levels (15 and 150 ng L(-1)) obtaining recovery rates in the range 70-120% for most of the target compounds. In terms of analyte coverage, results with HS-SPME were not satisfactory, since 14 of the compounds tested were not properly recovered and the overall performance was worse than the other two methods tested. LLE, SPE and HS-SPME (using polyacrylate fiber) procedures also showed good linearity and precision. Using any of the three methodologies tested, limits of quantitation obtained for most of the detected compounds were in the low nanogram per liter range. © 2013 Elsevier B.V. All rights reserved.

Developments in analytical instrumentation

NASA Astrophysics Data System (ADS)

Petrie, G.

The situation regarding photogrammetric instrumentation has changed quite dramatically over the last 2 or 3 years with the withdrawal of most analogue stereo-plotting machines from the market place and their replacement by analytically based instrumentation. While there have been few new developments in the field of comparators, there has been an explosive development in the area of small, relatively inexpensive analytical stereo-plotters based on the use of microcomputers. In particular, a number of new instruments have been introduced by manufacturers who mostly have not been associated previously with photogrammetry. Several innovative concepts have been introduced in these small but capable instruments, many of which are aimed at specialised applications, e.g. in close-range photogrammetry (using small-format cameras); for thematic mapping (by organisations engaged in environmental monitoring or resources exploitation); for map revision, etc. Another innovative and possibly significant development has been the production of conversion kits to convert suitable analogue stereo-plotting machines such as the Topocart, PG-2 and B-8 into fully fledged analytical plotters. The larger and more sophisticated analytical stereo-plotters are mostly being produced by the traditional mainstream photogrammetric systems suppliers with several new instruments and developments being introduced at the top end of the market. These include the use of enlarged photo stages to handle images up to 25 × 50 cm format; the complete integration of graphics workstations into the analytical plotter design; the introduction of graphics superimposition and stereo-superimposition; the addition of correlators for the automatic measurement of height, etc. The software associated with this new analytical instrumentation is now undergoing extensive re-development with the need to supply photogrammetric data as input to the more sophisticated G.I.S. systems now being installed by clients, instead of the data being used mostly in the digital mapping systems operated in-house by mapping organisations. These various new hardware and software developments are reported upon and analysed in this Invited Paper presented to ISPRS Commission II at the 1988 Kyoto Congress.

Accommodating subject and instrument variations in spectroscopic determinations

DOEpatents

Haas, Michael J [Albuquerque, NM; Rowe, Robert K [Corrales, NM; Thomas, Edward V [Albuquerque, NM

2006-08-29

A method and apparatus for measuring a biological attribute, such as the concentration of an analyte, particularly a blood analyte in tissue such as glucose. The method utilizes spectrographic techniques in conjunction with an improved instrument-tailored or subject-tailored calibration model. In a calibration phase, calibration model data is modified to reduce or eliminate instrument-specific attributes, resulting in a calibration data set modeling intra-instrument or intra-subject variation. In a prediction phase, the prediction process is tailored for each target instrument separately using a minimal number of spectral measurements from each instrument or subject.

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry.

PubMed

Grate, Jay W; Gonzalez, Jhanis J; O'Hara, Matthew J; Kellogg, Cynthia M; Morrison, Samuel S; Koppenaal, David W; Chan, George C-Y; Mao, Xianglei; Zorba, Vassilia; Russo, Richard E

2017-09-08

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standards.

Sharing the Data along with the Responsibility: Examining an Analytic Scale-Based Model for Assessing School Climate.

ERIC Educational Resources Information Center

Shindler, John; Taylor, Clint; Cadenas, Herminia; Jones, Albert

This study was a pilot effort to examine the efficacy of an analytic trait scale school climate assessment instrument and democratic change system in two urban high schools. Pilot study results indicate that the instrument shows promising soundness in that it exhibited high levels of validity and reliability. In addition, the analytic trait format…

Inorganic trace analysis by mass spectrometry

NASA Astrophysics Data System (ADS)

Becker, Johanna Sabine; Dietze, Hans-Joachim

1998-10-01

Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of high-purity materials and environmental samples) is used in order to improve the detection limits of trace elements. Furthermore, the determination of chemical elements in the trace and ultratrace concentration range is often difficult and can be disturbed through mass interferences of analyte ions by molecular ions at the same nominal mass. By applying double-focusing sector field mass spectrometry at the required mass resolution—by the mass spectrometric separation of molecular ions from the analyte ions—it is often possible to overcome these interference problems. Commercial instrumental equipment, the capability (detection limits, accuracy, precision) and the analytical application fields of mass spectrometric methods for the determination of trace and ultratrace elements and for surface analysis are discussed.

Method and apparatus for continuous fluid leak monitoring and detection in analytical instruments and instrument systems

DOEpatents

Weitz, Karl K [Pasco, WA; Moore, Ronald J [West Richland, WA

2010-07-13

A method and device are disclosed that provide for detection of fluid leaks in analytical instruments and instrument systems. The leak detection device includes a collection tube, a fluid absorbing material, and a circuit that electrically couples to an indicator device. When assembled, the leak detection device detects and monitors for fluid leaks, providing a preselected response in conjunction with the indicator device when contacted by a fluid.

Solid motor diagnostic instrumentation. [design of self-contained instrumentation

NASA Technical Reports Server (NTRS)

Nakamura, Y.; Arens, W. E.; Wuest, W. S.

1973-01-01

A review of typical surveillance and monitoring practices followed during the flight phases of representative solid-propellant upper stages and apogee motors was conducted to evaluate the need for improved flight diagnostic instrumentation on future spacecraft. The capabilities of the flight instrumentation package were limited to the detection of whether or not the solid motor was the cause of failure and to the identification of probable primary failure modes. Conceptual designs of self-contained flight instrumentation packages capable of meeting these reqirements were generated and their performance, typical cost, and unit characteristics determined. Comparisons of a continuous real time and a thresholded hybrid design were made on the basis of performance, mass, power, cost, and expected life. The results of this analysis substantiated the feasibility of a self-contained independent flight instrumentation module as well as the existence of performance margins by which to exploit growth option applications.

Method development and validation for simultaneous quantification of 15 drugs of abuse and prescription drugs and 7 of their metabolites in whole blood relevant in the context of driving under the influence of drugs--usefulness of multi-analyte calibration.

PubMed

Steuer, Andrea E; Forss, Anna-Maria; Dally, Annika M; Kraemer, Thomas

2014-11-01

In the context of driving under the influence of drugs (DUID), not only common drugs of abuse may have an influence, but also medications with similar mechanisms of action. Simultaneous quantification of a variety of drugs and medications relevant in this context allows faster and more effective analyses. Therefore, multi-analyte approaches have gained more and more popularity in recent years. Usually, calibration curves for such procedures contain a mixture of all analytes, which might lead to mutual interferences. In this study we investigated whether the use of such mixtures leads to reliable results for authentic samples containing only one or two analytes. Five hundred microliters of whole blood were extracted by routine solid-phase extraction (SPE, HCX). Analysis was performed on an ABSciex 3200 QTrap instrument with ESI+ in scheduled MRM mode. The method was fully validated according to international guidelines including selectivity, recovery, matrix effects, accuracy and precision, stabilities, and limit of quantification. The selected SPE provided recoveries >60% for all analytes except 6-monoacetylmorphine (MAM) with coefficients of variation (CV) below 15% or 20% for quality controls (QC) LOW and HIGH, respectively. Ion suppression >30% was found for benzoylecgonine, hydrocodone, hydromorphone, MDA, oxycodone, and oxymorphone at QC LOW, however CVs were always below 10% (n=6 different whole blood samples). Accuracy and precision criteria were fulfilled for all analytes except for MAM. Systematic investigation of accuracy determined for QC MED in a multi-analyte mixture compared to samples containing only single analytes revealed no relevant differences for any analyte, indicating that a multi-analyte calibration is suitable for the presented method. Comparison of approximately 60 samples to a former GC-MS method showed good correlation. The newly validated method was successfully applied to more than 1600 routine samples and 3 proficiency tests. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Two-year solid hydrogen cooler for the Cryogenic Limb Array Etalon Spectrometer (CLAES) instrument

NASA Technical Reports Server (NTRS)

Naes, L. G.; Nast, T. C.; Roche, A. E.; Forney, P. B.

1983-01-01

The Cryogenic Limb Array Etalon Spectrometer (CLAES) will be one of thirteen instruments on board the Upper Atmospheric Research Satellite (UARS) in late 1988. CLAES is to be employed for the measurement of stratospheric trace species concentrations affecting the ozone layer balance. It is an earth-limb viewing instrument which requires cryogenic cooling in order to obtain the necessary performance sensitivity. The present investigation is concerned with the solid hydrogen cryogen subsystem which provides the instrument temperature needed. Attention is given to the studies which led to the selection of solid hydrogen as cooling agent, the baseline cooler system, aspects of baseline performance sensitivity, and nominal cooler operations.

On-line solid-phase microextraction of triclosan, bisphenol A, chlorophenols, and selected pharmaceuticals in environmental water samples by high-performance liquid chromatography-ultraviolet detection.

PubMed

Kim, Dalho; Han, Jungho; Choi, Yongwook

2013-01-01

A method using on-line solid-phase microextraction (SPME) on a carbowax-templated fiber followed by liquid chromatography (LC) with ultraviolet (UV) detection was developed for the determination of triclosan in environmental water samples. Along with triclosan, other selected phenolic compounds, bisphenol A, and acidic pharmaceuticals were studied. Previous SPME/LC or stir-bar sorptive extraction/LC-UV for polar analytes showed lack of sensitivity. In this study, the calculated octanol-water distribution coefficient (log D) values of the target analytes at different pH values were used to estimate polarity of the analytes. The lack of sensitivity observed in earlier studies is identified as a lack of desorption by strong polar-polar interactions between analyte and solid-phase. Calculated log D values were useful to understand or predict the interaction between analyte and solid phase. Under the optimized conditions, the method detection limit of selected analytes by using on-line SPME-LC-UV method ranged from 5 to 33 ng L(-1), except for very polar 3-chlorophenol and 2,4-dichlorophenol which was obscured in wastewater samples by an interfering substance. This level of detection represented a remarkable improvement over the conventional existing methods. The on-line SPME-LC-UV method, which did not require derivatization of analytes, was applied to the determination of TCS including phenolic compounds and acidic pharmaceuticals in tap water and river water and municipal wastewater samples.

Study of a solid hydrogen cooler for spacecraft instruments and sensors

NASA Astrophysics Data System (ADS)

Sherman, A.

1980-08-01

The results of tests and studies to investigate the utilization of solid hydrogen for cooling of spacecraft instruments and sensors are presented. The results are presented in two sections; the first describing the tests in which an existing single stage solid cooler was filled and tested with solid hydrogen and the second which describes the analysis and design of a catalytic converter which will be tested in the vent line of the cooler.

Study of a solid hydrogen cooler for spacecraft instruments and sensors

NASA Technical Reports Server (NTRS)

Sherman, A.

1980-01-01

The results of tests and studies to investigate the utilization of solid hydrogen for cooling of spacecraft instruments and sensors are presented. The results are presented in two sections; the first describing the tests in which an existing single stage solid cooler was filled and tested with solid hydrogen and the second which describes the analysis and design of a catalytic converter which will be tested in the vent line of the cooler.

Analytical close-form solutions to the elastic fields of solids with dislocations and surface stress

NASA Astrophysics Data System (ADS)

Ye, Wei; Paliwal, Bhasker; Ougazzaden, Abdallah; Cherkaoui, Mohammed

2013-07-01

The concept of eigenstrain is adopted to derive a general analytical framework to solve the elastic field for 3D anisotropic solids with general defects by considering the surface stress. The formulation shows the elastic constants and geometrical features of the surface play an important role in determining the elastic fields of the solid. As an application, the analytical close-form solutions to the stress fields of an infinite isotropic circular nanowire are obtained. The stress fields are compared with the classical solutions and those of complex variable method. The stress fields from this work demonstrate the impact from the surface stress when the size of the nanowire shrinks but becomes negligible in macroscopic scale. Compared with the power series solutions of complex variable method, the analytical solutions in this work provide a better platform and they are more flexible in various applications. More importantly, the proposed analytical framework profoundly improves the studies of general 3D anisotropic materials with surface effects.

Assessment of analytical techniques for predicting solid propellant exhaust plumes

NASA Technical Reports Server (NTRS)

Tevepaugh, J. A.; Smith, S. D.; Penny, M. M.

1977-01-01

The calculation of solid propellant exhaust plume flow fields is addressed. Two major areas covered are: (1) the applicability of empirical data currently available to define particle drag coefficients, heat transfer coefficients, mean particle size and particle size distributions, and (2) thermochemical modeling of the gaseous phase of the flow field. Comparisons of experimentally measured and analytically predicted data are made. The experimental data were obtained for subscale solid propellant motors with aluminum loadings of 2, 10 and 15%. Analytical predictions were made using a fully coupled two-phase numerical solution. Data comparisons will be presented for radial distributions at plume axial stations of 5, 12, 16 and 20 diameters.

Detection of low-level PTFE contamination: An application of solid-state NMR to structure elucidation in the pharmaceutical industry.

PubMed

Pham, Tran N; Day, Caroline J; Edwards, Andrew J; Wood, Helen R; Lynch, Ian R; Watson, Simon A; Bretonnet, Anne-Sophie Z; Vogt, Frederick G

2011-01-25

We report a novel use of solid-state ¹⁹F nuclear magnetic resonance to detect and quantify polytetrafluoroethylene contamination from laboratory equipment, which due to low quantity (up to 1% w/w) and insolubility remained undetected by standard analytical techniques. Solid-state ¹⁹F NMR is shown to be highly sensitive to such fluoropolymers (detection limit 0.02% w/w), and is demonstrated as a useful analytical tool for structure elucidation of unknown solid materials. Copyright © 2010 Elsevier B.V. All rights reserved.

Results of the First Mars Organic Molecule Analyzer (MOMA) GC-MS Coupling

NASA Astrophysics Data System (ADS)

Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Danell, Ryan; Grand, Noel; Van Amerom, Friso; Glavin, Daniel; Freissinet, Caroline; Humeau, Olivier; Coll, Patrice; Arevalo, Ricardo; Stalport, Fabien; Brinckerhoff, William; Steininger, Harald; Goesmann, Fred; Mahaffy, Paul; Raulin, Francois

2014-11-01

The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars rover will be a key analytical tool in providing chemical (molecular) information from the solid samples collected by the rover, with a particular focus on the char-acterization of the organic content. The core of the MOMA instrument is a gas chromatograph coupled with a mass spectrometer (GC-MS) which provides the unique capability to characterize a broad range of compounds, including both of volatile and non-volatile species. Samples will be crushed and deposited into sample cups seated in a rotating carousel. Soil samples will be analyzed either by UV laser desorption / ionization (LDI) or pyrolysis gas chromatography ion trap mass spectrometry (pyr-GC-ITMS).The French GC brassboard was coupled to the US ion trap mass spectrometer brassboard in a flight-like con-figuration for several coupling campains. The MOMA GC setup is based on the SAM heritage design with a He reservoir and 4 separate analytical modules including traps, columns and Thermal Conductivity Detectors. Solid samples are sealed and heated in this setup using a manual tapping station, designed and built at MPS in Germany, for GC-MS analysis. The gaseous species eluting from the GC are then ionized by an electron impact ionization source in the MS chamber and analyzed by the linear ion trap mass spectrometer. Volatile and non-volatile compounds were injected in the MOMA instrumental suite. Both of these compounds classes were detected by the TCD and by the MS. MS signal (total ion current) and single mass spectra by comparison with the NIST library, gave us an unambiguous confirmation of these identifications. The mass spectra arise from an average of 10 mass spectra averaged around a given time point in the total ion chromatogram.Based on commercial instrument, the MOMA requirement for sensitivity in the GC-MS mode for organic molecules is 1 pmol. In this test, sensitivity was determined for the GC TCD and MS response to a dilution series containing isopropanol, hexane and benzene deposited onto silica beads in the MOMA oven. Generally, the MS was found to be 5 to10 times more sensitive than the GC TCD for hexane and benzene respectively.

Vibration characteristics of 1/8-scale dynamic models of the space-shuttle solid-rocket boosters

NASA Technical Reports Server (NTRS)

Leadbetter, S. A.; Stephens, W.; Sewall, J. L.; Majka, J. W.; Barret, J. R.

1976-01-01

Vibration tests and analyses of six 1/8 scale models of the space shuttle solid rocket boosters are reported. Natural vibration frequencies and mode shapes were obtained for these aluminum shell models having internal solid fuel configurations corresponding to launch, midburn (maximum dynamic pressure), and near endburn (burnout) flight conditions. Test results for longitudinal, torsional, bending, and shell vibration frequencies are compared with analytical predictions derived from thin shell theory and from finite element plate and beam theory. The lowest analytical longitudinal, torsional, bending, and shell vibration frequencies were within + or - 10 percent of experimental values. The effects of damping and asymmetric end skirts on natural vibration frequency were also considered. The analytical frequencies of an idealized full scale space shuttle solid rocket boosted structure are computed with and without internal pressure and are compared with the 1/8 scale model results.

A New Model for Temperature Jump at a Fluid-Solid Interface

PubMed Central

Shu, Jian-Jun; Teo, Ji Bin Melvin; Chan, Weng Kong

2016-01-01

The problem presented involves the development of a new analytical model for the general fluid-solid temperature jump. To the best of our knowledge, there are no analytical models that provide the accurate predictions of the temperature jump for both gas and liquid systems. In this paper, a unified model for the fluid-solid temperature jump has been developed based on our adsorption model of the interfacial interactions. Results obtained from this model are validated with available results from the literature. PMID:27764230

Comparison of methods for determination of total oil sands-derived naphthenic acids in water samples.

PubMed

Hughes, Sarah A; Huang, Rongfu; Mahaffey, Ashley; Chelme-Ayala, Pamela; Klamerth, Nikolaus; Meshref, Mohamed N A; Ibrahim, Mohamed D; Brown, Christine; Peru, Kerry M; Headley, John V; Gamal El-Din, Mohamed

2017-11-01

There are several established methods for the determination of naphthenic acids (NAs) in waters associated with oil sands mining operations. Due to their highly complex nature, measured concentration and composition of NAs vary depending on the method used. This study compared different common sample preparation techniques, analytical instrument methods, and analytical standards to measure NAs in groundwater and process water samples collected from an active oil sands operation. In general, the high- and ultrahigh-resolution methods, namely high performance liquid chromatography time-of-flight mass spectrometry (UPLC-TOF-MS) and Orbitrap mass spectrometry (Orbitrap-MS), were within an order of magnitude of the Fourier transform infrared spectroscopy (FTIR) methods. The gas chromatography mass spectrometry (GC-MS) methods consistently had the highest NA concentrations and greatest standard error. Total NAs concentration was not statistically different between sample preparation of solid phase extraction and liquid-liquid extraction. Calibration standards influenced quantitation results. This work provided a comprehensive understanding of the inherent differences in the various techniques available to measure NAs and hence the potential differences in measured amounts of NAs in samples. Results from this study will contribute to the analytical method standardization for NA analysis in oil sands related water samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

MERCURY MEASUREMENTS USING DIRECT-ANALYZER ...

EPA Pesticide Factsheets

Under EPA's Water Quality Research Program, exposure studies are needed to determine how well control strategies and guidance are working. Consequently, reliable and convenient techniques that minimize waste production are of special interest. While traditional methods for determining mercury in solid samples involve the use of aggressive chemicals to dissolve the matrix and the use of other chemicals to properly reduce the mercury to the volatile elemental form, pyrolysis-based analyzers can be used by directly weighing the solid in a sampling boat and initiating the instrumental analysis for total mercury. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-soluble pharmaceuticals in source waters at levels that could be environmentally significant (at con

Development of Processing Techniques for Advanced Thermal Protection Materials

NASA Technical Reports Server (NTRS)

Selvaduray, Guna; Cox, Michael; Srinivasan, Vijayakumar

1997-01-01

Thermal Protection Materials Branch (TPMB) has been involved in various research programs to improve the properties and structural integrity of the existing aerospace high temperature materials. Specimens from various research programs were brought into the analytical laboratory for the purpose of obtaining and refining the material characterization. The analytical laboratory in TPMB has many different instruments which were utilized to determine the physical and chemical characteristics of materials. Some of the instruments that were utilized by the SJSU students are: Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDX), X-ray Diffraction Spectrometer (XRD), Fourier Transform-Infrared Spectroscopy (FTIR), Ultra Violet Spectroscopy/Visible Spectroscopy (UV/VIS), Particle Size Analyzer (PSA), and Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). The above mentioned analytical instruments were utilized in the material characterization process of the specimens from research programs such as: aerogel ceramics (I) and (II), X-33 Blankets, ARC-Jet specimens, QUICFIX specimens and gas permeability of lightweight ceramic ablators. In addition to analytical instruments in the analytical laboratory at TPMB, there are several on-going experiments. One particular experiment allows the measurement of permeability of ceramic ablators. From these measurements, physical characteristics of the ceramic ablators can be derived.

Modern Instrumental Methods in Forensic Toxicology*

PubMed Central

Smith, Michael L.; Vorce, Shawn P.; Holler, Justin M.; Shimomura, Eric; Magluilo, Joe; Jacobs, Aaron J.; Huestis, Marilyn A.

2009-01-01

This article reviews modern analytical instrumentation in forensic toxicology for identification and quantification of drugs and toxins in biological fluids and tissues. A brief description of the theory and inherent strengths and limitations of each methodology is included. The focus is on new technologies that address current analytical limitations. A goal of this review is to encourage innovations to improve our technological capabilities and to encourage use of these analytical techniques in forensic toxicology practice. PMID:17579968

Carbon Nanotube Fiber Ionization Mass Spectrometry: A Fundamental Study of a Multi-Walled Carbon Nanotube Functionalized Corona Discharge Pin for Polycyclic Aromatic Hydrocarbons Analysis.

PubMed

Nahan, Keaton S; Alvarez, Noe; Shanov, Vesselin; Vonderheide, Anne

2017-11-01

Mass spectrometry continues to tackle many complicated tasks, and ongoing research seeks to simplify its instrumentation as well as sampling. The desorption electrospray ionization (DESI) source was the first ambient ionization source to function without extensive gas requirements and chromatography. Electrospray techniques generally have low efficiency for ionization of nonpolar analytes and some researchers have resorted to methods such as direct analysis in real time (DART) or desorption atmospheric pressure chemical ionization (DAPCI) for their analysis. In this work, a carbon nanotube fiber ionization (nanoCFI) source was developed and was found to be capable of solid phase microextraction (SPME) of nonpolar analytes as well as ionization and sampling similar to that of direct probe atmospheric pressure chemical ionization (DP-APCI). Conductivity and adsorption were maintained by utilizing a corona pin functionalized with a multi-walled carbon nanotube (MWCNT) thread. Quantitative work with the nanoCFI source with a designed corona discharge pin insert demonstrated linearity up to 0.97 (R 2 ) of three target PAHs with phenanthrene internal standard. Graphical Abstract ᅟ.

A comparative study between different alternatives to prepare gaseous standards for calibrating UV-Ion Mobility Spectrometers.

PubMed

Criado-García, Laura; Garrido-Delgado, Rocío; Arce, Lourdes; Valcárcel, Miguel

2013-07-15

An UV-Ion Mobility Spectrometer is a simple, rapid, inexpensive instrument widely used in environmental analysis among other fields. The advantageous features of its underlying technology can be of great help towards developing reliable, economical methods for determining gaseous compounds from gaseous, liquid and solid samples. Developing an effective method using UV-Ion Mobility Spectrometry (UV-IMS) to determine volatile analytes entails using appropriate gaseous standards for calibrating the spectrometer. In this work, two home-made sample introduction systems (SISs) and a commercial gas generator were used to obtain such gaseous standards. The first home-made SIS used was a static head-space to measure compounds present in liquid samples and the other home-made system was an exponential dilution set-up to measure compounds present in gaseous samples. Gaseous compounds generated by each method were determined on-line by UV-IMS. Target analytes chosen for this comparative study were ethanol, acetone, benzene, toluene, ethylbenzene and xylene isomers. The different alternatives were acceptable in terms of sensitivity, precision and selectivity. Copyright © 2013 Elsevier B.V. All rights reserved.

Three-phase double-arc plasma for spectrochemical analysis of environmental samples.

PubMed

Mohamed, M M; Ghatass, Z F; Shalaby, E A; Kotb, M M; El-Raey, M

2000-12-01

A new instrument, which uses a three-phase current to support a double-arc argon plasma torch for evaporation, atomization and excitation of solid or powder samples, is described. The sampling arc is ignited between the first and second electrode while the excitation arc is ignited between the second and third electrode. Aerosol generated from the sample (first electrode) is swept by argon gas, through a hole in the second electrode (carbon tubing electrode), into the excitation plasma. A tangential stream of argon gas is introduced through an inlet orifice as a coolant gas for the second electrode. This gas stream forces the excitation arc discharge to rotate reproducibly around the electrode surface. Discharge rotation increases the stability of the excitation plasma. Spectroscopic measurements are made directly in the current-carrying region of the excitation arc. An evaluation of each parameter influencing the device performance was performed. Analytical calibration curves were obtained for Fe, Al, K, and Pb. Finally, the present technique was applied for the analysis of environmental samples. The present method appears to have significant, low cost analytical utility for environmental measurements.

Carbon Nanotube Fiber Ionization Mass Spectrometry: A Fundamental Study of a Multi-Walled Carbon Nanotube Functionalized Corona Discharge Pin for Polycyclic Aromatic Hydrocarbons Analysis

NASA Astrophysics Data System (ADS)

Nahan, Keaton S.; Alvarez, Noe; Shanov, Vesselin; Vonderheide, Anne

2017-09-01

Mass spectrometry continues to tackle many complicated tasks, and ongoing research seeks to simplify its instrumentation as well as sampling. The desorption electrospray ionization (DESI) source was the first ambient ionization source to function without extensive gas requirements and chromatography. Electrospray techniques generally have low efficiency for ionization of nonpolar analytes and some researchers have resorted to methods such as direct analysis in real time (DART) or desorption atmospheric pressure chemical ionization (DAPCI) for their analysis. In this work, a carbon nanotube fiber ionization (nanoCFI) source was developed and was found to be capable of solid phase microextraction (SPME) of nonpolar analytes as well as ionization and sampling similar to that of direct probe atmospheric pressure chemical ionization (DP-APCI). Conductivity and adsorption were maintained by utilizing a corona pin functionalized with a multi-walled carbon nanotube (MWCNT) thread. Quantitative work with the nanoCFI source with a designed corona discharge pin insert demonstrated linearity up to 0.97 (R2) of three target PAHs with phenanthrene internal standard. [Figure not available: see fulltext.

Application of non-traditional stable isotopes in analytical ecogeochemistry assessed by MC ICP-MS--A critical review.

PubMed

Irrgeher, Johanna; Prohaska, Thomas

2016-01-01

Analytical ecogeochemistry is an evolving scientific field dedicated to the development of analytical methods and tools and their application to ecological questions. Traditional stable isotopic systems have been widely explored and have undergone continuous development during the last century. The variations of the isotopic composition of light elements (H, O, N, C, and S) have provided the foundation of stable isotope analysis followed by the analysis of traditional geochemical isotope tracers (e.g., Pb, Sr, Nd, Hf). Questions in a considerable diversity of scientific fields have been addressed, many of which can be assigned to the field of ecogeochemistry. Over the past 15 years, other stable isotopes (e.g., Li, Zn, Cu, Cl) have emerged gradually as novel tools for the investigation of scientific topics that arise in ecosystem research and have enabled novel discoveries and explorations. These systems are often referred to as non-traditional isotopes. The small isotopic differences of interest that are increasingly being addressed for a growing number of isotopic systems represent a challenge to the analytical scientist and push the limits of today's instruments constantly. This underlines the importance of a metrologically sound concept of analytical protocols and procedures and a solid foundation of data processing strategies and uncertainty considerations before these small isotopic variations can be interpreted in the context of applied ecosystem research. This review focuses on the development of isotope research in ecogeochemistry, the requirements for successful detection of small isotopic shifts, and highlights the most recent and innovative applications in the field.

Assessing the properties of internal standards for quantitative matrix-assisted laser desorption/ionization mass spectrometry of small molecules.

PubMed

Sleno, Lekha; Volmer, Dietrich A

2006-01-01

Growing interest in the ability to conduct quantitative assays for small molecules by matrix-assisted laser desorption/ionization (MALDI) has been the driving force for several recent studies. This present work includes the investigation of internal standards for these analyses using a high-repetition rate MALDI triple quadrupole instrument. Certain physicochemical properties are assessed for predicting possible matches for internal standards for different small molecules. The importance of similar molecular weight of an internal standard to its analyte is seen through experiments with a series of acylcarnitines, having a fixed charge site and growing alkyl chain length. Both acetyl- and hexanoyl-carnitine were systematically assessed with several other acylcarnitine compounds as internal standards. The results clearly demonstrate that closely matched molecular weights between analyte and internal standard are essential for acceptable quantitation results. Using alpha-cyano-4-hydroxycinnamic acid as the organic matrix, the similarities between analyte and internal standard remain the most important parameter and not necessarily their even distribution within the solid sample spot. Several 4-quinolone antibiotics as well as a diverse group of pharmaceutical drugs were tested as internal standards for the 4-quinolone, ciprofloxacin. Quantitative results were shown using the solution-phase properties, log D and pKa, of these molecules. Their distribution coefficients, log D, are demonstrated as a fundamental parameter for similar crystallization patterns of analyte and internal standard. In the end, it was also possible to quantify ciprofloxacin using a drug from a different compound class, namely quinidine, having a similar log D value as the analyte. Copyright 2006 John Wiley & Sons, Ltd.

Evaluation of performance of three different hybrid mesoporous solids based on silica for preconcentration purposes in analytical chemistry: From the study of sorption features to the determination of elements of group IB.

PubMed

Kim, Manuela Leticia; Tudino, Mabel Beatríz

2010-08-15

Several studies involving the physicochemical interaction of three silica based hybrid mesoporous materials with metal ions of the group IB have been performed in order to employ them for preconcentration purposes in the determination of traces of Cu(II), Ag(I) and Au(III). The three solids were obtained from mesoporous silica functionalized with 3-aminopropyl (APS), 3-mercaptopropyl (MPS) and N-[2-aminoethyl]-3-aminopropyl (NN) groups, respectively. Adsorption capacities for Au, Cu and Ag were calculated using Langmuir's isotherm model and then, the optimal values for the retention of each element onto each one of the solids were found. Physicochemical data obtained under thermodynamic equilibrium and under kinetic conditions - imposed by flow through experiments - allowed the design of simple analytical methodologies where the solids were employed as fillings of microcolumns held in continuous systems coupled on-line to an atomic absorption spectrometry. In order to control the interaction between the filling and the analyte at short times (flow through conditions) and thus, its effect on the analytical signal and the presence of interferences, the initial adsorption velocities were calculated using the pseudo second order model. All these experiments allowed the comparison of the solids in terms of their analytical behaviour at the moment of facing the determination of the three elements. Under optimized conditions mainly given by the features of the filling, the analytical methodologies developed in this work showed excellent performances with limits of detection of 0.14, 0.02 and 0.025 microg L(-1) and RSD % values of 3.4, 2.7 and 3.1 for Au, Cu and Ag, respectively. A full discussion of the main findings on the interaction metal ions/fillings will be provided. The analytical results for the determination of the three metals will be also presented. Copyright 2010 Elsevier B.V. All rights reserved.

Devitrification of amorphous celecoxib.

PubMed

Gupta, Piyush; Bansal, Arvind K

2005-09-30

The purpose of this research was to analyze the devitrification of amorphous celecoxib (CEL) in the presence of different stressors (temperature, pressure, and/or humidity) encountered during processing of solid dosage forms. Amorphous CEL was prepared in situ in the analytical instruments, as well as in laboratory, by quench-cooling of melt process, and analyzed by dynamic mechanical thermal analysis, differential scanning calorimetry, microscopy, and Fourier-transform infrared spectroscopy. Amorphous CEL prepared in situ in the analytical instruments was resistant to crystallization under the influence of temperature and/or pressure, because of its protection from the external environment during preparation. These samples exhibited structural relaxation during annealing at 25 degrees C/0% relative humidity (RH) for 16 hours. Generation of amorphous CEL in the laboratory resulted in partially crystalline samples, because of exposure to environmental temperature and humidity, resulting in incomplete vitrification. Subjection to thermal stress favored crystallization of amorphous CEL into metastable polymorphic forms, which were not obtained by solvent recrystallization approach. Temperature and humidity were identified as the major factors promoting devitrification of amorphous CEL, leading to loss of solubility advantage. Exposure to International Conference on Harmonization-specified accelerated stability storage conditions (40 degrees C/75% RH) resulted in complete devitrification of amorphous CEL within 15 days. The phase-transformation process of amorphous CEL along the temperature scale was examined visually, as well as spectrally. This propensity for devitrification of amorphous CEL seemed to depend on the strength of differential molecular interactions between the amorphous and crystalline form.

The rise of environmental analytical chemistry as an interdisciplinary activity.

PubMed

Brown, Richard

2009-07-01

Modern scientific endeavour is increasingly delivered within an interdisciplinary framework. Analytical environmental chemistry is a long-standing example of an interdisciplinary approach to scientific research where value is added by the close cooperation of different disciplines. This editorial piece discusses the rise of environmental analytical chemistry as an interdisciplinary activity and outlines the scope of the Analytical Chemistry and the Environmental Chemistry domains of TheScientificWorldJOURNAL (TSWJ), and the appropriateness of TSWJ's domain format in covering interdisciplinary research. All contributions of new data, methods, case studies, and instrumentation, or new interpretations and developments of existing data, case studies, methods, and instrumentation, relating to analytical and/or environmental chemistry, to the Analytical and Environmental Chemistry domains, are welcome and will be considered equally.

Dynamic and label-free high-throughput detection of biomolecular interactions based on phase-shift interferometry

NASA Astrophysics Data System (ADS)

Li, Qiang; Huang, Guoliang; Gan, Wupeng; Chen, Shengyi

2009-08-01

Biomolecular interactions can be detected by many established technologies such as fluorescence imaging, surface plasmon resonance (SPR)[1-4], interferometry and radioactive labeling of the analyte. In this study, we have designed and constructed a label-free, real-time sensing platform and its operating imaging instrument that detects interactions using optical phase differences from the accumulation of biological material on solid substrates. This system allows us to monitor biomolecular interactions in real time and quantify concentration changes during micro-mixing processes by measuring the changes of the optical path length (OPD). This simple interferometric technology monitors the optical phase difference resulting from accumulated biomolecular mass. A label-free protein chip that forms a 4×4 probe array was designed and fabricated using a commercial microarray robot spotter on solid substrates. Two positive control probe lines of BSA (Bovine Serum Albumin) and two experimental human IgG and goat IgG was used. The binding of multiple protein targets was performed and continuously detected by using this label-free and real-time sensing platform.

Computer fluid dynamics (CFD) study of a micro annular gear pump

NASA Astrophysics Data System (ADS)

Stan, Liviu-Constantin; Cǎlimǎnescu, Ioan

2016-12-01

Micro technology makes it possible to design products simply, efficiently and sustainably and at the same time, opens up the creation of new functionalities. The field of application of the micro annular gear pumps lies in analytical instrumentation, mechanical and plant engineering, chemical and pharmaceutical process engineering as well as in new markets like fuel cells or biotechnology, organic electronics or aerospace. The purpose of this paper is to investigate by using the powerful ANSYS 16 CFX module the hydrodynamic behavior of an 8/9 teeth annular gear pump. The solving of solids evolving inside fluids was very cumbersome until the advent of the Ansys immersed solid technology. By deploying this technology for very special topics like the CFD analysis of Micro annular gear pumps, credible and reliable results may be pulled leading thus the way for more in depth studies like geometrical a functional optimization of the existing devices. This paper is a valuable guide for the professionals working in the design field of micro pumps handing them a new and powerful design tool.

Solid-Phase Extraction Coupled to a Paper-Based Technique for Trace Copper Detection in Drinking Water.

PubMed

Quinn, Casey W; Cate, David M; Miller-Lionberg, Daniel D; Reilly, Thomas; Volckens, John; Henry, Charles S

2018-03-20

Metal contamination of natural and drinking water systems poses hazards to public and environmental health. Quantifying metal concentrations in water typically requires sample collection in the field followed by expensive laboratory analysis that can take days to weeks to obtain results. The objective of this work was to develop a low-cost, field-deployable method to quantify trace levels of copper in drinking water by coupling solid-phase extraction/preconcentration with a microfluidic paper-based analytical device. This method has the advantages of being hand-powered (instrument-free) and using a simple "read by eye" quantification motif (based on color distance). Tap water samples collected across Fort Collins, CO, were tested with this method and validated against ICP-MS. We demonstrate the ability to quantify the copper content of tap water within 30% of a reference technique at levels ranging from 20 to 500 000 ppb. The application of this technology, which should be sufficient as a rapid screening tool, can lead to faster, more cost-effective detection of soluble metals in water systems.

A new model for fluid velocity slip on a solid surface.

PubMed

Shu, Jian-Jun; Teo, Ji Bin Melvin; Chan, Weng Kong

2016-10-12

A general adsorption model is developed to describe the interactions between near-wall fluid molecules and solid surfaces. This model serves as a framework for the theoretical modelling of boundary slip phenomena. Based on this adsorption model, a new general model for the slip velocity of fluids on solid surfaces is introduced. The slip boundary condition at a fluid-solid interface has hitherto been considered separately for gases and liquids. In this paper, we show that the slip velocity in both gases and liquids may originate from dynamical adsorption processes at the interface. A unified analytical model that is valid for both gas-solid and liquid-solid slip boundary conditions is proposed based on surface science theory. The corroboration with the experimental data extracted from the literature shows that the proposed model provides an improved prediction compared to existing analytical models for gases at higher shear rates and close agreement for liquid-solid interfaces in general.

Analytical methods for dating modern writing instrument inks on paper.

PubMed

Ezcurra, Magdalena; Góngora, Juan M G; Maguregui, Itxaso; Alonso, Rosa

2010-04-15

This work reviews the different analytical methods that have been proposed in the field of forensic dating of inks from different modern writing instruments. The reported works have been classified according to the writing instrument studied and the ink component analyzed in relation to aging. The study, done chronologically, shows the advances experienced in the ink dating field in the last decades. Copyright 2009 Elsevier Ireland Ltd. All rights reserved.

JPRS Report, Science & Technology, USSR: Engineering & Equipment

DTIC Science & Technology

1987-08-05

working successfully in the " Veda " PO and at the analytical instruments plant. Characteristically, it was these very enterprises which were on top in...the 1985 review: the analytical instruments plant collective came in first, the " Veda " PO collective came in second, and the "Elektronmash" PO

Application of the correlation constrained multivariate curve resolution alternating least-squares method for analyte quantitation in the presence of unexpected interferences using first-order instrumental data.

PubMed

Goicoechea, Héctor C; Olivieri, Alejandro C; Tauler, Romà

2010-03-01

Correlation constrained multivariate curve resolution-alternating least-squares is shown to be a feasible method for processing first-order instrumental data and achieve analyte quantitation in the presence of unexpected interferences. Both for simulated and experimental data sets, the proposed method could correctly retrieve the analyte and interference spectral profiles and perform accurate estimations of analyte concentrations in test samples. Since no information concerning the interferences was present in calibration samples, the proposed multivariate calibration approach including the correlation constraint facilitates the achievement of the so-called second-order advantage for the analyte of interest, which is known to be present for more complex higher-order richer instrumental data. The proposed method is tested using a simulated data set and two experimental data systems, one for the determination of ascorbic acid in powder juices using UV-visible absorption spectral data, and another for the determination of tetracycline in serum samples using fluorescence emission spectroscopy.

Raman Hyperspectral Imaging of Microfossils: Potential Pitfalls

PubMed Central

Olcott Marshall, Alison

2013-01-01

Abstract Initially, Raman spectroscopy was a specialized technique used by vibrational spectroscopists; however, due to rapid advancements in instrumentation and imaging techniques over the last few decades, Raman spectrometers are widely available at many institutions, allowing Raman spectroscopy to become a widespread analytical tool in mineralogy and other geological sciences. Hyperspectral imaging, in particular, has become popular due to the fact that Raman spectroscopy can quickly delineate crystallographic and compositional differences in 2-D and 3-D at the micron scale. Although this rapid growth of applications to the Earth sciences has provided great insight across the geological sciences, the ease of application as the instruments become increasingly automated combined with nonspecialists using this techique has resulted in the propagation of errors and misunderstandings throughout the field. For example, the literature now includes misassigned vibration modes, inappropriate spectral processing techniques, confocal depth of laser penetration incorrectly estimated into opaque crystalline solids, and a misconstrued understanding of the anisotropic nature of sp2 carbons. Key Words: Raman spectroscopy—Raman imaging—Confocal Raman spectroscopy—Disordered sp2 carbons—Hematite—Microfossils. Astrobiology 13, 920–931. PMID:24088070

Subcritical water extractor for Mars analog soil analysis.

PubMed

Amashukeli, Xenia; Grunthaner, Frank J; Patrick, Steven B; Yung, Pun To

2008-06-01

Abstract Technologies that enable rapid and efficient extraction of biomarker compounds from various solid matrices are a critical requirement for the successful implementation of in situ chemical analysis of the martian regolith. Here, we describe a portable subcritical water extractor that mimics multiple organic solvent polarities by tuning the dielectric constant of liquid water through adjustment of temperature and pressure. Soil samples, collected from the Yungay region of the Atacama Desert (martian regolith analogue) in the summer of 2005, were used to test the instrument's performance. The total organic carbon was extracted from the samples at concentrations of 0.2-55.4 parts per million. The extraction data were compared to the total organic carbon content in the bulk soil, which was determined via a standard analytical procedure. The instrument's performance was examined over the temperature range of 25-250 degrees C at a fixed pressure of 20.7 MPa. Under these conditions, water remains in a subcritical fluid state with a dielectric constant varying between approximately 80 (at 25 degrees C) and approximately 30 (at 250 degrees C).

Use of a novel saline/bipolar radiofrequency energy instrument as an adjunct for arresting ongoing solid organ surface and laceration bleeding in critically injured patients.

PubMed

Ball, Chad G; Campbell, Andre; Grondin, Sean C; Dixon, Elijah; DuBose, Joseph; McBeth, Paul B; Lall, Rohan

2016-09-01

Solid organ (liver, spleen and kidney) haemorrhage is often life threatening and can be difficult to stop in critically ill patients. Traditional techniques for arresting this ongoing bleeding include coagulation by high voltage cautery (Bovie), topical haemostatic application, and the delivery of ignited argon gas. The goal of this study was to evaluate the efficacy of a new energy device for arresting persistent solid organ haemorrhage. A novel instrument utilizing bipolar radiofrequency (RF) energy which acts to ignite/boil dripping saline from a simple hand piece was employed to arrest ongoing bleeding from solid organ injuries at 2 high volume, level 1 trauma centres. This instrument is extrapolated from experience within elective hepatic resections. Standard statistics were employed (p<0.05=significant). From January 2013 to January 2015, 36 severely injured patients (mean injury severity score=31; blunt mechanisms=32/36 (89%)) underwent use of this new saline/RF energy instrument to arrest ongoing haemorrhage from the liver (29), spleen (5) and kidney (2). Of these patients, 25 received instrument use during an initial laparotomy, while 11 patients underwent use following removal of sponges during a return laparotomy after an initial damage control procedure. Success in arresting ongoing haemorrhage was 97% (35/36) in these highly selected cases. The surgeons reported an 'ease of use' score of 4.9 out of 5. No postoperative complications (including delayed haemorrhage) were noted as a direct result of the energy instrument. This simple saline/RF energy instrument has the potential to arrest ongoing solid organ surface/capsular bleeding, as well as moderate haemorrhage associated with deep lacerations. Copyright © 2016 Elsevier Ltd. All rights reserved.

A critical evaluation of liquid chromatography with hybrid linear ion trap-Orbitrap mass spectrometry for the determination of acidic contaminants in wastewater effluents.

PubMed

Cahill, Michael G; Dineen, Brian A; Stack, Mary A; James, Kevin J

2012-12-28

Acidic pesticide and pharmaceutical contaminants were pre-concentrated and extracted from wastewater samples (500 mL) using solid-phase extraction. Analyte recoveries were 79-96%, with % RSD values in the range, 1.7-7.4%. Analyte identification and quantification were carried out using liquid chromatography-mass spectrometry (LC-MS) with hybrid linear ion trap (LIT) Orbitrap instrumentation. Using a resolution setting of 30,000 FWHM, full-scan MS analysis was performed using heated electrospray ionization (HESI) in negative mode. The high mass resolution capabilities of the Orbitrap MS were exploited for the determination of trace contaminants allowing facile discrimination between analytes and matrix. The dependant scan functions of the Orbitrap MS using higher collisional dissociation (HCD) and LIT MS were evaluated for the confirmation of analytes at trace concentration levels. Mass accuracy for target contaminants using this method was less than 2 ppm. The limits of quantitation (LOQs) were in the range, 2.1-27 ng/L. The inter-day accuracy and precision were measured over a five-day period at two concentrations. The % relative errors were in the range, 0.30-7.7%, and the % RSD values were in the range, 1.5-5.5%. Using this method, 2,4-D, mecoprop, ibuprofen, naproxene and gemfibrozil were identified in several wastewater treatment plants in Ireland. Copyright © 2012 Elsevier B.V. All rights reserved.

Selected analytical challenges in the determination of pharmaceuticals in drinking/marine waters and soil/sediment samples.

PubMed

Białk-Bielińska, Anna; Kumirska, Jolanta; Borecka, Marta; Caban, Magda; Paszkiewicz, Monika; Pazdro, Ksenia; Stepnowski, Piotr

2016-03-20

Recent developments and improvements in advanced instruments and analytical methodologies have made the detection of pharmaceuticals at low concentration levels in different environmental matrices possible. As a result of these advances, over the last 15 years residues of these compounds and their metabolites have been detected in different environmental compartments and pharmaceuticals have now become recognized as so-called 'emerging' contaminants. To date, a lot of papers have been published presenting the development of analytical methodologies for the determination of pharmaceuticals in aqueous and solid environmental samples. Many papers have also been published on the application of the new methodologies, mainly to the assessment of the environmental fate of pharmaceuticals. Although impressive improvements have undoubtedly been made, in order to fully understand the behavior of these chemicals in the environment, there are still numerous methodological challenges to be overcome. The aim of this paper therefore, is to present a review of selected recent improvements and challenges in the determination of pharmaceuticals in environmental samples. Special attention has been paid to the strategies used and the current challenges (also in terms of Green Analytical Chemistry) that exist in the analysis of these chemicals in soils, marine environments and drinking waters. There is a particular focus on the applicability of modern sorbents such as carbon nanotubes (CNTs) in sample preparation techniques, to overcome some of the problems that exist in the analysis of pharmaceuticals in different environmental samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

NASA Astrophysics Data System (ADS)

Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

2011-07-01

A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL - 1 , respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

Using chromatography – desorption method of manufacturing gas mixtures for analytical instruments calibration

NASA Astrophysics Data System (ADS)

Platonov, I. A.; Kolesnichenko, I. N.; Lange, P. K.

2018-05-01

In this paper, the chromatography desorption method of obtaining gas mixtures of known compositions stable for a time sufficient to calibrate analytical instruments is considered. The comparative analysis results of the preparation accuracy of gas mixtures with volatile organic compounds using diffusion, polyabarbotage and chromatography desorption methods are presented. It is shown that the application of chromatography desorption devices allows one to obtain gas mixtures that are stable for 10...60 hours in a dynamic condition. These gas mixtures contain volatile aliphatic and aromatic hydrocarbons with a concentration error of no more than 7%. It is shown that it is expedient to use such gas mixtures for analytical instruments calibration (chromatographs, spectrophotometers, etc.)

Headspace versus direct immersion solid phase microextraction in complex matrixes: investigation of analyte behavior in multicomponent mixtures.

PubMed

Gionfriddo, Emanuela; Souza-Silva, Érica A; Pawliszyn, Janusz

2015-08-18

This work aims to investigate the behavior of analytes in complex mixtures and matrixes with the use of solid-phase microextraction (SPME). Various factors that influence analyte uptake such as coating chemistry, extraction mode, the physicochemical properties of analytes, and matrix complexity were considered. At first, an aqueous system containing analytes bearing different hydrophobicities, molecular weights, and chemical functionalities was investigated by using commercially available liquid and solid porous coatings. The differences in the mass transfer mechanisms resulted in a more pronounced occurrence of coating saturation in headspace mode. Contrariwise, direct immersion extraction minimizes the occurrence of artifacts related to coating saturation and provides enhanced extraction of polar compounds. In addition, matrix-compatible PDMS-modified solid coatings, characterized by a new morphology that avoids coating fouling, were compared to their nonmodified analogues. The obtained results indicate that PDMS-modified coatings reduce artifacts associated with coating saturation, even in headspace mode. This factor, coupled to their matrix compatibility, make the use of direct SPME very practical as a quantification approach and the best choice for metabolomics studies where wide coverage is intended. To further understand the influence on analyte uptake on a system where additional interactions occur due to matrix components, ex vivo and in vivo sampling conditions were simulated using a starch matrix model, with the aim of mimicking plant-derived materials. Our results corroborate the fact that matrix handling can affect analyte/matrix equilibria, with consequent release of high concentrations of previously bound hydrophobic compounds, potentially leading to coating saturation. Direct immersion SPME limited the occurrence of the artifacts, which confirms the suitability of SPME for in vivo applications. These findings shed light into the implementation of in vivo SPME strategies in quantitative metabolomics studies of complex plant-based systems.

Analytical thermal model for end-pumped solid-state lasers

NASA Astrophysics Data System (ADS)

Cini, L.; Mackenzie, J. I.

2017-12-01

Fundamentally power-limited by thermal effects, the design challenge for end-pumped "bulk" solid-state lasers depends upon knowledge of the temperature gradients within the gain medium. We have developed analytical expressions that can be used to model the temperature distribution and thermal-lens power in end-pumped solid-state lasers. Enabled by the inclusion of a temperature-dependent thermal conductivity, applicable from cryogenic to elevated temperatures, typical pumping distributions are explored and the results compared with accepted models. Key insights are gained through these analytical expressions, such as the dependence of the peak temperature rise in function of the boundary thermal conductance to the heat sink. Our generalized expressions provide simple and time-efficient tools for parametric optimization of the heat distribution in the gain medium based upon the material and pumping constraints.

Data Filtering in Instrumental Analyses with Applications to Optical Spectroscopy and Chemical Imaging

ERIC Educational Resources Information Center

Vogt, Frank

2011-01-01

Most measurement techniques have some limitations imposed by a sensor's signal-to-noise ratio (SNR). Thus, in analytical chemistry, methods for enhancing the SNR are of crucial importance and can be ensured experimentally or established via pre-treatment of digitized data. In many analytical curricula, instrumental techniques are given preference…

Incorporating Students' Self-Designed, Research-Based Analytical Chemistry Projects into the Instrumentation Curriculum

ERIC Educational Resources Information Center

Gao, Ruomei

2015-01-01

In a typical chemistry instrumentation laboratory, students learn analytical techniques through a well-developed procedure. Such an approach, however, does not engage students in a creative endeavor. To foster the intrinsic motivation of students' desire to learn, improve their confidence in self-directed learning activities and enhance their…

Juicing the Juice: A Laboratory-Based Case Study for an Instrumental Analytical Chemistry Course

ERIC Educational Resources Information Center

Schaber, Peter M.; Dinan, Frank J.; St. Phillips, Michael; Larson, Renee; Pines, Harvey A.; Larkin, Judith E.

2011-01-01

A young, inexperienced Food and Drug Administration (FDA) chemist is asked to distinguish between authentic fresh orange juice and suspected reconstituted orange juice falsely labeled as fresh. In an advanced instrumental analytical chemistry application of this case, inductively coupled plasma (ICP) spectroscopy is used to distinguish between the…

Automation, consolidation, and integration in autoimmune diagnostics.

PubMed

Tozzoli, Renato; D'Aurizio, Federica; Villalta, Danilo; Bizzaro, Nicola

2015-08-01

Over the past two decades, we have witnessed an extraordinary change in autoimmune diagnostics, characterized by the progressive evolution of analytical technologies, the availability of new tests, and the explosive growth of molecular biology and proteomics. Aside from these huge improvements, organizational changes have also occurred which brought about a more modern vision of the autoimmune laboratory. The introduction of automation (for harmonization of testing, reduction of human error, reduction of handling steps, increase of productivity, decrease of turnaround time, improvement of safety), consolidation (combining different analytical technologies or strategies on one instrument or on one group of connected instruments) and integration (linking analytical instruments or group of instruments with pre- and post-analytical devices) opened a new era in immunodiagnostics. In this article, we review the most important changes that have occurred in autoimmune diagnostics and present some models related to the introduction of automation in the autoimmunology laboratory, such as automated indirect immunofluorescence and changes in the two-step strategy for detection of autoantibodies; automated monoplex immunoassays and reduction of turnaround time; and automated multiplex immunoassays for autoantibody profiling.

Providing solid angle formalism for skyshine calculations.

PubMed

Gossman, Michael S; Pahikkala, A Jussi; Rising, Mary B; McGinley, Patton H

2010-08-17

We detail, derive and correct the technical use of the solid angle variable identified in formal guidance that relates skyshine calculations to dose-equivalent rate. We further recommend it for use with all National Council on Radiation Protection and Measurements (NCRP), Institute of Physics and Engineering in Medicine (IPEM) and similar reports documented. In general, for beams of identical width which have different resulting areas, within ± 1.0 % maximum deviation the analytical pyramidal solution is 1.27 times greater than a misapplied analytical conical solution through all field sizes up to 40 × 40 cm². Therefore, we recommend determining the exact results with the analytical pyramidal solution for square beams and the analytical conical solution for circular beams.

Advancements in the safe identification of explosives using a Raman handheld instrument (ACE-ID)

NASA Astrophysics Data System (ADS)

Arnó, Josep; Frunzi, Michael; Kittredge, Marina; Sparano, Brian

2014-05-01

Raman spectroscopy is the technology of choice to identify bulk solid and liquid phase unknown samples without the need to contact the substance. Materials can be identified through transparent and semi-translucent containers such as plastic and glass. ConOps in emergency response and military field applications require the redesign of conventional laboratory units for: field portability; shock, thermal and chemical attack resistance; easy and intuitive use in restrictive gear; reduced size, weight, and power. This article introduces a new handheld instrument (ACE-IDTM) designed to take Raman technology to the next level in terms of size, safety, speed, and analytical performance. ACE-ID is ruggedized for use in severe climates and terrains. It is lightweight and can be operated with just one hand. An intuitive software interface guides users through the entire identification process, making it easy-to-use by personnel of different skill levels including military explosive ordinance disposal technicians, civilian bomb squads and hazmat teams. Through the use of embedded advanced algorithms, the instrument is capable of providing fluorescence correction and analysis of binary mixtures. Instrument calibration is performed automatically upon startup without requiring user intervention. ACE-ID incorporates an optical rastering system that diffuses the laser energy over the sample. This important innovation significantly reduces the heat induced in dark samples and the probability of ignition of susceptible explosive materials. In this article, the explosives identification performance of the instrument will be provided in addition to a quantitative evaluation of the safety improvements derived from the reduced ignition probabilities.

Applications of reversible covalent chemistry in analytical sample preparation.

PubMed

Siegel, David

2012-12-07

Reversible covalent chemistry (RCC) adds another dimension to commonly used sample preparation techniques like solid-phase extraction (SPE), solid-phase microextraction (SPME), molecular imprinted polymers (MIPs) or immuno-affinity cleanup (IAC): chemical selectivity. By selecting analytes according to their covalent reactivity, sample complexity can be reduced significantly, resulting in enhanced analytical performance for low-abundance target analytes. This review gives a comprehensive overview of the applications of RCC in analytical sample preparation. The major reactions covered include reversible boronic ester formation, thiol-disulfide exchange and reversible hydrazone formation, targeting analyte groups like diols (sugars, glycoproteins and glycopeptides, catechols), thiols (cysteinyl-proteins and cysteinyl-peptides) and carbonyls (carbonylated proteins, mycotoxins). Their applications range from low abundance proteomics to reversible protein/peptide labelling to antibody chromatography to quantitative and qualitative food analysis. In discussing the potential of RCC, a special focus is on the conditions and restrictions of the utilized reaction chemistry.

The development of an integrated assessment instrument for measuring analytical thinking and science process skills

NASA Astrophysics Data System (ADS)

Irwanto, Rohaeti, Eli; LFX, Endang Widjajanti; Suyanta

2017-05-01

This research aims to develop instrument and determine the characteristics of an integrated assessment instrument. This research uses 4-D model, which includes define, design, develop, and disseminate. The primary product is validated by expert judgment, tested it's readability by students, and assessed it's feasibility by chemistry teachers. This research involved 246 students of grade XI of four senior high schools in Yogyakarta, Indonesia. Data collection techniques include interview, questionnaire, and test. Data collection instruments include interview guideline, item validation sheet, users' response questionnaire, instrument readability questionnaire, and essay test. The results show that the integrated assessment instrument has Aiken validity value of 0.95. Item reliability was 0.99 and person reliability was 0.69. Teachers' response to the integrated assessment instrument is very good. Therefore, the integrated assessment instrument is feasible to be applied to measure the students' analytical thinking and science process skills.

Investigation of a para-ortho hydrogen reactor for application to spacecraft sensor cooling

NASA Technical Reports Server (NTRS)

Nast, T. C.

1983-01-01

The utilization of solid hydrogen in space for sensor and instrument cooling is a very efficient technique for long term cooling or for cooling at high heat rates. The solid hydrogen can provide temperatures as low as 7 to 8 K to instruments. Vapor cooling is utilized to reduce parasitic heat inputs to the 7 to 8 K stage and is effective in providing intermediate cooling for instrument components operating at higher temperatures. The use of solid hydrogen in place of helium may lead to weight reductions as large as a factor of ten and an attendent reduction in system volume. The results of an investigation of a catalytic reactor for use with a solid hydrogen cooling system is presented. Trade studies were performed on several configurations of reactor to meet the requirements of high reactor efficiency with low pressure drop. Results for the selected reactor design are presented for both liquid hydrogen systems operating at near atmospheric pressure and the solid hydrogen cooler operating as low as 1 torr.

Critical evaluation of connectivity-based point of care testing systems of glucose in a hospital environment.

PubMed

Floré, Katelijne M J; Fiers, Tom; Delanghe, Joris R

2008-01-01

In recent years a number of point of care testing (POCT) glucometers were introduced on the market. We investigated the analytical variability (lot-to-lot variation, calibration error, inter-instrument and inter-operator variability) of glucose POCT systems in a university hospital environment and compared these results with the analytical needs required for tight glucose monitoring. The reference hexokinase method was compared to different POCT systems based on glucose oxidase (blood gas instruments) or glucose dehydrogenase (handheld glucometers). Based upon daily internal quality control data, total errors were calculated for the various glucose methods and the analytical variability of the glucometers was estimated. The total error of the glucometers exceeded by far the desirable analytical specifications (based on a biological variability model). Lot-to-lot variation, inter-instrument variation and inter-operator variability contributed approximately equally to total variance. As in a hospital environment, distribution of hematocrit values is broad, converting blood glucose into plasma values using a fixed factor further increases variance. The percentage of outliers exceeded the ISO 15197 criteria in a broad glucose concentration range. Total analytical variation of handheld glucometers is larger than expected. Clinicians should be aware that the variability of glucose measurements obtained by blood gas instruments is lower than results obtained with handheld glucometers on capillary blood.

Measurement of very low amounts of arsenic in soils and waters: is ICP-MS the indispensable analytical tool?

NASA Astrophysics Data System (ADS)

López-García, Ignacio; Marín-Hernández, Juan Jose; Perez-Sirvent, Carmen; Hernandez-Cordoba, Manuel

2017-04-01

The toxicity of arsenic and its wide distribution in the nature needs nowadays not to be emphasized, and the convenience of reliable analytical tools for arsenic determination at very low levels is clear. Leaving aside atomic fluorescence spectrometers specifically designed for this purpose, the task is currently carried out by using inductively coupled plasma mass spectrometry (ICP-MS), a powerful but expensive technique that is not available in all laboratories. However, as the recent literature clearly shows, a similar or even better analytical performance for the determination of several elements can be achieved by replacing the ICP-MS instrument by an AAS spectrometer (which is commonly present in any laboratory and involves low acquisition and maintenance costs) provided that a simple microextraction step is used to preconcentrate the sample. This communication reports the optimization and results obtained with a new analytical procedure based on this idea and focused to the determination of very low concentrations of arsenic in waters and extracts from soils and sediments. The procedure is based on a micro-solid phase extraction process for the separation and preconcentration of arsenic that uses magnetic particles covered with silver nanoparticles functionalized with the sodium salt of 2-mercaptoethane-sulphonate (MESNa). This composite is obtained in an easy way in the laboratory. After the sample is treated with a low amount (only a few milligrams) of the magnetic material, the solid phase is separated by means of a magnetic field, and then introduced into an electrothermal atomizer (ETAAS) for arsenic determination. The preconcentration factor is close to 200 with a detection limit below 0.1 µg L-1 arsenic. Speciation of As(III) and As(V) can be achieved by means of two extractions carried out at different acidity. The results for total arsenic are verified using certified reference materials. The authors are grateful to the Comunidad Autonóma de la Región de Murcia , Spain (Fundación Séneca, 19888/GERM/15) and to the Spanish MINECO (Project CTQ2015-68049-R) for financial support

Analytical techniques and instrumentation: A compilation

NASA Technical Reports Server (NTRS)

1974-01-01

Technical information on developments in instrumentation is arranged into four sections: (1) instrumentation for analysis; (2) analysis of matter; (3) analysis of electrical and mechanical phenomena; and (4) structural analysis. Patent information for two of the instruments described is presented.

Development of collaborative-creative learning model using virtual laboratory media for instrumental analytical chemistry lectures

NASA Astrophysics Data System (ADS)

Zurweni, Wibawa, Basuki; Erwin, Tuti Nurian

2017-08-01

The framework for teaching and learning in the 21st century was prepared with 4Cs criteria. Learning providing opportunity for the development of students' optimal creative skills is by implementing collaborative learning. Learners are challenged to be able to compete, work independently to bring either individual or group excellence and master the learning material. Virtual laboratory is used for the media of Instrumental Analytical Chemistry (Vis, UV-Vis-AAS etc) lectures through simulations computer application and used as a substitution for the laboratory if the equipment and instruments are not available. This research aims to design and develop collaborative-creative learning model using virtual laboratory media for Instrumental Analytical Chemistry lectures, to know the effectiveness of this design model adapting the Dick & Carey's model and Hannafin & Peck's model. The development steps of this model are: needs analyze, design collaborative-creative learning, virtual laboratory media using macromedia flash, formative evaluation and test of learning model effectiveness. While, the development stages of collaborative-creative learning model are: apperception, exploration, collaboration, creation, evaluation, feedback. Development of collaborative-creative learning model using virtual laboratory media can be used to improve the quality learning in the classroom, overcome the limitation of lab instruments for the real instrumental analysis. Formative test results show that the Collaborative-Creative Learning Model developed meets the requirements. The effectiveness test of students' pretest and posttest proves significant at 95% confidence level, t-test higher than t-table. It can be concluded that this learning model is effective to use for Instrumental Analytical Chemistry lectures.

Miniature GC-Minicell Ion Mobility Spectrometer (IMS) for In Situ Measurements in Astrobiology Planetary Missions

NASA Technical Reports Server (NTRS)

Kojiro, Daniel R.; Stimac, Robert M.; Kaye, William J.; Holland, Paul M.; Takeuchi, Norishige

2006-01-01

Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or ionger mission life for stationary landers/laboratories. The miniCometary Ice and Dust Experiment (miniCIDEX), which combined Gas Chromatography (GC) with helium Ion Mobility Spectrometry (IMS), was capable of providing the wide range of analytical information required for Astrobiology missions. The IMS used here was based on the PCP model 111 IMS. A similar system, the Titan Ice and Dust Experiment (TIDE), was proposed as part of the Titan Orbiter Aerorover Mission (TOAM). Newer GC systems employing Micro Electro- Mechanical System (MEMS) based technology have greatly reduced both the size and resource requirements for space GCs. These smaller GCs, as well as the continuing miniaturization of Astrobiology analytical instruments in general, has highlighted the need for smaller, dry helium IMS systems. We describe here the development of a miniature, MEMS GC-IMS system (MEMS GC developed by Thorleaf Research Inc.), employing the MiniCell Ion Mobility Spectrometer (IMS), from Ion Applications Inc., developed through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA s Small Business Innovative Research (SBIR) Program.

Advances in Instrumental Analysis of Brominated Flame Retardants: Current Status and Future Perspectives

PubMed Central

2014-01-01

This review aims to highlight the recent advances and methodological improvements in instrumental techniques applied for the analysis of different brominated flame retardants (BFRs). The literature search strategy was based on the recent analytical reviews published on BFRs. The main selection criteria involved the successful development and application of analytical methods for determination of the target compounds in various environmental matrices. Different factors affecting chromatographic separation and mass spectrometric detection of brominated analytes were evaluated and discussed. Techniques using advanced instrumentation to achieve outstanding results in quantification of different BFRs and their metabolites/degradation products were highlighted. Finally, research gaps in the field of BFR analysis were identified and recommendations for future research were proposed. PMID:27433482

Automated Mini-Column Solid-Phase Extraction Cleanup for High-Throughput Analysis of Chemical Contaminants in Foods by Low-Pressure Gas Chromatography-Tandem Mass Spectrometry.

PubMed

Lehotay, Steven J; Han, Lijun; Sapozhnikova, Yelena

2016-01-01

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO 4 /PSA (primary secondary amine)/C 18 /CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g -1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70-120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices ( n  = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.

40 CFR 1066.130 - Measurement instrument calibrations and verifications.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Measurement instrument calibrations... (CONTINUED) AIR POLLUTION CONTROLS VEHICLE-TESTING PROCEDURES Equipment, Measurement Instruments, Fuel, and Analytical Gas Specifications § 1066.130 Measurement instrument calibrations and verifications. The...

Evaluation of injection methods for fast, high peak capacity separations with low thermal mass gas chromatography.

PubMed

Fitz, Brian D; Mannion, Brandyn C; To, Khang; Hoac, Trinh; Synovec, Robert E

2015-05-01

Low thermal mass gas chromatography (LTM-GC) was evaluated for rapid, high peak capacity separations with three injection methods: liquid, headspace solid phase micro-extraction (HS-SPME), and direct vapor. An Agilent LTM equipped with a short microbore capillary column was operated at a column heating rate of 250 °C/min to produce a 60s separation. Two sets of experiments were conducted in parallel to characterize the instrumental platform. First, the three injection methods were performed in conjunction with in-house built high-speed cryo-focusing injection (HSCFI) to cryogenically trap and re-inject the analytes onto the LTM-GC column in a narrower band. Next, the three injection methods were performed natively with LTM-GC. Using HSCFI, the peak capacity of a separation of 50 nl of a 73 component liquid test mixture was 270, which was 23% higher than without HSCFI. Similar peak capacity gains were obtained when using the HSCFI with HS-SPME (25%), and even greater with vapor injection (56%). For the 100 μl vapor sample injected without HSCFI, the preconcentration factor, defined as the ratio of the maximum concentration of the detected analyte peak relative to the analyte concentration injected with the syringe, was determined to be 11 for the earliest eluting peak (most volatile analyte). In contrast, the preconcentration factor for the earliest eluting peak using HSCFI was 103. Therefore, LTM-GC is demonstrated to natively provide in situ analyte trapping, although not to as great an extent as with HSCFI. We also report the use of LTM-GC applied with time-of-flight mass spectrometry (TOFMS) detection for rapid, high peak capacity separations from SPME sampled banana peel headspace. Copyright © 2015 Elsevier B.V. All rights reserved.

A comparison of the analytical and experimental performance of the solid version of a cooled radial turbine

NASA Technical Reports Server (NTRS)

Tirres, Lizet

1991-01-01

An evaluation of the aerodynamic performance of the solid version of an Allison-designed cooled radial turbine was conducted at NASA Lewis' Warm Turbine Test Facility. The resulting pressure and temperature measurements are used to calculate vane, rotor, and overall stage performance. These performance results are then compared to the analytical results obtained by using NASA's MTSB (MERIDL-TSONIC-BLAYER) code.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

PubMed

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Composite Solid Propellant Predictability and Quality Assurance

NASA Technical Reports Server (NTRS)

Ramohalli, Kumar

1989-01-01

Reports are presented at the meeting at the University of Arizona on the study of predictable and reliable solid rocket motors. The following subject areas were covered: present state and trends in the research of solid propellants; the University of Arizona program in solid propellants, particularly in mixing (experimental and analytical results are presented).

Emerging technologies for the non-invasive characterization of physical-mechanical properties of tablets.

PubMed

Dave, Vivek S; Shahin, Hend I; Youngren-Ortiz, Susanne R; Chougule, Mahavir B; Haware, Rahul V

2017-10-30

The density, porosity, breaking force, viscoelastic properties, and the presence or absence of any structural defects or irregularities are important physical-mechanical quality attributes of popular solid dosage forms like tablets. The irregularities associated with these attributes may influence the drug product functionality. Thus, an accurate and efficient characterization of these properties is critical for successful development and manufacturing of a robust tablets. These properties are mainly analyzed and monitored with traditional pharmacopeial and non-pharmacopeial methods. Such methods are associated with several challenges such as lack of spatial resolution, efficiency, or sample-sparing attributes. Recent advances in technology, design, instrumentation, and software have led to the emergence of newer techniques for non-invasive characterization of physical-mechanical properties of tablets. These techniques include near infrared spectroscopy, Raman spectroscopy, X-ray microtomography, nuclear magnetic resonance (NMR) imaging, terahertz pulsed imaging, laser-induced breakdown spectroscopy, and various acoustic- and thermal-based techniques. Such state-of-the-art techniques are currently applied at various stages of development and manufacturing of tablets at industrial scale. Each technique has specific advantages or challenges with respect to operational efficiency and cost, compared to traditional analytical methods. Currently, most of these techniques are used as secondary analytical tools to support the traditional methods in characterizing or monitoring tablet quality attributes. Therefore, further development in the instrumentation and software, and studies on the applications are necessary for their adoption in routine analysis and monitoring of tablet physical-mechanical properties. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a solid surface fluorescence-based sensing system for aluminium monitoring in drinking water.

PubMed

Reyes, J F García; Barrales, P Ortega; Díaz, A Molina

2005-03-15

A novel, single and robust solid surface fluorescence-based sensing device assembled in a continuous flow system has been developed for the determination of trace amounts of aluminium in water samples. The proposed method is based on the transient immobilization of the target species on an appropriate active solid sensing zone (C(18) silica gel). The target species was the fluorogenic chelate, formed as a result of the on-line complexation of Al(III) with chromotropic acid (CA) at pH 4.1. The fluorescence of the complex is continuously monitored at an emission wavelength of 390nm upon excitation at 361nm. The instrumental, chemical and flow-injection variables affecting the fluorescence signal were carefully investigated and optimized. After selecting the most suitable conditions, the sensing system was calibrated in the range 10-500mugl(-1), obtaining a detection limit of 2.6mugl(-1), and a R.S.D. of 2.2%, with a sampling frequency of 24h(-1). In addition, the selectivity of the proposed methodology was evaluated by performing interference studies with different cations and anions which could affect the analytical response. Finally, the proposed method, which meets the EU regulations regarding the aluminium content in drinking waters, was satisfactorily applied to different water samples, with recoveries between 97 and 105%. The simplicity, low cost and easy operation are the main advantages of the present procedure.

PRESENTED 04/05/2006: MERCURY MEASUREMENTS ...

EPA Pesticide Factsheets

While traditional methods for determining mercury in solid samples involve the use of aggressive chemicals to dissolve the matrix and the use of other chemicals to properly reduce the mercury to the volatile elemental form, pyrolysis-based analyzers can be used by directly weighing the solid in a sampling boat and initiating the instrumental analysis for total mercury. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-soluble pharmaceuticals in source waters at levels that could be environmentally significant (at concentrations less than parts per billion, ppb). IAG with USGS ends in FY05. APM 20 due in FY05.Subtask 2: Coordination of interagency research and public outreach activities for PPCPs. Participate on NSTC Health and Environment subcommittee wo

TELEPHONIC PRESENTATION: MERCURY ...

EPA Pesticide Factsheets

While traditional methods for determining mercury in solid samples involve the use of aggressive chemicals to dissolve the matrix and the use of other chemicals to properly reduce the mercury to the volatile elemental form, pyrolysis-based analyzers can be used by directly weighing the solid in a sampling boat and initiating the instrumental analysis for total mercury. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water, and ORD in the area of Water Quality. Located In the subtasks are the various research projects being performed in support of this Task and more in-depth coverage of each project. Briefly, each project's objective is stated below.Subtask 1: To integrate state-of-the-art technologies (polar organic chemical integrative samplers, advanced solid-phase extraction methodologies with liquid chromatography/electrospray/mass spectrometry) and apply them to studying the sources and fate of a select list of PPCPs. Application and improvement of analytical methodologies that can detect non-volatile, polar, water-soluble pharmaceuticals in source waters at levels that could be environmentally significant (at concentrations less than parts per billion, ppb). IAG with USGS ends in FY05. APM 20 due in FY05.Subtask 2: Coordination of interagency research and public outreach activities for PPCPs. Participate on NSTC Health and Environment subcommittee wo

Conducting Reflective, Hands-On Research with Advanced Characterization Instruments: A High-Level Undergraduate Practical Exploring Solid-State Polymorphism

ERIC Educational Resources Information Center

Coles, S. J.; Mapp, L. K.

2016-01-01

An undergraduate practical exercise has been designed to provide hands-on, instrument-based experience of advanced characterization techniques. A research experience approach is taken, centered around the concept of solid-state polymorphism, which requires a detailed knowledge of molecular and crystal structure to be gained by advanced analytical…

Development and application of a multi-residue method for the determination of 53 pharmaceuticals in water, sediment, and suspended solids using liquid chromatography-tandem mass spectrometry.

PubMed

Aminot, Yann; Litrico, Xavier; Chambolle, Mélodie; Arnaud, Christine; Pardon, Patrick; Budzindki, Hélène

2015-11-01

Comprehensive source and fate studies of pharmaceuticals in the environment require analytical methods able to quantify a wide range of molecules over various therapeutic classes, in aqueous and solid matrices. Considering this need, the development of an analytical method to determine 53 pharmaceuticals in aqueous phase and in solid matrices using a combination of microwave-assisted extraction, solid phase extraction, and liquid chromatography coupled with tandem mass spectrometry is reported. Method was successfully validated regarding linearity, repeatability, and overall protocol recovery. Method detection limits (MDLs) do not exceed 1 ng L(-1) for 40 molecules in aqueous matrices (6 ng L(-1) for the 13 remaining), while subnanogram per gram MDLs were reached for 38 molecules in solid phase (29 ng g(-1) for the 15 remaining). Losses due to preparative steps were assessed for the 32 analytes associated to their labeled homologue, revealing an average loss of 40 % during reconcentration, the most altering step. Presence of analytes in wastewater treatment plant (WWTP) effluent aqueous phase and suspended solids (SS) as well as in river water, SS, and sediments was then investigated on a periurban river located in the suburbs of Bordeaux, France, revealing a major contribution of WWTP effluent to the river contamination. Sorption on river SS exceeded 5 % of total concentration for amitriptyline, fluoxetine, imipramine, ritonavir, sildenafil, and propranolol and appeared to be submitted to a seasonal influence. Sediment contamination was lower than the one of SS, organic carbon content, and sediment fine element proportion was accountable for the highest measured concentrations.

Use of mass spectrometry coupled with a solids insertion probe to prescreen soil samples for environmental samples

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

Check, C.E.; Bach, S.B.H.

1995-12-31

The contamination of air, water, and soils by a myriad of sources generates a large sample Currently, sample volume for hazardous constituent analyses is approximately half a million samples per year. The total analytical costs associated with this are astronomical. The analysis of these samples is vital in terms of assessing the types of contamination present and to what degree a site has been contaminated. The results of these analyses are very important for making an informed, knowledgeable decision as to the need for remediation and what type of remediation processes should be initiated based on site suitability vs non-actionmore » for the various sample sites. With an ever growing environmental consciousness in today`s society, the assessment and subsequent remediation of a site needs to be accomplished promptly despite the time constraints traditional methods place on such actions. In order to facilitate a rapid assessment, it is desirable to utilize instrumentation and equipment which afford the most information about a site allowing for optimization in environmental assessment while maintaining a realistic time schedule for the resulting remediation process. Because there are various types of environmental samples that can be taken at a site, different combinations of instrumentation and methods are required for assessing the level and type of contamination present whether it is in air, water, or soils. This study is limited to analyzing soil-like media that would normally fall under EPA Method 8270 which is used to analyze solid waste matrices, soils, and groundwater for semi-volatile organic compounds.« less

On-line solid phase extraction coupled to capillary LC-ESI-MS for determination of fluoxetine in human blood plasma.

PubMed

Saber, Amr L

2009-04-15

An instrumental setup including on-line solid phased extraction coupled to capillary liquid chromatography-electrospray ionization-mass spectrometry (SPE-capLC-ESI-MS) has been constructed to improve the sensitivity for quantification of fluoxetine hydrochloride in human plasma. Prior to injection, 0.5 mL of plasma spiked with metronidazole (internal standard) was mixed with ammonium formate buffer for effective chloroform liquid-liquid extraction. The method was validated in the range 5-60 ng mL(-1) fluoxetine, yielding a correlation coefficient of 0.999 (r(2)). The within-assay and between-assay precisions were between (8.5 and 11%) and (6.6 and 7.5%), respectively. The method was used to determine the amount of fluoxetine in a healthy male 14 h after an intake of one capsule of the antidepressant and anorectic Flutin, which contains 20mg fluoxetine per each capsule. Fluoxetine was detected, and the concentration was calculated to 9.0 ng mL(-1) plasma. In the preliminary experiments, conventional LC-UV instrumentation was employed. However, it was found that employing a capillary column with an inner diameter of (0.3mm I.D. x 50 mm, Zorbax C(18)) increased the sensitivity by a factor of approximately 100, when injecting the same mass of analyte. Incorporating an easily automated C(18) reversed phase column switching system with SPE (1.0mm I.D. x 5.0mm, 5 microm) made it possible to inject up to 100 microL of solution, and the total analysis time was 5.5 min.

Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

PubMed

Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

2018-09-18

The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous determination of PPCPs, EDCs, and artificial sweeteners in environmental water samples using a single-step SPE coupled with HPLC-MS/MS and isotope dilution.

PubMed

Tran, Ngoc Han; Hu, Jiangyong; Ong, Say Leong

2013-09-15

A high-throughput method for the simultaneous determination of 24 pharmaceuticals and personal care products (PPCPs), endocrine disrupting chemicals (EDCs) and artificial sweeteners (ASs) was developed. The method was based on a single-step solid phase extraction (SPE) coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and isotope dilution. In this study, a single-step SPE procedure was optimized for simultaneous extraction of all target analytes. Good recoveries (≥ 70%) were observed for all target analytes when extraction was performed using Chromabond(®) HR-X (500 mg, 6 mL) cartridges under acidic condition (pH 2). HPLC-MS/MS parameters were optimized for the simultaneous analysis of 24 PPCPs, EDCs and ASs in a single injection. Quantification was performed by using 13 isotopically labeled internal standards (ILIS), which allows correcting efficiently the loss of the analytes during SPE procedure, matrix effects during HPLC-MS/MS and fluctuation in MS/MS signal intensity due to instrument. Method quantification limit (MQL) for most of the target analytes was below 10 ng/L in all water samples. The method was successfully applied for the simultaneous determination of PPCPs, EDCs and ASs in raw wastewater, surface water and groundwater samples collected in a local catchment area in Singapore. In conclusion, the developed method provided a valuable tool for investigating the occurrence, behavior, transport, and the fate of PPCPs, EDCs and ASs in the aquatic environment. Copyright © 2013 Elsevier B.V. All rights reserved.

Scattering of focused ultrasonic beams by cavities in a solid half-space.

PubMed

Rahni, Ehsan Kabiri; Hajzargarbashi, Talieh; Kundu, Tribikram

2012-08-01

The ultrasonic field generated by a point focused acoustic lens placed in a fluid medium adjacent to a solid half-space, containing one or more spherical cavities, is modeled. The semi-analytical distributed point source method (DPSM) is followed for the modeling. This technique properly takes into account the interaction effect between the cavities placed in the focused ultrasonic field, fluid-solid interface and the lens surface. The approximate analytical solution that is available in the literature for the single cavity geometry is very restrictive and cannot handle multiple cavity problems. Finite element solutions for such problems are also prohibitively time consuming at high frequencies. Solution of this problem is necessary to predict when two cavities placed in close proximity inside a solid can be distinguished by an acoustic lens placed outside the solid medium and when such distinction is not possible.

Nitrogen-Functionalized Hydrothermal Carbon Materials by Using Urotropine as the Nitrogen Precursor.

PubMed

Straten, Jan Willem; Schleker, Philipp; Krasowska, Małgorzata; Veroutis, Emmanouil; Granwehr, Josef; Auer, Alexander A; Hetaba, Walid; Becker, Sylvia; Schlögl, Robert; Heumann, Saskia

2018-03-25

Nitrogen-containing hydrothermal carbon (N-HTC) materials of spherical particle morphology were prepared by means of hydrothermal synthesis with glucose and urotropine as precursors. The molar ratio of glucose to urotropine has been varied to achieve a continuous increase in nitrogen content. By raising the ratio of urotropine to glucose, a maximal nitrogen fraction of about 19 wt % could be obtained. Decomposition products of both glucose and urotropine react with each other; this opens up a variety of possible reaction pathways. The pH has a pronounced effect on the reaction pathway of the corresponding reaction steps. For the first time, a comprehensive analytical investigation, comprising a multitude of analytical tools and instruments, of a series of nitrogen-containing HTC materials was applied. Functional groups and structural motifs identified were analyzed by means of FTIR spectroscopy, thermogravimetric MS, and solid-state NMR spectroscopy. Information on reaction mechanisms and structural details were obtained by electronic structure calculations that were compared with vibrational spectra of polyfuran or polypyrrole-like groups, which represent structural motifs occurring in the present samples. © 2018 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

A model system to mimic environmentally active surface film roughness and hydrophobicity.

PubMed

Grant, Jacob S; Shaw, Scott K

2017-10-01

This work presents the development and initial assessment of a laboratory platform to allow quantitative studies on model urban films. The platform consists of stearic acid and eicosane mixtures that are solution deposited from hexanes onto smooth, solid substrates. We show that this model has distinctive capabilities to better mimic a naturally occurring film's morphology and hydrophobicity, two important parameters that have not previously been incorporated into model film systems. The physical and chemical properties of the model films are assessed using a variety of analytical instruments. The film thickness and roughness are probed via atomic force microscopy while the film composition, wettability, and water uptake are analyzed by Fourier transform infrared spectroscopy, contact angle goniometry, and quartz crystal microbalance, respectively. Simulated environmental maturation is achieved by exposing the film to regulated amounts of UV/ozone. Ultimately, oxidation of the film is monitored by the analytical techniques mentioned above and proceeds as expected to produce a utile model film system. Including variable roughness and tunable surface coverage results in several key advantages over prior model systems, and will more accurately represent native urban film behavior. Copyright © 2017 Elsevier Ltd. All rights reserved.

Chemical analysis of solid materials by a LIMS instrument designed for space research: 2D elemental imaging, sub-nm depth profiling and molecular surface analysis

NASA Astrophysics Data System (ADS)

Moreno-García, Pavel; Grimaudo, Valentine; Riedo, Andreas; Neuland, Maike B.; Tulej, Marek; Broekmann, Peter; Wurz, Peter

2016-04-01

Direct quantitative chemical analysis with high lateral and vertical resolution of solid materials is of prime importance for the development of a wide variety of research fields, including e.g., astrobiology, archeology, mineralogy, electronics, among many others. Nowadays, studies carried out by complementary state-of-the-art analytical techniques such as Auger Electron Spectroscopy (AES), X-ray Photoelectron Spectroscopy (XPS), Secondary Ion Mass Spectrometry (SIMS), Glow Discharge Time-of-Flight Mass Spectrometry (GD-TOF-MS) or Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) provide extensive insight into the chemical composition and allow for a deep understanding of processes that might have fashioned the outmost layers of an analyte due to its interaction with the surrounding environment. Nonetheless, these investigations typically employ equipment that is not suitable for implementation on spacecraft, where requirements concerning weight, size and power consumption are very strict. In recent years Laser Ablation/Ionization Mass Spectrometry (LIMS) has re-emerged as a powerful analytical technique suitable not only for laboratory but also for space applications.[1-3] Its improved performance and measurement capabilities result from the use of cutting edge ultra-short femtosecond laser sources, improved vacuum technology and fast electronics. Because of its ultimate compactness, simplicity and robustness it has already proven to be a very suitable analytical tool for elemental and isotope investigations in space research.[4] In this contribution we demonstrate extended capabilities of our LMS instrument by means of three case studies: i) 2D chemical imaging performed on an Allende meteorite sample,[5] ii) depth profiling with unprecedented sub-nm vertical resolution on Cu electrodeposited interconnects[6,7] and iii) preliminary molecular desorption of polymers without assistance of matrix or functionalized substrates.[8] On the whole, these results prove the adequacy of LMS as a powerful analytical tool able to address a great variety of topics in in situ space research. References: [1] U. Rohner, J. A. Whitby, P. Wurz, Meas. Sci. Technol. 2003, 14, 2159. [2] W. B. Brinckerhoff, G. G. Managadze, R. W. McEntire, A. F. Cheng, W. J. Green, Rev. Sci. Instrum. 2000, 71, 536. [3] G. G. Managadze, P. Wurz, R. Z. Sagdeev, A. E. Chumikov, M. Tuley, M. Yakovleva, N. G. Managadze, A. L. Bondarenko, Sol. Syst. Res. 2010, 44, 376. [4] A. Riedo, M. Neuland, S. Meyer, M. Tulej, P. Wurz, J. Anal. At. Spectrom. 2013, 28, 1256. [5] M.B. Neuland, S. Meyer, K. Mezger, A. Riedo, M. Tulej, P. Wurz, Planet. Space Sci. 2014, 101, 196. [6] V. Grimaudo, P. Moreno-García, A. Riedo, M. B. Neuland, M. Tulej, P. Broekmann, P. Wurz, Anal. Chem. 2015, 87, 2037. [7] A. Riedo, V. Grimaudo, P. Moreno-García, M. B. Neuland, M. Tulej, P. Wurz, P. Broekmann, J. Anal. At. Spectrom. 2015, 30, 2371. [8] P. Moreno-García, V. Grimaudo, A. Riedo, M. Tulej, P. Wurz, P. Broekmann, submitted to Rapid. Commun. Mass Spectrom., 2016.

Integrating laboratory robots with analytical instruments--must it really be so difficult?

PubMed

Kramer, G W

1990-09-01

Creating a reliable system from discrete laboratory instruments is often a task fraught with difficulties. While many modern analytical instruments are marvels of detection and data handling, attempts to create automated analytical systems incorporating such instruments are often frustrated by their human-oriented control structures and their egocentricity. The laboratory robot, while fully susceptible to these problems, extends such compatibility issues to the physical dimensions involving sample interchange, manipulation, and event timing. The workcell concept was conceived to describe the procedure and equipment necessary to carry out a single task during sample preparation. This notion can be extended to organize all operations in an automated system. Each workcell, no matter how complex its local repertoire of functions, must be minimally capable of accepting information (commands, data), returning information on demand (status, results), and being started, stopped, and reset by a higher level device. Even the system controller should have a mode where it can be directed by instructions from a higher level.

How to change environmental conditions for health.

PubMed

Commers, Matthew J; Gottlieb, Nell; Kok, Gerjo

2007-03-01

Since the Lalonde report, contemporary public-health theory has given steadily more attention to the role of environments in influencing health status. Environments, both social and physical, influence health directly or through complex interactions with behavior, genetics and health-care systems. They are also important for public-health because environments are the complex systems through which people are both empowered and exercise their empowerment. If public-health professionals are to play a significant role in influencing environments for health, they need analytical instruments that enable them to link specific environmental conditions with the actions necessary to improve them. These instruments must also enable public-health professionals to identify points of leverage for stimulating key actors to take the actions necessary to make environments more promoting of health. This article first presents one such analytical instrument. Then, building on examples relating to socio-economic health inequities, the analytical instrument is applied to reveal how it can add value to health professionals' effectiveness in planning interventions for more health-promoting environments.

Living Matter Observations with a Novel Hyperspectral Supercontinuum Confocal Microscope for VIS to Near-IR Reflectance Spectroscopy

PubMed Central

Bertani, Francesca R.; Ferrari, Luisa; Mussi, Valentina; Botti, Elisabetta; Costanzo, Antonio; Selci, Stefano

2013-01-01

A broad range hyper-spectroscopic microscope fed by a supercontinuum laser source and equipped with an almost achromatic optical layout is illustrated with detailed explanations of the design, implementation and data. The real novelty of this instrument, a confocal spectroscopic microscope capable of recording high resolution reflectance data in the VIS-IR spectral range from about 500 nm to 2.5 μm wavelengths, is the possibility of acquiring spectral data at every physical point as defined by lateral coordinates, X and Y, as well as at a depth coordinate, Z, as obtained by the confocal optical sectioning advantage. With this apparatus we collect each single scanning point as a whole spectrum by combining two linear spectral detector arrays, one CCD for the visible range, and one InGaAs infrared array, simultaneously available at the sensor output channel of the home made instrument. This microscope has been developed for biomedical analysis of human skin and other similar applications. Results are shown illustrating the technical performances of the instrument and the capability in extracting information about the composition and the structure of different parts or compartments in biological samples as well as in solid statematter. A complete spectroscopic fingerprinting of samples at microscopic level is shown possible by using statistical analysis on raw data or analytical reflectance models based on Abelés matrix transfer methods. PMID:24233077

Selected Analytical Methods for Environmental Remediation and Recovery (SAM) - Home

EPA Pesticide Factsheets

The SAM Home page provides access to all information provided in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM), and includes a query function allowing users to search methods by analyte, sample type and instrumentation.

Accounting for mudflow genesis in preliminary assessment of the maximum volume of solid mudflow sediments in the North Caucasus

NASA Astrophysics Data System (ADS)

Zalikhanov, M. Ch.; Kondratieva, N. V.; Adzhiev, A. Kh.; Razumov, V. V.

2016-09-01

The area of investigation was subject to multifactor analysis of the relationship between the maximum amount of mudflow solid sediments ( W) and parameters such as the mudflow basin area ( S), average channel slope (α), and mudflow channel length ( L). They were used to obtain analytical expressions in order to approximate the W( S, L, α) relation based on the mudflow genesis and source height. Statistical data on mudflow manifestations in different basins in the North Caucasus covering more than fifty years were used to obtain the analytical expressions in order to assess the maximum volume of mudflow solid sediments.

Analytical possibilities of different X-ray fluorescence systems for determination of trace elements in aqueous samples pre-concentrated with carbon nanotubes

NASA Astrophysics Data System (ADS)

Marguí, E.; Zawisza, B.; Skorek, R.; Theato, T.; Queralt, I.; Hidalgo, M.; Sitko, R.

2013-10-01

This study was aimed to achieve improved instrumental sensitivity and detection limits for multielement determination of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd in liquid samples by using different X-ray fluorescence (XRF) configurations (a benchtop energy-dispersive X-ray fluorescence spectrometer, a benchtop polarised energy-dispersive X-ray fluorescence spectrometer and a wavelength-dispersive X-ray fluorescence spectrometer). The preconcentration of metals from liquid solutions consisted on a solid-phase extraction using carbon nanotubes (CNTs) as solid sorbents. After the extraction step, the aqueous sample was filtered and CNTs with the absorbed elements were collected onto a filter paper which was directly analyzed by XRF. The calculated detection limits in all cases were in the low ng mL- 1 range. Nevertheless, results obtained indicate the benefits, in terms of sensitivity, of using polarized X-ray sources using different secondary targets in comparison to conventional XRF systems, above all if Cd determination is required. The developed methodologies, using the aforementioned equipments, have been applied for multielement determination in water samples from an industrial area of Poland.

Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

NASA Technical Reports Server (NTRS)

Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

2013-01-01

There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given in the Science Instruments.

Theoretical model of droplet wettability on a low-surface-energy solid under the influence of gravity.

PubMed

Yonemoto, Yukihiro; Kunugi, Tomoaki

2014-01-01

The wettability of droplets on a low surface energy solid is evaluated experimentally and theoretically. Water-ethanol binary mixture drops of several volumes are used. In the experiment, the droplet radius, height, and contact angle are measured. Analytical equations are derived that incorporate the effect of gravity for the relationships between the droplet radius and height, radius and contact angle, and radius and liquid surface energy. All the analytical equations display good agreement with the experimental data. It is found that the fundamental wetting behavior of the droplet on the low surface energy solid can be predicted by our model which gives geometrical information of the droplet such as the contact angle, droplet radius, and height from physical values of liquid and solid.

Infrared Imagery of Solid Rocket Exhaust Plumes

NASA Technical Reports Server (NTRS)

Moran, Robert P.; Houston, Janice D.

2011-01-01

The Ares I Scale Model Acoustic Test program consisted of a series of 18 solid rocket motor static firings, simulating the liftoff conditions of the Ares I five-segment Reusable Solid Rocket Motor Vehicle. Primary test objectives included acquiring acoustic and pressure data which will be used to validate analytical models for the prediction of Ares 1 liftoff acoustics and ignition overpressure environments. The test article consisted of a 5% scale Ares I vehicle and launch tower mounted on the Mobile Launch Pad. The testing also incorporated several Water Sound Suppression Systems. Infrared imagery was employed during the solid rocket testing to support the validation or improvement of analytical models, and identify corollaries between rocket plume size or shape and the accompanying measured level of noise suppression obtained by water sound suppression systems.

Analytical Applications of NMR: Summer Symposium on Analytical Chemistry.

ERIC Educational Resources Information Center

Borman, Stuart A.

1982-01-01

Highlights a symposium on analytical applications of nuclear magnetic resonance spectroscopy (NMR), discussing pulse Fourier transformation technique, two-dimensional NMR, solid state NMR, and multinuclear NMR. Includes description of ORACLE, an NMR data processing system at Syracuse University using real-time color graphics, and algorithms for…

Instrumental Analysis in Environmental Chemistry - Gas Phase Detection Systems

ERIC Educational Resources Information Center

Stedman, Donald H.; Meyers, Philip A.

1974-01-01

Discusses advances made in chemical analysis instrumentation used in environmental monitoring. This first of two articles is concerned with analytical instrumentation in which detection and dispersion depend ultimately on the properties of gaseous molecules. (JR)

Science Update: Analytical Chemistry.

ERIC Educational Resources Information Center

Worthy, Ward

1980-01-01

Briefly discusses new instrumentation in the field of analytical chemistry. Advances in liquid chromatography, photoacoustic spectroscopy, the use of lasers, and mass spectrometry are also discussed. (CS)

Advances in simultaneous DSC-FTIR microspectroscopy for rapid solid-state chemical stability studies: some dipeptide drugs as examples.

PubMed

Lin, Shan-Yang; Wang, Shun-Li

2012-04-01

The solid-state chemistry of drugs has seen growing importance in the pharmaceutical industry for the development of useful API (active pharmaceutical ingredients) of drugs and stable dosage forms. The stability of drugs in various solid dosage forms is an important issue because solid dosage forms are the most common pharmaceutical formulation in clinical use. In solid-state stability studies of drugs, an ideal accelerated method must not only be selected by different complicated methods, but must also detect the formation of degraded product. In this review article, an analytical technique combining differential scanning calorimetry and Fourier-transform infrared (DSC-FTIR) microspectroscopy simulates the accelerated stability test, and simultaneously detects the decomposed products in real time. The pharmaceutical dipeptides aspartame hemihydrate, lisinopril dihydrate, and enalapril maleate either with or without Eudragit E were used as testing examples. This one-step simultaneous DSC-FTIR technique for real-time detection of diketopiperazine (DKP) directly evidenced the dehydration process and DKP formation as an impurity common in pharmaceutical dipeptides. DKP formation in various dipeptides determined by different analytical methods had been collected and compiled. Although many analytical methods have been applied, the combined DSC-FTIR technique is an easy and fast analytical method which not only can simulate the accelerated drug stability testing but also at the same time enable to explore phase transformation as well as degradation due to thermal-related reactions. This technique offers quick and proper interpretations. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparative Variable Temperature Studies of Polyamide II with a Benchtop Fourier Transform and a Miniature Handheld Near-Infrared Spectrometer Using 2D-COS and PCMW-2D Analysis.

PubMed

Unger, Miriam; Pfeifer, Frank; Siesler, Heinz W

2016-07-01

The main objective of this communication is to compare the performance of a miniaturized handheld near-infrared (NIR) spectrometer with a benchtop Fourier transform near-infrared (FT-NIR) spectrometer. Generally, NIR spectroscopy is an extremely powerful analytical tool to study hydrogen-bonding changes of amide functionalities in solid and liquid materials and therefore variable temperature NIR measurements of polyamide II (PAII) have been selected as a case study. The information content of the measurement data has been further enhanced by exploiting the potential of two-dimensional correlation spectroscopy (2D-COS) and the perturbation correlation moving window two-dimensional (PCMW2D) evaluation technique. The data provide valuable insights not only into the changes of the hydrogen-bonding structure and the recrystallization of the hydrocarbon segments of the investigated PAII but also in their sequential order. Furthermore, it has been demonstrated that the 2D-COS and PCMW2D results derived from the spectra measured with the miniaturized NIR instrument are equivalent to the information extracted from the data obtained with the high-performance FT-NIR instrument. © The Author(s) 2016.

Preliminary design trade-offs for a multi-mission stored cryogen cooler

NASA Technical Reports Server (NTRS)

Sherman, A.

1978-01-01

Preliminary design studies were performed for a multi-mission solid cryogen cooler having a wide range of application for both the shuttle sortie and free flyer missions. This multi-mission cooler (MMC) is designed to be utilized with various solid cryogens to meet a wide range of instrument cooling from 10 K (with solid hydrogen) to 90 K. The baseline cooler utilizes two stages of solid cryogen and incorporates an optional, higher temperature third stage which is cooled by either a passive radiator or a thermoelectric cooler. The MMC has an interface which can accommodate a wide variety of instrument configurations. A shrink fit adapter is incorporated which allows a drop-in instrument integration. The baseline design provides cooling of approximately 1 watt over a 60 to 100 K temperature range and about 0.5 watts from 15 to 60 K for a one year lifetime. For low cooling loads and with use of the optional radiator shield, cooling lifetimes as great as 8 years are predicted.

Innovative instrumentation for mineralogical and elemental analyses of solid extraterrestrial surfaces: The Backscatter Moessbauer Spectrometer/X Ray Fluorescence analyzer (BaMS/XRF)

NASA Technical Reports Server (NTRS)

Shelfer, T. D.; Morris, Richard V.; Nguyen, T.; Agresti, D. G.; Wills, E. L.

1994-01-01

We have developed a four-detector research-grade backscatter Moessbauer spectrometer (BaMS) instrument with low resolution x-ray fluorescence analysis (XRF) capability. A flight-qualified instrument based on this design would be suitable for use on missions to the surfaces of solid solar-system objects (Moon, Mars, asteroids, etc.). Target specifications for the flight instrument are as follows: mass less than 500 g; volumes less than 300 cu cm; and power less than 2 W. The BaMS/XRF instrument would provide data on the oxidation state of iron and its distribution among iron-bearing mineralogies and elemental composition information. This data is a primary concern for the characterization of extraterrestrial surface materials.

Cellular telephone-based radiation detection instrument

DOEpatents

Craig, William W [Pittsburg, CA; Labov, Simon E [Berkeley, CA

2011-06-14

A network of radiation detection instruments, each having a small solid state radiation sensor module integrated into a cellular phone for providing radiation detection data and analysis directly to a user. The sensor module includes a solid-state crystal bonded to an ASIC readout providing a low cost, low power, light weight compact instrument to detect and measure radiation energies in the local ambient radiation field. In particular, the photon energy, time of event, and location of the detection instrument at the time of detection is recorded for real time transmission to a central data collection/analysis system. The collected data from the entire network of radiation detection instruments are combined by intelligent correlation/analysis algorithms which map the background radiation and detect, identify and track radiation anomalies in the region.

Transmission versus reflectance spectroscopy for quantitation.

PubMed

Gardner, Craig M

2018-01-01

The objective of this work was to compare the accuracy of analyte concentration estimation when using transmission versus diffuse reflectance spectroscopy of a scattering medium. Monte Carlo ray tracing of light through the medium was used in conjunction with pure component absorption spectra and Beer-Lambert absorption along each ray's pathlength to generate matched sets of pseudoabsorbance spectra, containing water and six analytes present in skin. PLS regression models revealed an improvement in accuracy when using transmission compared to reflectance for a range of medium thicknesses and instrument noise levels. An analytical expression revealed the source of the accuracy degradation with reflectance was due both to the reduced collection efficiency for a fixed instrument etendue and to the broad pathlength distribution that detected light travels in the medium before exiting from the incident side. (2018) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE).

Generation and analysis of chemical compound libraries

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

Gregoire, John M.; Jin, Jian; Kan, Kevin S.

2017-10-03

Various samples are generated on a substrate. The samples each includes or consists of one or more analytes. In some instances, the samples are generated through the use of gels or through vapor deposition techniques. The samples are used in an instrument for screening large numbers of analytes by locating the samples between a working electrode and a counter electrode assembly. The instrument also includes one or more light sources for illuminating each of the samples. The instrument is configured to measure the photocurrent formed through a sample as a result of the illumination of the sample.

Continuing evolution of in-vitro diagnostic instrumentation

NASA Astrophysics Data System (ADS)

Cohn, Gerald E.

2000-04-01

The synthesis of analytical instrumentation and analytical biochemistry technologies in modern in vitro diagnostic instrumentation continues to generate new systems with improved performance and expanded capability. Detection modalities have expanded to include multichip modes of fluorescence, scattering, luminescence and reflectance so as to accommodate increasingly sophisticated immunochemical and nucleic acid based reagent systems. The time line graph of system development now extends from the earliest automated clinical spectrophotometers through molecule recognition assays and biosensors to the new breakthroughs of biochip and DNA diagnostics. This brief review traces some of the major innovations in the evolution of system technologies and previews the conference program.

FDA Bacteriological Analytical Manual, Chapter 10, 2003: Listeria monocytogenes

EPA Pesticide Factsheets

FDA Bacteriological Analytical Manual, Chapter 10 describes procedures for analysis of food samples and may be adapted for assessment of solid, particulate, aerosol, liquid and water samples containing Listeria monocytogenes.

Manual Solid-Phase Peptide Synthesis of Metallocene-Peptide Bioconjugates

ERIC Educational Resources Information Center

Kirin, Srecko I.; Noor, Fozia; Metzler-Nolte, Nils; Mier, Walter

2007-01-01

A simple and relatively inexpensive procedure for preparing a biologically active peptide using solid phase peptide synthesis (SPPS) is described. Fourth-year undergraduate students have gained firsthand experience from the solid-phase synthesis techniques and they have become familiar with modern analytical techniques based on the particular…

A Robot or a Science Instrument?

NASA Image and Video Library

2009-10-20

Some say the science instrument on NASA Wide-field Infrared Survey Explorer mission resembles the Star Wars robot R2-D2. The instrument is enclosed in a solid-hydrogen cryostat, which cools the WISE telescope and detectors.

Raman Spectrometry.

ERIC Educational Resources Information Center

Gardiner, Derek J.

1980-01-01

Reviews mainly quantitative analytical applications in the field of Raman spectrometry. Includes references to other reviews, new and analytically untested techniques, and novel sampling and instrument designs. Cites 184 references. (CS)

Analysis of Volatile Compounds by Advanced Analytical Techniques and Multivariate Chemometrics.

PubMed

Lubes, Giuseppe; Goodarzi, Mohammad

2017-05-10

Smelling is one of the five senses, which plays an important role in our everyday lives. Volatile compounds are, for example, characteristics of food where some of them can be perceivable by humans because of their aroma. They have a great influence on the decision making of consumers when they choose to use a product or not. In the case where a product has an offensive and strong aroma, many consumers might not appreciate it. On the contrary, soft and fresh natural aromas definitely increase the acceptance of a given product. These properties can drastically influence the economy; thus, it has been of great importance to manufacturers that the aroma of their food product is characterized by analytical means to provide a basis for further optimization processes. A lot of research has been devoted to this domain in order to link the quality of, e.g., a food to its aroma. By knowing the aromatic profile of a food, one can understand the nature of a given product leading to developing new products, which are more acceptable by consumers. There are two ways to analyze volatiles: one is to use human senses and/or sensory instruments, and the other is based on advanced analytical techniques. This work focuses on the latter. Although requirements are simple, low-cost technology is an attractive research target in this domain; most of the data are generated with very high-resolution analytical instruments. Such data gathered based on different analytical instruments normally have broad, overlapping sensitivity profiles and require substantial data analysis. In this review, we have addressed not only the question of the application of chemometrics for aroma analysis but also of the use of different analytical instruments in this field, highlighting the research needed for future focus.

Analytical study on a two-dimensional plane of the off-design flow properties of tandem-bladed compressor stators

NASA Technical Reports Server (NTRS)

Sanger, N. L.

1973-01-01

The flow characteristics of several tandem bladed compressor stators were analytically evaluated over a range of inlet incidence angles. The ratios of rear-segment to front-segment chord and camber were varied. Results were also compared to the analytical performance of a reference solid blade section. All tandem blade sections exhibited lower calculated losses than the solid stator. But no one geometric configuration exhibited clearly superior characteristics. The front segment accepts the major effect of overall incidence angle change. Rear- to front-segment camber ratios of 4 and greater appeared to be limited by boundary-layer separation from the pressure surface of the rear segment.

Virial coefficients of anisotropic hard solids of revolution: The detailed influence of the particle geometry

NASA Astrophysics Data System (ADS)

Herold, Elisabeth; Hellmann, Robert; Wagner, Joachim

2017-11-01

We provide analytical expressions for the second virial coefficients of differently shaped hard solids of revolution in dependence on their aspect ratio. The second virial coefficients of convex hard solids, which are the orientational averages of the mutual excluded volume, are derived from volume, surface, and mean radii of curvature employing the Isihara-Hadwiger theorem. Virial coefficients of both prolate and oblate hard solids of revolution are investigated in dependence on their aspect ratio. The influence of one- and two-dimensional removable singularities of the surface curvature to the mutual excluded volume is analyzed. The virial coefficients of infinitely thin oblate and infinitely long prolate particles are compared, and analytical expressions for their ratios are derived. Beyond their dependence on the aspect ratio, the second virial coefficients are influenced by the detailed geometry of the particles.

Virial coefficients of anisotropic hard solids of revolution: The detailed influence of the particle geometry.

PubMed

Herold, Elisabeth; Hellmann, Robert; Wagner, Joachim

2017-11-28

We provide analytical expressions for the second virial coefficients of differently shaped hard solids of revolution in dependence on their aspect ratio. The second virial coefficients of convex hard solids, which are the orientational averages of the mutual excluded volume, are derived from volume, surface, and mean radii of curvature employing the Isihara-Hadwiger theorem. Virial coefficients of both prolate and oblate hard solids of revolution are investigated in dependence on their aspect ratio. The influence of one- and two-dimensional removable singularities of the surface curvature to the mutual excluded volume is analyzed. The virial coefficients of infinitely thin oblate and infinitely long prolate particles are compared, and analytical expressions for their ratios are derived. Beyond their dependence on the aspect ratio, the second virial coefficients are influenced by the detailed geometry of the particles.

Reaction wheel low-speed compensation using a dither signal

NASA Astrophysics Data System (ADS)

Stetson, John B., Jr.

1993-08-01

A method for improving low-speed reaction wheel performance on a three-axis controlled spacecraft is presented. The method combines a constant amplitude offset with an unbiased, oscillating dither to harmonically linearize rolling solid friction dynamics. The complete, nonlinear rolling solid friction dynamics using an analytic modification to the experimentally verified Dahl solid friction model were analyzed using the dual-input describing function method to assess the benefits of dither compensation. The modified analytic solid friction model was experimentally verified with a small dc servomotor actuated reaction wheel assembly. Using dither compensation abrupt static friction disturbances are eliminated and near linear behavior through zero rate can be achieved. Simulated vehicle response to a wheel rate reversal shows that when the dither and offset compensation is used, elastic modes are not significantly excited, and the uncompensated attitude error reduces by 34:1.

Statistical error in simulations of Poisson processes: Example of diffusion in solids

NASA Astrophysics Data System (ADS)

Nilsson, Johan O.; Leetmaa, Mikael; Vekilova, Olga Yu.; Simak, Sergei I.; Skorodumova, Natalia V.

2016-08-01

Simulations of diffusion in solids often produce poor statistics of diffusion events. We present an analytical expression for the statistical error in ion conductivity obtained in such simulations. The error expression is not restricted to any computational method in particular, but valid in the context of simulation of Poisson processes in general. This analytical error expression is verified numerically for the case of Gd-doped ceria by running a large number of kinetic Monte Carlo calculations.

Assessment of analytical techniques for predicting solid propellant exhaust plumes and plume impingement environments

NASA Technical Reports Server (NTRS)

Tevepaugh, J. A.; Smith, S. D.; Penny, M. M.

1977-01-01

An analysis of experimental nozzle, exhaust plume, and exhaust plume impingement data is presented. The data were obtained for subscale solid propellant motors with propellant Al loadings of 2, 10 and 15% exhausting to simulated altitudes of 50,000, 100,000 and 112,000 ft. Analytical predictions were made using a fully coupled two-phase method of characteristics numerical solution and a technique for defining thermal and pressure environments experienced by bodies immersed in two-phase exhaust plumes.

Post-analytical Issues in Hemostasis and Thrombosis Testing.

PubMed

Favaloro, Emmanuel J; Lippi, Giuseppe

2017-01-01

Analytical concerns within hemostasis and thrombosis testing are continuously decreasing. This is essentially attributable to modern instrumentation, improvements in test performance and reliability, as well as the application of appropriate internal quality control and external quality assurance measures. Pre-analytical issues are also being dealt with in some newer instrumentation, which are able to detect hemolysis, icteria and lipemia, and, in some cases, other issues related to sample collection such as tube under-filling. Post-analytical issues are generally related to appropriate reporting and interpretation of test results, and these are the focus of the current overview, which provides a brief description of these events, as well as guidance for their prevention or minimization. In particular, we propose several strategies for improved post-analytical reporting of hemostasis assays and advise that this may provide the final opportunity to prevent serious clinical errors in diagnosis.

A dipole-assisted solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for online determination of trace heavy metals in natural water.

PubMed

Shih, Tsung-Ting; Hsu, I-Hsiang; Chen, Shun-Niang; Chen, Ping-Hung; Deng, Ming-Jay; Chen, Yu; Lin, Yang-Wei; Sun, Yuh-Chang

2015-01-21

We employed a polymeric material, poly(methyl methacrylate) (PMMA), for fabricating a microdevice and then implanted the chlorine (Cl)-containing solid-phase extraction (SPE) functionality into the PMMA chip to develop an innovative on-chip dipole-assisted SPE technique. Instead of the ion-ion interactions utilized in on-chip SPE techniques, the dipole-ion interactions between the highly electronegative C-Cl moieties in the channel interior and the positively charged metal ions were employed to facilitate the on-chip SPE procedures. Furthermore, to avoid labor-intensive manual manipulation, a programmable valve manifold was designed as an interface combining the dipole-assisted SPE microchip and inductively coupled plasma-mass spectrometry (ICP-MS) to achieve the fully automated operation. Under the optimized operation conditions for the established system, the detection limits for each analyte ion were obtained based on three times the standard deviation of seven measurements of the blank eluent solution. The limits ranged from 3.48 to 20.68 ng L(-1), suggesting that this technique appears uniquely suited for determining the levels of heavy metal ions in natural water. Indeed, a series of validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Remarkably, the developed device was durable enough to be reused more than 160 times without any loss in its analytical performance. To the best of our knowledge, this is the first study reporting on the combination of a dipole-assisted SPE microchip and elemental analysis instrument for the online determination of trace heavy metal ions.

A core-shell column approach to a comprehensive high-performance liquid chromatography phenolic analysis of Vitis vinifera L. and interspecific hybrid grape juices, wines, and other matrices following either solid phase extraction or direct injection.

PubMed

Manns, David C; Mansfield, Anna Katharine

2012-08-17

Four high-throughput reverse-phase chromatographic protocols utilizing two different core-shell column chemistries have been developed to analyze the phenolic profiles of complex matrices, specifically targeting juices and wines produced from interspecific hybrid grape cultivars. Following pre-fractionation via solid-phase extraction or direct injection, individual protocols were designed to resolve, identify and quantify specific chemical classes of compounds including non-anthocyanin monomeric phenolics, condensed tannins following acid hydrolysis, and anthocyanins. Detection levels ranging from 1.2 ppb to 27.5 ppb, analyte %RSDs ranging from 0.04 to 0.38, and linear ranges of quantitation approaching five orders of magnitude were achieved using conventional HPLC instrumentation. Using C(18) column chemistry, the non-anthocyanin monomeric protocol effectively separated a set of 16 relevant phenolic compounds comprised flavan-3-ols, hydroxycinnamic acids, and flavonols in under 14 min. The same column was used to develop a 15-min protocol for hydrolyzed condensed tannin analysis. Two anthocyanin protocols are presented, one utilizing the same C(18) column, best suited for anthocyanidin and monoglucoside analysis, the other utilizing a pentafluorophenyl chemistry optimized to effectively separate complex mixtures of coexisting mono- and diglucoside anthocyanins. These protocols and column chemistries have been used initially to explore a wide variety of complex phenolic matrices, including red and white juices and wines produced from Vitis vinifera and interspecific hybrid grape cultivars, juices, teas, and plant extracts. Each protocol displayed robust matrix responses as written, yet are flexible enough to be easily modified to suit specifically tailored analytical requirements. Copyright © 2012 Elsevier B.V. All rights reserved.

Resonance Energy Transfer-Based Nucleic Acid Hybridization Assays on Paper-Based Platforms Using Emissive Nanoparticles as Donors.

PubMed

Doughan, Samer; Noor, M Omair; Han, Yi; Krull, Ulrich J

2017-01-01

Quantum dots (QDs) and upconverting nanoparticles (UCNPs) are luminescent nanoparticles (NPs) commonly used in bioassays and biosensors as resonance energy transfer (RET) donors. The narrow and tunable emissions of both QDs and UCNPs make them versatile RET donors that can be paired with a wide range of acceptors. Ratiometric signal processing that compares donor and acceptor emission in RET-based transduction offers improved precision, as it accounts for fluctuations in the absolute photoluminescence (PL) intensities of the donor and acceptor that can result from experimental and instrumental variations. Immobilizing NPs on a solid support avoids problems such as those that can arise with their aggregation in solution, and allows for facile layer-by-layer assembly of the interfacial chemistry. Paper is an attractive solid support for the development of point-of-care diagnostic assays given its ubiquity, low-cost, and intrinsic fluid transport by capillary action. Integration of nanomaterials with paper-based analytical devices (PADs) provides avenues to augment the analytical performance of PADs, given the unique optoelectronic properties of nanomaterials. Herein, we describe methodology for the development of PADs using QDs and UCNPs as RET donors for optical transduction of nucleic acid hybridization. Immobilization of green-emitting QDs (gQDs) on imidazole functionalized cellulose paper is described for use as RET donors with Cy3 molecular dye as acceptors for the detection of SMN1 gene fragment. We also describe the covalent immobilization of blue-emitting UCNPs on aldehyde modified cellulose paper for use as RET donors with orange-emitting QDs (oQDs) as acceptors for the detection of HPRT1 gene fragment. The data described herein is acquired using an epifluorescence microscope, and can also be collected using technology such as a typical electronic camera.

A multiresidue method for the analysis of 90 pesticides, 16 PAHs, and 22 PCBs in honey using QuEChERS-SPME.

PubMed

Al-Alam, Josephine; Fajloun, Ziad; Chbani, Asma; Millet, Maurice

2017-08-01

An optimized analytical method was developed for the simultaneous analysis of 90 pesticides, 16 polycyclic aromatic hydrocarbons, and 22 polychlorinated biphenyls. The method was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction using acetonitrile followed by a dispersive solid-phase extraction cleanup using primary-secondary amine and octadecyl (C 18 ). The extract obtained was concentrated by evaporation and then reconstituted with acetonitrile to prepare it for chromatographic analysis by liquid chromatography-triple-quadrupole tandem mass spectrometry and gas chromatography-ion-trap tandem mass spectrometry, which was preceded by a preconcentration step using solid-phase microextraction with appropriate fibers. The combination of the two extraction steps ensured efficient extract cleanup. The use of the two analytical instruments allowed the analysis of a large number of pollutants with a high reliability rate. The method developed was validated for linearity, which was studied with use of matrix-matched calibration curves in the concentration range between 10 and 3000 ng g -1 . The correlation coefficient (R 2 ) obtained was higher than 0.98 for most of the target compounds, with a relative standard deviation lower than 20% for repeatability and reproducibility. The limits of detection and quantification were lower than 20 and 60 ng g -1 respectively for the compounds analyzed, and the recoveries were between 60% and 103% for most compounds. Finally, the method was tested for its efficiency on real samples by the analysis of three honey samples in which seven pesticides and nine polycyclic aromatic hydrocarbons were determined. Graphical Abstract ᅟ.

Critical review of the analysis of brominated flame retardants and their environmental levels in Africa.

PubMed

Brits, Martin; de Vos, Jayne; Weiss, Jana M; Rohwer, Egmont R; de Boer, Jacob

2016-12-01

World-wide, the prevalence of brominated flame retardants (BFRs) is well documented for routine analysis of environmental and biological matrices. There is, however, limited information on these compounds in the African environment and insufficient information on the analytical approaches used to obtain data. This paper presents a review on BFR levels in the African environment and the various analytical methodologies specifically applied in Africa for polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls and alternative-BFRs. The analyses include liquid sample preparation using liquid-liquid and solid phase extraction and solid sample preparation involving Soxhlet extraction, with ultrasound-assisted extraction increasingly being applied. Instrumental detection techniques were limited to gas chromatography coupled with electron capture detector and electron impact ionisation with single quadrupole mass spectrometers. Information on congener profile prevalence in indoor dust, soil, aquatic environment (water, sediment, and aquatic organisms), eggs, wastewater treatment plant compartments, landfills (leachate and sediment) and breast milk are presented. Although PBDEs were inconsistently detected, contamination was reported for all investigated matrices in the African environment. The manifestation in remote regions indicates the ubiquitous prevalence and long-range transport of these compounds. Levels in sediment, and breast milk from some African countries were higher than reported for Asia and Europe. Due to limited data or non-detection of alternative-BFRs, it is unclear whether banned formulations were replaced in Africa. Most of the data reported for BFR levels in Africa were obtained in non-African laboratories or in South Africa and formed the basis for our discussion of reported contamination levels and related methodologies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microfluidic-Based sample chips for radioactive solutions

DOE PAGES

Tripp, J. L.; Law, J. D.; Smith, T. E.; ...

2015-01-01

Historical nuclear fuel cycle process sampling techniques required sample volumes ranging in the tens of milliliters. The radiation levels experienced by analytical personnel and equipment, in addition to the waste volumes generated from analysis of these samples, have been significant. These sample volumes also impacted accountability inventories of required analytes during process operations. To mitigate radiation dose and other issues associated with the historically larger sample volumes, a microcapillary sample chip was chosen for further investigation. The ability to obtain microliter volume samples coupled with a remote automated means of sample loading, tracking, and transporting to the analytical instrument wouldmore » greatly improve analytical efficiency while reducing both personnel exposure and radioactive waste volumes. Sample chip testing was completed to determine the accuracy, repeatability, and issues associated with the use of microfluidic sample chips used to supply µL sample volumes of lanthanide analytes dissolved in nitric acid for introduction to an analytical instrument for elemental analysis.« less

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

none, none; Tuchman, Nancy

The U.S. Department of Energy awarded Loyola University Chicago and the Institute of Environmental Sustainability (IES) $486,000.00 for the proposal entitled “Chicago clean air, clean water project: Environmental monitoring for a healthy, sustainable urban future.” The project supported the purchase of analytical instruments for the development of an environmental analytical laboratory. The analytical laboratory is designed to support the testing of field water and soil samples for nutrients, industrial pollutants, heavy metals, and agricultural toxins, with special emphasis on testing Chicago regional soils and water affected by coal-based industry. Since the award was made in 2010, the IES has beenmore » launched (fall 2013), and the IES acquired a new state-of-the-art research and education facility on Loyola University Chicago’s Lakeshore campus. Two labs were included in the research and education facility. The second floor lab is the Ecology Laboratory where lab experiments and analyses are conducted on soil, plant, and water samples. The third floor lab is the Environmental Toxicology Lab where lab experiments on environmental toxins are conducted, as well as analytical tests conducted on water, soil, and plants. On the south end of the Environmental Toxicology Lab is the analytical instrumentation collection purchased from the present DOE grant, which is overseen by a full time Analytical Chemist (hired January 2016), who maintains the instruments, conducts analyses on samples, and helps to train faculty and undergraduate and graduate student researchers.« less

Simple method for the determination of personal care product ingredients in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by GC-MS.

PubMed

Cabrera-Peralta, Jerónimo; Peña-Alvarez, Araceli

2018-05-01

A simple method for the simultaneous determination of personal care product ingredients: galaxolide, tonalide, oxybenzone, 4-methylbenzyliden camphor, padimate-o, 2-ethylhexyl methoxycinnamate, octocrylene, triclosan, and methyl triclosan in lettuce by ultrasound-assisted extraction combined with solid-phase microextraction followed by gas chromatography with mass spectrometry was developed. Lettuce was directly extracted by ultrasound-assisted extraction with methanol, this extract was combined with water, extracted by solid-phase microextraction in immersion mode, and analyzed by gas chromatography with mass spectrometry. Good linear relationships (25-250 ng/g, R 2  > 0.9702) and low detection limits (1.0-25 ng/g) were obtained for analytes along with acceptable precision for almost all analytes (RSDs < 20%). The validated method was applied for the determination of personal care product ingredients in commercial lettuce and lettuces grown in soil and irrigated with the analytes, identifying the target analytes in leaves and roots of the latter. This procedure is a miniaturized and environmentally friendly proposal which can be a useful tool for quality analysis in lettuce. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Active Neutron and Gamma-Ray Instrumentation for In Situ Planetary Science Applications

NASA Technical Reports Server (NTRS)

Parsons, A.; Bodnarik, J.; Evans, L.; Floyd, A.; Lim, L.; McClanahan, T.; Namkung, M.; Nowicki, S.; Schweitzer, J.; Starr, R.;

Cosmic-Ray Background Flux Model based on a Gamma-Ray Large-Area Space Telescope Balloon Flight Engineering Model

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

Mizuno, T

2004-09-03

Cosmic-ray background fluxes were modeled based on existing measurements and theories and are presented here. The model, originally developed for the Gamma-ray Large Area Space Telescope (GLAST) Balloon Experiment, covers the entire solid angle (4{pi} sr), the sensitive energy range of the instrument ({approx} 10 MeV to 100 GeV) and abundant components (proton, alpha, e{sup -}, e{sup +}, {mu}{sup -}, {mu}{sup +} and gamma). It is expressed in analytic functions in which modulations due to the solar activity and the Earth geomagnetism are parameterized. Although the model is intended to be used primarily for the GLAST Balloon Experiment, model functionsmore » in low-Earth orbit are also presented and can be used for other high energy astrophysical missions. The model has been validated via comparison with the data of the GLAST Balloon Experiment.« less

Cosmic-Ray Background Flux Model Baed on a Gamma-Ray Large Area Space Telescope Baloon Flight Engineering

NASA Technical Reports Server (NTRS)

2002-01-01

Cosmic-ray background fluxes were modeled based on existing measurements and theories and are presented here. The model, originally developed for the Gamma-ray Large Area Space Telescope (GLAST) Balloon Experiment, covers the entire solid angle (4(pi) sr), the sensitive energy range of the instrument ((approx) 10 MeV to 100 GeV) and abundant components (proton, alpha, e(sup -), e(sup +), (mu)(sup -), (mu)(sup +) and gamma). It is expressed in analytic functions in which modulations due to the solar activity and the Earth geomagnetism are parameterized. Although the model is intended to be used primarily for the GLAST Balloon Experiment, model functions in low-Earth orbit are also presented and can be used for other high energy astrophysical missions. The model has been validated via comparison with the data of the GLAST Balloon Experiment.

Publications of LASL research, 1972--1976

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

Petersen, L.

1977-04-01

This bibliography is a compilation of unclassified work done at the Los Alamos Scientific Laboratory and published during the years 1972 to 1976. Publications too late for inclusion in earlier compilations are also listed. Declassification of previously classified reports is considered to constitute publication. The bibliography includes LASL reports, journal articles, books, conference papers, papers published in congressional hearings, theses, patents, etc. The following subject areas are included: aerospace studies; analytical technology; astrophysics; atomic and molecular physics, equation of state, opacity; biology and medicine; chemical dynamics and kinetics; chemistry; cryogenics; crystallography; CTR and plasma physics; earth science and engineering; energymore » (nonnuclear); engineering and equipment; EPR, ESR, NMR studies; explosives and detonations; fission physics; health and safety; hydrodynamics and radiation transport; instruments; lasers; mathematics and computers; medium-energy physics; metallurgy and ceramics technology; neutronics and criticality studies; nuclear physics; nuclear safeguards; physics; reactor technology; solid state science; and miscellaneous (including Project Rover). (RWR)« less

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

Gundlach-Graham, Alexander W.; Dennis, Elise; Ray, Steven J.

An inductively coupled plasma distance-of-flight mass spectrometer (ICP-DOFMS) has been coupled with laser-ablation (LA) sample introduction for the elemental analysis of solids. ICP-DOFMS is well suited for the analysis of laser-generated aerosols because it offers both high-speed mass analysis and simultaneous multi-elemental detection. Here, we evaluate the analytical performance of the LA-ICP-DOFMS instrument, equipped with a microchannel plate-based imaging detector, for the measurement of steady-state LA signals, as well as transient signals produced from single LA events. Steady-state detection limits are 1 mg g1, and absolute single-pulse LA detection limits are 200 fg for uranium; the system is shown capablemore » of performing time-resolved single-pulse LA analysis. By leveraging the benefits of simultaneous multi-elemental detection, we also attain a good shot-to-shot reproducibility of 6% relative standard deviation (RSD) and isotope-ratio precision of 0.3% RSD with a 10 s integration time.« less

Detection systems for mass spectrometry imaging: a perspective on novel developments with a focus on active pixel detectors.

PubMed

Jungmann, Julia H; Heeren, Ron M A

2013-01-15

Instrumental developments for imaging and individual particle detection for biomolecular mass spectrometry (imaging) and fundamental atomic and molecular physics studies are reviewed. Ion-counting detectors, array detection systems and high mass detectors for mass spectrometry (imaging) are treated. State-of-the-art detection systems for multi-dimensional ion, electron and photon detection are highlighted. Their application and performance in three different imaging modes--integrated, selected and spectral image detection--are described. Electro-optical and microchannel-plate-based systems are contrasted. The analytical capabilities of solid-state pixel detectors--both charge coupled device (CCD) and complementary metal oxide semiconductor (CMOS) chips--are introduced. The Medipix/Timepix detector family is described as an example of a CMOS hybrid active pixel sensor. Alternative imaging methods for particle detection and their potential for future applications are investigated. Copyright © 2012 John Wiley & Sons, Ltd.

SRB Environment Evaluation and Analysis. Volume 2: RSRB Joint Filling Test/Analysis Improvements

NASA Technical Reports Server (NTRS)

Knox, E. C.; Woods, G. Hamilton

1991-01-01

Following the Challenger accident a very comprehensive solid rocket booster (SRB) redesign program was initiated. One objective of the program was to develop expertise at NASA/MSFC in the techniques for analyzing the flow of hot gases in the SRB joints. Several test programs were undertaken to provide a data base of joint performance with manufactured defects in the joints to allow hot gases to fill the joints. This data base was used also to develop the analytical techniques. Some of the test programs were Joint Environment Simulator (JES), Nozzle Joint Environment Simulator (NJES), Transient Pressure Test Article (TPTA), and Seventy-Pound Charge (SPC). In 1988 the TPTA test hardware was moved from the Utah site to MSFC and several RSRM tests were scheduled, to be followed by tests for the ASRM program. REMTECH Inc. supported these activities with pretest estimates of the flow conditions in the test joints, and post-test analysis and evaluation of the measurements. During this support REMTECH identified deficiencies in the gas-measurement instrumentation that existed in the TPTA hardware, made recommendations for its replacement, and identified improvements to the analytical tools used in the test support. Only one test was completed under the TPTA RSRM test program, and those scheduled for the ASRM were rescheduled to a time after the expiration of this contract. The attention of this effort was directed toward improvements in the analytical techniques in preparation for when the ASRM program begins.

Trends in Analytical Scale Separations.

ERIC Educational Resources Information Center

Jorgenson, James W.

1984-01-01

Discusses recent developments in the instrumentation and practice of analytical scale operations. Emphasizes detection devices and procedures in gas chromatography, liquid chromatography, electrophoresis, supercritical fluid chromatography, and field-flow fractionation. (JN)

Temperature field determination in slabs, circular plates and spheres with saw tooth heat generating sources

NASA Astrophysics Data System (ADS)

Diestra Cruz, Heberth Alexander

The Green's functions integral technique is used to determine the conduction heat transfer temperature field in flat plates, circular plates, and solid spheres with saw tooth heat generating sources. In all cases the boundary temperature is specified (Dirichlet's condition) and the thermal conductivity is constant. The method of images is used to find the Green's function in infinite solids, semi-infinite solids, infinite quadrants, circular plates, and solid spheres. The saw tooth heat generation source has been modeled using Dirac delta function and Heaviside step function. The use of Green's functions allows obtain the temperature distribution in the form of an integral that avoids the convergence problems of infinite series. For the infinite solid and the sphere, the temperature distribution is three-dimensional and in the cases of semi-infinite solid, infinite quadrant and circular plate the distribution is two-dimensional. The method used in this work is superior to other methods because it obtains elegant analytical or quasi-analytical solutions to complex heat conduction problems with less computational effort and more accuracy than the use of fully numerical methods.

Silicon carbide nanomaterial as a coating for solid-phase microextraction.

PubMed

Tian, Yu; Feng, Juanjuan; Wang, Xiuqin; Sun, Min; Luo, Chuannan

2018-01-26

Silicon carbide has excellent properties, such as corrosion resistance, high strength, oxidation resistance, high temperature, and so on. Based on these properties, silicon carbide was coated on stainless-steel wire and used as a solid-phase microextraction coating, and polycyclic aromatic hydrocarbons were employed as model analytes. Using gas chromatography, some important factors that affect the extraction efficiency were optimized one by one, and an analytical method was established. The analytical method showed wide linear ranges (0.1-30, 0.03-30, and 0.01-30 μg/L) with satisfactory correlation coefficients (0.9922-0.9966) and low detection limits (0.003-0.03 μg/L). To investigate the practical application of the method, rainwater and cigarette ash aqueous solution were collected as real samples for extraction and detection. The results indicate that silicon carbide has excellent application in the field of solid-phase microextraction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Metal-organic frameworks for analytical chemistry: from sample collection to chromatographic separation.

PubMed

Gu, Zhi-Yuan; Yang, Cheng-Xiong; Chang, Na; Yan, Xiu-Ping

2012-05-15

In modern analytical chemistry researchers pursue novel materials to meet analytical challenges such as improvements in sensitivity, selectivity, and detection limit. Metal-organic frameworks (MOFs) are an emerging class of microporous materials, and their unusual properties such as high surface area, good thermal stability, uniform structured nanoscale cavities, and the availability of in-pore functionality and outer-surface modification are attractive for diverse analytical applications. This Account summarizes our research on the analytical applications of MOFs ranging from sampling to chromatographic separation. MOFs have been either directly used or engineered to meet the demands of various analytical applications. Bulk MOFs with microsized crystals are convenient sorbents for direct application to in-field sampling and solid-phase extraction. Quartz tubes packed with MOF-5 have shown excellent stability, adsorption efficiency, and reproducibility for in-field sampling and trapping of atmospheric formaldehyde. The 2D copper(II) isonicotinate packed microcolumn has demonstrated large enhancement factors and good shape- and size-selectivity when applied to on-line solid-phase extraction of polycyclic aromatic hydrocarbons in water samples. We have explored the molecular sieving effect of MOFs for the efficient enrichment of peptides with simultaneous exclusion of proteins from biological fluids. These results show promise for the future of MOFs in peptidomics research. Moreover, nanosized MOFs and engineered thin films of MOFs are promising materials as novel coatings for solid-phase microextraction. We have developed an in situ hydrothermal growth approach to fabricate thin films of MOF-199 on etched stainless steel wire for solid-phase microextraction of volatile benzene homologues with large enhancement factors and wide linearity. Their high thermal stability and easy-to-engineer nanocrystals make MOFs attractive as new stationary phases to fabricate MOF-coated capillaries for high-resolution gas chromatography (GC). We have explored a dynamic coating approach to fabricate a MOF-coated capillary for the GC separation of important raw chemicals and persistent organic pollutants with high resolution and excellent selectivity. We have combined a MOF-coated fiber for solid-phase microextraction with a MOF-coated capillary for GC separation, which provides an effective MOF-based tandem molecular sieve platform for selective microextraction and high-resolution GC separation of target analytes in complex samples. Microsized MOFs with good solvent stability are attractive stationary phases for high-performance liquid chromatography (HPLC). These materials have shown high resolution and good selectivity and reproducibility in both the normal-phase HPLC separation of fullerenes and substituted aromatics on MIL-101 packed columns and position isomers on a MIL-53(Al) packed column and the reversed-phase HPLC separation of a wide range of analytes from nonpolar to polar and acidic to basic solutes. Despite the above achievements, further exploration of MOFs in analytical chemistry is needed. Especially, analytical application-oriented engineering of MOFs is imperative for specific applications.

Major advances in testing of dairy products: milk component and dairy product attribute testing.

PubMed

Barbano, D M; Lynch, J M

2006-04-01

Milk component analysis is relatively unusual in the field of quantitative analytical chemistry because an analytical test result determines the allocation of very large amounts of money between buyers and sellers of milk. Therefore, there is high incentive to develop and refine these methods to achieve a level of analytical performance rarely demanded of most methods or laboratory staff working in analytical chemistry. In the last 25 yr, well-defined statistical methods to characterize and validate analytical method performance combined with significant improvements in both the chemical and instrumental methods have allowed achievement of improved analytical performance for payment testing. A shift from marketing commodity dairy products to the development, manufacture, and marketing of value added dairy foods for specific market segments has created a need for instrumental and sensory approaches and quantitative data to support product development and marketing. Bringing together sensory data from quantitative descriptive analysis and analytical data from gas chromatography olfactometry for identification of odor-active compounds in complex natural dairy foods has enabled the sensory scientist and analytical chemist to work together to improve the consistency and quality of dairy food flavors.

Providing solid angle formalism for skyshine calculations

PubMed Central

Pahikkala, A. Jussi; Rising, Mary B.; McGinley, Patton H.

2010-01-01

We detail, derive and correct the technical use of the solid angle variable identified in formal guidance that relates skyshine calculations to dose‐equivalent rate. We further recommend it for use with all National Council on Radiation Protection and Measurements (NCRP), Institute of Physics and Engineering in Medicine (IPEM) and similar reports documented. In general, for beams of identical width which have different resulting areas, within ±1.0% maximum deviation the analytical pyramidal solution is 1.27 times greater than a misapplied analytical conical solution through all field sizes up to 40×40 cm2. Therefore, we recommend determining the exact results with the analytical pyramidal solution for square beams and the analytical conical solution for circular beams. PACS number(s): 87.52.‐g, 87.52.Df, 87.52.Tr, 87.53.‐j, 87.53.Bn, 87.53.Dq, 87.66.‐a, 89., 89.60.+x

An Integrated Hot-Stage Microscope-Direct Analysis in Real Time-Mass Spectrometry System for Studying the Thermal Behavior of Materials.

PubMed

Ashton, Gage P; Harding, Lindsay P; Parkes, Gareth M B

2017-12-19

This paper describes a new analytical instrument that combines a precisely temperature-controlled hot-stage with digital microscopy and Direct Analysis in Real Time-mass spectrometry (DART-MS) detection. The novelty of the instrument lies in its ability to monitor processes as a function of temperature through the simultaneous recording of images, quantitative color changes, and mass spectra. The capability of the instrument was demonstrated through successful application to four very varied systems including profiling an organic reaction, decomposition of silicone polymers, and the desorption of rhodamine B from an alumina surface. The multidimensional, real-time analytical data provided by this instrument allow for a much greater insight into thermal processes than could be achieved previously.

Needle-like instruments for steering through solid organs: A review of the scientific and patent literature.

PubMed

Scali, Marta; Pusch, Tim P; Breedveld, Paul; Dodou, Dimitra

2017-03-01

High accuracy and precision in reaching target locations inside the human body is necessary for the success of percutaneous procedures, such as tissue sample removal (biopsy), brachytherapy, and localized drug delivery. Flexible steerable needles may allow the surgeon to reach targets deep inside solid organs while avoiding sensitive structures (e.g. blood vessels). This article provides a systematic classification of possible mechanical solutions for three-dimensional steering through solid organs. A scientific and patent literature search of steerable instrument designs was conducted using Scopus and Web of Science Derwent Innovations Index patent database, respectively. First, we distinguished between mechanisms in which deflection is induced by the pre-defined shape of the instrument versus mechanisms in which an actuator changes the deflection angle of the instrument on demand. Second, we distinguished between mechanisms deflecting in one versus two planes. The combination of deflection method and number of deflection planes led to eight logically derived mechanical solutions for three-dimensional steering, of which one was dismissed because it was considered meaningless. Next, we classified the instrument designs retrieved from the scientific and patent literature into the identified solutions. We found papers and patents describing instrument designs for six of the seven solutions. We did not find papers or patents describing instruments that steer in one-plane on-demand via an actuator and in a perpendicular plane with a pre-defined deflection angle via a bevel tip or a pre-curved configuration.

Determination of organophosphorus pesticides in bovine tissue by an on-line coupled matrix solid-phase dispersion-solid phase extraction-high performance liquid chromatography with diode array detection method.

PubMed

Gutiérrez Valencia, Tania M; García de Llasera, Martha P

2011-09-28

A miniaturized method based on matrix solid-phase dispersion coupled to solid phase extraction and high performance liquid chromatography with diode array detection (MSPD-SPE-HPLC/DAD) was developed for the trace simultaneous determination of the following organophosphorus pesticides (OPPs) in bovine tissue: parathion-methyl, fenitrothion, parathion, chlorfenvinphos, diazinon, ethion, fenchlorphos, chlorpyrifos and carbophenothion. To perform the coupling between MSPD and SPE, 0.05 g of sample was dispersed with 0.2 g of C(18) silica sorbent and packed into a stainless steel cartridge containing 0.05 g of silica gel in the bottom. After a clean-up of high and medium polarity interferences with water and an acetonitrile:water mixture, the OPPs were desorbed from the MSPD cartridge with pure acetonitrile and directly transferred to a dynamic mixing chamber for dilution with water and preconcentration into an SPE 20 mm × 2.0 mm I.D. C(18) silica column. Subsequently, the OPPs were eluted on-line with the chromatographic mobile phase to the analytical column and the diode array detector for their separation and detection, respectively. The method was validated and yielded recovery values between 91% and 101% and precision values, expressed as relative standard deviations (RSD), which were less than or equal to 12%. Linearity was good and ranged from 0.5 to 10 μg g(-1), and the limits of detection of the OPPs were in the range of 0.04-0.25 μg g(-1). The method was satisfactorily applied to the analysis of real samples and is recommended for food control, research efforts when sample amounts are limited, and laboratories that have ordinary chromatographic instrumentation. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of the Antibiotic Oxytetracycline in Commercial Milk by Solid-Phase Extraction: A High-Performance Liquid Chromatography (HPLC) Experiment for Quantitative Instrumental Analysis

ERIC Educational Resources Information Center

Mei-Ratliff, Yuan

2012-01-01

Trace levels of oxytetracylcine spiked into commercial milk samples are extracted, cleaned up, and preconcentrated using a C[subscript 18] solid-phase extraction column. The extract is then analyzed by a high-performance liquid chromatography (HPLC) instrument equipped with a UV detector and a C[subscript 18] column (150 mm x 4.6 mm x 3.5 [mu]m).…

Buckling Testing and Analysis of Space Shuttle Solid Rocket Motor Cylinders

NASA Technical Reports Server (NTRS)

Weidner, Thomas J.; Larsen, David V.; McCool, Alex (Technical Monitor)

2002-01-01

A series of full-scale buckling tests were performed on the space shuttle Reusable Solid Rocket Motor (RSRM) cylinders. The tests were performed to determine the buckling capability of the cylinders and to provide data for analytical comparison. A nonlinear ANSYS Finite Element Analysis (FEA) model was used to represent and evaluate the testing. Analytical results demonstrated excellent correlation to test results, predicting the failure load within 5%. The analytical value was on the conservative side, predicting a lower failure load than was applied to the test. The resulting study and analysis indicated the important parameters for FEA to accurately predict buckling failure. The resulting method was subsequently used to establish the pre-launch buckling capability of the space shuttle system.

Flight qualified solid argon cooler for the BBXRT instrument. [Broad Band X Ray Telescope for ASTRO-1 payload

NASA Technical Reports Server (NTRS)

Cygnarowicz, Thomas A.; Schein, Michael E.; Lindauer, David A.; Scarlotti, Roger; Pederson, Robert

1990-01-01

A solid argon cooler (SAC) for attached Shuttle payloads has been developed and qualified to meet the need for low cost cooling of flight instruments to the temperature range of 60-120 K. The SACs have been designed and tested with the intent of flying them up to five times. Two coolers, as part of the Broad Band X-ray Telescope (BBXRT) instrument on the ASTRO-1 payload, are awaiting launch on Space Shuttle mission STS-35. This paper describes the design, testing and performance of the SAC and its vacuum maintenance system (VMS), used to maintain the argon as a solid during launch delays of up to 5 days. BBXRT cryogen system design features used to satisfy Shuttle safety requirements are discussed, along with SAC ground servicing equipment (GSE) and procedures used to fill, freeze and subcool the argon.

Star 48 solid rocket motor nozzle analyses and instrumented firings

NASA Technical Reports Server (NTRS)

Porter, R. L.

1986-01-01

The analyses and testing performed by NASA in support of an expanded and improved nozzle design data base for use by the U.S. solid rocket motor industry is presented. A production nozzle with a history of one ground failure and two flight failures was selected for analyses and testing. The stress analysis was performed with the Champion computer code developed by the U.S. Navy. Several improvements were made to the code. Strain predictions were made and compared to test data. Two short duration motor firings were conducted with highly instrumented nozzles. The first nozzle had 58 thermocouples, 66 strain gages, and 8 bondline pressure measurements. The second nozzle had 59 thermocouples, 68 strain measurements, and 8 bondline pressure measurements. Most of this instrumentation was on the nonmetallic parts, and provided significantly more thermal and strain data on the nonmetallic components of a nozzle than has been accumulated in a solid rocket motor test to date.

Potential sources of analytical bias and error in selected trace element data-quality analyses

USGS Publications Warehouse

Paul, Angela P.; Garbarino, John R.; Olsen, Lisa D.; Rosen, Michael R.; Mebane, Christopher A.; Struzeski, Tedmund M.

2016-09-28

Potential sources of analytical bias and error associated with laboratory analyses for selected trace elements where concentrations were greater in filtered samples than in paired unfiltered samples were evaluated by U.S. Geological Survey (USGS) Water Quality Specialists in collaboration with the USGS National Water Quality Laboratory (NWQL) and the Branch of Quality Systems (BQS).Causes for trace-element concentrations in filtered samples to exceed those in associated unfiltered samples have been attributed to variability in analytical measurements, analytical bias, sample contamination either in the field or laboratory, and (or) sample-matrix chemistry. These issues have not only been attributed to data generated by the USGS NWQL but have been observed in data generated by other laboratories. This study continues the evaluation of potential analytical bias and error resulting from matrix chemistry and instrument variability by evaluating the performance of seven selected trace elements in paired filtered and unfiltered surface-water and groundwater samples collected from 23 sampling sites of varying chemistries from six States, matrix spike recoveries, and standard reference materials.Filtered and unfiltered samples have been routinely analyzed on separate inductively coupled plasma-mass spectrometry instruments. Unfiltered samples are treated with hydrochloric acid (HCl) during an in-bottle digestion procedure; filtered samples are not routinely treated with HCl as part of the laboratory analytical procedure. To evaluate the influence of HCl on different sample matrices, an aliquot of the filtered samples was treated with HCl. The addition of HCl did little to differentiate the analytical results between filtered samples treated with HCl from those samples left untreated; however, there was a small, but noticeable, decrease in the number of instances where a particular trace-element concentration was greater in a filtered sample than in the associated unfiltered sample for all trace elements except selenium. Accounting for the small dilution effect (2 percent) from the addition of HCl, as required for the in-bottle digestion procedure for unfiltered samples, may be one step toward decreasing the number of instances where trace-element concentrations are greater in filtered samples than in paired unfiltered samples.The laboratory analyses of arsenic, cadmium, lead, and zinc did not appear to be influenced by instrument biases. These trace elements showed similar results on both instruments used to analyze filtered and unfiltered samples. The results for aluminum and molybdenum tended to be higher on the instrument designated to analyze unfiltered samples; the results for selenium tended to be lower. The matrices used to prepare calibration standards were different for the two instruments. The instrument designated for the analysis of unfiltered samples was calibrated using standards prepared in a nitric:hydrochloric acid (HNO3:HCl) matrix. The instrument designated for the analysis of filtered samples was calibrated using standards prepared in a matrix acidified only with HNO3. Matrix chemistry may have influenced the responses of aluminum, molybdenum, and selenium on the two instruments. The best analytical practice is to calibrate instruments using calibration standards prepared in matrices that reasonably match those of the samples being analyzed.Filtered and unfiltered samples were spiked over a range of trace-element concentrations from less than 1 to 58 times ambient concentrations. The greater the magnitude of the trace-element spike concentration relative to the ambient concentration, the greater the likelihood spike recoveries will be within data control guidelines (80–120 percent). Greater variability in spike recoveries occurred when trace elements were spiked at concentrations less than 10 times the ambient concentration. Spike recoveries that were considerably lower than 90 percent often were associated with spiked concentrations substantially lower than what was present in the ambient sample. Because the main purpose of spiking natural water samples with known quantities of a particular analyte is to assess possible matrix effects on analytical results, the results of this study stress the importance of spiking samples at concentrations that are reasonably close to what is expected but sufficiently high to exceed analytical variability. Generally, differences in spike recovery results between paired filtered and unfiltered samples were minimal when samples were analyzed on the same instrument.Analytical results for trace-element concentrations in ambient filtered and unfiltered samples greater than 10 and 40 μg/L, respectively, were within the data-quality objective for precision of ±25 percent. Ambient trace-element concentrations in filtered samples greater than the long-term method detection limits but less than 10 μg/L failed to meet the data-quality objective for precision for at least one trace element in about 54 percent of the samples. Similarly, trace-element concentrations in unfiltered samples greater than the long-term method detection limits but less than 40 μg/L failed to meet this data-quality objective for at least one trace-element analysis in about 58 percent of the samples. Although, aluminum and zinc were particularly problematic, limited re-analyses of filtered and unfiltered samples appeared to improve otherwise failed analytical precision.The evaluation of analytical bias using standard reference materials indicate a slight low bias for results for arsenic, cadmium, selenium, and zinc. Aluminum and molybdenum show signs of high bias. There was no observed bias, as determined using the standard reference materials, during the analysis of lead.

GFSSP Training Course Lectures

NASA Technical Reports Server (NTRS)

Majumdar, Alok K.

2008-01-01

GFSSP has been extended to model conjugate heat transfer Fluid Solid Network Elements include: a) Fluid nodes and Flow Branches; b) Solid Nodes and Ambient Nodes; c) Conductors connecting Fluid-Solid, Solid-Solid and Solid-Ambient Nodes. Heat Conduction Equations are solved simultaneously with Fluid Conservation Equations for Mass, Momentum, Energy and Equation of State. The extended code was verified by comparing with analytical solution for simple conduction-convection problem The code was applied to model: a) Pressurization of Cryogenic Tank; b) Freezing and Thawing of Metal; c) Chilldown of Cryogenic Transfer Line; d) Boil-off from Cryogenic Tank.

Measuring Fluctuating Pressure Levels and Vibration Response in a Jet Plume

NASA Technical Reports Server (NTRS)

Osterholt, Douglas J.; Knox, Douglas M.

2011-01-01

The characterization of loads due to solid rocket motor plume impingement allows for moreaccurate analyses of components subjected to such an environment. Typically, test verification of predicted loads due to these conditions is widely overlooked or unsuccessful. ATA Engineering, Inc., performed testing during a solid rocket motor firing to obtain acceleration and pressure responses in the hydrodynamic field surrounding the jet plume. The test environment necessitated a robust design to facilitate measurements being made in close proximity to the jet plume. This paper presents the process of designing a test fixture and an instrumentation package that could withstand the solid rocket plume environment and protect the required instrumentation.

Measuring the Internal Environment of Solid Rocket Motors During Ignition

NASA Technical Reports Server (NTRS)

Weisenberg, Brent; Smith, Doug; Speas, Kyle; Corliss, Adam

2003-01-01

A new instrumentation system has been developed to measure the internal environment of solid rocket test motors during motor ignition. The system leverages conventional, analog gages with custom designed, electronics modules to provide safe, accurate, high speed data acquisition capability. To date, the instrumentation system has been demonstrated in a laboratory environment and on subscale static fire test motors ranging in size from 5-inches to 24-inches in diameter. Ultimately, this system is intended to be installed on a full-scale Reusable Solid Rocket Motor. This paper explains the need for the data, the components and capabilities of the system, and the test results.

Hydrogen Isotopic Composition of Water in the Martian Atmosphere and Released from Rocknest Fines

NASA Technical Reports Server (NTRS)

Leshin, L. A.; Webster, C. R.; Mahaffy, P. R.; Flesh, G. J.; Christensen, L. E.; Stern, J. C.; Franz, H. B.; McAdam, A. C.; Niles, P. B.; Archer, P. B., Jr.;

Determination of trace zinc in seawater by coupling solid phase extraction and fluorescence detection in the Lab-On-Valve format.

PubMed

Grand, Maxime M; Chocholouš, Petr; Růžička, Jarda; Solich, Petr; Measures, Christopher I

2016-06-07

By virtue of their compactness, long-term stability, minimal reagent consumption and robustness, miniaturized sequential injection instruments are well suited for automation of assays onboard research ships. However, in order to reach the sensitivity and limit of detection required for open-ocean determinations of trace elements, it is necessary to preconcentrate the analyte prior its derivatization and subsequent detection by fluorescence. In this work, a novel method for the determination of dissolved zinc (Zn) at subnanomolar levels in seawater is described. The proposed method combines, for the first time, automated matrix removal, extraction of the target element, and fluorescence detection within a miniaturized flow manifold, based on the Lab-On-Valve (LOV) concept. The key feature of the microfluidic manipulation of the sample is flow programming, designed to pass sample through a mini-column where the target analyte and other complexable cations are retained, while the seawater matrix is washed out. Next, zinc is eluted and merged with a Zn selective fluorescent probe (FluoZin-3) at the confluence point of the LOV central channel using two high-precision stepper motor driven pumps that are operated in concert. Finally, the thus formed Zn complex is transported to the LOV flow cell for selective fluorescence measurement. This work describes the characterization and optimization of the method including Solid Phase Extraction using the Toyopearl AF-Chelate-650M resin, and detailed assay protocol controlled by a commercially available software and instrument. The proposed method features a LOD of 0.02 nM, high precision (<3% at 0.1 and 2 nM Zn levels), an assay cycle of 13 min and a reagent consumption of 150 μL FluoZin-3 per sample, which makes the method highly suitable for oceanographic shipboard analysis. The accuracy of the method has been validated through the analysis of seawater reference standards and comparison with ICP-MS determinations on seawater samples collected in the upper 1300 m of the subtropical south Indian Ocean. This work confirms that integration of sample pretreatment with optical detection in the LOV format offers a widely applicable approach to trace analysis of seawater. Copyright © 2016. Published by Elsevier B.V.

Analytical application of solid contact ion-selective electrodes for determination of copper and nitrate in various food products and drinking water.

PubMed

Wardak, Cecylia; Grabarczyk, Malgorzata

2016-08-02

A simple, fast and cheap method for monitoring copper and nitrate in drinking water and food products using newly developed solid contact ion-selective electrodes is proposed. Determination of copper and nitrate was performed by application of multiple standard additions technique. The reliability of the obtained results was assessed by comparing them using the anodic stripping voltammetry or spectrophotometry for the same samples. In each case, satisfactory agreement of the results was obtained, which confirms the analytical usefulness of the constructed electrodes.

What's the Bottom Line

EPA Science Inventory

Advances in analytical instrumentation have not only increased the number and types of chemicals measured, but reduced the quantitation limits, allowing these chemicals to be detected at progressively lower concentrations in various environmental matrices. Such analytical advanc...

Accurate mass measurements and their appropriate use for reliable analyte identification.

PubMed

Godfrey, A Ruth; Brenton, A Gareth

2012-09-01

Accurate mass instrumentation is becoming increasingly available to non-expert users. This data can be mis-used, particularly for analyte identification. Current best practice in assigning potential elemental formula for reliable analyte identification has been described with modern informatic approaches to analyte elucidation, including chemometric characterisation, data processing and searching using facilities such as the Chemical Abstracts Service (CAS) Registry and Chemspider.

An Integrated Instrumentation System for Velocity, Concentration and Mass Flow Rate Measurement of Solid Particles Based on Electrostatic and Capacitance Sensors.

PubMed

Li, Jian; Kong, Ming; Xu, Chuanlong; Wang, Shimin; Fan, Ying

2015-12-10

The online and continuous measurement of velocity, concentration and mass flow rate of pneumatically conveyed solid particles for the high-efficiency utilization of energy and raw materials has become increasingly significant. In this paper, an integrated instrumentation system for the velocity, concentration and mass flow rate measurement of dense phase pneumatically conveyed solid particles based on electrostatic and capacitance sensorsis developed. The electrostatic sensors are used for particle mean velocity measurement in combination with the cross-correlation technique, while the capacitance sensor with helical surface-plate electrodes, which has relatively homogeneous sensitivity distribution, is employed for the measurement of particle concentration and its capacitance is measured by an electrostatic-immune AC-based circuit. The solid mass flow rate can be further calculated from the measured velocity and concentration. The developed instrumentation system for velocity and concentration measurement is verified and calibrated on a pulley rig and through static experiments, respectively. Finally the system is evaluated with glass beads on a gravity-fed rig. The experimental results demonstrate that the system is capable of the accurate solid mass flow rate measurement, and the relative error is within -3%-8% for glass bead mass flow rates ranging from 0.13 kg/s to 0.9 kg/s.

Cellular telephone-based radiation sensor and wide-area detection network

DOEpatents

Craig, William W [Pittsburg, CA; Labov, Simon E [Berkeley, CA

2006-12-12

A network of radiation detection instruments, each having a small solid state radiation sensor module integrated into a cellular phone for providing radiation detection data and analysis directly to a user. The sensor module includes a solid-state crystal bonded to an ASIC readout providing a low cost, low power, light weight compact instrument to detect and measure radiation energies in the local ambient radiation field. In particular, the photon energy, time of event, and location of the detection instrument at the time of detection is recorded for real time transmission to a central data collection/analysis system. The collected data from the entire network of radiation detection instruments are combined by intelligent correlation/analysis algorithms which map the background radiation and detect, identify and track radiation anomalies in the region.

Cellular telephone-based wide-area radiation detection network

DOEpatents

Craig, William W [Pittsburg, CA; Labov, Simon E [Berkeley, CA

2009-06-09

A network of radiation detection instruments, each having a small solid state radiation sensor module integrated into a cellular phone for providing radiation detection data and analysis directly to a user. The sensor module includes a solid-state crystal bonded to an ASIC readout providing a low cost, low power, light weight compact instrument to detect and measure radiation energies in the local ambient radiation field. In particular, the photon energy, time of event, and location of the detection instrument at the time of detection is recorded for real time transmission to a central data collection/analysis system. The collected data from the entire network of radiation detection instruments are combined by intelligent correlation/analysis algorithms which map the background radiation and detect, identify and track radiation anomalies in the region.

Implementation of picoSpin Benchtop NMR Instruments into Organic Chemistry Teaching Laboratories through Spectral Analysis of Fischer Esterification Products

ERIC Educational Resources Information Center

Yearty, Kasey L.; Sharp, Joseph T.; Meehan, Emma K.; Wallace, Doyle R.; Jackson, Douglas M.; Morrison, Richard W.

2017-01-01

[Superscript 1]H NMR analysis is an important analytical technique presented in introductory organic chemistry courses. NMR instrument access is limited for undergraduate organic chemistry students due to the size of the instrument, price of NMR solvents, and the maintenance level required for instrument upkeep. The University of Georgia Chemistry…

42 CFR 493.1252 - Standard: Test systems, equipment, instruments, reagents, materials, and supplies.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 42 Public Health 5 2010-10-01 2010-10-01 false Standard: Test systems, equipment, instruments... REQUIREMENTS Quality System for Nonwaived Testing Analytic Systems § 493.1252 Standard: Test systems, equipment...) Temperature. (3) Humidity. (4) Protection of equipment and instruments from fluctuations and interruptions in...

Serendipity: Genesis of the Electrochemical Instrumentation at Princeton Applied Research Corporation

ERIC Educational Resources Information Center

Flato, J. B.

2007-01-01

Princeton Applied Research Corporation (PAR) was a small electronic instrument company in early 1960s but once they entered electrochemistry they were very successful. Since then they have developed and designed successful instruments with their tremendous knowledge and have made great contribution to the field of analytical chemistry.

Emission quantification using the tracer gas dispersion method: The influence of instrument, tracer gas species and source simulation.

PubMed

Delre, Antonio; Mønster, Jacob; Samuelsson, Jerker; Fredenslund, Anders M; Scheutz, Charlotte

2018-09-01

The tracer gas dispersion method (TDM) is a remote sensing method used for quantifying fugitive emissions by relying on the controlled release of a tracer gas at the source, combined with concentration measurements of the tracer and target gas plumes. The TDM was tested at a wastewater treatment plant for plant-integrated methane emission quantification, using four analytical instruments simultaneously and four different tracer gases. Measurements performed using a combination of an analytical instrument and a tracer gas, with a high ratio between the tracer gas release rate and instrument precision (a high release-precision ratio), resulted in well-defined plumes with a high signal-to-noise ratio and a high methane-to-tracer gas correlation factor. Measured methane emission rates differed by up to 18% from the mean value when measurements were performed using seven different instrument and tracer gas combinations. Analytical instruments with a high detection frequency and good precision were established as the most suitable for successful TDM application. The application of an instrument with a poor precision could only to some extent be overcome by applying a higher tracer gas release rate. A sideward misplacement of the tracer gas release point of about 250m resulted in an emission rate comparable to those obtained using a tracer gas correctly simulating the methane emission. Conversely, an upwind misplacement of about 150m resulted in an emission rate overestimation of almost 50%, showing the importance of proper emission source simulation when applying the TDM. Copyright © 2018 Elsevier B.V. All rights reserved.

Assessment of priority pesticides, degradation products, and pesticide adjuvants in groundwaters and top soils from agricultural areas of the Ebro river basin.

PubMed

Hildebrandt, Alain; Lacorte, Sílvia; Barceló, Damià

2007-02-01

Gas chromatography-mass spectrometry (GC/MS) was employed for the determination of 30 widely used pesticides including various transformation products and alkylphenols in water and agricultural soils with the aim of assessing the impact of these compounds in agricultural soils and the underlying aquifer. The extraction, clean-up, and analytical procedures were optimized for both water and soil samples to provide a highly robust method capable of determining target analytes at the ppb-ppt level with high precision. For water samples, different solid-phase extraction cartridges and conditions were optimized; similarly, pressurized liquid extraction conditions were tested to provide interference-free extracts and high sensitivity. Instrumental LODs of 3-4 pg were obtained. The multi-residue extraction procedures were applied to the analysis of groundwaters and agricultural soils from the Ebro river basin (NE Spain). Most ubiquitous herbicides detected were triazines but some acetanilides and organophosphorus pesticides were also found; the pesticide additive tributylphosphate was found in all water samples. Levels varied between 0.57 and 5.37 microg/L in groundwater, whereas nonylphenol was the sole compound detected in soil. Alkylphenols are used as adjuvants in pesticide formulations and are present in sludges employed as soil fertilizers. Occurrence was found to be similar to other environmental studies.

Determination of Human-Health Pharmaceuticals in Filtered Water by Chemically Modified Styrene-Divinylbenzene Resin-Based Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

USGS Publications Warehouse

Furlong, Edward T.; Werner, Stephen L.; Anderson, Bruce D.; Cahill, Jeffery D.

2008-01-01

In 1999, the Methods Research and Development Program of the U.S. Geological Survey National Water Quality Laboratory began the process of developing a method designed to identify and quantify human-health pharmaceuticals in four filtered water-sample types: reagent water, ground water, surface water minimally affected by human contributions, and surface water that contains a substantial fraction of treated wastewater. Compounds derived from human pharmaceutical and personal-care product use, which enter the environment through wastewater discharge, are a newly emerging area of concern; this method was intended to fulfill the need for a highly sensitive and highly selective means to identify and quantify 14 commonly used human pharmaceuticals in filtered-water samples. The concentrations of 12 pharmaceuticals are reported without qualification; the concentrations of two pharmaceuticals are reported as estimates because long-term reagent-spike sample recoveries fall below acceptance criteria for reporting concentrations without qualification. The method uses a chemically modified styrene-divinylbenzene resin-based solid-phase extraction (SPE) cartridge for analyte isolation and concentration. For analyte detection and quantitation, an instrumental method was developed that used a high-performance liquid chromatography/mass spectrometry (HPLC/MS) system to separate the pharmaceuticals of interest from each other and coextracted material. Immediately following separation, the pharmaceuticals are ionized by electrospray ionization operated in the positive mode, and the positive ions produced are detected, identified, and quantified using a quadrupole mass spectrometer. In this method, 1-liter water samples are first filtered, either in the field or in the laboratory, using a 0.7-micrometer (um) nominal pore size glass-fiber filter to remove suspended solids. The filtered samples then are passed through cleaned and conditioned SPE cartridges at a rate of about 15 milliliters per minute. Excess water is eliminated from the cartridge sorbent bed by passing air through the cartridges, and the analytes retained on the SPE bed are eluted from the cartridge sequentially, first with methanol, followed by acidified methanol, and combined in collection tubes. This sample extract then is reduced from about 10 milliliters (mL) to about 0.1 mL (or 100 microliters) under a stream of purified nitrogen gas with the collection tubes in a heated (40 degrees C) water bath. The reduced extracts then are fortified with an internal standard solution (when using internal standard quantitation), brought to a final volume of 1 mL with an aqueous ammonium formate buffer solution, and filtered through a 0.2-um Teflon syringe filter as they are transferred into vials for instrumental analysis. Instrumental analysis by the HPLC/MS procedure permits determination of individual pharmaceutical concentrations from 0.005 to 1.0 microgram per liter, based on the lowest and the highest calibration standards routinely used. The reporting levels for this method are compound dependent, and have been experimentally determined based on the precision of quantitation of compounds from eight fortified organic-free water samples in single-operator experiments. The method detection limits and interim reporting levels for the compounds determined by this method were calculated from recoveries of the pharmaceuticals from reagent-water samples amended at 0.05 microgram per liter, and ranged between 0.0069 and 0.0142 microgram per liter, and 0.015 and 0.10 microgram per liter, respectively. Concentrations for 12 compounds are reported without qualification, and for two compounds are reported as qualified estimates. After initial development, the method was applied to more than 1,800 surface-, ground-, and wastewater samples from 2002 to 2005 and documented in a number of published studies. This research application of the method provided the opportunity to collect a l

Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry.

PubMed

Lehmann, Sabrina; Kieliba, Tobias; Beike, Justus; Thevis, Mario; Mercer-Chalmers-Bender, Katja

2017-10-01

A detailed description is given of the development and validation of a fully automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method capable of detecting 90 central-stimulating new psychoactive substances (NPS) and 5 conventional amphetamine-type stimulants (amphetamine, 3,4-methylenedioxy-methamphetamine (MDMA), 3,4-methylenedioxy-amphetamine (MDA), 3,4-methylenedioxy-N-ethyl-amphetamine (MDEA), methamphetamine) in serum. The aim was to apply the validated method to forensic samples. The preparation of 150μL of serum was performed by an Instrument Top Sample Preparation (ITSP)-SPE with mixed mode cation exchanger cartridges. The extracts were directly injected into an LC-MS/MS system, using a biphenyl column and gradient elution with 2mM ammonium formate/0.1% formic acid and acetonitrile/0.1% formic acid as mobile phases. The chromatographic run time amounts to 9.3min (including re-equilibration). The total cycle time is 11min, due to the interlacing between sample preparation and analysis. The method was fully validated using 69 NPS and five conventional amphetamine-type stimulants, according to the guidelines of the Society of Toxicological and Forensic Chemistry (GTFCh). The guidelines were fully achieved for 62 analytes (with a limit of detection (LOD) between 0.2 and 4μg/L), whilst full validation was not feasible for the remaining 12 analytes. For the fully validated analytes, the method achieved linearity in the 5μg/L (lower limit of quantification, LLOQ) to 250μg/L range (coefficients of determination>0.99). Recoveries for 69 of these compounds were greater than 50%, with relative standard deviations≤15%. The validated method was then tested for its capability in detecting a further 21 NPS, thus totalling 95 tested substances. An LOD between 0.4 and 1.6μg/L was obtained for these 21 additional qualitatively-measured substances. The method was subsequently successfully applied to 28 specimens from routine forensic case work, of which 7 samples were determined to be positive for NPS consumption. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of an ultra-high-pressure liquid chromatography-tandem mass spectrometry multi-residue sulfonamide method and its application to water, manure slurry, and soils from swine rearing facilities.

PubMed

Shelver, Weilin L; Hakk, Heldur; Larsen, Gerald L; DeSutter, Thomas M; Casey, Francis X M

2010-02-19

An analytical method was developed using ultra-high-pressure liquid chromatography-triple quadrupole-tandem mass spectrometry (UHPLC-TQ-MS/MS) to simultaneously analyze 14 sulfonamides (SA) in 6 min. Despite the rapidity of the assay the system was properly re-equilibrated in this time. No carryover was observed even after high analyte concentrations. The instrumental detection limit based on signal-to-noise ratio (S/N)>3, was below 1 pg/microL (5 pg on column) for all SAs except sulfachloropyridazine. Surface water, ground water, soil, and slurry manure contained in storage ponds in and around swine [Sus scrofa domesticus] rearing facilities were analyzed. Sample cleanup for ground water and surface water included using solid phase extraction (SPE) using Oasis hydrophilic-lipophilic balance (HLB) cartridges. The soil and slurry manure required tandem strong anion exchange (SAX) and HLB solid phase extraction cartridges for sample cleanup. With few exceptions, the recoveries ranged from 60 to 100% for all matrices. The minimum detectable levels were below 2.0 ng/L for water, 30 ng/L for slurry manure, and 45 ng/kg for soil except for sulfachloropyridazine. The coefficient of variation (CV) was within 20% for most of the compounds analyzed. Using this method, sulfamethazine concentrations of 2250-5060 ng/L, sulfamethoxazole concentrations of 108-1.47 x 10(6)ng/L, and sulfathiazole concentrations of 785-1700 ng/L were found in the slurry manure. Sulfadimethoxine (2.0-32 ng/L), sulfamethazine (2.0-5.1 ng/L), and sulfamethoxazole (20.5-43.0 ng/L) were found in surface water and ground water. In top soil (0-15 cm), sulfamethazine ranged 34.5-663 ng/kg dry weight in those locations that received slurry manure as a nutrient; no SAs were found in the soil depths between 46 and 61 cm. The speed makes the method practical for medium to high throughput applications. The sensitivity and positive analyte identification make the method suitable for the demanding requirements for real world applications. Published by Elsevier B.V.

Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Schultz, John R.; Clarke, Mark S.

2007-01-01

Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

Development of Analytical Protocols For Organics and Isotopes Analysis on the 2009 MARS Science Laboratory.

NASA Technical Reports Server (NTRS)

Mahaffy, P. R.

2006-01-01

The Mars Science Laboratory, under development for launch in 2009, is designed explore and quantitatively asses a local region on Mars as a potential habitat for present or past life. Its ambitious goals are to (1) assess the past or present biological potential of the target environment, (2) to characterize the geology and geochemistry at the MSL landing site, and (3) to investigate planetary processes that influence habitability. The planned capabilities of the rover payload will enable a comprehensive search for organic molecules, a determination of definitive mineralogy of sampled rocks and fines, chemical and isotopic analysis of both atmospheric and solid samples, and precision isotope measurements of several volatile elements. A range of contact and remote surface and subsurface survey tools will establish context for these measurements and will facilitate sample identification and selection. The Sample Analysis at Mars (SAM) suite of MSL addresses several of the mission's core measurement goals. It includes a gas chromatograph, a mass spectrometer, and a tunable laser spectrometer. These instruments will be designed to analyze either atmospheric samples or gases extracted from solid phase samples such as rocks and fines. We will describe the range of measurement protocols under development and study by the SAM engineering and science teams for use on the surface of Mars.

MS-Based Analytical Techniques: Advances in Spray-Based Methods and EI-LC-MS Applications

PubMed Central

Medina, Isabel; Cappiello, Achille; Careri, Maria

2018-01-01

Mass spectrometry is the most powerful technique for the detection and identification of organic compounds. It can provide molecular weight information and a wealth of structural details that give a unique fingerprint for each analyte. Due to these characteristics, mass spectrometry-based analytical methods are showing an increasing interest in the scientific community, especially in food safety, environmental, and forensic investigation areas where the simultaneous detection of targeted and nontargeted compounds represents a key factor. In addition, safety risks can be identified at the early stage through online and real-time analytical methodologies. In this context, several efforts have been made to achieve analytical instrumentation able to perform real-time analysis in the native environment of samples and to generate highly informative spectra. This review article provides a survey of some instrumental innovations and their applications with particular attention to spray-based MS methods and food analysis issues. The survey will attempt to cover the state of the art from 2012 up to 2017. PMID:29850370

Reflectance Infrared Spectroscopy on Operating Surface Acoustic Wave Chemical Sensors During Exposure to Gas-Phase Analytes

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

Hierlemann, A.; Hill, M.; Ricco, A.J.

We have developed instrumentation to enable the combination of surface acoustic wave (SAW) sensor measurements with direct, in-situ molecular spectroscopic measurements to understand the response of the SAW sensors with respect to the interfacial chemistry of surface-confined sensing films interacting with gas-phase analytes. Specifically, the instrumentation and software was developed to perform in-situ Fourier-transform infrared external-reflectance spectroscopy (FTIR-ERS) on operating SAW devices during dosing of their chemically modified surfaces with analytes. By probing the surface with IR spectroscopy during gas exposure, it is possible to understand in unprecedented detail the interaction processes between the sorptive SAW coatings and the gaseousmore » analyte molecules. In this report, we provide details of this measurement system, and also demonstrate the utility of these combined measurements by characterizing the SAW and FTIR-ERS responses of organic thin-film sensor coatings interacting with gas-phase analytes.« less

Effect of Binding Components in Complex Sample Matrices on Recovery in Direct Immersion Solid-Phase Microextraction: Friends or Foe?

PubMed

Alam, Md Nazmul; Pawliszyn, Janusz

2018-02-20

The development of matrix compatible coatings for solid-phase microextraction (SPME) has enabled direct extraction of analytes from complex sample matrices. The direct immersion (DI) mode of SPME when utilized in conjunction with such extraction phases facilitates extraction of a wide range of analytes from complex matrices without the incurrence of fouling or coating saturation. In this work, mathematical models and computational simulations were employed to investigate the effect of binding components present in complex samples on the recovery of small molecules varying in logP for extractions carried out using the direct immersion approach. The presented findings corroborate that the studied approach indeed enables the extraction of both polar and nonpolar analytes from complex matrices, provided a suitable sorbent is employed. Further results indicated that, in certain cases, the kinetics of extraction of a given analyte in its free form might be dependent on the desorption kinetics of their bound form from matrix components, which might lower total recoveries of analytes with high affinity for the matrix. However, the binding of analytes to matrix components also enables SPME to extract a balanced quantity of different logP analytes, facilitated by multiphase equilibria, with a single extraction device.

Method and apparatus for optimized sampling of volatilizable target substances

DOEpatents

Lindgren, Eric R.; Phelan, James M.

2002-01-01

An apparatus for capturing, from gases such as soil gas, target analytes. Target analytes may include emanations from explosive materials or from residues of explosive materials. The apparatus employs principles of sorption common to solid phase microextraction, and is best used in conjunction with analysis means such as a gas chromatograph. To sorb target analytes, the apparatus functions using various sorptive structures to capture target analyte. Depending upon the embodiment, those structures may include 1) a conventional solid-phase microextraction (SPME) fiber, 2) a SPME fiber suspended in a capillary tube (with means provided for moving gases through the capillary tube so that the gases come into close proximity to the suspended fiber), and 3) a capillary tube including an interior surface on which sorptive material (similar to that on the surface of a SPME fiber) is supported (along with means for moving gases through the capillary tube so that the gases come into close proximity to the sorptive material). In one disclosed embodiment, at least one such sorptive structure is associated with an enclosure including an opening in communication with the surface of a soil region potentially contaminated with buried explosive material such as unexploded ordnance. Emanations from explosive materials can pass into and accumulate in the enclosure where they are sorbed by the sorptive structures. Also disclosed is the use of heating means such as microwave horns to drive target analytes into the soil gas from solid and liquid phase components of the soil.

Micro-focused ultrasonic solid-liquid extraction (muFUSLE) combined with HPLC and fluorescence detection for PAHs determination in sediments: optimization and linking with the analytical minimalism concept.

PubMed

Capelo, J L; Galesio, M M; Felisberto, G M; Vaz, C; Pessoa, J Costa

2005-06-15

Analytical minimalism is a concept that deals with the optimization of all stages of an analytical procedure so that it becomes less time, cost, sample, reagent and energy consuming. The guide-lines provided in the USEPA extraction method 3550B recommend the use of focused ultrasound (FU), i.e., probe sonication, for the solid-liquid extraction of Polycyclic Aromatic Hydrocarbons, PAHs, but ignore the principle of analytical minimalism. The problems related with the dead sonication zones, often present when high volumes are sonicated with probe, are also not addressed. In this work, we demonstrate that successful extraction and quantification of PAHs from sediments can be done with low sample mass (0.125g), low reagent volume (4ml), short sonication time (3min) and low sonication amplitude (40%). Two variables are here particularly taken into account for total extraction: (i) the design of the extraction vessel and (ii) the solvent used to carry out the extraction. Results showed PAHs recoveries (EPA priority list) ranged between 77 and 101%, accounting for more than 95% for most of the PAHs here studied, as compared with the values obtained after soxhlet extraction. Taking into account the results reported in this work we recommend a revision of the EPA guidelines for PAHs extraction from solid matrices with focused ultrasound, so that these match the analytical minimalism concept.

Determination of Total Solids and Ash in Algal Biomass: Laboratory Analytical Procedure (LAP)

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

Van Wychen, Stefanie; Laurens, Lieve M. L.

2016-01-13

This procedure describes the methods used to determine the amount of moisture or total solids present in a freeze-dried algal biomass sample, as well as the ash content. A traditional convection oven drying procedure is covered for total solids content, and a dry oxidation method at 575 deg. C is covered for ash content.

Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

PubMed

Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

2015-01-01

A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

The MIND PALACE: A Multi-Spectral Imaging and Spectroscopy Database for Planetary Science

NASA Astrophysics Data System (ADS)

Eshelman, E.; Doloboff, I.; Hara, E. K.; Uckert, K.; Sapers, H. M.; Abbey, W.; Beegle, L. W.; Bhartia, R.

2017-12-01

The Multi-Instrument Database (MIND) is the web-based home to a well-characterized set of analytical data collected by a suite of deep-UV fluorescence/Raman instruments built at the Jet Propulsion Laboratory (JPL). Samples derive from a growing body of planetary surface analogs, mineral and microbial standards, meteorites, spacecraft materials, and other astrobiologically relevant materials. In addition to deep-UV spectroscopy, datasets stored in MIND are obtained from a variety of analytical techniques obtained over multiple spatial and spectral scales including electron microscopy, optical microscopy, infrared spectroscopy, X-ray fluorescence, and direct fluorescence imaging. Multivariate statistical analysis techniques, primarily Principal Component Analysis (PCA), are used to guide interpretation of these large multi-analytical spectral datasets. Spatial co-referencing of integrated spectral/visual maps is performed using QGIS (geographic information system software). Georeferencing techniques transform individual instrument data maps into a layered co-registered data cube for analysis across spectral and spatial scales. The body of data in MIND is intended to serve as a permanent, reliable, and expanding database of deep-UV spectroscopy datasets generated by this unique suite of JPL-based instruments on samples of broad planetary science interest.

Solid and Gaseous Fuels.

ERIC Educational Resources Information Center

Schultz, Hyman; And Others

1989-01-01

This review covers methods of sampling, analyzing, and testing coal, coke, and coal-derived solids and methods for the chemical, physical, and instrumental analyses of gaseous fuels. The review covers from October 1986, to September 1988. (MVL)

A Single-Phase Analytic Equation of State for Solid Polyurea and Polyurea Aerogels

NASA Astrophysics Data System (ADS)

Whitworth, Nicholas; Lambourn, Brian

2017-06-01

Commercially available polymers are commonly used as impactors in high explosive gas-gun experiments. This paper presents a relatively simple, single-phase, analytic equation of state (EoS) for solid polyurea and polyurea aerogels suitable for use in hydrocode simulations. An exponential shock velocity-particle velocity relation is initially fit to available Hugoniot data on the solid material, which has a density of 1.13 g/cm3. This relation is then converted to a finite strain relation along the principal isentrope, which is used as the reference curve for a Mie-Gruneisen form of EoS with an assumed form for the variation of Gruneisen Γ with specific volume. Using the solid EoS in conjunction with the Snowplough model for porosity, experimental data on the shock response of solid polyurea and polyurea aerogels with initial densities of 0.20 and 0.35 g/cm3 can be reproduced to a reasonable degree of accuracy. A companion paper at this conference describes the application of this and other EoS in modelling shock-release-reshock gas-gun experiments on the insensitive high explosive PBX 9502.

Shipboard Analytical Capabilities on the Renovated JOIDES Resolution, IODP Riserless Drilling Vessel

NASA Astrophysics Data System (ADS)

Blum, P.; Foster, P.; Houpt, D.; Bennight, C.; Brandt, L.; Cobine, T.; Crawford, W.; Fackler, D.; Fujine, K.; Hastedt, M.; Hornbacher, D.; Mateo, Z.; Moortgat, E.; Vasilyev, M.; Vasilyeva, Y.; Zeliadt, S.; Zhao, J.

2008-12-01

The JOIDES Resolution (JR) has conducted 121 scientific drilling expeditions during the Ocean Drilling Program (ODP) and the first phase of the Integrated Ocean Drilling Program (IODP) (1983-2006). The vessel and scientific systems have just completed an NSF-sponsored renovation (2005-2008). Shipboard analytical systems have been upgraded, within funding constraints imposed by market driven vessel conversion cost increases, to include: (1) enhanced shipboard analytical services including instruments and software for sampling and the capture of chemistry, physical properties, and geological data; (2) new data management capabilities built around a laboratory information management system (LIMS), digital asset management system, and web services; (3) operations data services with enhanced access to navigation and rig instrumentation data; and (4) a combination of commercial and home-made user applications for workflow- specific data extractions, generic and customized data reporting, and data visualization within a shipboard production environment. The instrumented data capture systems include a new set of core loggers for rapid and non-destructive acquisition of images and other physical properties data from drill cores. Line-scan imaging and natural gamma ray loggers capture data at unprecedented quality due to new and innovative designs. Many instruments used to characterize chemical compounds of rocks, sediments, and interstitial fluids were upgraded with the latest technology. The shipboard analytical environment features a new and innovative framework (DESCinfo) and application (DESClogik) for capturing descriptive and interpretive data from geological sub-domains such as sedimentology, petrology, paleontology, structural geology, stratigraphy, etc. This system fills a long-standing gap by providing a global database, controlled vocabularies and taxa name lists with version control, a highly configurable spreadsheet environment for data capture, and visualization of context data collected with the shipboard core loggers and other instruments.

Methods for analysis of cracks in three-dimensional solids

NASA Technical Reports Server (NTRS)

Raju, I. S.; Newman, J. C., Jr.

1984-01-01

Analytical and numerical methods evaluating the stress-intensity factors for three-dimensional cracks in solids are presented, with reference to fatigue failure in aerospace structures. The exact solutions for embedded elliptical and circular cracks in infinite solids, and the approximate methods, including the finite-element, the boundary-integral equation, the line-spring models, and the mixed methods are discussed. Among the mixed methods, the superposition of analytical and finite element methods, the stress-difference, the discretization-error, the alternating, and the finite element-alternating methods are reviewed. Comparison of the stress-intensity factor solutions for some three-dimensional crack configurations showed good agreement. Thus, the choice of a particular method in evaluating the stress-intensity factor is limited only to the availability of resources and computer programs.

Further analytical study of hybrid rocket combustion

NASA Technical Reports Server (NTRS)

Hung, W. S. Y.; Chen, C. S.; Haviland, J. K.

1972-01-01

Analytical studies of the transient and steady-state combustion processes in a hybrid rocket system are discussed. The particular system chosen consists of a gaseous oxidizer flowing within a tube of solid fuel, resulting in a heterogeneous combustion. Finite rate chemical kinetics with appropriate reaction mechanisms were incorporated in the model. A temperature dependent Arrhenius type fuel surface regression rate equation was chosen for the current study. The governing mathematical equations employed for the reacting gas phase and for the solid phase are the general, two-dimensional, time-dependent conservation equations in a cylindrical coordinate system. Keeping the simplifying assumptions to a minimum, these basic equations were programmed for numerical computation, using two implicit finite-difference schemes, the Lax-Wendroff scheme for the gas phase, and, the Crank-Nicolson scheme for the solid phase.

Analysis of Pre-Analytic Factors Affecting the Success of Clinical Next-Generation Sequencing of Solid Organ Malignancies.

PubMed

Chen, Hui; Luthra, Rajyalakshmi; Goswami, Rashmi S; Singh, Rajesh R; Roy-Chowdhuri, Sinchita

2015-08-28

Application of next-generation sequencing (NGS) technology to routine clinical practice has enabled characterization of personalized cancer genomes to identify patients likely to have a response to targeted therapy. The proper selection of tumor sample for downstream NGS based mutational analysis is critical to generate accurate results and to guide therapeutic intervention. However, multiple pre-analytic factors come into play in determining the success of NGS testing. In this review, we discuss pre-analytic requirements for AmpliSeq PCR-based sequencing using Ion Torrent Personal Genome Machine (PGM) (Life Technologies), a NGS sequencing platform that is often used by clinical laboratories for sequencing solid tumors because of its low input DNA requirement from formalin fixed and paraffin embedded tissue. The success of NGS mutational analysis is affected not only by the input DNA quantity but also by several other factors, including the specimen type, the DNA quality, and the tumor cellularity. Here, we review tissue requirements for solid tumor NGS based mutational analysis, including procedure types, tissue types, tumor volume and fraction, decalcification, and treatment effects.

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Conventional sample enrichment strategies combined with high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance analysis allows analyte identification from a single minuscule Corydalis solida plant tuber.

PubMed

Sturm, Sonja; Seger, Christoph; Godejohann, Markus; Spraul, Manfred; Stuppner, Hermann

2007-09-07

Identification of putative biomarker molecules within the genus Corydalis (Papaveraceae) was pursued by combining conventional off-line sample enrichment with high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance (HPLC-SPE-NMR) based structure elucidation. Off-line reversed phase solid phase extraction (SPE) was used to enrich the desired analytes from a methanolic extract (93 mg dry weight) of a miniscule single tuber (233 mg dry weight) of C. solida. An aliquot of the SPE fraction (2.1 mg) was subjected to separation in the HPLC-SPE-NMR hyphenation. Chromatographic peaks bearing the metabolites under investigation were trapped in the SPE device in a single experiment and transferred to a 600 MHz NMR spectrometer equipped with a 30 microl cryofit insert fed into a 3 mm cryoprobe. Recorded homo- and heteronuclear 1D and 2D NMR data allowed the identification of the three analytes under investigation as protopine, allocryptopine, and N-methyl-laudanidinium acetate. The latter is a rare alkaloid, which has been isolated only once before.

An added-mass partition algorithm for fluid–structure interactions of compressible fluids and nonlinear solids

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

Banks, J.W., E-mail: banksj3@rpi.edu; Henshaw, W.D., E-mail: henshw@rpi.edu; Kapila, A.K., E-mail: kapila@rpi.edu

We describe an added-mass partitioned (AMP) algorithm for solving fluid–structure interaction (FSI) problems involving inviscid compressible fluids interacting with nonlinear solids that undergo large rotations and displacements. The computational approach is a mixed Eulerian–Lagrangian scheme that makes use of deforming composite grids (DCG) to treat large changes in the geometry in an accurate, flexible, and robust manner. The current work extends the AMP algorithm developed in Banks et al. [1] for linearly elasticity to the case of nonlinear solids. To ensure stability for the case of light solids, the new AMP algorithm embeds an approximate solution of a nonlinear fluid–solidmore » Riemann (FSR) problem into the interface treatment. The solution to the FSR problem is derived and shown to be of a similar form to that derived for linear solids: the state on the interface being fundamentally an impedance-weighted average of the fluid and solid states. Numerical simulations demonstrate that the AMP algorithm is stable even for light solids when added-mass effects are large. The accuracy and stability of the AMP scheme is verified by comparison to an exact solution using the method of analytical solutions and to a semi-analytical solution that is obtained for a rotating solid disk immersed in a fluid. The scheme is applied to the simulation of a planar shock impacting a light elliptical-shaped solid, and comparisons are made between solutions of the FSI problem for a neo-Hookean solid, a linearly elastic solid, and a rigid solid. The ability of the approach to handle large deformations is demonstrated for a problem of a high-speed flow past a light, thin, and flexible solid beam.« less

DETERMINATION OF CHLOROETHENES IN ENVIRONMENTAL BIOLOGICAL SAMPLES USING GAS CHROMATOGRAPHY COUPLED WITH SOLID PHASE MICRO EXTRACTION

EPA Science Inventory

An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase mi...

VOLATILE ORGANO-METALLOIDS IN BIO-SOLID MATERIALS: ANALYSIS BY VACUUM DISTILLATION-GC/MS

EPA Science Inventory

An analytical method based on vacuum distillation-gas chromatography-mass spectrometry (VD-GC-MS)

was developed for determining volatile organo-metalloid contaminants in bio-solid materials. Method

performance was evaluated for dimethylselenide (DMSe), dimethyldisel...

Digital Education Governance: Data Visualization, Predictive Analytics, and "Real-Time" Policy Instruments

ERIC Educational Resources Information Center

Williamson, Ben

2016-01-01

Educational institutions and governing practices are increasingly augmented with digital database technologies that function as new kinds of policy instruments. This article surveys and maps the landscape of digital policy instrumentation in education and provides two detailed case studies of new digital data systems. The Learning Curve is a…

Pods: a Powder Delivery System for Mars In-situ Organic, Mineralogic and Isotopic Analysis Instruments

NASA Technical Reports Server (NTRS)

Saha, C. P.; Bryson, C. E.; Sarrazin, P.; Blake, D. F.

2005-01-01

Many Mars in situ instruments require fine-grained high-fidelity samples of rocks or soil. Included are instruments for the determination of mineralogy as well as organic and isotopic chemistry. Powder can be obtained as a primary objective of a sample collection system (e.g., by collecting powder as a surface is abraded by a rotary abrasion tool (RAT)), or as a secondary objective (e.g, by collecting drill powder as a core is drilled). In the latter case, a properly designed system could be used to monitor drilling in real time as well as to deliver powder to analytical instruments which would perform complementary analyses to those later performed on the intact core. In addition, once a core or other sample is collected, a system that could transfer intelligently collected subsamples of power from the intact core to a suite of analytical instruments would be highly desirable. We have conceptualized, developed and tested a breadboard Powder Delivery System (PoDS) intended to satisfy the collection, processing and distribution requirements of powder samples for Mars in-situ mineralogic, organic and isotopic measurement instruments.

Analytical interference of drugs in clinical chemistry: I--Study of twenty drugs on seven different instruments.

PubMed

Letellier, G; Desjarlais, F

1985-12-01

We have investigated the effect of 20 drugs on the accuracy of results obtained from seven instruments now widely used in clinical biochemistry laboratories: Abbott VP, aca II, Cobas Bio, Ektachem 400, Hitachi 705, KDA and SMAC. Eleven to 18 constituents were analysed on each instrument. Our results lead us to the following conclusions: (1) only rarely does drug interference with a method lead to a clinically significant change in a measured value; (2) the magnitude of the change may relate linearly or non-linearly to the drug concentration but is usually independent of the target analyte concentration; (3) interference with a chemical reaction on one instrument does not always mean that the same reaction will be altered in the same way on other instruments; (4) no interferences were found for drugs with therapeutic levels in the low micro-molar range; (5) in most cases the interference could not be predicted from the chemical nature of drug.

Creating New Technologists of Research in the 1960s: The Case of the Reproduction of Automated Chromatography Specialists and Practitioners

NASA Astrophysics Data System (ADS)

Gerontas, Apostolos

2014-08-01

Chromatographic instrumentation has been really influential in shaping the modern chemical practice, and yet it has been largely overlooked by history of science.Gas chromatography in the 1960s was considered the analytical technique closer to becoming dominant, and being the first automated chromatography set the standards that all the subsequent chromatographic instrumentation had to fulfill. Networks of specialists, groups of actors, corporate strategies and the analytical practice itself, were all affected and in many ways because of the entrance of gas chromatography in the chemical laboratory and in the instrumentation market. This paper gives a view of the early history of the gas chromatography instrumentation, relates it to the broader research-technology phenomenon and discusses issues of education and group reproduction in the case of the groups of technologists of the era. The chaotic elements of knowledge transfer during the instrumentation revolution in chemistry are being highlighted and they are being connected to the observable radical innovation of the period.

Solid-phase microextraction with temperature-programmed desorption for the analysis of iodination disinfection byproducts.

PubMed

Frazey, P A; Barkley, R M; Sievers, R E

1998-02-01

An analytical approach for the determination of chlorination and iodination disinfection byproducts based on solid-phase microextraction (SPME) was developed. Solid-phase microextraction presents a simple, rapid, sensitive, and solvent-free approach to sample preparation in which analytes in either air or water matrixes are extracted into the polymeric coating of an optical fiber. Analytes are subsequently thermally desorbed in the injection port of a gas chromatograph for separation, detection, and quantitation. Thermal degradation of iodoform was observed during desorption from a polyacrylate fiber in initial GC/MS and GC/ECD experiments. Experiments were designed to determine SPME conditions that would allow quantification without significant degradation of analytes. Isothermal and temperature-programmed thermal desorptions were evaluated for efficacy in transferring analytes with wide-ranging volatilities and thermal stabilities into chromatographic analysis columns. A temperature-programmed desorption (TPD) (120-200 degrees C at 5 degrees C/min with an on-column injection port or 150-200 degrees C at 25 degrees C/min with a split/splitless injection port) was able to efficiently remove analytes with wide-ranging volatilities without causing thermal degradation. The SPME-TPD method was linear over 2-3 orders of magnitude with an electron capture detector and detection limits were in the submicrogram per liter range. Precision and detection limits for selected trihalomethanes were comparable to those of EPA method 551. Extraction efficiencies were not affected by the presence of 10 mg/L soap, 15 mg/L sodium iodide, and 6000 mg/L sodium thiosulfate. The SPME-TPD technique was applied to the determination of iodination disinfection byproducts from individual precursor compounds using GC/MS and to the quantitation of iodoform at trace levels in a water recycle system using GC/ECD.

Advancement of High Power Quasi-CW Laser Diode Arrays For Space-based Laser Instruments

NASA Technical Reports Server (NTRS)

Amzajerdian, Farzin; Meadows, Byron L.; Baker, nathaniel R.; Baggott, Renee S.; Singh, Upendra N.; Kavaya, Michael J.

2004-01-01

Space-based laser and lidar instruments play an important role in NASA s plans for meeting its objectives in both Earth Science and Space Exploration areas. Almost all the lidar instrument concepts being considered by NASA scientist utilize moderate to high power diode-pumped solid state lasers as their transmitter source. Perhaps the most critical component of any solid state laser system is its pump laser diode array which essentially dictates instrument efficiency, reliability and lifetime. For this reason, premature failures and rapid degradation of high power laser diode arrays that have been experienced by laser system designers are of major concern to NASA. This work addresses these reliability and lifetime issues by attempting to eliminate the causes of failures and developing methods for screening laser diode arrays and qualifying them for operation in space.

Analytical capabilities and services of Lawrence Livermore Laboratory's General Chemistry Division. [Methods available at Lawrence Livermore

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

Gutmacher, R.; Crawford, R.

This comprehensive guide to the analytical capabilities of Lawrence Livermore Laboratory's General Chemistry Division describes each analytical method in terms of its principle, field of application, and qualitative and quantitative uses. Also described are the state and quantity of sample required for analysis, processing time, available instrumentation, and responsible personnel.

Modular nonvolatile solid state recorder (MONSSTR) update

NASA Astrophysics Data System (ADS)

Klang, Mark R.; Small, Martin B.; Beams, Tom

2001-12-01

Solid state recorders have begun replacing traditional tape recorders in fulfilling the requirement to record images on airborne platforms. With the advances in electro-optical, IR, SAR, Multi and Hyper-spectral sensors and video recording requirements, solid state recorders have become the recorder of choice. Solid state recorders provide the additional storage, higher sustained bandwidth, less power, less weight and smaller footprint to meet the current and future recording requirements. CALCULEX, Inc., manufactures a non-volatile flash memory solid state recorder called the MONSSTR (Modular Non-volatile Solid State Recorder). MONSSTR is being used to record images from many different digital sensors on high performance aircraft such as the RF- 4, F-16 and the Royal Air Force Tornado. MONSSTR, with its internal multiplexer, is also used to record instrumentation data. This includes multiple streams of PCM and multiple channels of 1553 data. Instrumentation data is being recorded by MONSSTR systems in a range of platforms including F-22, F-15, F-16, Comanche Helicopter and US Navy torpedos. MONSSTR can also be used as a cockpit video recorder. This paper will provide an update of the MONSSTR.

Performances of the Mars Organic Molecule Analyzer (MOMA) GC-MS suite aboard ExoMars Mission

NASA Astrophysics Data System (ADS)

Buch, A.; Grand, N.; Pinnick, V. T.; Szopa, C.; Humeau, O.; Danell, R.; van Amerom, F. H. W.; Freissinet, C.; Glavin, D. P.; Belmahdi, I.; Coll, P. J.; Lustrement, B.; Brinckerhoff, W. B.; Arevalo, R. D., Jr.; Stalport, F.; Steininger, H.; Goesmann, F.; Raulin, F.; Mahaffy, P. R.

2014-12-01

The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars rover (Pasteur) will be a key analytical tool in providing chemical (molecular) information from the solid samples collected by the rover, with a particular focus on the characterization of the organic content. Samples will be extracted as deep as 2 meters below the martian surface to minimize effects of radiation and oxidation on organic materials. The core of the MOMA instrument is a dual source UV laser desorption / ionization (LDI) and pyrolysis gas chromatography (pyr-GC) ion trap mass spectrometer (ITMS) which provides the unique capability to characterize a broad range of compounds, including both of volatile and non-volatile species. Samples which undergo GC-ITMS analysis may be submitted to a derivatization process, consisting of the reaction of the sample components with specific reactants (MTBSTFA [1], DMF-DMA [2] or TMAH [3]) which increase the volatility of complex organic species. With the goal to optimize this instrumentation, and especially the GC-ITMS coupling, a series of tests is currently being carried out with prototypes of MOMA instrumentation and with the ETU models wich is similar to the flight model. The MOMA oven and tapping station are also part of these end-to-end experiments. Qualitative and quantitative tests has been done on gas, liquid and solid samples. The results obtained demonstrate the current status of the end-to-end performance of the gas chromatography-mass spectrometry mode of operation. Both prototypes individually meet the performance requirements, but this work particularly demonstrates the capabilities of the critical GC-MS interface. References: [1] Buch, A. et al. (2009) J chrom. A, 43, 143-151. [2] Freissinet et al. (2011) J Chrom A, 1306, 59-71. [3] Geffroy-Rodier, C. et al. (2009) JAAP, 85, 454-459. Acknowledgements: Funding provided by the Mars Exploration Program (point of contact, George Tahu, NASA/HQ). MOMA is a collaboration between NASA and ESA (PI Goesmann, MPS). MOMA-GC team acknowledges support from the French Space Agency (CNES), French National Programme of Planetology (PNP), National French Council (CNRS), Pierre Simon Laplace Institute.

Analytical methodologies based on LC-MS/MS for monitoring selected emerging compounds in liquid and solid phases of the sewage sludge.

PubMed

Boix, C; Ibáñez, M; Fabregat-Safont, D; Morales, E; Pastor, L; Sancho, J V; Sánchez-Ramírez, J E; Hernández, F

2016-01-01

In this work, two analytical methodologies based on liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) were developed for quantification of emerging pollutants identified in sewage sludge after a previous wide-scope screening. The target list included 13 emerging contaminants (EC): thiabendazole, acesulfame, fenofibric acid, valsartan, irbesartan, salicylic acid, diclofenac, carbamazepine, 4-aminoantipyrine (4-AA), 4-acetyl aminoantipyrine (4-AAA), 4-formyl aminoantipyrine (4-FAA), venlafaxine and benzoylecgonine. The aqueous and solid phases of the sewage sludge were analyzed making use of Solid-Phase Extraction (SPE) and UltraSonic Extraction (USE) for sample treatment, respectively. The methods were validated at three concentration levels: 0.2, 2 and 20 μg L(-1) for the aqueous phase, and 50, 500 and 2000 μg kg(-1) for the solid phase of the sludge. In general, the method was satisfactorily validated, showing good recoveries (70-120%) and precision (RSD < 20%). Regarding the limit of quantification (LOQ), it was below 0.1 μg L(-1) in the aqueous phase and below 50 μg kg(-1) in the solid phase for the majority of the analytes. The method applicability was tested by analysis of samples from a wider study on degradation of emerging pollutants in sewage sludge under anaerobic digestion. The key benefits of these methodologies are: • SPE and USE are appropriate sample procedures to extract selected emerging contaminants from the aqueous phase of the sewage sludge and the solid residue. • LC-MS/MS is highly suitable for determining emerging contaminants in both sludge phases. • Up to our knowledge, the main metabolites of dipyrone had not been studied before in sewage sludge.

The relative responsiveness of test instruments can be estimated using a meta-analytic approach: an illustration with treatments for depression.

PubMed

Kounali, Daphne Z; Button, Katherine S; Lewis, Glyn; Ades, Anthony E

2016-09-01

We present a meta-analytic method that combines information on treatment effects from different instruments from a network of randomized trials to estimate instrument relative responsiveness. Five depression-test instruments [Beck Depression Inventory (BDI I/II), Patient Health Questionnaire (PHQ9), Hamilton Rating for Depression 17 and 24 items, Montgomery-Asberg Depression Rating] and three generic quality of life measures [EuroQoL (EQ-5D), SF36 mental component summary (SF36 MCS), and physical component summary (SF36 PCS)] were compared. Randomized trials of treatments for depression reporting outcomes on any two or more of these instruments were identified. Information on the within-trial ratios of standardized treatment effects was pooled across the studies to estimate relative responsiveness. The between-instrument ratios of standardized treatment effects vary across trials, with a coefficient of variation of 13% (95% credible interval: 6%, 25%). There were important differences between the depression measures, with PHQ9 being the most responsive instrument and BDI the least. Responsiveness of the EQ-5D and SF36 PCS was poor. SF36 MCS performed similarly to depression instruments. Information on relative responsiveness of several test instruments can be pooled across networks of trials reporting at least two outcomes, allowing comparison and ranking of test instruments that may never have been compared directly. Copyright © 2016 Elsevier Inc. All rights reserved.

Effluent composition prediction of a two-stage anaerobic digestion process: machine learning and stoichiometry techniques.

PubMed

Alejo, Luz; Atkinson, John; Guzmán-Fierro, Víctor; Roeckel, Marlene

2018-05-16

Computational self-adapting methods (Support Vector Machines, SVM) are compared with an analytical method in effluent composition prediction of a two-stage anaerobic digestion (AD) process. Experimental data for the AD of poultry manure were used. The analytical method considers the protein as the only source of ammonia production in AD after degradation. Total ammonia nitrogen (TAN), total solids (TS), chemical oxygen demand (COD), and total volatile solids (TVS) were measured in the influent and effluent of the process. The TAN concentration in the effluent was predicted, this being the most inhibiting and polluting compound in AD. Despite the limited data available, the SVM-based model outperformed the analytical method for the TAN prediction, achieving a relative average error of 15.2% against 43% for the analytical method. Moreover, SVM showed higher prediction accuracy in comparison with Artificial Neural Networks. This result reveals the future promise of SVM for prediction in non-linear and dynamic AD processes. Graphical abstract ᅟ.

Calculation of Thermally-Induced Displacements in Spherically Domed Ion Engine Grids

NASA Technical Reports Server (NTRS)

Soulas, George C.

2006-01-01

An analytical method for predicting the thermally-induced normal and tangential displacements of spherically domed ion optics grids under an axisymmetric thermal loading is presented. A fixed edge support that could be thermally expanded is used for this analysis. Equations for the displacements both normal and tangential to the surface of the spherical shell are derived. A simplified equation for the displacement at the center of the spherical dome is also derived. The effects of plate perforation on displacements and stresses are determined by modeling the perforated plate as an equivalent solid plate with modified, or effective, material properties. Analytical model results are compared to the results from a finite element model. For the solid shell, comparisons showed that the analytical model produces results that closely match the finite element model results. The simplified equation for the normal displacement of the spherical dome center is also found to accurately predict this displacement. For the perforated shells, the analytical solution and simplified equation produce accurate results for materials with low thermal expansion coefficients.

Water-compatible molecularly imprinted polymers for efficient direct injection on-line solid-phase extraction of ropivacaine and bupivacaine from human plasma.

PubMed

Cobb, Zoe; Sellergren, Börje; Andersson, Lars I

2007-12-01

Two novel molecularly imprinted polymers (MIPs) selected from a combinatorial library of bupivacaine imprinted polymers were used for selective on-line solid-phase extraction of bupivacaine and ropivacaine from human plasma. The MIPs were prepared using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linking monomer and in addition hydroxyethylmethacrylate to render the polymer surface hydrophilic. The novel MIPs showed high selectivity for the analytes and required fewer and lower concentrations of additives to suppress non-specific adsorption compared with a conventional MIP. This enabled the development of an on-line system for direct extraction of buffered plasma. Selective extraction was achieved without the use of time-consuming solvent switch steps, and transfer of the analytes from the MIP column to the analytical column was carried out under aqueous conditions fully compatible with reversed-phase LC gradient separation of analyte and internal standard. The MIPs showed excellent aqueous compatibility and yielded extractions with acceptable recovery and high selectivity.

A first evaluation of the analytical capabilities of the new X-ray fluorescence facility at International Atomic Energy Agency-Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis

NASA Astrophysics Data System (ADS)

Marguí, Eva; Hidalgo, Manuela; Migliori, Alessandro; Leani, Juan José; Queralt, Ignasi; Kallithrakas-Kontos, Nikolaos; Streli, Christina; Prost, Josef; Karydas, Andreas Germanos

2018-07-01

The aim of the work is to present a systematic evaluation of the analytical capabilities of the new X-ray fluorescence facility jointly operated between the International Atomic Energy Agency and the Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis. The analytical performance of the XRF beamline end-station (IAEAXspe) was systematically evaluated under TXRF excitation geometry by analyzing different types of aqueous (lake, waste and fresh water) and solid (soil, vegetal, biological) certified reference materials using an excitation energy of 13.0 keV (for the purpose of multielemental analysis). The results obtained for both types of samples in terms of limits of detection and accuracy were also compared with those obtained using laboratory X-ray tube based TXRF systems with different features (including Mo and W X-ray tube systems). Taking advantage of the possibility to work under high vacuum, the IAEAXspe set-up instrumental sensitivity was also determined using an excitation energy of 6.2 keV to explore the possibilities for light elements determination. A clear improvement of the element detection limits is achieved when comparing this facility to conventional X-ray tube based TXRF systems highlighting the benefits of using the monoenergetic synchrotron exciting radiation and the ultra-high vacuum chamber in comparison with conventional laboratory systems. The results of the present work are discussed in view of further exploitation of the facility for different environmental and biological related applications.

Laboratory Production of Lemon Liqueur (Limoncello) by Conventional Maceration and a Two-Syringe System to Illustrate Rapid Solid-Liquid Dynamic Extraction

ERIC Educational Resources Information Center

Naviglio, Daniele; Montesano, Domenico; Gallo, Monica

2015-01-01

Two experimental techniques of solid-liquid extraction are compared relating to the lab-scale production of lemon liqueur, most commonly named "limoncello"; the first is the official method of maceration for the solid-liquid extraction of analytes and is widely used to extract active ingredients from a great variety of natural products;…

Nuclear Science Symposium, 4th, and Nuclear Power Systems Symposium, 9th, San Francisco, Calif., October 19-21, 1977, Proceedings

NASA Technical Reports Server (NTRS)

1978-01-01

Consideration is given to the following types of high energy physics instrumentation: drift chambers, multiwire proportional chambers, calorimeters, optical detectors, ionization and scintillation detectors, solid state detectors, and electronic and digital subsystems. Attention is also paid to reactor instrumentation, nuclear medicine instrumentation, data acquisition systems for nuclear instrumentation, microprocessor applications in nuclear science, environmental instrumentation, control and instrumentation of nuclear power generating stations, and radiation monitoring. Papers are also presented on instrumentation for the High Energy Astronomy Observatory.

Prediction of wood mechanical and chemical properties in the presence and absence of blue stain using two near infrared instruments

Treesearch

Brian K. Via; Chi-Leung So; Todd F. Shupe; Lori G. Eckhardt; Michael Stine; Leslie H. Groom

2005-01-01

The objective of this research was to (a) determine if blue stain in solid wood influenced calibration equations developed from a nonstained wood population, (b) assess the bias introduced when scanning was performed by the slave instrument without calibration transfer from the master instrument and (c) partition absorbance-based variation by instrument, stain and...

Laser Time-of-Flight Mass Spectrometry for Future In Situ Planetary Missions

NASA Technical Reports Server (NTRS)

Getty, S. A.; Brinckerhoff, W. B.; Cornish, T.; Ecelberger, S. A.; Li, X.; Floyd, M. A. Merrill; Chanover, N.; Uckert, K.; Voelz, D.; Xiao, X.;

The Effect of Emulsion Intensity on Selected Sensory and Instrumental Texture Properties of Full-Fat Mayonnaise

PubMed Central

Olsson, Viktoria; Håkansson, Andreas

2018-01-01

Varying processing conditions can strongly affect the microstructure of mayonnaise, opening up new applications for the creation of products tailored to meet different consumer preferences. The aim of the study was to evaluate the effect of emulsification intensity on sensory and instrumental characteristics of full-fat mayonnaise. Mayonnaise, based on a standard recipe, was processed at low and high emulsification intensities, with selected sensory and instrumental properties then evaluated using an analytical panel and a back extrusion method. The evaluation also included a commercial reference mayonnaise. The overall effects of a higher emulsification intensity on the sensory and instrumental characteristics of full-fat mayonnaise were limited. However, texture was affected, with a more intense emulsification resulting in a firmer mayonnaise according to both back extrusion data and the analytical sensory panel. Appearance, taste and flavor attributes were not affected by processing. PMID:29342128

Analytical Chemistry and the Microchip.

ERIC Educational Resources Information Center

Lowry, Robert K.

1986-01-01

Analytical techniques used at various points in making microchips are described. They include: Fourier transform infrared spectrometry (silicon purity); optical emission spectroscopy (quantitative thin-film composition); X-ray photoelectron spectroscopy (chemical changes in thin films); wet chemistry, instrumental analysis (process chemicals);…

Study of Surface Wave Propagation in Fluid-Saturated Porous Solids.

NASA Astrophysics Data System (ADS)

Azcuaga, Valery Francisco Godinez

1995-01-01

This study addresses the surface wave propagation phenomena on fluid-saturated porous solids. The analytical method for calculation of surface wave velocities (Feng and Johnson, JASA, 74, 906, 1983) is extended to the case of a porous solid saturated with a wetting fluid in contact with a non-wetting fluid, in order to study a material combination suitable for experimental investigation. The analytical method is further extended to the case of a non-wetting fluid/wetting fluid-saturated porous solid interface with an arbitrary finite surface stiffness. These extensions of the analytical method allows to theoretically study surface wave propagation phenomena during the saturation process. A modification to the 2-D space-time reflection Green's function (Feng and Johnson, JASA, 74, 915, 1983) is introduced in order to simulate the behavior of surface wave signals detected during the experimental investigation of surface wave propagation on fluid-saturated porous solids (Nagy, Appl. Phys. Lett., 60, 2735, 1992). This modification, together with the introduction of an excess attenuation for the Rayleigh surface mode, makes it possible to explain the apparent velocity changes observed on the surface wave signals during saturation. Experimental results concerning the propagation of surface waves on an alcohol-saturated porous glass are presented. These experiments were performed at frequencies of 500 and 800 kHz and show the simultaneous propagation of the two surface modes predicted by the extended analytical method. Finally an analysis of the displacements associated with the different surface modes is presented. This analysis reveals that it is possible to favor the generation of the Rayleigh surface mode or of the slow surface mode, simply by changing the type of transducer used in the generation of surface waves. Calculations show that a shear transducer couples more energy into the Rayleigh mode, whereas a longitudinal transducer couples more energy into the slow surface mode. Experimental results obtained with the modified experimental system show a qualitative agreement with the theoretical predictions.

Methods for analysis of cracks in three-dimensional solids

NASA Technical Reports Server (NTRS)

Raju, I. S.; Newman, J. C., Jr.

1984-01-01

Various analytical and numerical methods used to evaluate the stress intensity factors for cracks in three-dimensional (3-D) solids are reviewed. Classical exact solutions and many of the approximate methods used in 3-D analyses of cracks are reviewed. The exact solutions for embedded elliptic cracks in infinite solids are discussed. The approximate methods reviewed are the finite element methods, the boundary integral equation (BIE) method, the mixed methods (superposition of analytical and finite element method, stress difference method, discretization-error method, alternating method, finite element-alternating method), and the line-spring model. The finite element method with singularity elements is the most widely used method. The BIE method only needs modeling of the surfaces of the solid and so is gaining popularity. The line-spring model appears to be the quickest way to obtain good estimates of the stress intensity factors. The finite element-alternating method appears to yield the most accurate solution at the minimum cost.

The Sample Analysis at Mars Investigation and Instrument Suite

NASA Technical Reports Server (NTRS)

Mahaffy, Paul; Webster, Chris R.; Cabane, M.; Conrad, Pamela G.; Coll, Patrice; Atreya, Sushil K.; Arvey, Robert; Barciniak, Michael; Benna, Mehdi; Bleacher, L.;

Characterization of a turbomolecular-pumped magnetic sector mass spectrometer

NASA Technical Reports Server (NTRS)

Mehta, Narinder K.

1988-01-01

A Perkin Elmer MGA-1200, turbomolecular-pumped, magnetic sector, multiple gas analyzer mass spectrometer with modified inlet for fast response was characterized for the analysis of hydrogen, helium, oxygen and argon in nitrogen and helium background gases. This instrument was specially modified for the Vanderberg AFB SLC-6 Hydrogen Disposal Test Program, as a part of the Hydrogen Sampling System (H2S2). Linearity, precision, drift, detection limits and accuracy among other analytical parameters for each of the background gas were studied to evaluate the performance of the instrument. The result demonstrates that H2S2 mass spectrometer is a stable instrument and can be utilized for the quantitative analytical determination of hydrogen, helium, oxygen and argon in nitrogen and helium background gases.

Cell-model prediction of the melting of a Lennard-Jones solid

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

Holian, B.L.

The classical free energy of the Lennard-Jones 6-12 solid is computed from a single-particle anharmonic cell model with a correction to the entropy given by the classical correlational entropy of quasiharmonic lattice dynamics. The free energy of the fluid is obtained from the Hansen-Ree analytic fit to Monte Carlo equation-of-state calculations. The resulting predictions of the solid-fluid coexistence curves by this corrected cell model of the solid are in excellent agreement with the computer experiments.

Learning ion solid interactions hands-on: An activity based, inquiry oriented, graduate course

NASA Astrophysics Data System (ADS)

Braunstein, Gabriel

2005-12-01

Experimental work, using state of the art instrumentation, is integrated with lectures in a "real life", learning by discovery approach, in the Ion-Solid Interactions graduate/undergraduate course offered by the Department of Physics of the University of Central Florida. The lecture component of the course covers the underlying physical principles, and related scientific and technological applications, associated with the interaction of energetic ions with matter. In the experimental section the students form small groups and perform a variety of projects, experimental and computational, as part of a participative, inquiry oriented, learning process. In the most recent offering of the class, the students deposited a compound semiconductor thin film by dual-gun sputtering deposition, where each group aimed at a different stoichiometry of the same compound (Zn1-xSxOy). Then they analyzed the composition using Rutherford backscattering spectrometry, measured electrical transport properties using Hall effect and conductivity measurements, and determined the band gap using spectrophotometry. Finally the groups shared their results and each wrote a 'journal-like' technical article describing the entire work. In a different assignment, each group also developed a Monte Carlo computer program ('TRIM-like') to simulate the penetration of ions into a solid, in ion implantation, calculating the stopping cross-sections with approximate models, taught in class, which can be analytically solved. The combination of classroom/laboratory activities is very well received by the students. They gain real life experience operating state of the art equipment, and working in teams, while performing research-like projects, and simultaneously they learn the theoretical foundations of the discipline.

Effect of the Presence of Chlorates and Perchlorates on the Pyrolysis of Organic Compounds: Implications for Measurements Done with the SAM Experiment Onboard the Curiosity Rover

NASA Technical Reports Server (NTRS)

Millan, M.; Szopa, C.; Buch, A.; Belmahdi, I.; Coll, P.; Glavin, D. P.; Freissinet, C.; Archer, P. D., Jr.; Sutter, B.; Summons, R. E.;

Renewable Solid Electrodes in Microfluidics: Recovering the Electrochemical Activity without Treating the Surface.

PubMed

Teixeira, Carlos A; Giordano, Gabriela F; Beltrame, Maisa B; Vieira, Luis C S; Gobbi, Angelo L; Lima, Renato S

2016-11-15

The contamination, passivation, or fouling of the detection electrodes is a serious problem undermining the analytical performance of electroanalytical devices. The methods to regenerate the electrochemical activity of the solid electrodes involve mechanical, physical, or chemical surface treatments that usually add operational time, complexity, chemicals, and further instrumental requirements to the analysis. In this paper, we describe for the first time a reproducible method for renewing solid electrodes whenever their morphology or composition are nonspecifically changed without any surface treatment. These renewable electrodes are the closest analogue to the mercury drop electrodes. Our approach was applied in microfluidics, where the downsides related to nonspecific modifications of the electrode are more critical. The renewal consisted in manually sliding metal-coated microwires across a channel with the sample. For this purpose, the chip was composed of a single piece of polydimethylsiloxane (PDMS) with three parallel channels interconnected to one perpendicular and top channel. The microwires were inserted in each one of the parallel channels acting as working, counter, and pseudoreference electrodes for voltammetry. This assembly allowed the renewal of all the three electrodes by simply pulling the microwires. The absence of any interfaces in the chips and the elastomeric nature of the PDMS allowed us to pull the microwires without the occurrence of leakages for the electrode channels even at harsh flow rates of up to 40.0 mL min -1 . We expect this paper can assist the researchers to develop new microfluidic platforms that eliminate any steps of electrode cleaning, representing a powerful alternative for precise and robust analyses to real samples.

Man vs. Machine: A Junior-level Laboratory Exercise Comparing Human and Instrumental Detection Limits

ERIC Educational Resources Information Center

Elias, Ryan J.; Hopfer, Helene; Hofstaedter, Amanda N.; Hayes, John E.

2017-01-01

The human nose is a very sensitive detector and is able to detect potent aroma compounds down to low ng/L levels. These levels are often below detection limits of analytical instrumentation. The following laboratory exercise is designed to compare instrumental and human methods for the detection of volatile odor active compounds. Reference…

Jonathan W. Amy and the Amy Facility for Instrumentation Development.

PubMed

Cooks, R Graham

2017-05-16

This Perspective describes the unique Jonathan Amy Facility for Chemical Instrumentation in the Department of Chemistry at Purdue University, tracing its history and mode of operation. It also describes aspects of the career of its namesake and some of his insights which have been central to analytical instrumentation development, improvement, and utilization, both at Purdue and nationally.

Recognizing and Reducing Analytical Errors and Sources of Variation in Clinical Pathology Data in Safety Assessment Studies.

PubMed

Schultze, A E; Irizarry, A R

2017-02-01

Veterinary clinical pathologists are well positioned via education and training to assist in investigations of unexpected results or increased variation in clinical pathology data. Errors in testing and unexpected variability in clinical pathology data are sometimes referred to as "laboratory errors." These alterations may occur in the preanalytical, analytical, or postanalytical phases of studies. Most of the errors or variability in clinical pathology data occur in the preanalytical or postanalytical phases. True analytical errors occur within the laboratory and are usually the result of operator or instrument error. Analytical errors are often ≤10% of all errors in diagnostic testing, and the frequency of these types of errors has decreased in the last decade. Analytical errors and increased data variability may result from instrument malfunctions, inability to follow proper procedures, undetected failures in quality control, sample misidentification, and/or test interference. This article (1) illustrates several different types of analytical errors and situations within laboratories that may result in increased variability in data, (2) provides recommendations regarding prevention of testing errors and techniques to control variation, and (3) provides a list of references that describe and advise how to deal with increased data variability.

Laboratory evaluation of alcohol safety interlock systems. Volume 2 : instrument screening experiments

DOT National Transportation Integrated Search

1974-01-01

The report contains the results of an experimental and analytical evaluation of instruments and techniques designed to prevent an intoxicated driver from operating his automobile. The prototype 'Alcohol Safety Interlock Systems' tested were developed...

Carbon nanotubes as adsorbent of solid-phase extraction and matrix for laser desorption/ionization mass spectrometry.

PubMed

Pan, Chensong; Xu, Songyun; Zou, Hanfa; Guo, Zhong; Zhang, Yu; Guo, Baochuan

2005-02-01

A method with carbon nanotubes functioning both as the adsorbent of solid-phase extraction (SPE) and the matrix for matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) to analyze small molecules in solution has been developed. In this method, 10 microL suspensions of carbon nanotubes in 50% (vol/vol) methanol were added to the sample solution to extract analytes onto surface of carbon nanotubes because of their dramatic hydrophobicity. Carbon nanotubes in solution are deposited onto the bottom of tube with centrifugation. After removing the supernatant fluid, carbon nanotubes are suspended again with dispersant and pipetted directly onto the sample target of the MALDI-MS to perform a mass spectrometric analysis. It was demonstrated by analysis of a variety of small molecules that the resolution of peaks and the efficiency of desorption/ionization on the carbon nanotubes are better than those on the activated carbon. It is found that with the addition of glycerol and sucrose to the dispersant, the intensity, the ratio of signal to noise (S/N), and the resolution of peaks for analytes by mass spectrometry increased greatly. Compared with the previously reported method by depositing sample solution onto thin layer of carbon nanotubes, it is observed that the detection limit for analytes can be enhanced about 10 to 100 times due to solid-phase extraction of analytes in solution by carbon nanotubes. An acceptable result of simultaneously quantitative analysis of three analytes in solution has been achieved. The application in determining drugs spiked into urine has also been realized.

Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection.

PubMed

Azzouz, Abdelmonaim; Ballesteros, Evaristo

2014-09-19

A novel analytical method using a continuous solid-phase extraction system in combination with gas chromatography-mass spectrometry for the simultaneous separation and determination of endocrine disrupting compounds (EDCs) is reported. The method was applied to major EDCs of various types including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in water. Samples were preconcentrated by using an automatic solid-phase extraction module containing a sorbent column, and retained analytes eluted with acetonitrile for derivatization with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane. A number of variables potentially influencing recovery of the target compounds such as the type of SPE sorbent (Silica gel, Florisil, RP-C18, Amberlite XAD-2 and XAD-4, Oasis HLB and LiChrolut EN), eluent and properties of the water including pH and ionic strength, were examined. LiChrolut EN was found to be the most efficient sorbent for retaining the analytes, with ∼100% efficiency. The ensuing method was validated with good analytical results including low limits of detection (0.01-0.08ng/L for 100mL of sample) and good linearity (r(2)>0.997) throughout the studied concentration ranges. The method exhibited good accuracy (recoveries of 90-101%) and precision (relative standard deviations less than 7%) in the determination of EDCs in drinking, river, pond, well, swimming pool and waste water. Waste water samples were found to contain the largest number and highest concentrations of analytes (3.2-390ng/L). Copyright © 2014 Elsevier B.V. All rights reserved.

SEQUENTIAL EXTRACTIONS FOR PARTITIONING OF ARSENIC ON HYDROUS IRON OXIDES AND IRON SULFIDES

EPA Science Inventory

The objective of this study was to use model solids to test solutions designed to extract arsenic from relatively labile solid phase fractions. The use of sequential extractions provides analytical constraints on the identification of mineral phases that control arsenic mobility...

Space shuttle SRM plume expansion sensitivity analysis. [flow characteristics of exhaust gases from solid propellant rocket engines

NASA Technical Reports Server (NTRS)

Smith, S. D.; Tevepaugh, J. A.; Penny, M. M.

1975-01-01

The exhaust plumes of the space shuttle solid rocket motors can have a significant effect on the base pressure and base drag of the shuttle vehicle. A parametric analysis was conducted to assess the sensitivity of the initial plume expansion angle of analytical solid rocket motor flow fields to various analytical input parameters and operating conditions. The results of the analysis are presented and conclusions reached regarding the sensitivity of the initial plume expansion angle to each parameter investigated. Operating conditions parametrically varied were chamber pressure, nozzle inlet angle, nozzle throat radius of curvature ratio and propellant particle loading. Empirical particle parameters investigated were mean size, local drag coefficient and local heat transfer coefficient. Sensitivity of the initial plume expansion angle to gas thermochemistry model and local drag coefficient model assumptions were determined.

Laser ablation in analytical chemistry - A review

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

Russo, Richard E.; Mao, Xianglei; Liu, Haichen

Laser ablation is becoming a dominant technology for direct solid sampling in analytical chemistry. Laser ablation refers to the process in which an intense burst of energy delivered by a short laser pulse is used to sample (remove a portion of) a material. The advantages of laser ablation chemical analysis include direct characterization of solids, no chemical procedures for dissolution, reduced risk of contamination or sample loss, analysis of very small samples not separable for solution analysis, and determination of spatial distributions of elemental composition. This review describes recent research to understand and utilize laser ablation for direct solid sampling,more » with emphasis on sample introduction to an inductively coupled plasma (ICP). Current research related to contemporary experimental systems, calibration and optimization, and fractionation is discussed, with a summary of applications in several areas.« less

40 CFR 1066.101 - Overview.

Code of Federal Regulations, 2014 CFR

2014-07-01

... PROCEDURES Equipment, Measurement Instruments, Fuel, and Analytical Gas Specifications § 1066.101 Overview. (a) This subpart addresses equipment related to emission testing, as well as test fuels and... specifications for fuels, engine fluids, and analytical gases; these specifications apply for testing under this...

Analytical Chemistry of Surfaces: Part II. Electron Spectroscopy.

ERIC Educational Resources Information Center

Hercules, David M.; Hercules, Shirley H.

1984-01-01

Discusses two surface techniques: X-ray photoelectron spectroscopy (ESCA) and Auger electron spectroscopy (AES). Focuses on fundamental aspects of each technique, important features of instrumentation, and some examples of how ESCA and AES have been applied to analytical surface problems. (JN)

Recommended Inorganic Chemicals for Calibration.

ERIC Educational Resources Information Center

Moody, John R.; And Others

1988-01-01

All analytical techniques depend on the use of calibration chemicals to relate analyte concentration to instrumental parameters. Discusses the preparation of standard solutions and provides a critical evaluation of available materials. Lists elements by group and discusses the purity and uses of each. (MVL)

Analytical Chemistry Laboratory

NASA Technical Reports Server (NTRS)

Anderson, Mark

2013-01-01

The Analytical Chemistry and Material Development Group maintains a capability in chemical analysis, materials R&D failure analysis and contamination control. The uniquely qualified staff and facility support the needs of flight projects, science instrument development and various technical tasks, as well as Cal Tech.

Theoretical models for supercritical fluid extraction.

PubMed

Huang, Zhen; Shi, Xiao-Han; Jiang, Wei-Juan

2012-08-10

For the proper design of supercritical fluid extraction processes, it is essential to have a sound knowledge of the mass transfer mechanism of the extraction process and the appropriate mathematical representation. In this paper, the advances and applications of kinetic models for describing supercritical fluid extraction from various solid matrices have been presented. The theoretical models overviewed here include the hot ball diffusion, broken and intact cell, shrinking core and some relatively simple models. Mathematical representations of these models have been in detail interpreted as well as their assumptions, parameter identifications and application examples. Extraction process of the analyte solute from the solid matrix by means of supercritical fluid includes the dissolution of the analyte from the solid, the analyte diffusion in the matrix and its transport to the bulk supercritical fluid. Mechanisms involved in a mass transfer model are discussed in terms of external mass transfer resistance, internal mass transfer resistance, solute-solid interactions and axial dispersion. The correlations of the external mass transfer coefficient and axial dispersion coefficient with certain dimensionless numbers are also discussed. Among these models, the broken and intact cell model seems to be the most relevant mathematical model as it is able to provide realistic description of the plant material structure for better understanding the mass-transfer kinetics and thus it has been widely employed for modeling supercritical fluid extraction of natural matters. Copyright © 2012 Elsevier B.V. All rights reserved.

Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

2016-12-01

The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

A green analytical method using ultrasound in sample preparation for the flow injection determination of iron, manganese, and zinc in soluble solid samples by flame atomic absorption spectrometry.

PubMed

Yebra, M Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5-30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2-4.6%) and a sample throughput of ca. 25 samples h(-1) were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4-25.61 μg g(-1) for iron, 5.74-18.30 μg g(-1) for manganese, and 33.27-57.90 μg g(-1) for zinc in soluble solid food samples and 3.75-9.90 μg g(-1) for iron, 0.47-5.05 μg g(-1) for manganese, and 1.55-15.12 μg g(-1) for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors.

Determination of perfluorinated chemicals in food and drinking water using high-flow solid-phase extraction and ultra-high performance liquid chromatography/tandem mass spectrometry.

PubMed

Chang, Ying-Chia; Chen, Wen-Ling; Bai, Fang-Yu; Chen, Pau-Chung; Wang, Gen-Shuh; Chen, Chia-Yang

2012-01-01

For this study, we developed methods of determining ten perfluorinated chemicals in drinking water, milk, fish, beef, and pig liver using high-flow automated solid-phase extraction (SPE) and ultra-high performance liquid chromatography/tandem mass spectrometry. The analytes were separated on a core-shell Kinetex C18 column. The mobile phase was composed of methanol and 10-mM N-methylmorpholine. Milk was digested with 0.5 N potassium hydroxide in Milli-Q water, and was extracted with an Atlantic HLB disk to perform automated SPE at a flow rate ranged from 70 to 86 mL/min. Drinking water was directly extracted by the SPE. Solid food samples were digested in alkaline methanol and their supernatants were diluted and also processed by SPE. The disks were washed with 40% methanol/60% water and then eluted with 0.1% ammonium hydroxide in methanol. Suppression of signal intensity of most analytes by matrixes was lower than 50%; it was generally lower in fish and drinking water but higher in liver. Most quantitative biases and relative standard deviations were lower than 15%. The limits of detection for most analytes were sub-nanograms per liter for drinking water and sub-nanograms per gram for solid food samples. This method greatly shortened the time and labor needed for digestion, SPE, and liquid chromatography. This method has been applied to analyze 14 types of food samples. Perfluorooctanoic acid was found to be the highest among the analytes (median at 3.2-64 ng/g wet weight), followed by perfluorodecanoic acid (0.7-25 ng/g) and perfluorododecanoic acid (0.6-15 ng/g).

Combination of Cyclodextrin and Ionic Liquid in Analytical Chemistry: Current and Future Perspectives.

PubMed

Hui, Boon Yih; Raoov, Muggundha; Zain, Nur Nadhirah Mohamad; Mohamad, Sharifah; Osman, Hasnah

2017-09-03

The growth in driving force and popularity of cyclodextrin (CDs) and ionic liquids (ILs) as promising materials in the field of analytical chemistry has resulted in an exponentially increase of their exploitation and production in analytical chemistry field. CDs belong to the family of cyclic oligosaccharides composing of α-(1,4) linked glucopyranose subunits and possess a cage-like supramolecular structure. This structure enables chemical reactions to proceed between interacting ions, radical or molecules in the absence of covalent bonds. Conversely, ILs are an ionic fluids comprising of only cation and anion often with immeasurable vapor pressure making them as green or designer solvent. The cooperative effect between CD and IL due to their fascinating properties, have nowadays contributed their footprints for a better development in analytical chemistry nowadays. This comprehensive review serves to give an overview on some of the recent studies and provides an analytical trend for the application of CDs with the combination of ILs that possess beneficial and remarkable effects in analytical chemistry including their use in various sample preparation techniques such as solid phase extraction, magnetic solid phase extraction, cloud point extraction, microextraction, and separation techniques which includes gas chromatography, high-performance liquid chromatography, capillary electrophoresis as well as applications of electrochemical sensors as electrode modifiers with references to recent applications. This review will highlight the nature of interactions and synergic effects between CDs, ILs, and analytes. It is hoped that this review will stimulate further research in analytical chemistry.

Instrumentation of sampling aircraft for measurement of launch vehicle effluents

NASA Technical Reports Server (NTRS)

Wornom, D. E.; Woods, D. C.; Thomas, M. E.; Tyson, R. W.

1977-01-01

An aircraft was selected and instrumented to measure effluents emitted from large solid propellant rockets during launch activities. The considerations involved in aircraft selection, sampling probes, and instrumentation are discussed with respect to obtaining valid airborne measurements. Discussions of the data acquisition system used, the instrument power system, and operational sampling procedures are included. Representative measurements obtained from an actual rocket launch monitoring activity are also presented.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Developing automated analytical methods for scientific environments using LabVIEW.

PubMed

Wagner, Christoph; Armenta, Sergio; Lendl, Bernhard

2010-01-15

The development of new analytical techniques often requires the building of specially designed devices, each requiring its own dedicated control software. Especially in the research and development phase, LabVIEW has proven to be one highly useful tool for developing this software. Yet, it is still common practice to develop individual solutions for different instruments. In contrast to this, we present here a single LabVIEW-based program that can be directly applied to various analytical tasks without having to change the program code. Driven by a set of simple script commands, it can control a whole range of instruments, from valves and pumps to full-scale spectrometers. Fluid sample (pre-)treatment and separation procedures can thus be flexibly coupled to a wide range of analytical detection methods. Here, the capabilities of the program have been demonstrated by using it for the control of both a sequential injection analysis - capillary electrophoresis (SIA-CE) system with UV detection, and an analytical setup for studying the inhibition of enzymatic reactions using a SIA system with FTIR detection.

INTERNATIONAL CONFERENCE ON SEMICONDUCTOR INJECTION LASERS SELCO-87: Simple formula for the thermal conductivity of a quaternary solid solution

NASA Astrophysics Data System (ADS)

Nakwaski, W.

1988-11-01

An analysis is made of the thermal conductivity of quaternary solid solutions (alloys) allowing for their disordered structure on the basis of a phenomenological analysis proposed by Abeles. This method is applied to a quaternary solid solution In1 - xGaxAsyP1 - y. A simple analytic expression is derived for the thermal conductivity of this material.

Chemical Characterization of an Envelope B/D Sample from Hanford Tank 241-AZ-102

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

Hay, M.S.

2000-08-23

A sample from Hanford waste tank 241-AZ-102 was received at the Savannah River Technology Center (SRTC) and chemically characterized. The sample containing supernate and a small amount of sludge solids was analyzed as-received. The filtered supernatant liquid, the total dried solids of the sample, and the washed insoluble solids obtained from filtration of the sample were analyzed. A mass balance calculation of the three fractions of the sample analyzed indicate the analytical results appear relatively self-consistent for major components of the sample. However, some inconsistency was observed between results were more than one method of determination was employed and formore » species present in low concentrations. The actinides isotopes, plutonium, americium, and curium, present analytical challenges due to the low concentration of these species and the potential for introduction of small amounts of contamination during sampling handling resulting in large uncertainties. A direct comparison to previous analyses of material from tank 241-AZ-102 showed good agreement with the filtered supernatant liquid. However, the comparison of solids data showed poor agreement. The poor agreement shown between the current results for the solids samples and previous analyses most likely results from the uncertainties associated with obtaining small solids samples from a large non-homogenized waste tank.« less

White LEDs as broad spectrum light sources for spectrophotometry: demonstration in the visible spectrum range in a diode-array spectrophotometric detector.

PubMed

Piasecki, Tomasz; Breadmore, Michael C; Macka, Mirek

2010-11-01

Although traditional lamps, such as deuterium lamps, are suitable for bench-top instrumentation, their compatibility with the requirements of modern miniaturized instrumentation is limited. This study investigates the option of utilizing solid-state light source technology, namely white LEDs, as a broad band spectrum source for spectrophotometry. Several white light LEDs of both RGB and white phosphorus have been characterized in terms of their emission spectra and energy output and a white phosphorus Luxeon LED was then chosen for demonstration as a light source for visible-spectrum spectrophotometry conducted in CE. The Luxeon LED was fixed onto the base of a dismounted deuterium (D(2) ) lamp so that the light-emitting spot was geometrically positioned exactly where the light-emitting spot of the original D(2) lamp is placed. In this manner, the detector of a commercial CE instrument equipped with a DAD was not modified in any way. As the detector hardware and electronics remained the same, the change of the deuterium lamp for the Luxeon white LED allowed a direct comparison of their performances. Several anionic dyes as model analytes with absorption maxima between 450 and 600 nm were separated by CE in an electrolyte of 0.01 mol/L sodium tetraborate. The absorbance baseline noise as the key parameter was 5 × lower for the white LED lamp, showing clearly superior performance to the deuterium lamp in the available, i.e. visible part of the spectrum. Copyright © 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method and apparatus for optimized sampling of volatilizable target substances

DOEpatents

Lindgren, Eric R.; Phelan, James M.

2004-10-12

An apparatus for capturing, from gases such as soil gas, target analytes. Target analytes may include emanations from explosive materials or from residues of explosive materials. The apparatus employs principles of sorption common to solid phase microextraction, and is best used in conjunction with analysis means such as a gas chromatograph. To sorb target analytes, the apparatus functions using various sorptive structures to capture target analyte. Depending upon the embodiment, those structures may include a capillary tube including an interior surface on which sorptive material (similar to that on the surface of a SPME fiber) is supported (along with means for moving gases through the capillary tube so that the gases come into close proximity to the sorptive material). In one disclosed embodiment, at least one such sorptive structure is associated with an enclosure including an opening in communication with the surface of a soil region potentially contaminated with buried explosive material such as unexploded ordnance. Emanations from explosive materials can pass into and accumulate in the enclosure where they are sorbed by the sorptive structures. Also disclosed is the use of heating means such as microwave horns to drive target analytes into the soil gas from solid and liquid phase components of the soil.

Low-Cost Chemical-Responsive Adhesive Sensing Chips.

PubMed

Tan, Weirui; Zhang, Liyuan; Shen, Wei

2017-12-06

Chemical-responsive adhesive sensing chip is a new low-cost analytical platform that uses adhesive tape loaded with indicator reagents to detect or quantify the target analytes by directly sticking the tape to the samples of interest. The chemical-responsive adhesive sensing chips can be used with paper to analyze aqueous samples; they can also be used to detect and quantify solid, particulate, and powder analytes. The colorimetric indicators become immediately visible as the contact between the functionalized adhesives and target samples is made. The chemical-responsive adhesive sensing chip expands the capability of paper-based analytical devices to analyze solid, particulate, or powder materials via one-step operation. It is also a simpler alternative way, to the covalent chemical modification of paper, to eliminate indicator leaching from the dipstick-style paper sensors. Chemical-responsive adhesive chips can display analytical results in the form of colorimetric dot patterns, symbols, and texts, enabling clear understanding of assay results by even nonprofessional users. In this work, we demonstrate the analyses of heavy metal salts in silica powder matrix, heavy metal ions in water, and bovine serum albumin in an aqueous solution. The detection is one-step, specific, sensitive, and easy-to-operate.

Mixing of two co-directional Rayleigh surface waves in a nonlinear elastic material.

PubMed

Morlock, Merlin B; Kim, Jin-Yeon; Jacobs, Laurence J; Qu, Jianmin

2015-01-01

The mixing of two co-directional, initially monochromatic Rayleigh surface waves in an isotropic, homogeneous, and nonlinear elastic solid is investigated using analytical, finite element method, and experimental approaches. The analytical investigations show that while the horizontal velocity component can form a shock wave, the vertical velocity component can form a pulse independent of the specific ratios of the fundamental frequencies and amplitudes that are mixed. This analytical model is then used to simulate the development of the fundamentals, second harmonics, and the sum and difference frequency components over the propagation distance. The analytical model is further extended to include diffraction effects in the parabolic approximation. Finally, the frequency and amplitude ratios of the fundamentals are identified which provide maximum amplitudes of the second harmonics as well as of the sum and difference frequency components, to help guide effective material characterization; this approach should make it possible to measure the acoustic nonlinearity of a solid not only with the second harmonics, but also with the sum and difference frequency components. Results of the analytical investigations are then confirmed using the finite element method and the experimental feasibility of the proposed technique is validated for an aluminum specimen.

Transmission versus reflectance spectroscopy for quantitation

NASA Astrophysics Data System (ADS)

Gardner, Craig M.

2018-01-01

The objective of this work was to compare the accuracy of analyte concentration estimation when using transmission versus diffuse reflectance spectroscopy of a scattering medium. Monte Carlo ray tracing of light through the medium was used in conjunction with pure component absorption spectra and Beer-Lambert absorption along each ray's pathlength to generate matched sets of pseudoabsorbance spectra, containing water and six analytes present in skin. PLS regression models revealed an improvement in accuracy when using transmission compared to reflectance for a range of medium thicknesses and instrument noise levels. An analytical expression revealed the source of the accuracy degradation with reflectance was due both to the reduced collection efficiency for a fixed instrument etendue and to the broad pathlength distribution that detected light travels in the medium before exiting from the incident side.

Tunable lasers and their application in analytical chemistry

NASA Technical Reports Server (NTRS)

Steinfeld, J. I.

1975-01-01

The impact that laser techniques might have in chemical analysis is examined. Absorption, scattering, and heterodyne detection is considered. Particular emphasis is placed on the advantages of using frequency-tunable sources, and dye solution lasers are regarded as the outstanding example of this type of laser. Types of spectroscopy that can be carried out with lasers are discussed along with the ultimate sensitivity or minimum detectable concentration of molecules that can be achieved with each method. Analytical applications include laser microprobe analysis, remote sensing and instrumental methods such as laser-Raman spectroscopy, atomic absorption/fluorescence spectrometry, fluorescence assay techniques, optoacoustic spectroscopy, and polarization measurements. The application of lasers to spectroscopic methods of analysis would seem to be a rewarding field both for research in analytical chemistry and for investments in instrument manufacturing.

Cryogenic Caging for Science Instrumentation

NASA Technical Reports Server (NTRS)

Penanen, Konstantin; Chui, Talso C.

2011-01-01

A method has been developed for caging science instrumentation to protect from pyro-shock and EDL (entry, descent, and landing) acceleration damage. Caging can be achieved by immersing the instrument (or its critical parts) in a liquid and solidifying the liquid by cooling. After the launch shock and/or after the payload has landed, the solid is heated up and evaporated.

Laboratory evaluation of alcohol safety interlock systems. Volume 3 : instrument performance at high BAL

DOT National Transportation Integrated Search

1974-01-01

This report contains the results of an experimental and analytical evaluation of instruments and techniques designed to prevent an intoxicated driver from operating his automobile. The prototype 'Alcohol Safety Interlock Systems' tested were develope...

Assessing the Selectivity of Extractant Solutions for Recovering Labile Arsenic Associated with Iron (Hydr)oxides and Sulfides in Sediments

EPA Science Inventory

Sequential extractions can provide analytical constraints on the identification of mineral phases that control arsenic speciation in sediments. Model solids were used in this study to evaluate different solutions designed to extract arsenic from relatively labile solid phases. ...

Discovering Volatile Chemicals from Window Weatherstripping through Solid-Phase Microextraction/Gas Chromatography-Mass Spectrometry

ERIC Educational Resources Information Center

Rosu, Cornelia; Cueto, Rafael; Veillion, Lucas; David, Connie; Laine, Roger A.; Russo, Paul S.

2017-01-01

Volatile compounds from polymeric materials such as weatherstripping were identified by solid-phase microextraction (SPME), a solvent-free analytical method, coupled to gas chromatography-mass spectrometry (GC-MS). These compounds, originating from additives and fillers used in weatherstripping processing, were mostly polycyclic aromatic…

Determination of Plant Volatiles Using Solid Phase Microextraction GC-MS

ERIC Educational Resources Information Center

Van Bramer, Scott; Goodrich, Katherine R.

2015-01-01

This experiment combines analytical techniques of solid phase microextraction and gas chromatography-mass spectrometry with easily relatable and accessible plant volatile chemistry (floral and vegetative scents of local/available plants). The biosynthesis and structure of these chemicals are of interest in the areas of organic chemistry,…

Development of a Solid Phase Extraction Method for Agricultural Pesticides in Large-Volume Water Samples

EPA Science Inventory

An analytical method using solid phase extraction (SPE) and analysis by gas chromatography/mass spectrometry (GC/MS) was developed for the trace determination of a variety of agricultural pesticides and selected transformation products in large-volume high-elevation lake water sa...

Contributions of Analytical Chemistry to the Clinical Laboratory.

ERIC Educational Resources Information Center

Skogerboe, Kristen J.

1988-01-01

Highlights several analytical techniques that are being used in state-of-the-art clinical labs. Illustrates how other advances in instrumentation may contribute to clinical chemistry in the future. Topics include: biosensors, polarization spectroscopy, chemiluminescence, fluorescence, photothermal deflection, and chromatography in clinical…

Developments in spectrophotometry I: An instrument for high-resolution measurements of optical intensity and polarization

NASA Technical Reports Server (NTRS)

Fymat, A. L.

1975-01-01

Device has resolution required to analyze polarization of the spectra of unknown gases, liquids, or solids (or a mixture of these phases). Such resolution has not been available on conventional instruments.

Eight microprocessor-based instrument data systems in the Galileo Orbiter spacecraft

NASA Technical Reports Server (NTRS)

Barry, R. C.

1980-01-01

Instrument data systems consist of a microprocessor, 3K bytes of Read Only Memory and 3K bytes of Random Access Memory. It interfaces with the spacecraft data bus through an isolated user interface with a direct memory access bus adaptor, and/or parallel data from instrument devices such as registers, buffers, analog to digital converters, multiplexers, and solid state sensors. These data systems support the spacecraft hardware and software communication protocol, decode and process instrument commands, generate continuous instrument operating modes, control the instrument mechanisms, acquire, process, format, and output instrument science data.

Analytical instrument with apparatus and method for sample concentrating

DOEpatents

Zaromb, S.

1986-08-04

A system for analysis of trace concentrations of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

The Stanford-U.S. Geological Survey SHRIMP ion microprobe--a tool for micro-scale chemical and isotopic analysis

USGS Publications Warehouse

Bacon, Charles R.; Grove, Marty; Vazquez, Jorge A.; Coble, Matthew A.

2012-01-01

Answers to many questions in Earth science require chemical analysis of minute volumes of minerals, volcanic glass, or biological materials. Secondary Ion Mass Spectrometry (SIMS) is an extremely sensitive analytical method in which a 5–30 micrometer diameter "primary" beam of charged particles (ions) is focused on a region of a solid specimen to sputter secondary ions from 1–5 nanograms of the sample under high vacuum. The elemental abundances and isotopic ratios of these secondary ions are determined with a mass spectrometer. These results can be used for geochronology to determine the age of a region within a crystal thousands to billions of years old or to precisely measure trace abundances of chemical elements at concentrations as low as parts per billion. A partnership of the U.S. Geological Survey and the Stanford University School of Earth Sciences operates a large SIMS instrument, the Sensitive High-Resolution Ion Microprobe with Reverse Geometry (SHRIMP–RG) on the Stanford campus.

Application of Microextraction Techniques Including SPME and MESI to the Thermal Degradation of Polymers: A Review.

PubMed

Kaykhaii, Massoud; Linford, Matthew R

2017-03-04

Here, we discuss the newly developed micro and solventless sample preparation techniques SPME (Solid Phase Microextraction) and MESI (Membrane Extraction with a Sorbent Interface) as applied to the qualitative and quantitative analysis of thermal oxidative degradation products of polymers and their stabilizers. The coupling of these systems to analytical instruments is also described. Our comprehensive literature search revealed that there is no previously published review article on this topic. It is shown that these extraction techniques are valuable sample preparation tools for identifying complex series of degradation products in polymers. In general, the number of products identified by traditional headspace (HS-GC-MS) is much lower than with SPME-GC-MS. MESI is particularly well suited for the detection of non-polar compounds, therefore number of products identified by this technique is not also to the same degree of SPME. Its main advantage, however, is its ability of (semi-) continuous monitoring, but it is more expensive and not yet commercialized.

Pharmaceutical applications of dynamic mechanical thermal analysis.

PubMed

Jones, David S; Tian, Yiwei; Abu-Diak, Osama; Andrews, Gavin P

2012-04-01

The successful development of polymeric drug delivery and biomedical devices requires a comprehensive understanding of the viscoleastic properties of polymers as these have been shown to directly affect clinical efficacy. Dynamic mechanical thermal analysis (DMTA) is an accessible and versatile analytical technique in which an oscillating stress or strain is applied to a sample as a function of oscillatory frequency and temperature. Through cyclic application of a non-destructive stress or strain, a comprehensive understanding of the viscoelastic properties of polymers may be obtained. In this review, we provide a concise overview of the theory of DMTA and the basic instrumental/operating principles. Moreover, the application of DMTA for the characterization of solid pharmaceutical and biomedical systems has been discussed in detail. In particular we have described the potential of DMTA to measure and understand relaxation transitions and miscibility in binary and higher-order systems and describe the more recent applications of the technique for this purpose. © 2011 Elsevier B.V. All rights reserved.

Publications in biomedical and environmental sciences programs, 1981

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

Moody, J.B.

1982-07-01

This bibliography contains 698 references to articles in journals, books, and reports published in the subject area of biomedical and environmental sciences during 1981. There are 520 references to articles published in journals and books and 178 references to reports. Staff members in the Biomedical and Environmental Sciences divisions have other publications not included in this bibliography; for example, theses, book reviews, abstracts published in journals or symposia proceedings, pending journal publications and reports such as monthly, bimonthly, and quarterly progress reports, contractor reports, and reports for internal distribution. This document is sorted by the division, and then alphabetically bymore » author. The sorting by divisions separates the references by subject area in a simple way. The divisions represented in the order that they appear in the bibliography are Analytical Chemistry, Biology, Chemical Technology, Information R and D, Health and Safety Research, Instrumentation and Controls, Computer Sciences, Energy, Engineering Technology, Solid State, Central Management, Operations, and Environmental Sciences. Indexes are provided by author, title, and journal reference.« less

Analytical instrument with apparatus for sample concentrating

DOEpatents

Zaromb, Solomon

1989-01-01

A system for analysis of trace concentrations of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

A novel flow injection chemiluminescence method for automated and miniaturized determination of phenols in smoked food samples.

PubMed

Vakh, Christina; Evdokimova, Ekaterina; Pochivalov, Aleksei; Moskvin, Leonid; Bulatov, Andrey

2017-12-15

An easily performed fully automated and miniaturized flow injection chemiluminescence (CL) method for determination of phenols in smoked food samples has been proposed. This method includes the ultrasound assisted solid-liquid extraction coupled with gas-diffusion separation of phenols from smoked food sample and analytes absorption into a NaOH solution in a specially designed gas-diffusion cell. The flow system was designed to focus on automation and miniaturization with minimal sample and reagent consumption by inexpensive instrumentation. The luminol - N-bromosuccinimide system in an alkaline medium was used for the CL determination of phenols. The limit of detection of the proposed procedure was 3·10 -8 ·molL -1 (0.01mgkg -1 ) in terms of phenol. The presented method demonstrated to be a good tool for easy, rapid and cost-effective point-of-need screening phenols in smoked food samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Near-Infrared Spatially Resolved Spectroscopy for Tablet Quality Determination.

PubMed

Igne, Benoît; Talwar, Sameer; Feng, Hanzhou; Drennen, James K; Anderson, Carl A

2015-12-01

Near-infrared (NIR) spectroscopy has become a well-established tool for the characterization of solid oral dosage forms manufacturing processes and finished products. In this work, the utility of a traditional single-point NIR measurement was compared with that of a spatially resolved spectroscopic (SRS) measurement for the determination of tablet assay. Experimental designs were used to create samples that allowed for calibration models to be developed and tested on both instruments. Samples possessing a poor distribution of ingredients (highly heterogeneous) were prepared by under-blending constituents prior to compaction to compare the analytical capabilities of the two NIR methods. The results indicate that SRS can provide spatial information that is usually obtainable only through imaging experiments for the determination of local heterogeneity and detection of abnormal tablets that would not be detected with single-point spectroscopy, thus complementing traditional NIR measurement systems for in-line, and in real-time tablet analysis. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Characterization and measurement of natural gas trace constituents. Volume 1. Arsenic. Final report, June 1989-October 1993

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

Chao, S.S.; Attari, A.

1995-01-01

The discovery of arsenic compounds, as alkylarsines, in natural gas prompted this research program to develop reliable measurement techniques needed to assess the efficiency of removal processes for these environmentally sensitive substances. These techniques include sampling, speciation, quantitation and on-line instrumental methods for monitoring the total arsenic concentration. The current program has yielded many products, including calibration standards, arsenic-specific sorbents, sensitive analytical methods and instrumentation. Four laboratory analytical methods have been developed and successfully employed for arsenic determination in natural gas. These methods use GC-AED and GC-MS instruments to speciate alkylarsines, and peroxydisulfate extraction with FIAS, special carbon sorbent withmore » XRF and an IGT developed sorbent with GFAA for total arsenic measurement.« less

Solid-State Thermionic Power Generators: An Analytical Analysis in the Nonlinear Regime

NASA Astrophysics Data System (ADS)

Zebarjadi, M.

2017-07-01

Solid-state thermionic power generators are an alternative to thermoelectric modules. In this paper, we develop an analytical model to investigate the performance of these generators in the nonlinear regime. We identify dimensionless parameters determining their performance and provide measures to estimate an acceptable range of thermal and electrical resistances of thermionic generators. We find the relation between the optimum load resistance and the internal resistance and suggest guidelines for the design of thermionic power generators. Finally, we show that in the nonlinear regime, thermionic power generators can have efficiency values higher than the state-of-the-art thermoelectric modules.

Approximate analytical solution for induction heating of solid cylinders

DOE PAGES

Jankowski, Todd Andrew; Pawley, Norma Helen; Gonzales, Lindsey Michal; ...

2015-10-20

An approximate solution to the mathematical model for induction heating of a solid cylinder in a cylindrical induction coil is presented here. The coupled multiphysics model includes equations describing the electromagnetic field in the heated object, a heat transfer simulation to determine temperature of the heated object, and an AC circuit simulation of the induction heating power supply. A multiple-scale perturbation method is used to solve the multiphysics model. The approximate analytical solution yields simple closed-form expressions for the electromagnetic field and heat generation rate in the solid cylinder, for the equivalent impedance of the associated tank circuit, and formore » the frequency response of a variable frequency power supply driving the tank circuit. The solution developed here is validated by comparing predicted power supply frequency to both experimental measurements and calculated values from finite element analysis for heating of graphite cylinders in an induction furnace. The simple expressions from the analytical solution clearly show the functional dependence of the power supply frequency on the material properties of the load and the geometrical characteristics of the furnace installation. In conclusion, the expressions developed here provide physical insight into observations made during load signature analysis of induction heating.« less

Impact of surface chemistry

PubMed Central

Somorjai, Gabor A.; Li, Yimin

2011-01-01

The applications of molecular surface chemistry in heterogeneous catalyst technology, semiconductor-based technology, medical technology, anticorrosion and lubricant technology, and nanotechnology are highlighted in this perspective. The evolution of surface chemistry at the molecular level is reviewed, and the key roles of surface instrumentation developments for in situ studies of the gas–solid, liquid–solid, and solid–solid interfaces under reaction conditions are emphasized. PMID:20880833

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, Gregory C.; Barinaga, Charles J.; Koppenaal, David W.

1998-01-01

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer.

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, G.C.; Barinaga, C.J.; Koppenaal, D.W.

1998-06-16

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer. 7 figs.

Basic research needs and opportunities on interfaces in solar materials

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

Czanderna, A. W.; Gottschall, R. J.

1981-04-01

The workshop on research needs and recommended research programs on interfaces in solar energy conversion devices was held June 30-July 3, 1980. The papers deal mainly with solid-solid, solid-liquid, and solid-gas interfaces, sometimes involving multilayer solid-solid interfaces. They deal mainly with instrumental techniques of studying these interfaces so they can be optimized, so they can be fabricated with quality control and so changes with time can be forecast. The latter is required because a long lifetime (20 yrs is suggested) is necessary for economic reasons. Fifteen papers have been entered individually into EDB and ERA. (LTN)

Solid-State Division progress report for period ending March 31, 1983

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

Green, P.H.; Watson, D.M.

1983-09-01

Progress and activities are reported on: theoretical solid-state physics (surfaces; electronic, vibrational, and magnetic properties; particle-solid interactions; laser annealing), surface and near-surface properties of solids (surface, plasma-material interactions, ion implantation and ion-beam mixing, pulsed-laser and thermal processing), defects in solids (radiation effects, fracture, impurities and defects, semiconductor physics and photovoltaic conversion), transport properties of solids (fast-ion conductors, superconductivity, mass and charge transport in materials), neutron scattering (small-angle scattering, lattice dynamics, magnetic properties, structure and instrumentation), and preparation and characterization of research materials (growth and preparative methods, nuclear waste forms, special materials). (DLC)

40 CFR 92.102 - Definitions and abbreviations.

Code of Federal Regulations, 2011 CFR

2011-07-01

... engineering practice. Calibration means the act of calibrating an analytical instrument using known standards... be consistent with scientific and engineering principles. Hang-up refers to the process of... reaching the instrument detector. It also refers to any subsequent desorption of the molecules into the...

Introduction to Instrumental Analysis of Water Pollutants. Training Manual.

ERIC Educational Resources Information Center

Office of Water Program Operations (EPA), Cincinnati, OH. National Training and Operational Technology Center.

This course is designed for those requiring an introduction to instruments commonly used in water pollution analyses. Examples are: pH, conductivity, dissolved oxygen meters, spectrophotometers, turbidimeters, carbon analyzer, and gas chromatographs. Students should have a basic knowledge of analytical chemistry. (CO)

ANALYTICAL METHOD COMPARISONS BY ESTIMATES OF PRECISION AND LOWER DETECTION LIMIT

EPA Science Inventory

The paper describes the use of principal component analysis to estimate the operating precision of several different analytical instruments or methods simultaneously measuring a common sample of a material whose actual value is unknown. This approach is advantageous when none of ...

A technique for setting analytical thresholds in massively parallel sequencing-based forensic DNA analysis

PubMed Central

2017-01-01

Amplicon (targeted) sequencing by massively parallel sequencing (PCR-MPS) is a potential method for use in forensic DNA analyses. In this application, PCR-MPS may supplement or replace other instrumental analysis methods such as capillary electrophoresis and Sanger sequencing for STR and mitochondrial DNA typing, respectively. PCR-MPS also may enable the expansion of forensic DNA analysis methods to include new marker systems such as single nucleotide polymorphisms (SNPs) and insertion/deletions (indels) that currently are assayable using various instrumental analysis methods including microarray and quantitative PCR. Acceptance of PCR-MPS as a forensic method will depend in part upon developing protocols and criteria that define the limitations of a method, including a defensible analytical threshold or method detection limit. This paper describes an approach to establish objective analytical thresholds suitable for multiplexed PCR-MPS methods. A definition is proposed for PCR-MPS method background noise, and an analytical threshold based on background noise is described. PMID:28542338

A technique for setting analytical thresholds in massively parallel sequencing-based forensic DNA analysis.

PubMed

Young, Brian; King, Jonathan L; Budowle, Bruce; Armogida, Luigi

2017-01-01

Amplicon (targeted) sequencing by massively parallel sequencing (PCR-MPS) is a potential method for use in forensic DNA analyses. In this application, PCR-MPS may supplement or replace other instrumental analysis methods such as capillary electrophoresis and Sanger sequencing for STR and mitochondrial DNA typing, respectively. PCR-MPS also may enable the expansion of forensic DNA analysis methods to include new marker systems such as single nucleotide polymorphisms (SNPs) and insertion/deletions (indels) that currently are assayable using various instrumental analysis methods including microarray and quantitative PCR. Acceptance of PCR-MPS as a forensic method will depend in part upon developing protocols and criteria that define the limitations of a method, including a defensible analytical threshold or method detection limit. This paper describes an approach to establish objective analytical thresholds suitable for multiplexed PCR-MPS methods. A definition is proposed for PCR-MPS method background noise, and an analytical threshold based on background noise is described.

Sierra/SolidMechanics 4.48 Verification Tests Manual.

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

Plews, Julia A.; Crane, Nathan K; de Frias, Gabriel Jose

2018-03-01

Presented in this document is a small portion of the tests that exist in the Sierra / SolidMechanics (Sierra / SM) verification test suite. Most of these tests are run nightly with the Sierra / SM code suite, and the results of the test are checked versus the correct analytical result. For each of the tests presented in this document, the test setup, a description of the analytic solution, and comparison of the Sierra / SM code results to the analytic solution is provided. Mesh convergence is also checked on a nightly basis for several of these tests. This documentmore » can be used to confirm that a given code capability is verified or referenced as a compilation of example problems. Additional example problems are provided in the Sierra / SM Example Problems Manual. Note, many other verification tests exist in the Sierra / SM test suite, but have not yet been included in this manual.« less

Sierra/SolidMechanics 4.48 Verification Tests Manual.

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

Plews, Julia A.; Crane, Nathan K.; de Frias, Gabriel Jose

Presented in this document is a small portion of the tests that exist in the Sierra / SolidMechanics (Sierra / SM) verification test suite. Most of these tests are run nightly with the Sierra / SM code suite, and the results of the test are checked versus the correct analytical result. For each of the tests presented in this document, the test setup, a description of the analytic solution, and comparison of the Sierra / SM code results to the analytic solution is provided. Mesh convergence is also checked on a nightly basis for several of these tests. This documentmore » can be used to confirm that a given code capability is verified or referenced as a compilation of example problems. Additional example problems are provided in the Sierra / SM Example Problems Manual. Note, many other verification tests exist in the Sierra / SM test suite, but have not yet been included in this manual.« less

Diaion HP-2MG modified with 2-(2,6-dichlorobenzylideneamino) benzenethiol as new adsorbent for solid phase extraction and flame atomic absorption spectrometric determination of metal ions.

PubMed

Ghaedi, M; Montazerozohori, M; Haghdoust, S; Zaare, F; Soylak, M

2013-04-01

A solid phase extraction method for enrichment-separation and the determination of cobalt (Co(2+)), copper (Cu(2+)), nickel (Ni(2+)), zinc (Zn(2+)) and lead (Pb(2+)) ions in real samples has been proposed. The influences of some analytical parameters like pH, flow rate, eluent type and interference of matrix ions on recoveries of analytes were optimized. The limits of detection were found in the range of 1.6-3.9 µg L(-1), while preconcentration factor for all understudy metal ions were found to be 166 with loading half time (t 1/2) less than 10 min. The procedure was applied for the enrichment-separation of analyte ions in environmental samples with recoveries higher than 94.8% and relative SD <4.9% (N = 5).

Verification of spatial and temporal pressure distributions in segmented solid rocket motors

NASA Technical Reports Server (NTRS)

Salita, Mark

1989-01-01

A wide variety of analytical tools are in use today to predict the history and spatial distributions of pressure in the combustion chambers of solid rocket motors (SRMs). Experimental and analytical methods are presented here that allow the verification of many of these predictions. These methods are applied to the redesigned space shuttle booster (RSRM). Girth strain-gage data is compared to the predictions of various one-dimensional quasisteady analyses in order to verify the axial drop in motor static pressure during ignition transients as well as quasisteady motor operation. The results of previous modeling of radial flows in the bore, slots, and around grain overhangs are supported by approximate analytical and empirical techniques presented here. The predictions of circumferential flows induced by inhibitor asymmetries, nozzle vectoring, and propellant slump are compared to each other and to subscale cold air and water tunnel measurements to ascertain their validity.

Injection of coal by screw feed

NASA Technical Reports Server (NTRS)

Fisher, R.

1977-01-01

The use of the screw feeder for injecting solids through a 20 to 30 psi barrier is common practice in the cement making industry. An analytical extrapolation of that design, accounting for pressure holding characteristics of a column of solids, shows that coal can be fed to zones at several hundred psi with minimal or no loss of gas. A series of curves showing the calculated pressure gradient through a moving column of solids is presented. Mean particle size, solids velocity, and column length are parameters. Further study of this system to evaluate practicality is recommended.

Concentration of organic compounds in natural waters with solid-phase dispersion based on advesicle modified silica prior to liquid chromatography.

PubMed

Parisis, Nikolaos A; Giokas, Dimosthenis L; Vlessidis, Athanasios G; Evmiridis, Nicholaos P

2005-12-02

The ability of vesicle-coated silica to aid the extraction of organic compounds from water prior to liquid chromatographic analysis is presented for the first time. The method is based on the formation of silica supported cationic multi-lamellar vesicles of gemini surfactants inherently ensuring the presence of hydrophilic and hydrophobic sites for the partitioning of analytes bearing different properties. Method development is illustrated by studying the adsolubilization of UV absorbing chemicals from swimming pool water. Due to the requirement for external energy input (intense shearing) a method based on solid-phase dispersion (SPD) was applied producing better results than off-line solid-phase extraction (SPE). Meticulous investigation of the experimental parameters was conducted in order to elucidate the mechanisms behind the proposed extraction pattern. Analyte recoveries were quantitative under the optimum experimental conditions offering recoveries higher than 96% with RSD values below 5%.

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

PubMed

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Fifty years of solid-phase extraction in water analysis--historical development and overview.

PubMed

Liska, I

2000-07-14

The use of an appropriate sample handling technique is a must in an analysis of organic micropollutants in water. The efforts to use a solid phase for the recovery of analytes from a water matrix prior to their detection have a long history. Since the first experimental trials using activated carbon filters that were performed 50 years ago, solid-phase extraction (SPE) has become an established sample preparation technique. The initial experimental applications of SPE resulted in widespread use of this technique in current water analysis and also to adoption of SPE into standardized analytical methods. During the decades of its evolution, chromatographers became aware of the advantages of SPE and, despite many innovations that appeared in the last decade, new SPE developments are still expected in the future. A brief overview of 50 years of the history of the use of SPE in organic trace analysis of water is given in presented paper.

Trace and surface analysis of ceramic layers of solid oxide fuel cells by mass spectrometry.

PubMed

Becker, J S; Breuer, U; Westheide, J; Saprykin, A I; Holzbrecher, H; Nickel, H; Dietze, H J

1996-06-01

For the trace analysis of impurities in thick ceramic layers of a solid oxide fuel cell (SOFC) sensitive solid-state mass spectrometric methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and radiofrequency glow discharge mass spectrometry (rf-GDMS) have been developed and used. In order to quantify the analytical results of LA-ICP-MS, the relative sensitivity coefficients of elements in a La(0.6)Sr(0.35)MnO(3) matrix have been determined using synthetic standards. Secondary ion mass spectrometry (SIMS) - as a surface analytical method - has been used to characterize the element distribution and diffusion profiles of matrix elements on the interface of a perovskite/Y-stabilized ZrO(2) layer. The application of different mass spectrometric methods for process control in the preparation of ceramic layers for the SOFC is described.

77 FR 76457 - Howard Hughes Medical Institute, et al.; Notice of Consolidated Decision on Applications for Duty...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-12-28

... chemical state and their catalytic activity in various chemical reactions, by investigating solid... instrument. The unique features of this instrument include its small volume (0.045 L) reaction cell in which...

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

Green, D.W.; Heinrich, R.R.; Graczyk, D.G.

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for fiscal year 1988 (October 1987 through September 1988). The Analytical Chemistry Laboratory is a full-cost recovery service center, with the primary mission of providing a broad range of analytical chemistry support services to the scientific and engineering programs at ANL. In addition, the ACL conducts a research program in analytical chemistry, works on instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems, from routinemore » standard analyses to unique problems that require significant development of methods and techniques.« less

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

Green, D.W.; Heinrich, R.R.; Graczyk, D.G.

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year 1989 (October 1988 through September 1989). The Analytical Chemistry Laboratory is a full-cost-recovery service center, with the primary mission of providing a broad range of analytical chemistry support services to the scientific and engineering programs at ANL. In addition, the ACL conducts a research program in analytical chemistry, works on instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems, from routine standardmore » analyses to unique problems that require significant development of methods and techniques.« less

Laboratory Methods for the Measurement of Pollutants in Water and Waste Effluents

NASA Technical Reports Server (NTRS)

Ballinger, Dwight G.

1971-01-01

The requirement for accurate, precise, and rapid analytical procedures for the examination of water and waste samples requires the use of a variety of instruments. The instrumentation in water laboratories includes atomic absorption, UV-visible. and infrared spectrophotometers, automatic colorimetric analyzers, gas chromatographs and mass spectrometers. Because of the emphasis on regulatory action, attention is being directed toward quality control of analytical results. Among the challenging problems are the differentiation of metallic species in water at nanogram concentrations, rapid measurement of free cyanide and free ammonia, more sensitive methods for arsenic and selenium and improved characterization of organic contaminants.

Load Diffusion in Composite and Smart Structures

NASA Technical Reports Server (NTRS)

Horgan, C. O.

2003-01-01

The research carried out here builds on our previous NASA supported research on the general topic of edge effects and load diffusion in composite structures. Further fundamental solid mechanics studies were carried out to provide a basis for assessing the complicated modeling necessary for the multi-functional large scale structures used by NASA. An understanding of the fundamental mechanisms of load diffusion in composite subcomponents is essential in developing primary composite structures. Some specific problems recently considered were those of end effects in smart materials and structures, study of the stress response of pressurized linear piezoelectric cylinders for both static and steady rotating configurations, an analysis of the effect of pre-stressing and pre-polarization on the decay of end effects in piezoelectric solids and investigation of constitutive models for hardening rubber-like materials. Our goal in the study of load diffusion is the development of readily applicable results for the decay lengths in terms of non-dimensional material and geometric parameters. Analytical models of load diffusion behavior are extremely valuable in building an intuitive base for developing refined modeling strategies and assessing results from finite element analyses. The decay behavior of stresses and other field quantities provides a significant aid towards this process. The analysis is also amenable to parameter study with a large parameter space and should be useful in structural tailoring studies. Special purpose analytical models of load diffusion behavior are extremely valuable in building an intuitive base for developing refined modeling strategies and in assessing results from general purpose finite element analyses. For example, a rational basis is needed in choosing where to use three-dimensional to two-dimensional transition finite elements in analyzing stiffened plates and shells. The decay behavior of stresses and other field quantities furnished by this research provides a significant aid towards this element transition issue. A priori knowledge of the extent of boundary-layers induced by edge effects is also useful in determination of the instrumentation location in structural verification tests or in material characterization tests.

Development of TPS flight test and operational instrumentation

NASA Technical Reports Server (NTRS)

Carnahan, K. R.; Hartman, G. J.; Neuner, G. J.

1975-01-01

Thermal and flow sensor instrumentation was developed for use as an integral part of the space shuttle orbiter reusable thermal protection system. The effort was performed in three tasks: a study to determine the optimum instruments and instrument installations for the space shuttle orbiter RSI and RCC TPS; tests and/or analysis to determine the instrument installations to minimize measurement errors; and analysis using data from the test program for comparison to analytical methods. A detailed review of existing state of the art instrumentation in industry was performed to determine the baseline for the departure of the research effort. From this information, detailed criteria for thermal protection system instrumentation were developed.

Controls for Burning Solid Wastes

ERIC Educational Resources Information Center

Toro, Richard F.; Weinstein, Norman J.

1975-01-01

Modern thermal solid waste processing systems are becoming more complex, incorporating features that require instrumentation and control systems to a degree greater than that previously required just for proper combustion control. With the advent of complex, sophisticated, thermal processing systems, TV monitoring and computer control should…

An Integrated Approach to Thermal Analysis of Pharmaceutical Solids

ERIC Educational Resources Information Center

Riley, Shelley R. Rabel

2015-01-01

A three-tiered experiment for undergraduate Instrumental Analysis students is presented in which students characterize the solid-state thermal behavior of an active pharmaceutical ingredient (acetaminophen) and excipient (a-lactose hydrate) using differential scanning calorimetry, thermogravimetric analysis, and thermal microscopy. Students are…

Validating a Computer-Assisted Language Learning Attitude Instrument Used in Iranian EFL Context: An Evidence-Based Approach

ERIC Educational Resources Information Center

Aryadoust, Vahid; Mehran, Parisa; Alizadeh, Mehrasa

2016-01-01

A few computer-assisted language learning (CALL) instruments have been developed in Iran to measure EFL (English as a foreign language) learners' attitude toward CALL. However, these instruments have no solid validity argument and accordingly would be unable to provide a reliable measurement of attitude. The present study aimed to develop a CALL…

Detection and quantification of cocaine and benzoylecgonine in meconium using solid phase extraction and UPLC/MS/MS.

PubMed

Gunn, Josh; Kriger, Scott; Terrell, Andrea R

2010-01-01

The simultaneous determination and quantification of cocaine and its major metabolite, benzoylecgonine, in meconium using UPLC-MS/MS is described. Ultra-performance liquid chromatography (UPLC) is an emerging analytical technique which draws upon the principles of chromatography to run separations at higher flow rates for increased speed, while simultaneously achieving superior resolution and sensitivity. Extraction of cocaine and benzoylecgonine from the homogenized meconium matrix was achieved with a preliminary protein precipitation or protein 'crash' employing cold acetonitrile, followed by a mixed mode solid phase extraction (SPE). Following elution from the SPE cartridge, eluents were dried down under nitrogen, reconstituted in 200 microL of DI water:acetonitrile (ACN) (75:25), and injected onto the UPLC/MS/MS for analysis. The increased speed and separation efficiency afforded by UPLC, allowed for the separation and subsequent quantification of both analytes in less than 2 min. Analytes were quantified using multiple reaction monitoring (MRM) and six-point calibration curves constructed in negative blood. Limits of detection for both analytes were 3 ng/g and the lower limit of quantitation (LLOQ) was 30 ng/g.

Ionic liquids in solid-phase microextraction: a review.

PubMed

Ho, Tien D; Canestraro, Anthony J; Anderson, Jared L

2011-06-10

Solid-phase microextraction (SPME) has undergone a surge in popularity within the field of analytical chemistry in the past two decades since its introduction. Owing to its nature of extraction, SPME has become widely known as a quick and cost-effective sample preparation technique. Although SPME has demonstrated extraordinary versatility in sampling capabilities, the technique continues to experience a tremendous growth in innovation. Presently, increasing efforts have been directed towards the engineering of novel sorbent material in order to expand the applicability of SPME for a wider range of analytes and matrices. This review highlights the application of ionic liquids (ILs) and polymeric ionic liquids (PILs) as innovative sorbent materials for SPME. Characterized by their unique physico-chemical properties, these compounds can be structurally-designed to selectively extract target analytes based on unique molecular interactions. To examine the advantages of IL and PIL-based sorbent coatings in SPME, the field is reviewed by gathering available experimental data and exploring the sensitivity, linear calibration range, as well as detection limits for a variety of target analytes in the methods that have been developed. Copyright © 2011 Elsevier B.V. All rights reserved.

Magnetic solid-phase extraction using carbon nanotubes as sorbents: a review.

PubMed

Herrero-Latorre, C; Barciela-García, J; García-Martín, S; Peña-Crecente, R M; Otárola-Jiménez, J

2015-09-10

Magnetic solid-phase extraction (M-SPE) is a procedure based on the use of magnetic sorbents for the separation and preconcentration of different organic and inorganic analytes from large sample volumes. The magnetic sorbent is added to the sample solution and the target analyte is adsorbed onto the surface of the magnetic sorbent particles (M-SPs). Analyte-M-SPs are separated from the sample solution by applying an external magnetic field and, after elution with the appropriate solvent, the recovered analyte is analyzed. This approach has several advantages over traditional solid phase extraction as it avoids time-consuming and tedious on-column SPE procedures and it provides a rapid and simple analyte separation that avoids the need for centrifugation or filtration steps. As a consequence, in the past few years a great deal of research has been focused on M-SPE, including the development of new sorbents and novel automation strategies. In recent years, the use of magnetic carbon nanotubes (M-CNTs) as a sorption substrate in M-SPE has become an active area of research. These materials have exceptional mechanical, electrical, optical and magnetic properties and they also have an extremely large surface area and varied possibilities for functionalization. This review covers the synthesis of M-CNTs and the different approaches for the use of these compounds in M-SPE. The performance, general characteristics and applications of M-SPE based on magnetic carbon nanotubes for organic and inorganic analysis have been evaluated on the basis of more than 110 references. Finally, some important challenges with respect the use of magnetic carbon nanotubes in M-SPE are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

The Sample Analysis at Mars Investigation and Instrument Suite

NASA Technical Reports Server (NTRS)

Mahaffy, Paul; Webster, Christopher R.; Conrad, Pamela G.; Arvey, Robert; Bleacher, Lora; Brinckerhoff, William B.; Eigenbrode, Jennifer L.; Chalmers, Robert A.; Dworkin, Jason P.; Errigo, Therese;

First Detection of Non-Chlorinated Organic Molecules Indigenous to a Martian Sample

NASA Technical Reports Server (NTRS)

Freissinet, C.; Glavin, D. P.; Buch, A.; Szopa, C.; Summons, R. E.; Eigenbrode, J. L.; Archer, P. D., Jr.; Brinckerhoff, W. B.; Brunner, A. E.; Cabane, M.;

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI

NASA Astrophysics Data System (ADS)

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-06-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI.

PubMed

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-10-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

Code of Federal Regulations, 2014 CFR

2014-07-01

... (CONTINUED) SOLID WASTES (CONTINUED) HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL Rulemaking Petitions § 260.21... method; (2) A description of the types of wastes or waste matrices for which the proposed method may be... will be incorporated by reference in § 260.11 and added to “Test Methods for Evaluating Solid Waste...

40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

Code of Federal Regulations, 2013 CFR

2013-07-01

... (CONTINUED) SOLID WASTES (CONTINUED) HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL Rulemaking Petitions § 260.21... method; (2) A description of the types of wastes or waste matrices for which the proposed method may be... will be incorporated by reference in § 260.11 and added to “Test Methods for Evaluating Solid Waste...

40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

Code of Federal Regulations, 2012 CFR

2012-07-01

... (CONTINUED) SOLID WASTES (CONTINUED) HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL Rulemaking Petitions § 260.21... method; (2) A description of the types of wastes or waste matrices for which the proposed method may be... will be incorporated by reference in § 260.11 and added to “Test Methods for Evaluating Solid Waste...

EPA Method 525.3 - Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

EPA Science Inventory

Method 525.3 is an analytical method that uses solid phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) for the identification and quantitation of 125 selected semi-volatile organic chemicals in drinking water.

40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

Code of Federal Regulations, 2010 CFR

2010-07-01

... (CONTINUED) SOLID WASTES (CONTINUED) HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL Rulemaking Petitions § 260.21... will be incorporated by reference in § 260.11 and added to “Test Methods for Evaluating Solid Waste... method; (2) A description of the types of wastes or waste matrices for which the proposed method may be...

The role of light microscopy in aerospace analytical laboratories

NASA Technical Reports Server (NTRS)

Crutcher, E. R.

1977-01-01

Light microscopy has greatly reduced analytical flow time and added new dimensions to laboratory capability. Aerospace analytical laboratories are often confronted with problems involving contamination, wear, or material inhomogeneity. The detection of potential problems and the solution of those that develop necessitate the most sensitive and selective applications of sophisticated analytical techniques and instrumentation. This inevitably involves light microscopy. The microscope can characterize and often identify the cause of a problem in 5-15 minutes with confirmatory tests generally less than one hour. Light microscopy has and will make a very significant contribution to the analytical capabilities of aerospace laboratories.

Instrumental Surveillance of Water Quality.

ERIC Educational Resources Information Center

Miller, J. A.; And Others

The role analytical instrumentation performs in the surveillance and control of the quality of water resources is reviewed. Commonly performed analyses may range from simple tests for physical parameters to more highly sophisticated radiological or spectrophotometric methods. This publication explores many of these types of water quality analyses…

The Microcomputer as an Educational Laboratory Workstation.

ERIC Educational Resources Information Center

Ciociolo, James M.

1983-01-01

Describes laboratory workstations which provide direct connection for monitoring and control of analytical instruments such as pH meters, spectrophotometers, temperature, and chromatographic instruments. This is accomplished through analog/digital and digital/analog converters for analog signals and input/output devices for on/off signals.…

Black Boxes in Analytical Chemistry: University Students' Misconceptions of Instrumental Analysis

ERIC Educational Resources Information Center

Carbo, Antonio Domenech; Adelantado, Jose Vicente Gimeno; Reig, Francisco Bosch

2010-01-01

Misconceptions of chemistry and chemical engineering university students concerning instrumental analysis have been established from coordinated tests, tutorial interviews and laboratory lessons. Misconceptions can be divided into: (1) formal, involving specific concepts and formulations within the general frame of chemistry; (2)…

Opening Remarks for "Analytical Chemistry, Monitoring, and Environmental Fate and Transport" Session at Fluoros 2015

EPA Science Inventory

There have been a number of revolutionary developments during the past decade that have led to a much more comprehensive understanding of per- and polyfluoroalkyl substances (PFASs) in the environment. Improvements in analytical instrumentation have made liquid chromatography tri...

Biochemical Applications in the Analytical Chemistry Lab

ERIC Educational Resources Information Center

Strong, Cynthia; Ruttencutter, Jeffrey

2004-01-01

An HPLC and a UV-visible spectrophotometer are identified as instruments that helps to incorporate more biologically-relevant experiments into the course, in order to increase the students understanding of selected biochemistry topics and enhances their ability to apply an analytical approach to biochemical problems. The experiment teaches…

Effect of modulation of the particle size distributions in the direct solid analysis by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; Friedrich K., E. Josue; Redrejo, M. J.

2018-02-01

The main goal of this work was to investigate, in a systematic way, the influence of the controlled modulation of the particle size distribution of a representative solid sample with respect to the more relevant analytical parameters of the Direct Solid Analysis (DSA) by Total-reflection X-Ray Fluorescence (TXRF) quantitative method. In particular, accuracy, uncertainty, linearity and detection limits were correlated with the main parameters of their size distributions for the following elements; Al, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb. In all cases strong correlations were finded. The main conclusion of this work can be resumed as follows; the modulation of particles shape to lower average sizes next to a minimization of the width of particle size distributions, produce a strong increment of accuracy, minimization of uncertainties and limit of detections for DSA-TXRF methodology. These achievements allow the future use of the DSA-TXRF analytical methodology for development of ISO norms and standardized protocols for the direct analysis of solids by mean of TXRF.

Top-down synthesized TiO2 nanowires as a solid matrix for surface-assisted laser desorption/ionization time-of-flight (SALDI-TOF) mass spectrometry.

PubMed

Kim, Jo-Il; Park, Jong-Min; Hwang, Seung-Ju; Kang, Min-Jung; Pyun, Jae-Chul

2014-07-11

Top-down synthesized TiO2 nanowires are presented as an ideal solid matrix to analyze small biomolecules at a m/z of less than 500. The TiO2 nanowires were synthesized as arrays using a modified hydrothermal process directly on the surface of a Ti plate. Finally, the feasibility of the TiO2 nanowires in the anatase phase as a solid matrix. The crystal and electronic structures of the top-down TiO2 nanowires were analyzed at each step of the hydrothermal process, and the optimal TiO2 nanowires were identified by checking their performance toward the ionization of analytes in surface-assisted laser desorption/ionization time-of-flight (SALDI-TOF) mass spectrometry. Finally, the feasibility of the TiO2 nanowires in the anatase phase as a solid matrix for SALDI-TOF mass spectrometry was demonstrated using eight types of amino acids and peptides as model analytes. Copyright © 2014 Elsevier B.V. All rights reserved.

Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD) and Dispersive Solid Phase Extraction (d-SPE) of Plant Samples

PubMed Central

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

Polyaniline (PANI) is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME). In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI) was used for dispersive solid phase extraction (d-SPE) and matrix solid–phase extraction (MSPD). The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD) quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples. PMID:29565297

Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

PubMed

Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

2013-12-04

Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

Split Flow Online Solid-Phase Extraction Coupled with Inductively Coupled Plasma Mass Spectrometry System for One-Shot Data Acquisition of Quantification and Recovery Efficiency.

PubMed

Furukawa, Makoto; Takagai, Yoshitaka

2016-10-04

Online solid-phase extraction (SPE) coupled with inductively coupled plasma mass spectrometry (ICPMS) is a useful tool in automatic sequential analysis. However, it cannot simultaneously quantify the analytical targets and their recovery percentages (R%) in one-shot samples. We propose a system that simultaneously acquires both data in a single sample injection. The main flowline of the online solid-phase extraction is divided into main and split flows. The split flow line (i.e., bypass line), which circumvents the SPE column, was placed on the main flow line. Under program-controlled switching of the automatic valve, the ICPMS sequentially measures the targets in a sample before and after column preconcentration and determines the target concentrations and the R% on the SPE column. This paper describes the system development and two demonstrations to exhibit the analytical significance, i.e., the ultratrace amounts of radioactive strontium ( 90 Sr) using commercial Sr-trap resin and multielement adsorbability on the SPE column. This system is applicable to other flow analyses and detectors in online solid phase extraction.

Analytic Method for Computing Instrument Pointing Jitter

NASA Technical Reports Server (NTRS)

Bayard, David

2003-01-01

A new method of calculating the root-mean-square (rms) pointing jitter of a scientific instrument (e.g., a camera, radar antenna, or telescope) is introduced based on a state-space concept. In comparison with the prior method of calculating the rms pointing jitter, the present method involves significantly less computation. The rms pointing jitter of an instrument (the square root of the jitter variance shown in the figure) is an important physical quantity which impacts the design of the instrument, its actuators, controls, sensory components, and sensor- output-sampling circuitry. Using the Sirlin, San Martin, and Lucke definition of pointing jitter, the prior method of computing the rms pointing jitter involves a frequency-domain integral of a rational polynomial multiplied by a transcendental weighting function, necessitating the use of numerical-integration techniques. In practice, numerical integration complicates the problem of calculating the rms pointing error. In contrast, the state-space method provides exact analytic expressions that can be evaluated without numerical integration.

Mars Geochemical Instrument (MarGI): An instrument for the analysis of the Martian surface and the search for evidence of life

NASA Technical Reports Server (NTRS)

Kojiro, Daniel R.; Mancinelli, Rocco; Martin, Joe; Holland, Paul M.; Stimac, Robert M.; Kaye, William J.

2005-01-01

The Mars Geochemical Instrument, MarGI, was developed to provide a comprehensive analysis of the rocks and surface material on Mars. The instrument combines Differential Thermal Analysis (DTA) with miniature Gas Chromatography-Ion Mobility Spectrometry (GC-IMS) to identify minerals, the presence and state of water, and organic compounds. Miniature pyrolysis ovens are used to both, conduct DTA analysis of soil or crushed rocks samples, and pyrolyze the samples at temperatures up to 1000 degrees C for GC-IMS analysis of the released gases. This combination of analytical processes and techniques, which can characterize the mineralogy of the rocks and soil, and identify and quantify volatiles released during pyrolysis, has applications across a wide range of target sites including comets, planets, asteroids, and moons such as Titan and Europa. The MarGI analytical approach evolved from the Cometary Ice and Dust Experiment (CIDEX) selected to fly on the Comet Rendezvous Asteroid Flyby Mission (CRAF).

Predicting Team Performance through Human Behavioral Sensing and Quantitative Workflow Instrumentation

DTIC Science & Technology

2016-07-27

make risk-informed decisions during serious games . Statistical models of intra- game performance were developed to determine whether behaviors in...specific facets of the gameplay workflow were predictive of analytical performance and games outcomes. A study of over seventy instrumented teams revealed...more accurate game decisions. 2 Keywords: Humatics · Serious Games · Human-System Interaction · Instrumentation · Teamwork · Communication Analysis

Distributed photothermal spectroscopy in microstructured optical fibers: towards high-resolution mapping of gas presence over long distances.

PubMed

Garcia-Ruiz, Andres; Pastor-Graells, Juan; Martins, Hugo F; Tow, Kenny Hey; Thévenaz, Luc; Martin-Lopez, Sonia; Gonzalez-Herraez, Miguel

2017-02-06

Chemical sensing using optical fibers is often challenging, as it is generally difficult to achieve strong interaction between the guided light and the analyte at the wavelength of interest for performing the detection. Despite this difficulty, many schemes exist (and can be found in the literature) for point chemical fiber sensors. However, the challenge increases even further when it comes to performing fully distributed chemical sensing. In this case, the optical signal which interacts with the analyte is typically also the signal that has to travel to and from the interrogator: for a good sensitivity, the light should interact strongly with the analyte, leading inevitably to an increased loss and a reduced range. Few works in the literature actually provide demonstrations of truly distributed chemical sensing and, although there have been several attempts to realize these sensors (e.g. based on special fiber coatings), the vast majority of these attempts has failed to reach widespread use due to several reasons, among them: lack of sensitivity or selectivity, lack of range or resolution, cross sensitivity to temperature or strain, or need to work at specific wavelengths where fiber instrumentation becomes extremely expensive or unavailable. In this work we provide a preliminary demonstration of the possibility of achieving distributed detection of gas presence with spectroscopic selectivity, high spatial resolution, potential for long range measurements and feasibility of having most of the interrogator system working at conventional telecom wavelengths. For a full exploitation of this concept, new fibers (or more likely, fiber bundles) should be developed capable of guiding specific wavelengths in the IR (corresponding to gas absorption wavelengths) with good overlap with the analyte while also having a solid core with good transmission behavior at 1.55 μm, and good thermal coupling between the two guiding structures.

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

PubMed

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Enhanced performance of microfluidic soft pressure sensors with embedded solid microspheres

NASA Astrophysics Data System (ADS)

Shin, Hee-Sup; Ryu, Jaiyoung; Majidi, Carmel; Park, Yong-Lae

2016-02-01

The cross-sectional geometry of an embedded microchannel influences the electromechanical response of a soft microfluidic sensor to applied surface pressure. When a pressure is exerted on the surface of the sensor deforming the soft structure, the cross-sectional area of the embedded channel filled with a conductive fluid decreases, increasing the channel’s electrical resistance. This electromechanical coupling can be tuned by adding solid microspheres into the channel. In order to determine the influence of microspheres, we use both analytic and computational methods to predict the pressure responses of soft microfluidic sensors with two different channel cross-sections: a square and an equilateral triangular. The analytical models were derived from contact mechanics in which microspheres were regarded as spherical indenters, and finite element analysis (FEA) was used for simulation. For experimental validation, sensor samples with the two different channel cross-sections were prepared and tested. For comparison, the sensor samples were tested both with and without microspheres. All three results from the analytical models, the FEA simulations, and the experiments showed reasonable agreement confirming that the multi-material soft structure significantly improved its pressure response in terms of both linearity and sensitivity. The embedded solid particles enhanced the performance of soft sensors while maintaining their flexible and stretchable mechanical characteristic. We also provide analytical and experimental analyses of hysteresis of microfluidic soft sensors considering a resistive force to the shape recovery of the polymer structure by the embedded viscous fluid.

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

Green, D.W.; Heinrich, R.R.; Jensen, K.J.

Technical and administrative activities of the Analytical Chemistry Laboratory (ACL) are reported for fiscal year 1984. The ACL is a full-cost-recovery service center, with the primary mission of providing a broad range of technical support services to the scientific and engineering programs at ANL. In addition, ACL conducts a research program in analytical chemistry, works on instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL is administratively within the Chemical Technology Division, the principal user, but provides technical support for all of the technical divisions and programs at ANL. The ACL has threemore » technical groups - Chemical Analysis, Instrumental Analysis, and Organic Analysis. Under technical activities 26 projects are briefly described. Under professional activities, a list is presented for publications and reports, oral presentations, awards and meetings attended. 6 figs., 2 tabs.« less

A Green Analytical Method Using Ultrasound in Sample Preparation for the Flow Injection Determination of Iron, Manganese, and Zinc in Soluble Solid Samples by Flame Atomic Absorption Spectrometry

PubMed Central

Yebra, M. Carmen

2012-01-01

A simple and rapid analytical method was developed for the determination of iron, manganese, and zinc in soluble solid samples. The method is based on continuous ultrasonic water dissolution of the sample (5–30 mg) at room temperature followed by flow injection flame atomic absorption spectrometric determination. A good precision of the whole procedure (1.2–4.6%) and a sample throughput of ca. 25 samples h–1 were obtained. The proposed green analytical method has been successfully applied for the determination of iron, manganese, and zinc in soluble solid food samples (soluble cocoa and soluble coffee) and pharmaceutical preparations (multivitamin tablets). The ranges of concentrations found were 21.4–25.61 μg g−1 for iron, 5.74–18.30 μg g−1 for manganese, and 33.27–57.90 μg g−1 for zinc in soluble solid food samples and 3.75–9.90 μg g−1 for iron, 0.47–5.05 μg g−1 for manganese, and 1.55–15.12 μg g−1 for zinc in multivitamin tablets. The accuracy of the proposed method was established by a comparison with the conventional wet acid digestion method using a paired t-test, indicating the absence of systematic errors. PMID:22567553

High-Performance X-ray Detection in a New Analytical Electron Microscope

NASA Technical Reports Server (NTRS)

Lyman, C. E.; Goldstein, J. I.; Williams, D. B.; Ackland, D. W.; vonHarrach, S.; Nicholls, A. W.; Statham, P. J.

1994-01-01

X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.

Analysis of methylglyoxal in water and biological matrices by capillary zone electrophoresis with diode array detection.

PubMed

do Rosário, Pedro Miguel Alvaro; Cordeiro, Carlos A Alves; Freire, Ana Ponces; Nogueira, José M Florêncio

2005-05-01

We describe a new method for the determination of methylglyoxal in water and biological matrices, using o-phenylenediamine as derivatizing agent and solid-phase extraction followed by capillary zone electrophoresis with diode array detection. 25 mM sodium phosphate running buffers at pH 2.2, 30 kV, and 25 degrees C allowed the best instrumental conditions for the optimum separation of methylglyoxal in a suitable analytical time (< 10 min), using an uncoated fused-silica capillary of 75 microm inner diameter and an effective length of 45.1 cm with an extended light path and the wavelength set to 200 nm. Under optimized instrumental conditions, good reproducibility of the migration time (< 1.1%), precision (< 5%), an excellent linear dynamic range from 0.1 to 3.6 mg/L (r(2) = 0.9997), and low limits of detection (7.2 microg/L) were obtained for methylglyoxal measurements, using the internal standard methodology. Assays on laboratory-spiked tap and ground water samples allowed a remarkable accuracy, presenting yields of 95.0 +/- 4.3 and 94.0 +/- 1.1%, respectively, and good performance to determine methylglyoxal in beer and yeast cells suspensions matrices was also obtained at trace level. The present methodology is a cost-effective alternative for routine quality control analysis, showing to be reliable, sensitive, and with a low sample volume requirement to monitor methylglyoxal in water and biological matrices.

Initial SAM Calibration Gas Experiments on Mars: Quadrupole Mass Spectrometer Results and Implications

NASA Technical Reports Server (NTRS)

Franz, Heather B.; Trainer, Melissa G.; Malespin, Charles A.; Mahaffy, Paul R.; Atreya, Sushil K.; Becker, Richard H,; Benna, Mehdi; Conrad, Pamela G.; Eigenbrode, Jennifer L.; Freissinet, Caroline;

Design for gas chromatography-corona discharge-ion mobility spectrometry.

PubMed

Jafari, Mohammad T; Saraji, Mohammad; Sherafatmand, Hossein

2012-11-20

A corona discharge ionization-ion mobility spectrometry (CD-IMS) with a novel sample inlet system was designed and constructed as a detector for capillary gas chromatography. In this design, a hollow needle was used instead of a solid needle which is commonly used for corona discharge creation, helping us to have direct axial interfacing for GC-IMS. The capillary column was passed through the needle, resulting in a reaction of effluents with reactant ions on the upstream side of the corona discharge ionization source. Using this sample introduction design, higher ionization efficiency was achieved relative to the entrance direction through the side of the drift tube. In addition, the volume of the ionization region was reduced to minimize the resistance time of compounds in the ionization source, increasing chromatographic resolution of the instrument. The effects of various parameters such as drift gas flow, makeup gas flow, and column tip position inside the needle were investigated. The designed instrument was exhaustively validated in terms of sensitivity, resolution, and reproducibility by analyzing the standard solutions of methyl isobutyl ketone, heptanone, nonanone, and acetophenone as the test compounds. The results obtained by CD-IMS detector were compared with those of the flame ionization detector, which revealed the capability of the proposed GC-IMS for two-dimensional separation (based on the retention time and drift time information) and identification of an analyte in complex matrixes.

Initial SAM calibration gas experiments on Mars: Quadrupole mass spectrometer results and implications

NASA Astrophysics Data System (ADS)

Franz, Heather B.; Trainer, Melissa G.; Malespin, Charles A.; Mahaffy, Paul R.; Atreya, Sushil K.; Becker, Richard H.; Benna, Mehdi; Conrad, Pamela G.; Eigenbrode, Jennifer L.; Freissinet, Caroline; Manning, Heidi L. K.; Prats, Benito D.; Raaen, Eric; Wong, Michael H.

2017-04-01

The Sample Analysis at Mars (SAM) instrument suite of the Mars Science Laboratory (MSL) Curiosity rover is equipped to analyze both martian atmospheric gases and volatiles released by pyrolysis of solid surface materials, with target measurements including chemical and isotopic composition (Mahaffy et al., 2012). To facilitate assessment of instrument performance and validation of results obtained on Mars, SAM houses a calibration cell containing CO2, Ar, N2, Xe, and several fluorinated hydrocarbon compounds (Franz et al., 2014; Mahaffy et al., 2012). This report describes the first two experiments utilizing this calibration cell on Mars and gives results from analysis of data acquired with the SAM Quadrupole Mass Spectrometer (QMS). These data support the accuracy of isotope ratios obtained with the QMS (Conrad et al., 2016; Mahaffy et al., 2013) and provide ground-truth for reassessment of analytical constants required for atmospheric measurements, which were reported in previous contributions (Franz et al., 2015, 2014). The most significant implication of the QMS data involves reinterpretation of pre-launch contamination previously believed to affect only CO abundance measurements (Franz et al., 2015) to affect N2 abundances, as well. The corresponding adjustment to the N2 calibration constant presented here brings the atmospheric volume mixing ratios for Ar and N2 retrieved by SAM into closer agreement with those reported by the Viking mission (Owen et al., 1977; Oyama and Berdahl, 1977).

Miniaturised wireless smart tag for optical chemical analysis applications.

PubMed

Steinberg, Matthew D; Kassal, Petar; Tkalčec, Biserka; Murković Steinberg, Ivana

2014-01-01

A novel miniaturised photometer has been developed as an ultra-portable and mobile analytical chemical instrument. The low-cost photometer presents a paradigm shift in mobile chemical sensor instrumentation because it is built around a contactless smart card format. The photometer tag is based on the radio-frequency identification (RFID) smart card system, which provides short-range wireless data and power transfer between the photometer and a proximal reader, and which allows the reader to also energise the photometer by near field electromagnetic induction. RFID is set to become a key enabling technology of the Internet-of-Things (IoT), hence devices such as the photometer described here will enable numerous mobile, wearable and vanguard chemical sensing applications in the emerging connected world. In the work presented here, we demonstrate the characterisation of a low-power RFID wireless sensor tag with an LED/photodiode-based photometric input. The performance of the wireless photometer has been tested through two different model analytical applications. The first is photometry in solution, where colour intensity as a function of dye concentration was measured. The second is an ion-selective optode system in which potassium ion concentrations were determined by using previously well characterised bulk optode membranes. The analytical performance of the wireless photometer smart tag is clearly demonstrated by these optical absorption-based analytical experiments, with excellent data agreement to a reference laboratory instrument. © 2013 Elsevier B.V. All rights reserved.

Portable light-emitting diode-based photometer with one-shot optochemical sensors for measurement in the field.

PubMed

Palma, A J; Ortigosa, J M; Lapresta-Fernández, A; Fernández-Ramos, M D; Carvajal, M A; Capitán-Vallvey, L F

2008-10-01

This report describes the electronics of a portable, low-cost, light-emitting diode (LED)-based photometer dedicated to one-shot optochemical sensors. Optical detection is made through a monolithic photodiode with an on-chip single-supply transimpedance amplifier that reduces some drawbacks such as leakage currents, interferences, and parasitic capacitances. The main instrument characteristics are its high light source stability and thermal correction. The former is obtained by means of the optical feedback from the LED polarization circuit, implementing a pseudo-two light beam scheme from a unique light source with a built-in beam splitter. The feedback loop has also been used to adjust the LED power in several ranges. Moreover, the low-thermal coefficient achieved (-90 ppm/degrees C) is compensated by thermal monitoring and calibration function compensation in the digital processing. The hand-held instrument directly gives the absorbance ratio used as the analytical parameter and the analyte concentration after programming the calibration function in the microcontroller. The application of this photometer for the determination of potassium and nitrate, using one-shot sensors with ionophore-based chemistries is also demonstrated, with a simple analytical methodology that shortens the analysis time, eliminating some calibrating solutions (HCl, NaOH, and buffer). Therefore, this compact instrument is suitable for real-time analyte determination and operation in the field.

Introduction to the problem

NASA Technical Reports Server (NTRS)

Ramohalli, Kumar

1989-01-01

Solid propellant rockets were used extensively in space missions ranging from large boosters to orbit-raising upper stages. The smaller motors find exclusive use in various earth-based applications. The advantage of the solids include simplicity, readiness, volumetric efficiency, and storability. Important recent progress in related fields (combustion, rheology, micro-instrumentation/diagnostics, and chaos theory) can be applied to solid rockets to derive maximum advantage and avoid waste. Main objectives of research in solid propellants include: to identify critical parameters, to establish specification rules, and to develop quantitative criteria.

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.

Direct-injection mass spectrometric method for the rapid identification of fentanyl and norfentanyl in postmortem urine of six drug-overdose cases.

PubMed

Peer, Cody J; Shakleya, Diaa M; Younis, Islam R; Kraner, James C; Callery, Patrick S

2007-10-01

A rapid mass spectrometric method was developed for the identification of fentanyl and its major hepatic metabolite norfentanyl in postmortem urine of six drug-overdose victims involving fentanyl use. To reduce matrix effects or ion suppression, sample preparation consisted of centrifugation and solid-phase extraction. Deuterium-labeled internal standards ((2)H(5)-fentanyl and (2)H(5)-norfentanyl) were used to compensate for instrument variation in signal, analyte recovery during sample preparation, and ion suppression. Structural information for fentanyl and norfentanyl were collected using mass spectrometry (MS) with electrospray ionization (ESI) operated in the positive ion mode. Fentanyl (m/z 337) was found in each of the six overdose cases by the appearance of the MS-MS daughter ion on both an ion trap and a triple-quadrupole MS resulting from the fragmentation pathway of fentanyl (m/z 337 --> 188). Norfentanyl was detected in all six cases by the appearance of the MH(+) ion, m/z 233, with a single-quadrupole MS and confirmed in an ion trap MS. Ion suppression, as determined by the comparison of ion intensities from spiked samples in water with postmortem urine from the cases, ranged from 18% to 98% in three ESI sources. The use of stable isotope-labeled internal standards obviates sample preparation because ratios of analyte/internal standard remain constant in the presence of extensive matrix effects. This MS method provided sufficient sensitivity and selectivity for the rapid identification of fentanyl and norfentanyl in urine at levels >/= 10 ng/mL without prior analyte resolution by chromatography and with a total analysis time of less than 1 h.

Two-dimensional parallel array technology as a new approach to automated combinatorial solid-phase organic synthesis

PubMed

Brennan; Biddison; Frauendorf; Schwarcz; Keen; Ecker; Davis; Tinder; Swayze

1998-01-01

An automated, 96-well parallel array synthesizer for solid-phase organic synthesis has been designed and constructed. The instrument employs a unique reagent array delivery format, in which each reagent utilized has a dedicated plumbing system. An inert atmosphere is maintained during all phases of a synthesis, and temperature can be controlled via a thermal transfer plate which holds the injection molded reaction block. The reaction plate assembly slides in the X-axis direction, while eight nozzle blocks holding the reagent lines slide in the Y-axis direction, allowing for the extremely rapid delivery of any of 64 reagents to 96 wells. In addition, there are six banks of fixed nozzle blocks, which deliver the same reagent or solvent to eight wells at once, for a total of 72 possible reagents. The instrument is controlled by software which allows the straightforward programming of the synthesis of a larger number of compounds. This is accomplished by supplying a general synthetic procedure in the form of a command file, which calls upon certain reagents to be added to specific wells via lookup in a sequence file. The bottle position, flow rate, and concentration of each reagent is stored in a separate reagent table file. To demonstrate the utility of the parallel array synthesizer, a small combinatorial library of hydroxamic acids was prepared in high throughput mode for biological screening. Approximately 1300 compounds were prepared on a 10 μmole scale (3-5 mg) in a few weeks. The resulting crude compounds were generally >80% pure, and were utilized directly for high throughput screening in antibacterial assays. Several active wells were found, and the activity was verified by solution-phase synthesis of analytically pure material, indicating that the system described herein is an efficient means for the parallel synthesis of compounds for lead discovery. Copyright 1998 John Wiley & Sons, Inc.

Portable and wide-range solid-state transmission densitometer for quality control in film radiography

PubMed Central

Aramburo, Javier Morales; Gonzalez, Sigifredo Solano; Toledo, Jorge Toledo

2010-01-01

In biology, materials science, radiography quality control or film dosimetry in radiotherapy, a transmission densitometer is useful for measurements of optical density. The design proposed here is oriented to quality control in radiographic films. The instrument described here utilizes low-cost solid-state devices and is easy to construct. The use of 1-watt white light-emitting diode in this densitometer enables low power consumption and a cold light source. Moreover, the instrument does not need a reference light, which results in decreasing the number of parts and reducing the overall size of the apparatus. PMID:20927222

The Analog Revolution and Its On-Going Role in Modern Analytical Measurements.

PubMed

Enke, Christie G

2015-12-15

The electronic revolution in analytical instrumentation began when we first exceeded the two-digit resolution of panel meters and chart recorders and then took the first steps into automated control. It started with the first uses of operational amplifiers (op amps) in the analog domain 20 years before the digital computer entered the analytical lab. Their application greatly increased both accuracy and precision in chemical measurement and they provided an elegant means for the electronic control of experimental quantities. Later, laboratory and personal computers provided an unlimited readout resolution and enabled programmable control of instrument parameters as well as storage and computation of acquired data. However, digital computers did not replace the op amp's critical role of converting the analog sensor's output to a robust and accurate voltage. Rather it added a new role: converting that voltage into a number. These analog operations are generally the limiting portions of our computerized instrumentation systems. Operational amplifier performance in gain, input current and resistance, offset voltage, and rise time have improved by a remarkable 3-4 orders of magnitude since their first implementations. Each 10-fold improvement has opened the doors for the development of new techniques in all areas of chemical analysis. Along with some interesting history, the multiple roles op amps play in modern instrumentation are described along with a number of examples of new areas of analysis that have been enabled by their improvements.

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

Hurtubise, R.J.

Interaction models were developed for moisture effects on room-temperature fluorescence (RTF) and room-temperature phosphorescence (RTP) of compounds adsorbed on filter paper. The models described both dynamic and matrix quenching and also related the Young modulus of filter paper to quenching of phosphor on moist filter paper. Photophysical parameters for lumiphors in solution and on solid matrices were compared. Results showed that for some compounds, solid-matrix luminescence has greater analytical potential than solution luminescence. Also, the solid-matrix systems into one of two categories depending on how the intersystem crossing rate constants change with temperature. The first study was carried out onmore » effects of heavy atom on solid-matrix luminescence. With some heavy atoms, maximum solid-matrix phosphorescence quantum yield was obtained at room temperature, and there was no need to use low temperature to obtain a strong phosphorescence signal. By studying solid-matrix luminescence properties of phosphors adsorbed on sodium acetate and deuterated sodium acetate, an interaction model was developed for p-aminobenzoic acid anion adsorbed on sodium acetate. It was shown that the energy-gap law was applicable to solid-matrix luminescence. Also, deuterated phenanthrene and undeuterated phenanthrene were used to study nonradiative transition of excited triplet state of adsorbed phosphors. Heat capacities of several solid matrices were obtained vs temperature and related to vibrational coupling of solid matrix with phosphor. Photophysical study was performed on the hydrolysis products of benzo(a)pyrene-DNA adducts. Also, an analytical method was developed for tetrols in human lung fractions. Work was initiated on the formation of room temperature glasses with glucose and trehalose. Also, work has begun for the development of an oxygen sensor by measuring the RTP quenching of triphenylene on filter paper.« less

Complexometric Determination of Mercury Based on a Selective Masking Reaction

ERIC Educational Resources Information Center

Romero, Mercedes; Guidi, Veronica; Ibarrolaza, Agustin; Castells, Cecilia

2009-01-01

In the first analytical chemistry course, students are introduced to the concepts of equilibrium in water solutions and classical (non-instrumental) analytical methods. Our teaching experience shows that "real samples" stimulate students' enthusiasm for the laboratory work. From this diagnostic, we implemented an optional activity at the end of…

Keeping It Simple: Can We Estimate Malting Quality Potential Using an Isothermal Mashing Protocol and Common Laboratory Instrumentation?

USDA-ARS?s Scientific Manuscript database

Current methods for generating malting quality metrics have been developed largely to support commercial malting and brewing operations, providing accurate, reproducible analytical data to guide malting and brewing production. Infrastructure to support these analytical operations often involves sub...

Combining data visualization and statistical approaches for interpreting measurements and meta-data: Integrating heatmaps, variable clustering, and mixed regression models

EPA Science Inventory

The advent of new higher throughput analytical instrumentation has put a strain on interpreting and explaining the results from complex studies. Contemporary human, environmental, and biomonitoring data sets are comprised of tens or hundreds of analytes, multiple repeat measures...

Social Learning Analytics: Navigating the Changing Settings of Higher Education

ERIC Educational Resources Information Center

de Laat, Maarten; Prinsen, Fleur R.

2014-01-01

Current trends and challenges in higher education (HE) require a reorientation towards openness, technology use and active student participation. In this article we will introduce Social Learning Analytics (SLA) as instrumental in formative assessment practices, aimed at supporting and strengthening students as active learners in increasingly open…

Microprocessor Based Temperature Control of Liquid Delivery with Flow Disturbances.

ERIC Educational Resources Information Center

Kaya, Azmi

1982-01-01

Discusses analytical design and experimental verification of a PID control value for a temperature controlled liquid delivery system, demonstrating that the analytical design techniques can be experimentally verified by using digital controls as a tool. Digital control instrumentation and implementation are also demonstrated and documented for…

Instrumentation: Photodiode Array Detectors in UV-VIS Spectroscopy. Part II.

ERIC Educational Resources Information Center

Jones, Dianna G.

1985-01-01

A previous part (Analytical Chemistry; v57 n9 p1057A) discussed the theoretical aspects of diode ultraviolet-visual (UV-VIS) spectroscopy. This part describes the applications of diode arrays in analytical chemistry, also considering spectroelectrochemistry, high performance liquid chromatography (HPLC), HPLC data processing, stopped flow, and…

Automated Flow-Injection Instrument for Chemiluminescence Detection Using a Low-Cost Photodiode Detector

ERIC Educational Resources Information Center

Economou, A.; Papargyris, D.; Stratis, J.

2004-01-01

The development of an FI analyzer for chemiluminescence detection using a low-cost photoiodide is presented. The experiment clearly demonstrates in a single interdisciplinary project the way in which different aspects in chemical instrumentation fit together to produce a working analytical system.

Selecting Suicide Ideation Assessment Instruments: A Meta-Analytic Review

ERIC Educational Resources Information Center

Erford, Bradley T.; Jackson, Jessica; Bardhoshi, Gerta; Duncan, Kelly; Atalay, Zumra

2018-01-01

Psychometric meta-analyses and reviews were provided for four commonly used suicidal ideation instruments: the Beck Scale for Suicide Ideation, the Suicide Ideation Questionnaire, the Suicide Probability Scale, and Columbia--Suicide Severity Rating Scale. Practical and technical issues and best use recommendations for screening and outcome…

Report on Cosmic Dust Capture Research and Development for the Exobiology Program

NASA Technical Reports Server (NTRS)

Nishioka, Kenji

1997-01-01

Collaboration with Ames' personnel was in: 1) grant administration, 2) intellectual science support, 3) collaboration with the University of Paris for the Mir flight experiment, and 4) arranging scanning and X-ray probe analytical support from UCB and SUNYP. LNIMS provided access to: 1) analytical research instruments, 2) chemical analyses support, 3) cleanroom facilities, and 4) design and fabrication expertise of hardware and electronics. They also supported the hypervelocity testing along with test data acquisition and its reduction for the breadboard instrument. A&M Associates provided technical expertise and support on determining the expected charges on orbital particles and a conceptual design for a breadboard particle charge detection sensor. University of California provided analytical support for the recovered Mir flight modules using their unique scanning capability to detect particle tracks in the aerogel. SUNYP, along with help from the University of Chicago, analyzed particle tracks found in the aerogel for biogenic compounds using an x-ray probe instrument. Dr. Schultz provided access to his experiments and the benefits of his considerable hyper-velocity testing expertise at the Ames hypervelocity gun facility, and this proved beneficial to our development testing, significantly reducing the test time and cost for the breadboard instrument development testing. The participants in this activity acknowledge and thank the National Aeronautics and Space Administration and its Ames Research Center for providing the necessary support and resources to conduct this investigation on instrument technology for exobiology application and being able to acquire some interesting results. Primarily, the newly identified technology problems for future research are the important results of this research.

Point-of-care urine albumin in general practice offices: effect of participation in an external quality assurance scheme.

PubMed

Bukve, Tone; Røraas, Thomas; Riksheim, Berit Oddny; Christensen, Nina Gade; Sandberg, Sverre

2015-01-01

The Norwegian Quality Improvement of Primary Care Laboratories (Noklus) offers external quality assurance (EQA) schemes (EQASs) for urine albumin (UA) annually. This study analyzed the EQA results to determine how the analytical quality of UA analysis in general practice (GP) offices developed between 1998 (n=473) and 2012 (n=1160). Two EQA urine samples were distributed yearly to the participants by mail. The participants measured the UA of each sample and returned the results together with information about their instrument, the profession and number of employees at the office, frequency of internal quality control (IQC), and number of analyses per month. In the feedback report, they received an assessment of their analytical performance. The number of years that the GP office had participated in Noklus was inversely related to the percentage of "poor" results for quantitative but not semiquantitative instruments. The analytical quality improved for participants using quantitative instruments who received an initial assessment of "poor" and who subsequently changed their instrument. Participants using reagents that had expired or were within 3 months of the expiration date performed worse than those using reagents that were expiring in more than 3 months. Continuous participation in the Noklus program improved the performance of quantitative UA analyses at GP offices. This is probably in part attributable to the complete Noklus quality system, whereby in addition to participating in EQAS, participants are visited by laboratory consultants who examine their procedures and provide practical advice and education regarding the use of different instruments.

A Laboratory-Based System for Managing and Distributing Publically Funded Geochemical Data in a Collaborative Environment

NASA Astrophysics Data System (ADS)

McInnes, B.; Brown, A.; Liffers, M.

2015-12-01

Publically funded laboratories have a responsibility to generate, archive and disseminate analytical data to the research community. Laboratory managers know however, that a long tail of analytical effort never escapes researchers' thumb drives once they leave the lab. This work reports on a research data management project (Digital Mineralogy Library) where integrated hardware and software systems automatically archive and deliver analytical data and metadata to institutional and community data portals. The scientific objective of the DML project was to quantify the modal abundance of heavy minerals extracted from key lithological units in Western Australia. The selected analytical platform was a TESCAN Integrated Mineral Analyser (TIMA) that uses EDS-based mineral classification software to image and quantify mineral abundance and grain size at micron scale resolution. The analytical workflow used a bespoke laboratory information management system (LIMS) to orchestrate: (1) the preparation of grain mounts with embedded QR codes that serve as enduring links between physical samples and analytical data, (2) the assignment of an International Geo Sample Number (IGSN) and Digital Object Identifier (DOI) to each grain mount via the System for Earth Sample Registry (SESAR), (3) the assignment of a DOI to instrument metadata via Research Data Australia, (4) the delivery of TIMA analytical outputs, including spatially registered mineralogy images and mineral abundance data, to an institutionally-based data management server, and (5) the downstream delivery of a final data product via a Google Maps interface such as the AuScope Discovery Portal. The modular design of the system permits the networking of multiple instruments within a single site or multiple collaborating research institutions. Although sharing analytical data does provide new opportunities for the geochemistry community, the creation of an open data network requires: (1) adopting open data reporting standards and conventions, (2) requiring instrument manufacturers and software developers to deliver and process data in formats compatible with open standards, and (3) public funding agencies to incentivise researchers, laboratories and institutions to make their data open and accessible to consumers.

Sample analysis at Mars

NASA Astrophysics Data System (ADS)

Coll, P.; Cabane, M.; Mahaffy, P. R.; Brinckerhoff, W. B.; Sam Team

The next landed missions to Mars, such as the planned Mars Science Laboratory and ExoMars, will require sample analysis capabilities refined well beyond what has been flown to date. A key science objective driving this requirement is the determination of the carbon inventory of Mars, and particularly the detection of organic compounds. The Sample Analysis at Mars (SAM) suite consists of a group of tightly-integrated experiments that would analyze samples delivered directly from a coring drill or by a facility sample processing and delivery (SPAD) mechanism. SAM consists of an advanced GC/MS system and a laser desorption mass spectrometer (LDMS). The combined capabilities of these techniques can address Mars science objectives with much improved sensitivity, resolution, and analytical breadth over what has been previously possible in situ. The GC/MS system analyzes the bulk composition (both molecular and isotopic) of solid-phase and atmospheric samples. Solid samples are introduced with a highly flexible chemical derivatization/pyrolysis subsystem (Pyr/GC/MS) that is significantly more capable than the mass spectrometers on Viking. The LDMS analyzes local elemental and molecular composition in solid samples vaporized and ionized with a pulsed laser. We will describe how each of these capabilities has particular strengths that can achieve key measurement objectives at Mars. In addition, the close codevelopment of the GC/MS and LDMS along with a sample manipulation system enables the the sharing of resources, the correlation of results, and the utilization of certain approaches that would not be possible with separate instruments. For instance, the same samples could be analyzed with more than one technique, increasing efficiency and providing cross-checks for quantification. There is also the possibility of combining methods, such as by permitting TOF-MS analyses of evolved gas (Pyr/EI-TOF-MS) or GC/MS analyses of laser evaporated gas (LD-GC/MS).

Computational methods in preformulation study for pharmaceutical solid dosage forms of therapeutic proteins

NASA Astrophysics Data System (ADS)

Majee, Sutapa Biswas; Biswas, Gopa Roy

2017-06-01

Design and delivery of protein-based biopharmaceuticals needs detailed planning and strict monitoring of intermediate processing steps, storage conditions and container-closure system to ensure a stable, elegant and biopharmaceutically acceptable dosage form. Selection of manufacturing process variables and conditions along with packaging specifications can be achieved through properly designed preformulation study protocol for the formulation. Thermodynamic stability and biological activity of therapeutic proteins depend on folding-unfolding and three-dimensional packing dynamics of amino acid network in the protein molecule. Lack of favourable environment may cause protein aggregation with loss in activity and even fatal immunological reaction. Although lyophilization can enhance the stability of protein-based formulations in the solid state, it can induce protein unfolding leading to thermodynamic instability. Formulation stabilizers such as preservatives can also result in aggregation of therapeutic proteins. Modern instrumental techniques in conjunction with computational tools enable rapid and accurate prediction of amino acid sequence, thermodynamic parameters associated with protein folding and detection of aggregation "hot-spots." Globular proteins pose a challenge during investigations on their aggregation propensity. Biobetter therapeutic monoclonal antibodies with enhanced stability, solubility and reduced immunogenic potential can be designed through mutation of aggregation-prone zones. The objective of the present review article is to focus on the various analytical methods and computational approaches used in the study of thermodynamic stability and aggregation tendency of therapeutic proteins, with an aim to develop optimal and marketable formulation. Knowledge of protein dynamics through application of computational tools will provide the essential inputs and relevant information for successful and meaningful completion of preformulation studies on solid dosage forms of therapeutic proteins.

Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

PubMed

Masuck, Ines; Hutzler, Christoph; Luch, Andreas

2010-04-30

In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

Estimation of the curvature of the solid liquid interface during Bridgman crystal growth

NASA Astrophysics Data System (ADS)

Barat, Catherine; Duffar, Thierry; Garandet, Jean-Paul

1998-11-01

An approximate solution for the solid/liquid interface curvature due to the crucible effect in crystal growth is derived from simple heat flux considerations. The numerical modelling of the problem carried out with the help of the finite element code FIDAP supports the predictions of our analytical expression and allows to identify its range of validity. Experimental interface curvatures, measured in gallium antimonide samples grown by the vertical Bridgman method, are seen to compare satisfactorily to analytical and numerical results. Other literature data are also in fair agreement with the predictions of our models in the case where the amount of heat carried by the crucible is small compared to the overall heat flux.

Modeling of vortex generated sound in solid propellant rocket motors

NASA Technical Reports Server (NTRS)

Flandro, G. A.

1980-01-01

There is considerable evidence based on both full scale firings and cold flow simulations that hydrodynamically unstable shear flows in solid propellant rocket motors can lead to acoustic pressure fluctuations of significant amplitude. Although a comprehensive theoretical understanding of this problem does not yet exist, procedures were explored for generating useful analytical models describing the vortex shedding phenomenon and the mechanisms of coupling to the acoustic field in a rocket combustion chamber. Since combustion stability prediction procedures cannot be successful without incorporation of all acoustic gains and losses, it is clear that a vortex driving model comparable in quality to the analytical models currently employed to represent linear combustion instability must be formulated.

Silicon Sheet Quality is Improved By Meniscus Control

NASA Technical Reports Server (NTRS)

Yates, D. A.; Hatch, A. E.; Goldsmith, J. M.

1983-01-01

Better quality silicon crystals for solar cells are possible with instrument that monitors position of meniscus as sheet of solid silicon is drawn from melt. Using information on meniscus height, instrument generates feedback signal to control melt temperature. Automatic control ensures more uniform silicon sheets.

Numerical and analytical simulation of the production process of ZrO2 hollow particles

NASA Astrophysics Data System (ADS)

Safaei, Hadi; Emami, Mohsen Davazdah

2017-12-01

In this paper, the production process of hollow particles from the agglomerated particles is addressed analytically and numerically. The important parameters affecting this process, in particular, the initial porosity level of particles and the plasma gun types are investigated. The analytical model adopts a combination of quasi-steady thermal equilibrium and mechanical balance. In the analytical model, the possibility of a solid core existing in agglomerated particles is examined. In this model, a range of particle diameters (50μm ≤ D_{p0} ≤ 160 μ m) and various initial porosities ( 0.2 ≤ p ≤ 0.7) are considered. The numerical model employs the VOF technique for two-phase compressible flows. The production process of hollow particles from the agglomerated particles is simulated, considering an initial diameter of D_{p0} = 60 μm and initial porosity of p = 0.3, p = 0.5, and p = 0.7. Simulation results of the analytical model indicate that the solid core diameter is independent of the initial porosity, whereas the thickness of the particle shell strongly depends on the initial porosity. In both models, a hollow particle may hardly develop at small initial porosity values ( p < 0.3), while the particle disintegrates at high initial porosity values ( p > 0.6.

One-calibrant kinetic calibration for on-site water sampling with solid-phase microextraction.

PubMed

Ouyang, Gangfeng; Cui, Shufen; Qin, Zhipei; Pawliszyn, Janusz

2009-07-15

The existing solid-phase microextraction (SPME) kinetic calibration technique, using the desorption of the preloaded standards to calibrate the extraction of the analytes, requires that the physicochemical properties of the standard should be similar to those of the analyte, which limited the application of the technique. In this study, a new method, termed the one-calibrant kinetic calibration technique, which can use the desorption of a single standard to calibrate all extracted analytes, was proposed. The theoretical considerations were validated by passive water sampling in laboratory and rapid water sampling in the field. To mimic the variety of the environment, such as temperature, turbulence, and the concentration of the analytes, the flow-through system for the generation of standard aqueous polycyclic aromatic hydrocarbons (PAHs) solution was modified. The experimental results of the passive samplings in the flow-through system illustrated that the effect of the environmental variables was successfully compensated with the kinetic calibration technique, and all extracted analytes can be calibrated through the desorption of a single calibrant. On-site water sampling with rotated SPME fibers also illustrated the feasibility of the new technique for rapid on-site sampling of hydrophobic organic pollutants in water. This technique will accelerate the application of the kinetic calibration method and also will be useful for other microextraction techniques.

High throughput liquid absorption preconcentrator sampling instrument

DOEpatents

Zaromb, Solomon; Bozen, Ralph M.

1992-01-01

A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis.

High throughput liquid absorption preconcentrator sampling instrument

DOEpatents

Zaromb, S.; Bozen, R.M.

1992-12-22

A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis. 12 figs.

Analytical Solutions of the KDV-KZK Equation

NASA Astrophysics Data System (ADS)

Gan, W. S.

The KdV-KZK equation for fluids developed by me was presented at the ICSV 11 in St. Petersburg in July 2004. In this paper, I made an attempt on the analytical solutions of this equation using the perturbation method. Some physical interpretation of the solutions is given. A brief introduction to KdV-KZK equation for solids is given

Construction of a Chemical Sensor/Instrumentation Package Using Fiber Optic and Miniaturization Technology

NASA Technical Reports Server (NTRS)

Newton, R. L.

1999-01-01

The objective of this research was to construct a chemical sensor/instrumentation package that was smaller in weight and volume than conventional instrumentation. This reduction in weight and volume is needed to assist in further reducing the cost of launching payloads into space. To accomplish this, fiber optic sensors, miniaturized spectrometers, and wireless modems were employed. The system was evaluated using iodine as a calibration analyte.

Solid-state 27Al MRI and NMR thermometry for catalytic applications with conventional (liquids) MRI instrumentation and techniques.

PubMed

Koptyug, Igor V; Sagdeev, Dmitry R; Gerkema, Edo; Van As, Henk; Sagdeev, Renad Z

2005-07-01

Multidimensional images of Al2O3 pellets, cordierite monolith, glass tube, polycrystalline V2O5 and other materials have been detected by 27Al, 51V, and 23Na NMR imaging using techniques and instrumentation conventionally employed for imaging of liquids. These results demonstrate that, contrary to the widely accepted opinion, imaging of "rigid" solids does not necessarily require utilization of solid state NMR imaging approaches, pulse sequences and hardware even for quadrupolar nuclei which exhibit line widths in excess of 100 kHz, such as 51V in polycrystalline V2O5. It is further demonstrated that both 27Al NMR signal intensity and spin-lattice relaxation time decrease with increasing temperature and thus can potentially serve as temperature sensitive parameters for spatially resolved NMR thermometry.

Detection and Quantification of Nitrogen Compounds in the First Drilled Martian Solid Samples by the Sample Analysis at Mars (SAM) Instrument Suite on the Mars Science Laboratory (MSL)

NASA Technical Reports Server (NTRS)

Stern, Jennifer C.; Navarro-Gonzalez, Rafael; Freissinet, Caroline; McKay, Christopher P.; Archer, P. Douglas, Jr.; Buch, Arnaud; Coll, Patrice; Eigenbrode, Jennifer L.; Franz, Heather B.; Glavin, Daniel P.;

Solid-State Gas Sensors: Sensor System Challenges in the Civil Security Domain.

PubMed

Müller, Gerhard; Hackner, Angelika; Beer, Sebastian; Göbel, Johann

2016-01-20

The detection of military high explosives and illicit drugs presents problems of paramount importance in the fields of counter terrorism and criminal investigation. Effectively dealing with such threats requires hand-portable, mobile and affordable instruments. The paper shows that solid-state gas sensors can contribute to the development of such instruments provided the sensors are incorporated into integrated sensor systems, which acquire the target substances in the form of particle residue from suspect objects and which process the collected residue through a sequence of particle sampling, solid-vapor conversion, vapor detection and signal treatment steps. Considering sensor systems with metal oxide gas sensors at the backend, it is demonstrated that significant gains in sensitivity, selectivity and speed of response can be attained when the threat substances are sampled in particle as opposed to vapor form.

Solid-State Gas Sensors: Sensor System Challenges in the Civil Security Domain

PubMed Central

Müller, Gerhard; Hackner, Angelika; Beer, Sebastian; Göbel, Johann

2016-01-01

The detection of military high explosives and illicit drugs presents problems of paramount importance in the fields of counter terrorism and criminal investigation. Effectively dealing with such threats requires hand-portable, mobile and affordable instruments. The paper shows that solid-state gas sensors can contribute to the development of such instruments provided the sensors are incorporated into integrated sensor systems, which acquire the target substances in the form of particle residue from suspect objects and which process the collected residue through a sequence of particle sampling, solid-vapor conversion, vapor detection and signal treatment steps. Considering sensor systems with metal oxide gas sensors at the backend, it is demonstrated that significant gains in sensitivity, selectivity and speed of response can be attained when the threat substances are sampled in particle as opposed to vapor form. PMID:28787865

Ammonia Monitor

NASA Technical Reports Server (NTRS)

Sauer, Richard L. (Inventor); Akse, James R. (Inventor); Thompson, John O. (Inventor); Atwater, James E. (Inventor)

1999-01-01

Ammonia monitor and method of use are disclosed. A continuous, real-time determination of the concentration of ammonia in an aqueous process stream is possible over a wide dynamic range of concentrations. No reagents are required because pH is controlled by an in-line solid-phase base. Ammonia is selectively transported across a membrane from the process stream to an analytical stream to an analytical stream under pH control. The specific electrical conductance of the analytical stream is measured and used to determine the concentration of ammonia.

An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

ERIC Educational Resources Information Center

Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

2015-01-01

While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

Solid state electro-optic color filter and iris

NASA Technical Reports Server (NTRS)

1974-01-01

Test results obtained have confirmed the practicality of the solid state electro-optic filters as an optical control element in a television system. Neutral-density control range in excess of 1000:1 has been obtained on sample filters. Test results, measurements in a complete camera system, discussions of problem areas, analytical comparisons, and recommendations for future investigations are included.

Breckinridge Project, initial effort

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

None

1982-01-01

Report V, Volume 4 provides descriptions, data, and drawings pertaining to Instrument and Plant Air Systems (Plant 36), Telecommunication Systems (Plant 37), Inert Gas Systems (Plant 38), Purge and Flush Oil Systems (Plant 39), Site Development and Roads (Plant 40), Buildings (Plant 41), Solid Waste Management (Plant 42), and Landfill (Plant 44). Instrument and Plant Air Systems (Plant 36) includes all equipment and piping necessary to supply instrument and utility air to the process plants and offsite facilities. Telecommunication Systems (Plant 37) includes the equipment and wiring for: communication throughout the facility; communication between plant data processing systems and offsitemore » computing facilities; and communication with transportation carriers. Inert Gas Systems (Plant 38) provides high purity and low purity nitrogen streams for plant startup and normal operation. Purge and Flush Oil Systems (Plant 39) provides purge and flush oils to various plants. Site Development and Roads (Plant 40) provides site leveling, the addition of roads, fencing, and drainage, and the placement of fills, pilings, footings, and foundations for plants. Buildings (Plant 41) provides buildings for equipment and for personnel, including utilities, lighting, sanitary facilities, heating, air conditioning, and ventilation. Solid Waste Management (Plant 42) identifies, characterizes, segregates, and transports the various types of solid wastes to either Landfill (Plant 44) or outside disposal sites. Landfill (Plant 44) provides disposal of both nonhazardous and hazardous solid wastes. Information is included (as applicable) for each of the eight plants described.« less

INVESTIGATION OF RESPONSE DIFFERENCES BETWEEN DIFFERENT TYPES OF TOTAL ORGANIC CARBON (TOC) ANALYTICAL INSTRUMENT SYSTEMS

EPA Science Inventory

Total organic carbon (TOC) and dissolved organic carbon (DOC) have long been used to estimate the amount of natural organic matter (NOM) found in raw and finished drinking water. In recent years, computer automation and improved instrumental analysis technologies have created a ...

Existential Measurement: A Factor Analytic Study of Some Current Psychometric Instruments.

ERIC Educational Resources Information Center

Thauberger, Patrick C.; And Others

1982-01-01

Research in existentialism and ontology has given rise to several psychometric instruments. Used both exploratory and confirmatory principal-factor analyses to study relationships among 16 existential scales. Exploratory factor analysis provided some support of the theory that the avoidance of existential confrontation is a central function of…

THE COST-EFFECTIVENESS OF ALTERNATIVE INSTRUMENTS FOR ENVIRONMENTAL PROTECTION IN A SECOND-BEST SETTING. (R825313)

EPA Science Inventory

Abstract

This paper employs analytical and numerical general equilibrium models to examine the significance of pre-existing factor taxes for the costs of pollution reduction under a wide range of environmental policy instruments. Pre-existing taxes imply significantly ...

VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

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

Ekechukwu, A.

This document proposes to provide a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers, and books reviewed is given in Appendix 1. Available validation documents and guides are listed in the appendix; each has a brief description of application and use. In the referenced sources, there are varying approaches to validation and varying descriptions of validation at different stages in method development. This discussion focuses onmore » validation and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all documents were published in English.« less

Insights into the varnishes of historical musical instruments using synchrotron micro-analytical methods

NASA Astrophysics Data System (ADS)

Echard, J.-P.; Cotte, M.; Dooryhee, E.; Bertrand, L.

2008-07-01

Though ancient violins and other stringed instruments are often revered for the beauty of their varnishes, the varnishing techniques are not much known. In particular, very few detailed varnish analyses have been published so far. Since 2002, a research program at the Musée de la musique (Paris) is dedicated to a detailed description of varnishes on famous ancient musical instruments using a series of novel analytical methods. For the first time, results are presented on the study of the varnish from a late 16th century Venetian lute, using synchrotron micro-analytical methods. Identification of both organic and inorganic compounds distributed within the individual layers of a varnish microsample has been performed using spatially resolved synchrotron Fourier transform infrared microscopy. The univocal identification of the mineral phases is obtained through synchrotron powder X-ray diffraction. The materials identified may be of utmost importance to understand the varnishing process and its similarities with some painting techniques. In particular, the proteinaceous binding medium and the calcium sulfate components (bassanite and anhydrite) that have been identified in the lower layers of the varnish microsample could be related, to a certain extent, to the ground materials of earlier Italian paintings.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

Selective solid-phase extraction based on molecularly imprinted technology for the simultaneous determination of 20 triazole pesticides in cucumber samples using high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Zhao, Fengnian; She, Yongxin; Zhang, Chao; Cao, Xiaolin; Wang, Shanshan; Zheng, Lufei; Jin, Maojun; Shao, Hua; Jin, Fen; Wang, Jing

2017-10-01

A selective analytical method for the simultaneous determination of 20 triazole fungicides and plant growth regulators in cucumber samples was developed using solid-phase extraction with specific molecularly imprinted polymers (MIPs) as adsorbents. The MIPs were successfully prepared by precipitation polymerization using triadimefon as the template molecule, methacrylic acid as the functional monomer, trimethylolpropane trimethacrylate as the crosslinker, and acetonitrile as the porogen. The performance and recognition mechanism for both the MIPs and non-molecularly imprinted polymers were evaluated using adsorption isotherms and adsorption kinetics. Liquid chromatography-tandem quadrupole mass spectrometry was used to identify and quantify the target analytes. The solid-phase extraction using the MIPs was rapid, convenient, and efficient for extraction and enrichment of the 20 triazole pesticides from cucumber samples. The recoveries obtained at three concentration levels (1, 2, and 10μgL -1 ) ranged from 82.3% to 117.6% with relative standard deviations of less than 11.8% (n=5) for all analytes. The limits of detection for the 20 triazole pesticides were all less than 0.4μgL -1 , and were sufficient to meet international standards. Copyright © 2017 Elsevier B.V. All rights reserved.

3D Printed Surgical Instruments: The Design and Fabrication Process.

PubMed

George, Mitchell; Aroom, Kevin R; Hawes, Harvey G; Gill, Brijesh S; Love, Joseph

2017-01-01

3D printing is an additive manufacturing process allowing the creation of solid objects directly from a digital file. We believe recent advances in additive manufacturing may be applicable to surgical instrument design. This study investigates the feasibility, design and fabrication process of usable 3D printed surgical instruments. The computer-aided design package SolidWorks (Dassault Systemes SolidWorks Corp., Waltham MA) was used to design a surgical set including hemostats, needle driver, scalpel handle, retractors and forceps. These designs were then printed on a selective laser sintering (SLS) Sinterstation HiQ (3D Systems, Rock Hill SC) using DuraForm EX plastic. The final printed products were evaluated by practicing general surgeons for ergonomic functionality and performance, this included simulated surgery and inguinal hernia repairs on human cadavers. Improvements were identified and addressed by adjusting design and build metrics. Repeated manufacturing processes and redesigns led to the creation of multiple functional and fully reproducible surgical sets utilizing the user feedback of surgeons. Iterative cycles including design, production and testing took an average of 3 days. Each surgical set was built using the SLS Sinterstation HiQ with an average build time of 6 h per set. Functional 3D printed surgical instruments are feasible. Advantages compared to traditional manufacturing methods include no increase in cost for increased complexity, accelerated design to production times and surgeon specific modifications.

ASSESSMENT OF INSTRUMENTATION FOR MONITORING COAL FLOWRATE AND COMPOSITION

EPA Science Inventory

The report gives results of an assessment of instrumentation for the measurement of coal flowrate (either as a dry solid or in a coal/water slurry) and composition. Also investigated was the appropriateness of EPA/IERL-RTP involvement in the development or evaluation of such devi...

Instrument report: Planetary X-ray experiment

NASA Technical Reports Server (NTRS)

Anderson, K. A.

1972-01-01

Design studies for an X-ray experiment to investigate planetary magnetospheres using solid state detectors, or proportional counters are reported. The detectors, background counting rate, and leakage fluxes are discussed. It is concluded that the best choice of instruments appears to be two separate multiproportional counters for redundancy.

Application of the endochronic theory of viscoplasticity to solid propellants and sandasphalt concrete

NASA Technical Reports Server (NTRS)

Peng, S. T. J.; Valanis, K. C.

1977-01-01

Solid propellants, sand-asphalt concrete and hard plastics showed rate sensitive mechanical behavior which, in addition, indicated that these materials have a permanent memory of the strain (or loading) path by which their present state was attained. A constitutive equation was formulated in general three dimensional tensorial form by means of irreversible thermodynamics. By using a very simple analytical form, it was shown that the mechanical behavior of solid propellants and sand-asphalt concrete can be readily described.

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

PubMed

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Detecting Learning Strategies with Analytics: Links with Self-Reported Measures and Academic Performance

ERIC Educational Resources Information Center

Gaševic, Dragan; Jovanovic, Jelena; Pardo, Abelardo; Dawson, Shane

2017-01-01

The use of analytic methods for extracting learning strategies from trace data has attracted considerable attention in the literature. However, there is a paucity of research examining any association between learning strategies extracted from trace data and responses to well-established self-report instruments and performance scores. This paper…

Instrumental Analysis of Biodiesel Content in Commercial Diesel Blends: An Experiment for Undergraduate Analytical Chemistry

ERIC Educational Resources Information Center

Feng, Z. Vivian; Buchman, Joseph T.

2012-01-01

The potential of replacing petroleum fuels with renewable biofuels has drawn significant public interest. Many states have imposed biodiesel mandates or incentives to use commercial biodiesel blends. We present an inquiry-driven experiment where students are given the tasks to gather samples, develop analytical methods using various instrumental…

40 CFR Appendix B to Part 136 - Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11

Code of Federal Regulations, 2012 CFR

2012-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES... to a wide variety of sample types ranging from reagent (blank) water containing analyte to wastewater... times the standard deviation of replicate instrumental measurements of the analyte in reagent water. (c...

Evaluation of a reconfigurable portable instrument for copper determination based on luminescent carbon dots.

PubMed

Salinas-Castillo, Alfonso; Morales, Diego P; Lapresta-Fernández, Alejandro; Ariza-Avidad, María; Castillo, Encarnación; Martínez-Olmos, Antonio; Palma, Alberto J; Capitan-Vallvey, Luis Fermin

2016-04-01

A portable reconfigurable platform for copper (Cu(II)) determination based on luminescent carbon dot (Cdots) quenching is described. The electronic setup consists of a light-emitting diode (LED) as the carbon dot optical exciter and a photodiode as a light-to-current converter integrated in the same instrument. Moreover, the overall analog conditioning is simply performed with one integrated solution, a field-programmable analog array (FPAA), which makes it possible to reconfigure the filter and gain stages in real time. This feature provides adaptability to use the platform as an analytical probe for carbon dots coming from different batches with some variations in luminescence characteristics. The calibration functions obtained that fit a modified Stern-Volmer equation were obtained using luminescence signals from Cdots quenching by Cu(II). The analytical applicability of the reconfigurable portable instrument for Cu(II) using Cdots has been successfully demonstrated in tap water analysis.

The use of surface-enhanced Raman scattering for detecting molecular evidence of life in rocks, sediments, and sedimentary deposits.

PubMed

Bowden, Stephen A; Wilson, Rab; Cooper, Jonathan M; Parnell, John

2010-01-01

Raman spectroscopy is a versatile analytical technique capable of characterizing the composition of both inorganic and organic materials. Consequently, it is frequently suggested as a payload on many planetary landers. Only approximately 1 in every 10(6) photons are Raman scattered; therefore, the detection of trace quantities of an analyte dispersed in a sample matrix can be much harder to achieve. To overcome this, surface-enhanced Raman scattering (SERS) and surface-enhanced resonance Raman scattering (SERRS) both provide greatly enhanced signals (enhancements between 10(5) and 10(9)) through the analyte's interaction with the locally generated surface plasmons, which occur at a "roughened" or nanostructured metallic surface (e.g., Cu, Au, and Ag). Both SERS and SERRS may therefore provide a viable technique for trace analysis of samples. In this paper, we describe the development of SERS assays for analyzing trace amounts of compounds present in the solvent extracts of sedimentary deposits. These assays were used to detect biological pigments present in an Arctic microoasis (a small locale of elevated biological productivity) and its detrital regolith, characterize the pigmentation of microbial mats around hydrothermal springs, and detect fossil organic matter in hydrothermal deposits. These field study examples demonstrate that SERS technology is sufficiently mature to be applied to many astrobiological analog studies on Earth. Many current and proposed imaging systems intended for remote deployment already posses the instrumental components needed for SERS. The addition of wet chemistry sample processing facilities to these instruments could yield field-deployable analytical instruments with a broadened analytical window for detecting organic compounds with a biological or geological origin.

Considerations in detecting CDC select agents under field conditions

NASA Astrophysics Data System (ADS)

Spinelli, Charles; Soelberg, Scott; Swanson, Nathaneal; Furlong, Clement; Baker, Paul

2008-04-01

Surface Plasmon Resonance (SPR) has become a widely accepted technique for real-time detection of interactions between receptor molecules and ligands. Antibody may serve as receptor and can be attached to the gold surface of the SPR device, while candidate analyte fluids contact the detecting antibody. Minute, but detectable, changes in refractive indices (RI) indicate that analyte has bound to the antibody. A decade ago, an inexpensive, robust, miniature and fully integrated SPR chip, called SPREETA, was developed. University of Washington (UW) researchers subsequently developed a portable, temperature-regulated instrument, called SPIRIT, to simultaneously use eight of these three-channel SPREETA chips. A SPIRIT prototype instrument was tested in the field, coupled to a remote reporting system on a surrogate unmanned aerial vehicle (UAV). Two target protein analytes were released sequentially as aerosols with low analyte concentration during each of three flights and were successfully detected and verified. Laboratory experimentation with a more advanced SPIRIT instrument demonstrated detection of very low levels of several select biological agents that might be employed by bioterrorists. Agent detection under field-like conditions is more challenging, especially as analyte concentrations are reduced and complex matricies are introduced. Two different sample preconditioning protocols have been developed for select agents in complex matrices. Use of these preconditioning techniques has allowed laboratory detection in spiked heavy mud of Francisella tularensis at 10 3 CFU/ml, Bacillus anthracis spores at 10 3 CFU/ml, Staphylococcal enterotoxin B (SEB) at 1 ng/ml, and Vaccinia virus (a smallpox simulant) at 10 5 PFU/ml. Ongoing experiments are aimed at simultaneous detection of multiple agents in spiked heavy mud, using a multiplex preconditioning protocol.

Trapped-mode-induced Fano resonance and acoustical transparency in a one-dimensional solid-fluid phononic crystal

NASA Astrophysics Data System (ADS)

Quotane, Ilyasse; El Boudouti, El Houssaine; Djafari-Rouhani, Bahram

2018-01-01

We investigate theoretically and numerically the possibility of existence of Fano and acoustic-induced transparency (AIT) resonances in a simple though realistic one-dimensional acoustic structure made of solid-fluid layers inserted between two fluids. These resonances are obtained by combining appropriately the zeros of transmission (antiresonance) induced by the solid layers and the local resonances induced by the solid or combined solid-fluid layers with surface free boundary conditions. In particular, we show the possibility of trapped modes, also called bound states in continuum, which have recently found a high renewal interest. These modes appear as resonances with zero width in the transmission spectra as well as in the density of states (DOS). We consider three different structures: (i) a single solid layer inserted between two fluids. This simple structure shows the possibility of existence of trapped modes, which are discrete modes of the solid layer that lie in the continuum modes of the surrounding fluids. We give explicit analytical expressions of the dispersion relation of these eigenmodes of the solid layer which are found independent of the nature of the surrounding fluids. By slightly detuning the angle of incidence from that associated to the trapped mode, we get a well-defined Fano resonance characterized by an asymmetric Fano profile in the transmission spectra. (ii) The second structure consists of a solid-fluid-solid triple layer embedded between two fluids. This structure is found more appropriate to show both Fano and acoustic-induced transparency resonances. We provide detailed analytical expressions for the transmission and reflection coefficients that enable us to deduce a closed-form expression of the dispersion relation giving the trapped modes. Two situations can be distinguished in the triple-layer system: in the case of a symmetric structure (i.e., the same solid layers) we show, by detuning the incidence angle θ , the possibility of existence of Fano resonances that can be fitted following a Fano-type expression. The variation of the Fano parameter that describes the asymmetry of such resonances as well as their width versus θ is studied in detail. In the case of an asymmetric structure (i.e., different solid layers), we show the existence of an incidence angle that enables to squeeze a resonance between two transmission zeros induced by the two solid layers. This resonance behaves like an AIT resonance, its position and width depend on the nature of the fluid and solid layers as well as on the difference between the thicknesses of the solid layers. (iii) In the case of a periodic structure (phononic crystal), we show that trapped modes and Fano resonances give rise, respectively, to dispersionless flat bands with zero group velocity and nearly flat bands with negative or positive group velocities. The analytical results presented here are obtained by means of the Green's function method which enables to deduce in closed form: dispersion curves, transmission and reflection coefficients, DOS, as well as the displacement fields. The proposed solid-fluid layered structures should have important applications for designing acoustic mirrors and acoustic filters as well as supersonic and subsonic materials.

Improving the efficiency of quantitative (1)H NMR: an innovative external standard-internal reference approach.

PubMed

Huang, Yande; Su, Bao-Ning; Ye, Qingmei; Palaniswamy, Venkatapuram A; Bolgar, Mark S; Raglione, Thomas V

2014-01-01

The classical internal standard quantitative NMR (qNMR) method determines the purity of an analyte by the determination of a solution containing the analyte and a standard. Therefore, the standard must meet the requirements of chemical compatibility and lack of resonance interference with the analyte as well as a known purity. The identification of such a standard can be time consuming and must be repeated for each analyte. In contrast, the external standard qNMR method utilizes a standard with a known purity to calibrate the NMR instrument. The external standard and the analyte are measured separately, thereby eliminating the matter of chemical compatibility and resonance interference between the standard and the analyte. However, the instrumental factors, including the quality of NMR tubes, must be kept the same. Any deviations will compromise the accuracy of the results. An innovative qNMR method reported herein utilizes an internal reference substance along with an external standard to assume the role of the standard used in the traditional internal standard qNMR method. In this new method, the internal reference substance must only be chemically compatible and be free of resonance-interference with the analyte or external standard whereas the external standard must only be of a known purity. The exact purity or concentration of the internal reference substance is not required as long as the same quantity is added to the external standard and the analyte. The new method reduces the burden of searching for an appropriate standard for each analyte significantly. Therefore the efficiency of the qNMR purity assay increases while the precision of the internal standard method is retained. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of Cinnamaldehyde in Cinnamon by SPME-GC-MS: An Instrumental Analysis Experiment

ERIC Educational Resources Information Center

Wang, Yimin; Ocariz, Jessica; Hammersand, Jennifer; MacDonald, Evan; Bartczak, Ashley; Kero, Frank; Young, Vaneica Y.; Williams, Kathryn R.

2008-01-01

Students analyze "trans"-cinnamaldehyde in commercial cinnamon using solid-phase microextraction and GC-MS with ethyl benzoate as the internal standard. Aside from the instrumentation, the experiment utilizes readily available low hazard materials and can be completed within one four-hour laboratory period. (Contains 2 figures.)

Report of the Attitude Control and Attitude Determination Panel. [spacecraft instrumentation technology

NASA Technical Reports Server (NTRS)

1979-01-01

Failures and deficiencies in flight programs are reviewed and suggestions are made for avoiding them. The technology development problem areas considered are control configured vehicle design, gyros, solid state star sensors, control instrumentation, tolerant/accomodating control systems, large momentum exchange devices, and autonomous rendezvous and docking.

40 CFR 261.151 - Wording of the instruments.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 27 2012-07-01 2012-07-01 false Wording of the instruments. 261.151 Section 261.151 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Financial Requirements for Management of Excluded Hazardous Secondary Materials § 261.151...

40 CFR 264.151 - Wording of the instruments.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 26 2011-07-01 2011-07-01 false Wording of the instruments. 264.151 Section 264.151 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) STANDARDS FOR OWNERS AND OPERATORS OF HAZARDOUS WASTE TREATMENT, STORAGE, AND DISPOSAL FACILITIES Financial Requirements § 264.151 Wording o...

40 CFR 261.151 - Wording of the instruments.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 26 2011-07-01 2011-07-01 false Wording of the instruments. 261.151 Section 261.151 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) IDENTIFICATION AND LISTING OF HAZARDOUS WASTE Financial Requirements for Management of Excluded Hazardous Secondary Materials § 261.151...

Apparatus for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, Gregory C.; Barinaga, Charles J.; Koppenaal, David W.

2001-01-01

An apparatus for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the apparatus has an ion trap or a collision cell containing a reagent gas wherein the reagent gas accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the collision cell as employed in various locations within analytical instruments including an inductively coupled plasma mass spectrometer.

MARA (Multimode Airborne Radar Altimeter) system documentation. Volume 1: MARA system requirements document

NASA Technical Reports Server (NTRS)

Parsons, C. L. (Editor)

1989-01-01

The Multimode Airborne Radar Altimeter (MARA), a flexible airborne radar remote sensing facility developed by NASA's Goddard Space Flight Center, is discussed. This volume describes the scientific justification for the development of the instrument and the translation of these scientific requirements into instrument design goals. Values for key instrument parameters are derived to accommodate these goals, and simulations and analytical models are used to estimate the developed system's performance.

Specifying and calibrating instrumentations for wideband electronic power measurements. [in switching circuits

NASA Technical Reports Server (NTRS)

Lesco, D. J.; Weikle, D. H.

1980-01-01

The wideband electric power measurement related topics of electronic wattmeter calibration and specification are discussed. Tested calibration techniques are described in detail. Analytical methods used to determine the bandwidth requirements of instrumentation for switching circuit waveforms are presented and illustrated with examples from electric vehicle type applications. Analog multiplier wattmeters, digital wattmeters and calculating digital oscilloscopes are compared. The instrumentation characteristics which are critical to accurate wideband power measurement are described.

Does size matter? Study of performance of pseudo-ELISAs based on molecularly imprinted polymer nanoparticles prepared for analytes of different sizes.

PubMed

Cáceres, C; Canfarotta, F; Chianella, I; Pereira, E; Moczko, E; Esen, C; Guerreiro, A; Piletska, E; Whitcombe, M J; Piletsky, S A

2016-02-21

The aim of this work is to evaluate whether the size of the analyte used as template for the synthesis of molecularly imprinted polymer nanoparticles (nanoMIPs) can affect their performance in pseudo-enzyme linked immunosorbent assays (pseudo-ELISAs). Successful demonstration of a nanoMIPs-based pseudo-ELISA for vancomycin (1449.3 g mol(-1)) was demonstrated earlier. In the present investigation, the following analytes were selected: horseradish peroxidase (HRP, 44 kDa), cytochrome C (Cyt C, 12 kDa) biotin (244.31 g mol(-1)) and melamine (126.12 g mol(-1)). NanoMIPs with a similar composition for all analytes were synthesised by persulfate-initiated polymerisation in water. In addition, core-shell nanoMIPs coated with polyethylene glycol (PEG) and imprinted for melamine were produced in organics and tested. The polymerisation of the nanoparticles was done using a solid-phase approach with the correspondent template immobilised on glass beads. The performance of the nanoMIPs used as replacement for antibodies in direct pseudo-ELISA (for the enzymes) and competitive pseudo-ELISA for the smaller analytes was investigated. For the competitive mode we rely on competition for the binding to the nanoparticles between free analyte and corresponding analyte-HRP conjugate. The results revealed that the best performances were obtained for nanoMIPs synthesised in aqueous media for the larger analytes. In addition, this approach was successful for biotin but completely failed for the smallest template melamine. This problem was solved using nanoMIP prepared by UV polymerisation in an organic media with a PEG shell. This study demonstrates that the preparation of nanoMIP by solid-phase approach can produce material with high affinity and potential to replace antibodies in ELISA tests for both large and small analytes. This makes this technology versatile and applicable to practically any target analyte and diagnostic field.

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

Not Available

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year (FY) 1993 (October 1992 through September 1993). This annual report is the tenth for the ACL and describes continuing effort on projects, work on new projects, and contributions of the ACL staff to various programs at ANL. The Analytical Chemistry Laboratory is a full-cost-recovery service center, with the primary mission of providing a broad range of analytical chemistry support services to the scientific and engineering programs at ANL. The ACL also has research programs in analyticalmore » chemistry, conducts instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems. Some routine or standard analyses are done, but it is common for the Argonne programs to generate unique problems that require development or modification of methods and adaption of techniques to obtain useful analytical data. The ACL is administratively within the Chemical Technology Division (CMT), its principal ANL client, but provides technical support for many of the technical divisions and programs at ANL. The ACL has four technical groups--Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis--which together include about 45 technical staff members. Talents and interests of staff members cross the group lines, as do many projects within the ACL.« less

Acoustic Measurements for Small Solid Rocket Motors

NASA Technical Reports Server (NTRS)

Vargas, Magda B.; Kenny, R. Jeremy

2010-01-01

Models have been developed to predict large solid rocket motor acoustic loads based on the scaling of small solid rocket motors. MSFC has measured several small solid rocket motors in horizontal and launch configurations to anchor these models. Solid Rocket Test Motor (SRTM) has ballistics similar to the Reusable Solid Rocket Motor (RSRM) therefore a good choice for acoustic scaling. Acoustic measurements were collected during the test firing of the Insulation Configuration Extended Length (ICXL) 7,6, and 8 (in firing order) in order to compare to RSRM horizontal firing data. The scope of this presentation includes: Acoustic test procedures and instrumentation implemented during the three SRTM firings and Data analysis method and general trends observed in the data.

On-line solid phase extraction using the Prospekt-2 coupled with a liquid chromatography/tandem mass spectrometer for the determination of dextromethorphan, dextrorphan and guaifenesin in human plasma.

PubMed

Kuhlenbeck, Debbie L; Eichold, Thomas H; Hoke, Steven H; Baker, Timothy R; Mensen, Robert; Wehmeyer, Kenneth R

2005-01-01

An on-line liquid chromatography/tandem mass spectrometry (LC-MS/MS) procedure, using the Prospekt- 2 system, was developed and used for the determination of the levels of the active ingredients of cough/cold medications in human plasma matrix. The experimental configuration allows direct plasma injection by performing on- line solid phase extraction (SPE) on small cartridge columns prior to elution of the analyte(s) onto the analytical column and subsequent MS/MS detection. The quantitative analysis of three analytes with differing polarities, dextromethorphan (DEX), dextrorphan (DET) and guaifenesin (GG) in human plasma presented a significant challenge. Using stable-isotope-labeled internal standards for each analyte, the Prospekt-2 on-line methodology was evaluated for sensitivity, suppression, accuracy, precision, linearity, analyst time, analysis time, cost, carryover and ease of use. The lower limit of quantitation for the on-line SPE procedure for DEX, DET and GG was 0.05, 0.05 and 5.0 ng mL(-1), respectively, using a 0.1 mL sample volume. The linear range for DEX and DET was 0.05-50 ng mL(-1) and was 5-5,000 ng mL(-1) for GG. Accuracy and precision data for five different levels of QC samples were collected over three separate days. Accuracy ranged from 90% to 112% for all three analytes, while the precision, as measured by the %RSD, ranged from 1.5% to 16.0%

Using multiple isotopes to understand the source of ingredients used in golden beverages

NASA Astrophysics Data System (ADS)

Wynn, J. G.

2011-12-01

Traditionally, beer contains 4 simple ingredients: water, barley, hops and yeast. Each of these ingredients used in the brewing process contributes some combination of a number of "traditional" stable isotopes (i.e., isotopes of H, C, O, N and S) to the final product. As an educational exercise in an "Analytical Techniques in Geology" course, a group of students analyzed the isotopic composition of the gas, liquid and solid phases of a variety of beer samples collected from throughout the world (including other beverages). The hydrogen and oxygen isotopic composition of the water followed closely the isotopic composition of local meteoric water at the source of the brewery, although there is a systematic offset from the global meteoric water line that may be due to the effects of CO2-H2O equilibration. The carbon isotopic composition of the CO2 reflected that of the solid residue (the source of carbon used as a fermentation substrate), but may potentially be modified by addition of gas-phase CO2 from an inorganic source. The carbon isotopic composition of the solid residue similarly tracks that of the fermentation substrate, and may indicate some alcohol fermented from added sugars in some cases. The nitrogen isotopic composition of the solid residue was relatively constant, and may track the source of nitrogen in the barley, hops and yeast. Each of the analytical methods used is a relatively standard technique used in geological applications, making this a "fun" exercise for those involved, and gives the students hands-on experience with a variety of analytes from a non-traditional sample material.

Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry.

PubMed

Ponce-Robles, Laura; Rivas, Gracia; Esteban, Belen; Oller, Isabel; Malato, Sixto; Agüera, Ana

2017-10-01

An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l -1 in the aqueous phase and below 40 ng g -1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge.

High-throughput multipesticides residue analysis in earthworms by the improvement of purification method: Development and application of magnetic Fe3 O4 -SiO2 nanoparticles based dispersive solid-phase extraction.

PubMed

Sun, Yuhan; Qi, Peipei; Cang, Tao; Wang, Zhiwei; Wang, Xiangyun; Yang, Xuewei; Wang, Lidong; Xu, Xiahong; Wang, Qiang; Wang, Xinquan; Zhao, Changshan

2018-06-01

As a key representative organism, earthworms can directly illustrate the influence of pesticides on environmental organisms in soil ecosystems. The present work aimed to develop a high-throughput multipesticides residue analytical method for earthworms using solid-liquid extraction with acetonitrile as the solvent and magnetic material-based dispersive solid-phase extraction for purification. Magnetic Fe 3 O 4 nanoparticles were modified with a thin silica layer to form Fe 3 O 4 -SiO 2 nanoparticles, which were fully characterized by field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, X-ray diffractometry, and vibrating sample magnetometry. The Fe 3 O 4 -SiO 2 nanoparticles were used as the separation media in dispersive solid-phase extraction with primary secondary amine and ZrO 2 as the cleanup adsorbents to eliminate matrix interferences. The amounts of nanoparticles and adsorbents were optimized for the simultaneous determination of 44 pesticides and six metabolites in earthworms by liquid chromatography with tandem mass spectrometry. The method performance was systematically validated with satisfactory results. The limits of quantification were 20 μg/kg for all analytes studied, while the recoveries of the target analytes ranged from 65.1 to 127% with relative standard deviation values lower than 15.0%. The developed method was subsequently utilized to explore the bioaccumulation of bitertanol in earthworms exposed to contaminated soil, verifying its feasibility for real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Instrument Attitude Precision Control

NASA Technical Reports Server (NTRS)

Juang, Jer-Nan

2004-01-01

A novel approach is presented in this paper to analyze attitude precision and control for an instrument gimbaled to a spacecraft subject to an internal disturbance caused by a moving component inside the instrument. Nonlinear differential equations of motion for some sample cases are derived and solved analytically to gain insight into the influence of the disturbance on the attitude pointing error. A simple control law is developed to eliminate the instrument pointing error caused by the internal disturbance. Several cases are presented to demonstrate and verify the concept presented in this paper.

The Mars Organic Molecule Analyzer (MOMA) Instrument: Characterization of Organic Material in Martian Sediments

PubMed Central

Goesmann, Fred; Brinckerhoff, William B.; Raulin, François; Danell, Ryan M.; Getty, Stephanie A.; Siljeström, Sandra; Mißbach, Helge; Steininger, Harald; Arevalo, Ricardo D.; Buch, Arnaud; Freissinet, Caroline; Grubisic, Andrej; Meierhenrich, Uwe J.; Pinnick, Veronica T.; Stalport, Fabien; Szopa, Cyril; Vago, Jorge L.; Lindner, Robert; Schulte, Mitchell D.; Brucato, John Robert; Glavin, Daniel P.; Grand, Noel; Li, Xiang; van Amerom, Friso H. W.

2017-01-01

Abstract The Mars Organic Molecule Analyzer (MOMA) instrument onboard the ESA/Roscosmos ExoMars rover (to launch in July, 2020) will analyze volatile and refractory organic compounds in martian surface and subsurface sediments. In this study, we describe the design, current status of development, and analytical capabilities of the instrument. Data acquired on preliminary MOMA flight-like hardware and experimental setups are also presented, illustrating their contribution to the overall science return of the mission. Key Words: Mars—Mass spectrometry—Life detection—Planetary instrumentation. Astrobiology 17, 655–685.

Three modified activated carbons by different ligands for the solid phase extraction of copper and lead.

PubMed

Ghaedi, M; Ahmadi, F; Tavakoli, Z; Montazerozohori, M; Khanmohammadi, A; Soylak, M

2008-04-15

In the presented work, 5,5-diphenylimidazolidine-2,4-dione (phenytoin) (DFTD), 5,5-diphenylimidazolidine-2-thione-,4-one (thiophenytoin) (DFID) and 2-(4'-methoxy-benzylidenimine) thiophenole (MBIP) modified activated carbons have been used for the solid phase extraction of copper and lead ions prior to their flame atomic absorption spectrometric determinations. The influences of the various analytical parameters including pH, amounts of reagent, sample volume and eluent type, etc. on the recovery efficiencies of copper and lead ions were investigated. The influences of alkaline, earth alkaline and some transition metals on the adsorption of the analytes were also examined. The detection limits by three sigma for analyte ions were 0.65 and 0.42 microg L(-1) using activated carbon modified with DFID; 0.52 and 0.37 microg L(-1) using activated carbon modified with DFTD and 0.46 and 0.31 microg L(-1) using activated carbon modified with MBIP for Pb(II) and Cu(II), respectively. The procedure was applied to the determination of analytes in natural waters, soil, and blood samples with satisfactory results (recoveries greater than 95%, R.S.D.'s lower than 4%).

Determination of iodinated X-ray contrast media in sewage by solid-phase extraction and liquid chromatography tandem mass spectrometry.

PubMed

Echeverría, S; Borrull, F; Fontanals, N; Pocurull, E

2013-11-15

A method for the quantitative determination of five iodinated X-ray contrast media (ICMs) in sewage was developed by solid-phase extraction and high-performance liquid chromatography-tandem mass spectrometry. A fused-core analytical column was successfully applied for the first time for the separation of ICMs. Oasis HLB was selected from the sorbents tested because of its higher recoveries. The optimized method allowed the determination of the ICMs at low ng/L levels in both influent and effluent sewage, with detection limits of 40 ng/L and 10 ng/L for most compounds in influent and effluent sewage, respectively. The five ICMs studied were determined in all samples analysed, with iopromide being the analyte found at the highest concentration (8.9 µg/L), while iopamidol was the analyte found at lowest concentration (1.3 µg/L) in influent sewage. Effluent sewage did not show a significant decrease in ICM concentrations. © 2013 Elsevier B.V. All rights reserved.

Extraction of fullerenes from environmental matrices as affected by solvent characteristics and analyte concentration.

PubMed

Place, Benjamin J; Kleber, Markus; Field, Jennifer A

2013-03-01

Fullerenes possess unique chemical properties that make the isolation of these compounds from heterogeneous environmental matrices difficult. For example, previous reports indicate that toluene-based extraction techniques vary in their ability to extract C60, especially from highly carbonaceous solid matrices. Here, we examined the effects of (i) solvent type (toluene alone versus an 80:20 v/v mixture of toluene and 1-methylnaphthalene) and (ii) analyte concentration on the extraction efficiency of an isotopically labeled surrogate compound, (13)C60. The toluene/1-methylnaphthalene mixture increased fullerene extraction efficiency from carbon lampblack by a factor of five, but was not significantly different from 100% toluene when applied to wood stove soot or montmorillonite. Recovery of the (13)C60 surrogate declined with decreasing analyte concentration. The usefulness of isotopically labeled surrogate is demonstrated and the study provides a quantitative assessment regarding the dependence of fullerene extraction efficiencies on the geochemical characteristics of solid matrices. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Characterizing nonconstant instrumental variance in emerging miniaturized analytical techniques.

PubMed

Noblitt, Scott D; Berg, Kathleen E; Cate, David M; Henry, Charles S

2016-04-07

Measurement variance is a crucial aspect of quantitative chemical analysis. Variance directly affects important analytical figures of merit, including detection limit, quantitation limit, and confidence intervals. Most reported analyses for emerging analytical techniques implicitly assume constant variance (homoskedasticity) by using unweighted regression calibrations. Despite the assumption of constant variance, it is known that most instruments exhibit heteroskedasticity, where variance changes with signal intensity. Ignoring nonconstant variance results in suboptimal calibrations, invalid uncertainty estimates, and incorrect detection limits. Three techniques where homoskedasticity is often assumed were covered in this work to evaluate if heteroskedasticity had a significant quantitative impact-naked-eye, distance-based detection using paper-based analytical devices (PADs), cathodic stripping voltammetry (CSV) with disposable carbon-ink electrode devices, and microchip electrophoresis (MCE) with conductivity detection. Despite these techniques representing a wide range of chemistries and precision, heteroskedastic behavior was confirmed for each. The general variance forms were analyzed, and recommendations for accounting for nonconstant variance discussed. Monte Carlo simulations of instrument responses were performed to quantify the benefits of weighted regression, and the sensitivity to uncertainty in the variance function was tested. Results show that heteroskedasticity should be considered during development of new techniques; even moderate uncertainty (30%) in the variance function still results in weighted regression outperforming unweighted regressions. We recommend utilizing the power model of variance because it is easy to apply, requires little additional experimentation, and produces higher-precision results and more reliable uncertainty estimates than assuming homoskedasticity. Copyright © 2016 Elsevier B.V. All rights reserved.

Design, Implementation, and Operational Methodologies for Sub-arcsecond Attitude Determination, Control, and Stabilization of the Super-pressure Balloon-Borne Imaging Telescope (SuperBIT)

NASA Astrophysics Data System (ADS)

Javier Romualdez, Luis

Scientific balloon-borne instrumentation offers an attractive, competitive, and effective alternative to space-borne missions when considering the overall scope, cost, and development timescale required to design and launch scientific instruments. In particular, the balloon-borne environment provides a near-space regime that is suitable for a number of modern astronomical and cosmological experiments, where the atmospheric interference suffered by ground-based instrumentation is negligible at stratospheric altitudes. This work is centered around the analytical strategies and implementation considerations for the attitude determination and control of SuperBIT, a scientific balloon-borne payload capable of meeting the strict sub-arcsecond pointing and image stability requirements demanded by modern cosmological experiments. Broadly speaking, the designed stability specifications of SuperBIT coupled with its observational efficiency, image quality, and accessibility rivals state-of-the-art astronomical observatories such as the Hubble Space Telescope. To this end, this work presents an end-to-end design methodology for precision pointing balloon-borne payloads such as SuperBIT within an analytical yet implementationally grounded context. Simulation models of SuperBIT are analytically derived to aid in pre-assembly trade-off and case studies that are pertinent to the dynamic balloon-borne environment. From these results, state estimation techniques and control methodologies are extensively developed, leveraging the analytical framework of simulation models and design studies. This pre-assembly design phase is physically validated during assembly, integration, and testing through implementation in real-time hardware and software, which bridges the gap between analytical results and practical application. SuperBIT attitude determination and control is demonstrated throughout two engineering test flights that verify pointing and image stability requirements in flight, where the post-flight results close the overall design loop by suggesting practical improvements to pre-design methodologies. Overall, the analytical and practical results presented in this work, though centered around the SuperBIT project, provide generically useful and implementationally viable methodologies for high precision balloon-borne instrumentation, all of which are validated, justified, and improved both theoretically and practically. As such, the continuing development of SuperBIT, built from the work presented in this thesis, strives to further the potential for scientific balloon-borne astronomy in the near future.