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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS1976

Electrophoresis technology experiment MA-011

Experiment MA-011, electrophoresis technology, was designed to test electrophoresis hardware that would continue the development of technology for electrophoretic separation of materials in the near zero g environment of space. The experimental hardware generally functioned as planned. Frozen live cells were successfully transported into space, electrophoretic processing was performed, and viable cells were returned to earth. A separation of the three types of fixed red blood cells (rabbit, human, and horse) was demonstrated. The human lymphocytes, however, showed no apparent migration. The separation of human kidney cells produced the most exciting data. Analysis shows electrophoretic separation throughout the entire column with at least four bands of viable cells. The isotachophoresis experiment definitely demonstrated the isotachophoretic separation of biological cells in a near zero g environment.

Allen, R. E.↗
NASA NTRS1968

Nitric acid-organic mixtures surveyed for use in separation by anion exchange methods

Column elution-spectrographic analysis technique compares certain solvents directly to the methanol system, using inert rare earths instead of actinides. Distribution ratios for americium between 90 percent solvent, 10 percent 5 M nitric acid and Dowex 1 nitrate form resin for a large group of organics miscible in water was determined.

Bloomquist, C. A. A.↗
NASA NTRS2006

Ion-Exclusion Chromatography for Analyzing Organics in Water

A liquid-chromatography technique has been developed for use in the quantitative analysis of urea (and of other nonvolatile organic compounds typically found with urea) dissolved in water. The technique involves the use of a column that contains an ion-exclusion resin; heretofore, this column has been sold for use in analyzing monosaccharides and food softeners, but not for analyzing water supplies. The prior technique commonly used to analyze water for urea content has been one of high-performance liquid chromatography (HPLC), with reliance on hydrophobic interactions between analytes in a water sample and long-chain alkyl groups bonded to an HPLC column. The prior technique has proven inadequate because of a strong tendency toward co-elution of urea with other compounds. Co-elution often causes the urea and other compounds to be crowded into a narrow region of the chromatogram (see left part of figure), thereby giving rise to low chromatographic resolution and misidentification of compounds. It is possible to quantitate urea or another analyte via ultraviolet- and visible-light absorbance measurements, but in order to perform such measurements, it is necessary to dilute the sample, causing a significant loss of sensitivity. The ion-exclusion resin used in the improved technique is sulfonated polystyrene in the calcium form. Whereas the alkyl-chain column used in the prior technique separates compounds on the basis of polarity only, the ion-exclusion-resin column used in the improved technique separates compounds on the basis of both molecular size and electric charge. As a result, the degree of separation is increased: instead of being crowded together into a single chromatographic peak only about 1 to 2 minutes wide as in the prior technique, the chromatographic peaks of different compounds are now separated from each other and spread out over a range about 33 minutes wide (see right part of figure), and the urea peak can readily be distinguished from the other peaks. Although the analysis takes more time in the improved technique, this disadvantage is offset by two important advantages: Sensitivity is increased. The minimum concentration of urea that can be measured is reduced (to between 1/5 and 1/3 of that of the prior technique) because it is not necessary to dilute the sample. The separation of peaks facilitates the identification and quantitation of the various compounds. The resolution of the compounds other than urea makes it possible to identify those compounds by use of mass spectrometry.

Sauer, Richard↗
NASA NTRS1986

Organics in water contamination analyzer, phase 1

The requirements which would result in identifying the components of an automatic analytical system for the analysis of specific organic compounds in the space station potable water supply are defined. The gas chromatographic system for such an analysis is limited to commercially available off-the-shelf hardware and includes the sample inlet, an ionization detector, capillary columns as well as computerized compound identification. The sampling system will be a special variation of the purge and trap Tenax mode using six-port valves and a 500 microliter water sample. Capillary columns used for the separating of contaminants will be bonded phase fused silica with a silicone stationary phase. Two detectors can be used: photoionization and far ultraviolet, since they are sensitive and compatible with capillary columns. A computer system evaluation and program with the principle of compound identification based on the retention index is presented.

Source record↗
NASA NTRS1987

High-resolution ultraviolet observations of interstellar lines toward Zeta Persei observed with the balloon-borne ultraviolet stellar spectrometer

The balloon-borne ultraviolet stellar spectrometer payload has been used to obtain high-resolution data on interstellar absorption lines toward Zeta Per. The only lines clearly present in the 2150-2450 region were several Fe II features, which show double structure. The two velocity components were sufficiently well separated that it was possible to construct separate curves of growth to derive the Fe II column densities for the individual components. These column densities and the component velocity separation were then used to compute a realistic two-component curve of growth for the line of sight to Zeta Per, which was then used to reanalyze existing ultraviolet data from Copernicus. The results were generally similar to an earlier two-component analysis of the Copernicus data, with the important exception that the silicon depletion increased from near zero to about 1 dex. This makes the Zeta Per depletion pattern quite similar to those derived for other reddened lines of sight, supporting the viewpoint that the general diffuse interstellar medium has a nearly constant pattern of depletions.

Snow, Theodore P.↗
NASA NTRS1984

Gas chromatographic separation of nitrogen, oxygen, argon, and carbon monoxide using custom-made porous polymers from high purity divinylbenzene

Existing porous polymers were surveyed for their ability to separate the subject gases. Certain products that showed more promise than others were synthesized and the existing synthetic procedures studied and modified to produce new polymers with enhanced ability to separate the subject gases. Evaluation of the porous polymers was carried out practically by gas chromatography at ambient temperature. The modified synthetic procedures were somewhat simpler than the originals. The new porous polymers made with high purity divinylbenzene enabled use of shorter columns to obtain the separations desired.

Pollock, G. E.↗
NASA NTRS1991

A silicone column for GC analysis of polar and nonpolar chemicals

The investigation of the Saturnian System is being proposed jointly by NASA and the European Space Agency (ESA). The mission is scheduled for a launch in 1996. The mission provides an opportunity for close observation and exploration of Saturn's atmosphere, the complex Saturnian System of satellites and rings, Titan (Saturn's planet-sized moon), and Saturn's magnetosphere. The mission gives special attention to Titan which is blanketed by a thick, opaque atmosphere. An atmospheric probe will be deposited into the Titan Atmosphere for in situ measurement during a slow, three hour descent to the surface. The results from this analysis may provide the information which is important to the research of chemical evolution, and the origin of life. An analytical system was developed as a part of the Titan Aerosol Gas Experiment (TAGEX), a proposed experiment for the Cassini Mission. This system will use two highly sensitive detectors, the Metastable Ionization Detector (MID) and the Ion Mobility Spectrometer (IMS). Unfortunately, when commercial columns are utilized with these highly sensitive detectors, volatile components continuously bleed from the column and interfere with the detector. In addition, light columns must be able to separate polar and nonpolar organic chemicals within 10-15 minutes under isothermal conditions for the Titan Mission. Therefore, a highly crosslinked silicone polymeric packed column was developed which is able to efficiently separate amines, alcohols, and hydrocarbons with retention times less that 15 minutes at 100 C isothermal condition.

Shen, T. C.↗
NASA NTRS2001

Sources of Variability in the Stratospheric Column of Nitrogen Dioxide

Instruments such as the Global Ozone Monitoring Experiment (GOME, on the European Remote Sensing Satellite (ERS-2), launched 1995), the Scanning Imaging Absorption Spectrometer for Atmospheric Chartography (SCIAMACHY, on ENVISAT, to be launched July 2001) and the Ozone Monitoring Instrument (OMI on EOS Aura, to be launched 2003) make measurements of the total column of NO2. There is interest in separating the stratospheric and tropospheric contributions to the column, as the tropospheric column provides a measure of pollution. We are using a 3D chemistry and transport model driven by winds from the Goddard Space Flight Center Data Assimilation System to examine variability in the stratospheric NO2 column. Model results for NOx = NO + NO2 + 2N2O5 will be shown to compare well with sunset observations from the Halogen Occultation Experiment on the Upper Atmosphere Research Satellite, and to exhibit similar temporal and spatial dependence. Partitioning between NO, NO2, and N2O5 is also shown to compare well with observations. This good agreement supports the use of simulated fields in the stratosphere to derive the tropospheric column from the total column. Preliminary comparisons of the tropospheric column with model simulations for the troposphere will also be shown.

Douglass, Anne↗
NASA NTRS1996

Separation of 'Uncharged' Oligodeoxynucleotide Analogs by Anion-Exchange Chromatography at High pH

Ion-exchange chromatography is a well-established method for the analysis and purification of phosphodiester-linked oligonucleotides. If elution is carried out under alkaline conditions, the secondary structure of G- and C-rich oligomers is disrupted. Furthermore, elution times become more sensitive to the G and T content of the oligomer, because G and T are deprotonated at pH 10. In recent work on peptide-nucleic acids (PNAs) we noted that mixtures of PNA oligomers G(sub 4), G(sub 6), G(sub 8), and G9(sub 10) are readily separated by elution at pH 12 on an RPC-5 column. Here we show that this separation method is more generally applicable.

Schmidt, Jurgen G.↗
NASA NTRS1996

Separation of Uncharged Oligodeoxynucleotide Analogs by Anion-Exchange Chromatography at High pH

Ion-exchange chromatography is a well-established method for the analysis and purification of phosphodiester-linked oligonucleotides. If elution is carried out under alkaline conditions, the secondary structure of G- and C-rich oligomers is disrupted. Furthermore, elution times become more sensitive to the G and T content of the oligomer, because G and T are deprotonated at pH 10. In recent work on peptide-nucleic acids (PNAs) we noted that mixtures of PNA oligomers G(sub 4), G(Sub 6), G(sub 8), and G(sub 10) are readily separated by elution at pH 12 on an RPC-5 column. Here we show that this separation method is more generally applicable.

Schmidt, Jurgen G.↗
NASA NTRS1976

Nonlinear effects for the Taylor column for a hemisphere

When a flow is forced past an obstacle in a rapidly rotating fluid, a Taylor column forms. This is defined by a set of vertical detached shear layers circumscribing the obstacle which provide the smooth transition from an external inviscid potential flow to a stagnant core above the obstacle. For a hemispherical object, the main adjustment takes place in an external E to the 1/4 power layer and an internal E to the 2/7 power layer; here, the nonlinear flow in these layers is investigated. The problem in the E to the 1/4 power layer is identical to a problem occurring in magnetohydrodynamic flow; in addition, some features of the magnetohydrodynamic problem have been resolved. Numerical solutions are obtained for the steady nonlinear external E to the 1/4 power layer flow up to the point where unsteady flow separation from the Taylor column is imminent. The response of the internal E to the 2/7 power layer to the flow in the E to the 1/4 power layer is calculated, and the results suggest that the internal shear layer is unlikely to play any significant role in the separation process

Crisalli, A. J.↗
NASA NTRS1980

Deconvolution of gas chromatographic data

The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

Howard, S.↗
NASA NTRS2013

Atomic Force Microscope Mediated Chromatography

The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a sliding plate system, consisting of two flat surfaces, one of which has a recessed channel. A fluid flow is produced by axially sliding one plate past another, where the fluid has mechanical shear forces imposed at each point along the channel length. The shear-induced flow rates are very reproducible, and do not have pressure or voltage gradient limitations. SDC opens up a new range of enhanced separation kinetics by permitting the sample confinement with submicron dimensions. Small, highly confined liquid is advantageous for chromatographic separation because the separation rate is known to scale according to the square of the confined sample diameter. In addition, because shear-driven flows are not limited by fluid velocity, shear-driven liquid chromatography may provide up to 100,000 plate efficiency.

Anderson, Mark S.↗
NASA NTRS2017

Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

Franco, Carolina↗
NASA NTRS2004

Detecting Organic Compounds in Martian Soil Analogues Using Gas Chromatography Mass Spectrometry

One of the primary objectives of the 1976 Viking missions was to determine whether organic compounds, possibly of biological origin, were present in the Martian surface soils. The Viking gas chromatography mass spectrometry (GCMS) instruments found no evidence for any organic compounds of Martian origin above a few parts per billion in the upper 10 cm of surface soil [l], suggesting the absence of a widely distributed Martian biota. However, Benner et d. have suggested that significant amounts of non-volatile organic compounds, possibly including oxidation products of bioorganic molecules (e.g. carboxylic acids) would not have been detected by the Viking GCMS [2]. Moreover, other key organic compounds important to biology, such as amino acids and nucleobases, would also likely have been missed by the Viking GCMS as these compounds require chemical derivatization to be stable in a GC column [3]. Recent pyrolysis experiments with a Mars soil analogue that had been innoculated with Escherichia coli bacteria have shown that amino acid decomposition products (amines) and nucleobases are among the most abundant products generated after pyrolysis of the bacterial cells [4,5]. At the part per billion level (Viking GCMS detection limit), these pyrolysis products generated from several million bacterial cells per gram of Martian soil would not have been detected by the Viking GCMS instruments [4]. Analytical protocols are under development for upcoming in situ lander opportunities to target several important biological compounds including amino acids and nucleobases. For example, extraction and chemical derivatization techniques [3] are being adapted for space flight use to transform reactive or fragile molecules that would not have been detected by the Viking GCMS instruments, into species that are sufficiently volatile to be detected by GCMS. Recent experiments carried out at NASA Goddard have shown that using this derivatization technique all of the targeted compounds mentioned above can be separated on a GC column and detected by MS at sub-picomole (< 10(exp -l2 mole) levels. With these methods, the detection limit for amino acids, carboxylic acids and nucleobases is several orders of magnitude more sensitive than the Viking GCMS instruments for these compounds. Preliminary results using this analytical technique on a variety of Martian soil analogues will be presented.

Glavin, D. P.↗
NASA NTRS1994

Gas chromatographic column for the storage of sample profiles

The concept of a sample retention column that preserves the true time profile of an analyte of interest is studied. This storage system allows for the detection to be done at convenient times, as opposed to the nearly continuous monitoring that is required by other systems to preserve a sample time profile. The sample storage column is essentially a gas chromatography column, although its use is not the separation of sample components. The functions of the storage column are the selective isolation of the component of interest from the rest of the components present in the sample and the storage of this component as a function of time. Using octane as a test substance, the sample storage system was optimized with respect to such parameters as storage and readout temperature, flow rate through the storage column, column efficiency and storage time. A 3-h sample profile was collected and stored at 30 degrees C for 20 h. The profile was then retrieved, essentially intact, in 5 min at 130 degrees C.

NASA Program Exobiology↗
NASA NTRS1980

Isoelectric focusing of red blood cells in a density gradient stabilized column

The effects of Ficoll and cell application pH on red blood cell electrophoretic mobility and focusing pH were investigated by focusing cells in a density gradient stabilized column. Sample loading, cell dispersion, column conductivity, resolution of separation, and the effect of Ampholines were examined.

Smolka, A. J. K.↗