The carbon chemistry of the moon.

NASA Technical Reports Server (NTRS)

Eglinton, G.; Maxwell, J. R.; Pillinger, C. T.

1972-01-01

The analysis of lunar samples has shown that the carbon chemistry of the moon is entirely different from the carbon chemistry of the earth. Lunar carbon chemistry is more closely related to cosmic physics than to conventional organic chemistry. Sources of carbon on the moon are considered, giving attention to meteorites and the solar wind. The approaches used in the analysis of the samples are discussed, taking into account the method of gas chromatography employed and procedures used by bioscience investigators in the study of the lunar fines. The presence of indigenous methane and carbide in the lunar fines was established. Reactions and processes taking place on the lunar surface are discussed.

Micropowder collecting technique for stable isotope analysis of carbonates.

PubMed

Sakai, Saburo; Kodan, Tsuyoshi

2011-05-15

Micromilling is a conventional technique used in the analysis of the isotopic composition of geological materials, which improves the spatial resolution of sample collection for analysis. However, a problem still remains concerning the recovery ratio of the milled sample. We constructed a simple apparatus consisting of a vacuum pump, a sintered metal filter, electrically conductive rubber stopper and a stainless steel tube for transferring the milled powder into a reaction vial. In our preliminary experiments on carbonate powder, we achieved a rapid recovery of 5 to 100 µg of carbonate with a high recovery ratio (>90%). This technique shortens the sample preparation time, improves the recovery ratio, and homogenizes the sample quantity, which, in turn, improves the analytical reproducibility. Copyright © 2011 John Wiley & Sons, Ltd.

In-situ soil carbon analysis using inelastic neutron scattering

USDA-ARS?s Scientific Manuscript database

In situ soil carbon analysis using inelastic neutron scattering (INS) is based on the emission of 4.43 MeV gamma rays from carbon nuclei excited by fast neutrons. This in-situ method has excellent potential for easily measuring soil carbon since it does not require soil core sampling and processing ...

Assessing NIR & MIR Spectral Analysis as a Method for Soil C Estimation Across a Network of Sampling Sites

NASA Astrophysics Data System (ADS)

Spencer, S.; Ogle, S.; Borch, T.; Rock, B.

2008-12-01

Monitoring soil C stocks is critical to assess the impact of future climate and land use change on carbon sinks and sources in agricultural lands. A benchmark network for soil carbon monitoring of stock changes is being designed for US agricultural lands with 3000-5000 sites anticipated and re-sampling on a 5- to10-year basis. Approximately 1000 sites would be sampled per year producing around 15,000 soil samples to be processed for total, organic, and inorganic carbon, as well as bulk density and nitrogen. Laboratory processing of soil samples is cost and time intensive, therefore we are testing the efficacy of using near-infrared (NIR) and mid-infrared (MIR) spectral methods for estimating soil carbon. As part of an initial implementation of national soil carbon monitoring, we collected over 1800 soil samples from 45 cropland sites in the mid-continental region of the U.S. Samples were processed using standard laboratory methods to determine the variables above. Carbon and nitrogen were determined by dry combustion and inorganic carbon was estimated with an acid-pressure test. 600 samples are being scanned using a bench- top NIR reflectance spectrometer (30 g of 2 mm oven-dried soil and 30 g of 8 mm air-dried soil) and 500 samples using a MIR Fourier-Transform Infrared Spectrometer (FTIR) with a DRIFT reflectance accessory (0.2 g oven-dried ground soil). Lab-measured carbon will be compared to spectrally-estimated carbon contents using Partial Least Squares (PLS) multivariate statistical approach. PLS attempts to develop a soil C predictive model that can then be used to estimate C in soil samples not lab-processed. The spectral analysis of soil samples either whole or partially processed can potentially save both funding resources and time to process samples. This is particularly relevant for the implementation of a national monitoring network for soil carbon. This poster will discuss our methods, initial results and potential for using NIR and MIR spectral approaches to either replace or augment traditional lab-based carbon analyses of soils.

Fire debris analysis for forensic fire investigation using laser induced breakdown spectroscopy (LIBS)

NASA Astrophysics Data System (ADS)

Choi, Soojin; Yoh, Jack J.

2017-08-01

The possibility verification of the first attempt to apply LIBS to arson investigation was performed. LIBS has capabilities for real time in-situ analysis and depth profiling. It can provide valuable information about the fire debris that are complementary to the classification of original sample components and combustion residues. In this study, fire debris was analyzed to determine the ignition source and existence of a fire accelerant using LIBS spectra and depth profiling analysis. Fire debris chemical composition and carbon layer thickness determines the possible ignition source while the carbon layer thickness of combusted samples represents the degree of sample carbonization. When a sample is combusted with fire accelerants, a thicker carbon layer is formed because the burning rate is increased. Therefore, depth profiling can confirm the existence of combustion accelerants, which is evidence of arson. Also investigation of fire debris by depth profiling is still possible when a fire is extinguished with water from fire hose. Such data analysis and in-situ detection of forensic signals via the LIBS may assist fire investigation at crime scenes.

Sampling in freshwater environments: suspended particle traps and variability in the final data.

PubMed

Barbizzi, Sabrina; Pati, Alessandra

2008-11-01

This paper reports one practical method to estimate the measurement uncertainty including sampling, derived by the approach implemented by Ramsey for soil investigations. The methodology has been applied to estimate the measurements uncertainty (sampling and analyses) of (137)Cs activity concentration (Bq kg(-1)) and total carbon content (%) in suspended particle sampling in a freshwater ecosystem. Uncertainty estimates for between locations, sampling and analysis components have been evaluated. For the considered measurands, the relative expanded measurement uncertainties are 12.3% for (137)Cs and 4.5% for total carbon. For (137)Cs, the measurement (sampling+analysis) variance gives the major contribution to the total variance, while for total carbon the spatial variance is the dominant contributor to the total variance. The limitations and advantages of this basic method are discussed.

Titrimetric Determination of Carbon Dioxide in a Heterogeneous Sample ("Pop Rocks")

NASA Astrophysics Data System (ADS)

Davis, Craig M.; Mauck, Matthew C.

2003-05-01

A traditional exercise in quantitative analysis is the titration of mixtures of sodium hydroxide, sodium carbonate, and sodium bicarbonate. Often, consumer products are studied. A procedure to analyze the total volume of carbon dioxide bubbles in the candy "Pop Rocks" is presented. The popularity of the sample and the simplicity of the procedure make this exercise suitable for a wide variety of students: from non-science majors to chemistry majors in a quantitative analysis course.

[Proximate analysis of straw by near infrared spectroscopy (NIRS)].

PubMed

Huang, Cai-jin; Han, Lu-jia; Liu, Xian; Yang, Zeng-ling

2009-04-01

Proximate analysis is one of the routine analysis procedures in utilization of straw for biomass energy use. The present paper studied the applicability of rapid proximate analysis of straw by near infrared spectroscopy (NIRS) technology, in which the authors constructed the first NIRS models to predict volatile matter and fixed carbon contents of straw. NIRS models were developed using Foss 6500 spectrometer with spectra in the range of 1,108-2,492 nm to predict the contents of moisture, ash, volatile matter and fixed carbon in the directly cut straw samples; to predict ash, volatile matter and fixed carbon in the dried milled straw samples. For the models based on directly cut straw samples, the determination coefficient of independent validation (R2v) and standard error of prediction (SEP) were 0.92% and 0.76% for moisture, 0.94% and 0.84% for ash, 0.88% and 0.82% for volatile matter, and 0.75% and 0.65% for fixed carbon, respectively. For the models based on dried milled straw samples, the determination coefficient of independent validation (R2v) and standard error of prediction (SEP) were 0.98% and 0.54% for ash, 0.95% and 0.57% for volatile matter, and 0.78% and 0.61% for fixed carbon, respectively. It was concluded that NIRS models can predict accurately as an alternative analysis method, therefore rapid and simultaneous analysis of multicomponents can be achieved by NIRS technology, decreasing the cost of proximate analysis for straw.

A robust and fast method of sampling and analysis of delta13C of dissolved inorganic carbon in ground waters.

PubMed

Spötl, Christoph

2005-09-01

The stable carbon isotopic composition of dissolved inorganic carbon (delta13C(DIC)) is traditionally determined using either direct precipitation or gas evolution methods in conjunction with offline gas preparation and measurement in a dual-inlet isotope ratio mass spectrometer. A gas evolution method based on continuous-flow technology is described here, which is easy to use and robust. Water samples (100-1500 microl depending on the carbonate alkalinity) are injected into He-filled autosampler vials in the field and analysed on an automated continuous-flow gas preparation system interfaced to an isotope ratio mass spectrometer. Sample analysis time including online preparation is 10 min and overall precision is 0.1 per thousand. This method is thus fast and can easily be automated for handling large sample batches.

Simultaneous collection of airborne particulate matter on several collection substrates with a high-volume cascade impactor

NASA Astrophysics Data System (ADS)

Chan, Y. C.; Vowles, P. D.; McTainsh, G. H.; Simpson, R. W.; Cohen, D. D.; Bailey, G. M.; McOrist, G. D.

This paper describes a method for the simultaneous collection of size-fractionated aerosol samples on several collection substrates, including glass-fibre filter, carbon tape and silver tape, with a commercially available high-volume cascade impactor. This permitted various chemical analysis procedures, including ion beam analysis (IBA), instrumental neutron activation analysis (INAA), carbon analysis and scanning electron microscopy (SEM), to be carried out on the samples.

Correlation of soil and sediment organic matter polarity to aqueous sorption of nonionic compounds

USGS Publications Warehouse

Kile, D.E.; Wershaw, R. L.; Chiou, C.T.

1999-01-01

Polarities of the soiL/sediment organic matter (SOM) in 19 soil and 9 freshwater sediment sam pies were determined from solid-state 13C-CP/MAS NMR spectra and compared with published partition coefficients (K(oc)) of carbon tetrachloride (CT) from aqueous solution. Nondestructive analysis of whole samples by solid-state NMR permits a direct assessment of the polarity of SOM that is not possible by elemental analysis. The percent of organic carbon associated with polar functional groups was estimated from the combined fraction of carbohydrate and carboxylamide-ester carbons. A plot of the measured partition coefficients (K(oc)) of carbon tetrachloride (CT) vs. percent polar organic carbon (POC) shows distinctly different populations of soils and sediments as well as a roughly inverse trend among the soil/sediment populations. Plots of K(oc) values for CT against other structural group carbon fractions did not yield distinct populations. The results indicate that the polarity of SOM is a significant factor in accounting for differences in K(oc) between the organic matter in soils and sediments. The alternate direct correlation of the sum of aliphatic and aromatic structural carbons with K(oc) illustrates the influence of nonpolar hydrocarbon on solute partition interaction. Additional elemental analysis data of selected samples further substantiate the effect of the organic matter polarity on the partition efficiency of nonpolar solutes. The separation between soil and sediment samples based on percent POC reflects definite differences of the properties of soil and sediment organic matters that are attributable to diagenesis.Polarities of the soil/sediment organic matter (SOM) in 19 soil and 9 freshwater sediment samples were determined from solid-state 13C-CP/MAS NMR spectra and compared with published partition coefficients (Koc) of carbon tetrachloride (CT) from aqueous solution. Nondestructive analysis of whole samples by solid-state NMR permits a direct assessment of the polarity of SOM that is not possible by elemental analysis. The percent of organic carbon associated with polar functional groups was estimated from the combined fraction of carbohydrate and carboxyl-amide-ester carbons. A plot of the measured partition coefficients (Koc) of carbon tetrachloride (CT) vs. percent polar organic carbon (POC) shows distinctly different populations of soils and sediments as well as a roughly inverse trend among the soil/sediment populations. Plots of Koc values for CT against other structural group carbon fractions did not yield distinct populations. The results indicate that the polarity of SOM is a significant factor in accounting for differences in Koc between the organic matter in soils and sediments. The alternate direct correlation of the sum of aliphatic and aromatic structural carbons with Koc illustrates the influence of nonpolar hydrocarbon on solute partition interaction. Additional elemental analysis data of selected samples further substantiate the effect of the organic matter polarity on the partition efficiency of nonpolar solutes. The separation between soil and sediment samples based on percent POC reflects definite differences of the properties of soil and sediment organic matters that are attributable to diagenesis.

Pharmacokinetics Evaluation of Carbon Nanotubes Using FTIR Analysis and Histological Analysis.

PubMed

Gherman, Claudia; Tudor, Matea Cristian; Constantin, Bele; Flaviu, Tabaran; Stefan, Razvan; Maria, Bindea; Chira, Sergiu; Braicu, Cornelia; Pop, Laura; Petric, Roxana Cojocneanu; Berindan-Neagoe, Ioana

2015-04-01

Carbon nanotubes (CNTs) are biologically non-toxic and long-circulating nanostructures that have special physical properties. This study was focused on developing alternative methods that track carbon nanotubes, like FR-IR to classical tissue histological procedure. FT-IR absorption spectra were used to confirm the carboxylation of carbon nanotubes and to evaluate the presence of carbon nanotubes from bulk spleen samples and histologically prepared samples (control spleen and spleen with SWCNT-COOH). FT-IR spectrum of spleen sample from animals injected with CNTs shows major spectral differences consisting in infrared bands located at ~1173 cm(-1), ~ 1410 cm(-1); ~1658 cm(-1), ~1737 cm(-1) and around 1720 cm(-1) respectively. In terms of localization of carbon nanotubes, selective accumulation of marginal zone macrophages and splenic red pulp is observed for all treated groups, indicating the presence of carbon nanotubes even at 3, 4 and 7 days after treatment. In summary, we believe that histological evaluation and FT-IR can provide more characteristic information about the pharmacokinetcis and the clearance of carbon nanotubes.

Dissolution of barite for the analysis of strontium isotopes and other chemical and isotopic variations using aqueous sodium carbonate

USGS Publications Warehouse

Breit, G.N.; Simmons, E.C.; Goldhaber, M.B.

1985-01-01

A simple procedure for preparing barite samples for chemical and isotopic analysis is described. Sulfate ion, in barite, in the presence of high concentrations of aqueous sodium carbonate, is replaced by carbonate. This replacement forms insoluble carbonates with the cations commonly in barite: Ba, Sr, Ca and Pb. Sulfate is released into the solution by the carbonate replacement and is separated by filtration. The aqueous sulfate can then be reprecipitated for analysis of the sulfur and oxygen isotopes. The cations in the carbonate phase can be dissolved by acidifying the solid residue. Sr can be separated from the solution for Sr isotope analysis by ion-exchange chromatography. The sodium carbonate used contains amounts of Sr which will affect almost all barite 87Sr 86Sr ratios by less than 0.00001 at 1.95?? of the mean. The procedure is preferred over other techniques used for preparing barite samples for the determination of 87Sr 86Sr ratios because it is simple, rapid and enables simultaneous determination of many compositional parameters on the same material. ?? 1985.

Oxygen analyzer

DOEpatents

Benner, W.H.

1984-05-08

An oxygen analyzer which identifies and classifies microgram quantities of oxygen in ambient particulate matter and for quantitating organic oxygen in solvent extracts of ambient particulate matter. A sample is pyrolyzed in oxygen-free nitrogen gas (N/sub 2/), and the resulting oxygen quantitatively converted to carbon monoxide (CO) by contact with hot granular carbon (C). Two analysis modes are made possible: (1) rapid determination of total pyrolyzable obtained by decomposing the sample at 1135/sup 0/C, or (2) temperature-programmed oxygen thermal analysis obtained by heating the sample from room temperature to 1135/sup 0/C as a function of time. The analyzer basically comprises a pyrolysis tube containing a bed of granular carbon under N/sub 2/, ovens used to heat the carbon and/or decompose the sample, and a non-dispersive infrared CO detector coupled to a mini-computer to quantitate oxygen in the decomposition products and control oven heating.

Oxygen analyzer

DOEpatents

Benner, William H.

1986-01-01

An oxygen analyzer which identifies and classifies microgram quantities of oxygen in ambient particulate matter and for quantitating organic oxygen in solvent extracts of ambient particulate matter. A sample is pyrolyzed in oxygen-free nitrogen gas (N.sub.2), and the resulting oxygen quantitatively converted to carbon monoxide (CO) by contact with hot granular carbon (C). Two analysis modes are made possible: (1) rapid determination of total pyrolyzable oxygen obtained by decomposing the sample at 1135.degree. C., or (2) temperature-programmed oxygen thermal analysis obtained by heating the sample from room temperature to 1135.degree. C. as a function of time. The analyzer basically comprises a pyrolysis tube containing a bed of granular carbon under N.sub.2, ovens used to heat the carbon and/or decompose the sample, and a non-dispersive infrared CO detector coupled to a mini-computer to quantitate oxygen in the decomposition products and control oven heating.

Lunar carbon chemistry - Relations to and implications for terrestrial organic geochemistry.

NASA Technical Reports Server (NTRS)

Eglinton, G.; Maxwell, J. R.; Pillinger, C. T.

1972-01-01

Survey of the various ways in which studies of lunar carbon chemistry have beneficially affected terrestrial organic geochemistry. A lunar organic gas-analysis operating system is cited as the most important instrumental development in relation to terrestrial organic geochemistry. Improved methods of analysis and handling of organic samples are cited as another benefit derived from studies of lunar carbon chemistry. The problem of controlling contamination and minimizing organic vapors is considered, as well as the possibility of analyzing terrestrial samples by the techniques developed for lunar samples. A need for new methods of analyzing carbonaceous material which is insoluble in organic solvents is indicated.

Ammonia modification of activated carbon to enhance carbon dioxide adsorption: Effect of pre-oxidation

NASA Astrophysics Data System (ADS)

Shafeeyan, Mohammad Saleh; Daud, Wan Mohd Ashri Wan; Houshmand, Amirhossein; Arami-Niya, Arash

2011-02-01

A commercial granular activated carbon (GAC) was subjected to thermal treatment with ammonia for obtaining an efficient carbon dioxide (CO2) adsorbent. In general, CO2 adsorption capacity of activated carbon can be increased by introduction of basic nitrogen functionalities onto the carbon surface. In this work, the effect of oxygen surface groups before introduction of basic nitrogen functionalities to the carbon surface on CO2 adsorption capacity was investigated. For this purpose two different approaches of ammonia treatment without preliminary oxidation and amination of oxidized samples were studied. Modified carbons were characterized by elemental analysis and Fourier Transform Infrared spectroscopy (FT-IR) to study the impact of changes in surface chemistry and formation of specific surface groups on adsorption properties. The texture of the samples was characterized by conducting N2 adsorption/desorption at -196 °C. CO2 capture performance of the samples was investigated using a thermogravimetric analysis (TGA). It was found that in both modification techniques, the presence of nitrogen functionalities on carbon surface generally increased the CO2 adsorption capacity. The results indicated that oxidation followed by high temperature ammonia treatment (800 °C) considerably enhanced the CO2 uptake at higher temperatures.

Optoelectronic system of online measurements of unburned carbon in coal fly ash

NASA Astrophysics Data System (ADS)

Golas, Janusz; Jankowski, Henryk; Niewczas, Bogdan; Piechna, Janusz; Skiba, Antoni; Szkutnik, Wojciech; Szkutnik, Zdzislaw P.; Wartak, Ryszarda; Worek, Cezary

2001-08-01

Carbon-in-ash level is an important consideration for combustion efficiency as well as ash marketing. The optoelectronic analyzing system for on-line determination and monitoring of the u burned carbon content of ash samples is presented. The apparatus operates on the principle that carbon content is proportional to the reflectance of IR light. Ash samples are collected iso kinetically from the flue gas duct and placed in a sample tube with a flat glass bottom. The same is then exposed to a light. The reflectance intensity is used by the system's computer to determine residual carbon content from correlation curves. The sample is then air purged back to the duct or to the attached sample canister to enable laboratory check analysis. The total cycle time takes between 5 and 10 minutes. Real time result of carbon content with accuracy 0.3-0.7 percent are reported and can be used for boiler controlling.

THE NIST-EPA INTERAGENCY AGREEMENT ON MEASUREMENTS AND STANDARDS IN AEROSOL CARBON: SAMPLING REGIONAL PM 2.5 FOR THE CHEMOMETRIC OPTIMIZATION OF THERMAL-OPTICAL ANALYSIS

EPA Science Inventory

Results from the NIST-EPA Interagency Agreement on Measurements and Standards in Aerosol Carbon: Sampling Regional PM2.5 for the Chemometric Optimization of Thermal-Optical Analysis Study will be presented at the American Association for Aerosol Research (AAAR) 24th Annual Confer...

Multiple-element semiquantitative analysis of one-milligram geochemical samples by D.C. arc emission spectrography

USGS Publications Warehouse

Rait, N.

1981-01-01

A modified method is described for a 1-mg sample multi-element semiquantitative spectrographic analysis. This method uses a direct-current arc source, carbon instead of graphite electrodes, and an 80% argon-20% oxygen atmosphere instead of air. Although this is a destructive method, an analysis can be made for 68 elements in all mineral and geochemical samples. Carbon electrodes have been an aid in improving the detection limits of many elements. The carbon has a greater resistance to heat conductance and develops a better tip, facilitating sample volatilization and counter balancing the cooling effect of a flow of the argon-oxygen mixture around the anode. Where such an argon-oxygen atmosphere is used instead of air, the cyanogen band lines are greatly diminished in intensity, and thus more spectral lines of analysis elements are available for use; the spectral background is also lower. The main advantage of using the carbon electrode and the 80% argon-20% oxygen atmosphere is the improved detection limits of 36 out of 68 elements. The detection limits remain the same for 23 elements, and are not as good for only nine elements. ?? 1981.

Application of selected methods of remote sensing for detecting carbonaceous water pollution

NASA Technical Reports Server (NTRS)

Davis, E. M.; Fosbury, W. J.

1973-01-01

A reach of the Houston Ship Channel was investigated during three separate overflights correlated with ground truth sampling on the Channel. Samples were analyzed for such conventional parameters as biochemical oxygen demand, chemical oxygen demand, total organic carbon, total inorganic carbon, turbidity, chlorophyll, pH, temperature, dissolved oxygen, and light penetration. Infrared analyses conducted on each sample included reflectance ATR analysis, carbon tetrachloride extraction of organics and subsequent scanning, and KBr evaporate analysis of CCl4 extract concentrate. Imagery which was correlated with field and laboratory data developed from ground truth sampling included that obtained from aerial KA62 hardware, RC-8 metric camera systems, and the RS-14 infrared scanner. The images were subjected to analysis by three film density gradient interpretation units. Data were then analyzed for correlations between imagery interpretation as derived from the three instruments and laboratory infrared signatures and other pertinent field and laboratory analyses.

Carbon Isotopic Composition of CO2, Evolved During Perchlorate-Induced Reactions in Mars Analog Materials: Interpreting SAM/MSL Rocknest Data

NASA Technical Reports Server (NTRS)

Stern, J. C.; McAdam, A. C.; Archer, P. D., Jr.; Bower, H.; Buch, A.; Eigenbrode, J.; Freissinet, C.; Franz, H. B.; Glavin, D.; Jones, J. H.;

Nanophase Carbonates on Mars: Formation, Detection, and Implications

NASA Technical Reports Server (NTRS)

Archer, P. D.; Lauer, H. V.; Ming, D. W.; Niles, P. B.; Morris, R. V.; Rampe, E. B.; Sutter, B.

2014-01-01

Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered on Mars in small amounts in martian dust, in soils in the Northern Plains, and in outcrops of limited spatial extent. Recently, carbonates have been identified as the possible source of CO2 released during thermal analysis of material from an aeolian deposit named Rocknest and drilled sample from the sheepbed mudstone, both samples analyzed by the Mars Science Laboratory (MSL) in Gale Crater. Both the Phoenix lander and MSL carry thermal analysis instruments, the Thermal and Evolved Gas Analyzer (TEGA) on Phoenix and the Sample Analysis at Mars (SAM) instrument on MSL. While thermal analysis does not provide definitive mineralogy, it can detect volatile-bearing minerals present at very low abundance and the temperature profiles of evolved gases can reveal physical properties of the sample. For example, the decomposition temperature of volatilebearing minerals depends heavily on the particle size of the mineral.

Continuous versus pulse neutron induced gamma spectroscopy for soil carbon analysis

USDA-ARS?s Scientific Manuscript database

Neutron induced gamma spectra analysis (NGA) provides a means of measuring carbon in large soil volumes without destructive sampling. Calibration of the NGA system must account for system background and the interference of other nuclei on the carbon peak at 4.43 MeV. Accounting for these factors pro...

Improved method for the determination of nonpurgeable suspended organic carbon in natural water by silver filter filtration, wet chemical oxidation, and infrared spectrometry

USGS Publications Warehouse

Burkhardt, Mark R.; Brenton, Ronald W.; Kammer, James A.; Jha, Virenda K.; O'Mara-Lopez, Peggy G.; Woodworth, Mark T.

1999-01-01

Precision and accuracy are reported for the first time for the analysis of nonpurgeable suspended organic carbon by silver membrane filtration followed by wet chemical oxidation. A water sample is pressure filtered through a 0.45‐μm‐pore‐size, 47‐mm‐diameter silver membrane filter. The silver membrane filter then is cut into ribbons and placed in a flame‐sealable glass ampule. The organic material trapped on the membrane filter strips is acidified, purged with oxygen to remove inorganic carbonates and volatile organic compounds, and oxidized to carbon dioxide (CO2) using phosphoric acid and potassium persulfate in the sealed glass ampule. The resulting CO2 is measured by a nondispersive infrared CO2 detector. The amount of CO2 is proportional to the concentration of chemically oxidizable nonpurgeable organic carbon in the environmental water sample. The quantitation and method detection limit for routine analysis is 0.2 mg/L. The average percent recovery in five representative matrices was 97 ± 11%. The errors associated with sampling and sample preparation of nonpurgeable suspended organic carbon are also described.

Activated carbon production from bagasse and banana stem at various times of carbonization

NASA Astrophysics Data System (ADS)

Misran, E.; Maulina, S.; Dina, S. F.; Nazar, A.; Harahap, S. A.

2018-02-01

The utilization of bagasse and banana stem as activated carbon precursors has been conducted. In this study, the dried samples were impregnated using phosphoric acid (H3PO4) solution as the activator at a ratio of sample to the activator (w/w) was 1:1. The impregnation was conducted at room temperature for 24 hours. The samples then carbonized at 400 °C for 30, 45 and 60 minutes and finally washed and dried to obtain the activated carbon. The research aimed to investigate the effects of time of carbonization on the characteristics of activated carbon produced from bagasse and banana stem. The result showed that yield of activated carbon was in the range of 40.03 - 46.73 % with a high content of carbon as high 90.33 %. The result of BET analysis showed that the highest surface area reached1130.465 m2/g.

Carbon analysis for inspecting carbonation of concrete using a TEA CO2 laser-induced plasma.

PubMed

Kagawa, Kiichiro; Idris, Nasrullah; Wada, Munehide; Kurniawan, Hendrik; Tsuyuki, Kenichiro; Miura, Satoru

2004-08-01

It has been demonstrated that a spectrochemical analysis of carbon using the laser plasma method can be successfully applied to inspect the carbonation of concrete by detecting carbon produced in aged concrete by a chemical reaction of Ca(OH)2 with CO2 gas in environmental air, turning into CaCO3, which induces degradation of the quality of building concrete. A comparative study has been made using a TEA CO2 laser (500-1000 mJ) and a Q-switched Nd-YAG laser (50-200 mJ) to search for the optimum conditions for carbon analysis, proving the advantage of the TEA CO2 laser for this purpose. Also, it was clarified that laser irradiation with suitable defocusing conditions is a crucial point for obtaining high sensitivity in the detection of carbon. Practical experiments on the inspection of carbonation were carried out using both a concrete sample that had been intentionally carbonated by exposure to high concentrations of CO2 gas and a naturally carbonated concrete sample. As a result, good coincidence was observed between the laser method and the ordinary method, which uses the chemical indicator phenolphthalein, implying that this laser technique is applicable as an in situ quantitative method of inspection for carbonation of concrete.

Light attenuation versus evolved carbon (AVEC) - A new way to look at elemental and organic carbon analysis

NASA Astrophysics Data System (ADS)

Nicolosi, E. M. G.; Quincey, P.; Font, A.; Fuller, G. W.

2018-02-01

The Attenuation Versus Evolved Carbon (AVEC) plot is a new way to represent thermal-optical organic carbon/elemental carbon (OC/EC) analysis data. The accumulated carbon concentration is plotted against the attenuation (ln (I0/I)). Unlike the thermogram, it provides information about the sample properties rather than the instantaneous instrument sensor status. The plot can be used to refine the determination of OC and EC split point, either from consideration of laser instability or transit time within the instrument; to investigate the optical properties of the particles; and to spot the early evolution of pyrolysed carbon (PC) and/or EC during the inert phase. 168 samples from three sites were studied. The gradient of the AVEC plot curve in the oxygenated phase provides information about the mass absorption cross section (σ) of the particles leaving the filter. The σ of the PC generated in the higher temperature Quartz protocol was greater than the PC generated in the lower temperature EUSAAR_2 protocol. Also, in both cases the PC evolved at a lower temperature in the oxygenated phase than the native EC. To minimise the shadowing effect, σ was also measured for the particles leaving the filter at the end of the analysis. These σ values, which are expected to be a combination of inherent σ together with fixed instrumental factors, were consistent between the different sites (45 ± 10 m2 g-1 in rural samples, 42 ± 8 m2 g-1 in urban samples and 35 ± 14 m2 g-1 in roadside samples). The AVEC plot can be generated from the data routinely produced by the analytical instrument using the R-code supplied in the supplementary material.

Supercritical Water Oxidation Total Organic Carbon (TOC) Analysis

EPA Pesticide Factsheets

The work presented here is the evaluation of the modified wet‐oxidation method described as Supercritical Water Oxidation (SCWO) for the analysis of total organic carbon (TOC) in very difficult oil/gas produced water sample matrices.

Radiocarbon Analysis to Calculate New End-Member Values for Biomass Burning Source Samples Specific to the Bay Area

NASA Astrophysics Data System (ADS)

Yoon, S.; Kirchstetter, T.; Fairley, D.; Sheesley, R. J.; Tang, X.

2017-12-01

Elemental carbon (EC), also known as black carbon or soot, is an important particulate air pollutant that contributes to climate forcing through absorption of solar radiation and to adverse human health impacts through inhalation. Both fossil fuel combustion and biomass burning, via residential firewood burning, agricultural burning, wild fires, and controlled burns, are significant sources of EC. Our ability to successfully control ambient EC concentrations requires understanding the contribution of these different emission sources. Radiocarbon (14C) analysis has been increasingly used as an apportionment tool to distinguish between EC from fossil fuel and biomass combustion sources. However, there are uncertainties associated with this method including: 1) uncertainty associated with the isolation of EC to be used for radiocarbon analysis (e.g., inclusion of organic carbon, blank contamination, recovery of EC, etc.) 2) uncertainty associated with the radiocarbon signature of the end member. The objective of this research project is to utilize laboratory experiments to evaluate some of these uncertainties, particularly for EC sources that significantly impact the San Francisco Bay Area. Source samples of EC only and a mix of EC and organic carbon (OC) were produced for this study to represent known emission sources and to approximate the mixing of EC and OC that would be present in the atmosphere. These samples include a combination of methane flame soot, various wood smoke samples (i.e. cedar, oak, sugar pine, pine at various ages, etc.), meat cooking, and smoldering cellulose smoke. EC fractions were isolated using a Sunset Laboratory's thermal optical transmittance carbon analyzer. For 14C analysis, samples were sent to Woods Hole Oceanographic Institution for isotope analysis using an accelerated mass spectrometry. End member values and uncertainties for the EC isolation utilizing this method will be reported.

Perchlorate and volatiles of the brine of Lake Vida (Antarctica): Implication for the in situ analysis of Mars sediments

NASA Astrophysics Data System (ADS)

Kenig, Fabien; Chou, Luoth; McKay, Christopher P.; Jackson, W. Andrew; Doran, Peter T.; Murray, Alison E.; Fritsen, Christian H.

2016-07-01

The cold (-13.4°C), cryoencapsulated, anoxic, interstitial brine of the >27 m thick ice of Lake Vida (Victoria Valley, Antarctica) contains 49 µg · L-1 of perchlorate and 11 µg · L-1 of chlorate. Lake Vida brine (LVBr) may provide an analog for potential oxychlorine-rich subsurface brine on Mars. LVBr volatiles were analyzed by solid-phase microextraction (SPME) gas chromatography-mass spectrometry (GC-MS) with two different SPME fibers. With the exception of volatile organic sulfur compounds, most other volatiles observed were artifacts produced in the GC injector when the thermal decomposition products of oxychlorines reacted with reduced carbon derived from LVBr and the SPME fiber phases. Analysis of MilliQ water with perchlorate (40 µg · L-1) showed low level of organic artifacts, reflecting carbon limitation. In order to observe sample-derived organic compounds, both in analog samples and on Mars, the molar abundance of reduced carbon in a sample must exceed those of O2 and Cl2 produced during decomposition of oxychlorines. This suggests that the abundance of compounds observed by the Sample Analysis at Mars (SAM) instruments in Sheepbed samples (CB-3, CB5, and CB6) may be controlled by an increase in the reduced-carbon/oxychlorine ratio of these samples. To increase chances of in situ detection of Martian organics during pyrolysis-GC-MS, we propose that the derivatization agents stored on SAM may be used as an external source of reduced carbon, increasing artificially the reduced-carbon to perchlorate ratio during pyrolysis, allowing the expression of more abundant and perhaps more diverse Martian organic matter.

Perchlorate and Volatiles of the Brine of Lake Vida (Antarctica): Implication for the in Situ Analysis of Mars Sediments

NASA Technical Reports Server (NTRS)

Kenig, Fabien; Chou, Luoth; McKay, Christopher P.; Jackson, W. Andrew; Doran, Peter T.; Murray, Alison E.; Fritsen, Christian H.

2016-01-01

The cold (-13.4 C), cryoencapsulated, anoxic, interstitial brine of the 27 m-thick ice of Lake Vida (Victoria Valley, Antarctica) contains 49 microgram L-1 of perchlorate and 11 microgram L-1 of chlorate. Lake Vida brine (LVBr) may provide an analog for potential oxychlorine-rich subsurface brine on Mars. LVBr volatiles were analyzed by solid-phase microextraction (SPME) gas chromatography-mass spectrometry (GC-MS) with two different SPME fibers. With the exception of volatile organic sulfur compounds, most other volatiles observed were artifacts produced in the GC injector when the thermal decomposition products of oxychlorines reacted with reduced carbon derived from LVBr and the SPME fiber phases. Analysis of MilliQ water with perchlorate (40 microgram L-1) showed low level of organic artifacts, reflecting carbon limitation. In order to observe sample-derived organic compounds, both in analog samples and on Mars, the molar abundance of reduced carbon in a sample must exceed those of O2 and Cl2 produced during decomposition of oxychlorines. This suggests that the abundance of compounds observed by the Sample Analysis at Mars (SAM) instruments in Sheepbed samples (CB-3, CB5, and CB6) may be controlled by an increase in the reduced-carbon/oxychlorine ratio of these samples. To increase chances of in situ detection of Martian organics during pyrolysis-GC-MS, we propose that the derivatization agents stored on SAM may be used as an external source of reduced carbon, increasing artificially the reduced-carbon to perchlorate ratio during pyrolysis, allowing the expression of more abundant and perhaps more diverse Martian organic matter.

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.

Sample Analysis at Mars for Curiosity

NASA Image and Video Library

2010-10-08

The Sample Analysis at Mars SAM instrument will analyze samples of Martian rock and soil collected by the rover arm to assess carbon chemistry through a search for organic compounds, and to look for clues about planetary change.

METHOD 415.3 - MEASUREMENT OF TOTAL ORGANIC ...

EPA Pesticide Factsheets

2.0 SUMMARY OF METHOD2.1 In both TOC and DOC determinations, organic carbon in the water sample is oxidized to form carbon dioxide (CO2), which is then measured by a detection system. There are two different approaches for the oxidation of organic carbon in water samples to carbon dioxide gas: (a) combustion in an oxidizing gas and (b) UV promoted or heat catalized chemical oxidation with a persulfate solution. Carbon dioxide, which is released from the oxidized sample, is detected by a conductivity detector or by a nondispersive infrared (NDIR) detector. Instruments using any combination of the above technologies may be used in this method.2.2. Setteable solids and floating matter may cause plugging of valves, tubing, and the injection needle port. The TOC procedure allows the removal of settleable solids and floating matter. The suspended matter is considered part of the sample. The resulting water sample is then considered a close approximation of the original whole water sample for the purpose of TOC measurement.2.3. The DOC procedure requires that the sample be passed through a 0.45 um filter prior to analysis.2.4. The TOC and DOC procedures require that all inorganic carbon be removed from the sample before the sample is analyzed for organic carbon content. If the inorganic carbon (IC) is not completely removed, significant error will occur. The inorganic carbon interference is removed by converting the mineralized IC to CO2 by acidification and

The Role of (Delta)C-13 in the Search for Reduced Organics on the Surface of Mars

NASA Technical Reports Server (NTRS)

Stern, J. C.; McAdam, A. C.

2012-01-01

The capabilities of the Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) to detect trace amounts of organic carbon compounds are unprecedented, and MSL may be the first mission to reveal the presence of organic carbon on Mars. The search for reduced organic carbon on Mars is inextricably tied to: a) the preservation potential of the environment from which we take a solid sample, and b) the evolved gas analysis (EGA) techniques used by SAM to release volatiles from this solid sample. Several prospective targets have been identified for sample analysis at Gale Crater. Stratigraphic sequences of phyllosilicates and sulfates at Gale are thought to represent a period of global climate transition from a moderate pH lacustrine environment to an evaporitic environment, both of which could sequester organic carbon (Thomson et al. 2011). The sediment mound in Gale Crater contains a range of lithologies suggesting changes in redox conditions, and evidence of both lacustrine and fluvial depositional processes, which may have transported organic carbon from the layer in which it formed and resulted in its preservation elsewhere within the crater (Anderson and Bell, 2010). Inverted channel fills suggest erosion resistant material that could serve to preserve organics originally deposited in a low energy aqueous environment. The lithology sampled will affect not only the preservation of organics, but also our ability to detect organics during our evolved gas analysis, based on the sample matrix. For example, reduced organics may be trapped in the mineral structure, and thermal evolution of these organics will occur during thermal decomposition of the host mineral. If organics are occluded in minerals that have very high thermal decomposition temperatures, they may be, in effect, "too well preserved," and difficult to detect during EGA. Alternatively, the possible presence of perchlorate, or other strong oxidants in surface regolith, may result in destruction of structural information identifying organic molecules before reaching the QMS on SAM via oxidation to C02 during heating. If this is the case, the stable carbon isotopic composition (delta 13C) of the C02 evolved and measured by the Tunable Laser Spectrometer (TLS) on SAM may help identify the presence of organics. On Earth, biological activity can cause large fractionations of 13C/12C, which can preserved in sedimentary deposits and distinguish the organic products of biotic processes from inorganic atmospheric and geological reservoirs. It is plausible that similar fractionations could occur on Mars and be preserved in reduced organic matter in sediments. Bulk delta 13C measurements alone may not reveal a signature of trace organic carbon that may be present along with inorganic carbon. If both organic and inorganic carbon compounds are present, it may be possible to detect the organic carbon by comparing the 013C of pyrolysis and combustion experiments. The TLS on SAM is capable of obtaining high precision measurements of delta13C from C02 evolved during pyrolysis and combustion of solid regolith samples. Because carbonates are expected to be present at abundances of 0.1-1 % in Martian soil, and organics in the ppb range (Webster and Mahaffy, 2011), analog samples must represent this mix of reduced organic carbon and carbonate. The work presented here will examine the use of delta13C of C02 produced during combustion of bulk Mars analog samples as a proxy for detection of reduced organic carbon.

Optimizing sample pretreatment for compound-specific stable carbon isotopic analysis of amino sugars in marine sediment

NASA Astrophysics Data System (ADS)

Zhu, R.; Lin, Y.-S.; Lipp, J. S.; Meador, T. B.; Hinrichs, K.-U.

2014-01-01

Amino sugars are quantitatively significant constituents of soil and marine sediment, but their sources and turnover in environmental samples remain poorly understood. The stable carbon isotopic composition of amino sugars can provide information on the lifestyles of their source organisms and can be monitored during incubations with labeled substrates to estimate the turnover rates of microbial populations. However, until now, such investigation has been carried out only with soil samples, partly because of the much lower abundance of amino sugars in marine environments. We therefore optimized a procedure for compound-specific isotopic analysis of amino sugars in marine sediment employing gas chromatography-isotope ratio mass spectrometry. The whole procedure consisted of hydrolysis, neutralization, enrichment, and derivatization of amino sugars. Except for the derivatization step, the protocol introduced negligible isotopic fractionation, and the minimum requirement of amino sugar for isotopic analysis was 20 ng, i.e. equivalent to ~ 8 ng of amino sugar carbon. Our results obtained from δ13C analysis of amino sugars in selected marine sediment samples showed that muramic acid had isotopic imprints from indigenous bacterial activities, whereas glucosamine and galactosamine were mainly derived from organic detritus. The analysis of stable carbon isotopic compositions of amino sugars opens a promising window for the investigation of microbial metabolisms in marine sediments and the deep marine biosphere.

Methodologies for extraction of dissolved inorganic carbon for stable carbon isotope studies : evaluation and alternatives

USGS Publications Warehouse

Hassan, Afifa Afifi

1982-01-01

The gas evolution and the strontium carbonate precipitation techniques to extract dissolved inorganic carbon (DIC) for stable carbon isotope analysis were investigated. Theoretical considerations, involving thermodynamic calculations and computer simulation pointed out several possible sources of error in delta carbon-13 measurements of the DIC and demonstrated the need for experimental evaluation of the magnitude of the error. An alternative analytical technique, equilibration with out-gassed vapor phase, is proposed. The experimental studies revealed that delta carbon-13 of the DIC extracted from a 0.01 molar NaHC03 solution by both techniques agreed within 0.1 per mil with the delta carbon-13 of the DIC extracted by the precipitation technique, and an increase of only 0.27 per mil in that extracted by the gas evolution technique. The efficiency of extraction of DIC decreased with sulfate concentration in the precipitation technique but was independent of sulfate concentration in the gas evolution technique. Both the precipitation and gas evolution technique were found to be satisfactory for extraction of DIC from different kinds of natural water for stable carbon isotope analysis, provided appropriate precautions are observed in handling the samples. For example, it was found that diffusion of atmospheric carbon dioxide does alter the delta carbon-13 of the samples contained in polyethylene bottles; filtration and drying in the air change the delta carbon-13 of the samples contained in polyethylene bottles; filtration and drying in the air change the delta carbon-13 of the precipitation technique; hot manganese dioxide purification changes the delta carbon-13 of carbon dioxide. (USGS)

Comparison of methods for the quantification of the different carbon fractions in atmospheric aerosol samples

NASA Astrophysics Data System (ADS)

Nunes, Teresa; Mirante, Fátima; Almeida, Elza; Pio, Casimiro

2010-05-01

Atmospheric carbon consists of: organic carbon (OC, including various organic compounds), elemental carbon (EC, or black carbon [BC]/soot, a non-volatile/light-absorbing carbon), and a small quantity of carbonate carbon. Thermal/optical methods (TOM) have been widely used for quantifying total carbon (TC), OC, and EC in ambient and source particulate samples. Unfortunately, the different thermal evolution protocols in use can result in a wide elemental carbon-to-total carbon variation. Temperature evolution in thermal carbon analysis is critical to the allocation of carbon fractions. Another critical point in OC and EC quantification by TOM is the interference of carbonate carbon (CC) that could be present in the particulate samples, mainly in the coarse fraction of atmospheric aerosol. One of the methods used to minimize this interference consists on the use of a sample pre-treatment with acid to eliminate CC prior to thermal analysis (Chow et al., 2001; Pio et al., 1994). In Europe, there is currently no standard procedure for determining the carbonaceous aerosol fraction, which implies that data from different laboratories at various sites are of unknown accuracy and cannot be considered comparable. In the framework of the EU-project EUSAAR, a comprehensive study has been carried out to identify the causes of differences in the EC measured using different thermal evolution protocols. From this study an optimised protocol, the EUSAAR-2 protocol, was defined (Cavali et al., 2009). During the last two decades thousands of aerosol samples have been taken over quartz filters at urban, industrial, rural and background sites, and also from plume forest fires and biomass burning in a domestic closed stove. These samples were analysed for OC and EC, by a TOM, similar to that in use in the IMPROVE network (Pio et al., 2007). More recently we reduced the number of steps in thermal evolution protocols, without significant repercussions in the OC/EC quantifications. In order to evaluate the possibility of continue using, for trend analysis, the historical data set, we performed an inter-comparison between our method and an adaptation of EUSAAR-2 protocol, taking into account that this last protocol will possibly be recommended for analysing carbonaceous aerosols at European sites. In this inter-comparison we tested different types of samples (PM2,5, PM2,5-10, PM10) with large spectra of carbon loadings, with and without pre-treatment acidification. For a reduced number of samples, five replicates of each one were analysed by each method for statistical purposes. The inter-comparison study revealed that when the sample analysis were performed in similar room conditions, the two thermo-optic methods give similar results for TC, OC and EC, without significant differences at a 95% confidence level. The correlation between the methods, DAO and EUSAAR-2 for EC is smaller than for TC and OC, although showing a coefficient correlation over 0,95, with a slope close to one. For samples performed in different periods, room temperatures seem to have a significant effect over OC quantification. The sample pre-treatment with HCl fumigation tends to decrease TC quantification, mainly due to the more volatile organic fraction release during the first heating step. For a set of 20 domestic biomass burning samples analyzed by the DAO method we observed an average decrease in TC quantification of 3,7 % in relation to non-acidified samples, even though this decrease is accompanied by an average increase in the less volatile organic fraction. The indirect measurement of carbon carbonate, usually a minor carbon component in the carbonaceous aerosol, based on the difference between TC measured by TOM of acidified and non-acidified samples is not a robust measurement, considering the biases affecting his quantification. The present study show that the two thermo-optic temperature program used for OC and EC quantification give similar results, and if in the future the EUSAAR-2 protocol will be adopted the past measurement of carbonaceous fractions can be used for trend analysis. However this study demonstrates that the temperature control during post-sampling handling is a critical point in total OC and TC quantification that must be assigned in the new European protocol. References: Cavali et al., 2009, AMTD 2, 2321-2345, 2009 Chow et al., 2001, Aerosol. Sci. Technol., 34, 23-34, 2001. Pio et al., 1994, Proceedings of the Sixth European Symposium on Physico-Chemical Behavior of Atmospheric Pollutants. Report EUR 15609/2 EN, pp. 706-711. Pio et al, 2007, J. Geophys. Res. 112, D23S02 Acknowledgement: This work was funded by the Portuguese Science Foundation through the projects POCI/AMB/60267/2004 and PTDC/AMB/65706/2006 (BIOEMI). F. Mirante acknowledges the PhD grant SFRH/BD/45473/2008.

Chemical vapour deposition growth and Raman characterization of graphene layers and carbon nanotubes

NASA Astrophysics Data System (ADS)

Lai, Y.-C.; Rafailov, P. M.; Vlaikova, E.; Marinova, V.; Lin, S. H.; Yu, P.; Yu, S.-C.; Chi, G. C.; Dimitrov, D.; Sveshtarov, P.; Mehandjiev, V.; Gospodinov, M. M.

2016-02-01

Single-layer graphene films were grown by chemical vapour deposition (CVD) on Cu foil. The CVD process was complemented by plasma enhancement to grow also vertically aligned multiwalled carbon nanotubes using Ni nanoparticles as catalyst. The obtained samples were characterized by Raman spectroscopy analysis. Nature of defects in the samples and optimal growth conditions leading to achieve high quality of graphene and carbon nanotubes are discussed.

Publications - GMC 406 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 406 Publication Details Title: Carbon isotope and total organic carbon (TOC) analysis of organic carbon (TOC) analysis of washed and unwashed cuttings from the South Barrow Test #3 well: Alaska Table(s) gmc406_toc.xls (196.0 K) gmc406_samples.xls (144.0 K) Keywords Isotopes; Oil and Gas; Organic

Molecular Analysis of Flood Deposits in the Tennessee River Valley: Implications for Understanding Carbon Cycling in Fluvial Environments and Anthropogenic Impacts

NASA Astrophysics Data System (ADS)

Blackaby, E.; Craven, O. D.; Hockaday, W. C.; Forman, S. L.; Stinchcomb, G. E.

2017-12-01

The middle Tennessee River Valley contains both historic and prehistoric (>AD 1600) flood deposits. Stratigraphic sequences of stacked flood deposits that often bury soils provide new insights on organic matter transported and preserved prior to and after European colonization. This study focused on understanding carbon cycling within a dynamic fluvial system and quantifying the anthropogenic effect on flood processes through the analysis of molecular components of the organic matter. The data may be helpful in discerning the organic geochemical fingerprint for historic and prehistoric flood deposits. Ten samples were collected from three sites at varying depths and dated using optically stimulated luminescence (OSL). All samples underwent solid-state cross polar 13C NMR analysis at twelve kilohertz, and a molecular mixing model (MMM) was used to determine the molecular components of the organic matter present in each sample. The MMM categorized carbon molecules present in each sample in terms of carbohydrate, protein, lipid, lignin, char, or pure carbonyl. Char was the most prominent molecular component of all ten samples ranging from 28.7 to 55.9% and comprised larger percentages in prehistoric deposits. The historic deposits, while still char dominated, showed more molecular diversity with higher percentages in non-char carbon groups. The carbonyl, lipid, and carbohydrate groups are present throughout all the samples with the carbonyl ranging from 9.3 to 31.4%, the lipid from 5.5 to 16.7%, and the carbohydrate from 4.4 to 16.9%. The high amount of carbonyl throughout the samples indicates that the deposits existed in a highly oxidizing environment. Differences in the presence and amount of carbon groups between historic and prehistoric flood deposits potentially reflect diagenic alternation of organic matter through time, changes in human land use, or some combination processes. These preliminary results possibly indicate changes in carbon pools accessed with European cultivation and continued degradation of organic moieties during a ca. 400 years burial, and mostly in oxidizing conditions.

Analyzing indirect secondary electron contrast of unstained bacteriophage T4 based on SEM images and Monte Carlo simulations

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

Ogura, Toshihiko, E-mail: t-ogura@aist.go.jp

2009-03-06

The indirect secondary electron contrast (ISEC) condition of the scanning electron microscopy (SEM) produces high contrast detection with minimal damage of unstained biological samples mounted under a thin carbon film. The high contrast image is created by a secondary electron signal produced under the carbon film by a low acceleration voltage. Here, we show that ISEC condition is clearly able to detect unstained bacteriophage T4 under a thin carbon film (10-15 nm) by using high-resolution field emission (FE) SEM. The results show that FE-SEM provides higher resolution than thermionic emission SEM. Furthermore, we investigated the scattered electron area within themore » carbon film under ISEC conditions using Monte Carlo simulation. The simulations indicated that the image resolution difference is related to the scattering width in the carbon film and the electron beam spot size. Using ISEC conditions on unstained virus samples would produce low electronic damage, because the electron beam does not directly irradiate the sample. In addition to the routine analysis, this method can be utilized for structural analysis of various biological samples like viruses, bacteria, and protein complexes.« less

An effective method of UV-oxidation of dissolved organic carbon in natural waters for radiocarbon analysis by accelerator mass spectrometry

NASA Astrophysics Data System (ADS)

Xue, Yuejun; Ge, Tiantian; Wang, Xuchen

2015-12-01

Radiocarbon (14C) measurement of dissolved organic carbon (DOC) is a very powerful tool to study the sources, transformation and cycling of carbon in the ocean. The technique, however, remains great challenges for complete and successful oxidation of sufficient DOC with low blanks for high precision carbon isotopic ratio analysis, largely due to the overwhelming proportion of salts and low DOC concentrations in the ocean. In this paper, we report an effective UV-Oxidation method for oxidizing DOC in natural waters for radiocarbon analysis by accelerator mass spectrometry (AMS). The UV-oxidation system and method show 95%±4% oxidation efficiency and high reproducibility for DOC in both river and seawater samples. The blanks associated with the method was also low (about 3 µg C) that is critical for 14C analysis. As a great advantage of the method, multiple water samples can be oxidized at the same time so it reduces the sample processing time substantially compared with other UV-oxidation method currently being used in other laboratories. We have used the system and method for 14C studies of DOC in rivers, estuaries, and oceanic environments and have received promise results.

Geochemistry of Precambrian carbonates - 3-shelf seas and non-marine environments of the Archean

NASA Technical Reports Server (NTRS)

Veizer, Jan; Clayton, R. N.; Hinton, R. W.; Von Brunn, Victor; Mason, T. R.

1990-01-01

Samples from the Pangola and Ventersdorp Supergroups (Kaapvaal Craton, South Africa) and from the Fortescue and Hamersley Groups (Pilbara Block, Australia) were analyzed, using XRF, AAS, and isotope-analysis techniques to investigate the mineralogical, chemical, and isotopic features of these representatives of contemporary shelf carbonates (Pangola and Hamersley samples) and nonmarine carbonates (the Ventersdorp and Fortescue samples). Results show that, mineralogically, the shelf carbonates are almost exclusively dolostones, while the lacustrine facies are predominantly limestones. Geological, trace-element, and oxygen-isotope results of the shelf carbonates suggest that their original mineralogy may have been aragonite, and that the Pangola dolostones may represent a direct dolomitization product of this precursor. By contrast, the stabilization of the Hamersley carbonates may have involved an additional step of transformation of a metastable precursor into limestone.

Surface characterization of LDEF carbon fiber/polymer matrix composites

NASA Technical Reports Server (NTRS)

Grammer, Holly L.; Wightman, James P.; Young, Philip R.; Slemp, Wayne S.

1995-01-01

XPS (x-ray photoelectron spectroscopy) and SEM (scanning electron microscopy) analysis of both carbon fiber/epoxy matrix and carbon fiber/polysulfone matrix composites revealed significant changes in the surface composition as a result of exposure to low-earth orbit. The carbon 1s curve fit XPS analysis in conjunction with the SEM photomicrographs revealed significant erosion of the polymer matrix resins by atomic oxygen to expose the carbon fibers of the composite samples. This erosion effect on the composites was seen after 10 months in orbit and was even more obvious after 69 months.

[Estimation of Hunan forest carbon density based on spectral mixture analysis of MODIS data].

PubMed

Yan, En-ping; Lin, Hui; Wang, Guang-xing; Chen, Zhen-xiong

2015-11-01

With the fast development of remote sensing technology, combining forest inventory sample plot data and remotely sensed images has become a widely used method to map forest carbon density. However, the existence of mixed pixels often impedes the improvement of forest carbon density mapping, especially when low spatial resolution images such as MODIS are used. In this study, MODIS images and national forest inventory sample plot data were used to conduct the study of estimation for forest carbon density. Linear spectral mixture analysis with and without constraint, and nonlinear spectral mixture analysis were compared to derive the fractions of different land use and land cover (LULC) types. Then sequential Gaussian co-simulation algorithm with and without the fraction images from spectral mixture analyses were employed to estimate forest carbon density of Hunan Province. Results showed that 1) Linear spectral mixture analysis with constraint, leading to a mean RMSE of 0.002, more accurately estimated the fractions of LULC types than linear spectral and nonlinear spectral mixture analyses; 2) Integrating spectral mixture analysis model and sequential Gaussian co-simulation algorithm increased the estimation accuracy of forest carbon density to 81.5% from 74.1%, and decreased the RMSE to 5.18 from 7.26; and 3) The mean value of forest carbon density for the province was 30.06 t · hm(-2), ranging from 0.00 to 67.35 t · hm(-2). This implied that the spectral mixture analysis provided a great potential to increase the estimation accuracy of forest carbon density on regional and global level.

Forensic analysis of explosives using isotope ratio mass spectrometry (IRMS)--preliminary study on TATP and PETN.

PubMed

Benson, Sarah J; Lennard, Christopher J; Maynard, Philip; Hill, David M; Andrew, Anita S; Roux, Claude

2009-06-01

The application of isotopic techniques to investigations requiring the provision of evidence to a Court is limited. The objective of this research was to investigate the application of light stable isotopes and isotope ratio mass spectrometry (IRMS) to solve complex forensic cases by providing a level of discrimination not achievable utilising traditional forensic techniques. Due to the current threat of organic peroxide explosives, such as triacetone triperoxide (TATP), research was undertaken to determine the potential of IRMS to differentiate samples of TATP that had been manufactured utilising different starting materials and/or manufacturing processes. In addition, due to the prevalence of pentaerythritoltetranitrate (PETN) in detonators, detonating cord, and boosters, the potential of the IRMS technique to differentiate PETN samples from different sources was also investigated. Carbon isotope values were measured in fourteen TATP samples, with three definite groups appearing in the initial sample set based on the carbon data alone. Four additional TATP samples (in a second set of samples) were distinguishable utilising the carbon and hydrogen isotopic compositions individually, and also in combination with the oxygen isotope values. The 3D plot of the carbon, oxygen and hydrogen data demonstrated the clear discrimination of the four samples of TATP. The carbon and nitrogen isotope values measured from fifteen PETN samples, allowed samples from different sources to be readily discriminated. This paper demonstrates the successful application of IRMS to the analysis of explosives of forensic interest to assist in discriminating samples from different sources. This research represents a preliminary evaluation of the IRMS technique for the measurement of stable isotope values in TATP and PETN samples, and supports the dedication of resources for a full evaluation of this application in order to achieve Court reportable IRMS results.

Quantity of dates trumps quality of dates for dense Bayesian radiocarbon sediment chronologies - Gas ion source 14C dating instructed by simultaneous Bayesian accumulation rate modeling

NASA Astrophysics Data System (ADS)

Rosenheim, B. E.; Firesinger, D.; Roberts, M. L.; Burton, J. R.; Khan, N.; Moyer, R. P.

2016-12-01

Radiocarbon (14C) sediment core chronologies benefit from a high density of dates, even when precision of individual dates is sacrificed. This is demonstrated by a combined approach of rapid 14C analysis of CO2 gas generated from carbonates and organic material coupled with Bayesian statistical modeling. Analysis of 14C is facilitated by the gas ion source on the Continuous Flow Accelerator Mass Spectrometry (CFAMS) system at the Woods Hole Oceanographic Institution's National Ocean Sciences Accelerator Mass Spectrometry facility. This instrument is capable of producing a 14C determination of +/- 100 14C y precision every 4-5 minutes, with limited sample handling (dissolution of carbonates and/or combustion of organic carbon in evacuated containers). Rapid analysis allows over-preparation of samples to include replicates at each depth and/or comparison of different sample types at particular depths in a sediment or peat core. Analysis priority is given to depths that have the least chronologic precision as determined by Bayesian modeling of the chronology of calibrated ages. Use of such a statistical approach to determine the order in which samples are run ensures that the chronology constantly improves so long as material is available for the analysis of chronologic weak points. Ultimately, accuracy of the chronology is determined by the material that is actually being dated, and our combined approach allows testing of different constituents of the organic carbon pool and the carbonate minerals within a core. We will present preliminary results from a deep-sea sediment core abundant in deep-sea foraminifera as well as coastal wetland peat cores to demonstrate statistical improvements in sediment- and peat-core chronologies obtained by increasing the quantity and decreasing the quality of individual dates.

A Novel Method for Analysis of Dissolved Inorganic Carbon Concentration and δ13C by Cavity Ring-Down Spectroscopy

NASA Astrophysics Data System (ADS)

Smith, E.; Gonneea, M. E.; Boze, L. G.; Casso, M.; Pohlman, J.

2017-12-01

Dissolved inorganic carbon (DIC) is the largest pool of carbon in the oceans and is where about half of anthropogenic carbon dioxide (CO2) emissions are being sequestered. Determining the concentration and stable carbon isotopic content (δ13C) of DIC allows us to delineate carbon sources that contribute to marine DIC. A simple and reliable method for measuring DIC concentration and δ13C can be used to apportion contributions from external sources and identify effects from biogeochemical reactions that contribute or remove DIC. The U.S. Geological Survey has developed a discrete sample analysis module (DSAM) that interfaces to a Picarro G-2201i cavity ring-down spectrometer (CRDS, Picarro Inc.) to analyze CO2 and methane concentrations and δ13C from discrete gas samples. In this study, we adapted the USGS DSAM-CRDS analysis system to include an AutoMate prep device (Automate FX, Inc.) for analysis of DIC concentration and δ13C from aqueous samples. The Automate prep device was modified to deliver CO2 extracted from DIC to the DSAM, which conditions and transfers the gas to the CRDS. LabVIEW software (National Instruments) triggers the Automate Prep device, controls the DSAM and collects data from the CRDS. CO2 mass concentration data are obtained by numerical integration of the CO2 volumetric concentrations output by the CRDS and subsequent comparison to standard materials. CO2 carbon isotope values from the CRDS (iCO2) are converted to δ13C values using a slope and offset correction calibration procedure. The system design and operation was optimized using sodium bicarbonate (NaHCO3) standards and a certified reference material. Surface water and pore water samples collected from Sage Lot Pond, a salt marsh in Cape Cod MA, have been analyzed for concentration by coulometry and δ13C by isotope ratio mass spectrometry and will be used to validate the DIC-DSAM-CRDS method for field applications.

Biomarker Analysis of Samples Visually Identified as Microbial in the Eocene Green River Formation: An Analogue for Mars.

PubMed

Olcott Marshall, Alison; Cestari, Nicholas A

2015-09-01

One of the major exploration targets for current and future Mars missions are lithofacies suggestive of biotic activity. Although such lithofacies are not confirmation of biotic activity, they provide a way to identify samples for further analyses. To test the efficacy of this approach, we identified carbonate samples from the Eocene Green River Formation as "microbial" or "non-microbial" based on the macroscale morphology of their laminations. These samples were then crushed and analyzed by gas chromatography/mass spectroscopy (GC/MS) to determine their lipid biomarker composition. GC/MS analysis revealed that carbonates visually identified as "microbial" contained a higher concentration of more diverse biomarkers than those identified as "non-microbial," suggesting that this could be a viable detection strategy for selecting samples for further analysis or caching on Mars.

Advances in spectroscopic methods for quantifying soil carbon

USGS Publications Warehouse

Reeves, James B.; McCarty, Gregory W.; Calderon, Francisco; Hively, W. Dean

2012-01-01

The current gold standard for soil carbon (C) determination is elemental C analysis using dry combustion. However, this method requires expensive consumables, is limited by the number of samples that can be processed (~100/d), and is restricted to the determination of total carbon. With increased interest in soil C sequestration, faster methods of analysis are needed, and there is growing interest in methods based on diffuse reflectance spectroscopy in the visible, near-infrared or mid-infrared spectral ranges. These spectral methods can decrease analytical requirements and speed sample processing, be applied to large landscape areas using remote sensing imagery, and be used to predict multiple analytes simultaneously. However, the methods require localized calibrations to establish the relationship between spectral data and reference analytical data, and also have additional, specific problems. For example, remote sensing is capable of scanning entire watersheds for soil carbon content but is limited to the surface layer of tilled soils and may require difficult and extensive field sampling to obtain proper localized calibration reference values. The objective of this chapter is to discuss the present state of spectroscopic methods for determination of soil carbon.

Analysis of mineral matrices of planetary soil analogues from the Utah Desert

NASA Astrophysics Data System (ADS)

Kotler, J. M.; Quinn, R. C.; Foing, B. H.; Martins, Z.; Ehrenfreund, P.

2011-07-01

Phyllosilicate minerals and hydrated sulphate minerals have been positively identified on the surface of Mars. Studies conducted on Earth indicate that micro-organisms influence various geochemical and mineralogical transitions for the sulphate and phyllosilicate minerals. These minerals in turn provide key nutrients to micro-organisms and influence microbial ecology. Therefore, the presence of these minerals in astrobiology studies of Earth-Mars analogue environments could help scientists better understand the types and potential abundance of micro-organisms and/or biosignatures that may be encountered on Mars. Bulk X-ray diffraction of samples collected during the EuroGeoMars 2009 campaign from the Mancos Shale, the Morrison and the Dakota formations near the Mars Desert Research Station in Utah show variable but common sedimentary mineralogy with all samples containing quantities of hydrated sulphate minerals and/or phyllosilicates. Analysis of the clay fractions indicate that the phyllosilicates are interstratified illite-smectites with all samples showing marked changes in the diffraction pattern after ethylene glycol treatment and the characteristic appearance of a solvated peak at ˜17 Å. The smectite phases were identified as montmorillonite and nontronite using a combination of the X-ray diffraction data and Fourier-Transform Infrared Spectroscopy. The most common sulphate mineral in the samples is hydrated calcium sulphate (gypsum), although one sample contained detectable amounts of strontium sulphate (celestine). Carbonates detected in the samples are variable in composition and include pure calcium carbonate (calcite), magnesium-bearing calcium carbonate (dolomite), magnesium, iron and manganese-bearing calcium carbonate (ankerite) and iron carbonate (siderite). The results of these analyses when combined with organic extractions and biological analysis should help astrobiologists and planetary geologists better understand the potential relationships between mineralogy and microbiology for planetary missions.

A comparison of freeze-drying and oven-drying preparation methods for bulk and compound-specific carbon stable isotope analyses: examples using the benthic macroinvertebrates Stenopsyche marmorata and Epeorus latifolium.

PubMed

Akamatsu, Fumikazu; Suzuki, Yaeko; Kato, Yoshikazu; Yoshimizu, Chikage; Tayasu, Ichiro

2016-01-15

Carbon stable isotope analysis of bulk samples and fatty acids is an established method for tracing carbon flow pathways and reconstructing trophic interactions, but there is no consensus on which sample drying method should be used for sample preparation. The aim of this study was to determine if freeze-drying and oven-drying treatments used to prepare samples of the benthic macroinvertebrates Stenopsyche marmorata and Epeorus latifolium for bulk and fatty-acid-specific carbon stable isotope analysis yield different isotopic ratio values. Five individuals each from two species were split in half; one half was freeze-dried and the other half was oven-dried. The samples were ground and the δ(13)C values of the bulk samples and eight fatty acids were measured following combustion using an isotope ratio mass spectrometer coupled to an elemental analyzer or gas chromatography system. The mean difference in the bulk and fatty acid δ(13)C values between freeze-dried and oven-dried samples was small (≤0.1‰ in both cases), although relatively large variations were observed in individual fatty-acid-specific δ(13)C values (maximum of ≤0.9 ‰). There were no significant differences in either bulk sample or fatty-acid-specific δ(13)C values between freeze-dried or oven-dried samples of the same species. Freeze-drying and oven-drying are equally acceptable methods for preparing freshly caught S. marmorata and E. latifolium samples for bulk and fatty-acid-specific carbon stable isotope analyses. Copyright © 2015 John Wiley & Sons, Ltd.

The determination of the energy values and the composition analysis of M-16 rifle black powders

NASA Astrophysics Data System (ADS)

Satee, R.; Dararutana, P.; Phutdhawong, W.

2017-09-01

The determination of the energy values, specifically the heat of combustion of various M-16 black powders was the important part of the bullet efficiency investigations. The calorimetric bomb is commonly used for these determinations. Four M-16 black powders from the different sources were used as samples for this research. It was found that, after using calorimetric bomb technique, the gross heating value in Joules/g of sample S1-S4 were 10,647, 10,416, 5,281 and 3,878 respectively. The chemical compositions of carbon (C), hydrogen (H), nitrogen (N) and sulfer (S) have also been determined. The results indicated that carbon and nitrogen compositions of sample S1 shown the highest values and provided little differences with sample S2 while sample S3 and S4 shown the lowest carbon and nitrogen percentage composition. The hydrogen composition of all samples was equally valued, however, only sample 3 and 4 displayed sulfur values while no sulfur values were detected from sample 1 and 2. From these results, the heat values and chemical composition of M-16 black powders were characterized their sources and the energy values might be estimated from the amount of carbon and nitrogen in the black powders. Thus, it would be possible to use this determination analysis in the forensic investigation.

Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes.

PubMed

Blomquist, G; Nilsson, C A; Nygren, O

1983-12-01

Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes. Scand j work environ & health 9 (1983) 489-495. In view of the serious health effects of hexavalent chromium, the problems involved in its sampling and analysis in workroom air have been the subject of much concern. In this paper, the stability problems arising from the reduction of hexavalent to trivalent chromium during sampling, sample storage, and analysis are discussed. Replacement of sulfuric acid by a sodium acetate buffer (pH 4) as a leaching solution prior to analysis with the diphenylcarbazide (DPC) method is suggested and is demonstrated to be necessary in order to avoid reduction. Field samples were taken from two different industrial processes-manual metal arc welding on stainless steel without shield gas and chromium plating. A comparison was made of the DPC method, acidic dissolution with atomic absorption spectrophotometric (AAS) analysis, and the carbonate method. For chromic acid mist, the DPC method and AAS analysis were shown to give the same results. In the analysis of welding fumes, the modified DPC method gave the same results as the laborious and less sensitive carbonate method.

Quality-assurance data for routine water quality analyses by the U. S. Geological Survey laboratory in Troy, New York; July 1993 through June 1995

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2001-01-01

A laboratory for analysis of low-ionic strength water has been developed at the U.S. Geological Survey (USGS) office in Troy, N.Y., to analyze samples collected by USGS projects in the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures developed to ensure proper sample collection, processing, and analysis. The quality-assurance/quality-control data are stored in the laboratory's SAS data-management system, which provides efficient review, compilation, and plotting of quality-assurance/quality-control data. This report presents and discusses samples analyzed from July 1993 through June 1995. Quality-control results for 18 analytical procedures were evaluated for bias and precision. Control charts show that data from seven of the analytical procedures were biased throughout the analysis period for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, dissolved inorganic carbon, dissolved organic carbon (soil expulsions), chloride, magnesium, nitrate (colorimetric method), and pH. Three of the analytical procedures were occasionally biased but were within control limits; they were: calcium (high for high-concentration samples for May 1995), dissolved organic carbon (high for highconcentration samples from January through September 1994), and fluoride (high in samples for April and June 1994). No quality-control sample has been developed for the organic monomeric aluminum procedure. Results from the filter-blank and analytical-blank analyses indicate that all analytical procedures in which blanks were run were within control limits, although values for a few blanks were outside the control limits. Blanks were not analyzed for acid-neutralizing capacity, dissolved inorganic carbon, fluoride, nitrate (colorimetric method), or pH. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in 14 of the 18 procedures. Data-quality objectives were met by more than 90 percent of the samples analyzed in all procedures except total monomeric aluminum (85 percent of samples met objectives), total aluminum (70 percent of samples met objectives), and dissolved organic carbon (85 percent of samples met objectives). Triplicate samples were not analyzed for ammonium, fluoride, dissolved inorganic carbon, or nitrate (colorimetric method). Results of the USGS interlaboratory Standard Reference Sample Program indicated high data quality with a median result of 3.6 of a possible 4.0. Environment Canada's LRTAP interlaboratory study results indicated that more than 85 percent of the samples met data-quality objectives in 6 of the 12 analyses; exceptions were calcium, dissolved organic carbon, chloride, pH, potassium, and sodium. Data-quality objectives were not met for calcium samples in one LRTAP study, but 94 percent of samples analyzed were within control limits for the remaining studies. Data-quality objectives were not met by 35 percent of samples analyzed for dissolved organic carbon, but 94 percent of sample values were within 20 percent of the most probable value. Data-quality objectives were not met for 30 percent of samples analyzed for chloride, but 90 percent of sample values were within 20 percent of the most probable value. Measurements of samples with a pH above 6.0 were biased high in 54 percent of the samples, although 85 percent of the samples met data-quality objectives for pH measurements below 6.0. Data-quality objectives for potassium and sodium were not met in one study (only 33 percent of the samples analyzed met the objectives), although 85 percent of the sample values were within control limits for the other studies. Measured sodium values were above the upper control limit in all studies. Results from blind reference-sample analyses indicated that data

Determining the bio-based content of bio-plastics used in Thailand by radiocarbon analysis

NASA Astrophysics Data System (ADS)

Ploykrathok, T.; Chanyotha, S.

2017-06-01

Presently, there is an increased interest in the development of bio-plastic products from agricultural materials which are biodegradable in order to reduce the problem of waste disposal. Since the amount of modern carbon in bio-plastics can indicate how much the amount of agricultural materials are contained in the bio-plastic products, this research aims to determine the modern carbon in bio-plastic using the carbon dioxide absorption method. The radioactivity of carbon-14 contained in the sample is measured by liquid scintillation counter (Tri-carb 3110 TR, PerkinElmer). The percentages of bio-based content in the samples were determined by comparing the observed modern carbon content with the values contained in agricultural raw materials. The experimental results show that only poly(lactic acid) samples have the modern carbon content of 97.4%, which is close to the agricultural materials while other bio-plastics types are found to have less than 50% of the modern carbon content. In other words, most of these bio-plastic samples were mixed with other materials which are not agriculturally originated.

A pressure-affected headspace-gas chromatography method for determining calcium carbonate content in paper sample.

PubMed

Dai, Yi; Yu, Zhen-Hua; Zhan, Jian-Bo; Chai, Xin-Sheng; Zhang, Shu-Xin; Xie, Wei-Qi; He, Liang

2017-07-21

The present work reports on the development of a pressure-affected based headspace (HS) analytical technique for the determination of calcium carbonate content in paper samples. By the acidification, the carbonate in the sample was converted to CO 2 and released into the headspace of a closed vial and then measured by gas chromatography (GC). When the amount of carbonate in the sample is significant, the pressure created by the CO 2 affects the accuracy of the method. However, the pressure also causes a change in the O 2 signal in the HS-GC measurement, which is a change that can be used as an indirect measure of the carbonate in the sample. The results show that the present method has a good precision (the relative standard deviation<2.32%), and good accuracy (the relative differences compared to a reference method was<5.76%). Coupled with the fact that the method is simple, rapid, and accurate, it is suitable for a variety of applications that call for the analysis of high carbonate content in paper samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Electron spin resonance as a high sensitivity technique for environmental magnetism: determination of contamination in carbonate sediments

NASA Astrophysics Data System (ADS)

Crook, Nigel P.; Hoon, Stephen R.; Taylor, Kevin G.; Perry, Chris T.

2002-05-01

This study investigates the application of high sensitivity electron spin resonance (ESR) to environmental magnetism in conjunction with the more conventional techniques of magnetic susceptibility, vibrating sample magnetometry (VSM) and chemical compositional analysis. Using these techniques we have studied carbonate sediment samples from Discovery Bay, Jamaica, which has been impacted to varying degrees by a bauxite loading facility. The carbonate sediment samples contain magnetic minerals ranging from moderate to low concentrations. The ESR spectra for all sites essentially contain three components. First, a six-line spectra centred around g = 2 resulting from Mn2+ ions within a carbonate matrix; second a g = 4.3 signal from isolated Fe3+ ions incorporated as impurities within minerals such as gibbsite, kaolinite or quartz; third a ferrimagnetic resonance with a maxima at 230 mT resulting from the ferrimagnetic minerals present within the bauxite contamination. Depending upon the location of the sites within the embayment these signals vary in their relative amplitude in a systematic manner related to the degree of bauxite input. Analysis of the ESR spectral components reveals linear relationships between the amplitude of the Mn2+ and ferrimagnetic signals and total Mn and Fe concentrations. To assist in determining the origin of the ESR signals coral and bauxite reference samples were employed. Coral representative of the matrix of the sediment was taken remote from the bauxite loading facility whilst pure bauxite was collected from nearby mining facilities. We find ESR to be a very sensitive technique particularly appropriate to magnetic analysis of ferri- and para-magnetic components within environmental samples otherwise dominated by diamagnetic (carbonate) minerals. When employing typical sample masses of 200 mg the practical detection limit of ESR to ferri- and para-magnetic minerals within a diamagnetic carbonate matrix is of the order of 1 ppm and 1 ppb respectively, approximately 102 and 105 times the sensitivity achievable employing the VSM in our laboratory.

Effects of acidification, lipid removal and mathematical normalization on carbon and nitrogen stable isotope compositions in beaked whale (Ziphiidae) bone.

PubMed

Tatsch, Ana Carolina C; Secchi, Eduardo R; Botta, Silvina

2016-02-15

The analysis of stable isotopes in tissues such as teeth and bones has been used to study long-term trophic ecology and habitat use in marine mammals. However, carbon isotope ratios (δ(13) C values) can be altered by the presence of (12) C-rich lipids and carbonates. Lipid extraction and acidification are common treatments used to remove these compounds. The impact of lipids and carbonates on carbon and nitrogen isotope ratios (δ(15) N values), however, varies among tissues and/or species, requiring taxon-specific protocols to be developed. The effects of lipid extraction and acidification and their interaction on carbon and nitrogen isotope values were studied for beaked whale (Ziphiidae) bone samples. δ(13) C and δ(15) N values were determined in quadruplicate samples: control, lipid-extracted, acidified and lipid-extracted followed by acidification. Samples were analyzed by means of elemental analysis isotope ratio mass spectrometry. Furthermore, the efficiency of five mathematical models developed for estimating lipid-normalized δ(13) C values from untreated δ(13) C values was tested. Significant increases in δ(13) C values were observed after lipid extraction. No significant changes in δ(13) C values were found in acidified samples. An interaction between both treatments was demonstrated for δ(13) C but not for δ(15) N values. No change was observed in δ(15) N values for lipid-extracted and/or acidified samples. Although all tested models presented good predictive power to estimate lipid-free δ(13) C values, linear models performed best. Given the observed changes in δ(13) C values after lipid extraction, we recommend a priori lipid extraction or a posteriori lipid normalization, through simple linear models, for beaked whale bones. Furthermore, acidification seems to be an unnecessary step before stable isotope analysis, at least for bone samples of ziphiids. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Year-round Source Contributions of Fossil Fuel and Biomass Combustion to Elemental Carbon on the North Slope Alaska Utilizing Radiocarbon Analysis

NASA Astrophysics Data System (ADS)

Barrett, T. E.; Gustafsson, O.; Winiger, P.; Moffett, C.; Back, J.; Sheesley, R. J.

2015-12-01

It is well documented that the Arctic has undergone rapid warming at an alarming rate over the past century. Black carbon (BC) affects the radiative balance of the Arctic directly and indirectly through the absorption of incoming solar radiation and by providing a source of cloud and ice condensation nuclei. Among atmospheric aerosols, BC is the most efficient absorber of light in the visible spectrum. The solar absorbing efficiency of BC is amplified when it is internally mixed with sulfates. Furthermore, BC plumes that are fossil fuel dominated have been shown to be approximately 100% more efficient warming agents than biomass burning dominated plumes. The renewal of offshore oil and gas exploration in the Arctic, specifically in the Chukchi Sea, will introduce new BC sources to the region. This study focuses on the quantification of fossil fuel and biomass combustion sources to atmospheric elemental carbon (EC) during a year-long sampling campaign in the North Slope Alaska. Samples were collected at the Department of Energy Atmospheric Radiation Measurement (ARM) climate research facility in Barrow, AK, USA. Particulate matter (PM10) samples collected from July 2012 to June 2013 were analyzed for EC and sulfate concentrations combined with radiocarbon (14C) analysis of the EC fraction. Radiocarbon analysis distinguishes fossil fuel and biomass burning contributions based on large differences in end members between fossil and contemporary carbon. To perform isotope analysis on EC, it must be separated from the organic carbon fraction of the sample. Separation was achieved by trapping evolved CO2 produced during EC combustion in a cryo-trap utilizing liquid nitrogen. Radiocarbon results show an average fossil contribution of 85% to atmospheric EC, with individual samples ranging from 47% to 95%. Source apportionment results will be combined with back trajectory (BT) analysis to assess geographic source region impacts on the EC burden in the western Arctic.

Change detection for soil carbon in the forest inventory and analysis

Treesearch

An-Min Wu; Edward A. Nater; Charles H. Perry; Brent J. Dalzell; Barry T. Wilson

2015-01-01

Estimates of carbon stocks and stock changes in the U.S. Department of Agriculture Forest Service’s Forest Inventory and Analysis (FIA) Program are reported as the official United States submission to the UN Framework Convention on Climate Change. Soil, as a critical component of the forest carbon stocks, has been sampled in about 10-year intervals in FIA with the re-...

Investigation of a systematic offset in the measurement of organic carbon with a semicontinuous analyzer.

PubMed

Offenberg, John H; Lewandowski, Michael; Edney, Edward O; Kleindienst, Tadeusz E; Jaoui, Mohammed

2007-05-01

Organic carbon (OC) was measured semicontinuously in laboratory experiments of steady-state secondary organic aerosol formed by hydrocarbon + nitrogen oxide irradiations. Examination of the mass of carbon measured on the filter for various sample volumes reveals a systematic offset that is not observed when performing an instrumental blank. These findings suggest that simple subtraction of instrumental blanks determined as the standard analysis without sample collection (i.e., by cycling the pump and valves yet filtering zero liters of air followed by routine chemical analysis) from measured concentrations may be inadequate. This may be especially true for samples collected through the filtration of small air volumes wherein the influence of the systematic offset is greatest. All of the experiments show that filtering a larger volume of air minimizes the influence of contributions from the systematic offset. Application of these results to measurements of ambient concentrations of carbonaceous aerosol suggests a need for collection of sufficient carbon mass to minimize the relative influence of the offset signal.

State-Space Estimation of Soil Organic Carbon Stock

NASA Astrophysics Data System (ADS)

Ogunwole, Joshua O.; Timm, Luis C.; Obidike-Ugwu, Evelyn O.; Gabriels, Donald M.

2014-04-01

Understanding soil spatial variability and identifying soil parameters most determinant to soil organic carbon stock is pivotal to precision in ecological modelling, prediction, estimation and management of soil within a landscape. This study investigates and describes field soil variability and its structural pattern for agricultural management decisions. The main aim was to relate variation in soil organic carbon stock to soil properties and to estimate soil organic carbon stock from the soil properties. A transect sampling of 100 points at 3 m intervals was carried out. Soils were sampled and analyzed for soil organic carbon and other selected soil properties along with determination of dry aggregate and water-stable aggregate fractions. Principal component analysis, geostatistics, and state-space analysis were conducted on the analyzed soil properties. The first three principal components explained 53.2% of the total variation; Principal Component 1 was dominated by soil exchange complex and dry sieved macroaggregates clusters. Exponential semivariogram model described the structure of soil organic carbon stock with a strong dependence indicating that soil organic carbon values were correlated up to 10.8m.Neighbouring values of soil organic carbon stock, all waterstable aggregate fractions, and dithionite and pyrophosphate iron gave reliable estimate of soil organic carbon stock by state-space.

Lipid Correction for Carbon Stable Isotope Analysis of Deep-sea Fishes

EPA Science Inventory

Lipid extraction is used prior to stable isotope analysis of fish tissues to remove variability in the carbon stable isotope ratio (d13C) caused by varying lipid content among samples. Our objective was to evaluate an application of a mass balance correction for the effect of lip...

40 CFR 98.337 - Records that must be retained.

Code of Federal Regulations, 2010 CFR

2010-07-01

... analysis records for carbon content of zinc bearing materials, flux materials (e.g., limestone, dolomite...). (7) Sampling and analysis records for carbon content of electrode materials. (8) You must keep... records specified in paragraphs (b)(1) through (b)(7) of this section. (1) Records of all analyses and...

Method for isotopic analysis of chlorinated organic compounds

DOEpatents

Holt, Ben D.; Sturchio, Neil C.

1999-01-01

The present invention provides a method for preparing a VOC sample for carbon and chlorine isotope ratio analysis by mass spectrometer. A VOC sample is placed in a combustion tube and reacted with CuO to form CO.sub.2 and CuCl. The CO.sub.2 is then extracted and analyzed for the carbon isotope ratio. The CuCl is separated from the excess CuO and reacted with CH.sub.3 I to form CH.sub.3 Cl, extracted and analyzed for chlorine isotope ratio.

Solubility of α-Tocopheryl Succinate in Supercritical Carbon Dioxide Using Offline HPLC-MS/MS Analysis

PubMed Central

Hybertson, Brooks M.

2010-01-01

The solubility of the vitamin E-related compound α-tocopheryl succinate in supercritical carbon dioxide was measured at pressures ranging from (15.0 to 30.0) MPa and temperatures of (40 and 50) °C using a simple microsampling type apparatus with a 100.5 μL sample loop to remove aliquots and collect them in ethanol for off line analysis. α-Tocopheryl succinate concentrations in the collected samples were measured using HPLC-MS/MS analysis. The solubility of α-tocopheryl succinate in supercritical carbon dioxide ranged from mole fractions of 0.28 × 10−5 at 15.0 MPa and 50 °C to 2.56 × 10−5 at 30.0 MPa and 50 °C. PMID:20953319

Using Isotope Ratio Infrared Spectrometer to determine δ13C and δ18O of carbonate samples

NASA Astrophysics Data System (ADS)

Smajgl, Danijela; Stöbener, Nils; Mandic, Magda

2017-04-01

The isotopic composition of calcifying organisms is a key tool for reconstruction past seawater temperature and water chemistry. Therefore stable carbon and oxygen isotopes (δ13C and δ18O) in carbonates have been widely used for reconstruction of paleoenvironments. Precise and accurate determination of isotopic composition of carbon (13C) and oxygen (18O) from carbonate sample with proper referencing and data evaluation algorithm presents a challenge for scientists. Mass spectrometry was the only widely used technique for this kind of analysis, but recent advances make laser based spectroscopy a viable alternative. The Thermo Scientific Delta Ray Isotope Ratio Infrared Spectrometer (IRIS) analyzer with the Universal Reference Interface (URI) Connect is one of those alternatives and with TELEDYNE Cetac ASX-7100 autosampler extends the traditional offerings with a system of high precision and throughput of samples. To establish precision and accuracy of measurements and also to develop optimal sample preparation method for measurements with Delta Ray IRIS and URI Connect, IAEA reference materials were used. Preparation is similar to a Gas Bench II method. Carbonate material is added into the vials, flushed with CO2 free synthetic air and acidified with few droplets of 104% H3PO4. Sample amount used for analysis can be as low as 200 μg. Samples are measured after acidification and equilibration time of one hour at 70°C. The CO2 gas generated by reaction is flushed into the variable volume inside the URI Connect through the Nafion based built-in water trap. For this step, carrier gas (CO2 free air) is used to flush the gas from the vial into the variable volume with a maximum volume of 100 ml. A small amount of the sample is then used for automatic concentration determination present in the variable volume. The Thermo Scientific Qtegra Software automatically adjusts any additional dilution of the sample to achieve the desired concentration (usually 400 ppm) in the analyzer. As part of the workflow, reference gas measurements are regularly measured at the same concentration as the sample to allow for automatic drift and linearity correction. With described sample preparation and measurement method, samples are measured with standard deviation less than 0.1‰ δ13C and δ18O, respectively and accuracy of <0.01‰. The system can measure up to 100 samples per day. Equivalent of about 80 µg of pure CO2 gas is needed to complete an analysis. Due to it's small weight and robustness, sample analysis can be performed in the field. Applying new technology of Isotope Ratio Infrared Spectrometers in environmental and paleoenvironmental research can extend the knowledge of complex seawater history and CO2 cycle.

Carbon based sample supports and matrices for laser desorption/ ionization mass spectrometry.

PubMed

Rainer, Matthias; Najam-ul-Haq, Muhammad; Huck, Christian W; Vallant, Rainer M; Heigl, Nico; Hahn, Hans; Bakry, Rania; Bonn, Günther K

2007-01-01

Laser desorption/ionization mass spectrometry (LDI-MS) is a widespread and powerful technique for mass analysis allowing the soft ionization of molecules such as peptides, proteins and carbohydrates. In many applications, an energy absorbing matrix has to be added to the analytes in order to protect them from being fragmented by direct laser beam. LDI-MS in conjunction with matrix is commonly referred as matrix-assisted LDI (MALDI). One of the striking disadvantages of this method is the desorption of matrix molecules, which causes interferences originating from matrix background ions in lower mass range (< 1000 Da). This has been led to the development of a variety of different carbon based LDI sample supports, which are capable of absorbing laser light and simultaneously transfering energy to the analytes for desorption. Furthermore carbon containing sample supports are used as carrier materials for the specific binding and preconcentration of molecules out of complex samples. Their subsequent analysis with MALDI mass spectrometry allows performing studies in metabolomics and proteomics. Finally a thin layer of carbon significantly improves sensitivity concerning detection limit. Analytes in low femtomole and attomole range can be detected in this regard. In the present article, these aspects are reviewed from patents where nano-based carbon materials are comprehensively utilized.

ORGANIC AEROSOL SAMPLING AND ANALYSIS METHODS RESEARCH

EPA Science Inventory

Carbonaceous material is a major component of ambient PM at all locations in the U.S. and it is composed of two major classes: organic carbon (OC, composed of hundreds of individual compounds) and elemental carbon (EC, also referred to as soot, black carbon, or light adsorbing ca...

Importance of Temperature Calibration for Sunset Laboratory Carbon Analyzer: NIOSH and IMPROVE Temperature Protocols

EPA Science Inventory

The Sunset Laboratory Dual-Optical Carbonaceous Analyzer that simultaneously measures transmission and reflectance signals is widely used in thermal-optical analysis of particulate matter samples. Most often it is used to measure total carbon (TC), organic carbon (OC), and eleme...

Trends and anomalies in gas evolution from coal samples

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

Vorres, K.S.

1993-09-01

As part of the stability studies on these sealed samples a number of the samples were given to the Analytical Chemistry Laboratory at ANL for periodic gas analysis. 1. Higher rank coals evolve methane, and lower rank coals evolve carbon dioxide with some evolution of both gases for the intermediate ranks. 2. The evolution proceeds over times of years for pulverized coals in sealed ampules. 3. Gas concentrations are higher above -20 mesh samples than above -100 mesh material. 4. Carbon monoxide is not evolved.

Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

NASA Astrophysics Data System (ADS)

Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

2009-12-01

Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

Preparation of activated carbon monolith by application of phenolic resins as carbon precursors

NASA Astrophysics Data System (ADS)

Sajad, Mehran; Kazemzad, Mahmood; Hosseinnia, Azarmidokht

2014-04-01

In the current work, activated carbon monoliths have been prepared by application of different phenolic hydrocarbons namely catechol and resorcinol as carbon precursors. For synthesis of carbon monolith, the precursors have been mixed with Genapol PF-10 as template and then polymerized in the presence of lysine as catalyst. Then the polymerized monolith carbonized in inert atmosphere at 700°C and activated by water steam at 550°C. It was found that resorcinol polymerization is easier than catechol and occurred at 90°C while for polymerization of catechol elevated temperature of 120°C at hydrothermal condition is necessary. The prepared activated carbon samples have been characterized by various analysis methods including scanning electron microscopy (SEM), surface area measurement, and transmission electron microscopy (TEM). The adsorptions of three different aromatic hydrocarbons by the prepared activated carbon samples have also been investigated by high performance liquid chromatography (HPLC) and UV-Vis spectroscopy. It was found that carbon monolith prepared by catechol as carbon precursor has higher adsorpability and strength in comparison with the other sample. The higher performance of carbon monolith prepared by catechol can be associated with its higher active sites in comparison with resorcinol.

Contamination risk of stable isotope samples during milling.

PubMed

Isaac-Renton, M; Schneider, L; Treydte, K

2016-07-15

Isotope analysis of wood is an important tool in dendrochronology and ecophysiology. Prior to mass spectrometry analysis, wood must be homogenized, and a convenient method involves a ball mill capable of milling samples directly in sample tubes. However, sample-tube plastic can contaminate wood during milling, which could lead to biological misinterpretations. We tested possible contamination of whole wood and cellulose samples during ball-mill homogenization for carbon and oxygen isotope measurements. We used a multi-factorial design with two/three steel milling balls, two sample amounts (10 mg, 40 mg), and two milling times (5 min, 10 min). We further analyzed abrasion by milling empty tubes, and measured the isotope ratios of pure contaminants. A strong risk exists for carbon isotope bias through plastic contamination: the δ(13) C value of polypropylene deviated from the control by -6.77‰. Small fibers from PTFE filter bags used during cellulose extraction also present a risk as the δ(13) C value of this plastic deviated by -5.02‰. Low sample amounts (10 mg) showed highest contamination due to increased abrasion during milling (-1.34‰), which is further concentrated by cellulose extraction (-3.38‰). Oxygen isotope measurements were unaffected. A ball mill can be used to homogenize samples within test tubes prior to oxygen isotope analysis, but not prior to carbon or radiocarbon isotope analysis. There is still a need for a fast, simple and contamination-free sample preparation procedure. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

The active and passive sampling of benzene, toluene, ethyl benzene and xylenes compounds using the inside needle capillary adsorption trap device.

PubMed

Shojania, S; Oleschuk, R D; McComb, M E; Gesser, H D; Chow, A

1999-08-23

A new and simple method of solventless extraction of volatile organic compounds (VOCs) from air is presented. The sampling device has an adsorbing carbon coating on the interior surface of a hollow needle, and is called the inside needle capillary adsorption trap (INCAT). This paper describes a study of the reproducibility in the preparation and sampling of the INCAT device. In addition, this paper examines the effects of sample volume in active sampling and exposure time in passive sampling on the analyte adsorption. Analysis was achieved by sampling the air from an environmental chamber doped with benzene, toluene, ethyl benzene and xylenes (BTEX) compounds. Initial rates of adsorption were found to vary among the different compounds, but ranged from 0.0099 to 0.016 nmol h(-1) for passive sampling and from 2.2 to 10 nmol h(-1) for active sampling. Analysis was done by thermal desorption of the adsorbed compounds directly into a gas chromatograph injection port. Quantification of the analysis was done by comparison to actively sampled activated carbon solid phase extraction (SPE) measurements.

Study of the structure of 3-D composites based on carbon nanotubes in bovine serum albumin matrix by X-ray microtomography

NASA Astrophysics Data System (ADS)

Ignatov, D.; Zhurbina, N.; Gerasimenko, A.

2017-01-01

3-D composites are widely used in tissue engineering. A comprehensive analysis by X-ray microtomography was conducted to study the structure of the 3-D composites. Comprehensive analysis of the structure of the 3-D composites consisted of scanning, image reconstruction of shadow projections, two-dimensional and three-dimensional visualization of the reconstructed images and quantitative analysis of the samples. Experimental samples of composites were formed by laser vaporization of the aqueous dispersion BSA and single-walled (SWCNTs) and multi-layer (MWCNTs) carbon nanotubes. The samples have a homogeneous structure over the entire volume, the percentage of porosity of 3-D composites based on SWCNTs and MWCNTs - 16.44%, 28.31%, respectively. An average pore diameter of 3-D composites based on SWCNTs and MWCNTs - 45 μm 93 μm. 3-D composites based on carbon nanotubes in bovine serum albumin matrix can be used in tissue engineering of bone and cartilage, providing cell proliferation and blood vessel sprouting.

Optimizing sample pretreatment for compound-specific stable carbon isotopic analysis of amino sugars in marine sediment

NASA Astrophysics Data System (ADS)

Zhu, R.; Lin, Y.-S.; Lipp, J. S.; Meador, T. B.; Hinrichs, K.-U.

2014-09-01

Amino sugars are quantitatively significant constituents of soil and marine sediment, but their sources and turnover in environmental samples remain poorly understood. The stable carbon isotopic composition of amino sugars can provide information on the lifestyles of their source organisms and can be monitored during incubations with labeled substrates to estimate the turnover rates of microbial populations. However, until now, such investigation has been carried out only with soil samples, partly because of the much lower abundance of amino sugars in marine environments. We therefore optimized a procedure for compound-specific isotopic analysis of amino sugars in marine sediment, employing gas chromatography-isotope ratio mass spectrometry. The whole procedure consisted of hydrolysis, neutralization, enrichment, and derivatization of amino sugars. Except for the derivatization step, the protocol introduced negligible isotopic fractionation, and the minimum requirement of amino sugar for isotopic analysis was 20 ng, i.e., equivalent to ~8 ng of amino sugar carbon. Compound-specific stable carbon isotopic analysis of amino sugars obtained from marine sediment extracts indicated that glucosamine and galactosamine were mainly derived from organic detritus, whereas muramic acid showed isotopic imprints from indigenous bacterial activities. The δ13C analysis of amino sugars provides a valuable addition to the biomarker-based characterization of microbial metabolism in the deep marine biosphere, which so far has been lipid oriented and biased towards the detection of archaeal signals.

Application of a spectrum standardization method for carbon analysis in coal using laser-induced breakdown spectroscopy (LIBS).

PubMed

Li, Xiongwei; Wang, Zhe; Fu, Yangting; Li, Zheng; Liu, Jianmin; Ni, Weidou

2014-01-01

Measurement of coal carbon content using laser-induced breakdown spectroscopy (LIBS) is limited by its low precision and accuracy. A modified spectrum standardization method was proposed to achieve both reproducible and accurate results for the quantitative analysis of carbon content in coal using LIBS. The proposed method used the molecular emissions of diatomic carbon (C2) and cyanide (CN) to compensate for the diminution of atomic carbon emissions in high volatile content coal samples caused by matrix effect. The compensated carbon line intensities were further converted into an assumed standard state with standard plasma temperature, electron number density, and total number density of carbon, under which the carbon line intensity is proportional to its concentration in the coal samples. To obtain better compensation for fluctuations of total carbon number density, the segmental spectral area was used and an iterative algorithm was applied that is different from our previous spectrum standardization calculations. The modified spectrum standardization model was applied to the measurement of carbon content in 24 bituminous coal samples. The results demonstrate that the proposed method has superior performance over the generally applied normalization methods. The average relative standard deviation was 3.21%, the coefficient of determination was 0.90, the root mean square error of prediction was 2.24%, and the average maximum relative error for the modified model was 12.18%, showing an overall improvement over the corresponding values for the normalization with segmental spectrum area, 6.00%, 0.75, 3.77%, and 15.40%, respectively.

Activated carbon derived from chitosan as air cathode catalyst for high performance in microbial fuel cells

NASA Astrophysics Data System (ADS)

Liu, Yi; Zhao, Yong; Li, Kexun; Wang, Zhong; Tian, Pei; Liu, Di; Yang, Tingting; Wang, Junjie

2018-02-01

Chitosan with rich of nitrogen is used as carbon precursor to synthesis activated carbon through directly heating method in this study. The obtained carbon is activated by different amount of KOH at different temperatures, and then prepared as air cathodes for microbial fuel cells. Carbon sample treated with double amount of KOH at 850 °C exhibits maximum power density (1435 ± 46 mW m-2), 1.01 times improved, which ascribes to the highest total surface area, moderate micropore and mesoporous structure and the introduction of nitrogen. The electrochemical impedance spectroscopy and powder resistivity state that carbon treated with double amount of KOH at 850 °C possesses lower resistance. The other electrochemical measurements demonstrate that the best kinetic activity make the above treated sample to show the best oxygen reduction reaction activity. Besides, the degree of graphitization of samples increases with the activated temperature increasing, which is tested by Raman. According to elemental analysis and X-ray photoelectron spectroscopy, all chitosan samples are nitrogen-doped carbon, and high content nitrogen (pyridinic-N) improves the electrochemical activity of carbon treated with KOH at 850 °C. Thus, carbon materials derived from chitosan would be an optimized catalyst for oxygen reduction reaction in microbial fuel cell.

The influence of temperature calibration on the OC–EC results from a dual-optics thermal carbon analyzer

EPA Science Inventory

The Sunset Laboratory Dual-Optical Carbonaceous Analyzer that simultaneously measures transmission and reflectance signals is widely used in thermal-optical analysis of particulate matter samples. Most often this instrument is used to measure total carbon (TC), organic carbon (O...

Iron-Rich Carbonates as the Potential Source of Evolved CO2 Detected by the Sample Analysis at Mars (SAM) Instrument in Gale Crater

NASA Technical Reports Server (NTRS)

Sutter, B.; Heil, E.; Rampe, E. B.; Morris, R. V.; Ming, D. W.; Archer, P. D.; Eigenbrode, J. L.; Franz, H. B.; Glavin, D. P.; McAdam, A. C.;

Analysis of YBCO high temperature superconductor doped with silver nanoparticles and carbon nanotubes using Williamson-Hall and size-strain plot

NASA Astrophysics Data System (ADS)

Dadras, Sedigheh; Davoudiniya, Masoumeh

2018-05-01

This paper sets out to investigate and compare the effects of Ag nanoparticles and carbon nanotubes (CNTs) doping on the mechanical properties of Y1Ba2Cu3O7-δ (YBCO) high temperature superconductor. For this purpose, the pure and doped YBCO samples were synthesized by sol-gel method. The microstructural analysis of the samples is performed using X-ray diffraction (XRD). The crystalline size, lattice strain and stress of the pure and doped YBCO samples were estimated by modified forms of Williamson-Hall analysis (W-H), namely, uniform deformation model (UDM), uniform deformation stress model (UDSM) and the size-strain plot method (SSP). These results show that the crystalline size, lattice strain and stress of the YBCO samples declined by Ag nanoparticles and CNTs doping.

Novel Tool for Simultaneous Carbon and Nitrogen Stable Isotope Analyses in Aqueous Samples

NASA Astrophysics Data System (ADS)

Federherr, E.; Schmidt, T. C.; Cerli, C.; Kalbitz, K.; Kupka, H. J.; Lange, L.; Dunsbach, R.; Panetta, R. J.; Kasson, A.

2014-12-01

Investigation of transformation and transport processes of carbon and nitrogen in ecosystems plays an important role to understand and predict their dynamics and role in biogeochemistry. Consequently, suitable and accurate methods for concentration as well as stable isotopic composition analysis of carbon and nitrogen in waters and aqueous solutions play a significant role. Traditionally dissolved carbon and nitrogen stable isotope analysis (SIA) is performed using either offline sample preparation followed by elemental analysis isotope ratio mass spectrometry (EA/IRMS) or modified wet chemical oxidation based device coupled to IRMS. Recently we presented a high temperature combustion system (HTC), which significantly improves upon these methods for dissolved organic carbon (DOC) SIA. The analysis of δ15N of dissolved nitrogen still has large limitations. Its low concentration makes EA/IRMS laborious, time and sample consuming. Systems based on wet chemical oxidation-IRMS bare the risk of sensitivity loss as well as of fractionation due to incomplete mineralization. In addition, the high solubility of molecular nitrogen in water remains a technical challenge, as it requires additional separation steps to distinguish between physically dissolved nitrogen and bound nitrogen. Further development of our HTC system lead to the implementation of the δ15N determination which now coupled, into a novel total organic carbon (TOC) analyzing system, especially designed for SIA of both, carbon and nitrogen. Integrated, innovative purge and trap technique (peak focusing) for nitrogen with aluminosilicate adsorber and peltier element based cooling system, in combination with high injection volume (up to 3 mL) as well as favorable carrier gas flow significantly improves sensitivity. Down to 1ppm and less total nitrogen can be measured with precision of ≤ 0.5‰. To lower the background caused by physically dissolved nitrogen new, membrane-vacuum based, degasser was designed for online separation of physically dissolved nitrogen. This novel HTC system, "iso TOC cube", provides an innovative tool with large potential in investigation of biogeochemical carbon and nitrogen cycles.

AMS 14C analysis of teeth from archaeological sites showing anomalous esr dating results

NASA Astrophysics Data System (ADS)

Grün, Rainer; Abeyratne, Mohan; Head, John; Tuniz, Claudio; Hedges, Robert E. M.

We have carried out AMS radiocarbon analysis on two groups of samples: the first one gave reasonable ESR age estimates and the second one yielded serious age underestinations. All samples were supposedly older than 35 ka, the oldest being around 160 ka. Two pretreatment techniques were used for radiocarbon dating: acid evolution and thermal release. Heating to 600, 750 and 900°C combined with total de-gassing at these temperatures was chosen to obtain age estimates on the organic fraction, secondary carbonates and original carbonate present in the hydroxyapatite mineral phase, respectively. All radiocarbon results present serious age underestimations. The secondary carbonate fraction gives almost modern results indicating an extremely rapid exchange of this component. Owing to this very rapid carbonate exchange it is not likely that the ESR signals used for dating are associated with the secondary carbonates. One tooth from Tabun with independent age estimates of >150 ka was further investigated by the Oxford AMS laboratory, yielding an age estimate of 1930±100 BP on the residual collagen from dentine and 18,000±160 BP on the carbonate component of the enamel bioapatite. We did not, however, find an explanation of why some samples give serious ESR underestimatioils whilst many others provide reasonable results.

Using Isotope Ratio Infrared Spectrometer to determine δ13C of CaCO3 carbonate and DIC samples and δ18O of water

NASA Astrophysics Data System (ADS)

Mandic, M.; Stöbener, N.; Mandic, L.; Smajgl, D.; Jost, H. J. H.

2016-12-01

Precise and accurate determination of isotopic composition of carbon (13C) and oxygen (18O) from carbonate or DIC sample with proper referencing and data evaluation algorithm presents a challenge for scientists. Mass spectrometry was the only widely used technique for this kind of analysis, but recent advances make laser based isotope ratio infrared spectroscopy (IRIS) a viable alternative. To analyze discrete samples, the Universal Reference Interface (URI) Connect was developed. CO2 free syntethic air is used to flush out the contents of a sample container into a variable volume. If necessary, the sample is further diluted before entering the analysis chamber. Reference gas measurements are automatically performed at the same concentration as sample measurements to compensate for instrument drifts and non linearity. The URI Connect can handle about 100 samples per day from an autosampler, or samples can be injected one at a time through a septum on the front of the instrument. Gas samples collected in flasks, bags, syringes, or vials can be analyzed. The system only needs the equivalent of about 80µg - or 40µL - of pure CO2 gas to complete an analysis. Due to it's small weight and robustness, sample analysis can be performed in the field, e.g. aboard a research vessel. To demonstrate the performance, a test experiment with 1% CO2 in 12 ml vials was performed. We achieved an internal precision of better than 0.07‰ and 0.1‰ for δ13C and δ18O, respectively. Analyses with sample amounts as low as 200 μg of carbonate can also be performed reliably with IRIS. We present measurements of three international reference materials, and one of them treated as an unknown. Five samples each of approximately 1mg each were acidified using a few droplets of 43% H3PO4 and left for equilibration overnight at 25°C. The standard deviation was less than 0.1‰ δ13C and the accuracy <0.01‰ As another example of head space analysis in 12 ml vials, we determined δ18O of aliquots of 500 µl of water using equilibration with 1% CO2 in the volume above the water. The agreement with traditional IRMS methods was <0.06‰ was found.

Climatically driven loss of calcium in steppe soil as a sink for atmospheric carbon

Treesearch

A.G. Lapenis; G.B. Lawrence; S.W. Bailey; B.F. Aparin; A.I. Shiklomanov; N.A. Speranskaya; M.S. Torn; M. Calef

2008-01-01

During the last several thousand years the semi-arid, cold climate of the Russian steppe formed highly fertile soils rich in organic carbon and calcium (classified as Chernozems in the Russian system). Analysis of archived soil samples collected in Kemannaya Steppe Preserve in 1920, 1947, 1970, and fresh samples collected in 1998 indicated that the native steppe...

Application of thermal analysis techniques in activated carbon production

USGS Publications Warehouse

Donnals, G.L.; DeBarr, J.A.; Rostam-Abadi, M.; Lizzio, A.A.; Brady, T.A.

1996-01-01

Thermal analysis techniques have been used at the ISGS as an aid in the development and characterization of carbon adsorbents. Promising adsorbents from fly ash, tires, and Illinois coals have been produced for various applications. Process conditions determined in the preparation of gram quantities of carbons were used as guides in the preparation of larger samples. TG techniques developed to characterize the carbon adsorbents included the measurement of the kinetics of SO2 adsorption, the performance of rapid proximate analyses, and the determination of equilibrium methane adsorption capacities. Thermal regeneration of carbons was assessed by TG to predict the life cycle of carbon adsorbents in different applications. TPD was used to determine the nature of surface functional groups and their effect on a carbon's adsorption properties.

Accuracy Enhancement of Raman Spectroscopy Using Complementary Laser-Induced Breakdown Spectroscopy (LIBS) with Geologically Mixed Samples.

PubMed

Choi, Soojin; Kim, Dongyoung; Yang, Junho; Yoh, Jack J

2017-04-01

Quantitative Raman analysis was carried out with geologically mixed samples that have various matrices. In order to compensate the matrix effect in Raman shift, laser-induced breakdown spectroscopy (LIBS) analysis was performed. Raman spectroscopy revealed the geological materials contained in the mixed samples. However, the analysis of a mixture containing different matrices was inaccurate due to the weak signal of the Raman shift, interference, and the strong matrix effect. On the other hand, the LIBS quantitative analysis of atomic carbon and calcium in mixed samples showed high accuracy. In the case of the calcite and gypsum mixture, the coefficient of determination of atomic carbon using LIBS was 0.99, while the signal using Raman was less than 0.9. Therefore, the geological composition of the mixed samples is first obtained using Raman and the LIBS-based quantitative analysis is then applied to the Raman outcome in order to construct highly accurate univariate calibration curves. The study also focuses on a method to overcome matrix effects through the two complementary spectroscopic techniques of Raman spectroscopy and LIBS.

Voltammetric analysis of ceftazidime after preconcentration at various mercury and carbon electrodes: application to sub-ppb level determination in urine samples.

PubMed

El-Maali, N A

2000-04-28

The electrochemical behavior of ceftazidime (CFZ) at four different kinds of electrodes viz. static mercury drop electrode (SMDE), controlled growth mercury electrode (CGME), glassy carbon electrode (GCE) and carbon paste electrode (CPE) has been presented. Optimal operational parameters have been selected for the drug preconcentration and determination in aqueous medium. Down to 2x10(-10) M CFZ is achieved as detection limit at the CGME. Modification of the CPE with polyvinyl alcohol (PVA) enhances both the sensitivity and selectivity for the drug accumulation and, therefore, its determination at very low levels. Application of the proposed method for CFZ analysis in spiked urine samples or those taken after metabolism has been easily assessed. Down to 1x10(-9) M CFZ (0.695 ng ml(-1)) could be easily achieved in such samples.

Volatile, isotope, and organic analysis of martian fines with the Mars Curiosity rover.

PubMed

Leshin, L A; Mahaffy, P R; Webster, C R; Cabane, M; Coll, P; Conrad, P G; Archer, P D; Atreya, S K; Brunner, A E; Buch, A; Eigenbrode, J L; Flesch, G J; Franz, H B; Freissinet, C; Glavin, D P; McAdam, A C; Miller, K E; Ming, D W; Morris, R V; Navarro-González, R; Niles, P B; Owen, T; Pepin, R O; Squyres, S; Steele, A; Stern, J C; Summons, R E; Sumner, D Y; Sutter, B; Szopa, C; Teinturier, S; Trainer, M G; Wray, J J; Grotzinger, J P

2013-09-27

Samples from the Rocknest aeolian deposit were heated to ~835°C under helium flow and evolved gases analyzed by Curiosity's Sample Analysis at Mars instrument suite. H2O, SO2, CO2, and O2 were the major gases released. Water abundance (1.5 to 3 weight percent) and release temperature suggest that H2O is bound within an amorphous component of the sample. Decomposition of fine-grained Fe or Mg carbonate is the likely source of much of the evolved CO2. Evolved O2 is coincident with the release of Cl, suggesting that oxygen is produced from thermal decomposition of an oxychloride compound. Elevated δD values are consistent with recent atmospheric exchange. Carbon isotopes indicate multiple carbon sources in the fines. Several simple organic compounds were detected, but they are not definitively martian in origin.

Multiwavelength absorbance of filter deposits for determination of environmental tobacco smoke and black carbon

NASA Astrophysics Data System (ADS)

Lawless, Phil A.; Rodes, Charles E.; Ensor, David S.

A multiwavelength optical absorption technique has been developed for Teflon filters used for personal exposure sampling with sufficient sensitivity to allow apportionments of environmental tobacco smoke and soot (black) carbon to be made. Measurements on blank filters show that the filter material itself contributes relatively little to the total absorbance and filters from the same lot have similar characteristics; this makes retrospective analysis of filters quite feasible. Using an integrating sphere radiometer and multiple wavelengths to provide specificity, the determination of tobacco smoke and carbon with reasonable accuracy is possible on filters not characterized before exposure. This technique provides a low cost, non-destructive exposure assessment alternative to both standard thermo-gravimetric elemental carbon evaluations on quartz filters and cotinine analyses from urine or saliva samples. The method allows the same sample filter to be used for assessment of mass, carbon, and tobacco smoke without affecting the deposit.

An innovative molybdenum column liner for oxygen and hydrogen stable isotope analysis by pyrolysis.

PubMed

Stuart-Williams, Hilary; Wong, S Chin; Farquhar, Graham D; Keitel, Claudia; Clayton, Stephen

2008-04-01

The most widely used method for pyrolysing samples for hydrogen or oxygen isotopic analysis involves heating them to greater than 1300 degrees C in a helium stream passed through a glassy carbon tube in an alumina casing. There are a number of difficulties with this. Glassy carbon tubes are expensive and interaction between the carbon tube and the outer casing produces unwanted carbon monoxide by reduction of the alumina at high temperatures. The latter effect is overwhelming if temperatures of 1400 degrees C or greater are used for pyrolysis. We experimented with lining alumina casings with pure molybdenum sheet. It is relatively cheap, conforms well to the interior of the reactor tube (to avoid carrier and sample bypassing of the carbon pack), resists high temperatures and neither oxidises excessively nor absorbs the gases. The main disadvantages are that silver sample cups must be used and that the molybdenum degrades over time by formation of the carbide. We can maintain sharp peaks, high precision and good accuracy over more than 700 solid samples for both hydrogen and oxygen. The reactors last longer for water injections. The molybdenum in the columns does not contribute greatly to memory effects. The precision of analysis is dependent on other factors as well as the pyrolysis column, but for oxygen we typically achieve approximately <0.2 per thousand (sucrose), <0.25 per thousand (water) and <0.25 per thousand (leaf), sometimes using only a linear correction of drift, after dividing the run into 1 to 3 segments.

Method for isotopic analysis of chlorinated organic compounds

DOEpatents

Holt, B.D.; Sturchio, N.C.

1999-08-24

The present invention provides a method for preparing a VOC sample for carbon and chlorine isotope ratio analysis by mass spectrometer. A VOC sample is placed in a combustion tube and reacted with CuO to form CO{sub 2} and CuCl. The CO{sub 2} is then extracted and analyzed for the carbon isotope ratio. The CuCl is separated from the excess CuO and reacted with CH{sub 3}I to form CH{sub 3}Cl, extracted and analyzed for chlorine isotope ratio. 9 figs.

Analysis of drugs in human tissues by supercritical fluid extraction/immunoassay

NASA Astrophysics Data System (ADS)

Furton, Kenneth G.; Sabucedo, Alberta; Rein, Joseph; Hearn, W. L.

1997-02-01

A rapid, readily automated method has been developed for the quantitative analysis of phenobarbital from human liver tissues based on supercritical carbon dioxide extraction followed by fluorescence enzyme immunoassay. The method developed significantly reduces sample handling and utilizes the entire liver homogenate. The current method yields comparable recoveries and precision and does not require the use of an internal standard, although traditional GC/MS confirmation can still be performed on sample extracts. Additionally, the proposed method uses non-toxic, inexpensive carbon dioxide, thus eliminating the use of halogenated organic solvents.

Correlation analysis between forest carbon stock and spectral vegetation indices in Xuan Lien Nature Reserve, Thanh Hoa, Viet Nam

NASA Astrophysics Data System (ADS)

Dung Nguyen, The; Kappas, Martin

2017-04-01

In the last several years, the interest in forest biomass and carbon stock estimation has increased due to its importance for forest management, modelling carbon cycle, and other ecosystem services. However, no estimates of biomass and carbon stocks of deferent forest cover types exist throughout in the Xuan Lien Nature Reserve, Thanh Hoa, Viet Nam. This study investigates the relationship between above ground carbon stock and different vegetation indices and to identify the most likely vegetation index that best correlate with forest carbon stock. The terrestrial inventory data come from 380 sample plots that were randomly sampled. Individual tree parameters such as DBH and tree height were collected to calculate the above ground volume, biomass and carbon for different forest types. The SPOT6 2013 satellite data was used in the study to obtain five vegetation indices NDVI, RDVI, MSR, RVI, and EVI. The relationships between the forest carbon stock and vegetation indices were investigated using a multiple linear regression analysis. R-square, RMSE values and cross-validation were used to measure the strength and validate the performance of the models. The methodology presented here demonstrates the possibility of estimating forest volume, biomass and carbon stock. It can also be further improved by addressing more spectral bands data and/or elevation.

Worldwide Organic Soil Carbon and Nitrogen Data (1986) (NDP-018)

DOE Data Explorer

Zinke, P. J. [Univ. of California, Berkeley, CA (United States); Stangenberger, A. G. [Univ. of California, Berkeley, CA (United States); Post, W. M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Emanuel, W. R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Olson, J. S. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Millemann, R. E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Boden, T. A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

1986-01-01

This data base was begun with the collection and analysis of soil samples from California. Additional data came from soil surveys of Italy, Greece, Iran, Thailand, Vietnam, various tropical Amazonian areas, and U.S. forests and from the soil-survey literature. The analyzed samples were collected at uniform soil-depth increments and included bulk-density determinations. The data on each sample are soil profile number; soil profile carbon content; soil profile nitrogen content; sampling site latitude and longitude; site elevation; profile literature reference source; and soil profile codes for Holdridge life zone, Olson ecosystem type, and parent material. These data may be used to estimate the size of the soil organic carbon and nitrogen pools at equilibrium with natural soil-forming factors.

Symposium on the Tropospheric Chemistry of the Antarctic Region: Pre- Conference Abstracts

DTIC Science & Technology

1991-06-01

and composition); elemental carbon particles can scatter and absorb solar radiation. In addition, molecular species present as organic carbon aerosol ...elemental carbon to organic carbon aerosol particles are measured. This accounting pro- vides useful information needed to describe the ambient levels... Particle Analysis of Five Years of Aerosol Sampling in the Antarctic Peninsula P. Artaxo, W. M aenhaut and Rend Van Grieken

Aging of ceramic carbonized hydroxyapatite at room temperature

NASA Astrophysics Data System (ADS)

Tkachenko, M. V.; Kamzin, A. S.

2016-08-01

The process of aging of ceramic carbonized hydroxyapatite (CHA) produced in a dry carbon dioxide atmosphere at temperatures of 800-1200°C has been studied by chemical and X-ray structural analysis, infrared spectroscopy, and scanning electron microscopy methods. The phase composition and structure of initial prepared ceramics samples and those aged for a year have been compared. It has been shown that relaxation of internal stresses occurring during pressed sample sintering causes plastic deformation of crystallites at room temperature, accompanied by redistribution of carbonate ions between A1, A2, B1, and B2 sites and CHA decomposition with the formation of CaO separations.

Quantitative Hydrocarbon Surface Analysis

NASA Technical Reports Server (NTRS)

Douglas, Vonnie M.

2000-01-01

The elimination of ozone depleting substances, such as carbon tetrachloride, has resulted in the use of new analytical techniques for cleanliness verification and contamination sampling. The last remaining application at Rocketdyne which required a replacement technique was the quantitative analysis of hydrocarbons by infrared spectrometry. This application, which previously utilized carbon tetrachloride, was successfully modified using the SOC-400, a compact portable FTIR manufactured by Surface Optics Corporation. This instrument can quantitatively measure and identify hydrocarbons from solvent flush of hardware as well as directly analyze the surface of metallic components without the use of ozone depleting chemicals. Several sampling accessories are utilized to perform analysis for various applications.

Capillary absorption spectrometer and process for isotopic analysis of small samples

DOEpatents

Alexander, M. Lizabeth; Kelly, James F.; Sams, Robert L.; Moran, James J.; Newburn, Matthew K.; Blake, Thomas A.

2016-03-29

A capillary absorption spectrometer and process are described that provide highly sensitive and accurate stable absorption measurements of analytes in a sample gas that may include isotopologues of carbon and oxygen obtained from gas and biological samples. It further provides isotopic images of microbial communities that allow tracking of nutrients at the single cell level. It further targets naturally occurring variations in carbon and oxygen isotopes that avoids need for expensive isotopically labeled mixtures which allows study of samples taken from the field without modification. The method also permits sampling in vivo permitting real-time ambient studies of microbial communities.

Capillary absorption spectrometer and process for isotopic analysis of small samples

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

Alexander, M. Lizabeth; Kelly, James F.; Sams, Robert L.

A capillary absorption spectrometer and process are described that provide highly sensitive and accurate stable absorption measurements of analytes in a sample gas that may include isotopologues of carbon and oxygen obtained from gas and biological samples. It further provides isotopic images of microbial communities that allow tracking of nutrients at the single cell level. It further targets naturally occurring variations in carbon and oxygen isotopes that avoids need for expensive isotopically labeled mixtures which allows study of samples taken from the field without modification. The process also permits sampling in vivo permitting real-time ambient studies of microbial communities.

Fabrication method and microstructural characteristics of coal-tar-pitch-based 2D carbon/carbon composites

NASA Astrophysics Data System (ADS)

Esmaeeli, Mohammad; Khosravi, Hamed; Mirhabibi, Alireza

2015-02-01

The lignin-cellulosic texture of wood was used to produce two-dimensional (2D) carbon/carbon (C/C) composites using coal tar pitch. Ash content tests were conducted to select two samples among the different kinds of woods present in Iran, including walnut, white poplar, cherry, willow, buttonwood, apricots, berry, and blue wood. Walnut and white poplar with ash contents of 1.994wt% and 0.351wt%, respectively, were selected. The behavior of these woods during pyrolysis was investigated by differential thermal analysis (DTA) and thermo gravimetric (TG) analysis. The bulk density and open porosity were measured after carbonization and densification. The microstructural characteristics of samples were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier-transform infrared (FT-IR) spectroscopy. The results indicate that the density of both the walnut and white poplar is increased, and the open porosity is decreased with the increasing number of carbonization cycles. The XRD patterns of the wood charcoal change gradually with increasing pyrolysis temperature, possibly as a result of the ultra-structural changes in the charcoal or the presence of carbonized coal tar pitch in the composite's body.

Evaluation of thermal optical analysis method of elemental carbon for marine fuel exhaust.

PubMed

Lappi, Maija K; Ristimäki, Jyrki M

2017-12-01

The awareness of black carbon (BC) as the second largest anthropogenic contributor in global warming and an ice melting enhancer has increased. Due to prospected increase in shipping especially in the Arctic reliability of BC emissions and their invented amounts from ships is gaining more attention. The International Maritime Organization (IMO) is actively working toward estimation of quantities and effects of BC especially in the Arctic. IMO has launched work toward constituting a definition for BC and agreeing appropriate methods for its determination from shipping emission sources. In our study we evaluated the suitability of elemental carbon (EC) analysis by a thermal-optical transmittance (TOT) method to marine exhausts and possible measures to overcome the analysis interferences related to the chemically complex emissions. The measures included drying with CaSO 4, evaporation at 40-180ºC, H 2 O treatment, and variation of the sampling method (in-stack and diluted) and its parameters (e.g., dilution ratio, Dr). A reevaluation of the nominal organic carbon (OC)/EC split point was made. Measurement of residual carbon after solvent extraction (TC-C SOF ) was used as a reference, and later also filter smoke number (FSN) measurement, which is dealt with in a forthcoming paper by the authors. Exhaust sources used for collecting the particle sample were mainly four-stroke marine engines operated with variable loads and marine fuels ranging from light to heavy fuel oils (LFO and HFO) with a sulfur content range of <0.1-2.4% S. The results were found to be dependent on many factors, namely, sampling, preparation and analysis method, and fuel quality. It was found that the condensed H 2 SO 4 + H 2 O on the particulate matter (PM) filter had an effect on the measured EC content, and also promoted the formation of pyrolytic carbon (PyC) from OC, affecting the accuracy of EC determination. Thus, uncertainty remained regarding the EC results from HFO fuels. The work supports one part of the decision making in black carbon (BC) determination methodology. If regulations regarding BC emissions from marine engines will be implemented in the future, a well-defined and at best unequivocal method of BC determination is required for coherent and comparable emission inventories and estimating BC effects. As the aerosol from marine emission sources may be very heterogeneous and low in BC, special attention to the effects of sampling conditions and sample pretreatments on the validity of the results was paid in developing the thermal-optical analysis methodology (TOT).

Modified thermal-optical analysis using spectral absorption selectivity to distinguish black carbon from pyrolized organic carbon.

PubMed

Hadley, Odelle L; Corrigan, Craig E; Kirchstetter, Thomas W

2008-11-15

This study presents a method for analyzing the black carbon (BC) mass loading on a quartz fiber filter using a modified thermal-optical analysis method, wherein light transmitted through the sample is measured over a spectral region instead of at a single wavelength. Evolution of the spectral light transmission signal depends on the relative amounts of light-absorbing BC and char, the latter of which forms when organic carbon in the sample pyrolyzes during heating. Absorption selectivities of BC and char are found to be distinct and are used to apportion the amount of light attenuated by each component in the sample. Light attenuation is converted to mass concentration on the basis of derived mass attenuation efficiencies (MAEs) of BC and char. The fractions of attenuation due to each component are scaled by their individual MAE values and added together as the total mass of light absorbing carbon (LAC). An iterative algorithm is used to find the MAE values for both BC and char that provide the best fit to the carbon mass remaining on the filter (derived from direct measurements of thermally evolved CO2) at temperatures higher than 480 degrees C. This method was applied to measure the BC concentration in precipitation samples collected in northern California. The uncertainty in the measured BC concentration of samples that contained a high concentration of organics susceptible to char ranged from 12% to 100%, depending on the mass loading of BC on the filter. The lower detection limit for this method was approximately 0.35 microg of BC, and the uncertainty approached 20% for BC mass loading greater than 1.0 microg of BC.

Analysis Of Condensate Samples In Support Of The Antifoam Degradation Study

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

Hay, M.; Martino, C.

2016-01-12

The degradation of Antifoam 747 to form flammable decomposition products has resulted in declaration of a Potential Inadequacy in the Safety Analysis (PISA) for the Defense Waste Processing Facility (DWPF). Savannah River National Laboratory (SRNL) testing with simulants showed that hexamethyldisiloxane (HMDSO), trimethylsilanol (TMS), and 1-propanal are formed in the offgas from the decomposition of the antifoam. A total of ten DWPF condensate samples from Batch 735 and 736 were analyzed by SRNL for three degradation products and additional analytes. All of the samples were analyzed to determine the concentrations of HMDSO, TMS, and propanal. The results of the organicmore » analysis found concentrations for propanal and HMDSO near or below the detection limits for the analysis. The TMS concentrations ranged from below detection to 11 mg/L. The samples from Batch 736 were also analyzed for formate and oxalate anions, total organic carbon, and aluminum, iron, manganese, and silicon. Most of the samples contained low levels of formate and therefore low levels of organic carbon. These two values for each sample show reasonable agreement in most cases. Low levels of all the metals (Al, Fe, Mn, and Si) were present in most of the samples.« less

ANALYSIS OF CONDENSATE SAMPLES IN SUPPORT OF THE ANTIFOAM DEGRADATION STUDY

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

Hay, M.; Martino, C.

2016-02-29

The degradation of Antifoam 747 to form flammable decomposition products has resulted in declaration of a Potential Inadequacy in the Safety Analysis (PISA) for the Defense Waste Processing Facility (DWPF). Savannah River National Laboratory (SRNL) testing with simulants showed that hexamethyldisiloxane (HMDSO), trimethylsilanol (TMS), and 1-propanal are formed in the offgas from the decomposition of the antifoam. A total of ten DWPF condensate samples from Batch 735 and 736 were analyzed by SRNL for three degradation products and additional analytes. All of the samples were analyzed to determine the concentrations of HMDSO, TMS, and propanal. The results of the organicmore » analysis found concentrations for propanal and HMDSO near or below the detection limits for the analysis. The TMS concentrations ranged from below detection to 11 mg/L. The samples from Batch 736 were also analyzed for formate and oxalate anions, total organic carbon, and aluminum, iron, manganese, and silicon. Most of the samples contained low levels of formate and therefore low levels of organic carbon. These two values for each sample show reasonable agreement in most cases. Low levels of all the metals (Al, Fe, Mn, and Si) were present in most of the samples.« less

Uranium-series dated authigenic carbonates and Acheulian sites in southern Egypt

NASA Technical Reports Server (NTRS)

Szabo, B. J.; Mchugh, W. P.; Schaber, G. G.; Breed, C. S.; Haynes, C. V., Jr.

1989-01-01

Field investigations of aggraded paleovalleys, which were identified in southern Egypt using SIR, are discussed. Acheulian artifacts were found in authigenic carbonate deposites along the edges of the paleovalleys. Uranium series dating of 25 carbonate samples shows that widespread carbonate deposition in the area occurred about 45, 141, and 212 thousand years ago. Analysis of the carbonate suggests that the deposition may be related to late Pleistocene humid climates that facilitated human settlement in the region.

Abundant pre-industrial carbon detected in Canadian Arctic headwaters: implications for the permafrost carbon feedback

NASA Astrophysics Data System (ADS)

Dean, J. F.; van der Velde, Y.; Garnett, M. H.; Dinsmore, K. J.; Baxter, R.; Lessels, J. S.; Smith, P.; Street, L. E.; Subke, J.-A.; Tetzlaff, D.; Washbourne, I.; Wookey, P. A.; Billett, M. F.

2018-03-01

Mobilization of soil/sediment organic carbon into inland waters constitutes a substantial, but poorly-constrained, component of the global carbon cycle. Radiocarbon (14C) analysis has proven a valuable tool in tracing the sources and fate of mobilized carbon, but aquatic 14C studies in permafrost regions rarely detect ‘old’ carbon (assimilated from the atmosphere into plants and soil prior to AD1950). The emission of greenhouse gases derived from old carbon by aquatic systems may indicate that carbon sequestered prior to AD1950 is being destabilized, thus contributing to the ‘permafrost carbon feedback’ (PCF). Here, we measure directly the 14C content of aquatic CO2, alongside dissolved organic carbon, in headwater systems of the western Canadian Arctic—the first such concurrent measurements in the Arctic. Age distribution analysis indicates that the age of mobilized aquatic carbon increased significantly during the 2014 snow-free season as the active layer deepened. This increase in age was more pronounced in DOC, rising from 101-228 years before sampling date (a 120%-125% increase) compared to CO2, which rose from 92-151 years before sampling date (a 59%-63% increase). ‘Pre-industrial’ aged carbon (assimilated prior to ~AD1750) comprised 15%-40% of the total aquatic carbon fluxes, demonstrating the prevalence of old carbon to Arctic headwaters. Although the presence of this old carbon is not necessarily indicative of a net positive PCF, we provide an approach and baseline data which can be used for future assessment of the PCF.

The enhancement in electrical analysis of the nitrogen doped amorphous carbon thin films (a-C:N) prepared by aerosol-assisted CVD

NASA Astrophysics Data System (ADS)

Fadzilah, A. N.; Dayana, K.; Rusop, M.

2018-05-01

This paper reports on the deposition of Nitrogen doped amorphous carbon (a-C:N) by Aerosol-assisted Chemical Vapor Deposition (AACVD) using natural source of camphor oil as the precursor material. 5 samples were deposited at 5 different deposition times from 15 min to 90 min, with 15 min interval for each sample. The highest slope of linear graph was noted at the sample with 45 min deposition time, showing the lowest electrical resistance of the sample. From I-V characteristic, the sample deposited at 45 min has the highest electrical conductivity due to high sp2 carbon bonding ratio. Nanostructured behavior of N doped a-C:N was also investigated by FESEM micrograph resulting with the particle size less than 100nm.

Isotopic and Geochemical Investigation of Two Distinct Mars Analog Environments Using Evolved Gas Techniques in Svalbard, Norway

NASA Technical Reports Server (NTRS)

Stern, Jennifer Claire; Mcadam, Amy Catherine; Ten Kate, Inge L.; Bish, David L.; Blake, David F.; Morris, Richard V.; Bowden, Roxane; Fogel, Marilyn L.; Glamoclija, Mihaela; Mahaffy, Paul R.;

The carbon functional group budget of a peatland

NASA Astrophysics Data System (ADS)

Moody, Catherine; Worrall, Fred; Clay, Gareth; Apperley, David

2016-04-01

Organic matter samples were taken from each organic matter reservoir and fluvial flux found in a peatland and analysed by elemental analysis for carbon, hydrogen, nitrogen and oxygen content, and by 13C solid state nuclear magnetic resonance (NMR) for functional group composition. The samples analysed were: aboveground, belowground, heather, mosses and sedges, litter layer, four different depths from a peat core, and monthly samples of fluvial particulate and dissolved organic matter. All organic matter samples were taken from a 100% peat catchment within Moor House National Nature Reserve in the North Pennines, UK. The proportion of carbon atoms from each of the eight carbon functional groups (C-alkyl, N-alkyl/methoxyl C, O-alkyl, O2-alkyl/acetal C, aromatic/unsaturated C, phenolic C, aldehyde/ketone C and amide/carboxyl C) from each type of organic matter were combined with an existing carbon budget from the same site, to give a functional group carbon budget. The budget results show that the ecosystem is accumulating N-alkyl/methoxyl C, O-alkyl, O2-alkyl/acetal C and phenolic C groups, but losing C-alkyl, aromatic/unsaturated C, amide/carboxyl C and aldehyde/ketone C. Comparing the functional group compositions between the sampled organic matter pools shows that DOM arises from two distinct sources; from the peat itself and from a vegetation source.

Field Characterization of the Mineralogy and Organic Chemistry of Carbonates from the 2010 Arctic Mars Analog Svalbard Expedition by Evolved Gas Analysis

NASA Technical Reports Server (NTRS)

McAdam, A. C.; Ten Kate, I. L.; Stern, J. C.; Mahaffy, P. R.; Blake, D. F.; Morris, R. V.; Steele, A.; Amundson, H. E. F.

2011-01-01

The 2010 Arctic Mars Analog Svalbard Expedition (AMASE) investigated two geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return. The Sample Analysis at Mars (SAM) [1] instrument suite, which will be on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser mass spectrometer (TLS); all will be applied to analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-MS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples [e.g., 2]. Field-portable versions of CheMin were used during AMASE. AMASE 2010 focused on two sites that represented biotic and abiotic analogs. The abiotic site was the basaltic Sigurdfjell vent complex, which contains Mars-analog carbonate cements including carbonate globules which are excellent analogs for the globules in the ALH84001 martian meteorite [e.g., 3, 4]. The biotic site was the Knorringfjell fossil methane seep, which featured carbonates precipitated in a methane-supported chemosynthetic community [5]. This contribution focuses on EGA-MS analyses of samples from each site, with mineralogy comparisons to CheMin team results. The results give insight into organic content and organic-mineral associations, as well as some constraints on the minerals present.

Influences of carbon content and coating carbon thickness on properties of amorphous CoSnO3@C composites as anode materials for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Fan, Fuqiang; Fang, Guoqing; Zhang, Ruixue; Xu, Yanhui; Zheng, Junwei; Li, Decheng

2014-08-01

A series of core-shell carbon coated amorphous CoSnO3 (CoSnO3@C) with different carbon content are synthesized. Effects of carbon content and coating carbon thickness on the physical and electrochemical performances of the samples were studied in detail. The samples were analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA), galvanostatic charge-discharge and AC impedance spectroscopy, respectively. The results indicate that controlling the concentration of aqueous glucose solution influences the generation of in-situ carbon layer thickness. The optimal concentration of aqueous glucose solution, carbon content and carbon layer thickness are suggested as 0.25 M, 35.1% and 20 nm, respectively. CoSnO3@C composite prepared under the optimal conditions exhibits excellent cycling performance, whose reversible capacity could reach 491 mA h g-1 after 100 cycles.

Electrochemical behavior of platinum nanoparticles on a carbon xerogel support modified with a [(trifluoromethyl)-benzenesulfonyl]imide electrolyte.

PubMed

Liu, Bing; Mei, Hua; DesMarteau, Darryl; Creager, Stephen E

2014-12-11

A monoprotic [(trifluoromethyl)benzenesulfonyl]imide (SI) superacid electrolyte was used to covalently modify a mesoporous carbon xerogel (CX) support via reaction of the corresponding trifluoromethyl aryl sulfonimide diazonium zwitterion with the carbon surface. Electrolyte attachment was demonstrated by elemental analysis, acid-base titration, and thermogravimetric analysis. The ion-exchange capacity of the fluoroalkyl-aryl-sulfonimide-grafted carbon xerogel (SI-CX) was ∼0.18 mequiv g(-1), as indicated by acid-base titration. Platinum nanoparticles were deposited onto the SI-grafted carbon xerogel samples by the impregnation and reduction method, and these materials were employed to fabricate polyelectrolyte membrane fuel-cell (PEMFC) electrodes by the decal transfer method. The SI-grafted carbon-xerogel-supported platinum (Pt/SI-CX) was characterized by X-ray diffraction and transmission electron microscopy to determine platinum nanoparticle size and distribution, and the findings are compared with CX-supported platinum catalyst without the grafted SI electrolyte (Pt/CX). Platinum nanoparticle sizes are consistently larger on Pt/SI-CX than on Pt/CX. The electrochemically active surface area (ESA) of platinum catalyst on the Pt/SI-CX and Pt/CX samples was measured with ex situ cyclic voltammetry (CV) using both hydrogen adsorption/desorption and carbon monoxide stripping methods and by in situ CV within membrane electrode assemblies (MEAs). The ESA values for Pt/SI-CX are consistently lower than those for Pt/CX. Some possible reasons for the behavior of samples with and without grafted SI layers and implications for the possible use of SI-grafted carbon layers in PEMFC devices are discussed.

Detection of Organic Matter in Sediments with Near-Infrared Reflectance Spectroscopy: Effects of Mineralogy, Albedo and Hydration

NASA Astrophysics Data System (ADS)

Kaplan, H. H.; Milliken, R.

2014-12-01

Laboratory, field-, and satellite-based visible-near infrared reflectance spectroscopy allows for rapid, remote, and non-destructive analysis of geologic materials to identify mineralogy as well as organic compounds. This type of analysis has potential to aid the search for organics on Mars as a means of first detection of reduced carbon, or to study organic matter nondestructively in valuable samples such as meteorites. In order to assess potential applications of this method we aim to answer fundamental questions about detection limits and quantification of organic matter using reflectance spectroscopy. Laboratory mixtures and natural samples are measured for total organic carbon (TOC in wt.%) with standard methods and reflectance spectroscopy. Absorption features due to C-H2 and C-H3 bonds are observed in the 3.3 to 3.5μm (3000 to 2850 cm-1) wavelength region. A strong H2O feature near 3μm, as well as carbonate-related absorptions near 3.4µm, are also found in this spectral region and can complicate detection of organic material, particularly at low TOC values. In natural samples without carbonate there appears to be a linear trend between TOC and the band depth of organic absorptions; samples that have low albedo, or strong 3μm water features deviate from this trend line. Spectra of samples with carbonate may be modeled with Gaussians to remove the influence of the carbonate features and better match the organic absorption trend. Early results indicate that quantification of organic matter in natural fine-grained samples using reflectance spectroscopy will need to take low-albedo components and water content into account. Detection limits may also depend on these properties; organic absorption features are clearly seen in the lowest TOC sample measured so far (0.08wt% or 800ppm), which is a relatively bright, carbonate-free, quartz- and clay-dominated outcrop sample. A series of laboratory experiments have been undertaken in which known amounts of organic compounds are mixed with smectitic clay in order to understand detection limits and the effects of albedo and hydration in a controlled setting. These laboratory results are compared with findings from natural samples that represent a wide range of ages and depositional settings.

40 CFR 600.112-78 - Exhaust sample analysis.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 29 2010-07-01 2010-07-01 false Exhaust sample analysis. 600.112-78 Section 600.112-78 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy Regulations for 1978...

40 CFR 600.112-08 - Exhaust sample analysis.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 29 2010-07-01 2010-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy Regulations for 1978...

40 CFR 600.112-08 - Exhaust sample analysis.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 31 2013-07-01 2013-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and Carbon-Related...

40 CFR 600.112-08 - Exhaust sample analysis.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 31 2012-07-01 2012-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and Carbon-Related...

40 CFR 600.112-08 - Exhaust sample analysis.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 30 2014-07-01 2014-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and Carbon-Related...

Soil Carbon Variability and Change Detection in the Forest Inventory Analysis Database of the United States

NASA Astrophysics Data System (ADS)

Wu, A. M.; Nater, E. A.; Dalzell, B. J.; Perry, C. H.

2014-12-01

The USDA Forest Service's Forest Inventory Analysis (FIA) program is a national effort assessing current forest resources to ensure sustainable management practices, to assist planning activities, and to report critical status and trends. For example, estimates of carbon stocks and stock change in FIA are reported as the official United States submission to the United Nations Framework Convention on Climate Change. While the main effort in FIA has been focused on aboveground biomass, soil is a critical component of this system. FIA sampled forest soils in the early 2000s and has remeasurement now underway. However, soil sampling is repeated on a 10-year interval (or longer), and it is uncertain what magnitude of changes in soil organic carbon (SOC) may be detectable with the current sampling protocol. We aim to identify the sensitivity and variability of SOC in the FIA database, and to determine the amount of SOC change that can be detected with the current sampling scheme. For this analysis, we attempt to answer the following questions: 1) What is the sensitivity (power) of SOC data in the current FIA database? 2) How does the minimum detectable change in forest SOC respond to changes in sampling intervals and/or sample point density? Soil samples in the FIA database represent 0-10 cm and 10-20 cm depth increments with a 10-year sampling interval. We are investigating the variability of SOC and its change over time for composite soil data in each FIA region (Pacific Northwest, Interior West, Northern, and Southern). To guide future sampling efforts, we are employing statistical power analysis to examine the minimum detectable change in SOC storage. We are also investigating the sensitivity of SOC storage changes under various scenarios of sample size and/or sample frequency. This research will inform the design of future FIA soil sampling schemes and improve the information available to international policy makers, university and industry partners, and the public.

Characterization of Malaysian coals for carbon dioxide sequestration

NASA Astrophysics Data System (ADS)

Abunowara, M.; Bustam, M. A.; Sufian, S.; Eldemerdash, U.

2016-06-01

Coal samples from Mukah-Balingian and Merit-Pila coal mines were characterized with ultimate, approximate, petrographic analysis, FT-IR spectra patterns, FESEM images and BET measurements to obtain information on the chemical composition and chemical structure in the samples. Two coal samples were obtained from Merit-Pila coal mine namely sample1 (S1) and sample2 (S2). The other two coal samples were obtained from Mukah-Balingian coal mine namely sample3 (S3) and sample4 (S4), Sarawak, Malaysia. The results of ultimate analysis show that coal S1 has the highest carbon percentage by 54.47%, the highest hydrogen percentage by 10.56% and the lowest sulfur percentage by 0.19% and the coal S4 has the highest moisture content by 31.5%. The coal S1 has the highest fixed carbon percentage by 42.6%. The coal S4 has BET surface area by 2.39 m2/g and Langmuir surface area by 3.0684 m2/g respectively. Fourier-Transform Infrared (FT-IR) spectroscopy analysis of all coal samples shows a presence of oxygen containing functional groups which considered are as active sites on coal surface. The oxygen functional groups are mainly carboxyl (-COOH), hydroxyl (-OH), alkyl (-CH, -CH2, -CH3), aliphatic (C-O-C stretching associated with -OH), amino (-NH stretching vibrations), (-NH stretching vibrations), aromatic (C=C), vinylic (C=C) and clay minerals. In all FE-SEM images of coal samples matrix, it can be seen that there are luminous and as non luminous features which refer to the existence of various minerals types distributed in the coal organic matrix. The bright luminosity is due to the presence of sodium, potassium or aluminium. According to petrographic analysis, all coal sample samples are range in vitrinite reflectance from 0.38% to 56% (VRr) are sub-bituminous coals.

Identification of atmospheric organic sources using the carbon hollow tube-gas chromatography method and factor analysis

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

Cobb, G.P.; Braman, R.S.; Gilbert, R.A.

Atmospheric organics were sampled and analyzed by using the carbon hollow tube-gas chromatography method. Chromatograms from spice mixtures, cigarettes, and ambient air were analyzed. Principal factor analysis of row order chromatographic data produces factors which are eigenchromatograms of the components in the samples. Component sources are identified from the eigenchromatograms in all experiments and the individual eigenchromatogram corresponding to a particular source is determined in most cases. Organic sources in ambient air and in cigaretts are identified with 87% certainty. Analysis of clove cigarettes allows the determination of the relative amount of clove in different cigarettes. A new nondestructive qualitymore » control method using the hollow tube-gas chromatography analysis is discussed.« less

Methods for collection and analysis of geopressured geothermal and oil field waters

USGS Publications Warehouse

Lico, Michael S.; Kharaka, Yousif K.; Carothers, William W.; Wright, Victoria A.

1982-01-01

Present methods are described for the collection, preservation, and chemical analysis of waters produced from geopressured geothermal and petroleum wells. Detailed procedures for collection include precautions and equipment necessary to ensure that the sample is representative of the water produced. Procedures for sample preservation include filtration, acidification, dilution for silica, methyl isobutyl ketone (MIBK) extraction of aluminum, addition of potassium permanganate to preserve mercury, and precipitation of carbonate species as strontium carbonate for stable carbon isotopes and total dissolved carbonate analysis. Characteristics determined at the well site are sulfide, pH, ammonia, and conductivity. Laboratory procedures are given for the analysis of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, iron, manganese, zinc, lead, aluminum, .and mercury by atomic absorption and flame emission spectroscopy. Chloride is determined by silver nitrate titration and fluoride by ion-specific electrode. Bromide and iodide concentrations are determined by the hypochlorite oxidation method. Sulfate is analyzed by titration using barium chloride with thorin indicator after pretreatment with alumina. Boron and silica are determined colorimetrically by the carmine and molybdate-blue methods, respectively. Aliphatic acid anions (C2 through C5) are determined by gas chromatography after separation and concentration in a chloroform-butanol mixture.

An effective and low cost carbon based clean-up method for PCDD/Fs and PCBs analysis in food.

PubMed

Kedikoglou, Kleopatra; Costopoulou, Danae; Vassiliadou, Irene; Bakeas, Evangelos; Leondiadis, Leondios

2018-09-01

Sample preparation is of critical importance in dioxin analysis of food and feed samples. It is a complex procedure that includes lipid extraction followed by the application of chromatographic separation techniques, aiming in removing undesirable interferences from the matrix. The separation of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) from polychlorinated biphenyls (PCBs) is achieved by carbon-based materials which should have high fat capacity in order to be suitable for lipid-containing matrices. Automated methods are available but due to high cost and use of high amounts of solvents, manual methods are also applied. An active carbon material (Carbosphere) with high fat capacity that has been used in the past for manual methods is no longer commercially available. The present study assesses an alternative active carbon material, FU 4652, that can be used for the separation of PCDD/Fs and non-ortho PCBs. Mono-ortho and 6 non-dioxin-like PCBs are also analyzed. The method was validated according to the analytical criteria set in EU regulations 589/2014 and 709/2014. Control samples analyzed for the evaluation of the above material were olive oil reference samples spiked with PCDD/Fs and dioxin-like PCBs at two concentration levels. The new method was tested successfully on food samples of interlaboratory trials organized in previous years. Farmed fish samples collected within national surveillance programs for the years 2016-2017 were analyzed with the method developed. The results obtained indicate that the FU 4652 carbon sorbent has high fat capacity and is capable of separating congeners with good recoveries. Copyright © 2018 Elsevier Ltd. All rights reserved.

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.

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.

Ion microprobe measurement of strontium isotopes in calcium carbonate with application to salmon otoliths

USGS Publications Warehouse

Weber, P.K.; Bacon, C.R.; Hutcheon, I.D.; Ingram, B.L.; Wooden, J.L.

2005-01-01

The ion microprobe has the capability to generate high resolution, high precision isotopic measurements, but analysis of the isotopic composition of strontium, as measured by the 87Sr/ 86Sr ratio, has been hindered by isobaric interferences. Here we report the first high precision measurements of 87Sr/ 86Sr by ion microprobe in calcium carbonate samples with moderate Sr concentrations. We use the high mass resolving power (7000 to 9000 M.R.P.) of the SHRIMP-RG ion microprobe in combination with its high transmission to reduce the number of interfering species while maintaining sufficiently high count rates for precise isotopic measurements. The isobaric interferences are characterized by peak modeling and repeated analyses of standards. We demonstrate that by sample-standard bracketing, 87Sr/86Sr ratios can be measured in inorganic and biogenic carbonates with Sr concentrations between 400 and 1500 ppm with ???2??? external precision (2??) for a single analysis, and subpermil external precision with repeated analyses. Explicit correction for isobaric interferences (peak-stripping) is found to be less accurate and precise than sample-standard bracketing. Spatial resolution is ???25 ??m laterally and 2 ??m deep for a single analysis, consuming on the order of 2 ng of material. The method is tested on otoliths from salmon to demonstrate its accuracy and utility. In these growth-banded aragonitic structures, one-week temporal resolution can be achieved. The analytical method should be applicable to other calcium carbonate samples with similar Sr concentrations. Copyright ?? 2005 Elsevier Ltd.

Guidelines for collection and field analysis of ground-water samples for selected unstable constituents

USGS Publications Warehouse

Wood, Warren W.

1976-01-01

The unstable nature of many chemical and physical constituents in ground water requires special collection procedures and field analysis immediately after collection. This report describes the techniques and equipment commonly used m the collection and field analysis of samples for pH, temperature, carbonate, bicarbonate, specific conductance, Eh, and dissolved oxygen.

60-day safety screen results and final report for tank 241-C-111, auger samples 95-Aug-002, 95-Aug-003, 95-Aug-016, and 95-Aug-017

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

Rice, A.D.

1995-05-30

This report presents the details of the auger sampling events for underground waste tank C-111. The samples were shipped to the 222-S laboratories were they underwent safety screening analysis and primary ferricyanide analysis. The samples were analyzed for alpha total, total organic carbon, cyanide, Ni, moisture, and temperature differentials. The results of this analysis are presented in this document.

The measurement of unburned carbon in fly ash using infrared photoacoustics

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

Waller, D.J.; Brown, R.C.

1995-12-31

Unburned carbon in fly ash yields valuable information on coal combustion efficiency in coal-fired boilers. The carbon content of fly ash is also an important parameters in the sale of fly ash for Portland cement. Unfortunately, a reliable and inexpensive instrument for measuring unburned carbon is not commercially available. The authors have developed an off-line instrument that detects carbon in fly ash via the photoacoustic effect. In this process, amplitude-modulated radiation is absorbed by a bulk sample of fly ash. The wavelength of the radiation is chosen such that mineral compounds and moisture in the fly ash are transparent tomore » the radiation but carbon is strongly absorbing. The modulated absorption generates a periodic pressure wave at the surface of the sample which propagates through the surrounding air as an acoustic wave. This wave is detected by a sensitive microphone, and is dependent on the carbon content of the sample. The resulting instrument has been used to measure fly ash carbon concentrations from less than 0.1% to nearly 7% by mass. The precision of these measurements is nominally within 4%, which is equivalent to the precision of the chemical analysis used to develop the calibration standards. The applicability of a theoretical model to the empirical results is discussed with respect to fly ash sample preparation.« less

Heterogeneity of shale documented by micro-FTIR and image analysis.

PubMed

Chen, Yanyan; Mastalerz, Maria; Schimmelmann, Arndt

2014-12-01

In this study, four New Albany Shale Devonian and Mississippian samples, with vitrinite reflectance [Ro ] values ranging from 0.55% to 1.41%, were analyzed by micro-FTIR mapping of chemical and mineralogical properties. One additional postmature shale sample from the Haynesville Shale (Kimmeridgian, Ro = 3.0%) was included to test the limitation of the method for more mature substrates. Relative abundances of organic matter and mineral groups (carbonates, quartz and clays) were mapped across selected microscale regions based on characteristic infrared peaks and demonstrated to be consistent with corresponding bulk compositional percentages. Mapped distributions of organic matter provide information on the organic matter abundance and the connectivity of organic matter within the overall shale matrix. The pervasive distribution of organic matter mapped in the New Albany Shale sample MM4 is in agreement with this shale's high total organic carbon abundance relative to other samples. Mapped interconnectivity of organic matter domains in New Albany Shale samples is excellent in two early mature shale samples having Ro values from 0.55% to 0.65%, then dramatically decreases in a late mature sample having an intermediate Ro of 1.15% and finally increases again in the postmature sample, which has a Ro of 1.41%. Swanson permeabilities, derived from independent mercury intrusion capillary pressure porosimetry measurements, follow the same trend among the four New Albany Shale samples, suggesting that micro-FTIR, in combination with complementary porosimetric techniques, strengthens our understanding of porosity networks. In addition, image processing and analysis software (e.g. ImageJ) have the capability to quantify organic matter and total organic carbon - valuable parameters for highly mature rocks, because they cannot be analyzed by micro-FTIR owing to the weakness of the aliphatic carbon-hydrogen signal. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

Fabrication of Fe3O4 Nanoparticle-coalesced Hydroxylated Multi-walled Carbon Nanotubes for the Analysis of Strychnine in Human Serum.

PubMed

Feng, Zufei; Xu, Yuehong; Wei, Shuguang; Zhang, Bao; Guan, Fanglin; Li, Shengbin

2015-01-01

A magnetic carbon nanomaterial for Fe3O4-modified hydroxylated multi-walled carbon nanotubes (Fe3O4-MWCNTs-OH) was prepared by the aggregating effect of Fe3O4 nanoparticles on MWCNTs-OH, and this material was combined with high-performance liquid chromatography (HPLC)/photodiode array detector (PAD) to determine strychnine in human serum samples. Some important parameters that could influence the extraction efficiency of strychnine were optimized, including the extraction time, amounts of Fe3O4-MWCNTs-OH, pH of sample solution, desorption solvent and desorption time. Under optimal conditions, the recoveries of spiked serum samples were between 98.3 and 102.7%, and the relative standard deviations (RSDs) ranged from 0.9 to 5.3%. The correlation coefficient was 0.9997. The LODs and LOQs of strychnine were 6.2 and 20.5 ng mL(-1), at signal-to-noise ratios of 3 and 10, respectively. These experimental results showed that the proposed method is feasible for the analysis of strychnine in serum samples.

The influencing factors of China carbon price: a study based on carbon trading market in hubei province

NASA Astrophysics Data System (ADS)

Li, Hao; Lei, Ming

2018-02-01

For the carbon market, good trading mechanism is the basis for the healthy development of the carbon trading market. In order to explore the core problem of carbon price formation, our research explores the influencing factors of the price of carbon trading market. After the preliminary statistical analysis, our study found that Hubei Province is in the leading position among seven pilots in the carbon trading volume and the transaction, so our study of carbon price takes Hubei Province as sample of the empirical research. Multi-time series model and ARCH model analysis method are used in the research, we use the data of Hubei carbon trading pilot from June 2014 to December 2016 to carry out empirical research, the results found that industrial income, energy price, government intervention and the number of participating corporation have significant effect on the carbon price, which provides a meaningful reference for the other pilots in-depth study, as well as the construction of a national carbon trading market.

Measurement of carbon distribution in nuclear fuel pin cladding specimens by means of a secondary ion mass spectrometer

NASA Astrophysics Data System (ADS)

Bart, Gerhard; Aerne, Ernst Tino; Burri, Martin; Zwicky, Hans-Urs

1986-11-01

Cladding carburization during irradiation of advanced mixed uranium plutonium carbide fast breeder reactor fuel is possibly a life limiting fuel pin factor. The quantitative assessment of such clad carbon embrittlement is difficult to perform by electron microprobe analysis because of sample surface contamination, and due to the very low energy of the carbon K α X-ray transition. The work presented here describes a method developed at the Swiss Federal Institute for Reactor Research (EIR) to use shielded secondary ion mass spectrometry (SIMS) as an accurate tool to determine radial distribution profiles of carbon in radioactive stainless steel fuel pin cladding. Compared with nuclear microprobe analysis (NMA) [1], which is also an accurate method for carbon analysis, the SIMS method distinguishes itself by its versatility for simultaneous determination of additional impurities.

Rapid analysis of pesticide residues in drinking water samples by dispersive solid-phase extraction based on multiwalled carbon nanotubes and pulse glow discharge ion source ion mobility spectrometry.

PubMed

Zou, Nan; Gu, Kejia; Liu, Shaowen; Hou, Yanbing; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

2016-03-01

An analytical method based on dispersive solid-phase extraction with a multiwalled carbon nanotubes sorbent coupled with positive pulse glow discharge ion mobility spectrometry was developed for analysis of 30 pesticide residues in drinking water samples. Reduced ion mobilities and the mass-mobility correlation of 30 pesticides were measured. The pesticides were divided into five groups to verify the separation capability of pulse glow discharge in mobility spectrometry. The extraction conditions such as desorption solvent, ionic strength, conditions of adsorption and desorption, the amounts of multiwalled carbon nanotubes, and solution pH were optimized. The enrichment factors of pesticides were 5.4- to 48.7-fold (theoretical enrichment factor was 50-fold). The detection limits of pesticides were 0.01∼0.77 μg/kg. The linear range was 0.005-0.2 mg/L for pesticide standard solutions, with determination coefficients from 0.9616 to 0.9999. The method was applied for the analysis of practical and spiked drinking water samples. All results were confirmed by high-performance liquid chromatography with tandem mass spectrometry. The proposed method was proven to be a commendably rapid screening qualitative and semiquantitative technique for the analysis of pesticide residues in drinking water samples on site. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York--July 1999 through June 2001

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance and quality-control data were stored in the laboratory's LabMaster data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality-control samples analyzed from July 1999 through June 2001. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, calcium, chloride and nitrate (ion chromatography and colormetric method) and sulfate. The total aluminum and dissolved organic carbon procedures were biased throughout the analysis period for the high-concentration sample, but were within control limits. The calcium and specific conductance procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The magnesium procedure was biased for the high-concentration and low concentration samples, but was within control limits. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 14 of 15 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for dissolved organic carbon. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 17 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except ammonium (81 percent of samples met objectives), chloride (75 percent of samples met objectives), and sodium (86 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality over the time period, with most ratings for each sample in the good to excellent range. The P-sample (low-ionic-strength constituents) analysis had one satisfactory rating for the specific conductance procedure in one study. The T-sample (trace constituents) analysis had one satisfactory rating for the aluminum procedure in one study and one unsatisfactory rating for the sodium procedure in another. The remainder of the samples had good or excellent ratings for each study. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 89 percent of the samples met data-quality objectives for 10 of the 14 analytes; the exceptions were ammonium, total aluminum, dissolved organic carbon, and sodium. Results indicate a positive bias for the ammonium procedure in all studies. Data-quality objectives were not met in 50 percent of samples analyzed for total aluminum, 38 percent of samples analyzed for dissolved organic carbon, and 27 percent of samples analyzed for sodium. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 91 percent of the samples analyzed for calcium, chloride, fluoride, magnesium, pH, potassium, and sulfate. Data-quality objectives were met by 75 percent of the samples analyzed for sodium and 58 percent of the samples analyzed for specific conductance.

Searching for Reduced Carbon on the Surface of Mars: The SAM Combustion Experiment

NASA Technical Reports Server (NTRS)

Stern, J. C.; Malespin, C. A.; Mahaffy, P. R.; Webster, C. R.; Eigenbrode, J. L.; Archer, P. D., Jr.; Brunner, A. E.; Freissinet, C.; Franz, H. B.; Glavin, D. P.;

Carbon ions irradiation on nano- and microcrystalline CaSO4 : Dy

NASA Astrophysics Data System (ADS)

Salah, Numan

2008-08-01

Nanoparticles of CaSO4 : Dy phosphor with a particle size of around 30 nm have been prepared by the chemical co-precipitation technique. Pellet samples of the nanomaterials were irradiated by a 75 MeV C6+ ion beam at the fluence range 1 × 109-1 × 1013 ions cm-2. Thermoluminescence (TL) glow curves of the irradiated samples were recorded and studied. The microcrystalline form of this sample is also included in the study with the aim of reporting a comparative measurement. The TL analysis shows that the glow curve of the nanomaterial has two peaks at around 166 and 210 °C. These peaks are similar to those induced in the microcrystalline sample with a slight difference in their TL response. The second peak is more prominent in the case of the microcrystalline sample at low fluences, while the first one dominates in the nanostructured sample mainly at higher fluences. The TRIM code based on Monte Carlo simulation was also used for calculating some ion beam parameters. Dosimetric properties of the carbon ion beam irradiated materials show that the nanostructure material has excellent features such as a simple glow curve structure and a linear TL response over a wider range than the corresponding microcrystalline sample. These results show that the nanostructure form of CaSO4 : Dy might be useful for detecting the high doses of carbon ions used in radiotherapy. Thermal analysis of the prepared nano- and microcrystalline materials was also done in the range 50-500 °C using thermogravimetry analysis and differential thermal analysis. No phase transitions within this range of heating for both the materials are observed.

Catalytic graphitization behavior of phenolic resins by addition of in situ formed nano-Fe particles

NASA Astrophysics Data System (ADS)

Rastegar, H.; Bavand-vandchali, M.; Nemati, A.; Golestani-Fard, F.

2018-07-01

This work presents the catalytic graphitization process of phenolic resins (PR's) by addition of in situ nano-Fe particles as catalyst. Pyrolysis treatments of prepared compositions including various contents of nano-Fe particles were carried out at 600-1200 °C for 3 h under reducing atmosphere and graphitization process were evaluated by different techniques such as X-Ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), High Resolution Transmission Electron Microscopy (HRTEM), Simultaneous Thermal Analysis (STA) and Raman spectroscopy that mainly performed to identify the phase and microstructural analysis, oxidation resistance and extend of graphitized carbon formation. Results indicate that, in situ graphitic carbon development were already observed after firing the samples at 800 °C for 3 h under reducing atmosphere, increasing temperature and amount of nano-Fe led to a more effective graphitization level. In addition, the different nano crystalline carbon shapes such as onion and bamboo like and carbon nanotubes (CNTs) were in situ identified during graphitization process of nano-Fe containing samples. It was suggested that formation of these different nano carbon structures related to nano-Fe catalyst behavior and the carbon shell growth.

Calcium Carbonate Precipitation by Bacillus and Sporosarcina Strains Isolated from Concrete and Analysis of the Bacterial Community of Concrete.

PubMed

Kim, Hyun Jung; Eom, Hyo Jung; Park, Chulwoo; Jung, Jaejoon; Shin, Bora; Kim, Wook; Chung, Namhyun; Choi, In-Geol; Park, Woojun

2016-03-01

Microbially induced calcium carbonate precipitation (CCP) is a long-standing but re-emerging environmental engineering process for production of self-healing concrete, bioremediation, and long-term storage of CO2. CCP-capable bacteria, two Bacillus strains (JH3 and JH7) and one Sporosarcina strain (HYO08), were isolated from two samples of concrete and characterized phylogenetically. Calcium carbonate crystals precipitated by the three strains were morphologically distinct according to field emission scanning electron microscopy. Energy dispersive X-ray spectrometry mapping confirmed biomineralization via extracellular calcium carbonate production. The three strains differed in their physiological characteristics: growth at alkali pH and high NaCl concentrations, and urease activity. Sporosarcina sp. HYO08 and Bacillus sp. JH7 were more alkali- and halotolerant, respectively. Analysis of the community from the same concrete samples using barcoded pyrosequencing revealed that the relative abundance of Bacillus and Sporosarcina species was low, which indicated low culturability of other dominant bacteria. This study suggests that calcium carbonate crystals with different properties can be produced by various CCP-capable strains, and other novel isolates await discovery.

Dispersion and characterization of Thermoplastic Polyurethane/Multiwalled Carbon Nanotubes in co-rotative twin screw extruder

NASA Astrophysics Data System (ADS)

Benedito, Adolfo; Buezas, Ignacio; Giménez, Enrique; Galindo, Begoña

2010-06-01

The dispersion of multi-walled carbon nanotubes in thermoplastic polyurethanes has been done in co-rotative twin screw extruder through a melt blending process. A specific experimental design was prepared taking into account different compounding parameters such as feeding, temperature profile, screw speed, screw design, and carbon nanotube loading. The obtained samples were characterized by thermogravimetric analysis (TGA), light transmission microscopy, dynamic rheometry, and dynamic mechanical analysis. The objective of this work has been to study the dispersion quality of the carbon nanotubes and the effect of different compounding parameters to optimize them for industrial scale-up to final applications.

ASTM clustering for improving coal analysis by near-infrared spectroscopy.

PubMed

Andrés, J M; Bona, M T

2006-11-15

Multivariate analysis techniques have been applied to near-infrared (NIR) spectra coals to investigate the relationship between nine coal properties (moisture (%), ash (%), volatile matter (%), fixed carbon (%), heating value (kcal/kg), carbon (%), hydrogen (%), nitrogen (%) and sulphur (%)) and the corresponding predictor variables. In this work, a whole set of coal samples was grouped into six more homogeneous clusters following the ASTM reference method for classification prior to the application of calibration methods to each coal set. The results obtained showed a considerable improvement of the error determination compared with the calibration for the whole sample set. For some groups, the established calibrations approached the quality required by the ASTM/ISO norms for laboratory analysis. To predict property values for a new coal sample it is necessary the assignation of that sample to its respective group. Thus, the discrimination and classification ability of coal samples by Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) in the NIR range was also studied by applying Soft Independent Modelling of Class Analogy (SIMCA) and Linear Discriminant Analysis (LDA) techniques. Modelling of the groups by SIMCA led to overlapping models that cannot discriminate for unique classification. On the other hand, the application of Linear Discriminant Analysis improved the classification of the samples but not enough to be satisfactory for every group considered.

Thermal decomposition of alkane hydrocarbons inside a porous Ni anode for fuel supply of direct carbon fuel cell: Effects of morphology and crystallinity of carbon

NASA Astrophysics Data System (ADS)

Li, Chengguo; Yi, Hakgyu; Jalalabadi, Tahereh; Lee, Donggeun

2015-10-01

This study improved the physical contact between anode and fuel in a direct carbon fuel cell (DCFC) by directly generating carbon in a porous Ni anode through thermal decomposition of three kinds of hydrocarbons (CH4, C2H6, C3H8). From electron microscope observations of the carbon particles generated from each hydrocarbon, carbon spheres (CS), carbon nanotubes (CNT) and carbon nanofibers (CNF) were identified with increasing carbon number. Raman scattering analysis was performed to determine the crystallinity of the carbon samples. As a result, the carbon samples (CS, CNT, and CNF) produced from CH4, C2H6 and C3H8 were found to be less crystalline and more flexible with increasing the carbon number. DCFC performance was measured at 700 °C for the anode fueled with the same mass of the carbon sample. It was found that the 1-dimensional CNT and CNF were more active to produce 148% and 210% times higher power density than the CS. The difference was partly attributed to the finding that the less-crystalline CNT and CNF had much lower charge transfer resistances than the CS. A lifetime test found that the CNT and CNF, which are capable of transporting electrons for much longer periods, maintained the power density much longer, as compared to the CS which can lose their point contacts between the particles shortly at high current density.

Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Sanghapi, Hervé K.; Jain, Jinesh; Bol'shakov, Alexander; Lopano, Christina; McIntyre, Dustin; Russo, Richard

2016-08-01

In this study laser induced breakdown spectroscopy (LIBS) is used for elemental characterization of outcrop samples from the Marcellus Shale. Powdered samples were pressed to form pellets and used for LIBS analysis. Partial least squares regression (PLS-R) and univariate calibration curves were used for quantification of analytes. The matrix effect is substantially reduced using the partial least squares calibration method. Predicted results with LIBS are compared to ICP-OES results for Si, Al, Ti, Mg, and Ca. As for C, its results are compared to those obtained by a carbon analyzer. Relative errors of the LIBS measurements are in the range of 1.7 to 12.6%. The limits of detection (LODs) obtained for Si, Al, Ti, Mg and Ca are 60.9, 33.0, 15.6, 4.2 and 0.03 ppm, respectively. An LOD of 0.4 wt.% was obtained for carbon. This study shows that the LIBS method can provide a rapid analysis of shale samples and can potentially benefit depleted gas shale carbon storage research.

Salinity of the Eocene Arctic Ocean from oxygen isotope analysis of fish bone carbonate

NASA Astrophysics Data System (ADS)

Waddell, Lindsey M.; Moore, Theodore C.

2008-03-01

Stable isotope analysis was performed on the structural carbonate of fish bone apatite from early and early middle Eocene samples (˜55 to ˜45 Ma) recently recovered from the Lomonosov Ridge by Integrated Ocean Drilling Program Expedition 302 (the Arctic Coring Expedition). The δ18O values of the Eocene samples ranged from -6.84‰ to -2.96‰ Vienna Peedee belemnite, with a mean value of -4.89‰, compared to 2.77‰ for a Miocene sample in the overlying section. An average salinity of 21 to 25‰ was calculated for the Eocene Arctic, compared to 35‰ for the Miocene, with lower salinities during the Paleocene Eocene thermal maximum, the Azolla event at ˜48.7 Ma, and a third previously unidentified event at ˜47.6 Ma. At the Azolla event, where the organic carbon content of the sediment reaches a maximum, a positive δ13C excursion was observed, indicating unusually high productivity in the surface waters.

Determination of total carbonates in soil archaeometry using a new pressure method with temperature compensation

NASA Astrophysics Data System (ADS)

Barouchas, Pantelis; Koulos, Vasilios; Melfos, Vasilios

2017-04-01

For the determination of total carbonates in soil archaeometry a new technique was applied using a multi-sensor philosophy, which combines simultaneous measurement of pressure and temperature. This technology is innovative and complies with EN ISO 10693:2013, ASTM D4373-02(2007) and Soil Science Society of America standard test methods for calcium carbonate content in soils and sediments. The total carbonates analysis is based on a pressure method that utilizes the FOGII Digital Soil CalcimeterTM, which is a portable apparatus. The total carbonate content determined by treating a 1.000 g (+/- 0.001 g) dried sample specimens with 6N hydrochloric acid (HCL) reagent grade, in an enclosed reaction vessel. Carbon dioxide gas evolved during the reaction between the acid and carbonate fraction of the specimen, was measured by the resulting pressure generated, taking in account the temperature conditions during the reaction. Prior to analysis the procedure was validated with Sand/Soil mixtures from BIPEA proficiency testing program with soils of different origins. For applying this new method in archaeometry a total number of ten samples were used from various rocks which are related with cultural constructions and implements in Greece. They represent a large range of periods since the Neolithic times, and were selected because there was an uncertainty about their accurate mineralogical composition especially regarding the presence of carbonate minerals. The results were compared to the results from ELTRA CS580 inorganic carbon analyzer using an infrared cell. The determination of total carbonates for 10 samples from different ancient sites indicated a very good correlation (R2 >0.97) between the pressure method with temperature compensation and the infrared method. The proposed method is quickly and accurate in archaeometry and can replace easily other techniques for total carbonates testing. The FOGII Digital Soil CalcimeterTM is portable and easily can be carried for field work in archaeology.

Niche and neutral processes both shape community structure in parallelized, aerobic, single carbon-source enrichments

DOE Data Explorer

Flynn, Theodore M.; Koval, Jason C.; Greenwald, Stephanie M.; Owens, Sarah M.; Kemner, Kenneth M.; Antonopoulos, Dionysios A.

2017-01-01

We present DNA sequence data in FASTA-formatted files from aerobic environmental microcosms inoculated with a sole carbon source. DNA sequences are of 16S rRNA genes present in DNA extracted from each microcosm along with the environmental samples (soil, water) used to inoculate them. These samples were sequenced using the Illumina MiSeq platform at the Environmental Sample Preparation and Sequencing Facility at Argonne National Laboratory. This data is compatible with standard microbiome analysis pipelines (e.g., QIIME, mothur, etc.).

Natural cotton as precursor for the refractory boron carbide—a hydrothermal synthesis and characterization

NASA Astrophysics Data System (ADS)

Saritha Devi, H. V.; Swapna, M. S.; Raj, Vimal; Ambadas, G.; Sankararaman, S.

2018-01-01

Boron carbide (B4C) is an excellent covalent carbide that finds applications in industries and nuclear power plants. The present synthesis methods of boron carbide are expensive and involve the use of toxic chemicals that adversely affect environment. In the present work, we report for the first time the use of the hydrothermal method for converting the cellulose from cotton as the carbon precursor for B4C. The carbon precursor is converted into functionalized porous carbonaceous material by hydrothermal treatment followed by sodium borohydride. It is further treated with boric acid to make it a B4C precursor. The precursor is characterized by UV-visible diffuse reflectance, Raman, Fourier transform infrared, photoluminescent and energy dispersive spectroscopy. The morphology and structure analysis is carried out using field emission scanning electron microscopy and x-ray diffraction techniques. The results of structural and optical characterization of the sample synthesized are compared with the commercial B4C. The thermal stability of the sample is studied by thermogravimetric analysis. The sample annealed at 700 °C is found to be B4C devoid of amorphous carbon with a yield of 44.7%. The analysis reveals the formation of boron carbide from the sample.

Stable Isotope Dilution Assays for Clinical Analyses of Folates and Other One-Carbon Metabolites: Application to Folate-Deficiency Studies

PubMed Central

Kopp, Markus; Morisset, Rosalie; Koehler, Peter

2016-01-01

Folate deficiency is generally accepted as a potential direct or indirect risk factor for diseases including spina bifida, coronary heart diseases, malfunctions of the central nervous system, and cancer. The direct inclusion of folates in the methylation cycle, including the remethylation of homocysteine and regeneration of S-adenosylmethionine, underlines the importance of these vitamins and other components of one-carbon metabolism. Therefore, the aim of the present study was to develop a multiple stable isotope dilution assay (SIDA) for the respective analytes in plasma and tissue samples to allow for a closer look at the interaction between a severe folate deficiency and local folate status, as well as further interactions with circulating S-adenosylmethionine, S-adenosylhomocysteine, and homocysteine. The analytical methods were based on SIDAs coupled with liquid chromatography—tandem mass spectrometry (LC-MS/MS) analysis using the deuterated folates [2H4]-5-methyltetrahydrofolic acid, [2H4]-5-formyltetrahydrofolic acid, [2H4]-tetrahydrofolic acid, [2H4]-10-formylfolic acid, and [2H4]-folic acid and the deuterated one-carbon metabolites [2H4]-homocysteine, [2H4]-S-adenosylhomocysteine, and [2H3]-S-adenosylmethionine as internal standards. Three analytical methods have been developed for the analysis of homocysteine, S-adenosylmethionine, S-adenosylhomocysteine, and six folate vitamers. Validation data for the analysis of C1-metabolites in plasma and tissue samples or folate analysis in tissue samples revealed excellent sensitivity, precision, and recovery for all analytes studied. The miniaturized methods using sample volumes as low as 50 μL and weighed portions of 5–25 mg will allow the assessment of the status of folates and additional biomarkers of impaired one-carbon metabolism during folate deficiency. PMID:27276031

Spatially resolved δ13C analysis using laser ablation isotope ratio mass spectrometry

NASA Astrophysics Data System (ADS)

Moran, J.; Riha, K. M.; Nims, M. K.; Linley, T. J.; Hess, N. J.; Nico, P. S.

2014-12-01

Inherent geochemical, organic matter, and microbial heterogeneity over small spatial scales can complicate studies of carbon dynamics through soils. Stable isotope analysis has a strong history of helping track substrate turnover, delineate rhizosphere activity zones, and identifying transitions in vegetation cover, but most traditional isotope approaches are limited in spatial resolution by a combination of physical separation techniques (manual dissection) and IRMS instrument sensitivity. We coupled laser ablation sampling with isotope measurement via IRMS to enable spatially resolved analysis over solid surfaces. Once a targeted sample region is ablated the resulting particulates are entrained in a helium carrier gas and passed through a combustion reactor where carbon is converted to CO2. Cyrotrapping of the resulting CO2 enables a reduction in carrier gas flow which improves overall measurement sensitivity versus traditional, high flow sample introduction. Currently we are performing sample analysis at 50 μm resolution, require 65 ng C per analysis, and achieve measurement precision consistent with other continuous flow techniques. We will discuss applications of the laser ablation IRMS (LA-IRMS) system to microbial communities and fish ecology studies to demonstrate the merits of this technique and how similar analytical approaches can be transitioned to soil systems. Preliminary efforts at analyzing soil samples will be used to highlight strengths and limitations of the LA-IRMS approach, paying particular attention to sample preparation requirements, spatial resolution, sample analysis time, and the types of questions most conducive to analysis via LA-IRMS.

Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

PubMed

Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

2013-10-21

A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

Ion beam promoted lithium absorption in glassy polymeric carbon

NASA Astrophysics Data System (ADS)

Zimmerman, R. L.; Ila, D.; Jenkins, G. M.; Maleki, H.; Poker, D. B.

1995-12-01

Glassy Polymeric Carbon (GPC) samples prepared from a precursor possess accessible pore volume that depends on the heat treatment temperature [G.M. Jenkins and K. Kawamura, Polymeric Carbons - Carbon Fiber, Glass and Char (Cambridge University Press, Cambridge, 1976) p. 140]. We have shown that lithium percolates without diffusion into the accessible pores of GPC samples immersed in a molten lithium salt bath at 700°C [D. Ila, G.M. Jenkins, L.R. Holland, A.L. Evelyn and H. Jena, Vacuum 45 (1994) 451]. Ion bombardment with 10 MeV Au atoms increases the total pore volume available for lithium occupation even for samples normally impermeable to lithium. The lithium concentration depth profile is measured using Li 7(p,2α) nuclear reaction analysis. We will report on lithium percolation into GPC prepared at temperatures between 500°C and 1000°C and activated by a 10 MeV gold ion bombardment.

Fractal and spectroscopic analysis of soot from internal combustion engines

NASA Astrophysics Data System (ADS)

Swapna, M. S.; Saritha Devi, H. V.; Raj, Vimal; Sankararaman, S.

2018-03-01

Today diesel engines are used worldwide for various applications and very importantly in transportation. Hydrocarbons are the most widespread precursors among carbon sources employed in the production of carbon nanotubes (CNTs). The aging of internal combustion engine is an important parameter in deciding the carbon emission and particulate matter due to incomplete combustion of fuel. In the present work, an attempt has been made for the effective utilization of the aged engines for potential applicationapplications in fuel cells and nanoelectronics. To analyze the impact of aging, the particulate matter rich in carbon content areis collected from diesel engines of different ages. The soot with CNTs is purified by the liquid phase oxidation method and analyzed by Field Emission Scanning Electron Microscopy, High-Resolution Transmission Electron Microscopy, Energy Dispersive Spectroscopy, UV-Visible spectroscopy, Raman spectroscopy and Thermogravimetric analysis. The SEM image contains self-similar patterns probing fractal analysis. The fractal dimensions of the samples are determined by the box counting method. We could find a greater amount of single-walled carbon nanotubes (SWCNTs) in the particulate matter emitted by aged diesel engines and thereby giving information about the combustion efficiency of the engine. The SWCNT rich sample finds a wide range of applicationapplications in nanoelectronics and thereby pointing a potential use of these aged engines.

Distribution, Sources, and Association of Polycyclic Aromatic Hydrocarbons, Black Carbon, and Total Organic Carbon in Size-Segregated Soil Samples Along a Background–Urban–Rural Transect

PubMed Central

Ray, Sharmila; Khillare, Pandit Sudan; Kim, Ki-Hyun; Brown, Richard J.C.

2012-01-01

Abstract Soil samples were collected over a year-long period along a background–urban–rural transect in Delhi, India for the analysis of polycyclic aromatic hydrocarbons (PAHs), black carbon (BC), and total organic carbon (TOC) in five grain size fractions, x, in μm of 0≤x<53 (I), 53≤x<250 (II), 250≤x<500 (III), 500≤x<2000 (IV), and their sum (total: T). Maximum concentrations of PAH, BC, and TOC were observed in the smallest fraction (I) comprising silt and clay, irrespective of site or season. Results of the molecular diagnostic ratios and principal component analysis (PCA) identified coal, wood, biomass burning, and vehicular emissions as major sources of PAHs at all the three sites, while BC/TOC ratios pointed toward biomass combustion as the chief source of carbonaceous species. This work presents the first such rural-urban transect study considering PAH, BC, and TOC in soil. PMID:23133309

Storage effects on quantity and composition of dissolved organic carbon and nitrogen of lake water, leaf leachate and peat soil water.

PubMed

Heinz, Marlen; Zak, Dominik

2018-03-01

This study aimed to evaluate the effects of freezing and cold storage at 4 °C on bulk dissolved organic carbon (DOC) and nitrogen (DON) concentration and SEC fractions determined with size exclusion chromatography (SEC), as well as on spectral properties of dissolved organic matter (DOM) analyzed with fluorescence spectroscopy. In order to account for differences in DOM composition and source we analyzed storage effects for three different sample types, including a lake water sample representing freshwater DOM, a leaf litter leachate of Phragmites australis representing a terrestrial, 'fresh' DOM source and peatland porewater samples. According to our findings one week of cold storage can bias DOC and DON determination. Overall, the determination of DOC and DON concentration with SEC analysis for all three sample types were little susceptible to alterations due to freezing. The findings derived for the sampling locations investigated here may not apply for other sampling locations and/or sample types. However, DOC size fractions and DON concentration of formerly frozen samples should be interpreted with caution when sample concentrations are high. Alteration of some optical properties (HIX and SUVA 254 ) due to freezing were evident, and therefore we recommend immediate analysis of samples for spectral analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterisation of Dissolved Organic Carbon by Thermal Desorption - Proton Transfer Reaction - Mass Spectrometry

NASA Astrophysics Data System (ADS)

Materić, Dušan; Peacock, Mike; Kent, Matthew; Cook, Sarah; Gauci, Vincent; Röckmann, Thomas; Holzinger, Rupert

2017-04-01

Dissolved organic carbon (DOC) is an integral component of the global carbon cycle. DOC represents an important terrestrial carbon loss as it is broken down both biologically and photochemically, resulting in the release of carbon dioxide (CO2) to the atmosphere. The magnitude of this carbon loss can be affected by land management (e.g. drainage). Furthermore, DOC affects autotrophic and heterotrophic processes in aquatic ecosystems, and, when chlorinated during water treatment, can lead to the release of harmful trihalomethanes. Numerous methods have been used to characterise DOC. The most accessible of these use absorbance and fluorescence properties to make inferences about chemical composition, whilst high-performance size exclusion chromatography can be used to determine apparent molecular weight. XAD fractionation has been extensively used to separate out hydrophilic and hydrophobic components. Thermochemolysis or pyrolysis Gas Chromatography - Mass Spectrometry (GC-MS) give information on molecular properties of DOC, and 13C NMR spectroscopy can provide an insight into the degree of aromaticity. Proton Transfer Reaction - Mass Spectrometry (PTR-MS) is a sensitive, soft ionisation method suitable for qualitative and quantitative analysis of volatile and semi-volatile organic vapours. So far, PTR-MS has been used in various environmental applications such as real-time monitoring of volatile organic compounds (VOCs) emitted from natural and anthropogenic sources, chemical composition measurements of aerosols etc. However, as the method is not compatible with water, it has not been used for analysis of organic traces present in natural water samples. The aim of this work was to develop a method based on thermal desorption PTR-MS to analyse water samples in order to characterise chemical composition of dissolved organic carbon. We developed a clean low-pressure evaporation/sublimation system to remove water from samples and thermal desorption system to introduce the samples to the PTR-MS. With thermal desorption lasting just 5 min (at 200˚ C) we successfully detected more than 200 organic ions in the water samples yielding up to 800 ng/mL in total (which corresponds to 1.5% of total DOC present in the sample). Samples were from tropical peatlands in Borneo and Malaysia. Principle component analysis showed a clear separation of the samples when comparing intact and degraded peat swamp forest, and between an oil palm plantation and natural forest. This suggests that the degradation and conversion of tropical peatlands result in distinct changes to DOC composition, with possible implications for associated CO2 emissions. As the method is sensitive and reproducible it has wide potential application in the characterisation of water and of soils. It could provide important information on how land management, microbial activity, vegetation and water treatment control the chemical composition of DOC.

Qualitative analysis of Pb liquid sample using laser-induced breakdown spectroscopy (LIBS)

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

Suyanto, Hery; Rupiasih, Ni Nyoman; Winardi, T. B.

2013-09-03

Qualitative analysis of liquid sample containing 1,000 ppm of Pb was performed by using LIBS technique. In order to avoid splashing off of the liquid sample during laser irradiation, a sample pretreatment was done, namely the liquid sample was absorbed by using commercial available stomach medicine. Two kinds of absorbent materials were chosen in this experiment, first containing 125 mg activated carbon and second 600 mg activated attapulgite. These absorbent materials were used since carbon sample gives better absorption of infrared laser irradiation used in this experiment. In order to characterize the absorption process, three treatments were conducted in thismore » experiment; first, without heating the sample but varying the absorption time before laser irradiation; second by varying the heating temperature after certain time of absorption process and third by varying the temperature only. The maximum emission intensity of Pb I 405.7 nm was found in the second treatment of heating the sample till 85°C after 30 minutes absorption of the liquid sample in both absorbent materials.« less

Characterization of fly ash from low-sulfur and high-sulfur coal sources: Partitioning of carbon and trace elements with particle size

USGS Publications Warehouse

Hower, J.C.; Trimble, A.S.; Eble, C.F.; Palmer, C.A.; Kolker, A.

1999-01-01

Fly ash samples were collected in November and December of 1994, from generating units at a Kentucky power station using high- and low-sulfur feed coals. The samples are part of a two-year study of the coal and coal combustion byproducts from the power station. The ashes were wet screened at 100, 200, 325, and 500 mesh (150, 75, 42, and 25 ??m, respectively). The size fractions were then dried, weighed, split for petrographic and chemical analysis, and analyzed for ash yield and carbon content. The low-sulfur "heavy side" and "light side" ashes each have a similar size distribution in the November samples. In contrast, the December fly ashes showed the trend observed in later months, the light-side ash being finer (over 20 % more ash in the -500 mesh [-25 ??m] fraction) than the heavy-side ash. Carbon tended to be concentrated in the coarse fractions in the December samples. The dominance of the -325 mesh (-42 ??m) fractions in the overall size analysis implies, though, that carbon in the fine sizes may be an important consideration in the utilization of the fly ash. Element partitioning follows several patterns. Volatile elements, such as Zn and As, are enriched in the finer sizes, particularly in fly ashes collected at cooler, light-side electrostatic precipitator (ESP) temperatures. The latter trend is a function of precipitation at the cooler-ESP temperatures and of increasing concentration with the increased surface area of the finest fraction. Mercury concentrations are higher in high-carbon fly ashes, suggesting Hg adsorption on the fly ash carbon. Ni and Cr are associated, in part, with the spinel minerals in the fly ash. Copyright ?? 1999 Taylor & Francis.

Carbon and oxygen isotope ratios of ecosystem respiration along an Oregon conifer transect: preliminary observations based on small-flask sampling.

PubMed

Ehleringer, J. R.; Cook, C. S.

1998-01-01

Isotope ratio analyses of atmospheric CO(2) at natural abundance have significant potential for contributing to our understanding of photosynthetic and respiration processes in forest ecosystems. Recent advances in isotope ratio mass spectrometry allow for rapid, on-line analysis of small volumes of CO(2) in air, and open new research opportunities at the ecophysiological, whole-organism, and atmospheric levels. Among the immediate applications are the carbon and oxygen isotope ratio analyses of carbon dioxide in atmospheric air. Routine analysis of carbon dioxide in air volumes of approximately 50-300 &mgr;l is accomplished by linking a commercially available, trace gas condenser and gas chromatograph to an isotope ratio mass spectrometer operated in continuous-flow mode. Samples collected in the field are stored in either gas-tight syringes or 100-ml flasks. The small sample volume required makes it possible to subsample the air in flasks for CO(2) and then to sample the remaining air volume for the analysis of the isotopic composition of either methane or nitrous oxide. Reliable delta(13)C and delta(18)O values can be obtained from samples collected and stored for 1-3 days. Longer-term storage, on the order of weeks, is possible for delta(13)C measurements without drift in the isotope ratio signal, and should also be possible for delta(18)O measurements. When linked with an infrared gas analyzer, pump and flask sampling system, it is feasible to sample CO(2) extensively in remote forest locations. The air-sampling system was used to measure the isotope ratios of atmospheric CO(2) and to conduct a regression analysis of the relationship between these two parameters. From the regression, we calculated the delta(13)C of ecosystem respiration of four coniferous ecosystems along a precipitation gradient in central Oregon. The ecosystems along the coast-to-interior Oregon (OTTER) gradient are dominated by spruce-hemlock forests at the wet, coastal sites (> 200 cm precipitation annually) to juniper woodlands (20 cm precipitation) at the interior, dry end of the transect. The delta(13)C values of ecosystem respiration along this transect differed by only 1.3 per thousand (range of -25.2 to -23.9 per thousand ) during August at the peak of the summer drought. Following autumn rains in September, the delta(13)C of ecosystem respiration in the four stands decreased; overall the difference in the carbon isotope ratio of ecosystem respiration among sites increased to 3.9 per thousand (-26.8 to -22.9 per thousand ).

Interference of oxygen, carbon dioxide, and water vapor on the analysis for oxides of nitrogen by chemiluminescence

NASA Technical Reports Server (NTRS)

Maahs, H. G.

1975-01-01

The interference of small concentrations (less than 4 percent by volume) of oxygen, carbon dioxide, and water vapor on the analysis for oxides of nitrogen by chemiluminescence was measured. The sample gas consisted primarily of nitrogen, with less than 100 parts per million concentration of nitric oxide, and with small concentrations of oxygen, carbon dioxide, and water vapor added. Results obtained under these conditions indicate that although oxygen does not measurably affect the analysis for nitric oxide, the presence of carbon dioxide and water vapor causes the indicated nitric oxide concentration to be too low. An interference factor - defined as the percentage change in indicated nitric oxide concentration (relative to the true nitric oxide concentration) divided by the percent interfering gas present - was determined for carbon dioxide to be -0.60 + or - 0.04 and for water vapor to be -2.1 + or - 0.3.

Designing a dynamic data driven application system for estimating real-time load of dissolved organic carbon in a river

Treesearch

Ying Ouyang

2012-01-01

Understanding the dynamics of naturally occurring dissolved organic carbon (DOC) in a river is central to estimating surface water quality, aquatic carbon cycling, and global climate change. Currently, determination of the DOC in surface water is primarily accomplished by manually collecting samples for laboratory analysis, which requires at least 24 h. In other words...

Studying the impact of air/brine displacement on acoustic velocities in carbonates. El Amin Mokhtar and Sandra Vega

NASA Astrophysics Data System (ADS)

Mokhtar, E.; Vega, D.

2012-12-01

The impact of air/brine displacement on acoustic velocities of carbonate rocks is not fully comprehended yet. In order to improve our understanding of this effect, we conducted laboratory measurements of porosity and acoustic velocities (Vp and Vs) under both dry and brine saturated conditions at ambient pressure and temperature. The core plug samples in this study were collected from a hydrocarbon reservoir in the Middle East. A petrographic analysis was also performed on thin sections taken from the core plugs using a microscope and a digital camera. The aim of this analysis was to study depositional facies and the extent of diagenetic overprint that caused the observed variations in rock fabrics. Cross-plots were generated to analyze the trends of behavior between acoustic velocities and porosities taking into account the influence of different rock fabrics, in both dry and brine saturated samples. Acoustic velocities of brine saturated samples were higher than velocities of dry samples, as expected. However, their differences also respond to both, total porosity and carbonate rock fabrics. This result can be attributed to the different carbonate pore structures and rock frames formed during deposition and diagenesis. Similarly, the Vp/Vs ratio cross-plots display an increase in Vp/Vs ratios for the brine saturated samples compared to the dry ones. In conclusion, differences in acoustic velocities between dry and brine saturated carbonate rocks seem to be highly effected by porosity, rock fabric, and fluid content. This information can help to better understand the differences in acoustic response between gas and brine saturated zones in well logs and seismic.

Factors affecting the behavior of unburned carbon upon steam activation

NASA Astrophysics Data System (ADS)

Lu, Zhe

The main objective of this study is to investigate the factors that could affect the behavior of unburned carbon samples upon steam activation. Through this work, the relationships among the factors that could influence the carbon-steam reaction with the surface area of the produced activated carbon were explored. Statistical analysis was used to relate the chemical and physical properties of the unburned carbon to the surface area of the activated carbon. Six unburned carbons were selected as feedstocks for activated carbon, and marked as UCA through UCF. The unburned carbons were activated using steam at 850°C for 90 minutes, and the surface areas of their activated counterparts were measured using N2 adsorption isotherms at 77K. The activated carbons produced from different unburned carbon precursors presented different surface areas at similar carbon burn-off levels. Moreover, in different carbon burn-off regions, the sequences for surface area of activated carbons from different unburned carbon samples were different. The factors that may affect the carbon-steam gasification reactions, including the concentration of carbon active sites, the crystallite size of the carbon, the intrinsic porous structure of carbon, and the inorganic impurities, were investigated. All unburned carbons investigated in this study were similar in that they showed the very broad (002) and (10 ) carbon peaks, which are characteristic of highly disordered carbonaceous materials. In this study, the unburned carbon samples contained about 17--48% of inorganic impurities. Compared to coals, the unburned carbon samples contain a larger amount of inorganic impurities as a result of the burn-off, or at lease part, of the carbon during the combustion process. These inorganic particles were divided into two groups in terms of the way they are associated with carbon particles: free single particles, and particles combined with carbon particles. As indicated from the present work, unburned carbons with one of the following properties will produce activated carbons with high surface areas. These properties include: (a) large amount of O2 chemisorption capacity; (b) high concentration of surface C-O complex; and (c) small crystallite diameter; (d) high concentration of Na+K particles that are combined with carbon; (e) high concentration of isotropic carbon. (Abstract shortened by UMI.)

Evaluation of DNA extraction methods for the analysis of microbial community in biological activated carbon.

PubMed

Zheng, Lu; Gao, Naiyun; Deng, Yang

2012-01-01

It is difficult to isolate DNA from biological activated carbon (BAC) samples used in water treatment plants, owing to the scarcity of microorganisms in BAC samples. The aim of this study was to identify DNA extraction methods suitable for a long-term, comprehensive ecological analysis of BAC microbial communities. To identify a procedure that can produce high molecular weight DNA, maximizes detectable diversity and is relatively free from contaminants, the microwave extraction method, the cetyltrimethylammonium bromide (CTAB) extraction method, a commercial DNA extraction kit, and the ultrasonic extraction method were used for the extraction of DNA from BAC samples. Spectrophotometry, agarose gel electrophoresis and polymerase chain reaction (PCR)-restriction fragment length polymorphisms (RFLP) analysis were conducted to compare the yield and quality of DNA obtained using these methods. The results showed that the CTAB method produce the highest yield and genetic diversity of DNA from BAC samples, but DNA purity was slightly less than that obtained with the DNA extraction-kit method. This study provides a theoretical basis for establishing and selecting DNA extraction methods for BAC samples.

Quantitative ion beam analysis of M-C-O systems: application to an oxidized uranium carbide sample

NASA Astrophysics Data System (ADS)

Martin, G.; Raveu, G.; Garcia, P.; Carlot, G.; Khodja, H.; Vickridge, I.; Barthe, M. F.; Sauvage, T.

2014-04-01

A large variety of materials contain both carbon and oxygen atoms, in particular oxidized carbides, carbon alloys (as ZrC, UC, steels, etc.), and oxycarbide compounds (SiCO glasses, TiCO, etc.). Here a new ion beam analysis methodology is described which enables quantification of elemental composition and oxygen concentration profile over a few microns. It is based on two procedures. The first, relative to the experimental configuration relies on a specific detection setup which is original in that it enables the separation of the carbon and oxygen NRA signals. The second concerns the data analysis procedure i.e. the method for deriving the elemental composition from the particle energy spectrum. It is a generic algorithm and is here successfully applied to characterize an oxidized uranium carbide sample, developed as a potential fuel for generation IV nuclear reactors. Furthermore, a micro-beam was used to simultaneously determine the local elemental composition and oxygen concentration profiles over the first microns below the sample surface. This method is adapted to the determination of the composition of M?C?O? compounds with a sensitivity on elemental atomic concentrations around 1000 ppm.

Detailed description of oil shale organic and mineralogical heterogeneity via fourier transform infrared mircoscopy

USGS Publications Warehouse

Washburn, Kathryn E.; Birdwell, Justin E.; Foster, Michael; Gutierrez, Fernando

2015-01-01

Mineralogical and geochemical information on reservoir and source rocks is necessary to assess and produce from petroleum systems. The standard methods in the petroleum industry for obtaining these properties are bulk measurements on homogenized, generally crushed, and pulverized rock samples and can take from hours to days to perform. New methods using Fourier transform infrared (FTIR) spectroscopy have been developed to more rapidly obtain information on mineralogy and geochemistry. However, these methods are also typically performed on bulk, homogenized samples. We present a new approach to rock sample characterization incorporating multivariate analysis and FTIR microscopy to provide non-destructive, spatially resolved mineralogy and geochemistry on whole rock samples. We are able to predict bulk mineralogy and organic carbon content within the same margin of error as standard characterization techniques, including X-ray diffraction (XRD) and total organic carbon (TOC) analysis. Validation of the method was performed using two oil shale samples from the Green River Formation in the Piceance Basin with differing sedimentary structures. One sample represents laminated Green River oil shales, and the other is representative of oil shale breccia. The FTIR microscopy results on the oil shales agree with XRD and LECO TOC data from the homogenized samples but also give additional detail regarding sample heterogeneity by providing information on the distribution of mineral phases and organic content. While measurements for this study were performed on oil shales, the method could also be applied to other geological samples, such as other mudrocks, complex carbonates, and soils.

Pore structure of raw and purified HiPco single-walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Cinke, Martin; Li, Jing; Chen, Bin; Cassell, Alan; Delzeit, Lance; Han, Jie; Meyyappan, M.

2002-10-01

Very high purity single-walled carbon nanotubes (SWNTs) were obtained from HiPco SWNT samples containing Fe particles by a two-step purification process. The raw and purified samples were characterized using high resolution transmission electron microscopy (HRTEM), Raman spectroscopy and thermogravimetric analysis (TGA). The purified sample consists of ˜0.4% Fe and the process does not seem to introduce any additional defects. The N 2 adsorption isotherm studies at 77 K reveal that the total surface area of the purified sample increases to 1587 m 2/g from 567 m 2/g for the raw material, which is the highest value reported for SWNTs.

Bulk and compound-specific isotope analysis of long-chain n-alkanes from a 85,000 year sediment core from Lake Peten Petén Itzá, Guatemala

NASA Astrophysics Data System (ADS)

Mays, J.; Brenner, M.; Curtis, J. H.; Curtis, K.; Hodell, D. A.; Correa-Metrio, A.; Escobar, J.; Dutton, A. L.; Zimmerman, A. R.; Guilderson, T. P.

2013-12-01

Sediment core PI-6 from Lake Petén Itzá, Guatemala possesses an 85-ka record of climate from lowland Central America. Variations in sediment lithology suggest large, abrupt changes in precipitation during the last glacial and deglacial periods, and into the early Holocene. Study of cores from nearby Lake Quexil demonstrated the utility of using the carbon isotopic composition of leaf wax n-alkanes to infer changes in terrestrial vegetation (Huang et al. 2001). Forty-nine samples were taken from composite Petén Itzá core PI-6 to measure carbon isotopes of bulk organic carbon and long-chain n alkanes. Changes in δ13C values indicate shifts in the relative proportion of C3 to C4 biomass. The record shows largest δ13C variations are associated with Heinrich Events. Carbon isotope values in sediments deposited during the Last Glacial Maximum (LGM) indicate moderate precipitation and little rainfall fluctuation. The deglacial was a period of pronounced climate variability, e.g. the Bölling-Allerod and Younger Dryas. Arid times of the deglacial were inferred from samples with the greatest δ13C values in organic matter, reflecting the largest proportion of C4 plants. Such inferences are supported by stable isotope measurements on ostracod shells and analysis of pollen from the same sample depths in core PI-6. Carbon stable isotope measures on bulk organic carbon and n alkane compounds show similar trends throughout the record and the C:N ratio of Petén Itzá sediments indicates a predominantly allochthonous source for bulk organic matter. Hence, isotope measures on bulk organic carbon (δ13CTOC) in sediments from this lake are sufficient to infer climate-driven shifts in vegetation, making n-alkane extraction and isotope analysis superfluous.

Quantification of airborne fossil and biomass carbonylic carbon by combined radiocarbon and liquid chromatography mass spectrometry

NASA Astrophysics Data System (ADS)

Larsen, B. R.; Tudos, A.; Slanina, J.; Van der Borg, K.; Kotzias, D.

Airborne carbonyl compounds have been sampled at three European semi-remote to semi-urban test sites for radiocarbon ( 14C) analysis. The used methodology included collection on 2,4-dinitrophenylhydrazine coated silica gel cartridges, chromatographic isolation of the formed hydrazones, combustion into CO 2, reduction into graphite followed by accelerator mass spectrometry. In combination with this, liquid chromatography coupled to atmospheric pressure chemical ionisation mass spectrometry was used for chemical speciation of the collected carbonyls. At all sites the carbonyls were found to be of a mixed biogenic/anthropogenic origin. The determining factor for the proportion of fossil (anthropogenic) carbon in the samples was the vicinity of urban sources for carbonyls and their photochemical precursors. At meteorological conditions, which gave the test sites semi-rural/semi-remote characteristics the samples contained an average of 24% (range: 10-34%) of fossil carbonylic carbon. When air masses were transported from urban areas to the test-sites significantly higher proportions of fossil carbonylic carbon were determined with a maximum of 61%. Principal component analysis on this limited data set indicated that a low fossil proportion of carbonylic carbon is associated with high proportions of acetaldehyde, acetone, pentanone and acrolein. Until further radicarbon studies are carried out the conclusion remains that for the carbonyl compounds measured European background levels are of a predominant biogenic origin.

[Preparation of a novel activated carbon coating fiber for solid phase micro-extraction and its application for halocarbon compound analysis in water].

PubMed

Wang, Shutao; Wang, Yan; You, Hong; Liang, Zhihua

2004-09-01

A novel activated carbon coating fiber used for solid phase micro-extraction (SPME) was prepared using activated carbon powder and silica resin adhesive. The extraction properties of the novel activated carbon coating fiber were investigated. The results indicate that this coating fiber has high concentration ability, with enrichment factors for chloroform, carbon tetrachloride, trichloroethylene and tetrachloroethylene in the range of 13.8 to 18.7. The fiber is stable at temperature as high as 290 degrees C and it can be used for over 140 times at 250 degrees C. The activated carbon coating fiber was then applied to the analysis of the four halocarbon compounds mentioned above. A linear correlation with correlation coefficients between 0.995 2 and 0.999 4 and the detection limits between 0.008 and 0.05 microg/L were observed. The method was also applied to a real water sample analysis and the recoveries of these halocarbon compounds were from 95.5% to 104.6%.

Riverine Carbon and the Sedimentary Record on the Continental Shelves

DTIC Science & Technology

2005-09-30

focused on the Gulf of Lions: collecting sediment samples and carrying out elemental and stable carbon isotopic analysis . The field work was carried...organisms. For example, the predominance of nitrogen-free biomacromolecules (e.g. tannin , lignin, cellulose, cutin and suberin) over proteins (C:N ≈ 3-4...are cooperating with J. Fabres and A. Calafat (CRG Marine Geosciences) in carrying out elemental and isotopic analysis on suspended material

δ13C and δ18O measurements of carbonate rocks using Cavity Ring-Down Spectroscopy

NASA Astrophysics Data System (ADS)

Lucic, G.; Kim-Hak, D.; Curtis, J. H.

2017-12-01

We present a novel, user friendly and cost effective method for the analysis of δ13C and δ18O in CO2 gas obtained from acid digestion of carbonate rocks. 2 to 3 milligrams of pure carbonate, ground to a powder, is digested in a pre-evacuated glass vial using 100% phosphoric acid at 70° C. Vials with the reacted samples are then loaded onto an automated carousel sampler where produced CO2 gas in the headspace is extracted and sent to a Picarro CRDS isotopic C and O analyzer. Once loaded onto the carousel, 49 samples may be analyzed automatically at a rate of one sample every 15 minutes. δ13C and δ18O of the sample are reported in real time with a precision of 0.2 and 0.4 per mil, respectively. The portability and simplicity of the autosampler and CRDS setup opens up potential for permanent and mobile deployments, enabling near-realtime sampling feedback in the lab or on the go in the field. Consumable and operating costs are small when compared to other technology in use, making the CRDS-Carbonate system suitable for large and small research labs. Finally, we present a summary results from a series of validation tests in which standards and natural carbonate rock samples were analyzed and compared to traditional Kiel-IRMS results.

Breakdown Characteristic Analysis of Paper- Oil Insulation under AC and DC Voltage

NASA Astrophysics Data System (ADS)

Anuar, N. F.; Jamail, N. A. M.; Rahman, R. A.; Kamarudin, M. S.

2017-08-01

This paper presents the study of breakdown characteristic of Kraft paper insulated with two different types of insulating fluid, which are Palm oil and Coconut oil. Palm oil and Coconut oil are chosen as the alternative fluid to the transformer oil because it has high potential and environmentally-friendly. The Segezha Kraft papers with various thicknesses (65.5 gsm, 75 gsm, 85gsm, 90 gsm) have been used in this research. High Voltage Direct Current (HVDC), High Voltage Alternating Current (HVAC) and carbon track and severity analysis is conducted to observe the sample of aging Kraft paper. These samples have been immersed using Palm oil and Coconut oil up to 90 days to observe the absorption rate. All samples started to reach saturation level at 70 days of immersion. HVDC and HVAC breakdown experiments have been done after the samples had reached the saturation level based on normal condition, immersed in Palm oil and immersed in Coconut oil. All samples immersed in liquid show different breakdown voltage reading compared to normal condition. The analysis of carbon track and severity on surface has been done using Analytical Scanning Electron Microscope (SEM) Analysis. The results of the experiment show that the sample of Kraft paper immersed in Palm oil was better than Coconut oil immersed sample. Therefore the sample condition was the main factor that determines the value of breakdown voltage test. Introduction

Dielectric and microstructure properties of polymer carbon black composites

NASA Astrophysics Data System (ADS)

Brosseau, C.; Boulic, F.; Queffelec, P.; Bourbigot, C.; Le Mest, Y.; Loaec, J.; Beroual, A.

1997-01-01

Dielectric and physicochemical properties of a composite material prepared by incorporating carbon black particles into a polymer matrix were investigated. Two types of carbon blacks, having very different structures of aggregates, were used. The volume fraction of the carbon blacks ranged from 0.2% to 7%, i.e. below and above the percolation threshold concentration observed from the measurements of dc conductivity. The composite samples were characterized in terms of: swelling by a compatible solvent, electron paramagnetic resonance (EPR) response, and frequency variation of permittivity. First, the article attempts to evaluate the diffusion coefficient of an appropriate solvent in these materials. Sorption kinetics experiments with toluene indicate that the initial uptake of solvent exhibits a square root dependence in time as a consequence of Fick's law and permit to evaluate the effective diffusion coefficient in the range 10-11-10-12 m2 s-1 depending on the volume fraction of the carbon black in the sample. Second, the analysis of the carbon black concentration dependence of the intensity and linewidth of the EPR signals indicates that EPR is an important experimental probe of the structure of the elasticity network. The most notable feature of the present work is that we find a correlation of the percolation threshold concentration which is detected from the dc electrical conductivity with moments of the EPR lines. The conclusions on the elasticity networks deduced from swelling measurements are confirmed by EPR data carried out on swollen samples. On qualitative grounds the role of the specific surface of carbon black is further analyzed. It is suggested that the elasticity network is mainly controlled by secondary (respectively primary) aggregates for samples containing low (respectively high) specific surface carbon blacks. Last, the article reports precise experimental data on the permittivity of these composite materials as a function of frequency. Thanks to a sensitive measurement technique using an impedance analyzer, we are able to measure the complex permittivity and permeability values of the samples in the frequency range from 108 to 1010 Hz. It is found that the real part of the permittivity is a function of frequency f, via a power law expression ɛ'=af-b, where a and b are two parameters depending upon carbon black concentration, in the range of frequency investigated. The data analysis reaffirms the result that percolation threshold is a key parameter for characterizing the topological arrangement in these structures.

Behavior of Quartz and Carbon Black Pellets at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Li, Fei; Tangstad, Merete

This paper studies the quartz and carbon black pellets at elevated temperature with varying temperature and gas atmosphere. High-purity quartz and commercial ultra-pure carbon black was mixed (carbon content vet. 15%), and then pelletized into particles of l-3mm in diameter. The stoichiometric analysis of the pellet during heating is studied in thermogravimetric analysis (TGA) furnace at different temperature in CO and Ar atmosphere. The microstructure, phase changes and element content of sample before/after heating is characterized by X-ray diffraction, scanning electron microscope, X-ray fluorescence and LECO analyzer. The reaction process can be divided into two stages. Higher temperature and argon atmosphere are the positive parameters for SiC formation.

Carbon nanodots as a matrix for the analysis of low-molecular-weight molecules in both positive- and negative-ion matrix-assisted laser desorption/ionization time-of-flight mass spectrometry and quantification of glucose and uric acid in real samples.

PubMed

Chen, Suming; Zheng, Huzhi; Wang, Jianing; Hou, Jian; He, Qing; Liu, Huihui; Xiong, Caiqiao; Kong, Xianglei; Nie, Zongxiu

2013-07-16

Carbon nanodots were applied for the first time as a new matrix for the analysis of low-molecular-weight compounds by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) in both positive- and negative-ion modes. A wide range of small molecules including amino acids, peptides, fatty acids, as well as β-agonists and neutral oligosaccharides were analyzed by MALDI MS with carbon nanodots as the matrix, and the lowest 0.2 fmol limits-of-detection were obtained for octadecanoic acid. Clear sodium and potassium adducts and deprotonated signals were produced in positive- and negative-ion modes. Furthermore, the glucose and uric acid in real samples were quantitatively determined by the internal standard method with the linear range of 0.5-9 mM and 0.1-1.8 mM (R(2) > 0.999), respectively. This work gives new insight into the application of carbon nanodots and provides a general approach for rapid analysis of low-molecular-weight compounds.

Carbon-13 and proton nuclear magnetic resonance analysis of shale-derived refinery products and jet fuels and of experimental referee broadened-specification jet fuels

NASA Technical Reports Server (NTRS)

Dalling, D. K.; Bailey, B. K.; Pugmire, R. J.

1984-01-01

A proton and carbon-13 nuclear magnetic resonance (NMR) study was conducted of Ashland shale oil refinery products, experimental referee broadened-specification jet fuels, and of related isoprenoid model compounds. Supercritical fluid chromatography techniques using carbon dioxide were developed on a preparative scale, so that samples could be quantitatively separated into saturates and aromatic fractions for study by NMR. An optimized average parameter treatment was developed, and the NMR results were analyzed in terms of the resulting average parameters; formulation of model mixtures was demonstrated. Application of novel spectroscopic techniques to fuel samples was investigated.

Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

PubMed

Jafari, Mohammad T; Riahi, Farhad

2014-05-23

The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS. Copyright © 2014 Elsevier B.V. All rights reserved.

Searching for Reduced Carbon on the Surface of Mars: The SAM Combustion Experiment

NASA Astrophysics Data System (ADS)

Stern, J. C.; Malespin, C. A.; Mahaffy, P. R.; Webster, C. R.; Eigenbrode, J. L.; Archer, P. D.; Brunner, A. E.; Freissinet, C.; Franz, H. B.; Glavin, D. P.; Graham, H. V.; McAdam, A. C.; Ming, D. W.; Navarro-Gonzalez, R.; Niles, P. B.; Steele, A.; Sutter, B.; Trainer, M. G.; MSL Science Team

2014-07-01

The SAM Combustion Experiment combusts reduced materials in solid samples for oxidized species quantification and C and H isotopic analysis of CO2 and H2O, with the goal of understanding the inventory of organic carbon and history of water on Mars.

MODELING REFLECTANCE AND TRANSMITTANCE OF QUARTZ-FIBER FILTER SAMPLES CONTAINING ELEMENTAL CARBON PARTICLES: IMPLICATIONS FOR THERMAL/OPTICAL ANALYSIS. (R831086)

EPA Science Inventory

A radiative transfer scheme that considers absorption, scattering, and distribution of light-absorbing elemental carbon (EC) particles collected on a quartz-fiber filter was developed to explain simultaneous filter reflectance and transmittance observations prior to and during...

Applying Monte-Carlo simulations to optimize an inelastic neutron scattering system for soil carbon analysis

USDA-ARS?s Scientific Manuscript database

Computer Monte-Carlo (MC) simulations (Geant4) of neutron propagation and acquisition of gamma response from soil samples was applied to evaluate INS system performance characteristic [sensitivity, minimal detectable level (MDL)] for soil carbon measurement. The INS system model with best performanc...

40 CFR 98.286 - Data reporting requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... petroleum coke consumed). (7) Sampling analysis results for carbon content of consumed petroleum coke as... content factor of petroleum coke from the supplier or as measured by the applicable method in § 98.284(c) for each month (percent by weight expressed as a decimal fraction). (5) Whether carbon content of the...

Development of sampling method and chromatographic analysis of volatile organic compounds emitted from human skin.

PubMed

Grabowska-Polanowska, Beata; Miarka, Przemysław; Skowron, Monika; Sułowicz, Joanna; Wojtyna, Katarzyna; Moskal, Karolina; Śliwka, Ireneusz

2017-10-01

The studies on volatile organic compounds emitted from skin are an interest for chemists, biologists and physicians due to their role in development of different scientific areas, including medical diagnostics, forensic medicine and the perfume design. This paper presents a proposal of two sampling methods applied to skin odor collection: the first one uses a bag of cellulose film, the second one, using cellulose sachets filled with active carbon. Volatile organic compounds were adsorbed on carbon sorbent, removed via thermal desorption and analyzed using gas chromatograph with mass spectrometer. The first sampling method allowed identification of more compounds (52) comparing to the second one (30). Quantitative analyses for acetone, butanal, pentanal and hexanal were done. The skin odor sampling method using a bag of cellulose film, allowed the identification of many more compounds when compared with the method using a sachet filled with active carbon.

Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples.

PubMed

Zheng, Hao-Bo; Ding, Jun; Zheng, Shu-Jian; Zhu, Gang-Tian; Yuan, Bi-Feng; Feng, Yu-Qi

2016-01-01

In this study, we proposed a method to fabricate magnetic carbon nitride (CN) nanosheets by simple physical blending. Low-cost CN nanosheets prepared by urea possessed a highly π-conjugated structure; therefore the obtained composites were employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of polycyclic aromatic hydrocarbons (PAHs) in edible oil samples. Moreover, sample pre-treatment time could be carried out within 10 min. Thus, a simple and cheap method for the analysis of PAHs in edible oil samples was established by coupling magnetic CN nanosheets-based MSPE with gas chromatography-mass spectrometry (GC/MS) analysis. Limits of quantitation (LOQs) for eight PAHs ranged from 0.4 to 0.9 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 15.0%. The recoveries of PAHs for spiked soybean oil samples ranged from 91.0% to 124.1%, with RSDs of less than 10.2%. Taken together, the proposed method offers a simple and cost-effective option for the convenient analysis of PAHs in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Schumacher,M.; Christl, I.; Vogt, R.

The chemical composition and carbon isotope signature of aquatic dissolved organic matter (DOM) in five boreal forest catchments in Scandinavia were investigated. The DOM was isolated during spring and fall seasons using a reverse osmosis technique. The DOM samples were analyzed by elemental analysis, FT-IR, solid-state CP-MAS {sup 13}C-NMR, and C-1s NEXAFS spectroscopy. In addition, the relative abundance of carbon isotopes ({sup 12}C, {sup 13}C, {sup 14}C) in the samples was measured. There were no significant differences in the chemical composition or carbon isotope signature of the DOM sampled in spring and fall seasons. Also, differences in DOM composition betweenmore » the five catchments were minor. Compared to reference peat fulvic and humic acids, all DOM samples were richer in O-alkyl carbon and contained less aromatic and phenolic carbon, as shown by FT-IR, {sup 13}C-NMR, and C-1s NEXAFS spectroscopy. The DOM was clearly enriched in {sup 14}C relative to the NBS oxalic acid standard of 1950, indicating that the aquatic DOM contained considerable amounts of organic carbon younger than about 50 years. The weight-based C:N ratios of 31 {+-} 6 and the {delta}{sup 13}Cvalues of -29 {+-} 2{per_thousand}indicate that the isolated DOM is of terrestrial rather than aquatic origin. We conclude that young, hydrophilic carbon compounds of terrestrial origin are predominant in the samples investigated, and that the composition of the aquatic DOM in the studied boreal forest catchments is rather stable during low to intermediate flow conditions.« less

Cross sectional TEM analysis of duplex HIPIMS and DC magnetron sputtered Mo and W doped carbon coatings

NASA Astrophysics Data System (ADS)

Sharp, J.; Castillo Muller, I.; Mandal, P.; Abbas, A.; West, G.; Rainforth, W. M.; Ehiasarian, A.; Hovsepian, P.

2015-10-01

A FIB lift-out sample was made from a wear-resistant carbon coating deposited by high power impulse magnetron sputtering (HIPIMS) with Mo and W. TEM analysis found columnar grains extending the whole ∼1800 nm thick film. Within the grains, the carbon was found to be organised into clusters showing some onion-like structure, with amorphous material between them; energy dispersive X-ray spectroscopy (EDS) found these clusters to be Mo- and W-rich in a later, thinner sample of the same material. Electron energy-loss spectroscopy (EELS) showed no difference in C-K edge, implying the bonding type to be the same in cluster and matrix. These clusters were arranged into stripes parallel to the film plane, of spacing 7-8 nm; there was a modulation in spacing between clusters within these stripes that produced a second, coarser set of striations of spacing ∼37 nm.

Removal of BrO₃⁻ from drinking water samples using newly developed agricultural waste-based activated carbon and its determination by ultra-performance liquid chromatography-mass spectrometry.

PubMed

Naushad, Mu; Khan, Mohammad R; ALOthman, Zeid A; AlSohaimi, Ibrahim; Rodriguez-Reinoso, Francisco; Turki, Turki M; Ali, Rahmat

2015-10-01

Activated carbon was prepared from date pits via chemical activation with H3PO4. The effects of activating agent concentration and activation temperature on the yield and surface area were studied. The optimal activated carbon was prepared at 450 °C using 55 % H3PO4. The prepared activated carbon was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer, Emmett, and Teller (BET) surface area. The prepared date pit-based activated carbon (DAC) was used for the removal of bromate (BrO3 (-)). The concentration of BrO3 (-) was determined by ultra-performance liquid chromatography-mass tandem spectrometry (UPLC-MS/MS). The experimental equilibrium data for BrO3 (-) adsorption onto DAC was well fitted to the Langmuir isotherm model and showed maximum monolayer adsorption capacity of 25.64 mg g(-1). The adsorption kinetics of BrO3 (-) adsorption was very well represented by the pseudo-first-order equation. The analytical application of DAC for the analysis of real water samples was studied with very promising results.

CARBON STARS IN THE SATELLITES AND HALO OF M31

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

Hamren, Katherine; Guhathakurta, Puragra; Rockosi, Constance M.

2016-09-01

We spectroscopically identify a sample of carbon stars in the satellites and halo of M31 using moderate-resolution optical spectroscopy from the Spectroscopic and Photometric Landscape of Andromeda’s Stellar Halo survey. We present the photometric properties of our sample of 41 stars, including their brightness with respect to the tip of the red giant branch (TRGB) and their distributions in various color–color spaces. This analysis reveals a bluer population of carbon stars fainter than the TRGB and a redder population of carbon stars brighter than the TRGB. We then apply principal component analysis to determine the sample’s eigenspectra and eigencoefficients. Correlatingmore » the eigencoefficients with various observable properties reveals the spectral features that trace effective temperature and metallicity. Putting the spectroscopic and photometric information together, we find the carbon stars in the satellites and halo of M31 to be minimally impacted by dust and internal dynamics. We also find that while there is evidence to suggest that the sub-TRGB stars are extrinsic in origin, it is also possible that they are are particularly faint members of the asymptotic giant branch.« less

Preparation of nanobiochar as magnetic solid acid catalyst by pyrolysis-carbonization from oil palm empty fruit bunches

NASA Astrophysics Data System (ADS)

Jenie, S. N. Aisyiyah; Kristiani, Anis; Kustomo, Simanungkalit, Sabar; Mansur, Dieni

2017-11-01

Nanomaterials based on carbon exhibits unique properties, both physical and chemical, that can be utilized in various application, including catalyst. These nanomaterials were prepared through pyrolysis-carbonization process of biomass, oil palm empty fruit bunches. The effect of carbonization temperature in range of 500°C-600°C were also studied. The magnetic nanobiochar samples, MBC, were sulfonated by using sulfuric acid to increase their properties as solid acid catalyst. Their chemical and physical properties were characterized by Surface Area Analyzer and Porositymeter, X-Ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infra-Red. The magnetic biochar samples obtained from carbonization at 873 K, MBC02-SO3H, was proven to have higher surface area, crystallinity properties and surface chemical composition after sulfonation process, which were confirmed by the BET, XRD and FT-IR analysis. Moreover, sample MBC02-SO3H exhibit promising catalytic acitivity in a catalysed esterification reaction, producing an ester yield of 64%. The result from this work opens new opportunities for the development of magnetic heterogenous acid catalyst from biomass waste.

Vanadium Recovery from Oil Fly Ash by Carbon Removal and Roast-Leach Process

NASA Astrophysics Data System (ADS)

Jung, Myungwon; Mishra, Brajendra

2018-02-01

This research mainly focuses on the recovery of vanadium from oil fly ash by carbon removal and the roast-leach process. The oil fly ash contained about 85% unburned carbon and 2.2% vanadium by weight. A vanadium-enriched product was obtained after carbon removal, and the vanadium content of this product was 19% by weight. Next, the vanadium-enriched product was roasted with sodium carbonate to convert vanadium oxides to water-soluble sodium metavanadate. The roasted sample was leached with water at 60°C, and the extraction percentage of vanadium was about 92% by weight. Several analytical techniques, such as inductively coupled plasma atomic emission spectroscopy (ICP-AES), x-ray fluorescence (XRF), and thermogravimetric and differential thermal analysis (TG-DTA), were utilized for sample analyses. Thermodynamic modeling was also conducted with HSC chemistry software to explain the experimental results.

Measurements of the global distribution of carbon monoxide in the troposphere

NASA Technical Reports Server (NTRS)

Hinton, R. R.

1982-01-01

Carbon monoxide and methane grab samples were obtained simultaneously with ozone, aerosol, nitric oxide and DACOM CO measurements. Eighty grab samples were collected at various altitudes up to 19,000 ft. along a north-south flight path from Wallops Flight Center, VA to 11 N. CO and CH were analyzed by flame ionization gas chromatography with cryogenic preconcentration. The relationship between CO and O3 concentrated is examined. A comparative analysis between trends in aerosol and CO concentration is performed.

Petrological, geochemical and isotopic characteristics of lignite and calcified lignite from mining area Pesje, Velenje Basin, Slovenia

NASA Astrophysics Data System (ADS)

Vrabec, Mirijam; Markič, Miloš; Vrabec, Marko; Jaćimović, Radojko; Kanduč, Tjaša

2014-05-01

Lignite (organic rich) and calcified lignite (inorganic rich) samples from excavation field -50c mining area Pesje, Velenje Basin, Slovenia were investigated. During geological and structural mapping lignite and calcified lignite samples were systematically taken for determination of their petrological, geochemical and isotopic characteristics. Lignite is composed of fine detritical gelified matrix. At least five different types of calcified lignite were recognized forming laminations, calcifications after wood, petrified wood and complete replacements of lignite with carbonate. All measured parameters so far indicate geochemical processes during sedimentation of the Velenej Basin. After macroscopic description samples were split to organic and inorganic component (Ward, 1984) and powdered in an agate mortar for geochemical and isotopic analyses. Major and trace elements (As, B, Ba, Cd, Co, Cr, Cu, Hg, Mn, Mo, Sb, Se, Th, U, Zn) in these samples were determined by instrumental neutron activation analysis (INAA) using k-0 standardization method (Jaćimović et al, 2002). The isotopic composition of carbon and nitrogen was determined using a Europa 20-20 continuous flow IRMS ANCA-SL preparation module. A 1 mg amount of a sample was weighed in a tin capsule for carbon and 10 mg for nitrogen analysis. Samples for carbon analyses were pretreated with 1 M HCl to remove carbonates. Carbonate samples from carbonate-rich strata and calcified xylite were first roasted at 450 deg C (Krantz et al., 1987). Three miligrams of carbonate sample was transformed into CO2 by reaction with anhydrous H3PO4 at 55 deg C under vacuum (McCrea, 1950) and measured with GV 2003 isotope ratio mass spectrometer. Measured isotopic composition of oxygen as VPDB values was recalculated to the VSMOW reference standard to enable the comparison with data from other coal basins. SEM/EDXS of carbonate rich sediments was performed with JEOL JSM 5800 electron microanalyzer scanning electron microscope energy dispersive X-ray spectroscopy at the Department of Ceramics at the Jožef Stefan Institute. Geochemical characteristics of major and trace elements indicate that the values of major and trace elements are comparable to world average coal (Zhang et al., 2004). Isotopic composition of carbon and isotopic composition of nitrogen of investigated samples indicate values from to -29.4o to -23.7o and 1.8o to 5.9o respectively. Lower value of isotopic composition of carbon indicates higher gelification (values up to -29.4) and higher value of isotopic composition of nitrogen (values up to 5.9) indicate higher mineralization. The results of SEM/EDXS microscopy revealed that in calcified lignite chemical composition of calcite prevails. Traces of diagenetic pyrite were also found, indicating localized anoxic conditions during sedimentation. Values of isotopic composition of CCaCO3 range from -2 to +13 and indicate temperature of precipitation from 17.3 to 35 deg C, which is similar to results obtained in previous studies (Kanduč et al., 2012). References Krantz, D.E., Williams, D.F., Jones, D.S., 1987: Ecological and paleoenvironmental information using stable isotope profiles from living and fossil mollusks. Palaeogeography, Palaeoclimatology, Palaeoecology 58, 249-266. Kanduč T., Markič M., Zavšek S., McIntosh J. 2012: carbon cycling in the Pliocene Velenje Coal Basin, Slovenia, inferred from stable carbon isotopes. International Journal of Coal Geology 89, 70-83. Jaćimović, R., Lazaru, A., Mihajlović, D., Ilić, R., Stafilov, T., 2002: Determination of major and trace elements in some minerals by k0-instrumental neutron activation analysis. Journal of Radioanalytical Nuclear Chemistry, 253, 427-434. McCrea, JM., 1950. On the isotopic chemistry of carbonates and a paleotemperature scale. Journal of Chemical Physics 18, 849. Ward C.R. (Ed.), 1984: Coal Geology and Coal Technology. Black-well, Oxford, 345 pp. Zhang J.Y., Zheng C.G., Ren D.Y., Chou C.L., Zheng R.S., Wang Z.P., Zhao F. H., Ge Y.T. 2004: Distribution of potentially hazardous trace elements in coals from Shoxi provinces, China. Fuel 83: 129-135.

Use of nanotomographic images for structure analysis of carbonate rocks

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

Nagata, Rodrigo; Appoloni, Carlos Roberto

Carbonate rocks store more than 50% of world's petroleum. These rocks' structures are highly complex and vary depending on many factors regarding their formation, e.g., lithification and diagenesis. In order to perform an effective extraction of petroleum it is necessary to know petrophysical parameters, such as total porosity, pore size and permeability of the reservoir rocks. Carbonate rocks usually have a range of pore sizes that goes from nanometers to meters or even dozen of meters. The nanopores and micropores might play an important role in the pores connectivity of carbonate rocks. X-ray computed tomography (CT) has been widely usedmore » to analyze petrophysical parameters in recent years. This technique has the capability to generate 2D images of the samples' inner structure and also allows the 3D reconstruction of the actual analyzed volume. CT is a powerful technique, but its results depend on the spatial resolution of the generated image. Spatial resolution is a measurement parameter that indicates the smallest object that can be detected. There are great difficulties to generate images with nanoscale resolution (nanotomographic images). In this work three carbonate rocks, one dolomite and two limestones (that will be called limestone A and limestone B) were analyzed by nanotomography. The measurements were performed with the SkyScan2011 nanotomograph, operated at 60 kV and 200 μA to measure the dolomite sample and 40 kV and 200 μA to measure the limestone samples. Each sample was measured with a given spatial resolution (270 nm for the dolomite sample, 360 nm for limestone A and 450 nm for limestone B). The achieved results for total porosity were: 3.09 % for dolomite, 0.65% for limestone A and 3.74% for limestone B. This paper reports the difficulties to acquire nanotomographic images and further analysis about the samples' pore sizes.« less

Urbanization effect on groundwater quality (Paleohydrogeological study)

NASA Astrophysics Data System (ADS)

Sabri, Raghid; Merkel, Broder; Tichomirowa, Marion

2015-04-01

Speleothem growing in caves usually contain hydrological information. Carbonates precipitation growing in tunnels under cities contain information about anthropological influence on water system. Carbonate samples were taken from Roman tunnels in rural and urban area in Nablus district- Palestine. These laminated samples were analyzed for rare earth elements (REE), 13C and 18O. For REE, five samples were examined, each lamination was extracted and diluted with 0.1 ml 65% HNO3 and measured using ICP-MS. Yet, limited number of lamination was used for isotope analysis using Isotope ratio mass spectrometry. Total concentration of rare earth elements were calculated for each of the five samples. In all examined samples, the newer laminations show higher peaks than the older one of each sample. On the other hand, one sample (8 measurements) of 13C show values between -31.6° and -36°. These values mean that the carbonate is from organic origin. In an urban area, wastewater infiltration into groundwater system can be the source of organic matter. 18O measurements show continues enrichments within the growth of the carbonate. This increase of the 18O values reflects drier weather. Our results can be explained by the increase of water consumption in the household in the recent 100 years, rather than the increase of using detergents and cleaning products which have influenced groundwater quality as appeared in the carbonate samples. On the other hand, 18O results could be linked with the expansion of the building up area in the city and subsequently reduction of groundwater recharge

The isotope record of short- and long-term dietary changes in sheep tooth enamel: Implications for quantitative reconstruction of paleodiets

NASA Astrophysics Data System (ADS)

Zazzo, A.; Balasse, M.; Passey, B. H.; Moloney, A. P.; Monahan, F. J.; Schmidt, O.

2010-06-01

Quantitative reconstruction of paleodiet by means of sequential sampling and carbon isotope analysis in hypsodont tooth enamel requires a precise knowledge of the isotopic enrichment between dietary carbon and carbon from enamel apatite ( ɛD-E), as well as of the timing and duration of the enamel mineralization process (amelogenesis). To better constrain these parameters, we performed a series of controlled feeding experiments on sheep ranging in age from 6 to 24 months-old. Twenty-eight lambs and 14 ewes were fed isotopically distinct diets for different periods of time, and then slaughtered, allowing the timing and rate of molar growth to be determined. High resolution sampling and stable carbon isotope analysis of breath CO 2 performed on six individuals following a diet-switch showed that 70-90% of dietary carbon had turned over in less than 24 h. Sequential sampling and carbon isotopic analysis was performed on the first (M 1) and second (M 2) lower molars of four lambs as well as on the third lower molar (M 3) of 11 ewes. The changes in diet were recorded in all molars. We found that the length of enamel matrix apposition is approximately one-quarter of the final tooth length during crown extension, and that enamel maturation spans slightly less than 3 months in M 1, and 4 months in M 2 and M 3. Portions of enamel in equilibrium with dietary carbon were used to calculate ɛD-E values. Animals on grass silage diets had values similar to previous observations, whereas animal switched to pelleted corn diets had values ca. 4‰ lower, a pattern consistent with lower methane production observed for animals fed concentrate diets. The tooth enamel forward model of Passey and Cerling (2002) closely predicted the amplitude of isotope changes recorded in tooth enamel, but slightly underestimated the rate of isotope change, suggesting that the rate of accumulation of carbonate during maturation may not be constant over time. Although stable isotope profiles in tooth enamel represent underdetermined systems, our results demonstrate that they can provide useful information about dietary variability if the mineralization process is taken into account.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-07-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

NASA Astrophysics Data System (ADS)

Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

2018-04-01

Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

Solid-phase microextraction fiber development for sampling and analysis of volatile organohalogen compounds in air.

PubMed

Attari, Seyed Ghavameddin; Bahrami, Abdolrahman; Shahna, Farshid Ghorbani; Heidari, Mahmoud

2014-01-01

A green, environmental friendly and sensitive method for determination of volatile organohalogen compounds was described in this paper. The method is based on a homemade sol-gel single-walled carbon nanotube/silica composite coated solid-phase microextraction to develop for sampling and analysis of Carbon tetrachloride, Benzotrichloride, Chloromethyl methyl ether and Trichloroethylene in air. Application of this method was investigated under different laboratory conditions. Predetermined concentrations of each analytes were prepared in a home-made standard chamber and the influences of experimental parameters such as temperature, humidity, extraction time, storage time, desorption temperature, desorption time and the sorbent performance were investigated. Under optimal conditions, the use of single-walled carbon nanotube/silica composite fiber showed good performance, high sensitive and fast sampling of volatile organohalogen compounds from air. For linearity test the regression correlation coefficient was more than 98% for analyte of interest and linear dynamic range for the proposed fiber and the applied Gas Chromatography-Flame Ionization Detector technique was from 1 to 100 ngmL(-1). Method detection limits ranged between 0.09 to 0.2 ngmL(-1) and method quantification limits were between 0.25 and 0.7 ngmL(-1). Single-walled carbon nanotube/silica composite fiber was highly reproducible, relative standard deviations were between 4.3 to 11.7 percent.

Relative effectiveness of kinetic analysis vs single point readings for classifying environmental samples based on community-level physiological profiles (CLPP)

NASA Technical Reports Server (NTRS)

Garland, J. L.; Mills, A. L.; Young, J. S.

2001-01-01

The relative effectiveness of average-well-color-development-normalized single-point absorbance readings (AWCD) vs the kinetic parameters mu(m), lambda, A, and integral (AREA) of the modified Gompertz equation fit to the color development curve resulting from reduction of a redox sensitive dye from microbial respiration of 95 separate sole carbon sources in microplate wells was compared for a dilution series of rhizosphere samples from hydroponically grown wheat and potato ranging in inoculum densities of 1 x 10(4)-4 x 10(6) cells ml-1. Patterns generated with each parameter were analyzed using principal component analysis (PCA) and discriminant function analysis (DFA) to test relative resolving power. Samples of equivalent cell density (undiluted samples) were correctly classified by rhizosphere type for all parameters based on DFA analysis of the first five PC scores. Analysis of undiluted and 1:4 diluted samples resulted in misclassification of at least two of the wheat samples for all parameters except the AWCD normalized (0.50 abs. units) data, and analysis of undiluted, 1:4, and 1:16 diluted samples resulted in misclassification for all parameter types. Ordination of samples along the first principal component (PC) was correlated to inoculum density in analyses performed on all of the kinetic parameters, but no such influence was seen for AWCD-derived results. The carbon sources responsible for classification differed among the variable types with the exception of AREA and A, which were strongly correlated. These results indicate that the use of kinetic parameters for pattern analysis in CLPP may provide some additional information, but only if the influence of inoculum density is carefully considered. c2001 Elsevier Science Ltd. All rights reserved.

Hyperspectral Analysis of Soil Nitrogen, Carbon, Carbonate, and Organic Matter Using Regression Trees

PubMed Central

Gmur, Stephan; Vogt, Daniel; Zabowski, Darlene; Moskal, L. Monika

2012-01-01

The characterization of soil attributes using hyperspectral sensors has revealed patterns in soil spectra that are known to respond to mineral composition, organic matter, soil moisture and particle size distribution. Soil samples from different soil horizons of replicated soil series from sites located within Washington and Oregon were analyzed with the FieldSpec Spectroradiometer to measure their spectral signatures across the electromagnetic range of 400 to 1,000 nm. Similarity rankings of individual soil samples reveal differences between replicate series as well as samples within the same replicate series. Using classification and regression tree statistical methods, regression trees were fitted to each spectral response using concentrations of nitrogen, carbon, carbonate and organic matter as the response variables. Statistics resulting from fitted trees were: nitrogen R2 0.91 (p < 0.01) at 403, 470, 687, and 846 nm spectral band widths, carbonate R2 0.95 (p < 0.01) at 531 and 898 nm band widths, total carbon R2 0.93 (p < 0.01) at 400, 409, 441 and 907 nm band widths, and organic matter R2 0.98 (p < 0.01) at 300, 400, 441, 832 and 907 nm band widths. Use of the 400 to 1,000 nm electromagnetic range utilizing regression trees provided a powerful, rapid and inexpensive method for assessing nitrogen, carbon, carbonate and organic matter for upper soil horizons in a nondestructive method. PMID:23112620

Microorganisms, Organic Carbon, and Their Relationship with Oxidant Activity in Hyper-Arid Mars-Like Soils: Implications for Soil Habitability

NASA Technical Reports Server (NTRS)

Valdivia-Silva, Julio E.; Karouia, Fathi; Navarro-Gonzalez, Rafael; McKay, Christopher

2016-01-01

Soil samples from the hyper-arid region in the Atacama 23 Desert in Southern Peru (La Joya Desert) were analyzed for total and labile organic carbon (TOC & LOC), phospholipid fatty acids analysis (PLFA), quantitative real time polymerase chain reaction (qRT-PCR), 4',6- diamidino-2-phenylindole (DAPI)-fluorescent microscopy, culturable microorganisms, and oxidant activity, in order to understand the relationship between the presence of organic matter and microorganisms in these types of soils. TOC content levels were similar to the labile pool of carbon suggesting the absence of recalcitrant carbon in these soils. The range of LOC was from 2 to 60 micro-g/g of soil. PLFA analysis indicated a maximum of 2.3 x 10(exp 5) cell equivalents/g. Culturing of soil extracts yielded 1.1 x 10(exp 2)-3.7 x 10(exp 3) CFU/g. qRT-PCR showed between 1.0 x 10(exp 2) and 8 x 10(exp 3) cells/g; and DAPI fluorescent staining indicated bacteria counts up to 5 x 104 cells/g. Arid and semiarid samples (controls) showed values between 10(exp 7) and 10(exp 11) cells/g with all of the methods used. Importantly, the concentration of microorganisms in hyper-arid soils did not show any correlation with the organic carbon content; however, there was a significant dependence on the oxidant activity present in these soil samples evaluated as the capacity to decompose sodium formate in 10 hours. We suggest that the analysis of oxidant activity could be a useful indicator of the microbial habitability in hyper-arid soils, obviating the need to measure water activity over time. This approach could be useful in astrobiological studies on other worlds.

14CO2 processing using an improved and robust molecular sieve cartridge

NASA Astrophysics Data System (ADS)

Wotte, Anja; Wordell-Dietrich, Patrick; Wacker, Lukas; Don, Axel; Rethemeyer, Janet

2017-06-01

Radiocarbon (14C) analysis on CO2 can provide valuable information on the carbon cycle as different carbon pools differ in their 14C signature. While fresh, biogenic carbon shows atmospheric 14C concentrations, fossil carbon is 14C free. As shown in previous studies, CO2 can be collected for 14C analysis using molecular sieve cartridges (MSC). These devices have previously been made of plastic and glass, which can easily be damaged during transport. We thus constructed a robust MSC suitable for field application under tough conditions or in remote areas, which is entirely made of stainless steel. The new MSC should also be tight over several months to allow long sampling campaigns and transport times, which was proven by a one year storage test. The reliability of the 14CO2 results obtained with the MSC was evaluated by detailed tests of different procedures to clean the molecular sieve (zeolite type 13X) and for the adsorption and desorption of CO2 from the zeolite using a vacuum rig. We show that the 14CO2 results are not affected by any contamination of modern or fossil origin, cross contamination from previous samples, and by carbon isotopic fractionation. In addition, we evaluated the direct CO2 transfer from the MSC into the automatic graphitization equipment AGE with the subsequent 14C AMS analysis as graphite. This semi-automatic approach can be fully automated in the future, which would allow a high sample throughput. We obtained very promising, low blank values between 0.0018 and 0.0028 F14C (equivalent to 50,800 and 47,200 yrs BP), which are within the analytical background and lower than results obtained in previous studies.

Comparison of deformation mechanics for two different carbonates: oolitic limestone and laminites

NASA Astrophysics Data System (ADS)

Zihms, Stephanie; Lewis, Helen; Couples, Gary; Hall, Stephen; Somerville, Jim

2016-04-01

Carbonate rocks form under a range of conditions which leads to a diverse rock group. Even though carbonates are overall mineralogically simple, the solid-space distribution ranges from simple compositions such as oolitic limestones to highly complex networks of pores and solids as seen in coquinas. Their fundamental mechanical behaviour has been identified to be like clastic rocks (Vajdova 2004, Brantut, Heap et al. 2014). However it is very likely that this observation is not true for more complex carbonates. Triaxial tests were performed on cylindrical samples of two different carbonates; a) oolitic limestone (Bicqueley quarry, France) and b) laminite (Ariripe basin, Brazil). The samples were deformed under confining pressures of 8, 12 and 20MPa, and 20, 30 and 40MPa, respectively. All tests were stopped as soon as peak load was observed to preserve as many deformation characteristics as possible. Photographs of the samples were taken before and after deformation to allow surface analysis of deformation features. Additionally, samples were analysed post-deformation with X-ray tomography (XRT) (using the Zeiss XRadia XRM 520 at the 4D Imaging Lab at Lund University). The 3D tomography images represent the post-deformation samples' density distribution, allowing detailed, non-destructive, 3D analysis of the deformation features that developed in the triaxial testing, including the complex geometries and interactions of fractures, deformation bands and sedimentary layering. They also provide an insight into the complexity of deformation features produced due to the carbonate response. Initial results show that the oolitic limestone forms single shear bands almost the length of the sample, exhibiting similar characteristics to sandstones deformed under similar conditions. These features are observed for all three applied loads. The laminate sample deformed at the lowest confining pressure exhibits compactive features. However, the laminite samples deformed at the two higher confining pressures both show highly complex fracture networks comprising open fractures and fracture propagation. This suggests that the laminate changes from compactive to dilational responses over the selected confining conditions. The XRT analysis indicates that a more complex fracture distribution could be linked to rock component properties e.g. grain size and composition. For the laminite these are variable with the layers. This is in agreement with field observations of laminite microfabrics (Calvo, Rodriguez-Pascua et al. 1998). Additionally, the typical grain size of the laminate (μm) is much smaller than the oolitic limestone (mm), which suggests that fracture network complexity can also be linked to bulk system complexity i.e. pore & grain network. These deformation experiments show that, as previously observed, oolitic limestones seem to behave similarly to sandstones. However this observation is not true for laminites and it is very likely that more complex carbonates will develop even more complicated deformation behaviour. It is therefore necessary to systematically test different carbonate rocks to understand the impact of geometry and composition, as well as the interplay with the pore network. Brantut, N., et al. (2014). Journal of Geophysical Research: Solid Earth 119(7): 5444-5463. Calvo, J. P., et al. (1998). Sedimentology 45: 279-292. Vajdova, V. (2004). Journal of Geophysical Research 109(B5).

Assessment of 14C AMS dating of phytoliths as a new paleoenvironmental and archaeological tool

NASA Astrophysics Data System (ADS)

Corbineau, R.; Alexandre, A. E.; Santos, G. M.; Reyerson, P. E.

2011-12-01

14C AMS analysis of occluded carbon in phytoliths (phytC) is a promising dating tool for palaeoenvironmental and archaeological studies. In order to assess the accuracy of this method, different tests were recently carried out on large phytolith concentrates of phytC samples extracted from soils and harvested plants, in association with blank samples of SiO2 powder to check the absence of carbon contamination during the treatments. Despite this precaution, 14C values from recent harvested plants were inexplicably old (2 - 8 ka years BP). Nevertheless, we noticed that many chemical extraction protocols that were used did not lead to samples totally free of organic matter. In order to tackle this problem, and as a first step, the efficiency of common extraction protocols from the literature were tested. Samples were analyzed by SEM/EDX in order to assess the purity of the siliceous material following extraction. As a result of these tests, a new extraction protocol combining acid digestion, oxidation and dry ashing to acquire pure samples of phytoliths from harvested plants is proposed. In a second step, modern and well dated archaeological materials (harvested plants grown within a FACE experiment and plant residues from a 17th century French mummy) were analyzed in 14C-AMS. Results should allow either to demonstrate the reliability of 14C-AMS analysis of phytolith occluded carbon as a dating tool or trigger further investigations of possible sources of old occluded carbon in phytoliths if the 14C ages are still older than expected.

Deposition of amorphous carbon thin films by aerosol-assisted CVD method

NASA Astrophysics Data System (ADS)

Fadzilah, A. N.; Dayana, K.; Rusop, M.

2018-05-01

This paper reports on the deposition of amorphous carbon (a-C) by Aerosol-assisted Chemical Vapor Deposition (AACVD) using natural source of camphor oil as the precursor material. 4 samples were deposited at 4 different deposition flow rate from 15 sccm to 20 sccm, with 5 sccm interval for each sample. The analysis includes the electrical, optical and structural analysis of the data. The a-C structure which came from the manipulation of synthesis parameter was characterized by the solar simulator system, UV-VIS-NIR, Raman spectroscope and AFM. The properties of a-C are highly dependent on the deposition techniques and deposition parameters; hence the influences of gas flow rate were studied.

Diffuse Reflectance Spectroscopy for Total Carbon Analysis of Hawaiian Soils

NASA Astrophysics Data System (ADS)

McDowell, M. L.; Bruland, G. L.; Deenik, J. L.; Grunwald, S.; Uchida, R.

2010-12-01

Accurate assessment of total carbon (Ct) content is important for fertility and nutrient management of soils, as well as for carbon sequestration studies. The non-destructive analysis of soils by diffuse reflectance spectroscopy (DRS) is a potential supplement or alternative to the traditional time-consuming and costly combustion method of Ct analysis, especially in spatial or temporal studies where sample numbers are large. We investigate the use of the visible to near-infrared (VNIR) and mid-infrared (MIR) spectra of soils coupled with chemometric analysis to determine their Ct content. Our specific focus is on Hawaiian soils of agricultural importance. Though this technique has been introduced to the soil community, it has yet to be fully tested and used in practical applications for all soil types, and this is especially true for Hawaii. In short, DRS characterizes and differentiates materials based on the variation of the light reflected by a material at certain wavelengths. This spectrum is dependent on the material’s composition, structure, and physical state. Multivariate chemometric analysis unravels the information in a set of spectra that can help predict a property such as Ct. This study benefits from the remarkably diverse soils of Hawaii. Our sample set includes 216 soil samples from 145 pedons from the main Hawaiian Islands archived at the National Soil Survey Center in Lincoln, NE, along with more than 50 newly-collected samples from Kauai, Oahu, Molokai, and Maui. In total, over 90 series from 10 of the 12 soil orders are represented. The Ct values of these samples range from < 1% - 55%. We anticipate that the diverse nature of our sample set will ensure a model with applicability to a wide variety of soils, both in Hawaii and globally. We have measured the VNIR and MIR spectra of these samples and obtained their Ct values by dry combustion. Our initial analyses are conducted using only samples obtained from the Lincoln archive. In this preliminary case, we use Partial Least Squares (PLS) regression with cross validation to develop a prediction model for soils of unknown carbon content given only their spectral signature. We find R2 values of greater than 0.93 for the MIR spectra and 0.87 for the VNIR spectra, indicating a strong ability to correlate a soil’s spectrum with its Ct content. We build on these encouraging results by continuing chemometric analyses using the full data set, different data subsets, separate model calibration and validation groups, combined VNIR and MIR spectra, and exploring different data pretreatment options and variations to the PLS parameters.

Synthesis, characterisation and applications of coiled carbon nanotubes.

PubMed

Hanus, Monica J; Harris, Andrew T

2010-04-01

Coiled carbon nanotubes are helical carbon structures formed when heptagonal and pentagonal rings are inserted into the hexagonal backbone of a 'straight' nanotube. Coiled carbon nanotubes have been reported with both regular and irregular helical structures. In this work the structure, growth mechanism(s), synthesis, properties and potential applications of coiled carbon nanotubes are reviewed. Published data suggests that coiled carbon nanotube synthesis occurs due to nonuniform extrusion of carbon from a catalyst surface. To date, coiled carbon nanotubes have been synthesised using catalyst modification techniques including: (i) the addition of S or P containing compounds during synthesis; (ii) the use of binary or ternary metal catalysts; (iii) the use of microwaves to create a local temperature gradient around individual catalyst particles and; (iv) the use of pH control during catalyst preparation. In most instances coiled carbon nanotubes are produced as a by-product; high yield and/or large-scale synthesis of coiled carbon nanotubes remains problematic. The qualitative analysis of coiled carbon nanotubes is currently hindered by the absence of specific characterisation data in the literature, e.g., oxidation profiles measured by thermogravimetric analysis and Raman spectra of pure coiled carbon nanotube samples.

Constraints on primary and secondary particulate carbon sources using chemical tracer and 14C methods during CalNex-Bakersfield

EPA Science Inventory

The present study investigates primary and secondary sources of organic carbon for Bakersfield, CA, USA as part of the 2010 CalNex study. The method used here involves integrated sampling that is designed to allow for detailed and specific chemical analysis of particulate matter ...

Clumped Isotope Values from the Doushantuo Formation of South China: Evaluation of Hydrothermal Influence, Disequilibria and Diagenetic Effects

NASA Astrophysics Data System (ADS)

Foster, I. S.; Zhu, M.; Lu, M.; Bristow, T.; Bonifacie, M.; Tripati, A.

2015-12-01

The Ediacaran Doushantuo Formation (635 - 551 Ma) of southern China is a phosphate-dolostone-black shale sequence following the Marinoan "Snowball Earth" episode that represents an important period in Earth history. It contains abundant phosphate-preserved microfossils, and extremely low carbon isotope values in the cap dolostone unit that have been interpreted to reflect formation in a methane seep environment [1]. Previous clumped isotope analysis of 13C-depleted carbonate veins from the basal Doushantuo samples have been interpreted to reflect hydrothermally-derived thermogenic methane oxidation [2], however recent work on modern and ancient cold seep samples suggests clumped isotope signatures in these environments are influenced by disequilibria effects [3] and are vulnerable to post-depositional diagenesis via internal reordering at temperatures exceeding ~ 100 - 120 ˚C [4]. Here we present initial data from the cap-carbonates overlying the Nantuo diamictite. Our analysis includes a variety of micro-facies from the cap-carbonate including pure calcite and micrite, with a range of carbonate carbon isotopic values. Data presented here will be used to attempt to determine if the samples exhibit disequilibria effects such as those observed in modern cold seep environments, as well as to evaluate the role of hydrothermal activity in the Doushantuo Formation. [1] Jiang, G., Kennedy, M.J., Christie-Blick, N., 2003. Stable isotope evidence for methane seeps in Neoproterozoic postglacial cap carbonates. Nature 426, 822-826. [2] Bristow, T.F., Bonifacie, M., Derkowski, A., Eiler, J.M., Grotzinger, J.P., 2011. A hydrothermal origin for isotopically anomalous cap dolostone cements from south China. Nature 474, 68-72. [3] Loyd, S., Sample, J.C., Orphan, V.J., Marlow, J., Eagle, R., Tripati, A.K., 2012. Clumped isotope analyses of cold seep carbonates: Insights into formation environment and mechanisms. Abstract B51G-0639 presented at 2012 Fall Meeting, AGU, San Francisco, Calif., 3-7 Dec. [4] Henkes, G.A., Passey, B.H., Grossman, E.L., Shenton, B.J., Pérez-Huerta, A., Yancey, E.L., 2014. Temperature limits for preservation of primary calcite clumped isotope paleotemperatures. Geochemica et Cosmochimica Acta 139, 362-382.

Nonprevalence of biochemical fossils in kerogen from pre-Phanerozoic sediments

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

Leventhal, J.; Suess, S. E.; Cloud, P.

Evidence of biochemical and geochemical evolution was sought in insoluble carbonaceous matter from 30 selected pre-Phanerozoic sediments ranging in age from about 3.8 to about 0.7 x 10 9 years. The carbon isotope ratios observed were in the range of -20 to -32 per mil with reference to the Peedee belemnite standard, similar to those previously reported. No systematic trends are obvious to us. Stepwise pyrolysis-gas-chromatography showed only molecules with fewer than 8 carbon atoms at the level of sensitivity of 10 -9 g of organics in a 10 mg rock sample. Carbon, hydrogen, and nitrogen analyses showed noncarbonate carbonmore » from less than 0.1 percent to more than 3 percent, with very small amounts of N. The H/C (atomic) ratios on HCl-leached and HF-treated samples were generally less than 0.3. Evidence of low pyrolysis yields (micro-analysis) and low H/C atomic ratios (macro-analysis) implies that the carbonaceous solids in even the least metamorphosed of these ancient sediments have evolved far toward amorphous carbon or graphite and do not yield useful ''biochemical fossils.''« less

Iron-carbonate interaction at Earth's core-mantle boundary

NASA Astrophysics Data System (ADS)

Dorfman, S. M.; Badro, J.; Nabiei, F.; Prakapenka, V.; Gillet, P.

2015-12-01

Carbon storage and flux in the deep Earth are moderated by oxygen fugacity and interactions with iron-bearing phases. The amount of carbon stored in Earth's mantle versus the core depends on carbon-iron chemistry at the core-mantle boundary. Oxidized carbonates subducted from Earth's surface to the lowermost mantle may encounter reduced Fe0 metal from disproportionation of Fe2+ in lower mantle silicates or mixing with the core. To understand the fate of carbonates in the lowermost mantle, we have performed experiments on sandwiches of single-crystal (Ca0.6Mg0.4)CO3 dolomite and Fe foil in the laser-heated diamond anvil cell at lower mantle conditions of 49-110 GPa and 1800-2500 K. Syntheses were conducted with in situ synchrotron X-ray diffraction to identify phase assemblages. After quench to ambient conditions, samples were sectioned with a focused Ga+ ion beam for composition analysis with transmission electron microscopy. At the centers of the heated spots, iron melted and reacted completely with the carbonate to form magnesiowüstite, iron carbide, diamond, magnesium-rich carbonate and calcium carbonate. In samples heated at 49 and 64 GPa, the two carbonates exhibit a eutectoid texture. In the sample heated at 110 GPa, the carbonates form rounded ~150-nm-diameter grains with a higher modal proportion of interspersed diamonds. The presence of reduced iron in the deep lower mantle and core-mantle boundary region will promote the formation of diamonds in carbonate-bearing subducted slabs. The complete reaction of metallic iron to oxides and carbides in the presence of mantle carbonate supports the formation of these phases at the Earth's core-mantle boundary and in ultra-low velocity zones.

Determination of fossil carbon content in Swedish waste fuel by four different methods.

PubMed

Jones, Frida C; Blomqvist, Evalena W; Bisaillon, Mattias; Lindberg, Daniel K; Hupa, Mikko

2013-10-01

This study aimed to determine the content of fossil carbon in waste combusted in Sweden by using four different methods at seven geographically spread combustion plants. In total, the measurement campaign included 42 solid samples, 21 flue gas samples, 3 sorting analyses and 2 investigations using the balance method. The fossil carbon content in the solid samples and in the flue gas samples was determined using (14)C-analysis. From the analyses it was concluded that about a third of the carbon in mixed Swedish waste (municipal solid waste and industrial waste collected at Swedish industry sites) is fossil. The two other methods (the balance method and calculations from sorting analyses), based on assumptions and calculations, gave similar results in the plants in which they were used. Furthermore, the results indicate that the difference between samples containing as much as 80% industrial waste and samples consisting of solely municipal solid waste was not as large as expected. Besides investigating the fossil content of the waste, the project was also established to investigate the usability of various methods. However, it is difficult to directly compare the different methods used in this project because besides the estimation of emitted fossil carbon the methods provide other information, which is valuable to the plant owner. Therefore, the choice of method can also be controlled by factors other than direct determination of the fossil fuel emissions when considering implementation in the combustion plants.

Pico-CSIA: Picomolar Scale Compound-Specific Isotope Analyses

NASA Astrophysics Data System (ADS)

Baczynski, A. A.; Polissar, P. J.; Juchelka, D.; Schwieters, J. B.; Hilkert, A.; Freeman, K. H.

2016-12-01

The basic approach to analyzing molecular isotopes has remained largely unchanged since the late 1990s. Conventional compound-specific isotope analyses (CSIA) are conducted using capillary gas chromatography (GC), a combustion interface, and an isotope-ratio mass spectrometer (IRMS). Commercially available GC-IRMS systems are comprised of components with inner diameters ≥0.25 mm and employ helium flow rates of 1-4 mL/min. These flow rates are an order of magnitude larger than what the IRMS can accept. Consequently, ≥90% of the sample is lost through the open split, and 1-10s of nanomoles of carbon are required for analysis. These sample requirements are prohibitive for many biomarkers, which are often present in picomolar concentrations. We utilize the resolving power and low flows of narrow-bore capillary GC to improve the sensitivity of CSIA. Narrow bore capillary columns (<0.25 mm ID) allow low helium flow rates of ≤0.5mL/min for more efficient sample transfer to the ion source of the IRMS while maintaining the high linear flow rates necessary to preserve narrow peak widths ( 250 ms). The IRMS has been fitted with collector amplifiers configured to 25 ms response times for rapid data acquisition across narrow peaks. Previous authors (e.g., Sacks et al., 2007) successfully demonstrated improved sensitivity afforded by narrow-bore GC columns. They reported an accuracy and precision of 1.4‰ for peaks with an average width at half maximum of 720 ms for 100 picomoles of carbon on column. Our method builds on their advances and further reduces peak widths ( 600 ms) and the amount of sample lost prior to isotopic analysis. Preliminary experiments with 100 picomoles of carbon on column show an accuracy and standard deviation <1‰. With further improvement, we hope to demonstrate robust isotopic analysis of 10s of picomoles of carbon, more than 2 orders of magnitude lower than commercial systems. The pico-CSIA method affords high-precision isotopic analyses for picomoles of carbon in organic biomarkers, which significantly lowers sample size requirements and broadens analytical windows in paleoclimate, astrobiological, and biogeochemical research.

Time-resolved analysis of nonlinear optical limiting for laser synthesized carbon nanoparticles

NASA Astrophysics Data System (ADS)

Chen, G. X.; Hong, M. H.

2010-11-01

Nonlinear optical limiting materials have attracted much research interest in recent years. Carbon nanoparticles suspended in liquids show a strong nonlinear optical limiting function. It is important to investigate the nonlinear optical limiting process of carbon nanoparticles for further improving their nonlinear optical limiting performance. In this study, carbon nanoparticles were prepared by laser ablation of a carbon target in tetrahydrofuran (THF). Optical limiting properties of the samples were studied with 532-nm laser light, which is in the most sensitive wavelength band for human eyes. The shape of the laser pulse plays an important role for initializing the nonlinear optical limiting effect. Time-resolved analysis of laser pulses discovered 3 fluence stages of optical limiting. Theoretical simulation indicates that the optical limiting is initialized by a near-field optical enhancement effect.

A spectroscopic method for identifying terrestrial biocarbonates and application to Mars

NASA Astrophysics Data System (ADS)

Blanco, A.; Orofino, V.; D'Elia, M.; Fonti, S.; Mastandrea, A.; Guido, A.; Russo, F.

2011-06-01

Searching for traces of extinct and/or extant life on Mars is one of the major objectives for remote-sensing and in situ exploration of the planet. In previous laboratory works we have investigated the infrared spectral modifications induced by thermal processing on different carbonate samples, in the form of fresh shells and fossils of different ages, whose biotic origin is easily recognizable. The goal was to discriminate them from their abiotic counterparts. In general, it is difficult to identify biotic signatures, especially when the organisms inducing the carbonate precipitation have low fossilization potential (i.e. microbes, bacteria, archaea). A wide variety of microorganisms are implicated in carbonate genesis, and their direct characterization is very difficult to evaluate by traditional methods, both in ancient sedimentary systems and even in recent environments. In the present work we apply our analysis to problematic carbonate samples, in which there is no clear evidence of controlled or induced biomineralization. This analysis indicates a very likely biotic origin of the aragonite samples under study, in agreement with the conclusion previously reported by Guido et al. (2007) who followed a completely different approach based on a complex set of sedimentary, petrographic, geochemical and biochemical analyses. We show that our method is reliable for discriminating between biotic and abiotic carbonates, and therefore it is a powerful tool in the search for life on Mars in the next generation of space missions to the planet.

Electrical, structural and thermal studies of carbon nanotubes from natural legume seeds: kala chana

NASA Astrophysics Data System (ADS)

Ranu, Rachana; Chauhan, Yatishwar; Singh, Pramod K.; Bhattacharya, B.; Tomar, S. K.

2016-12-01

Carbon nanotubes (CNTs) are the carbon materials measured at nanoscale level and they are defined in two types according to the number of concentric layers, i.e. single-layer tube is single-walled nanotubes, while multi-layer tube structure is called multi-walled nanotubes. The green method synthesis for the preparation of CNTs begins with the smashing of legume seeds kala chana, and then they form complex with cobalt salt. Desiccation of the complex compound forms cobalt salt and seed protein. The complex is then decomposed at 625 °C in muffle furnace for 20 min. Purification of the decomposed sample is done through acid wash treatment and dried in vacuum oven. The confirmations of CNTs are done by nuclear magnetic resonance and Fourier transform infrared, which analyzes the denatured protein, reacted to the metal salt. X-Ray diffraction determines the MWNTs with transmission electron microscope (TEM) reports the network structure of CNTs. thermal gravimetric analysis (TGA)-differential thermal analysis (DTA)-thermogravimetric analysis (DTG) tests the amount of sample under thermal treatment. Vibrating sample magnetometer determines the paramagnetic nature of CNTs. CNTs thus prepared can be used in mechanical fields, in solar cells, in electronics fields, etc. because of their multidisciplinary properties. The synthesized CNTs are eco-friendly in nature, prepared by the legume seed natural precursor.

Multivariate carbon and nitrogen stable isotope model for the reconstruction of prehistoric human diet.

PubMed

Froehle, A W; Kellner, C M; Schoeninger, M J

2012-03-01

Using a sample of published archaeological data, we expand on an earlier bivariate carbon model for diet reconstruction by adding bone collagen nitrogen stable isotope values (δ(15) N), which provide information on trophic level and consumption of terrestrial vs. marine protein. The bivariate carbon model (δ(13) C(apatite) vs. δ(13) C(collagen) ) provides detailed information on the isotopic signatures of whole diet and dietary protein, but is limited in its ability to distinguish between C(4) and marine protein. Here, using cluster analysis and discriminant function analysis, we generate a multivariate diet reconstruction model that incorporates δ(13) C(apatite) , δ(13) C(collagen) , and δ(15) N holistically. Inclusion of the δ(15) N data proves useful in resolving protein-related limitations of the bivariate carbon model, and splits the sample into five distinct dietary clusters. Two significant discriminant functions account for 98.8% of the sample variance, providing a multivariate model for diet reconstruction. Both carbon variables dominate the first function, while δ(15) N most strongly influences the second. Independent support for the functions' ability to accurately classify individuals according to diet comes from a small sample of experimental rats, which cluster as expected from their diets. The new model also provides a statistical basis for distinguishing between food sources with similar isotopic signatures, as in a previously analyzed archaeological population from Saipan (see Ambrose et al.: AJPA 104(1997) 343-361). Our model suggests that the Saipan islanders' (13) C-enriched signal derives mainly from sugarcane, not seaweed. Further development and application of this model can similarly improve dietary reconstructions in archaeological, paleontological, and primatological contexts. Copyright © 2011 Wiley Periodicals, Inc.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York - July 2001 Through June 2003

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2009-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance and quality-control data were stored in the laboratory's Lab Master data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality control samples analyzed from July 2001 through June 2003. Results for the quality-control samples for 19 analytical procedures were evaluated for bias and precision. Control charts indicate that data for six of the analytical procedures were occasionally biased for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, chloride, magnesium, nitrate (ion chromatography), potassium, and sodium. The calcium procedure was biased throughout the analysis period for the high-concentration sample, but was within control limits. The total monomeric aluminum and fluoride procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The total aluminum, pH, specific conductance, and sulfate procedures were biased for the high-concentration and low-concentration samples, but were within control limits. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 16 of 18 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for the dissolved organic carbon or specific conductance procedures. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 18 of the 21 analytes. At least 90 percent of the samples met data-quality objectives for all procedures except total monomeric aluminum (83 percent of samples met objectives), total aluminum (76 percent of samples met objectives), ammonium (73 percent of samples met objectives), dissolved organic carbon (86 percent of samples met objectives), and nitrate (81 percent of samples met objectives). The data-quality objective was not met for the nitrite procedure. Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated satisfactory or above data quality over the time period, with most performance ratings for each sample in the good-to-excellent range. The N-sample (nutrient constituents) analysis had one unsatisfactory rating for the ammonium procedure in one study. The T-sample (trace constituents) analysis had one unsatisfactory rating for the magnesium procedure and one marginal rating for the potassium procedure in one study and one unsatisfactory rating for the sodium procedure in another. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 90 percent of the samples met data-quality objectives for 10 of the 14 analytes; the exceptions were acid-neutralizing capacity, ammonium, dissolved organic carbon, and sodium. Data-quality objectives were not met in 37 percent of samples analyzed for acid-neutralizing capacity, 28 percent of samples analyzed for dissolved organic carbon, and 30 percent of samples analyzed for sodium. Results indicate a positive bias for the ammonium procedure in one study and a negative bias in another. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 90 percent of the samples analyzed for calcium, chloride, magnesium, pH, potassium, and sodium. Data-quality objectives were met by 78 percent of

Advances in the Determination of the Speciation of the Carbon Associated with Biogenic Silica Produced by Plants

NASA Astrophysics Data System (ADS)

Masion, A.; Alexandre, A. E.; Ziarelli, F.; Viel, S.; Santos, G.

2016-12-01

Biogenic silica resulting from the precipitation of dissolved Si through biological processes in plants, often contains small amounts of occluded organic carbon. These phases, called phytoliths, have a long persistence in soils, making them tracers of past conditions. In this context, the knowledge of the carbon speciation associated with phytoliths bears significant importance in examining the carbon dynamics in soils. With carbon concentrations as low as the 0.1% range, examining the nature of organic carbon remains very challenging, and available tools (e.g. pyrolysis) are often prone to serious artifacts. Recent improvements of microwave sources enabled the application of the Dynamic Nuclear Polarization (DNP) technique to NMR, thereby establishing a new non-destructive tool for the qualitative and quantitative determination of the carbon speciation. Applied to the analysis of phytoliths, this method showed the presence of carbons from different sources within the sample: About 20% of the signal correspond to carbohydrates, and are assigned to photosynthetic carbon; the marked alkyl, N-alkyl and carbonyl signals indicate a significant proportion of proteins. This is consistent with the hypothesis that parts of the carbon associated with the phytoliths is imported into the host plant via uptake from the soil. Finally, lignins, glomalin-like and/or humic-like compounds are minor species associated with biogenic silica. This speciation was obtained overnight with a DNP-NMR set-up with an excellent sensitivity (few tens of weight ppm); the same spectrum on a standard NMR spectrometer would have required at least 250 days of data acquisition. The considerable gain in sensitivity associated with the use of DNP now makes NMR a relevant technique for the analysis of environmental samples.

Development of program package for investigation and modeling of carbon nanostructures in diamond like carbon films with the help of Raman scattering and infrared absorption spectra line resolving

NASA Astrophysics Data System (ADS)

Hayrapetyan, David B.; Hovhannisyan, Levon; Mantashyan, Paytsar A.

2013-04-01

The analysis of complex spectra is an actual problem for modern science. The work is devoted to the creation of a software package, which analyzes spectrum in the different formats, possesses by dynamic knowledge database and self-study mechanism, performs automated analysis of the spectra compound based on knowledge database by application of certain algorithms. In the software package as searching systems, hyper-spherical random search algorithms, gradient algorithms and genetic searching algorithms were used. The analysis of Raman and IR spectrum of diamond-like carbon (DLC) samples were performed by elaborated program. After processing the data, the program immediately displays all the calculated parameters of DLC.

Thermal analysis, phase equilibria, and superconducting properties in magnesium boride and carbon doped magnesium boride

NASA Astrophysics Data System (ADS)

Bohnenstiehl, Scot David

In this work, the low temperature synthesis of MgB2 from Mg/B and MgH2/B powder mixtures was studied using Differential Scanning Calorimetry (DSC). For the Mg/B powder mixture, two exothermic reaction events were observed and the first reaction event was initiated by the decomposition of Mg(OH)2 on the surface of the magnesium powder. For the MgH 2/B powder mixture, there was an endothermic event at ˜375 °C (the decomposition of MgH2 into H2 and Mg) and an exothermic event ˜600 °C (the reaction of Mg and B). The Kissinger analysis method was used to estimate the apparent activation energy of the Mg and B reaction using DSC data with different furnace ramp rates. The limitations of MgB2 low temperature synthesis led to the development of a high pressure induction furnace that was constructed using a pressure vessel and an induction heating power supply. The purpose was to not only synthesize more homogeneous MgB2 samples, but also to determine whether MgB2 melts congruently or incongruently. A custom implementation of the Smith Thermal Analysis method was developed and tested on aluminum and AlB2, the closest analogue to MgB2. Measurements on MgB2 powder and a high purity Mg/B elemental mixture confirmed that MgB2 melts incongruently and decomposes into a liquid and MgB4 at ˜1445 °C at 10 MPa via peritectic decomposition. Another measurement using a Mg/B elemental mixture with impure boron suggested that ˜0.7 wt% carbon impurity in the boron raised the incongruent melting temperature to ˜1490-1500 °C. Lastly, the solubility limit for carbon in MgB2 was studied by making samples from B4C and Mg at 1530 °C, 1600 °C and 1700 °C in the high pressure furnace. All three samples had three phases: Mg, MgB2C2, and carbon doped MgB2. The MgB 2C2 and carbon doped MgB2 grain size increased with temperature and the 1700 °C sample had needle-like grains for both phases. The presence of the ternary phase, MgB2C2, suggested that the maximum doping limit for carbon in MgB2 had been reached. The 1530 °C sample was characterized by Electron Probe Microanalysis at the University of Oregon and the average carbon concentration was estimated to be ˜5.9 at%. Further investigation using TEM found MgO inclusions in the 1530 °C sample which were not detected with X-ray diffraction.

Investigating the Use of a Diffusion Flame to Produce Black Carbon Standards for Thermal- Optical Analysis of Carbonaceous Aerosols

NASA Astrophysics Data System (ADS)

Ortiz Montalvo, D. L.; Kirchstetter, T. W.; Soto-García, L. L.; Mayol-Bracero, O. L.

2006-12-01

Combustion generated particles are a concern to both climate and public health due to their ability to scatter and absorb solar radiation and alter cloud properties, and because they are small enough to be inhaled and deposit in the lungs where they may cause respiratory and other health problems. Specific concern is focused on particles that originate from the combustion of diesel fuel. Diesels particles are composed mainly of carbonaceous material, especially in locations where diesel fuel sulfur is low. These particles are black due to the strongly light absorbing nature of the refractory carbon components, appropriately called black carbon (BC). This research project focuses on the uncertainty in the measurement of BC mass concentration, which is typically determined by analysis of particles collected on a filter using a thermal-optical analysis (TOA) method. Many studies have been conducted to examine the accuracy of the commonly used variations of the TOA method, which vary in their sample heating protocol, carrier gas, and optical measurement. These studies show that BC measurements are inaccurate due to the presence of organic carbon (OC) in the aerosols. OC may co-evolve with BC or char to form BC during analysis, both of which make it difficult to distinguish between the OC and BC in the sample. The goal of this study is to develop the capability of producing standard samples of known amounts of BC, either alone or mixed with other aerosol constituents, and then evaluate which TOA methods accurately determine the BC amount. An inverted diffusion flame of methane and air was used to produce particle samples containing only BC as well as samples of BC mixed with humic acid (HA). Our study found that HA is light absorbing and catalyzes the combustion of BC. It is expected that both of these attributes will challenge the ability of TOA methods in distinguishing between OC and BC, such as the simple two step TOA method which relies solely on temperature to distinguish between OC and BC. These samples were analyzed using two TOA methods to compare the estimates of BC concentration. Future work will focus on the preparation of a variety of BC standards and comparing measurements of the prepared samples using a range of other TOA methods.

Caution on the use of Viton® or FETFE® O-rings in carbon dioxide sample containers for δ180 analysis

USGS Publications Warehouse

Revesz, Kinga M.; Coplen, Tyler B.

1991-01-01

Caution needs to be exercised in selecting sample containers for CO2 isotope-ratio samples of < 200 μmol. If stopcocks are used in construction of containers for such samples, the use of all-glass stopcocks with Apiezon N® hydrocarbon-based grease will eliminate the fractionation of oxygen isotopes.

Crystallization of carbonate hydroxyapatite in the presence of strontium ranelate

NASA Astrophysics Data System (ADS)

Izmailov, R. R.; Golovanova, O. A.

2015-11-01

The influence of strontium ranelate on the crystallization of carbonate hydroxyapatite from a prototype of synovial fluid of humans has been investigated. The synthesis products are studied by IR Fourier spectroscopy, X-ray diffraction, and differential thermal analysis. The amount of strontium in the samples is determined by atomic emission analysis. The sizes of crystallites in the synthesized phases are calculated from the Selyakov-Scherrer formula; the lattice parameters are also determined. The phases obtained are found to be species of calcium-deficient strontium-containing carbonate hydroxyapatite of mixed A and B types. Schemes of chemical reactions occurring during heat treatment are proposed.

Accuracy and Precision in Measurements of Biomass Oxidative Ratio and Carbon Oxidation State

NASA Astrophysics Data System (ADS)

Gallagher, M. E.; Masiello, C. A.; Randerson, J. T.; Chadwick, O. A.; Robertson, G. P.

2007-12-01

Ecosystem oxidative ratio (OR) is a critical parameter in the apportionment of anthropogenic CO2 between the terrestrial biosphere and ocean carbon reservoirs. OR is the ratio of O2 to CO2 in gas exchange fluxes between the terrestrial biosphere and atmosphere. Ecosystem OR is linearly related to biomass carbon oxidation state (Cox), a fundamental property of the earth system describing the bonding environment of carbon in molecules. Cox can range from -4 to +4 (CH4 to CO2). Variations in both Cox and OR are driven by photosynthesis, respiration, and decomposition. We are developing several techniques to accurately measure variations in ecosystem Cox and OR; these include elemental analysis, bomb calorimetry, and 13C nuclear magnetic resonance spectroscopy. A previous study, comparing the accuracy and precision of elemental analysis versus bomb calorimetry for pure chemicals, showed that elemental analysis-based measurements are more accurate, while calorimetry- based measurements yield more precise data. However, the limited biochemical range of natural samples makes it possible that calorimetry may ultimately prove most accurate, as well as most cost-effective. Here we examine more closely the accuracy of Cox and OR values generated by calorimetry on a large set of natural biomass samples collected from the Kellogg Biological Station-Long Term Ecological Research (KBS-LTER) site in Michigan.

Comparison of nitrogen adsorption and transmission electron microscopy analyses for structural characterization of carbon nanotubes

NASA Astrophysics Data System (ADS)

Abbaslou, Reza Malek; Vosoughi, Vahid; Dalai, Ajay K.

2017-10-01

Carbon nanotubes (CNTs) are different from other porous substrates such as activated carbon due to their high external surfaces. This structural feature can lead in some uncertainties in the results of nitrogen adsorption analysis for characterization of CNTs. In this paper, the results of microscopic analyses and nitrogen adsorption method for characterization of carbon nanotubes were compared. Five different types of CNTs with different structures were either synthesized or purchased. The CNT samples were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and N2 adsorption analysis. The comparisons between the results from the microscopic analyses and N2 adsorption showed that the total pore volume and BET surface measurements include the internal and external porosity of CNTs. Therefore, the interpretation of N2 adsorption data required accurate TEM analysis. In addition, the evaluation of pore size distribution curves from all CNT samples in this study and several instances in the literature revealed the presence of a common peak in the range of 2-5 nm. This peak does not explain the inner pore size distribution. The presence of this common peak can be attributed to the strong adsorption of N2 on the junction of touched and crossed nanotubes.

Examining spectral properties of Landsat 8 OLI for predicting above-ground carbon of Labanan Forest, Berau

NASA Astrophysics Data System (ADS)

Suhardiman, A.; Tampubolon, B. A.; Sumaryono, M.

2018-04-01

Many studies revealed significant correlation between satellite image properties and forest data attributes such as stand volume, biomass or carbon stock. However, further study is still relevant due to advancement of remote sensing technology as well as improvement on methods of data analysis. In this study, the properties of three vegetation indices derived from Landsat 8 OLI were tested upon above-ground carbon stock data from 50 circular sample plots (30-meter radius) from ground survey in PT. Inhutani I forest concession in Labanan, Berau, East Kalimantan. Correlation analysis using Pearson method exhibited a promising results when the coefficient of correlation (r-value) was higher than 0.5. Further regression analysis was carried out to develop mathematical model describing the correlation between sample plots data and vegetation index image using various mathematical models.Power and exponential model were demonstrated a good result for all vegetation indices. In order to choose the most adequate mathematical model for predicting Above-ground Carbon (AGC), the Bayesian Information Criterion (BIC) was applied. The lowest BIC value (i.e. -376.41) shown by Transformed Vegetation Index (TVI) indicates this formula, AGC = 9.608*TVI21.54, is the best predictor of AGC of study area.

Application of X-ray microcomputed tomography in the characterization of irradiated nuclear fuel and material specimens

DOE PAGES

Silva, Chinthaka M.; Snead, Lance Lewis; Hunn, John D.; ...

2015-08-03

X-ray microcomputed tomography (µCT) was applied in characterizing the internal structures of a number of irradiated materials, including carbon-carbon fibre composites, nuclear-grade graphite and tristructural isotropic-coated fuel particles. Local cracks in carbon-carbon fibre composites associated with their synthesis process were observed with µCT without any destructive sample preparation. Pore analysis of graphite samples was performed quantitatively, and qualitative analysis of pore distribution was accomplished. It was also shown that high-resolution µCT can be used to probe internal layer defects of tristructural isotropic-coated fuel particles to elucidate the resulting high release of radioisotopes. Layer defects of sizes ranging from 1 tomore » 5 µm and up could be isolated by to-mography. As an added advantage, µCT could also be used to identify regions with high densities of radioisotopes to deter-mine the proper plane and orientation of particle mounting for further analytical characterization, such as materialographic sectioning followed by optical and electron microscopy. Lastly, in fully ceramic matrix fuel forms, despite the highly absorbing matrix, characterization of tristructural isotropic-coated particles embedded in a silicon carbide matrix was accomplished usingµCT and related advanced image analysis techniques.« less

Nanophase Carbonates on Mars: Implications for Carbonate Formation and Habitability

NASA Technical Reports Server (NTRS)

Archer, P. Douglas, Jr.; Lauer, H. Vern; Ming, Douglas W.; Niles, Paul B.; Morris, Richard V.; Rampe, Elizabeth B.; Sutter, Brad

2014-01-01

Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered in small amounts in martian dust [1], in outcrops of very limited extent [2, 3], in soils in the Northern Plains (the landing site of the 2007 Phoenix Mars Scout Mission) [4] and may have recently been detected in aeolian material and drilled and powdered sedimentary rock in Gale Crater (the Mars Science Laboratory [MSL] landing site) [5]. Thermal analysis of martian soils by instruments on Phoenix and MSL has demonstrated a release of CO2 at temperatures as low as 250-300 degC, much lower than the traditional decomposition temperatures of calcium or magnesium carbonates. Thermal decomposition temperature can depend on a number of factors such as instrument pressure and ramp rate, and sample particle size [6]. However, if the CO2 released at low temperatures is from carbonates, small particle size is the only effect that could have such a large impact on decomposition temperature, implying the presence of extremely fine-grained (i.e., "nanophase" or clay-sized) carbonates. We hypothesize that this lower temperature release is the signature of small particle-sized (clay-sized) carbonates formed by the weathering of primary minerals in dust or soils through interactions with atmospheric water and carbon dioxide and that this process may persist under current martian conditions. Preliminary work has shown that clay-sized carbonate grains can decompose at much lower temperatures than previously thought. The first work took carbonate, decomposed it to CaO, then flowed CO2 over these samples held at temperatures >100 degC to reform carbonates. Thermal analysis confirmed that carbonates were indeed formed and transmission electron microsopy was used to determine crystal sized were on the order of 10 nm. The next step used minerals such as diopside and wollastonite that were sealed in a glass tube with a CO2 and H2O source. After reacting these materials for a number of hours, thermal analysis demonstrated the formations of carbonates that decomposed at temperatures as low as 500 degC [7]. Further work is underway to carry out the weathering process under more Mars-like conditions (low pressure and low temperature) to determine if the carbonate decomposition temperature can be shifted to even lower temperatures, consistent with what has been detected by thermal analysis instruments on Mars.

Thermal/optical methods for elemental carbon quantification in soils and urban dusts: equivalence of different analysis protocols.

PubMed

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method.

Hydrogen storage studies on palladium-doped carbon materials (AC, CB, CNMs) @ metal-organic framework-5.

PubMed

Viditha, V; Srilatha, K; Himabindu, V

2016-05-01

Metal organic frameworks (MOFs) are a rapidly growing class of porous materials and are considered as best adsorbents for their high surface area and extraordinary porosity. The MOFs are synthesized by using various chemicals like triethylamine, terepthalic acid, zinc acetate dihydrate, chloroform, and dimethylformamide (DMF). Synthesized MOFs are intercalated with palladium/activated carbon, carbon black, and carbon nanomaterials by chemical reduction method for the purpose of enhancing the hydrogen adsorption capacities. We have observed that the palladium doped activated carbon on MOF-5 showed high hydrogen storage capacity. This may be due to the affinity of the palladium toward hydrogen molecule. The samples are characterized by X-ray diffraction, scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. We have observed a clear decrease in the BET surface area and pore volume. The obtained results show a better performance for the synthesized sample. To our best knowledge, no one has reported the work on palladium-doped carbon materials (activated carbon, carbon black, carbon nanomaterials) impregnated to the metal-organic framework-5. We have attempted to synthesize carbon nanomaterials using indigenously fabricated chemical vapor deposition (CVD) unit as a support. We have observed an increase in the hydrogen storage capacities.

Forecasting carbon dioxide emissions based on a hybrid of mixed data sampling regression model and back propagation neural network in the USA.

PubMed

Zhao, Xin; Han, Meng; Ding, Lili; Calin, Adrian Cantemir

2018-01-01

The accurate forecast of carbon dioxide emissions is critical for policy makers to take proper measures to establish a low carbon society. This paper discusses a hybrid of the mixed data sampling (MIDAS) regression model and BP (back propagation) neural network (MIDAS-BP model) to forecast carbon dioxide emissions. Such analysis uses mixed frequency data to study the effects of quarterly economic growth on annual carbon dioxide emissions. The forecasting ability of MIDAS-BP is remarkably better than MIDAS, ordinary least square (OLS), polynomial distributed lags (PDL), autoregressive distributed lags (ADL), and auto-regressive moving average (ARMA) models. The MIDAS-BP model is suitable for forecasting carbon dioxide emissions for both the short and longer term. This research is expected to influence the methodology for forecasting carbon dioxide emissions by improving the forecast accuracy. Empirical results show that economic growth has both negative and positive effects on carbon dioxide emissions that last 15 quarters. Carbon dioxide emissions are also affected by their own change within 3 years. Therefore, there is a need for policy makers to explore an alternative way to develop the economy, especially applying new energy policies to establish a low carbon society.

Application of multiwalled carbon nanotubes as sorbents for the extraction of mycotoxins in water samples and infant milk formula prior to high performance liquid chromatography mass spectrometry analysis.

PubMed

Socas-Rodríguez, Bárbara; González-Sálamo, Javier; Hernández-Borges, Javier; Rodríguez Delgado, Miguel Ángel

2016-05-01

In this work, a simple and environmental friendly methodology has been developed for the analysis of a group of six mycotoxins with estrogenic activity produced by Fusarium species (i.e. zearalanone, zearalenone, α-zearalanol, β-zearalanol, α-zearalenol, and β-zearalenol), using microdispersive SPE the symbol micro should de before dSPE with multiwalled carbon nanotubes as sorbent. Separation, determination, and quantification were achieved by HPLC coupled to ion trap MS with an ESI interface. Parameters affecting the extraction efficiency of µ-dSPE such as pH of the sample, amount of multiwalled carbon nanotubes, and type and volume of elution solvent, were studied and optimized. The methodology was validated for mineral, pond, and wastewater as well as for powdered infant milk using 17β-estradiol-2,4,16,16,17-d5 (17β-E2 -D5 ) as internal standard, obtaining recoveries ranging from 85 to 120% for the three types of water samples and from 77 to 115% for powdered infant milk. RSD values were lower than 10%. The LOQs achieved were in the range 0.05-2.90 μg/L for water samples and 2.02-31.9 μg/L for powdered infant milk samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Bakhshi, Hamed; Shokuhfar, Ali; Vahdati, Nima

2016-09-01

Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C2H2) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C2H2 ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples' magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.

Composite electrodes of activated carbon derived from cassava peel and carbon nanotubes for supercapacitor applications

NASA Astrophysics Data System (ADS)

Taer, E.; Iwantono, Yulita, M.; Taslim, R.; Subagio, A.; Salomo, Deraman, M.

2013-09-01

In this paper, a composite electrode was prepared from a mixture of activated carbon derived from precarbonization of cassava peel (CP) and carbon nanotubes (CNTs). The activated carbon was produced by pyrolysis process using ZnCl2 as an activation agent. A N2 adsorption-desorption analysis for the sample indicated that the BET surface area of the activated carbon was 1336 m2 g-1. Difference percentage of CNTs of 0, 5, 10, 15 and 20% with 5% of PVDF binder were added into CP based activated carbon in order to fabricate the composite electrodes. The morphology and structure of the composite electrodes were investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. The SEM image observed that the distribution of CNTs was homogeneous between carbon particles and the XRD pattern shown the amorphous structure of the sample. The electrodes were fabricated for supercapacitor cells with 316L stainless steel as current collector and 1 M sulfuric acid as electrolyte. An electrochemical characterization was performed by using an electrochemical impedance spectroscopy (EIS) method using a Solatron 1286 instrument and the addition of CNTs revealed to improve the resistant and capacitive properties of supercapacitor cell.

Structural and surface changes in glassy carbon due to strontium implantation and heat treatment

NASA Astrophysics Data System (ADS)

Odutemowo, O. S.; Malherbe, J. B.; Prinsloo, L. C.; Njoroge, E. G.; Erasmus, R.; Wendler, E.; Undisz, A.; Rettenmayr, M.

2018-01-01

There are still questions around the microstructure of glassy carbon (GC), like the observation of the micropores. These were proposed to explain the low density of GC. This paper explains the effect of ion bombardment (200 keV Sr+, 1 × 1016 Sr+/cm2 at RT) on the microstructure of GC. TEM and AFM show that micropores in pristine GC are destroyed leading to densification of GC from 1.42 g/cm3 to 2.03 g/cm3. The amorphisation of glassy carbon was also not complete with graphitic strands embedded within the GC. These were relatively few, as Raman analysis showed that the Sr implantation resulted in a typical amorphous Raman spectrum. Annealing of the sample at 900 °C only resulted in a slight recovery of the GC structure. AFM and SEM analysis showed that the surface of the sample became rougher after Sr implantation. The roughness increased after the sample was annealed at 600 °C due to segregation of Sr towards the surface of the GC. SEM measurements of a sample with both implanted and un-implanted edges after annealing at 900 °C, showed that the high temperature heat treatment did not affect the surface topography of un-irradiated GC.

Fabrication of a Low Density Carbon Fiber Foam and Its Characterization as a Strain Gauge

PubMed Central

Luhrs, Claudia C.; Daskam, Chris D.; Gonzalez, Edwin; Phillips, Jonathan

2014-01-01

Samples of carbon nano-fiber foam (CFF), essentially a 3D solid mat of intertwined nanofibers of pure carbon, were grown using the Constrained Formation of Fibrous Nanostructures (CoFFiN) process in a steel mold at 550 °C from a palladium particle catalysts exposed to fuel rich mixtures of ethylene and oxygen. The resulting material was studied using Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDX), Surface area analysis (BET), and Thermogravimetric Analysis (TGA). Transient and dynamic mechanical tests clearly demonstrated that the material is viscoelastic. Concomitant mechanical and electrical testing of samples revealed the material to have electrical properties appropriate for application as the sensing element of a strain gauge. The sample resistance versus strain values stabilize after a few compression cycles to show a perfectly linear relationship. Study of microstructure, mechanical and electrical properties of the low density samples confirm the uniqueness of the material: It is formed entirely of independent fibers of diverse diameters that interlock forming a tridimensional body that can be grown into different shapes and sizes at moderate temperatures. It regains its shape after loads are removed, is light weight, presents viscoelastic behavior, thermal stability up to 550 °C, hydrophobicity, and is electrically conductive. PMID:28788644

A large column analog experiment of stable isotope variations during reactive transport: II. Carbon mass balance, microbial community structure and predation

NASA Astrophysics Data System (ADS)

Druhan, Jennifer L.; Bill, Markus; Lim, HsiaoChien; Wu, Cindy; Conrad, Mark E.; Williams, Kenneth H.; DePaolo, Donald J.; Brodie, Eoin L.

2014-01-01

Here we report a combined analysis of carbon mass balance based on isotopic labeling and microbiological characterization during organic carbon stimulated bioreduction of a subsurface sediment in a large laboratory column experimental system. This combination of approaches allows quantification of both the cycling of carbon through multiple redox pathways and the associated spatial and temporal evolution of bacterial communities in response to this nutrient source. Carbon isotope mass balance facilitated by the use of 13C-labeled acetate as the electron donor showed evidence for a net loss of sediment organic carbon over the course of the amendment experiment. Furthermore, these data clearly demonstrated a source of isotopically labeled inorganic carbon that was not attributable to primary metabolism by acetate-oxidizing microorganisms. Fluid samples collected weekly over the duration of the 43-day amendment at <20 cm intervals along the flow path were analyzed for microbial composition by pyrosequencing of ribosomal RNA genes. The microbial community composition was transient, with distinct occurrences of Azoarcus, Geobacter and multiple sulfate reducing species over the course of the experiment. In combination with DNA sequencing data, the anomalous carbon cycling process is shown to occur exclusively during the period of predominant Geobacter species growth. Pyrosequencing indicated, and targeted cloning and sequencing confirmed the presence of several bacteriovorous protozoa, including species of the Breviata, Planococcus and Euplotes genera. Cloning and qPCR analysis demonstrated that Euplotes species were most abundant and displayed a growth trajectory that closely followed that of the Geobacter population. These results suggest a previously undocumented secondary turnover of biomass carbon related to protozoan grazing that was not sufficiently prevalent to be observed in bulk concentrations of carbon species in the system, but was clearly identified in the partitioning of carbon isotopes. This study demonstrates evidence for predator-prey relationships that impact subsurface microbial community dynamics and provides a novel indication of the impact of this relationship on the flux of carbon through a system via the microbial biomass pool. Overall, our approach provides high temporal and spatial sampling resolution at field relevant flow rates, while minimizing effects of mixing and transverse dispersion. The result is a quantitative carbon budget accounting for a diversity of processes that should be considered for inclusion in reactive transport models that aim to predict carbon turnover, nutrient flux, and redox reactions in natural and stimulated subsurface systems. the mobilization of previously stabilized, sediment-bound carbon; a carbon mass balance for a through-flowing sediment column over the course of a 43-day amendment using 13C-labeled acetate; a phylogenetic microbial community structure at <20 cm sampling resolution with distance away from the organic carbon source weekly over the 43-day amendment; protozoan grazing on the active Geobacteraceae population and the rapid turnover of microbial biomass carbon as a secondary cycling pathway. Such a high resolution, combined analysis of microbial populations and the associated carbon mass balance in a through-flowing system at field relevant flow rates provides novel, quantitative insights into the interface between biogeochemical cycling and bulk carbon fluxes in the near-surface environment.

Magnetic N-doped mesoporous carbon as an adsorbent for the magnetic solid-phase extraction of phthalate esters from soft drinks.

PubMed

Li, Menghua; Jiao, Caina; Yang, Xiumin; Wang, Chun; Wu, Qiuhua; Wang, Zhi

2017-04-01

A new kind of magnetic N-doped mesoporous carbon was prepared by the one-step carbonization of a hybrid precursor (glucose, melamine, and iron chloride) in a N 2 atmosphere with a eutectic salt (KCl/ZnCl 2 ) as the porogen. The obtained magnetic N-doped mesoporous carbon showed excellent characteristics, such as strong magnetic response, high surface area, large pore volume, and abundant π-electron system, which endow it with a great potential as a magnetic solid-phase extraction adsorbent. To evaluate its adsorption performance, the magnetic N-doped mesoporous carbon was used for the extraction of three phthalate esters from soft drink samples followed by high-performance liquid chromatographic analysis. Under the optimum conditions, the developed method showed a good linearity (1.0-120.0 ng/mL), low limit of detection (0.1-0.3 ng/mL, S/N = 3), and good recoveries (83.2-119.0%) in soft drink samples. The results indicated that the magnetic N-doped mesoporous carbon has an excellent adsorption capacity for phthalate esters and the present method is simple, accurate, and highly efficient for the extraction and determination of phthalate esters in complex matrix samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Developing and evaluating rapid field methods to estimate peat carbon

Treesearch

Rodney A. Chimner; Cassandra A. Ott; Charles H. Perry; Randall K. Kolka

2014-01-01

Many international protocols (e.g., REDD+) are developing inventories of ecosystem carbon stocks and fluxes at country and regional scales, which can include peatlands. As the only nationally implemented field inventory and remeasurement of forest soils in the US, the USDA Forest Service Forest Inventory and Analysis Program (FIA) samples the top 20 cm of organic soils...

Selectivity and limitations of carbon sorption tubes for capturing siloxanes in biogas during field sampling.

PubMed

Tansel, Berrin; Surita, Sharon C

2016-06-01

Siloxane levels in biogas can jeopardize the warranties of the engines used at the biogas to energy facilities. The chemical structure of siloxanes consists of silicon and oxygen atoms, alternating in position, with hydrocarbon groups attached to the silicon side chain. Siloxanes can be either in cyclic (D) or linear (L) configuration and referred with a letter corresponding to their structure followed by a number corresponding to the number of silicon atoms present. When siloxanes are burned, the hydrocarbon fraction is lost and silicon is converted to silicates. The purpose of this study was to evaluate the adequacy of activated carbon gas samplers for quantitative analysis of siloxanes in biogas samples. Biogas samples were collected from a landfill and an anaerobic digester using multiple carbon sorbent tubes assembled in series. One set of samples was collected for 30min (sampling 6-L gas), and the second set was collected for 60min (sampling 12-L gas). Carbon particles were thermally desorbed and analyzed by Gas Chromatography Mass Spectrometry (GC/MS). The results showed that biogas sampling using a single tube would not adequately capture octamethyltrisiloxane (L3), hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6). Even with 4 tubes were used in series, D5 was not captured effectively. The single sorbent tube sampling method was adequate only for capturing trimethylsilanol (TMS) and hexamethyldisiloxane (L2). Affinity of siloxanes for activated carbon decreased with increasing molecular weight. Using multiple carbon sorbent tubes in series can be an appropriate method for developing a standard procedure for determining siloxane levels for low molecular weight siloxanes (up to D3). Appropriate quality assurance and quality control procedures should be developed for adequately quantifying the levels of the higher molecular weight siloxanes in biogas with sorbent tubes. Copyright © 2016 Elsevier Ltd. All rights reserved.

Feasibility of coupling a thermal/optical carbon analyzer to a quadrupole mass spectrometer for enhanced PM2.5 speciation.

PubMed

Riggio, Gustavo M; Chow, Judith C; Cropper, Paul M; Wang, Xiaoliang; Yatavelli, Reddy L N; Yang, Xufei; Watson, John G

2018-05-01

A thermal/optical carbon analyzer (TOA), normally used for quantification of organic carbon (OC) and elemental carbon (EC) in PM 2.5 (fine particulate matter) speciation networks, was adapted to direct thermally evolved gases to an electron impact quadrupole mass spectrometer (QMS), creating a TOA-QMS. This approach produces spectra similar to those obtained by the Aerodyne aerosol mass spectrometer (AMS), but the ratios of the mass to charge (m/z) signals differ and must be remeasured using laboratory-generated standards. Linear relationships are found between TOA-QMS signals and ammonium (NH 4 + ), nitrate (NO 3 - ), and sulfate (SO 4 2- ) standards. For ambient samples, however, positive deviations are found for SO 4 2- , compensated by negative deviations for NO 3 - , at higher concentrations. This indicates the utility of mixed-compound standards for calibration or separate calibration curves for low and high ion concentrations. The sum of the QMS signals across all m/z after removal of the NH 4 + , NO 3 - , and SO 4 2- signals was highly correlated with the carbon content of oxalic acid (C₂H₂O₄) standards. For ambient samples, the OC derived from the TOA-QMS method was the same as the OC derived from the standard IMPROVE_A TOA method. This method has the potential to reduce complexity and costs for speciation networks, especially for highly polluted urban areas such as those in Asia and Africa. Ammonium, nitrate, and sulfate can be quantified by the same thermal evolution analysis applied to organic and elemental carbon. This holds the potential to replace multiple parallel filter samples and separate laboratory analyses with a single filter and a single analysis to account for a large portion of the PM 2.5 mass concentration.

Research and development of a luminol-carbon monoxide flow system

NASA Technical Reports Server (NTRS)

Thomas, R. R.

1977-01-01

Adaption of the luminol-carbon monoxide injection system to a flowing type system is reported. Analysis of actual wastewater samples was carried out and revealed that bacteria can be associated with particles greater than 10 microns in size in samples such as mixed liquor. Research into the luminol reactive oxidation state indicates that oxidized iron porphyrins, cytochrome-c in particular, produce more luminol chemiluminescence than the reduced form. Correlation exists between the extent of porphyrin oxidation and relative chemiluminescence. In addition, the porphyrin nucleus is apparently destroyed under the current chemiluminescent reaction conditions.

Constraints on primary and secondary particulate carbon sources using chemical tracer and 14C methods during CalNex-Bakersfield

NASA Astrophysics Data System (ADS)

Sheesley, Rebecca J.; Nallathamby, Punith Dev; Surratt, Jason D.; Lee, Anita; Lewandowski, Michael; Offenberg, John H.; Jaoui, Mohammed; Kleindienst, Tadeusz E.

2017-10-01

The present study investigates primary and secondary sources of organic carbon for Bakersfield, CA, USA as part of the 2010 CalNex study. The method used here involves integrated sampling that is designed to allow for detailed and specific chemical analysis of particulate matter (PM) in the Bakersfield airshed. To achieve this objective, filter samples were taken during thirty-four 23-hr periods between 19 May and 26 June 2010 and analyzed for organic tracers by gas chromatography - mass spectrometry (GC-MS). Contributions to organic carbon (OC) were determined by two organic tracer-based techniques: primary OC by chemical mass balance and secondary OC by a mass fraction method. Radiocarbon (14C) measurements of the total organic carbon were also made to determine the split between the modern and fossil carbon and thereby constrain unknown sources of OC not accounted for by either tracer-based attribution technique. From the analysis, OC contributions from four primary sources and four secondary sources were determined, which comprised three sources of modern carbon and five sources of fossil carbon. The major primary sources of OC were from vegetative detritus (9.8%), diesel (2.3%), gasoline (<1.0%), and lubricating oil impacted motor vehicle exhaust (30%); measured secondary sources resulted from isoprene (1.5%), α-pinene (<1.0%), toluene (<1.0%), and naphthalene (<1.0%, as an upper limit) contributions. The average observed organic carbon (OC) was 6.42 ± 2.33 μgC m-3. The 14C derived apportionment indicated that modern and fossil components were nearly equivalent on average; however, the fossil contribution ranged from 32 to 66% over the five week campaign. With the fossil primary and secondary sources aggregated, only 25% of the fossil organic carbon could not be attributed. Whereas, nearly 80% of the modern carbon could not be attributed to primary and secondary sources accessible to this analysis, which included tracers of biomass burning, vegetative detritus and secondary biogenic carbon. The results of the current study contributes source-based evaluation of the carbonaceous aerosol at CalNex Bakersfield.

Constraints on primary and secondary particulate carbon sources using chemical tracer and 14C methods during CalNex-Bakersfield

PubMed Central

Sheesley, Rebecca J.; Nallathamby, Punith Dev; Surratt, Jason D.; Lee, Anita; Lewandowski, Michael; Offenberg, John H.; Jaoui, Mohammed; Kleindienst, Tadeusz E.

2018-01-01

The present study investigates primary and secondary sources of organic carbon for Bakersfield, CA, USA as part of the 2010 CalNex study. The method used here involves integrated sampling that is designed to allow for detailed and specific chemical analysis of particulate matter (PM) in the Bakersfield airshed. To achieve this objective, filter samples were taken during thirty-four 23-hr periods between 19 May and 26 June 2010 and analyzed for organic tracers by gas chromatography – mass spectrometry (GC-MS). Contributions to organic carbon (OC) were determined by two organic tracer-based techniques: primary OC by chemical mass balance and secondary OC by a mass fraction method. Radiocarbon (14C) measurements of the total organic carbon were also made to determine the split between the modern and fossil carbon and thereby constrain unknown sources of OC not accounted for by either tracer-based attribution technique. From the analysis, OC contributions from four primary sources and four secondary sources were determined, which comprised three sources of modern carbon and five sources of fossil carbon. The major primary sources of OC were from vegetative detritus (9.8%), diesel (2.3%), gasoline (<1.0%), and lubricating oil impacted motor vehicle exhaust (30%); measured secondary sources resulted from isoprene (1.5%), α-pinene (<1.0%), toluene (<1.0%), and naphthalene (<1.0%, as an upper limit) contributions. The average observed organic carbon (OC) was 6.42 ± 2.33 μgC m−3. The 14C derived apportionment indicated that modern and fossil components were nearly equivalent on average; however, the fossil contribution ranged from 32-66% over the five week campaign. With the fossil primary and secondary sources aggregated, only 25% of the fossil organic carbon could not be attributed. Whereas, nearly 80% of the modern carbon could not be attributed to primary and secondary sources accessible to this analysis, which included tracers of biomass burning, vegetative detritus and secondary biogenic carbon. The results of the current study contributes source-based evaluation of the carbonaceous aerosol at CalNex Bakersfield. PMID:29681757

Sequential derivatization of polar organic compounds in cloud water using O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride, N,O-bis(trimethylsilyl)trifluoroacetamide, and gas-chromatography/mass spectrometry analysis.

PubMed

Sagona, Jessica A; Dukett, James E; Hawley, Harmonie A; Mazurek, Monica A

2014-10-03

Cloud water samples from Whiteface Mountain, NY were used to develop a combined sampling and gas chromatography-mass spectrometric (GCMS) protocol for evaluating the complex mixture of highly polar organic compounds (HPOC) present in this atmospheric medium. Specific HPOC of interest were mono- and di keto-acids which are thought to originate from photochemical reactions of volatile unsaturated hydrocarbons from biogenic and manmade emissions and be a major fraction of atmospheric carbon. To measure HPOC mixtures and the individual keto-acids in cloud water, samples first must be derivatized for clean elution and measurement, and second, have low overall background of the target species as validated by GCMS analysis of field and laboratory blanks. Here, we discuss a dual derivatization method with PFBHA and BSTFA which targets only organic compounds that contain functional groups reacting with both reagents. The method also reduced potential contamination by minimizing the amount of sample processing from the field through the GCMS analysis steps. Once derivatized only gas chromatographic separation and selected ion monitoring (SIM) are needed to identify and quantify the polar organic compounds of interest. Concentrations of the detected total keto-acids in individual cloud water samples ranged from 27.8 to 329.3ngmL(-1) (ppb). Method detection limits for the individual HPOC ranged from 0.17 to 4.99ngmL(-1) and the quantification limits for the compounds ranged from 0.57 to 16.64ngmL(-1). The keto-acids were compared to the total organic carbon (TOC) results for the cloud water samples with concentrations of 0.607-3.350mgL(-1) (ppm). GCMS analysis of all samples and blanks indicated good control of the entire collection and analysis steps. Selected ion monitoring by GCMS of target keto-acids was essential for screening the complex organic carbon mixtures present at low ppb levels in cloud water. It was critical for ensuring high levels of quality assurance and quality control and for the correct identification and quantification of key marker compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

Phenotypic constraints promote latent versatility and carbon efficiency in metabolic networks.

PubMed

Bardoscia, Marco; Marsili, Matteo; Samal, Areejit

2015-07-01

System-level properties of metabolic networks may be the direct product of natural selection or arise as a by-product of selection on other properties. Here we study the effect of direct selective pressure for growth or viability in particular environments on two properties of metabolic networks: latent versatility to function in additional environments and carbon usage efficiency. Using a Markov chain Monte Carlo (MCMC) sampling based on flux balance analysis (FBA), we sample from a known biochemical universe random viable metabolic networks that differ in the number of directly constrained environments. We find that the latent versatility of sampled metabolic networks increases with the number of directly constrained environments and with the size of the networks. We then show that the average carbon wastage of sampled metabolic networks across the constrained environments decreases with the number of directly constrained environments and with the size of the networks. Our work expands the growing body of evidence about nonadaptive origins of key functional properties of biological networks.

RADIOCARBON ANALYSIS OF PM 2.5 AMBIENT AEROSOL

EPA Science Inventory

The radiocarbon (14C) content of an ambient aerosol sample can be directly related to the fraction of the sample's total carbon mass contributed by natural (biogenic) sources. Such knowledge is difficult to determine by other means, and important for devising ambient PM contro...

A procedure for partitioning bulk sediments into distinct grain-size fractions for geochemical analysis

USGS Publications Warehouse

Barbanti, A.; Bothner, Michael H.

1993-01-01

A method to separate sediments into discrete size fractions for geochemical analysis has been tested. The procedures were chosen to minimize the destruction or formation of aggregates and involved gentle sieving and settling of wet samples. Freeze-drying and sonication pretreatments, known to influence aggregates, were used for comparison. Freeze-drying was found to increase the silt/clay ratio by an average of 180 percent compared to analysis of a wet sample that had been wet sieved only. Sonication of a wet sample decreased the silt/clay ratio by 51 percent. The concentrations of metals and organic carbon in the separated fractions changed depending on the pretreatment procedures in a manner consistent with the hypothesis that aggregates consist of fine-grained organic- and metal-rich particles. The coarse silt fraction of a freeze-dried sample contained 20–44 percent higher concentrations of Zn, Cu, and organic carbon than the coarse silt fraction of the wet sample. Sonication resulted in concentrations of these analytes that were 18–33 percent lower in the coarse silt fraction than found in the wet sample. Sonication increased the concentration of lead in the clay fraction by an average of 40 percent compared to an unsonicated sample. Understanding the magnitude of change caused by different analysis protocols is an aid in designing future studies that seek to interpret the spatial distribution of contaminated sediments and their transport mechanisms.

Analysis of PEG oligomers in black gel inks: Discrimination and ink dating.

PubMed

Sun, Qiran; Luo, Yiwen; Xiang, Ping; Yang, Xu; Shen, Min

2017-08-01

Carbon-based black gel inks are common samples in forensic practice of questioned document examination in China, but there are few analytical methods for this type of ink. In this study, a liquid chromatography-.high resolution mass spectrometry (LC-HRMS) method was established for the analysis of PEG oligomers in carbon-based black gel ink entries. The coupled instruments achieve both the identification and quantification of PEG oligomers in ink entries with reproducible results. Twenty carbon-based black gel inks, whose Raman spectra appeared identical, were analyzed using the LC-HRMS method. As a result, the twenty gel inks were classified into four groups according to the distribution of PEG oligomers. Artificially aging of PEG 400 and a gel ink showed that as PEG degraded, the relative amounts of low molecular weight PEG oligomers increased, while those of high molecular weight decreased. The degradation of PEG oligomers in a naturally aged gel ink was consistent with those in the artificially aged samples, but occurred more slowly. This study not only provided a new method for discriminating carbon-based black gel ink entries, but also offered a new approach for studying the relative ink dating of carbon-based black gel ink entries. Copyright © 2017 Elsevier B.V. All rights reserved.

A New Method for Carbon Isotopic Analysis of Nanogram Quantities of Carbon from Dissolved Chitin Using A Spooling-wire Microcombustion Interface

NASA Astrophysics Data System (ADS)

Zhao, Y.; Nelson, D. M.; Clegg, B. F.; Berry, J.; Hu, F.

2016-12-01

δ13C analysis of specific taxa or compounds is commonly used for investigating past environmental change, including methane dynamics in lakes. However, most analytical methods require large sample sizes, prohibiting routine analysis of fossils of individual taxa found in sediment deposits. For example, 10-100 individual head capsules of fossil midges are required for δ13C analysis using an elemental analyzer (EA) interfaced with an isotope-ratio mass spectrometer (IRMS). Here we present a new method that uses a spooling-wire microcombustion (SWiM) device interfaced with an IRMS for measuring δ13C values of carbon dissolved from individual head capsules of chitinous aquatic zooplankton. We extracted chitin (a major biochemical component of insect exoskeleton) from modern midge material obtained from four commercial suppliers. We first assessed the effects of sample treatments on carbon yields and δ13C values of dissolved chitin by varying the concentration of HCl used for dissolution, the duration of reaction in HCl, and the temperature of dissolution. We then investigated potential fractionation of carbon isotopes associated with chitin dissolution, by comparing δ13C values of dissolved chitin obtained via SWiM-IRMS with those from untreated head capsules obtained via a EA-IRMS. The average δ13C values of untreated head capsules varied between -25.1 and -30.1‰. Higher acid concentrations and temperatures, as well as longer reaction times, increased dissolution of carbon from the head capsules and the precision of δ13C values. For example, carbon yields from reaction of head capsules with 6N HCl at 25°C increased from 1 to 3 Vs as reaction times increased from 1 to 24 hours. Acid concentration and reaction time had the greatest influence on carbon yields and isotopic precision. The δ13C values of dissolved chitin mirrored the δ13C values of untreated head capsules with minimal offset of absolute values, which suggests no systematic fractionation associated with dissolution. Overall, these results indicate that carbon isotopic analysis of dissolved chitin using the SWiM-IRMS system offers a reliable new method to determine taxa-specific δ13C values for chitinous aquatic zooplankton. In ongoing work, we are applying this tool to reconstruct past methane dynamics in Arctic lakes during the Holocene.

Exploring effective sampling design for monitoring soil organic carbon in degraded Tibetan grasslands.

PubMed

Chang, Xiaofeng; Bao, Xiaoying; Wang, Shiping; Zhu, Xiaoxue; Luo, Caiyun; Zhang, Zhenhua; Wilkes, Andreas

2016-05-15

The effects of climate change and human activities on grassland degradation and soil carbon stocks have become a focus of both research and policy. However, lack of research on appropriate sampling design prevents accurate assessment of soil carbon stocks and stock changes at community and regional scales. Here, we conducted an intensive survey with 1196 sampling sites over an area of 190 km(2) of degraded alpine meadow. Compared to lightly degraded meadow, soil organic carbon (SOC) stocks in moderately, heavily and extremely degraded meadow were reduced by 11.0%, 13.5% and 17.9%, respectively. Our field survey sampling design was overly intensive to estimate SOC status with a tolerable uncertainty of 10%. Power analysis showed that the optimal sampling density to achieve the desired accuracy would be 2, 3, 5 and 7 sites per 10 km(2) for lightly, moderately, heavily and extremely degraded meadows, respectively. If a subsequent paired sampling design with the optimum sample size were performed, assuming stock change rates predicted by experimental and modeling results, we estimate that about 5-10 years would be necessary to detect expected trends in SOC in the top 20 cm soil layer. Our results highlight the utility of conducting preliminary surveys to estimate the appropriate sampling density and avoid wasting resources due to over-sampling, and to estimate the sampling interval required to detect an expected sequestration rate. Future studies will be needed to evaluate spatial and temporal patterns of SOC variability. Copyright © 2016. Published by Elsevier Ltd.

Determination of mutagenic amines in water and food samples by high pressure liquid chromatography with amperometric detection using a multiwall carbon nanotubes-glassy carbon electrode.

PubMed

Bueno, Ana María; Marín, Miguel Ángel; Contento, Ana María; Ríos, Ángel

2016-02-01

A chromatographic method, using amperometric detection, for the sensitive determination of six representative mutagenic amines was developed. A glassy carbon electrode (GCE), modified with multiwall carbon nanotubes (GCE-CNTs), was prepared and its response compared to a conventional glassy carbon electrode. The chromatographic method (HPLC-GCE-CNTs) allowed the separation and the determination of heterocyclic aromatic amines (HAAs) classified as mutagenic amines by the International Agency for Research of Cancer. The new electrode was systematically studied in terms of stability, sensitivity, and reproducibility. Statistical analysis of the obtained data demonstrated that the modified electrode provided better sensitivity than the conventional unmodified ones. Detection limits were in the 3.0 and 7.5 ng/mL range, whereas quantification limits ranged between 9.5 and 25.0 ng/mL were obtained. The applicability of the method was demonstrated by the determination of the amines in several types of samples (water and food samples). Recoveries indicate very good agreement between amounts added and those found for all HAAs (recoveries in the 92% and 105% range). Copyright © 2015 Elsevier Ltd. All rights reserved.

Control of Origin of Sesame Oil from Various Countries by Stable Isotope Analysis and DNA Based Markers—A Pilot Study

PubMed Central

Horacek, Micha; Hansel-Hohl, Karin; Burg, Kornel; Soja, Gerhard; Okello-Anyanga, Walter; Fluch, Silvia

2015-01-01

The indication of origin of sesame seeds and sesame oil is one of the important factors influencing its price, as it is produced in many regions worldwide and certain provenances are especially sought after. We joined stable carbon and hydrogen isotope analysis with DNA based molecular marker analysis to study their combined potential for the discrimination of different origins of sesame seeds. For the stable carbon and hydrogen isotope data a positive correlation between both isotope parameters was observed, indicating a dominant combined influence of climate and water availability. This enabled discrimination between sesame samples from tropical and subtropical/moderate climatic provenances. Carbon isotope values also showed differences between oil from black and white sesame seeds from identical locations, indicating higher water use efficiency of plants producing black seeds. DNA based markers gave independent evidence for geographic variation as well as provided information on the genetic relatedness of the investigated samples. Depending on the differences in ambient environmental conditions and in the genotypic fingerprint, a combination of both analytical methods is a very powerful tool to assess the declared geographic origin. To our knowledge this is the first paper on food authenticity combining the stable isotope analysis of bio-elements with DNA based markers and their combined statistical analysis. PMID:25831054

Control of origin of sesame oil from various countries by stable isotope analysis and DNA based markers--a pilot study.

PubMed

Horacek, Micha; Hansel-Hohl, Karin; Burg, Kornel; Soja, Gerhard; Okello-Anyanga, Walter; Fluch, Silvia

2015-01-01

The indication of origin of sesame seeds and sesame oil is one of the important factors influencing its price, as it is produced in many regions worldwide and certain provenances are especially sought after. We joined stable carbon and hydrogen isotope analysis with DNA based molecular marker analysis to study their combined potential for the discrimination of different origins of sesame seeds. For the stable carbon and hydrogen isotope data a positive correlation between both isotope parameters was observed, indicating a dominant combined influence of climate and water availability. This enabled discrimination between sesame samples from tropical and subtropical/moderate climatic provenances. Carbon isotope values also showed differences between oil from black and white sesame seeds from identical locations, indicating higher water use efficiency of plants producing black seeds. DNA based markers gave independent evidence for geographic variation as well as provided information on the genetic relatedness of the investigated samples. Depending on the differences in ambient environmental conditions and in the genotypic fingerprint, a combination of both analytical methods is a very powerful tool to assess the declared geographic origin. To our knowledge this is the first paper on food authenticity combining the stable isotope analysis of bio-elements with DNA based markers and their combined statistical analysis.

Proteomic analysis of carbon concentrating chemolithotrophic bacteria Serratia sp. for sequestration of carbon dioxide.

PubMed

Bharti, Randhir K; Srivastava, Shaili; Thakur, Indu Shekhar

2014-01-01

A chemolithotrophic bacterium enriched in the chemostat in presence of sodium bicarbonate as sole carbon source was identified as Serratia sp. by 16S rRNA sequencing. Carbon dioxide sequestering capacity of bacterium was detected by carbonic anhydrase enzyme and ribulose-1, 5- bisphosphate carboxylase/oxygenase (RuBisCO). The purified carbonic anhydrase showed molecular weight of 29 kDa. Molecular weight of RuBisCO was 550 kDa as determined by fast protein liquid chromatography (FPLC), however, sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) showed presence of two subunits whose molecular weights were 56 and 14 kDa. The Western blot analysis of the crude protein and purified sample cross reacted with RuBisCO large-subunit polypeptides antibodies showed strong band pattern at molecular weight around 56 kDa regions. Whole cell soluble proteins of Serratia sp. grown under autotrophic and heterotrophic conditions were resolved by two-dimensional gel electrophoresis and MALDI-TOF/MS for differential expression of proteins. In proteomic analysis of 63 protein spots, 48 spots were significantly up-regulated in the autotrophically grown cells; seven enzymes showed its utilization in autotrophic carbon fixation pathways and other metabolic activities of bacterium including lipid metabolisms indicated sequestration potency of carbon dioxide and production of biomaterials.

Proteomic Analysis of Carbon Concentrating Chemolithotrophic Bacteria Serratia sp. for Sequestration of Carbon Dioxide

PubMed Central

Bharti, Randhir K.; Srivastava, Shaili; Thakur, Indu Shekhar

2014-01-01

A chemolithotrophic bacterium enriched in the chemostat in presence of sodium bicarbonate as sole carbon source was identified as Serratia sp. by 16S rRNA sequencing. Carbon dioxide sequestering capacity of bacterium was detected by carbonic anhydrase enzyme and ribulose-1, 5- bisphosphate carboxylase/oxygenase (RuBisCO). The purified carbonic anhydrase showed molecular weight of 29 kDa. Molecular weight of RuBisCO was 550 kDa as determined by fast protein liquid chromatography (FPLC), however, sodium dodecyl sulphate polyacrylamide gel electrophoresis (SDS-PAGE) showed presence of two subunits whose molecular weights were 56 and 14 kDa. The Western blot analysis of the crude protein and purified sample cross reacted with RuBisCO large-subunit polypeptides antibodies showed strong band pattern at molecular weight around 56 kDa regions. Whole cell soluble proteins of Serratia sp. grown under autotrophic and heterotrophic conditions were resolved by two-dimensional gel electrophoresis and MALDI-TOF/MS for differential expression of proteins. In proteomic analysis of 63 protein spots, 48 spots were significantly up-regulated in the autotrophically grown cells; seven enzymes showed its utilization in autotrophic carbon fixation pathways and other metabolic activities of bacterium including lipid metabolisms indicated sequestration potency of carbon dioxide and production of biomaterials. PMID:24619032

Trace level and highly selective determination of urea in various real samples based upon voltammetric analysis of diacetylmonoxime-urea reaction product on the carbon nanotube/carbon paste electrode.

PubMed

Alizadeh, Taher; Ganjali, Mohammad Reza; Rafiei, Faride

2017-06-29

In this study an innovative method was introduced for selective and precise determination of urea in various real samples including urine, blood serum, soil and water. The method was based on the square wave voltammetry determination of an electroactive product, generated during diacetylmonoxime reaction with urea. A carbon paste electrode, modified with multi-walled carbon nanotubes (MWCNTs) was found to be an appropriate electrochemical transducer for recording of the electrochemical signal. It was found that the chemical reaction conditions influenced the analytical signal directly. The calibration graph of the method was linear in the range of 1 × 10 -7 - 1 × 10 -2  mol L -1 . The detection limit was calculated to be 52 nmol L -1 . Relative standard error of the method was also calculated to be 3.9% (n = 3). The developed determination procedure was applied for urea determination in various real samples including soil, urine, plasma and water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

SEM morphological studies of carbonates and the search for ancient life on Mars

NASA Astrophysics Data System (ADS)

D'Elia, M.; Blanco, A.; Galiano, A.; Orofino, V.; Fonti, S.; Mancarella, F.; Guido, A.; Russo, F.; Mastandrea, A.

2017-04-01

Next space missions will investigate the possibility of extinct or extant life on Mars. Studying the infrared spectral modifications, induced by thermal processing on different carbonate samples (recent shells and fossils of different ages), we developed a method able to discriminate biogenic carbonates from their abiogenic counterparts. The method has been successfully applied to microbialites, i.e. bio-induced carbonates deposits, and particularly to stromatolites, the laminated fabric of microbialites, some of which can be ascribed to among the oldest traces of biological activity known on Earth. These results are of valuable importance since such carbonates are linked to primitive living organisms that can be considered as good analogues for putative Martian life forms. Considering that the microstructures of biogenic carbonate are different from those of abiogenic origin, we investigated the micromorphology of shells, skeletal grains and microbialites at different scale with a scanning electron microscope. The results show that this line of research may provide an alternative and complementary approach to other techniques developed in the past by our group to distinguish biotic from abiotic carbonates. In this paper, we present some results that can be of valuable interest since they demonstrate the utility for a database of images concerning the structures and textures of relevant carbonate minerals. Such data may be useful for the analysis of Martian samples, coming from sample return missions or investigated by future in situ explorations, aimed to characterize the near-subsurface of Mars in search for past or present life.

The feasibility of TEA CO2 laser-induced plasma for spectrochemical analysis of geological samples in simulated Martian conditions

NASA Astrophysics Data System (ADS)

Savovic, Jelena; Stoiljkovic, Milovan; Kuzmanovic, Miroslav; Momcilovic, Milos; Ciganovic, Jovan; Rankovic, Dragan; Zivkovic, Sanja; Trtica, Milan

2016-04-01

The present work studies the possibility of using pulsed Transversely Excited Atmospheric (TEA) carbon dioxide laser as an energy source for laser-induced breakdown spectroscopy (LIBS) analysis of rocks under simulated Martian atmospheric conditions. Irradiation of a basaltic rock sample with the laser intensity of 56 MW cm- 2, in carbon-dioxide gas at a pressure of 9 mbar, created target plasma with favorable conditions for excitation of all elements usually found in geological samples. Detection limits of minor constituents (Ba, Cr, Cu, Mn, Ni, Sr, V, and Zr) were in the 3 ppm-30 ppm range depending on the element. The precision varied between 5% and 25% for concentration levels of 1% to 10 ppm, respectively. Generally, the proposed relatively simple TEA CO2 laser-LIBS system provides good sensitivity for geological studies under reduced CO2 pressure.

Fire assisted pastoralism vs. sustainable forestry--the implications of missing markets for carbon in determining optimal land use in the wet-dry tropics of Australia.

PubMed

Ockwell, David; Lovett, Jon C

2005-04-01

Using Cape York Peninsula, Queensland, Australia as a case study, this paper combines field sampling of woody vegetation with cost-benefit analysis to compare the social optimality of fire-assisted pastoralism with sustainable forestry. Carbon sequestration is estimated to be significantly higher in the absence of fire. Integration of carbon sequestration benefits for mitigating future costs of climate change into cost-benefit analysis demonstrates that sustainable forestry is a more socially optimal land use than fire-assisted pastoralism. Missing markets for carbon, however, imply that fire-assisted pastoralism will continue to be pursued in the absence of policy intervention. Creation of markets for carbon represents a policy solution that has the potential to drive land use away from fire-assisted pastoralism towards sustainable forestry and environmental conservation.

Assessment of diagenetic alteration of dinosaur eggshells through petrography and geochemical analysis

NASA Astrophysics Data System (ADS)

Enriquez, M. V.; Eagle, R.; Eiler, J. M.; Tripati, A. K.; Ramirez, P. C.; Loyd, S. J.; Chiappe, L.; Montanari, S.; Norell, M.; Tuetken, T.

2012-12-01

Carbonate clumped isotope analysis of fossil eggshells has the potential to constrain both the physiology of extinct animals and, potentially, paleoenvironmental conditions, especially when coupled with isotopic measurements of co-occurring soil carbonates. Eggshell samples from both modern vertebrates and Cretaceous Hadrosaurid, Oviraptorid, Titanosaur, Hypselosaurus, Faveoolithus, dinosaur fossils have been collected from Auca Mahuevo, Argentina and Rousett, France, amongst other locations, for geochemical analysis to determine if isotopic signatures could be used to indicate warm- or cold-bloodedness. In some locations soil carbonates were also analyzed to constrain environmental temperatures. In order to test the validity of the geochemical results, an extensive study was undertaken to establish degree of diagenetic alteration. Petrographic and cathodoluminescence characterization of the eggshells were used to assess diagenetic alteration. An empirical 1-5 point scale was used to assign each sample an alteration level, and the observations were then compared with the geochemical results. Specimens displayed a wide range of alteration states. Some of which were well preserved and others highly altered. Another group seemed to be structural intact and only under cathodoluminescence was alteration clearly observed. In the majority of samples, alteration level was found to be predictably related to geochemical results. From specimens with little evidence for diagenesis, carbonate clumped isotope signatures support high (37-40°C) body temperature for Titanosaurid dinosaurs, but potentially lower body temperatures for other taxa. If these data do, in fact, represent original eggshell growth temperatures, these results support variability in body temperature amongst Cretaceous dinosaurs and potentially are consistent with variations between adult body temperature and size — a characteristic of 'gigantothermy'.

Carbon fiber content measurement in composite

NASA Astrophysics Data System (ADS)

Wang, Qiushi

Carbon fiber reinforced polymers (CFRPs) have been widely used in various structural applications in industries such as aerospace and automotive because of their high specific stiffness and specific strength. Their mechanical properties are strongly influenced by the carbon fiber content in the composites. Measurement of the carbon fiber content in CFRPs is essential for product quality control and process optimization. In this work, a novel carbonization-in-nitrogen method (CIN) is developed to characterize the fiber content in carbon fiber reinforced thermoset and thermoplastic composites. In this method, a carbon fiber composite sample is carbonized in a nitrogen environment at elevated temperatures, alongside a neat resin sample. The carbon fibers are protected from oxidization while the resin (the neat resin and the resin matrix in the composite sample) is carbonized under the nitrogen environment. The residue of the carbonized neat resin sample is used to calibrate the resin carbonization rate and calculate the amount of the resin matrix in the composite sample. The new method has been validated on several thermoset and thermoplastic resin systems and found to yield an accurate measurement of fiber content in carbon fiber polymer composites. In order to further understand the thermal degradation behavior of the high temperature thermoplastic polymer during the carbonization process, the mechanism and the kinetic model of thermal degradation behavior of carbon fiber reinforced poly (phenylene sulfide) (CPPS) are studied using thermogravimetry analysis (TGA). The CPPS is subjected to TGA in an air and nitrogen atmosphere at heating rates from 5 to 40°C min--1. The TGA curves obtained in air are different from those in nitrogen. This demonstrates that weight loss occurs in a single stage in nitrogen but in two stages in air. To elucidate this difference, thermal decomposition kinetics is analyzed by applying the Kissinger, Flynn-Wall-Ozawa, Coat-Redfern and Malek methods. The activation energy (Ea) of the solid-state process is determined to be 202 kJ mol--1 in an oxidative atmosphere using Kissinger's method, which is 10-15 kJ mol--1 more than the results calculated in a nitrogen atmosphere. The value of the activation energy obtained using Ozawa-Flynn methods is in agreement with that using the Kissinger method. Different degradation mechanisms are used to compare with this value. Based on the analytical result, the actual thermal degradation mechanism of the CPPS is a Dn deceleration type. The carbonization temperature range of the CPPS is the same as pure PPS resin.

Structural analysis of geochemical samples by solid-state nuclear magnetic resonance spectrometry. Role of paramagnetic material

USGS Publications Warehouse

Vassallo, A.M.; Wilson, M.A.; Collin, P.J.; Oades, J.M.; Waters, A.G.; Malcolm, R.L.

1987-01-01

An examination of coals, coal tars, a fulvic acid, and soil fractions by solid-state 13C NMR spectrometry has demonstrated widely differing behavior regarding quantitative representation in the spectrum. Spin counting experiments on coal tars and the fulvic acid show that almost all the sample carbon is observed in both solution and solid-state NMR spectra. Similar experiments on two coals (a lignite and a bituminous coal) show that most (70-97%) of the carbon is observed; however, when the lignite is ion exchanged with 3% (w/w) Fe3+, the fraction of carbon observed drops to below 10%. In additional experiments signal intensity from soil samples is enhanced by a simple dithionite treatment. This is illustrated by 13C, 27Al, and 29Si solid-state NMR experiments on soil fractions. ?? 1987 American Chemical Society.

Use of different spectroscopic techniques in the analysis of Roman age wall paintings.

PubMed

Agnoli, Francesca; Calliari, Irene; Mazzocchin, Gian-Antonio

2007-01-01

In this paper the analysis of samples of Roman age wall paintings coming from: Pordenone, Vicenza and Verona is carried out by using three different techniques: energy dispersive x-rays spectroscopy (EDS), x-rays fluorescence (XRF) and proton induced x-rays emission (PIXE). The features of the three spectroscopic techniques in the analysis of samples of archaeological interest are discussed. The studied pigments were: cinnabar, yellow ochre, green earth, Egyptian blue and carbon black.

Phylogenetic identification of methanogens assimilating acetate-derived carbon in dairy and swine manures.

PubMed

Barret, Maialen; Gagnon, Nathalie; Morissette, Bruno; Kalmokoff, Martin L; Topp, Edward; Brooks, Stephen P J; Matias, Fernando; Neufeld, Josh D; Talbot, Guylaine

2015-02-01

In order to develop approaches for reducing the carbon footprint of the swine and dairy industries, it is important first to identify the methanogenic communities that drive methane emissions from stored manure. In this study, the metabolically active methanogens in substrate-starved manure samples taken from two dairy and one swine manure storage tanks were identified using [(13)C]-acetate and DNA stable-isotope probing (DNA-SIP). Molecular analysis of recovered genomic [(13)C]-DNA revealed that two distinct clusters of unclassified methanogen populations affiliated with the Methanoculleus genus, and the populations affiliated with Methanoculleus chikugoensis assimilated acetate-derived carbon (acetate-C) in swine and dairy starved manure samples, respectively. Furthermore, carbon flow calculations indicated that these populations were the primary contributors to methane emissions during these anoxic SIP incubations. Comparative analysis of mcrA gene abundance (coding for a key enzyme of methanogenesis) for Methanoculleus spp. in fresh feces and a wider range of stored dairy or swine manure samples, by real-time quantitative PCR using newly designed specific primers, demonstrated that the abundance of this genus significantly increased during storage. The findings supported the involvement of these particular methanogen populations as methane emitters from swine and dairy manure storage tanks. The study revealed that the ability to assimilate acetate-C for growth in manure differed within the Methanoculleus genus. Crown Copyright © 2014. Published by Elsevier GmbH. All rights reserved.

Aerosol Emission Monitoring and Assessment of Potential Exposure to Multi-walled Carbon Nanotubes in the Manufacture of Polymer Nanocomposites

PubMed Central

Thompson, Drew; Chen, Sheng-Chieh; Wang, Jing; Pui, David Y.H.

2015-01-01

Recent animal studies have shown that carbon nanotubes (CNTs) may pose a significant health risk to those exposed in the workplace. To further understand this potential risk, effort must be taken to measure the occupational exposure to CNTs. Results from an assessment of potential exposure to multi-walled carbon nanotubes (MWCNTs) conducted at an industrial facility where polymer nanocomposites were manufactured by an extrusion process are presented. Exposure to MWCNTs was quantified by the thermal-optical analysis for elemental carbon (EC) of respirable dust collected by personal sampling. All personal respirable samples collected (n = 8) had estimated 8-h time weighted average (TWA) EC concentrations below the limit of detection for the analysis which was about one-half of the recommended exposure limit for CNTs, 1 µg EC/m3 as an 8-h TWA respirable mass concentration. Potential exposure sources were identified and characterized by direct-reading instruments and area sampling. Area samples analyzed for EC yielded quantifiable mass concentrations inside an enclosure where unbound MWCNTs were handled and near a pelletizer where nanocomposite was cut, while those analyzed by electron microscopy detected the presence of MWCNTs at six locations throughout the facility. Through size selective area sampling it was identified that the airborne MWCNTs present in the workplace were in the form of large agglomerates. This was confirmed by electron microscopy where most of the MWCNT structures observed were in the form of micrometer-sized ropey agglomerates. However, a small fraction of single, free MWCNTs was also observed. It was found that the high number concentrations of nanoparticles, ~200000 particles/cm3, present in the manufacturing facility were likely attributable to polymer fumes produced in the extrusion process. PMID:26209597

Comparison of carbon and biomass estimation methods for European forests

NASA Astrophysics Data System (ADS)

Neumann, Mathias; Mues, Volker; Harkonen, Sanna; Mura, Matteo; Bouriaud, Olivier; Lang, Mait; Achten, Wouter; Thivolle-Cazat, Alain; Bronisz, Karol; Merganicova, Katarina; Decuyper, Mathieu; Alberdi, Iciar; Astrup, Rasmus; Schadauer, Klemens; Hasenauer, Hubert

2015-04-01

National and international reporting systems as well as research, enterprises and political stakeholders require information on carbon stocks of forests. Terrestrial assessment systems like forest inventory data in combination with carbon calculation methods are often used for this purpose. To assess the effect of the calculation method used, a comparative analysis was done using the carbon calculation methods from 13 European countries and the research plots from ICP Forests (International Co-operative Programme on Assessment and Monitoring of Air Pollution Effects on Forests). These methods are applied for five European tree species (Fagus sylvatica L., Quercus robur L., Betula pendula Roth, Picea abies (L.) Karst. and Pinus sylvestris L.) using a standardized theoretical tree dataset to avoid biases due to data collection and sample design. The carbon calculation methods use allometric biomass and volume functions, carbon and biomass expansion factors or a combination thereof. The results of the analysis show a high variation in the results for total tree carbon as well as for carbon in the single tree compartments. The same pattern is found when comparing the respective volume estimates. This is consistent for all five tree species and the variation remains when the results are grouped according to the European forest regions. Possible explanations are differences in the sample material used for the biomass models, the model variables or differences in the definition of tree compartments. The analysed carbon calculation methods have a strong effect on the results both for single trees and forest stands. To avoid misinterpretation the calculation method has to be chosen carefully along with quality checks and the calculation method needs consideration especially in comparative studies to avoid biased and misleading conclusions.

CO2 Radiocarbon Analysis to Quantify Organic Contaminant Degradation, MNA, and Engineered Remediation Approaches

DTIC Science & Technology

2014-12-18

carbon backbone). This may be analytically relevant where soil gas is sampled under anaerobic conditions. However, at the soil:air interface, methane is...of the ambient CO2 on-site coming from the fossil end-member (i.e. the contaminant). Sampling , processing and analysis of soil gas 14CO2 and 14CH4...gasoline service station having fuel-contaminated soil and groundwater. The SVE system ran for ~3 months prior to sampling . Soil gas and groundwater

A morphological investigation of soot produced by the detonation of munitions.

PubMed

Pantea, Dana; Brochu, Sylvie; Thiboutot, Sonia; Ampleman, Guy; Scholz, Günter

2006-10-01

The morphology of three different detonation soot samples along with other common soot materials such as carbon black, diesel soot and chimney soot was studied by elemental and proximate analysis, X-ray diffraction and electron microscopy. The goal of this study was to better define the morphology of the detonation soot in order to better assess the interactions of this type of soot with explosive residues. The detonation soot samples were obtained by the detonation of artillery 155mm projectiles filled with either pure TNT (2,4,6-trinitrotoluene) or composition B, a military explosive based on a mixture of TNT and RDX (trimethylentrinitramine). The carbon content of the soot samples varied considerably depending on the feedstock composition. Detonation soot contains less carbon and more nitrogen than the other carbonaceous samples studied, due to the molecular structure of the energetic materials detonated such as TNT and RDX. The ash concentration was higher for detonation soot samples due to the high metal content coming from the projectiles shell and to the soil contamination which occurred during the detonation. By X-ray diffraction, diamond and graphite were found to be the major crystalline carbon forms in the detonation soot. Two electron microscopy techniques were used in this study to visualise the primary particles and to try to explain the formation mechanism of detonation soot samples.

Rates and Mechanisms of Oil Shale Pyrolysis: A Chemical Structure Approach

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

Fletcher, Thomas; Pugmire, Ronald

2015-01-01

Three pristine Utah Green River oil shale samples were obtained and used for analysis by the combined research groups at the University of Utah and Brigham Young University. Oil shale samples were first demineralized and the separated kerogen and extracted bitumen samples were then studied by a host of techniques including high resolution liquid-state carbon-13 NMR, solid-state magic angle sample spinning 13C NMR, GC/MS, FTIR, and pyrolysis. Bitumen was extracted from the shale using methanol/dichloromethane and analyzed using high resolution 13C NMR liquid state spectroscopy, showing carbon aromaticities of 7 to 11%. The three parent shales and the demineralized kerogensmore » were each analyzed with solid-state 13C NMR spectroscopy. Carbon aromaticity of the kerogen was 23-24%, with 10-12 aromatic carbons per cluster. Crushed samples of Green River oil shale and its kerogen extract were pyrolyzed at heating rates from 1 to 10 K/min at pressures of 1 and 40 bar and temperatures up to 1000°C. The transient pyrolysis data were fit with a first-order model and a Distributed Activation Energy Model (DAEM). The demineralized kerogen was pyrolyzed at 10 K/min in nitrogen at atmospheric pressure at temperatures up to 525°C, and the pyrolysis products (light gas, tar, and char) were analyzed using 13C NMR, GC/MS, and FTIR. Details of the kerogen pyrolysis have been modeled by a modified version of the chemical percolation devolatilization (CPD) model that has been widely used to model coal combustion/pyrolysis. This refined CPD model has been successful in predicting the char, tar, and gas yields of the three shale samples during pyrolysis. This set of experiments and associated modeling represents the most sophisticated and complete analysis available for a given set of oil shale samples.« less

Composition analysis of a polymer electrolyte membrane fuel cell microporous layer using scanning transmission X-ray microscopy and near edge X-ray absorption fine structure analysis

NASA Astrophysics Data System (ADS)

George, Michael G.; Wang, Jian; Banerjee, Rupak; Bazylak, Aimy

2016-03-01

The novel application of scanning transmission X-ray microscopy (STXM) to the microporous layer (MPL) of a polymer electrolyte membrane fuel cell is investigated. A spatially resolved chemical component distribution map is obtained for the MPL of a commercially available SGL 25 BC sample. This is achieved with near edge X-ray absorption fine structure spectroscopic analysis. Prior to analysis the sample is embedded in non-reactive epoxy and ultra-microtomed to a thickness of 100 nm. Polytetrafluoroethylene (PTFE), carbon particle agglomerates, and supporting epoxy resin distributions are identified and reconstructed for a scanning area of 6 μm × 6 μm. It is observed that the spatial distribution of PTFE is strongly correlated to the carbon particle agglomerations. Additionally, agglomerate structures of PTFE are identified, possibly indicating the presence of a unique mesostructure in the MPL. STXM analysis is presented as a useful technique for the investigation of chemical species distributions in the MPL.

Heteroatom-enriched and renewable banana-stem-derived porous carbon for the electrochemical determination of nitrite in various water samples.

PubMed

Madhu, Rajesh; Veeramani, Vediyappan; Chen, Shen-Ming

2014-04-23

For the first time, high-surface-area (approximately 1465 m(2) g(-1)), highly porous and heteroatom-enriched activated carbon (HAC) was prepared from banana stems (Musa paradisiaca, Family: Musaceae) at different carbonization temperatures of 700, 800 and 900 °C (HAC) using a simple and eco-friendly method. The amounts of carbon, hydrogen, nitrogen and sulfur in the HAC are 61.12, 2.567, 0.4315, and 0.349%, respectively. Using X-ray diffraction (XRD), CHNS elemental analysis, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy, the prepared activated carbon appears amorphous and disordered in nature. Here, we used HAC for an electrochemical application of nitrite (NO2(-)) sensor to control the environmental pollution. In addition, HAC exhibits noteworthy performance for the highly sensitive determination of nitrite. The limit of detection (LODs) of the nitrite sensor at HAC-modified GCE is 0.07 μM. In addition, the proposed method was applied to determine nitrite in various water samples with acceptable results.

Heteroatom-enriched and renewable banana-stem-derived porous carbon for the electrochemical determination of nitrite in various water samples

NASA Astrophysics Data System (ADS)

Madhu, Rajesh; Veeramani, Vediyappan; Chen, Shen-Ming

2014-04-01

For the first time, high-surface-area (approximately 1465 m2 g-1), highly porous and heteroatom-enriched activated carbon (HAC) was prepared from banana stems (Musa paradisiaca, Family: Musaceae) at different carbonization temperatures of 700, 800 and 900°C (HAC) using a simple and eco-friendly method. The amounts of carbon, hydrogen, nitrogen and sulfur in the HAC are 61.12, 2.567, 0.4315, and 0.349%, respectively. Using X-ray diffraction (XRD), CHNS elemental analysis, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy, the prepared activated carbon appears amorphous and disordered in nature. Here, we used HAC for an electrochemical application of nitrite (NO2-) sensor to control the environmental pollution. In addition, HAC exhibits noteworthy performance for the highly sensitive determination of nitrite. The limit of detection (LODs) of the nitrite sensor at HAC-modified GCE is 0.07 μM. In addition, the proposed method was applied to determine nitrite in various water samples with acceptable results.

Effect of alkali earth oxides on hydroxy-carbonated apatite nano layer formation for SiO2-BaO-CaO-Na2O-P2O5 glass system

NASA Astrophysics Data System (ADS)

Kiran, P.; Ramakrishna, V.; Shashikala, H. D.; Udayashankar, N. K.

2017-11-01

Barium soda lime phosphosilicate [(58SiO2-(32 - x)BaO- xCao-6Na2O-4P2O5 (where x = 15, 20, 25 and 30 mol%)] samples were synthesised using conventional sol-gel method at 700 °C sintering temperature. Thermal, structural properties were studied using thermo gravimetric analysis and differential thermal analysis, X-ray diffraction, scanning electron microscopy, fourier transform infrared and Raman spectroscopy. Using Raman spectra non-bridging oxygen concentrations were estimated. The hydroxy-carbonated apatite (HCA) layer formation on samples was analysed for 7 days using simulated body fluid (SBF) soaked samples. The growth of HCA layers self-assembled on the sample surface was discussed as a function of NBO/BO ratio. Results indicated that the number of Ca2+ ions released into SBF solution in dissolution process and weight loss of SB-treated samples vary with NBO/BO ratio. The changes in NBO/BO ratios were observed to be proportional to HCA forming ability of barium soda lime phosphosilicate glasses.

Thermal behavior of phenol-furfuryl alcohol resin/carbon nanotubes composites

NASA Astrophysics Data System (ADS)

Conejo, L. S.; Costa, M. L.; Oishi, S. S.; Botelho, E. C.

2018-04-01

Phenol-furfuryl alcohol resins (PFA) are excellent candidates to replace existing thermoset matrices used in obtaining insulating systems or carbon materials, both in its pure form and reinforced with nanoscale structures. This work had as main purpose synthesize and investigate thermal characterization of PFA resin and its nanostructured composites with different concentrations of carbon nanotubes (0, 0.1, 0.5 and 1.0 wt%). The DSC analysis was performed to estimate the specific heat (cp) of the cured samples and thermomechanical analysis to find the linear thermal expansion coefficient (α). From these results, the cp values found for the PFA system was similar to that described in the literature for the phenolic resin. The cp increased with the increase in the CNT concentration in the system up to 0.5%. The coefficient of linear thermal expansion obtained by TMA technique for PFA sample was 33.10‑6/°C which was close to the α value of phenolic resin (40 to 80.10‑6/°C).

Using of multi-walled carbon nanotubes electrode for adsorptive stripping voltammetric determination of ultratrace levels of RDX explosive in the environmental samples.

PubMed

Rezaei, Behzad; Damiri, Sajjad

2010-11-15

A study of the electrochemical behavior and determination of RDX, a high explosive, is described on a multi-walled carbon nanotubes (MWCNTs) modified glassy carbon electrode (GCE) using adsorptive stripping voltammetry and electrochemical impedance spectroscopy (EIS) techniques. The results indicated that MWCNTs electrode remarkably enhances the sensitivity of the voltammetric method and provides measurements of this explosive down to the sub-mg/l level in a wide pH range. The operational parameters were optimized and a sensitive, simple and time-saving cyclic voltammetric procedure was developed for the analysis of RDX in ground and tap water samples. Under optimized conditions, the reduction peak have two linear dynamic ranges of 0.6-20.0 and 8.0-200.0 mM with a detection limit of 25.0 nM and a precision of <4% (RSD for 8 analysis). Copyright © 2010 Elsevier B.V. All rights reserved.

Structural and magnetic properties of Fe and carbon nanotubes derived from coconut shells

NASA Astrophysics Data System (ADS)

Qadri, S. B.; Gorzkowski, E. P.; Bussmann, K.; Rath, B. B.; Feng, J.

2018-05-01

Ferric oxide (Fe2O3) was directly reduced to metallic Fe using the carbon source from the coconut shells at temperatures above 1400 °C in argon gas atmospheres. X-ray diffraction analysis showed the presence of α-, γ- phases of Fe in addition to the presence of carbon nanotubes (CNTs). By selecting the appropriate ratios of coconut shell powder to Fe2O3, it is demonstrated that pure Fe is produced without any residual ferric oxide. The quantitative analysis of each of the Fe phases and carbon nanotubes was dependent on the temperature and the duration of processing at high temperature. Transmission electron microcopy results showed copious amount of carbon nanotubes in the samples. Magnetic property measurements suggested that, the average magnetic moment is consistent with presence of α-phase and the ferromagnetic γ-phase of Fe. This novel method of producing pure α- and γ-Fe in the presence of carbon nanotubes using coconut shells has potential applications as nanocomposites.

Formation Pathways of Carbon Allotropes in Detonation Condensates

NASA Astrophysics Data System (ADS)

Nielsen, Michael; Bagge-Hansen, Michael; Hammons, Josh; Lauderbach, Lisa; Hodgin, Ralph; Bastea, Sorin; Fried, Larry; Lee, Jonathan; van Buuren, Tony; Pagoria, Phil; May, Chadd; Aloni, Shaul; Willey, Trevor

2017-06-01

Time-resolved small-angle scattering (TR-SAXS) data reveal evolution in the size and morphology of nano-carbon particles that form during the first microsecond during the detonation of high explosive (HE) materials, but do not provide chemical or phase information. Herein, we present analysis of complementary post-detonation soots collected with minimal environmental carbon or other contamination: HE samples are detonated whithin clean ice capture layers to yield aqueous dispersions of the carbonaceous soot. We report substantial variation in soots formed through the detonation of HE materials that attain a variety of temperatures and pressures during detonation. Transmission electron microscopy analysis of these recovered soots provides physical and chemical information that we compare directly to TR-SAXS data and SAXS measurements from recovered soots. We observe various structures including graphitic and amorphous carbon, nanodiamond, and spherical carbon onions. These experimental data correlate to models of how products from HE materials traverse the carbon phase diagram during detonation. Prepared by LLNL under Contract DE-AC52-07NA27344.

Magnetic Properties and the Giant Magnetoimpedance of Amorphous Co-Based Wires with a Carbon Coating

NASA Astrophysics Data System (ADS)

Golubeva, E. V.; Stepanova, E. A.; Balymov, K. G.; Volchkov, S. O.; Kurlyandskaya, G. V.

2018-04-01

A comparative analysis of the magnetic properties and specific features of the giant magnetoimpedance has been carried out for amorphous rapidly quenched wires with a composition of (Co0.94Fe0.06)72.5Si12.5B15 in the initial state and after the deposition of a carbon coating. The deposition of the defective graphene-like carbon layer was carried out under normal conditions during the exposure in toluene (methylbenzene). The method of the energy-dispersive X-ray spectroscopy made it possible to reliably show that after the modification in toluene, the carbon content on the surface significantly exceeds the natural amount of carbon. The deposition of the carbon coating induced changes in the distribution of the initial quenching stresses in the near-surface layer of amorphous wires. A comparative analysis of the magnetic and magnetoimpedance properties of the samples before and after exposure in the aromatic solvent confirms the occurrence of changes in the effective magnetic anisotropy as a result of this surface treatment.

Evolved Gas Analysis of Mars Analog Samples from the Arctic Mars Analog Svalbard Expedition: Implications for Analyses by the Mars Science Laboratory

NASA Technical Reports Server (NTRS)

McAdam, A.; Stern, J. C.; Mahaffy, P. R.; Blake, D. F.; Bristow, T.; Steele, A.; Amundsen, H. E. F.

2012-01-01

The 2011 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings on Svalbard, using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL). The Sample Analysis at Mars (SAM) instrument suite on MSL consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS), which analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-QMS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during AMASE. AMASE 2011 sites spanned a range of environments relevant to understanding martian surface materials, processes and habitability. They included the basaltic Sverrefjell volcano, which hosts carbonate globules, cements and coatings, carbonate and sulfate units at Colletth0gda, Devonian sandstone redbeds in Bockfjorden, altered basaltic lava delta deposits at Mt. Scott Keltie, and altered dolerites and volcanics at Botniahalvoya. Here we focus on SAM-like EGA-MS of a subset of the samples, with mineralogy comparisons to CheMin team results. The results allow insight into sample organic content as well as some constraints on sample mineralogy.

Template confined synthesis of amorphous carbon nanotubes and its confocal Raman microscopy

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

Maity, Supratim; Roychowdhury, Tuhin; Chattopadhyay, Kalyan Kumar, E-mail: kalyan-chattopadhyay@yahoo.com

2014-04-24

Amorphous carbon nanotubes (aCNTs) were synthesized by AAO (anodic aluminum oxide) template at a temperature 500 °C in nitrogen atmosphere using the citric acid as a carbon source without the help of any catalyst particles. Morphological analysis of the as prepared samples was carried out by field emission scanning electron microscopy (FESEM). Confocal Raman imaging has been studied and an attempt has been made to find out the graphitic (sp{sup 2}) and disordered phase of the CNTs.

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

Adib, F.; Bagreev, A.; Bandosz, T.J.

The H{sub 2}S breakthrough capacity was measured on two series of activated carbons of a coconut shell and a bituminous coal origins. To broaden the spectrum of surface features the samples were oxidized using nitric acid or ammonium persulfate under conditions chosen to preserve their pore structures. Then the carbons were characterized using Boehm titration, potentiometric titration, thermal analysis, temperature programmed desorption, sorption of nitrogen, and sorption of water. It was found that the choice of unimpregnated carbon for application as H{sub 2}S adsorbent should be made based on parameters of its acidity such as number of acidic groups, pHmore » of surface, amount of surface groups oxygen, or weight loss associated to decomposition of surface oxygen species. The results obtained from the analyses of six unimpregnated carbon samples suggest that there are certain threshold values of these quantities which, when exceeded, have a dramatic effect on the H{sub 2}S breakthrough capacity.« less

delta 15N and non-carbonate delta 13C values for two petroleum source rock reference materials and a marine sediment reference material

USGS Publications Warehouse

Dennen, Kristin O.; Johnson, Craig A.; Otter, Marshall L.; Silva, Steven R.; Wandless, Gregory A.

2006-01-01

Samples of United States Geological Survey (USGS) Certified Reference Materials USGS Devonian Ohio Shale (SDO-1), and USGS Eocene Green River Shale (SGR-1), and National Research Council Canada (NRCC) Certified Marine Sediment Reference Material (PACS-2), were sent for analysis to four separate analytical laboratories as blind controls for organic rich sedimentary rock samples being analyzed from the Red Dog mine area in Alaska. The samples were analyzed for stable isotopes of carbon (delta13Cncc) and nitrogen (delta15N), percent non-carbonate carbon (Wt % Cncc) and percent nitrogen (Wt % N). SDO-1, collected from the Huron Member of the Ohio Shale, near Morehead, Kentucky, and SGR-1, collected from the Mahogany zone of the Green River Formation are petroleum source rocks used as reference materials for chemical analyses of sedimentary rocks. PACS-2 is modern marine sediment collected from the Esquimalt, British Columbia harbor. The results presented in this study are, with the exceptions noted below, the first published for these reference materials. There are published information values for the elemental concentrations of 'organic' carbon (Wt % Corg measured range is 8.98 - 10.4) and nitrogen (Wt % Ntot 0.347 with SD 0.043) only for SDO-1. The suggested values presented here should be considered 'information values' as defined by the NRCC Institute for National Measurement Reference Materials and should be useful for the analysis of 13C, 15N, C and N in organic material in sedimentary rocks.

Hydrogen recombiner catalyst test supporting data

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

Britton, M.D.

1995-01-19

This is a data package supporting the Hydrogen Recombiner Catalyst Performance and Carbon Monoxide Sorption Capacity Test Report, WHC-SD-WM-TRP-211, Rev 0. This report contains 10 appendices which consist of the following: Mass spectrometer analysis reports: HRC samples 93-001 through 93-157; Gas spectrometry analysis reports: HRC samples 93-141 through 93-658; Mass spectrometer procedure PNL-MA-299 ALO-284; Alternate analytical method for ammonia and water vapor; Sample log sheets; Job Safety analysis; Certificate of mixture analysis for feed gases; Flow controller calibration check; Westinghouse Standards Laboratory report on Bois flow calibrator; and Sorption capacity test data, tables, and graphs.

preparation of microgram samples on iron wool for radiocarbon analysis via accelerator mass spectrometry: A closed-system approach

NASA Astrophysics Data System (ADS)

Verkouteren, R. Michael; Klouda, George A.; Currie, Lloyd A.; Donahue, Douglas J.; Jull, A. J. Timothy; Linick, T. W.

1987-11-01

A technique has been developed at NBS for the production of high quality targets for radiocarbon analysis by accelerator mass spectrometry (AMS). Our process optimizes chemical yields, ion currents and characterizes the chemical blank. The approach encompasses sample combustion to CO 2, catalytic reduction of CO 2 by Zn to CO, reduction to graphitic carbon on high-purity iron wool and in situ formation of a homogeneous iron-carbon bead; all steps are performed in a closed system. The total measurement system blank and variability are considered in the light of contributions from combustion, iron wool, reduction, bead formation and instrument blank. Additionally, use of this approach provides an increase in throughput, i.e. the effective management of large numbers of samples. Chemical yields for 50-800 μg C samples deposited on 15 mg iron wool were greater than 90%. Integrated 12C - ion currents observed were significant, being 4-64% of those observed in pure graphite. These currents are about an order of magnitude greater than those expected from dilution of graphite with an inert substrate. Isotopic accuracy, precision and blank were assessed by measuring the {14C }/{13C } ratios of a series of targets prepared from dead carbon and oxalic acid (SRM 4990C). Each target was typically measured for one hour; bead consumption was estimated at 5% to 10%. System blank subsequent to combustion was equivalent to (2.2 ± 0.5) μg modern carbon (chemistry + instrument); combustion blank currently stands at (0.4 ± 0.1) (SE, n = 6) μg C.

Ion beam promoted lithium absorption in glassy polymeric carbon

NASA Astrophysics Data System (ADS)

Ila, D.; Zimmerman, R. L.; Jenkins, G. M.; Maleki, H.; Poker, D. B.

1995-12-01

Glassy Polymeric Carbon (GPC) samples prepared from a precursor possess accessible pore volume that depends on the heat treatment temperature. We have shown that lithium percolates without diffusion into the accessible pores of GPC samples immersed in a molten lithium salt bath at 700°C. Ion bombardment with 10 MeV Au atoms increases the total pore volume available for lithium occupation even for samples normally impermeable to lithium. The lithium concentration depth profile is measured using Li7(p,2α) nuclear reaction analysis. We will report on lithium percolation into GPC prepared at temperatures between 500°C and 1000°C and activated by a 10 MeV gold ion bombardment.

The zero inflation of standing dead tree carbon stocks

Treesearch

Christopher W. Woodall; David W. MacFarlane

2012-01-01

Given the importance of standing dead trees in numerous forest ecosystem attributes/processes such as carbon (C) stocks, the USDA Forest Service’s Forest Inventory and Analysis (FIA) program began consistent nationwide sampling of standing dead trees in 1999. Modeled estimates of standing dead tree C stocks are currently used as the official C stock estimates for the...

Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

NASA Astrophysics Data System (ADS)

Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

2016-08-01

Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

Cellulose and Lignin Carbon Isotope Signatures in Sphagnum Moss Reveal Complementary Environmental Properties

NASA Astrophysics Data System (ADS)

Loisel, J.; Nichols, J. E.; Kaiser, K.; Beilman, D. W.; Yu, Z.

2016-12-01

The carbon isotope signature (δ13C) of Sphagnum moss is increasingly used as a proxy for past surface wetness in peatlands. However, conflicting interpretations of these carbon isotope records have recently been published. While the water film hypothesis suggests that the presence of a thick (thin) water film around hollow (hummock) mosses leads to less (more) negative δ13C values, the carbon source hypothesis poses that a significant (insignificant) amount of CH4 assimilation by hollow (hummock) mosses leads to more (less) negative δ13C values. To evaluate these competing mechanisms and their impact on moss δ13C, we gathered 30 moss samples from 6 peatlands in southern Patagonia. Samples were collected along a strong hydrological gradient, from very dry hummocks (80 cm above water table depth) to submerged hollows (5 cm below water surface). These peat bogs have the advantage of being colonized by a single cosmopolitan moss species, Sphagnum magellanicum, limiting potential biases introduced by species-specific carbon discrimination. We measured δ13C from stem cellulose and leaf waxes on the same samples to quantify compound-specific carbon signatures. We found that stem cellulose and leaf-wax lipids were both strongly negatively correlated with moss water content, suggesting a primary role of water film thickness on carbon assimilation. In addition, isotopic fractionation during wax synthesis was greater than for cellulose. This offset decreases as conditions get drier, due to (i) a more effective carbon assimilation, or (ii) CH4 uptake through symbiosis with methanotrophic bacteria within the leaves of wet mosses. Biochemical analysis (carbohydrates, amino acids, hydrophenols, cutin acids) of surface moss are currently being conducted to characterize moss carbon allocation under different hydrological conditions. Overall, this modern calibration work should be of use for interpreting carbon isotope records from peatlands.

Delta13C and delta18O isotopic composition of CaCO3 measured by continuous flow isotope ratio mass spectrometry: statistical evaluation and verification by application to Devils Hole core DH-11 calcite.

PubMed

Révész, Kinga M; Landwehr, Jurate M

2002-01-01

A new method was developed to analyze the stable carbon and oxygen isotope ratios of small samples (400 +/- 20 micro g) of calcium carbonate. This new method streamlines the classical phosphoric acid/calcium carbonate (H(3)PO(4)/CaCO(3)) reaction method by making use of a recently available Thermoquest-Finnigan GasBench II preparation device and a Delta Plus XL continuous flow isotope ratio mass spectrometer. Conditions for which the H(3)PO(4)/CaCO(3) reaction produced reproducible and accurate results with minimal error had to be determined. When the acid/carbonate reaction temperature was kept at 26 degrees C and the reaction time was between 24 and 54 h, the precision of the carbon and oxygen isotope ratios for pooled samples from three reference standard materials was

High performance supercapacitor from activated carbon derived from waste orange skin

NASA Astrophysics Data System (ADS)

Ahmed, Sultan; Hussain, S.; Ahmed, Ahsan; Rafat, M.

2018-05-01

Activated carbon due to its inherent properties such as large surface area and low cost is most frequently used electrode material for supercapacitor. Activated carbon has been previously derived from various biomass such as coconut shell, coffee bean etc. Herein, we report the synthesis of activated carbon from waste orange skin. The material was synthesized employing chemical activation method and the success of synthesis was confirmed by its physical and electrochemical properties. The physical properties of the as-prepared sample were studied using the techniques of XRD, SEM, Raman spectroscopy and N2 adsorption/desorption analysis while its electrochemical properties were studied in two-electrode assembly using liquid electrolyte (consisting of 1 M solution of LiTFSI dispersed in ionic liquid EMITFSI) and employing the techniques of cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge- discharge. The synthesized sample of activated carbon exhibits high specific capacitance of 115 F g-1 at 10 mV s-1. Also, the activated carbon electrode shows the retention of ˜75% in initial capacitance value for more than 2000 initial cycles, indicating the as-prepared activated carbon can be profitably used as electrode material for energy storage devices.

A statistical comparison of two carbon fiber/epoxy fabrication techniques

NASA Technical Reports Server (NTRS)

Hodge, A. J.

1991-01-01

A statistical comparison of the compression strengths of specimens that were fabricated by either a platen press or an autoclave were performed on IM6/3501-6 carbon/epoxy composites of 16-ply (0,+45,90,-45)(sub S2) lay-up configuration. The samples were cured with the same parameters and processing materials. It was found that the autoclaved panels were thicker than the platen press cured samples. Two hundred samples of each type of cure process were compression tested. The autoclaved samples had an average strength of 450 MPa (65.5 ksi), while the press cured samples had an average strength of 370 MPa (54.0 ksi). A Weibull analysis of the data showed that there is only a 30 pct. probability that the two types of cure systems yield specimens that can be considered from the same family.

Dissolved and particulate organic carbon in the melt water of Icelandic glaciers

NASA Astrophysics Data System (ADS)

Chifflard, Peter; Reiss, Martin

2017-04-01

Recently, glaciers have been recognized as unique ecosystems with potential effects on the global carbon cycle. Among other transport processes organic carbon stored in glacier ecosystems is released from the glaciers through melt at the glaciers surface that discharges into proglacial streams and finally into the ocean. Nevertheless, the potential role of glaciers in the carbon cycle remains poorly understood (Hood et al. 2015). One particular problem in this respect is that there is a lack in regional and global analysis of the total amount of organic carbon released from glaciers. Although, the release of organic carbon has been investigated in proglacial streams in Alaska, the European Alps and Greenland, to our knowledge, there is no information available for Icelandic proglacial streams. Thus, the aims of this study are: 1) to develop a first base information about the concentration of dissolved and particulate organic carbon (DOC and POC) in several Icelandic proglacial streams and 2) to detect the variability of DOC and POC along a proglacial stream from the glacier source to the mouth into the Atlantic Ocean. Therefore, a field trip was conducted between 23 and 31 July 2016, whereby, 25 water samples were taken. The sampling points cover melt water from the following Icelandic glaciers Vatnajökull, Langjökull, Hofsjökull, Myrdalsjökull and Tungnafellsjökull. Further water samples were taken along the river Hvitá starting at the glacier Langjökull and ending at the mouth into the Atlantic ocean in the southwest of Iceland. At every sample point electrical conductivity, water temperate and the pH-value were measured in situ using a calibrated portable water quality meter (Hanna Combo HI98129). The water samples (130 ml) were filtered using pre-combusted GF/F filters (Whatman, pore sizes 0.7 µm) and stored in a cooling box until the shipment to the laboratory of the Department for Geography, Philipps-University of Marburg. The DOC concentrations in the filtered water samples were measured using a TOC analyzer using high-temperature combustion of organic matter (OM) followed by thermal detection of CO2 (TOC-L, Shimadzu, Japan). POC was measured by determining mass lost upon combustion of the samples. Therefore all glass fiber membranes were dried after sampling at 65°C to a constant weight, reweighed to calculate the total suspended solids (TSS), combusted via heating the filter to 550° C and finally reweighed to calculate the amount of particulate organic matter. Spectroscopic characteristics were detected by using a spectrophotometer (ThermoFisher, Genesys 10S) for UV-VIS analysis and a fluorescence spectrometer (Shimadzu RF-6000) for fluorescence analysis. Spectroscopic indices will be calculated based on these UV-VIS and fluorescence data. First results show that the DOC-concentrations are very low and range from 0.113 mg/l to 0.937 mg/l. These concentrations are comparable with values measured in the melt water in other regions (Alaska, Greenland and European Alps) (Hood et al. 2015). POC concentrations range from 0.667 mg/l to 173.333 mg/l and exceed the DOC-concentration at every sampling location. This differences can be compared with results of the Greenland Ice Sheet, but not with some small glaciers in the European Alps, where the concentrations of DOC and POC more or less equal (Hood et al. 2015). Nevertheless, the export of POC plays a very important factor within the organic carbon export budget of glaciers in Iceland and further measurements are required. Hood, E., Battin, T. J., Fellman, J., O'Neel, S., & Spencer, R. G. (2015). Storage and release of organic carbon from glaciers and ice sheets. Nature Geoscience, 8(2), 91-96.

Evidence for an Extraterrestrial Impact Event 12,900 years ago that Contributed to Megafaunal Extinctions and the Younger Dryas Cooling

NASA Astrophysics Data System (ADS)

Firestone, R. B.; West, A.; Kennett, J. P.; Becker, L.; Bunch, T. E.; Revay, Z.; Schultz, P. H.; Belgya, T.; Dickenson, O. J.; Erlandson, J. M.; Goodyear, A. C.; Harris, R. S.; Howard, G. A.; Kennett, D. J.; Kloosterman, J. B.; Lechler, P.; Montgomery, J.; Poreda, R.; Darrah, T.; Que Hee, S. S.; Smith, A. R.; Stich, A.; Topping, W.; Wittke, J. H.; Wolbach, W. S.

2007-05-01

The Younger Dryas event boundary (YDB) is a thin sedimentary layer of 12.9 ka age containing an assemblage of materials formed due to a major ET impact centered over northern North America. The event coincided with the megafaunal extinctions and the Younger Dryas cooling episode. The YDB layer contains peaks in magnetic grains, microspherules, and iridium, in addition to charcoal and soot that resulted from extensive wildfires. Two impact-related carbon-rich markers, glass-like carbon and carbon spherules, have not been reported previously in North America. Vesicular, glass-like carbon, in pieces up to several cm, occurs in the YDB at 22 sites with concentrations ranging up to 16 g/kg. Their glassy texture suggests melting during formation, with some fragments grading into charcoal, and CF-IRMS analysis reveals a composition of >70 percent carbon. One sample exhibited a strong fullerene signature containing ET helium with a ratio of 84× that of air, comparable to the Tagish Lake meteorite (90×). Similar glass-like carbon has been reported from the Azuara crater in Spain (Ernstson, et al. 2001). Carbon spherules (0.15-2.5 mm) are black, highly vesicular, low-density, subspherical-to-spherical objects found in 18 widely distributed sites at varying concentrations up to 1500/kg. SEM analysis shows that the spherules have cracked and patterned surfaces, honeycombed cells, no inclusions, and sometimes display hollow cores. SEM/EDS and microprobe analyses show the carbon spherules to be >75 percent carbon. Similar carbon spherules are reported from the a crater in Germany (Rösler, et al., 2005). The carbon spherules most likely are either ablation products from the impactor or combustion products of the impact. Sediment samples were analyzed for Ir, and YDB samples from 9 sites exhibited elevated Ir values up to 3.75 ppb, while there was no detectable Ir above or below the YDB. Extracted magnetic grains have values up to 117 ppb, which is 25 percent that of typical chondrites and up to 5000× crustal abundance. The YDB layer, representing a major ET impact event at 12.9 ka, appears to coincide with the late Pleistocene megafaunal extinction and the onset of Younger Dryas cooling. We propose that neither this cooling nor the extinction would have occurred in the absence of this impact event.

The composition and degradability of upland dissolved organic matter

NASA Astrophysics Data System (ADS)

Moody, Catherine; Worrall, Fred; Clay, Gareth

2016-04-01

In order to assess controls on the degradability of DOM in stream water, samples of dissolved organic matter (DOM) and particulate organic matter (POM) were collected every month for a period of 24 months from an upland, peat-covered catchment in northern England. Each month the degradability of the DOM was assessed by exposing river water to light for up to 24 hours, and the change in the dissolved organic carbon (DOC) concentration in the water was measured. To provide context for the analysis of DOM and its degradability, samples of peat, vegetation, and litter were also taken from the same catchment and analysed. The organic matter samples were analysed by several methods including: elemental analysis (CHN and O), bomb calorimetry, thermogravimetric analysis, pyrolysis GC/MS, ICP-OES, stable isotope analysis (13C and 15N) and 13C solid state nuclear magnetic resonance (NMR). The water samples were analysed for pH, conductivity, absorbance at 400nm, anions, cations, particulate organic carbon (POC) and DOC concentrations. River flow conditions and meteorology were also recorded at the site and included in the analysis of the composition and degradability of DOM. The results of multiple regression models showed that the rates of DOC degradation were affected by the N-alkyl, O-alkyl, aldehyde and aromatic relative intensities, gross heat, OR and C:N. Of these, the N-alkyl relative intensity had the greatest influence, and this in turn was found to be dependent on the rainfall and soil temperature in the week before sampling.

Small-scale enzymatic digestion of glycoproteins and proteoglycans for analysis of oligosaccharides by LC-MS and FACE gel electrophoresis.

PubMed

Estrella, Ruby P; Whitelock, John M; Roubin, Rebecca H; Packer, Nicolle H; Karlsson, Niclas G

2009-01-01

Structural characterization of oligosaccharides from proteoglycans and other glycoproteins is greatly enhanced through the use of mass spectrometry and gel electrophoresis. Sample preparation for these sensitive techniques often requires enzymatic treatments to produce oligosaccharide sequences for subsequent analysis. This chapter describes several small-scale methods for in-gel, on-blot, and in-solution enzymatic digestions in preparation for graphitized carbon liquid chromatography-mass spectrometry (LC-MS) analysis, with specific applications indicated for glycosaminoglycans (GAGs) and N-linked oligosaccharides. In addition, accompanying procedures for oligosaccharide reduction by sodium borohydride, sample desalting via carbon microcolumn, desialylation by sialidase enzyme treatment, and small-scale oligosaccharide species fractionation are included. Fluorophore-assisted carbohydrate electrophoresis (FACE) is another useful method to isolate derivatized oligosaccharides. Overall, the modularity of these techniques provides ease and flexibility for use in conjunction with mass spectrometric and electrophoretic tools for glycomic research studies.

Sedimentology and geochemistry of mud volcanoes in the Anaximander Mountain Region from the Eastern Mediterranean Sea.

PubMed

Talas, Ezgi; Duman, Muhammet; Küçüksezgin, Filiz; Brennan, Michael L; Raineault, Nicole A

2015-06-15

Investigations carried out on surface sediments collected from the Anaximander mud volcanoes in the Eastern Mediterranean Sea to determine sedimentary and geochemical properties. The sediment grain size distribution and geochemical contents were determined by grain size analysis, organic carbon, carbonate contents and element analysis. The results of element contents were compared to background levels of Earth's crust. The factors that affect element distribution in sediments were calculated by the nine push core samples taken from the surface of mud volcanoes by the E/V Nautilus. The grain size of the samples varies from sand to sandy silt. Enrichment and Contamination factor analysis showed that these analyses can also be used to evaluate of deep sea environmental and source parameters. It is concluded that the biological and cold seep effects are the main drivers of surface sediment characteristics from the Anaximander mud volcanoes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Testing sample stability using four storage methods and the macroalgae Ulva and Gracilaria

EPA Science Inventory

Concern over the relative importance of different sample preparation and storage techniques frequently used in stable isotope analysis of particulate nitrogen (δ15N) and carbon (δ13C) prompted an experiment to determine how important such factors were to measured values in marine...

Petrophysical, Lithological and Mineralogical Characteristics of the Shale Strata of the Volga- Ural Region

NASA Astrophysics Data System (ADS)

Morozov, Vladimir P.; Plotnikova, Irina N.; Pronin, Nikita V.; Nosova, Fidania F.; Pronina, Nailya R.

2014-05-01

The objects of the study are Upper Devonian carbonate rocks in the territory of South-Tatar arch and Melekess basin in the Volga- Urals region. We studied core material of Domanicoid facies from the sediments of Mendymski and Domanik horizons of middle substage of Frasnian stage of the Upper Devonian. Basic analytical research methods included the following: study of the composition, structural and textural features of the rocks, the structure of their voids, filter and reservoir properties and composition of the fluid. The complex research consisted of macroscopic description of the core material, optical microscopy analysis, radiographical analysis, thermal analysis, x-ray tomography, electron microscopy, gas-liquid chromatography, chromate-mass spectrometry, light hydrocarbons analysis using paraphase assay, adsorbed gases analysis, and thermal vacuum degassing method. In addition, we performed isotopic studies of hydrocarbons saturating shale rocks. Shale strata are mainly represented by carbonate-chert rocks. They consist mainly of calcite and quartz. The ratio of these rock-forming minerals varies widely - from 25 to 75 percent. Pyrite, muscovite, albite, and microcline are the most common inclusions. Calcareous and ferruginous dolomite (ankerite), as well as magnesian calcite are tracked down as secondary minerals. While performing the tests we found out that the walls of open fractures filled with oil are stacked by secondary dolomite, which should be considered as an indication moveable oil presence in the open-cut. Electron microscopy data indicate that all the studied samples have porosity - both carbonates and carbonate-siliceous rocks. Idiomorphism of the rock-forming grains and pores that are visible under a microscope bring us to that conclusion. The analysis of the images indicates that the type of reservoir is either porous or granular. The pores are distributed evenly in the volume of rock. Their size is very unstable and varies from 0.5 microns to 100 microns. The lowest value are observed in long carbonate-siliceous rocks, the highest values are found in carbonate rocks. The latter is caused by the fact that there is a very strong recrystallization of calcite and its dolomite substitution in carbonates. Open porosity ranges from 0.65 to 7.98 percent, average value is 4.1percent . Effective porosity has an average value of 0.44 percent, ranging from 0.22 to 1.97. Permeability varies from 0.043 to 1.49 mD, average value is 0,191 mD. Organic matter was found in all samples. Its content varies within the section. The fluctuation range of from 1.0 to 20 percent. The lowest content of carbonates is found in carbonates, while the highest is observed in carbonate-siliceous rocks with a high content of chalcedony. Average organic matter content is 5-7 percent. According to Rock-Eval studies of the core, the catagenetic maturity of organic matter corresponds to MK1 - MK2 degree. We found a connection between the type of organic matter and the composition of adsorbed gas. We also could see that the samples with humic organics present in their organic matter and can be characterized by a fair dominance of methane over other gases. There is a clear relationship between organic matter content and the intensity of the gas saturation of the rock. Organic matter is characteristic mainly of the most siliceous formations. In "pure" carbonates, which are represented by micro-layers with different capacities, OM is not observed at all or its content is quite low.

Suitability of selected free-gas and dissolved-gas sampling containers for carbon isotopic analysis.

PubMed

Eby, P; Gibson, J J; Yi, Y

2015-07-15

Storage trials were conducted for 2 to 3 months using a hydrocarbon and carbon dioxide gas mixture with known carbon isotopic composition to simulate typical hold times for gas samples prior to isotopic analysis. A range of containers (both pierced and unpierced) was periodically sampled to test for δ(13)C isotopic fractionation. Seventeen containers were tested for free-gas storage (20°C, 1 atm pressure) and 7 containers were tested for dissolved-gas storage, the latter prepared by bubbling free gas through tap water until saturated (20°C, 1 atm) and then preserved to avoid biological activity by acidifying to pH 2 with phosphoric acid and stored in the dark at 5°C. Samples were extracted using valves or by piercing septa, and then introduced into an isotope ratio mass spectrometer for compound-specific δ(13)C measurements. For free gas, stainless steel canisters and crimp-top glass serum bottles with butyl septa were most effective at preventing isotopic fractionation (pierced and unpierced), whereas silicone and PTFE-butyl septa allowed significant isotopic fractionation. FlexFoil and Tedlar bags were found to be effective only for storage of up to 1 month. For dissolved gas, crimp-top glass serum bottles with butyl septa were again effective, whereas silicone and PTFE-butyl were not. FlexFoil bags were reliable for up to 2 months. Our results suggest a range of preferred containers as well as several that did not perform very well for isotopic analysis. Overall, the results help establish better QA/QC procedures to avoid isotopic fractionation when storing environmental gas samples. Recommended containers for air transportation include steel canisters and glass serum bottles with butyl septa (pierced and unpierced). Copyright © 2015 John Wiley & Sons, Ltd.

Characterization of the biosolids composting process by hyperspectral analysis.

PubMed

Ilani, Talli; Herrmann, Ittai; Karnieli, Arnon; Arye, Gilboa

2016-02-01

Composted biosolids are widely used as a soil supplement to improve soil quality. However, the application of immature or unstable compost can cause the opposite effect. To date, compost maturation determination is time consuming and cannot be done at the composting site. Hyperspectral spectroscopy was suggested as a simple tool for assessing compost maturity and quality. Nevertheless, there is still a gap in knowledge regarding several compost maturation characteristics, such as dissolved organic carbon, NO3, and NH4 contents. In addition, this approach has not yet been tested on a sample at its natural water content. Therefore, in the current study, hyperspectral analysis was employed in order to characterize the biosolids composting process as a function of composting time. This goal was achieved by correlating the reflectance spectra in the range of 400-2400nm, using the partial least squares-regression (PLS-R) model, with the chemical properties of wet and oven-dried biosolid samples. The results showed that the proposed method can be used as a reliable means to evaluate compost maturity and stability. Specifically, the PLS-R model was found to be an adequate tool to evaluate the biosolids' total carbon and dissolved organic carbon, total nitrogen and dissolved nitrogen, and nitrate content, as well as the absorbance ratio of 254/365nm (E2/E3) and C/N ratios in the dry and wet samples. It failed, however, to predict the ammonium content in the dry samples since the ammonium evaporated during the drying process. It was found that in contrast to what is commonly assumed, the spectral analysis of the wet samples can also be successfully used to build a model for predicting the biosolids' compost maturity. Copyright © 2015 Elsevier Ltd. All rights reserved.

Bioanalysis works in the IAA AMS facility: Comparison of AMS analytical method with LSC method in human mass balance study

NASA Astrophysics Data System (ADS)

Miyaoka, Teiji; Isono, Yoshimi; Setani, Kaoru; Sakai, Kumiko; Yamada, Ichimaro; Sato, Yoshiaki; Gunji, Shinobu; Matsui, Takao

2007-06-01

Institute of Accelerator Analysis Ltd. (IAA) is the first Contract Research Organization in Japan providing Accelerator Mass Spectrometry (AMS) analysis services for carbon dating and bioanalysis works. The 3 MV AMS machines are maintained by validated analysis methods using multiple control compounds. It is confirmed that these AMS systems have reliabilities and sensitivities enough for each objective. The graphitization of samples for bioanalysis is prepared by our own purification lines including the measurement of total carbon content in the sample automatically. In this paper, we present the use of AMS analysis in human mass balance and metabolism profiling studies with IAA 3 MV AMS, comparing results obtained from the same samples with liquid scintillation counting (LSC). Human samples such as plasma, urine and feces were obtained from four healthy volunteers orally administered a 14C-labeled drug Y-700, a novel xanthine oxidase inhibitor, of which radioactivity was about 3 MBq (85 μCi). For AMS measurement, these samples were diluted 100-10,000-fold with pure-water or blank samples. The results indicated that AMS method had a good correlation with LSC method (e.g. plasma: r = 0.998, urine: r = 0.997, feces: r = 0.997), and that the drug recovery in the excreta exceeded 92%. The metabolite profiles of plasma, urine and feces obtained with HPLC-AMS corresponded to radio-HPLC results measured at much higher radioactivity level. These results revealed that AMS analysis at IAA is useful to measure 14C-concentration in bioanalysis studies at very low radioactivity level.

Analysis of dissolved organic carbon concentration and 13C isotopic signature by TOC-IRMS - assessment of analytical performance

NASA Astrophysics Data System (ADS)

Kirkels, Frédérique; Cerli, Chiara; Federherr, Eugen; Kalbitz, Karsten

2013-04-01

Stable carbon isotopes provide a powerful tool to assess carbon pools and their dynamics. Dissolved organic carbon (DOC) has been recognized to play an important role in ecosystem functioning and carbon cycling and has therefore gained increased research interest. However, direct measurement of 13C isotopic signature of carbon in the dissolved phase is technically challenging particularly using high temperature combustion. Until recently, mainly custom-made systems existed which were modified for coupling of TOC instruments with IRMS for simultaneous assessment of C content and isotopic signature. The variety of coupled systems showed differences in their analytical performances. For analysis of DOC high temperature combustion is recognized as best performing method, owing to its high efficiency of conversion to CO2 also for highly refractory components (e.g. humic, fulvic acids) present in DOC and soil extracts. Therefore, we tested high temperature combustion TOC coupled to IRMS (developed by Elementar Group) for bulk measurements of DOC concentration and 13C signature. The instruments are coupled via an Interface to exchange the carrier gas from O2 to He and to concentrate the derived CO2 for the isotope measurement. Analytical performance of the system was assessed for a variety of organic compounds characterized by different stability and complexity, including humic acid and DOM. We tested injection volumes between 0.2-3 ml, thereby enabling measurement of broad concentration ranges. With an injection volume of 0.5 ml (n=3, preceded by 1 discarded injection), DOC and 13C signatures for concentrations between 5-150 mg C/L were analyzed with high precision (standard deviation (SD) predominantly <0.1‰), good accuracy and linearity (overall SD <0.9‰). For the same settings, slightly higher variation in precision was observed among the lower concentration range and depending upon specific system conditions. Differences in 13C signatures of about 50‰ among samples did not affect the precision of the analysis of natural abundance and labeled samples. Natural DOM, derived from different soils and assessed at various concentrations, was measured with similar good analytical performance, and also tested for the effect of freezing and re-dissolving. We found good performance of TOC-IRMS in comparison with other systems capable of determining C concentration and isotopic signatures. We recognize the advantages of this system providing: - High sample throughput, short measurement time (15 minutes), flexible sample volume - Easy maintenance, handling, rapid sample preparation (no pretreatment) This preliminary assessment highlights wide-ranging opportunities for further research on concentrations and isotopic signatures by TOC-IRMS to elucidate the role of dissolved carbon in terrestrial and aquatic systems.

A Carbon Free Filter for Collection of Large Volume Samples of Cellular Biomass from Oligotrophic Waters

PubMed Central

Mailloux, Brian J.; Dochenetz, Audra; Bishop, Michael; Dong, Hailiang; Ziolkowski, Lori A.; Wommack, K. Eric; Sakowski, Eric G.; Onstott, Tullis C.; Slater, Greg F.

2018-01-01

Isotopic analysis of cellular biomass has greatly improved our understanding of carbon cycling in the environment. Compound specific radiocarbon analysis (CSRA) of cellular biomass is being increasingly applied in a number of fields. However, it is often difficult to collect sufficient cellular biomass for analysis from oligotrophic waters because easy-to-use filtering methods that are free of carbon contaminants do not exist. The goal of this work was to develop a new column based filter to autonomously collect high volume samples of biomass from oligotrophic waters for CSRA using material that can be baked at 450°C to remove potential organic contaminants. A series of filter materials were tested, including uncoated sand, ferrihydrite-coated sand, goethite-coated sand, aluminum-coated sand, uncoated glass wool, ferrihydrite-coated glass wool, and aluminum-coated glass wool, in the lab with 0.1 and 1.0 µm microspheres and E. coli. Results indicated that aluminum-coated glass wool was the most efficient filter and that the retention capacity of the filter far exceeded the biomass requirements for CSRA. Results from laboratory tests indicate that for oligotrophic waters with 1×105 cells ml−1, 117 L of water would need to be filtered to collect 100 µg of PLFA for bulk PLFA analysis and 2000 L for analysis of individual PLFAs. For field sampling, filtration tests on South African mine water indicated that after filtering 5955 liters, 450 µg of total PLFAs were present, ample biomass for radiocarbon analysis. In summary, we have developed a filter that is easy to use and deploy for collection of biomass for CSRA including total and individual PLFAs. PMID:22561839

[Awareness of health co-benefits of carbon emissions reduction in urban residents in Beijing: a cross-sectional survey].

PubMed

Gao, J H; Zhang, Y; Wang, J; Chen, H J; Zhang, G B; Liu, X B; Wu, H X; Li, J; Li, J; Liu, Q Y

2017-05-10

Objective: To understand the awareness of the health co-benefits of carbon emission reduction in urban residents in Beijing and the influencing factors, and provide information for policy decision on carbon emission reduction and health education campaigns. Methods: Four communities were selected randomly from Fangshan, Haidian, Huairou and Dongcheng districts of Beijing, respectively. The sample size was estimated by using Kish-Leslie formula for descriptive analysis. 90 participants were recruited from each community. χ (2) test was conducted to examine the associations between socio-demographic variables and individuals' awareness of the health co-benefits of carbon emission reduction. Ordinal logistic regression analysis was performed to investigate the factors influencing the awareness about the health co-benefits. Results: In 369 participants surveyed, 12.7 % reported they knew the health co-benefits of carbon emission reduction. The final logistic regression analysis revealed that age ( OR =0.98), attitude to climate warming ( OR =0.72) and air pollution ( OR =1.59), family monthly average income ( OR =1.27), and low carbon lifestyle ( OR =2.36) were important factors influencing their awareness of the health co-benefits of carbon emission reduction. Conclusion: The awareness of the health co-benefits of carbon emissions reduction were influenced by people' socio-demographic characteristics (age and family income), concerns about air pollution and climate warming, and low carbon lifestyle. It is necessary to take these factors into consideration in future development and implementation of carbon emission reduction policies and related health education campaigns.

Source attribution of black carbon in Arctic snow.

PubMed

Hegg, Dean A; Warren, Stephen G; Grenfell, Thomas C; Doherty, Sarah J; Larson, Timothy V; Clarke, Antony D

2009-06-01

Snow samples obtained at 36 sites in Alaska, Canada, Greenland, Russia, and the Arctic Ocean in early 2007 were analyzed for light-absorbing aerosol concentration together with a suite of associated chemical species. The light absorption data, interpreted as black carbon concentrations, and other chemical data were input into the EPA PMF 1.1 receptor model to explore the sources for black carbon in the snow. The analysis found four factors or sources: two distinct biomass burning sources, a pollution source, and a marine source. The first three of these were responsible for essentially all of the black carbon, with the two biomass sources (encompassing both open and closed combustion) together accounting for >90% of the black carbon.

Spectroscopic quantification of extremely rare molecular species in the presence of interfering optical absorption

DOEpatents

Ognibene, Ted; Bench, Graham; McCartt, Alan Daniel; Turteltaub, Kenneth; Rella, Chris W.; Tan, Sze; Hoffnagle, John A.; Crosson, Eric

2017-05-09

Optical spectrometer apparatus, systems, and methods for analysis of carbon-14 including a resonant optical cavity configured to accept a sample gas including carbon-14, an optical source configured to deliver optical radiation to the resonant optical cavity, an optical detector configured to detect optical radiation emitted from the resonant cavity and to provide a detector signal; and a processor configured to compute a carbon-14 concentration from the detector signal, wherein computing the carbon-14 concentration from the detector signal includes fitting a spectroscopic model to a measured spectrogram, wherein the spectroscopic model accounts for contributions from one or more interfering species that spectroscopically interfere with carbon-14.

Conductive carbon tape used for support and mounting of both whole animal and fragile heat-treated tissue sections for MALDI MS imaging and quantitation.

PubMed

Goodwin, Richard J A; Nilsson, Anna; Borg, Daniel; Langridge-Smith, Pat R R; Harrison, David J; Mackay, C Logan; Iverson, Suzanne L; Andrén, Per E

2012-08-30

Analysis of whole animal tissue sections by MALDI MS imaging (MSI) requires effective sample collection and transfer methods to allow the highest quality of in situ analysis of small or hard to dissect tissues. We report on the use of double-sided adhesive conductive carbon tape during whole adult rat tissue sectioning of carboxymethyl cellulose (CMC) embedded animals, with samples mounted onto large format conductive glass and conductive plastic MALDI targets, enabling MSI analysis to be performed on both TOF and FT-ICR MALDI mass spectrometers. We show that mounting does not unduly affect small molecule MSI detection by analyzing tiotropium abundance and distribution in rat lung tissues, with direct on-tissue quantitation achieved. Significantly, we use the adhesive tape to provide support to embedded delicate heat-stabilized tissues, enabling sectioning and mounting to be performed that maintained tissue integrity on samples that had previously been impossible to adequately prepare section for MSI analysis. The mapping of larger peptidomic molecules was not hindered by tape mounting samples and we demonstrate this by mapping the distribution of PEP-19 in both native and heat-stabilized rat brains. Furthermore, we show that without heat stabilization PEP-19 degradation fragments can detected and identified directly by MALDI MSI analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

The Combustion Experiment on the Sample Analysis at Mars (SAM) Instrument Suite on the Curiosity Rover

NASA Technical Reports Server (NTRS)

Stern, J. C.; Malespin, C. A.; Eigenbrode, J. L.; Graham, H. V.; Archer, P. D., Jr.; Brunner, A. E.; Freissinet, C.; Franz, H. B.; Fuentes, J.; Glavin, D. P.;

Extraneous carbon assessment in ultra-microscale radiocarbon analysis using benzene polycarboxylic acids (BPCA)

NASA Astrophysics Data System (ADS)

Hanke, Ulrich M.; McIntyre, Cameron P.; Schmidt, Michael W. I.; Wacker, Lukas; Eglinton, Timothy I.

2016-04-01

Measurements of the natural abundance of radiocarbon (14C) concentrations in inorganic and organic carbon-containing materials can be used to investigate their date of origin. Particularly, the biogeochemical cycling of specific compounds in the environment may be investigated applying molecular marker analyses. However, the isolation of specific molecules from environmental matrices requires a complex processing procedure resulting in small sample sizes that often contain less than 30 μg C. Such small samples are sensitive to extraneous carbon (Cex) that is introduced during the purification of the compounds (Shah and Pearson, 2007). We present a thorough radiocarbon blank assessment for benzene polycarboxylic acids (BPCA), a proxy for combustion products that are formed during the oxidative degradation of condensed polyaromatic structures (Wiedemeier et al, in press). The extraneous carbon assessment includes reference material for (1) chemical extraction, (2) preparative liquid chromatography (3) wet chemical oxidation which are subsequently measured with gas ion source AMS (Accelerator Mass Spectrometer, 5-100 μg C). We always use pairs of reference materials, radiocarbon depleted (14Cfossil) and modern (14Cmodern) to determine the fraction modern (F14C) of Cex.Our results include detailed information about the quantification of Cex in radiocarbon molecular marker analysis using BPCA. Error propagation calculations indicate that ultra-microscale samples (20-30 μg) are feasible with uncertainties of less than 10 %. Calculations of the constant contamination reveal important information about the source (F14C) and mass (μg) of Cex (Wacker and Christl, 2011) for each sub procedure. An external correction of compound specific radiocarbon data is essential for robust results that allow for a high degree of confidence in the 14C results. References Shah and Pearson, 2007. Ultra-microscale (5-25μg C) analysis of individual lipids by 14C AMS: Assessment and correction for sample processing blanks. Radiocarbon 49(1), 69-82. Wacker, L. and M. Christl. 2011. Data reduction for small radiocarbon samples - error propagation using the model of constant contamination. Ion Beam Physics, ETH Zurich, Annual report 2011. Wiedemeier, D.B., S.Q. Lang, M. Gierga, S. Abiven, S.M. Bernasconi, G.L. Bernasconi-Green, I. Hajdas, U.M. Hanke, M.D. Hilf, C.P. McIntyre, M.P.W. Schneider, R.H. Smittenberg, L. Wacker, G.L.B. Wiesenberg, M.W.I. Schmidt. Characterization, quantification and compound-specific isotopic analysis of pyrogenic carbon using benzene polycarboxylic acids (BPCA). Journal of Visualized Experiments. In press.

Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

PubMed

Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

2006-12-22

Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

A study on the cytotoxicity of carbon-based materials

DOE PAGES

Saha, Dipendu; Heldt, Caryn L.; Gencoglu, Maria F.; ...

2016-05-25

With an aim to understand the origin and key contributing factors towards carboninduced cytotoxicity, we have studied five different carbon samples with diverse surface area, pore width, shape and size, conductivity and surface functionality. All the carbon materials were characterized with surface area and pore size distribution, x-ray photoelectron spectroscopy (XPS) and electron microscopic imaging. We performed cytotoxicity study in Caco-2 cells by colorimetric assay, oxidative stress analysis by reactive oxygen species (ROX) detection, cellular metabolic activity measurement by adenosine triphosphate (ATP) depletion and visualization of cellular internalization by TEM imaging. The carbon materials demonstrated a varying degree of cytotoxicitymore » in contact with Caco-2 cells. The lowest cell survival rate was observed for nanographene, which possessed the minimal size amongst all the carbon samples under study. None of the carbons induced oxidative stress to the cells as indicated by the ROX generation results. Cellular metabolic activity study revealed that the carbon materials caused ATP depletion in cells and nanographene caused the highest depletion. Visual observation by TEM imaging indicated the cellular internalization of nanographene. This study confirmed that the size is the key cause of carbon-induced cytotoxicity and it is probably caused by the ATP depletion within the cell.« less

Effect of Carbon Nanotubes Upon Emissions From Cutting and Sanding Carbon Fiber-Epoxy Composites

PubMed Central

Heitbrink, William A.; Lo, Li-Ming

2015-01-01

Carbon nanotubes (CNTs) are being incorporated into structural composites to enhance material strength. During fabrication or repair activities, machining nanocomposites may release CNTs into the workplace air. An experimental study was conducted to evaluate the emissions generated by cutting and sanding on three types of epoxy-composite panels: Panel A containing graphite fibers, Panel B containing graphite fibers and carbon-based mat, and Panel C containing graphite fibers, carbon-based mat, and multi-walled CNTs. Aerosol sampling was conducted with direct-reading instruments, and filter samples were collected for measuring elemental carbon (EC) and fiber concentrations. Our study results showed that cutting Panel C with a band saw did not generate detectable emissions of fibers inspected by transmission electron microscopy but did increase the particle mass, number, and EC emission concentrations by 20% to 80% compared to Panels A and B. Sanding operation performed on two Panel C resulted in fiber emission rates of 1.9×108 and 2.8×106 fibers per second (f/s), while no free aerosol fibers were detected from sanding Panels A and B containing no CNTs. These free CNT fibers may be a health concern. However, the analysis of particle and EC concentrations from these same samples cannot clearly indicate the presence of CNTs, because extraneous aerosol generation from machining the composite epoxy material increased the mass concentrations of the EC. PMID:26478716

Analysis of vibrational response in graphite oxide nanoplatelets

NASA Astrophysics Data System (ADS)

Prias Barragan, Jhon Jairo; Gross, Katherine; Lajaunie, Luc; Arenal, Raul; Ariza Calderon, Hernando; Prieto, Pedro

In this work, we present a new low-cost fabrication process to obtain graphite oxide nanoplatelets from bamboo pyroligneous acid (GO-BPA) by thermal decomposition method using a pyrolysis system for different carbonization temperatures from 673 to 973 K. The GO-BPA samples were characterized by using Raman, FTIR, XRD, SEM and TEM techniques, whose results suggest that increased carbonization temperature increases graphite conversion, boundary defects, desorption of some organic compounds and phonon response, respectively. We discuss potential applications of the GO-BPA samples involving phonon response that would benefit from a fully scaled technology, advanced electronic sensors and devices.

A Passive Earth-Entry Capsule for Mars Sample Return

NASA Technical Reports Server (NTRS)

Mitcheltree, Robert A.; Kellas, Sotiris

1999-01-01

A combination of aerodynamic analysis and testing, aerothermodynamic analysis, structural analysis and testing, impact analysis and testing, thermal analysis, ground characterization tests, configuration packaging, and trajectory simulation are employed to determine the feasibility of an entirely passive Earth entry capsule for the Mars Sample Return mission. The design circumvents the potential failure modes of a parachute terminal descent system by replacing that system with passive energy absorbing material to cushion the Mars samples during ground impact. The suggested design utilizes a spherically blunted 45-degree half-angle cone forebody with an ablative heat shield. The primary structure is a hemispherical, composite sandwich enclosing carbon foam energy absorbing material. Though no demonstration test of the entire system is included, results of the tests and analysis presented indicate that the design is a viable option for the Mars Sample Return Mission.

Mechanisms contributing to the thermal analysis of waste incineration bottom ash and quantification of different carbon species.

PubMed

Rocca, Stefania; van Zomeren, André; Costa, Giulia; Dijkstra, Joris J; Comans, Rob N J; Lombardi, Francesco

2013-02-01

The focus of this study was to identify the main compounds affecting the weight changes of bottom ash (BA) in conventional loss on ignition (LOI) tests and to obtain a better understanding of the individual processes in heterogeneous (waste) materials such as BA. Evaluations were performed on BA samples from a refuse derived fuel incineration (RDF-I) plant and a hospital waste incineration (HW-I) plant using thermogravimetric analysis and subsequent mass spectrometry (TG-MS) analysis of the gaseous thermal decomposition products. Results of TG-MS analysis on RDF-I BA indicated that the LOI measured at 550°C was due to moisture evaporation and dehydration of Ca(OH)(2) and hydrocalumite. Results for the HW-I BA showed that LOI at 550°C was predominantly related to the elemental carbon (EC) content of the sample. Decomposition of CaCO(3) around 700°C was identified in both materials. In addition, we have identified reaction mechanisms that underestimate the EC and overestimate the CaCO(3) contents of the HW-I BA during TG-MS analyses. These types of artefacts are expected to occur also when conventional LOI methods are adopted, in particular for materials that contain CaO/Ca(OH)(2) in combination with EC and/or organic carbon, such as e.g. municipal solid waste incineration (MSWI) bottom and fly ashes. We suggest that the same mechanisms that we have found (i.e. in situ carbonation) can also occur during combustion of the waste in the incinerator (between 450 and 650°C) demonstrating that the presence of carbonate in bottom ash is not necessarily indicative for weathering. These results may also give direction to further optimization of waste incineration technologies with regard to stimulating in situ carbonation during incineration and subsequent potential improvement of the leaching behavior of bottom ash. Copyright © 2012 Elsevier Ltd. All rights reserved.

Elucidating Adsorptive Fractions of Natural Organic Matter on Carbon Nanotubes.

PubMed

Ateia, Mohamed; Apul, Onur G; Shimizu, Yuta; Muflihah, Astri; Yoshimura, Chihiro; Karanfil, Tanju

2017-06-20

Natural organic matter (NOM) is a heterogeneous mixture of organic compounds that is omnipresent in natural waters. To date, the understanding of the adsorption of NOM components by carbon nanotubes (CNTs) is limited because of the limited number of comprehensive studies in the literature examining the adsorption of NOM by CNTs. In this study, 11 standard NOM samples from various sources were characterized, and their adsorption behaviors on four different CNTs were examined side-by-side using total organic carbon, fluorescence, UV-visible spectroscopy, and high-performance size-exclusion chromatography (HPSEC) analysis. Adsorption was influenced by the chemical properties of the NOM, including aromaticity, degree of oxidation, and carboxylic acidity. Fluorescence excitation-emission matrix (EEM) analysis showed preferential adsorption of decomposed and terrestrial-derived NOM compared to freshly produced and microbial-derived NOM. HPSEC analysis revealed preferential adsorption of fractions in the molecular weight range of 0.5-2 kDa for humic acids but in the molecular weight range of 1-3 kDa for all fulvic acids and reverse-osmosis isolates. However, the smallest characterized fraction (MW < 0.4 kDa) in all samples did not adsorb on the CNTs.

Rapid Measurement of Soil Carbon in Rice Paddy Field of Lombok Island Indonesia Using Near Infrared Technology

NASA Astrophysics Data System (ADS)

Kusumo, B. H.; Sukartono, S.; Bustan, B.

2018-02-01

Measuring soil organic carbon (C) using conventional analysis is tedious procedure, time consuming and expensive. It is needed simple procedure which is cheap and saves time. Near infrared technology offers rapid procedure as it works based on the soil spectral reflectance and without any chemicals. The aim of this research is to test whether this technology able to rapidly measure soil organic C in rice paddy field. Soil samples were collected from rice paddy field of Lombok Island Indonesia, and the coordinates of the samples were recorded. Parts of the samples were analysed using conventional analysis (Walkley and Black) and some other parts were scanned using near infrared spectroscopy (NIRS) for soil spectral collection. Partial Least Square Regression (PLSR) Models were developed using data of soil C analysed using conventional analysis and data from soil spectral reflectance. The models were moderately successful to measure soil C in rice paddy field of Lombok Island. This shows that the NIR technology can be further used to monitor the C change in rice paddy soil.

Changes in the dissolved organic matter leaching from soil under severe temperature and N-deposition.

PubMed

Nguyen, Hang Vo-Minh; Choi, Jung Hyun

2015-06-01

In this study, we conducted growth chamber experiments using three types of soil (wetland, rice paddy, and forest) under the conditions of a severe increase in the temperature and N-deposition in order to investigate how extreme weather influences the characteristics of the dissolved organic matter (DOM) leaching from different soil types. This leachate controls the quantity and quality of DOM in surface water systems. After 5 months of incubation, the dissolved organic carbon (DOC) concentrations decreased in the range of 21.1 to 88.9 %, while the specific UV absorption (SUVA) values increased substantially in the range of 19.9 to 319.9 % for all of the samples. Higher increases in the SUVA values were observed at higher temperatures, whereas the opposite trend was observed for samples with N-addition. The parallel factor analysis (PARAFAC) results showed that four fluorescence components: terrestrial humic-like (component 1 (C1)), microbial humic-like (component 2 (C2)), protein-like (component 3 (C3)), and anthropogenic humic-like (component 4 (C4)) constituted the fluorescence matrices of soil samples. During the experiment, labile DOM from the soils was consumed and transformed into resistant aromatic carbon structures and less biodegradable components via microbial processes. The principle component analysis (PCA) results indicated that severe temperatures and N-deposition could enhance the contribution of the aromatic carbon compounds and humic-like components in the soil samples.

Nitrogen-doped carbon quantum dots as a fluorescence probe combined with magnetic solid-phase extraction purification for analysis of folic acid in human serum.

PubMed

Wang, Meng; Jiao, Yang; Cheng, Chunsheng; Hua, Jianhao; Yang, Yaling

2017-12-01

A novel and sensitive method based on nitrogen-doped carbon quantum dots as a fluorescence probe coupled with magnetic solid-phase extraction (MSPE) purification for analysis of folic acid (FA) in human serum samples has been established for the first time. In the developed system, magnetic nanoparticles coated with hexanoic acid (Fe 3 O 4 @C 6 ) were synthesized by a one-step chemical co-precipitation method with good magnetic properties and dispersibility for sample purification, and it is better to be separated from the sample. High fluorescence nitrogen-doped carbon quantum dots (N-CQDs), simply prepared using a one-step hydrothermal method with nitrilotriacetic acid, could be selectively quenched by FA. Based on this phenomenon, a fluorescence assay was proposed for specific determination of FA. Various operational experiment parameters have been studied and optimized in detail. Under the optimum experimental conditions, the detection limit of the proposed method for FA was evaluated to be 0.5 nM (S/N = 3), while the relative standard deviation (RSD) was 1.2% (n = 6). Finally, the proposed method was applied for determination of trace levels of FA from human serum samples and quantitative recoveries were achieved within the range of 95.7-103.5%. All of the results showed that the proposed method had significant application in further research. Graphical abstract Schematic of synthesis of N-CQDs and schematic of suggested mode for analysis of folic acid (FA).

Decomposition and particle release of a carbon nanotube/epoxy nanocomposite at elevated temperatures

NASA Astrophysics Data System (ADS)

Schlagenhauf, Lukas; Kuo, Yu-Ying; Bahk, Yeon Kyoung; Nüesch, Frank; Wang, Jing

2015-11-01

Carbon nanotubes (CNTs) as fillers in nanocomposites have attracted significant attention, and one of the applications is to use the CNTs as flame retardants. For such nanocomposites, possible release of CNTs at elevated temperatures after decomposition of the polymer matrix poses potential health threats. We investigated the airborne particle release from a decomposing multi-walled carbon nanotube (MWCNT)/epoxy nanocomposite in order to measure a possible release of MWCNTs. An experimental set-up was established that allows decomposing the samples in a furnace by exposure to increasing temperatures at a constant heating rate and under ambient air or nitrogen atmosphere. The particle analysis was performed by aerosol measurement devices and by transmission electron microscopy (TEM) of collected particles. Further, by the application of a thermal denuder, it was also possible to measure non-volatile particles only. Characterization of the tested samples and the decomposition kinetics were determined by the usage of thermogravimetric analysis (TGA). The particle release of different samples was investigated, of a neat epoxy, nanocomposites with 0.1 and 1 wt% MWCNTs, and nanocomposites with functionalized MWCNTs. The results showed that the added MWCNTs had little effect on the decomposition kinetics of the investigated samples, but the weight of the remaining residues after decomposition was influenced significantly. The measurements with decomposition in different atmospheres showed a release of a higher number of particles at temperatures below 300 °C when air was used. Analysis of collected particles by TEM revealed that no detectable amount of MWCNTs was released, but micrometer-sized fibrous particles were collected.

An interface for the direct coupling of small liquid samples to AMS

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

Ognibene, T. J.; Thomas, A. T.; Daley, P. F.

We describe the moving wire interface attached to the 1-MV AMS system at LLNL’s Center for Accelerator Mass Spectrometry for the analysis of nonvolatile liquid samples as either discrete drops or from the direct output of biochemical separatory instrumentation, such as high-performance liquid chromatography (HPLC). Discrete samples containing at least a few 10 s of nanograms of carbon and as little as 50 zmol 14C can be measured with a 3–5% precision in a few minutes. The dynamic range of our system spans approximately 3 orders in magnitude. Sample to sample memory is minimized by the use of fresh targetsmore » for each discrete sample or by minimizing the amount of carbon present in a peak generated by an HPLC containing a significant amount of 14C. As a result, liquid sample AMS provides a new technology to expand our biomedical AMS program by enabling the capability to measure low-level biochemicals in extremely small samples that would otherwise be inaccessible.« less

An interface for the direct coupling of small liquid samples to AMS

DOE PAGES

Ognibene, T. J.; Thomas, A. T.; Daley, P. F.; ...

2015-05-28

We describe the moving wire interface attached to the 1-MV AMS system at LLNL’s Center for Accelerator Mass Spectrometry for the analysis of nonvolatile liquid samples as either discrete drops or from the direct output of biochemical separatory instrumentation, such as high-performance liquid chromatography (HPLC). Discrete samples containing at least a few 10 s of nanograms of carbon and as little as 50 zmol 14C can be measured with a 3–5% precision in a few minutes. The dynamic range of our system spans approximately 3 orders in magnitude. Sample to sample memory is minimized by the use of fresh targetsmore » for each discrete sample or by minimizing the amount of carbon present in a peak generated by an HPLC containing a significant amount of 14C. As a result, liquid sample AMS provides a new technology to expand our biomedical AMS program by enabling the capability to measure low-level biochemicals in extremely small samples that would otherwise be inaccessible.« less

Characterization of a Carbon Nanotube Field Emission Electron Gun for the VAPoR Miniaturized Pyrolysis-Time-of-Flight Mass Spectrometer

NASA Technical Reports Server (NTRS)

Getty, Stephanie; Li, Mary; Costen, Nicholas; Hess, Larry; Feng, Steve; King, Todd; Brinckerhoff, William; Mahaffy, Paul; Glavin, Daniel

2009-01-01

We are developing the VAPoR (Volatile Analysis by Pyrolysis of Regolith) instrument towards studying soil composition, volatiles, and trapped noble gases in the polar regions of the Moon. VAPOR will ingest a soil sample and conduct analysis by pyrolysis and time-of-flight mass spectrometry (ToF-MS). Here, we describe miniaturization efforts within this development, including a carbon nanotube (CNT) field emission electron gun that is under consideration for use as the electron impact ionization source for the ToF-MS.

Photolysis of RDX in Aqueous Solution, With and Without Ozone

DTIC Science & Technology

1979-02-09

and compared with a standard prepared from the same TNT solution and an accurately weighed RDX sample in acetone ( 40 ppm). The GC analysis of the...aqueous carbon-14 RDX agreed with the weight ( 40 ppm). A stock solution of carbon-12 RDX in tap water was prepared by stirring an excess of RDX in 2 liters...as volatiles 8.4% " i10 7, 77 Y 40 ’ NSWC/WOL TR 78-175 Chemical Analysis of Acidified Reaction Mixture Nitrate ion: 4.91 x 10- M Ammonia: 2.5 x 10 -4

Characterization of the Particulate Emissions from the BP ...

EPA Pesticide Factsheets

Opportunistic particle samples were gathered from the sail of a tethered aerostat during at-sea plume sampling of the purposely-burned surface oil during the BP Deepwater Horizon disaster in the Gulf of Mexico. Particles were analyzed for polycyclic aromatic hydrocarbons (PAHs), organic carbon (OC), elemental carbon (EC), metals, and polychlorinated dibenzodioxins/dibenzofurans (PCDDs/PCDFs). Emission factors were calculated using previous sampling values of background-adjusted CO2 and particulate matter (PM)-bound C. The mean of five thermal-optical analyses indicated that the burned crude oil particulate matter was 93% carbon (w/w) with the predominance being refractory elemental carbon (82% w/w) on average. PAHs accounted for roughly 60 ug/g of the PM mass or 4.5 mg/kg oil burned, at least an order of magnitude less than earlier laboratory based studies. Microscopy indicates that the soot from the in situ oil burns is distinct from more common soot by its aggregate size, primary particle size, and nanostructure within the primary particles. The PCDD/PCDF concentration of the PM was 1.5 to 3.3 ng toxic equivalency (TEQ)/kg PM sampled, about 10-fold lower than from a previous dedicated gas/solid sample, indicating loss of small particle-bound and more volatile PCDD/PCDF congeners through the aerostat sail. This work presents an analysis of smoke particles opportunistically caught during the in situ surface oil burns during the 2010 BP Deepwater Horizon di

Organic geochemical analysis of sedimentary organic matter associated with uranium

USGS Publications Warehouse

Leventhal, J.S.; Daws, T.A.; Frye, J.S.

1986-01-01

Samples of sedimentary organic matter from several geologic environments and ages which are enriched in uranium (56 ppm to 12%) have been characterized. The three analytical techniqyes used to study the samples were Rock-Eval pyrolysis, pyrolysis-gas chromatography-mass spectrometry, and solid-state C-13 nuclear magnetic resonance (NMR) spectroscopy. In samples with low uranium content, the pyrolysis-gas chromatography products contain oxygenated functional groups (as hydroxyl) and molecules with both aliphatic and aromatic carbon atoms. These samples with low uranium content give measurable Rock-Eval hydrocarbon and organic-CO2 yields, and C-13 NMR values of > 30% aliphatic carbon. In contrast, uranium-rich samples have few hydrocarbon pyrolysis products, increased Rock-Eval organic-CO2 contents and > 70% aromatic carbon contents from C-13 NMR. The increase in aromaticity and decrease in hydrocarbon pyrolysis yield are related to the amount of uranium and the age of the uranium minerals, which correspond to the degree of radiation damage. The three analytical techniques give complementary results. Increase in Rock-Eval organic-CO2 yield correlates with uranium content for samples from the Grants uranium region. Calculations show that the amount of organic-CO2 corresponds to the quantity of uranium chemically reduced by the organic matter for the Grants uranium region samples. ?? 1986.

Carbonate system at Iheya North in Okinawa Trough~IODP drilling and post drilling environment~

NASA Astrophysics Data System (ADS)

Noguchi, T.; Hatta, M.; Sunamura, M.; Fukuba, T.; Suzue, T.; Kimoto, H.; Okamura, K.

2012-12-01

The Iheya North hydrothermal field in middle Okinawa Trough is covered with thick hemipelagic and volcanic sediment. Geochemical characteristics of Okinawa Trough is to provide abundant of CO2, CH4, NH4, H2, and H2S which originated from magmatic gases, sedimentary organic matters. On this hydrothermal field, a scientific drilling by Integrated Ocean Drilling Program (IODP) Expedition 331 was conducted to investigate metabolically diverse subseafloor microbial ecosystem and their physical and chemical settings. To clarify the spatial distribution of physical condition beneath seafloor around the hydrothermal filed, we focus on the carbonate species analysis to reconstruct in-situ pH, which regulate the diversities of microbial community and mineral composition. We developed the small sample volume dissolved total inorganic carbon (DIC) analyzer and conducted the onboard analysis for the interstitial water during IODP Exp.331. Total alkalinity, boron, phosphate, and ammonium also analyzed for thermodynamic calculation. In this presentation, we represent the spatial distribution of pH beneath the Iheya North hydrothermal field. In addition, we developed a 128 bottles multiple water sampler (ANEMONE) for post drilling environmental monitoring. ANEMONE sampler was deployed on the manned submersible Shinkai 6500 with other chemical sensors (CTD, turbidity, pH, ORP, and H2S), and collected the hydrothermal plume samples every 5 minutes during YK12-05 cruise by R/V Yokosuka (Japan Agency for Marine-Earth Science and Technology, JAMSTEC). DIC concentration of plume samples collected by ANEMONE sampler were analyzed just after submersible retrieve, and nutrients, manganese, density, and total cell counts determination were conducted onshore analysis. Based on these results, we describe the spatial distribution of DIC and carbonate system on Iheya North hydrothermal field (interstitial water, hydrothermal fluid, and hydrothermal plume).

Biosorption of phenanthrene by pure algae and field-collected planktons and their fractions.

PubMed

Zhang, Dainan; Ran, Chenyang; Yang, Yu; Ran, Yong

2013-09-01

The biosorption isotherms for phenanthrene (Phen) by cultured algae, field-collected plankton, and market algae samples (OSs) and their fractions (lipid-LP, lipid free carbon-LF, alkaline nonhydrolyzable carbon-ANHC, and acid nonhydrolyzable carbon-NHC) were established. All the biosorption isotherms are well fitted by the Freundlich model. The biosorption isotherms for the ANHC and NHC fractions are nonlinear and for the other fractions are linear. It was found that the NHC fractions are chemically and structurally different from other fractions by using elemental analysis and Fourier transformed infrared spectroscopy (FTIR), consisting mainly of aliphatic polymethylene carbon. The average KOC values for Phen at Ce=0.005Sw are 10706±2768mLg(-1) and 95843±55817mLg(-1) for the bulk market algal samples and their NHC isolates, respectively. As the NHC fraction for Porphyra contains higher polymethylene carbon than that for Seaweed or Spirulina, it exhibits higher biosorption capacity. Moreover, the logKOC values are significantly higher for the field-collected samples than for the market algae and cultured algae samples. The multivariate correlation shows that the logKOC values are positively related to the LP contents, and negatively to the C/N ratios for the original algal samples. Furthermore, the logKOC values are negatively related to the polarity indices (O/C and O+N/C) for the original samples and their fractions excluding LP fractions. These observations help to understand the role of polarity, LP and NHC fractions, and aliphatic structures in the biosorption of Phen, which requires more attention in the examination of sorption processes in the natural environment. Copyright © 2013 Elsevier Ltd. All rights reserved.

Sorption of Groundwater Dissolved Organic Carbon onto Minerals

NASA Astrophysics Data System (ADS)

Rutlidge, H.; Oudone, P.; McDonough, L.; Meredith, K.; Andersen, M. S.; O'Carrol, D. M.; Baker, A.

2017-12-01

Our understanding of groundwater organic matter (OM) as a carbon source or sink in the environmental carbon cycle is limited. The dynamics of groundwater OM is mainly governed by biological processing and its sorption to minerals. In saturated groundwaters, dissolved OM (DOM) represents one part of the groundwater organic carbon pool. Without consideration of the DOM sorption, it is not possible to quantify governing groundwater OM processes. This research explores the rate and extent of DOM sorption on different minerals. Groundwater DOM samples, and International Humic Substances Society (IHSS) standard solutions, were analysed. Each was mixed with a range of masses of iron coated quartz, clean quartz, and calcium carbonate, and shaken for 2 hours to reach equilibrium before being filtered through 0.2 μm for total dissolved organic carbon (DOC) and composition analysis by size-exclusion chromatography-organic carbon detection (LC-OCD). Sorption isotherms were constructed and groundwater DOM sorption were compared to the sorption of IHSS standards. Initial results suggest that for the IHSS standards, the operationally-defined humic substances fraction had the strongest sorption compared to the other LC-OCD fractions and total DOC. Some samples exhibited a small increase in the low molecular weight neutral (LMW-N) aqueous concentration with increasing humic substances sorption. This gradual increase observed could be the result of humic substances desorbing or their breakdown during the experiment. Further results comparing these IHSS standards with groundwater samples will be presented. In conjunction with complementary studies, these results can help provide more accurate prediction of whether groundwater OM is a carbon source or sink, which will enable the management of the groundwater resources as part of the carbon economy.

Three field tests of a gas filter correlation radiometer

NASA Technical Reports Server (NTRS)

Campbell, S. A.; Casas, J. C.; Condon, E. P.

1977-01-01

Test flights to remotely measure nonurban carbon monoxide (CO) concentrations by gas filter correlation radiometry are discussed. The inferred CO concentrations obtained through use of the Gas Filter Correlation Radiometer (GFCR) agreed with independent measurements obtained by gas chromatography air sample bottle analysis to within 20 percent. The equipment flown on board the aircraft, the flight test procedure, the gas chromatograph direct air sampling procedure, and the GFCR data analysis procedure are reported.

Investigation into calculating tree biomass and carbon in the FIADB using a biomass expansion factor approach

Treesearch

Linda S. Heath; Mark Hansen; James E. Smith; Patrick D. Miles

2009-01-01

The official U.S. forest carbon inventories (U.S. EPA 2008) have relied on tree biomass estimates that utilize diameter based prediction equations from Jenkins and others (2003), coupled with U.S. Forest Service, Forest Inventory and Analysis (FIA) sample tree measurements and forest area estimates. However, these biomass prediction equations are not the equations used...

Deep-Sea Carbonate Accumulation and Surface Ocean Saturation State in the Aftermath of the Cretaceous-Paleogene extinction

NASA Astrophysics Data System (ADS)

Pruss, S. B.; Higgins, J. A.; Bush, A. M.; Leckie, R. M.; Deeg, C.; Getzin, B. L.

2016-12-01

The role of the K-Pg extinction on biogeochemical cycling has been intensively studied in recent years. However, it remains unknown how extinctions in marine pelagic calcifiers impacted carbon cycling in the ocean. Low accumulation rates of microfossils in the aftermath of the extinction have been attributed to lowered production, which triggered a reduction in carbonate delivery to the seafloor. Interestingly, although microfossil abundance is lower and foraminifera are significantly smaller than in the latest Cretaceous, carbonate accumulated on the seafloor in the earliest Paleogene even in areas that should have been below the CCD. One such deep-water site in the South Pacific (U1370) was cored during IODP Expedition 329 in November 2010. We examined 16 samples from an anomalous carbonate layer provisionally assigned to lower Paleocene planktonic foraminiferal Zones P1a and P1b that preserves benthic and planktonic foraminifera. Carbon isotope values of the benthic species Nuttalies orealis range from 1.45 to 1.95‰ VPDB in the 16 samples. The planktonic species Parasubbotina pseudobulloides was only abundant enough for analysis in 4 samples, and these values range from 1.41 to 1.91‰ VPDB. We note, as others have, that no carbon isotope gradient existed between the benthic and planktonic foraminifera during the deposition of this carbonate layer, perhaps due to reduced primary production and/or export of organic carbon. The presence of this carbonate layer in the deep ocean and its preservation of a collapsed isotopic gradient are both consistent with a reduction in the surface-to-deep water gradient in carbonate saturation state during the unusual oceanographic conditions that followed the extinction. We speculate that this was associated with a sustained reduction in surface ocean saturation state with adverse consequences for neritic carbonate producers in the aftermath of the K-T extinction.

Carbon isotope analysis of dissolved organic carbon in fresh and saline (NaCl) water via continuous flow cavity ring-down spectroscopy following wet chemical oxidation

USGS Publications Warehouse

Conaway, Christopher; Thomas, Randal B.; Saad, Nabil; Thordsen, James J.; Kharaka, Yousif K.

2015-01-01

This work examines the performance and limitations of a wet chemical oxidation carbon analyser interfaced with a cavity ring-down spectrometer (WCO-CRDS) in a continuous flow (CF) configuration for measuring δ13C of dissolved organic carbon (δ13C-DOC) in natural water samples. Low-chloride matrix (<5 g Cl/L) DOC solutions were analysed with as little as 2.5 mg C/L in a 9 mL aliquot with a precision of 0.5 ‰. In high-chloride matrix (10–100 g Cl/L) DOC solutions, bias towards lighter δ13C-DOC was observed because of incomplete oxidation despite using high-concentration oxidant, extended reaction time, or post-wet chemical oxidation gas-phase combustion. However, through a combination of dilution, chloride removal, and increasing the oxidant:sample ratio, high-salinity samples with sufficient DOC (>22.5 µg C/aliquot) may be analysed. The WCO-CRDS approach requires more total carbon (µg C/aliquot) than conventional CF-isotope ratio mass spectrometer, but is nonetheless applicable to a wide range of DOC concentration and water types, including brackish water, produced water, and basinal brines.

Larnite powders and larnite/silica aerogel composites as effective agents for CO2 sequestration by carbonation.

PubMed

Santos, A; Ajbary, M; Morales-Flórez, V; Kherbeche, A; Piñero, M; Esquivias, L

2009-09-15

This paper presents the results of the carbonation reaction of two sample types: larnite (Ca(2)SiO(4)) powders and larnite/silica aerogel composites, the larnite acting as an active phase in a process of direct mineral carbonation. First, larnite powders were synthesized by the reaction of colloidal silica and calcium nitrate in the presence of ethylene glycol. Then, to synthesize the composites, the surface of the larnite powders was chemically modified with 3-aminopropyltriethoxysilane (APTES), and later this mixture was added to a silica sol previously prepared from tetraethylorthosilicate (TEOS). The resulting humid gel was dried in an autoclave under supercritical conditions for the ethanol. The textures and chemical compositions of the powders and composites were characterized.The carbonation reaction of both types of samples was evaluated by means of X-ray diffraction and thermogravimetric analysis. Both techniques confirm the high efficiency of the reaction at room temperature and atmospheric pressure. A complete transformation of the silicate into carbonate resulted after submitting the samples to a flow of pure CO(2) for 15 min. This indicates that for this reaction time, 1t of larnite could eliminate about 550 kg of CO(2). The grain size, porosity, and specific surface area are the factors controlling the reaction.

Effect of coating mild steel with CNTs on its mechanical properties and corrosion behaviour in acidic medium

NASA Astrophysics Data System (ADS)

Abdulmalik Abdulrahaman, Mahmud; Kamaldeeen Abubakre, Oladiran; Ambali Abdulkareem, Saka; Oladejo Tijani, Jimoh; Aliyu, Ahmed; Afolabi, Ayo Samuel

2017-03-01

The study investigated the mechanical properties and corrosion behaviour of mild steel coated with carbon nanotubes at different coating conditions. Multi-walled carbon nanotubes (MWCNTs) were synthesized via the conventional chemical vapour deposition reaction using bimetallic Fe-Ni catalyst supported on kaolin, with acetylene gas as a carbon source. The HRSEM/HRTEM analysis of the purified carbon materials revealed significant reduction in the diameters of the purified MWCNT bundles from 50 nm to 2 nm and was attributed to the ultrasonication assisted dispersion with surfactant (gum arabic) employed in purification process. The network of the dispersed MWCNTs was coated onto the surfaces of mild steel samples, and as the coating temperature and holding time increased, the coating thickness reduced. The mechanical properties (tensile strength, yield strength, hardness value) of the coated steel samples increased with increase in coating temperature and holding time. Comparing the different coating conditions, coated mild steels at the temperature of 950 °C for 90 min holding time exhibited high hardness, yield strength and tensile strength values compared to others. The corrosion current and corrosion rate of the coated mild steel samples decreased with increase in holding time and coating temperature. The lowest corrosion rate was observed on sample coated at 950 °C for 90 min.

Detection of Evolved Carbon Dioxide in the Rocknest Eolian Bedform by the Sample Analysis at Mars(SAM) Instrument at the Mars Curiosity Landing Site

NASA Technical Reports Server (NTRS)

Sutter, B.; Archer, D.; McAdam, A.; Franz, H.; Ming, D. W.; Eigenbrode, J. L.; Glavin, D. P.; Mahaffy, P.; Stern, J.; Navarro-Gonzalez, R.

2013-01-01

The Sample Analysis at Mars (SAM) instrument detected four releases of carbon dioxide (CO2) that ranged from 100 to 700 C from the Rocknest eolian bedform material (Fig. 1). Candidate sources of CO2 include adsorbed CO2, carbonate(s), combusted organics that are either derived from terrestrial contamination and/or of martian origin, occluded or trapped CO2, and other sources that have yet to be determined. The Phoenix Lander s Thermal Evolved Gas Analyzer (TEGA) detected two CO2 releases (400-600, 700-840 C) [1,2]. The low temperature release was attributed to Fe- and/or Mg carbonates [1,2], per-chlorate interactions with carbonates [3], nanophase carbonates [4] and/or combusted organics [1]. The high temperature CO2 release was attributed to a calcium bearing carbonate [1,2]. No evidence of a high temperature CO2 release similar to the Phoenix material was detected in the Rocknest materials by SAM. The objectives of this work are to evaluate the temperature and total contribution of each Rocknest CO2 release and their possible sources. Four CO2 releases from the Rocknest material were detected by SAM. Potential sources of CO2 are adsorbed CO2, (peak 1) and Fe/Mg carbonates (peak 4). Only a fraction of peaks 2 and 3 (0.01 C wt.%) may be partially attributed to combustion of organic contamination. Meteoritic organics mixed in the Rocknest bedform could be present, but the peak 2 and 3 C concentration (approx.0.21 C wt. %) is likely too high to be attributed solely to meteoritic organic C. Other inorganic sources of C such as interactions of perchlorates and carbonates and sources yet to be identified will be evaluated to account for CO2 released from the thermal decomposition of Rocknest material.

Implanted Deuterium Retention and Release in Carbon-Coated Beryllium

NASA Astrophysics Data System (ADS)

Anderl, R. A.; Longhurst, G. R.; Pawelko, R. J.; Oates, M. A.

1997-06-01

Deuterium implantation experiments have been conducted on samples of clean and carbon-coated beryllium. These studies entailed preparation and characterization of beryllium samples coated with carbon thicknesses of 100, 500, and 1000 Å. Heat treatment of a beryllium sample coated with carbon to a thickness of approximately 100 Å revealed that exposure to a temperature of 400°C under high vacuum conditions was sufficient to cause substantial diffusion of beryllium through the carbon layer, resulting in more beryllium than carbon at the surface. Comparable concentrations of carbon and beryllium were observed in the bulk of the coating layer. Higher than expected oxygen levels were observed throughout the coating layer as well. Samples were exposed to deuterium implantation followed by thermal desorption without exposure to air. Differences were observed in deuterium retention and postimplantation release behavior in the carbon-coated samples as compared with bare samples. For comparable implantation conditions (sample temperature of 400°C and an incident deuterium flux of approximately 6 × 1019 D/m2-s), the quantity of deuterium retained in the bare sample was less than that retained in the carbon-coated samples. Further, the release of the deuterium took place at lower temperatures for the bare beryllium surfaces than for carbon-coated beryllium samples.

Particle size analysis on density, surface morphology and specific capacitance of carbon electrode from rubber wood sawdust

NASA Astrophysics Data System (ADS)

Taer, E.; Kurniasih, B.; Sari, F. P.; Zulkifli, Taslim, R.; Sugianto, Purnama, A.; Apriwandi, Susanti, Y.

2018-02-01

The particle size analysis for supercapacitor carbon electrodes from rubber wood sawdust (SGKK) has been done successfully. The electrode particle size was reviewed against the properties such as density, degree of crystallinity, surface morphology and specific capacitance. The variations in particle size were made by different treatment on the grinding and sieving process. The sample particle size was distinguished as 53-100 µm for 20 h (SA), 38-53 µm for 20 h (SB) and < 38 µm with variations of grinding time for 40 h (SC) and 80 h (SD) respectively. All of the samples were activated by 0.4 M KOH solution. Carbon electrodes were carbonized at temperature of 600oC in N2 gas environment and then followed by CO2 gas activation at a temperature of 900oC for 2 h. The densities for each variation in the particle size were 1.034 g cm-3, 0.849 g cm-3, 0.892 g cm-3 and 0.982 g cm-3 respectively. The morphological study identified the distance between the particles more closely at 38-53 µm (SB) particle size. The electrochemical properties of supercapacitor cells have been investigated using electrochemical methods such as impedance spectroscopy and charge-discharge at constant current using Solatron 1280 tools. Electrochemical properties testing results have shown SB samples with a particle size of 38-53 µm produce supercapacitor cells with optimum capacitive performance.

Potential artifacts associated with historical preparation of joint compound samples and reported airborne asbestos concentrations.

PubMed

Brorby, G P; Sheehan, P J; Berman, D W; Bogen, K T; Holm, S E

2011-05-01

Airborne samples collected in the 1970s for drywall workers using asbestos-containing joint compounds were likely prepared and analyzed according to National Institute of Occupational Safety and Health Method P&CAM 239, the historical precursor to current Method 7400. Experimentation with a re-created, chrysotile-containing, carbonate-based joint compound suggested that analysis following sample preparation by the historical vs. current method produces different fiber counts, likely because of an interaction between the different clearing and mounting chemicals used and the carbonate-based joint compound matrix. Differences were also observed during analysis using Method 7402, depending on whether acetic acid/dimethylformamide or acetone was used during preparation to collapse the filter. Specifically, air samples of sanded chrysotile-containing joint compound prepared by the historical method yielded fiber counts significantly greater (average of 1.7-fold, 95% confidence interval: 1.5- to 2.0-fold) than those obtained by the current method. In addition, air samples prepared by Method 7402 using acetic acid/dimethylformamide yielded fiber counts that were greater (2.8-fold, 95% confidence interval: 2.5- to 3.2-fold) than those prepared by this method using acetone. These results indicated (1) there is an interaction between Method P&CAM 239 preparation chemicals and the carbonate-based joint compound matrix that reveals fibers that were previously bound in the matrix, and (2) the same appeared to be true for Method 7402 preparation chemicals acetic acid/dimethylformamide. This difference in fiber counts is the opposite of what has been reported historically for samples of relatively pure chrysotile dusts prepared using the same chemicals. This preparation artifact should be considered when interpreting historical air samples for drywall workers prepared by Method P&CAM 239. Copyright © 2011 JOEH, LLC

Experimental Investigation on the Specific Heat of Carbonized Phenolic Resin-Based Ablative Materials

NASA Astrophysics Data System (ADS)

Zhao, Te; Ye, Hong; Zhang, Lisong; Cai, Qilin

2017-10-01

As typical phenolic resin-based ablative materials, the high silica/phenolic and carbon/phenolic composites are widely used in aerospace field. The specific heat of the carbonized ablators after ablation is an important thermophysical parameter in the process of heat transfer, but it is rarely reported. In this investigation, the carbonized samples of the high silica/phenolic and carbon/phenolic were obtained through carbonization experiments, and the specific heat of the carbonized samples was determined by a 3D DSC from 150 °C to 970 °C. Structural and compositional characterizations were performed to determine the mass fractions of the fiber and the carbonized product of phenolic which are the two constituents of the carbonized samples, while the specific heat of each constituent was also measured by 3D DSC. The masses of the carbonized samples were reduced when heated to a high temperature in the specific heat measurements, due to the thermal degradation of the carbonized product of phenolic resin in the carbonized samples. The raw experimental specific heat of the two carbonized samples and the carbonized product of phenolic resin was modified according to the quality changes of the carbonized samples presented by TGA results. Based on the mass fraction and the specific heat of each constituent, a weighted average method was adopted to obtain the calculated results of the carbonized samples. Due to the unconsolidated property of the fiber samples which impacts the reliability of the DSC measurement, there is a certain deviation between the experimental and calculated results of the carbonized samples. Considering the similarity of composition and structure, the data of quartz glass and graphite were used to substitute the specific heat of the high silica fiber and carbon fiber, respectively, resulting in better agreements with the experimental ones. Furthermore, the accurate specific heat of the high silica fiber and carbon fiber bundles was obtained by inversion, enabling the prediction of the specific heat of the carbonized ablators with different constituent mass fractions by means of the weighted average method in engineering.

Novel nitrogen doped carbon dots for corrosion inhibition of carbon steel in 1 M HCl solution

NASA Astrophysics Data System (ADS)

Cui, Mingjun; Ren, Siming; Zhao, Haichao; Wang, Liping; Xue, Qunji

2018-06-01

Nitrogen doped carbon dots (NCDs) were synthesized and used for inhibiting the corrosion of Q235 carbon steel in hydrochloric acid (HCl) solution. Inhibition effectiveness in short- and long-term immersion was examined using electrochemical measurements, weight loss and surface analysis. Results revealed the inhibition efficiency was improved significantly after adding NCDs and strongly dependent on the concentration of NCDs. SVET results showed that the sample immersed in HCl solution with NCDs showed lower anodic current density mapping than that in blank HCl solution. According to the data extracted from the Langmuir adsorption, the absorption of NCDs involved both chemisorption and physisorption.

Integrated investigation of the mixed origin of lunar sample 72161,11

NASA Technical Reports Server (NTRS)

Basu, A.; Des Marais, D. J.; Hayes, J. M.; Meinschein, W. G.

1975-01-01

The comminution-agglutination model and the solar-wind implantation-retention model are used to postulate the origins of the particulate components of lunar sample (72161,11), a submillimeter fraction of a surface sample for the dark mantle regolith at LRV-3. Grain-size analysis was performed by wet sieving with liquid argon, and analyses for CO2, CO, CH4, and H2 were carried out by stepwise pyrolysis in a helium atmosphere. The results indicate that the present sample is from a mature regolith, but the agglutinate content is only 30% in the particle-size range between 90 and 177 microns, indicating an apparent departure from steady state. Analyses of the carbon, methane, and hydrogen concentrations in size fractions larger than 149 microns show that the volume-correlated component of these species increases with increased grain size. It is suggested that the observed increase can be explained in terms of mixing of a dominant local population of coarser agglutinates having high carbon and hydrogen concentrations with an imported population of finer agglutinates relatively poor in carbon and hydrogen.

Carbon-monoxide poisoning in young drug addicts due to indoor use of a gasoline-powered generator.

PubMed

Marc, B; Bouchez-Buvry, A; Wepierre, J L; Boniol, L; Vaquero, P; Garnier, M

2001-06-01

We report six fatal cases of unintentional carbon-monoxide poisoning which occurred in a house occupied by young people. The source of carbon monoxide was a gasoline-powered generator. For all victims, an external body examination was carried out and blood and urine samples collected. Blood carboxyhaemoglobin (COHb) was performed using an automated visible spectrophotometric analysis. Blood-alcohol level quantification was performed using gas chromatography and drug screening in urine was performed by a one-step manual qualitative immunochromatography (Syva Rapid test, Behring Diagnostics Inc.) for benzoylecgonine (the main metabolite of cocaine in urine), morphine, 11-nor-Delta(9)-THC-9-COOH (cannabinoids) and d-methamphetamine. In all victims the COHb value was as high or higher than 65%. No alcohol was found in blood samples, but urine samples were positive for methamphetamine, cocaine and cannabis in five cases and for opiates in one case. In four victims, the urine sample was positive for at least three drugs. The availability and accuracy of rapid toxicological screening is an important tool for the medical examiner at the immediate scene of a clinical forensic examination.

Copper Decoration of Carbon Nanotubes and High Resolution Electron Microscopy

NASA Astrophysics Data System (ADS)

Probst, Camille

A new process of decorating carbon nanotubes with copper was developed for the fabrication of nanocomposite aluminum-nanotubes. The process consists of three stages: oxidation, activation and electroless copper plating on the nanotubes. The oxidation step was required to create chemical function on the nanotubes, essential for the activation step. Then, catalytic nanoparticles of tin-palladium were deposited on the tubes. Finally, during the electroless copper plating, copper particles with a size between 20 and 60 nm were uniformly deposited on the nanotubes surface. The reproducibility of the process was shown by using another type of carbon nanotube. The fabrication of nanocomposites aluminum-nanotubes was tested by aluminum vacuum infiltration. Although the infiltration of carbon nanotubes did not produce the expected results, an interesting electron microscopy sample was discovered during the process development: the activated carbon nanotubes. Secondly, scanning transmitted electron microscopy (STEM) imaging in SEM was analysed. The images were obtained with a new detector on the field emission scanning electron microscope (Hitachi S-4700). Various parameters were analysed with the use of two different samples: the activated carbon nanotubes (previously obtained) and gold-palladium nanodeposits. Influences of working distance, accelerating voltage or sample used on the spatial resolution of images obtained with SMART (Scanning Microscope Assessment and Resolution Testing) were analysed. An optimum working distance for the best spatial resolution related to the sample analysed was found for the imaging in STEM mode. Finally, relation between probe size and spatial resolution of backscattered electrons (BSE) images was studied. An image synthesis method was developed to generate the BSE images from backscattered electrons coefficients obtained with CASINO software. Spatial resolution of images was determined using SMART. The analysis shown that using a probe size smaller than the size of the observed object (sample features) does not improve the spatial resolution. In addition, the effects of the accelerating voltage, the current intensity and the sample geometry and composition were analysed.

Hyphenation of a carbon analyzer to photo-ionization mass spectrometry to unravel the organic composition of particulate matter on a molecular level.

PubMed

Grabowsky, Jana; Streibel, Thorsten; Sklorz, Martin; Chow, Judith C; Watson, John G; Mamakos, Athanasios; Zimmermann, Ralf

2011-12-01

The carbonaceous fraction of airborne particulate matter (PM) is of increasing interest due to the adverse health effects they are linked to. Its analytical ascertainment on a molecular level is still challenging. Hence, analysis of carbonaceous fractions is often carried out by determining bulk parameters such as the overall content of organic compounds (OC) and elemental carbon (EC) as well as the total carbon content, TC (sum of OC and EC), however, no information about the individual substances or substance classes, of which the single fractions consist can be obtained. In this work, a carbon analyzer and a photo-ionization time-of-flight mass spectrometer (PI-TOF-MS) were hyphenated to investigate individual compounds especially from the OC fractions. The carbon analyzer enables the stepwise heating of particle samples and provides the bulk parameters. With the PI-TOF-MS, it is possible to detect the organic compounds released during the single-temperature steps due to soft ionization and fast detection of the molecular ions. The hyphenation was designed, built up, characterized by standard substances, and applied to several kinds of samples, such as ambient aerosol, gasoline, and diesel emission as well as wood combustion emission samples. The ambient filter sample showed a strong impact of wood combustion markers. This was revealed by comparison to the product pattern of the similar analysis of pure cellulose and lignin and the wood combustion PM. At higher temperatures (450 °C), a shift to smaller molecules occurred due to the thermal decomposition of larger structures of oligomeric or polymeric nature comparable to lignocelluloses and similar oxygenated humic-like substances. Finally, particulate matter from gasoline and diesel containing 10% biodiesel vehicle exhaust has been analyzed. Gasoline-derived PM exhibited large polycyclic aromatic hydrocarbons, whereas diesel PM showed a much higher total organic content. The detected pattern revealed a strong influence of the biodiesel content on the nature of the particulate organic material.

Dissolved organic carbon concentrations and compositions, and trihalomethane formation potentials in waters from agricultural peat soils, Sacramento-San Joaquin Delta, California; implications for drinking-water quality

USGS Publications Warehouse

Fujii, Roger; Ranalli, Anthony J.; Aiken, George R.; Bergamaschi, Brian A.

1998-01-01

Water exported from the Sacramento-San Joaquin River delta (Delta) is an important drinking-water source for more than 20 million people in California. At times, this water contains elevated concentrations of dissolved organic carbon and bromide, and exceeds the U.S. Environmental Protection Agency's maximum contaminant level for trihalomethanes of 0.100 milligrams per liter if chlorinated for drinking water. About 20 to 50 percent of the trihalomethane precursors to Delta waters originates from drainage water from peat soils on Delta islands. This report elucidates some of the factors and processes controlling and affecting the concentration and quality of dissolved organic carbon released from peat soils and relates the propensity of dissolved organic carbon to form trihalomethanes to its chemical composition.Soil water was sampled from near-surface, oxidized, well-decomposed peat soil (upper soil zone) and deeper, reduced, fibrous peat soil (lower soil zone) from one agricultural field in the west central Delta over 1 year. Concentrations of dissolved organic carbon in the upper soil zone were highly variable, with median concentrations ranging from 46.4 to 83.2 milligrams per liter. Concentrations of dissolved organic carbon in samples from the lower soil zone were much less variable and generally slightly higher than samples from the upper soil zone, with median concentrations ranging from 49.3 to 82.3 milligrams per liter. The dissolved organic carbon from the lower soil zone had significantly higher aromaticity (as measured by specific ultraviolet absorbance) and contained significantly greater amounts of aromatic humic substances (as measured by XAD resin fractionation and carbon-13 nuclear magnetic resonance analysis of XAD isolates) than the dissolved organic carbon from the upper soil zone. These results support the conclusion that more aromatic forms of dissolved organic carbon are produced under anaerobic conditions compared to aerobic conditions. Dissolved organic carbon concentration, trihalomethane formation potential, and ultraviolet absorbance were all highly correlated, showing that trihalomethane precursors increased with increasing dissolved organic carbon and ultraviolet absorbance for whole water samples. Contrary to the generally accepted conceptual model for trihalomethane formation that assumes that aromatic forms of carbon are primary precursors to trihalomethanes, results from this study indicate that dissolved organic carbon aromaticity appears unrelated to trihalomethane formation on a carbon-normalized basis. Thus, dissolved organic carbon aromaticity alone cannot fully explain or predict trihalomethane precursor content, and further investigation of aromatic and nonaromatic forms of carbon will be needed to better identify trihalomethane precursors.

Summary of data from onsite and laboratory analyses of surface water and marsh porewater from South Florida Water Management District Water Conservation Areas, the Everglades, South Florida, March 1995

USGS Publications Warehouse

Reddy, Michael M.; Gunther, Charmaine D.

2012-01-01

This report presents results of chemical analysis for samples collected during March, 1995, as part of a study to quantify the interaction of aquatic organic material (referred to here as dissolved organic carbon with dissolved metal ions). The work was done in conjunction with the South Florida Water Management District, the U.S. Environmental Protection Agency, the U.S. Geological Survey South Florida Ecosystems Initiative, and the South Florida National Water Quality Assessment Study Unit. Samples were collected from surface canals and from marsh sites. Results are based on onsite and laboratory measurements for 27 samples collected at 10 locations. The data file contains sample description, dissolved organic carbon concentration and specific ultraviolet absorbance, and additional analytical data for samples collected at several sites in the Water Conservation Areas, the Everglades, south Florida.

Absorbent Analysis of Anniston Chemical Agent Disposal Facility Munition Demilitarization Building (MDB) Banks 1 and 2 Filter Samples Following Completion of The GB Agent and VX Rocket Campaigns

DTIC Science & Technology

2013-01-01

adsorbed on wet carbon (13 wt% water ). Left to right: initial and t = 6, 13, and 16 days ..............................3 2. 31 P MAS NMR spectra...obtained for 10 wt% VX adsorbed on wet carbon (13 wt% water ) Left to right: initial and t = 24 days ...............................................4...of feed air. Each Class A Type II filter contained approximately 48.2 lb of granular, activated, coconut shell-based carbon. A given filter bank

14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

NASA Astrophysics Data System (ADS)

Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

2017-12-01

Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

The Potential of Isotope Ratio Mass Spectrometry (IRMS) and Gas Chromatography-IRMS Analysis of Triacetone Triperoxide in Forensic Explosives Investigations.

PubMed

Bezemer, Karlijn D B; Koeberg, Mattijs; van der Heijden, Antoine E D M; van Driel, Chris A; Blaga, Cornelia; Bruinsma, Jildert; van Asten, Arian C

2016-09-01

Studying links between triacetone triperoxide (TATP) samples from crime scenes and suspects can assist in criminal investigations. Isotope ratio mass spectrometry (IRMS) and gas chromatography (GC)-IRMS were used to measure the isotopic compositions of TATP and its precursors acetone and hydrogen peroxide. In total, 31 TATP samples were synthesized with different raw material combinations and reaction conditions. For carbon, a good differentiation and a linear relationship were observed for acetone-TATP combinations. The extent of negative (δ(13) C) fractionation depended on the reaction yield. Limited enrichment was observed for the hydrogen isotope (δ(2) H) values of the TATP samples probably due to a constant exchange of hydrogen atoms in aqueous solution. For oxygen (δ(18) O), the small isotopic range and excess of water in hydrogen peroxide resulted in poor differentiation. GC-IRMS and IRMS data were comparable except for one TATP sample prepared with high acid concentration demonstrating the potential of compound-specific isotope analysis. Carbon IRMS has practical use in forensic TATP investigations. © 2016 American Academy of Forensic Sciences.

Improved Segmented-Flow Tracer-Monitored Titration for Automated Measurement of Total Alkalinity in Seawater

NASA Astrophysics Data System (ADS)

Spaulding, R. S.; Hales, B.; Beck, J. C.; Degrandpre, M. D.

2008-12-01

The four measurable inorganic carbon parameters commonly measured as part of oceanic carbon cycle studies are total dissolved inorganic carbon (DIC), total alkalinity (AT), hydrogen ion concentration (pH) and partial pressure of CO2 (pCO2). AT determination is critical for anthropogenic CO2 inventory calculations and for quantifying CaCO3 saturation. Additionally, measurement of AT in combination with one other carbonate parameter can be used to describe the inorganic carbon equilibria. Current methods for measuring AT require calibrated volumetric flasks and burettes, gravimetry, or precise flow measurements. These methods also require analysis times of ˜15 min and sample volumes of ˜200 mL, and sample introduction is not automated, resulting in labor-intensive measurements and low temporal resolution. The Tracer Monitored Titration (TMT) system was previously developed at the University of Montana for AT measurements. The TMT is not dependent on accurate gravimetric, volumetric or flow rate measurements because it relies on a pH-sensitive indicator (tracer) to track the amount of titrant added to the sample. Sample and a titrant-indicator mixture are mechanically stirred in an optical flow cell and pH is calculated using the indicator equilibrium constant and the spectrophotometrically determined concentrations of the acid and base forms of the indicator. AT is then determined using these data in a non-linear least squares regression of the AT mass and proton balances. The precision and accuracy of the TMT are 2 and 4 micromol per kg in 16 min using 110-mL of sample. The TMT is dependent on complete mixing of titrant with the sample and accurate absorbance measurements. We have developed the segmented-flow TMT (SF- TMT) to improve on these aspects and decrease sample analysis time. The TMT uses segmented flow instead of active mixing and a white LED instead of a tungsten-halogen light source. Air is added to the liquid flow stream, producing segments of liquid separated by air bubbles. Because liquid is not transferred between flow segments, there is rapid flushing which reduces sample volume to <10 mL. Additionally, the slower movement of liquid at the tube walls compared to that at the tube center creates circulation within each liquid segment, mixing the sample and eliminating the need for mechanical stirring. The white LED has higher output at the wavelengths of interest, thus improving the precision of absorbance measurements. These improvements result in a faster, simpler method for measuring AT.

Influence of surface properties on the mechanism of H2S removal by alkaline activated carbons.

PubMed

Yan, Rong; Chin, Terence; Ng, Yuen Ling; Duan, Huiqi; Liang, David Tee; Tay, Joo Hwa

2004-01-01

Alkaline activated carbons are widely used as adsorbents of hydrogen sulfide (H2S), one of the major odorous compounds arising from sewage treatment facilities. Although a number of studies have explored the effects of various parameters, mechanisms of H2S adsorption by alkaline carbons are not yet fully understood. The major difficulty seems to lie in the fact that little is known with certainty about the predominant reactions occurring on the carbon surface. In this study, the surface properties of alkaline activated carbons were systematically investigated to further exploit and better understand the mechanisms of H2S adsorption by alkaline activated carbons. Two commercially available alkaline activated carbons and their representative exhausted samples (8 samples collected at different height of the column after H2S breakthrough tests) were studied. The 8 portions of the exhausted carbon were used to represent the H2S/carbon reaction process. The surface properties of both the original and the exhausted carbons were characterized using the sorption of nitrogen (BET test), surface pH, Boehm titration, thermal and FTIR analysis. Porosity and surface area provide detailed information about the pore structure of the exhausted carbons with respect to the reaction extent facilitating the understanding of potential pore blockages. Results of Boehm titration and FTIR both demonstrate the significant effects of surface functional groups, and identification of oxidation products confirmed the different mechanisms involved with the two carbons. From the DTG curves of thermal analysis, two well-defined peaks representing two products of surface reactions (i.e., sulfur and sulfuric acid) were observed from the 8 exhausted portions with gradually changing patterns coinciding with the extent of the reaction. Surface pH values of the exhausted carbons show a clear trend of pH drop along the reaction extent, while pH around 2 was observed for the bottom of the bed indicating sulfuric acid as the predominant products. Although both carbons are coal-based and of KOH impregnated type, performances of different carbons differ significantly. A correlation is well established to link the reaction extent with various surface properties. In summary, not only the homogeneous alkali impregnation and physical porosity but also the carbon surface chemistry are significant factors influencing the performances of alkaline activated carbons as H2S adsorbents.

Thermogravimetric analysis of the interaction of ferromagnetic metal atom and multiwalled carbon nanotubes.

PubMed

Rawat, Naveen; Gudyaka, Russel; Kumar, Mohit; Joshi, Bharat; Santhanam, Kalathur S V

2008-04-01

This paper describes the thermal oxidative behavior of atomized iron or atomized cobalt in the presence of multiwalled carbon nanotubes (MWCNT). The thermogravimetric analysis shows the atomized iron thermal oxidation starts at about 500 degrees C that is absent when the atomized iron is sintered with multiwalled carbon naonotubes. The thermal oxidation of iron in the sintered samples requires the collapse of the multiwalled carbon nanotubes. A similar behavior is observed with atomized cobalt when its oxidation requires the collapse of the nanotubes. This thermal oxidative shift is interpreted as due to the atomized iron or atomized cobalt atom experiencing extensive overlap and confinement effect with multiwalled carbon nanotubes causing a spin transfer. This confinement effect is suggested to produce a transformation of iron from the outermost electronic distribution of 3d64s2 to an effective configuration of 3d84s0 and for cobalt 3d74s2 to 3d94s0 producing spintronics effect.

Thermal and Evolved Gas Analysis of "Nanophase" Carbonates: Implications for Thermal and Evolved Gas Analysis on Mars Missions

NASA Technical Reports Server (NTRS)

Lauer, Howard V., Jr.; Archer, P. D., Jr.; Sutter, B.; Niles, P. B.; Ming, Douglas W.

2012-01-01

Data collected by the Mars Phoenix Lander's Thermal and Evolved Gas Analyzer (TEGA) suggested the presence of calcium-rich carbonates as indicated by a high temperature CO2 release while a low temperature (approx.400-680 C) CO2 release suggested possible Mg- and/or Fe-carbonates [1,2]. Interpretations of the data collected by Mars remote instruments is done by comparing the mission data to a database on the thermal properties of well-characterized Martian analog materials collected under reduced and Earth ambient pressures [3,4]. We are proposing that "nano-phase" carbonates may also be contributing to the low temperature CO2 release. The objectives of this paper is to (1) characterize the thermal and evolved gas proper-ties of carbonates of varying particle size, (2) evaluate the CO2 releases from CO2 treated CaO samples and (3) examine the secondary CO2 release from reheated calcite of varying particle size.

Closing the carbon balance for fermentation by Clostridium thermocellum (ATCC 27405).

PubMed

Ellis, Lucas D; Holwerda, Evert K; Hogsett, David; Rogers, Steve; Shao, Xiongjun; Tschaplinski, Timothy; Thorne, Phil; Lynd, Lee R

2012-01-01

Our lab and most others have not been able to close a carbon balance for fermentation by the thermophilic, cellulolytic anaerobe, Clostridium thermocellum. We undertook a detailed accounting of product formation in C. thermocellum ATCC 27405. Elemental analysis revealed that for both cellulose (Avicel) and cellobiose, ≥92% of the substrate carbon utilized could be accounted for in the pellet, supernatant and off-gas when including sampling. However, 11.1% of the original substrate carbon was found in the liquid phase and not in the form of commonly-measured fermentation products--ethanol, acetate, lactate, and formate. Further detailed analysis revealed all the products to be <720 da and have not usually been associated with C. thermocellum fermentation, including malate, pyruvate, uracil, soluble glucans, and extracellular free amino acids. By accounting for these products, 92.9% and 93.2% of the final product carbon was identified during growth on cellobiose and Avicel, respectively. Copyright © 2011 Elsevier Ltd. All rights reserved.

Carbon fiber based composites stress analysis. Experimental and computer comparative studies

NASA Astrophysics Data System (ADS)

Sobek, M.; Baier, A.; Buchacz, A.; Grabowski, Ł.; Majzner, M.

2015-11-01

Composite materials used nowadays for the production of composites are the result of advanced research. This allows assuming that they are among the most elaborate tech products of our century. That fact is evidenced by the widespread use of them in the most demanding industries like aerospace and space industry. But the heterogeneous materials and their advantages have been known to mankind in ancient times and they have been used by nature for millions of years. Among the fibers used in the industry most commonly used are nylon, polyester, polypropylene, boron, metal, glass, carbon and aramid. Thanks to their physical properties last three fiber types deserve special attention. High strength to weight ratio allow the use of many industrial solutions. Composites based on carbon and glass fibers are widely used in the automotive. Aramid fibers ideal for the fashion industry where the fabric made from the fibers used to produce the protective clothing. In the paper presented issues of stress analysis of composite materials have been presented. The components of composite materials and principles of composition have been discussed. Particular attention was paid to the epoxy resins and the fabrics made from carbon fibers. The article also includes basic information about strain measurements performed on with a resistance strain gauge method. For the purpose of the laboratory tests a series of carbon - epoxy composite samples were made. For this purpose plain carbon textile was used with a weight of 200 g/mm2 and epoxy resin LG730. During laboratory strain tests described in the paper Tenmex's delta type strain gauge rosettes were used. They were arranged in specific locations on the surface of the samples. Data acquisition preceded using HBM measurement equipment, which included measuring amplifier and measuring head. Data acquisition was performed using the Easy Catman. In order to verify the results of laboratory tests numerical studies were carried out in a computing environment, Siemens PLM NX 9.0. For this purpose, samples were modeled composite corresponding to real samples. Tests were made for boundary conditions compatible with the laboratory tests boundary conditions.

Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

PubMed

O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

2014-08-19

Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

PubMed Central

Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

2010-01-01

The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

Heteroatom-enriched and renewable banana-stem-derived porous carbon for the electrochemical determination of nitrite in various water samples

PubMed Central

Madhu, Rajesh; Veeramani, Vediyappan; Chen, Shen-Ming

2014-01-01

For the first time, high-surface-area (approximately 1465 m2 g−1), highly porous and heteroatom-enriched activated carbon (HAC) was prepared from banana stems (Musa paradisiaca, Family: Musaceae) at different carbonization temperatures of 700, 800 and 900°C (HAC) using a simple and eco-friendly method. The amounts of carbon, hydrogen, nitrogen and sulfur in the HAC are 61.12, 2.567, 0.4315, and 0.349%, respectively. Using X-ray diffraction (XRD), CHNS elemental analysis, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy, the prepared activated carbon appears amorphous and disordered in nature. Here, we used HAC for an electrochemical application of nitrite (NO2−) sensor to control the environmental pollution. In addition, HAC exhibits noteworthy performance for the highly sensitive determination of nitrite. The limit of detection (LODs) of the nitrite sensor at HAC-modified GCE is 0.07 μM. In addition, the proposed method was applied to determine nitrite in various water samples with acceptable results. PMID:24755990

Climatically driven loss of calcium in steppe soil as a sink for atmospheric carbon

USGS Publications Warehouse

Lapenis, A.G.; Lawrence, G.B.; Bailey, S.W.; Aparin, B.F.; Shiklomanov, A.I.; Speranskaya, N.A.; Torn, M.S.; Calef, M.

2008-01-01

During the last several thousand years the semi-arid, cold climate of the Russian steppe formed highly fertile soils rich in organic carbon and calcium (classified as Chernozems in the Russian system). Analysis of archived soil samples collected in Kemannaya Steppe Preserve in 1920, 1947, 1970, and fresh samples collected in 1998 indicated that the native steppe Chernozems, however, lost 17-28 kg m-2 of calcium in the form of carbonates in 1970-1998. Here we demonstrate that the loss of calcium was caused by fundamental shift in the steppe hydrologic balance. Previously unleached soils where precipitation was less than potential evapotranspiration are now being leached due to increased precipitation and, possibly, due to decreased actual evapotranspiration. Because this region receives low levels of acidic deposition, the dissolution of carbonates involves the consumption of atmospheric CO2. Our estimates indicate that this climatically driven terrestrial sink of atmospheric CO2 is ???2.1-7.4 g C m-2 a-1. In addition to the net sink of atmospheric carbon, leaching of pedogenic carbonates significantly amplified seasonal amplitude of CO2 exchange between atmosphere and steppe soil. Copyright 2008 by the American Geophysical Union.

Estimates of residence time and related variations in quality of ground water beneath Submarine Base Bangor and vicinity, Kitsap County, Washington

USGS Publications Warehouse

Cox, S.E.

2003-01-01

Estimates of residence time of ground water beneath Submarine Base Bangor and vicinity ranged from less than 50 to 4,550 years before present, based on analysis of the environmental tracers tritium, chlorofluorocarbons (CFCs), and carbon-14 (14C), in 33 ground-water samples collected from wells tapping the ground-water system. The concentrations of multiple environmental tracers tritium, CFCs, and 14C were used to classify ground water as modern (recharged after 1953), pre-modern (recharged prior to 1953), or indeterminate. Estimates of the residence time of pre-modern ground water were based on evaluation of 14C of dissolved inorganic carbon present in ground water using geochemical mass-transfer modeling to account for the interactions of the carbon in ground water with carbon of the aquifer sediments. Ground-water samples were obtained from two extensive aquifers and from permeable interbeds within the thick confining unit separating the sampled aquifers. Estimates of ground-water residence time for all ground-water samples from the shallow aquifer were less than 45 years and were classified as modern. Estimates of the residence time of ground water in the permeable interbeds within the confining unit ranged from modern to 4,200 years and varied spatially. Near the recharge area, residence times in the permeable interbeds typically were less than 800 years, whereas near the discharge area residence times were in excess of several thousand years. In the deeper aquifers, estimates of ground-water residence times typically were several thousand years but ranged from modern to 4,550 years. These estimates of ground-water residence time based on 14C were often larger than estimates of ground-water residence time developed by particle-tracking analysis using a ground-water flow model. There were large uncertainties?on the order of 1,000-2,000 years?in the estimates based on 14C. Modern ground-water tracers found in some samples from large-capacity production wells screened in the deeper aquifer may be the result of preferential ground-water pathways or induced downward flow caused by pumping stress. Spatial variations in water quality were used to develop a conceptual model of chemical evolution of ground water. Stable isotope ratios of deuterium and oxygen-18 in the 33 ground-water samples were similar, indicating similar climatic conditions and source of precipitation recharge for all of the sampled ground water. Oxidation of organic matter and mineral dissolution increased the concentrations of dissolved inorganic carbon and common ions in downgradient ground waters. However, the largest concentrations were not found near areas of ground-water discharge, but at intermediate locations where organic carbon concentrations were greatest. Dissolved methane, derived from microbial methanogenesis, was present in some ground waters. Methanogenesis resulted in substantial alteration of the carbon isotopic composition of ground water. The NETPATH geochemical model code was used to model mass-transfers of carbon affecting the 14C estimate of ground-water residence time. Carbon sources in ground water include dispersed particulate organic matter present in the confining unit separating the two aquifers and methane present in some ground water. Carbonate minerals were not observed in the lithologic material of the ground-water system but may be present, because they have been found in the bedrock of stream drainages that contribute sediment to the study area.

A Multiscale Approach to Modeling Carbon and Nitrogen Cycling within a High Elevation Watershed

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

Lawrence, Corey

This funding represents a small sub-award related the larger project titled: A Multiscale Approach to Modeling Carbon and Nitrogen Cycling within a High Elevation Watershed. The goal of the sub-award was to facilitate the characterization of carbon and radiocarbon data collected from the East River watershed outside Gothic, Colorado USA. During the period of funding from 8/1/15 until 7/31/17, we sampled 40 soil profiles and collected ~325 soil samples. This funding supported the collection, processing, and elemental analysis of each of these samples. In addition, the funding allowed for the further density separation of a subset of soil resulting inmore » 60 measurements of 13C and 14C of bulk soil and density separates. Funding also supported installation of temperature and moisture data sensors arrays, soil gas wells, and soil water lysimeters. From this infrastructure, a steady stream data including soil gas, water, and physical information have been generated to support the larger research project.« less

δ13C Analysis of Dissolved Organic Carbon in Eastern Canadian Coastal Waters

NASA Astrophysics Data System (ADS)

Gelinas, Y.; Barber, A.

2016-12-01

The application of carbon stable isotope analysis on dissolved organic carbon (δ13C-DOC) from natural seawater samples has been limited owing to the difficulty of such analysis, with order of magnitude differences between interfering ions and analyte concentrations. High temperature catalytic oxidation allows for the separation of interferences from the organic carbon by precipitation on quartz chips upstream from the oxidation catalyst. Unlike wet chemical oxidation, where salts inhibit the oxidation of organic matter to CO2 via side reactions between the salt anions and the persulfate oxidizing agent, high temperature combustion ensures complete organic matter oxidation in a stream of O2. Using a programmable chemical trap to switch carrier gasses from O2 to He, the OI 1030C combustion unit can be coupled to and IRMS, allowing for the analysis of low DOC content saline waters with relatively high throughput. The analytical limitations and large water volumes traditionally required for these types of analyses have prevented any large-scale δ13C-DOC studies. Here we present DOC concentrations and δ13C-DOC signatures for surface and bottom waters obtained along Canada's East Coast. Included in the study are samples from the Esquiman channel (between Newfoundland and Labrador), Lake Melville, the Saglek and Nachvak Fjords, the Hudson Strait and finally covering the salinity gradient across the Gulf of the St. Lawrence, the St. Lawrence Estuary and the Saguenay Fjord. Measured δ13C-DOC signatures ranged from predominantly marine values of -21.3 ± 0.6 ‰ (vs. VPDB) off the coast of Newfoundland to predominantly terrestrial signatures of -25.8 ± 0.1‰ in Lake Melville. Overall, proper blank subtraction using the isotope mass balance equation and four replicate injections are crucial for the collection of meaningful high quality δ13C-DOC signatures on natural abundance, seawater samples.

Sampling and analytical methods of stable isotopes and dissolved inorganic carbon from CO2 injection sites

NASA Astrophysics Data System (ADS)

van Geldern, Robert; Myrttinen, Anssi; Becker, Veith; Barth, Johannes A. C.

2010-05-01

The isotopic composition (δ13C) of dissolved inorganic carbon (DIC), in combination with DIC concentration measurements, can be used to quantify geochemical trapping of CO2 in water. This is of great importance in monitoring the fate of CO2 in the subsurface in CO2 injection projects. When CO2 mixes with water, a shift in the δ13C values, as well as an increase in DIC concentrations is observed in the CO2-H2O system. However, when using standard on-site titration methods, it is often challenging to determining accurate in-situ DIC concentrations. This may be due to CO2 degassing and CO2-exchange between the sample and the atmosphere during titration, causing a change in the pH value or due to other unfavourable conditions such as turbid water samples or limited availability of fluid samples. A way to resolve this problem is by simultaneously determining the DIC concentration and carbon isotopic composition using a standard continuous flow Isotope Ratio Mass Spectrometry (CF-IRMS) setup with a Gasbench II coupled to Delta plusXP mass spectrometer. During sampling, in order to avoid atmospheric contact, water samples taken from the borehole-fluid-sampler should be directly transferred into a suitable container, such as a gasbag. Also, to avoid isotope fractionation due to biological activity in the sample, it is recommended to stabilize the gasbags prior to sampling with HgCl2 for the subsequent stable isotope analysis. The DIC concentration of the samples can be determined from the area of the sample peaks in a chromatogram from a CF-IRMS analysis, since it is directly proportional to the CO2 generated by the reaction of the water with H3PO4. A set of standards with known DIC concentrations should be prepared by mixing NaHCO3 with DIC free water. Since the DIC concentrations of samples taken from CO2 injection sites are expected to be exceptionally high due to the additional high amounts of added CO2, the DIC concentration range of the standards should be set high enough to cover the sample concentrations. In order to assure methodological reproducibility, this 'calibration set' should be included in every sequence analysed with the Gasbench CF-IRMS system. The standards, therefore, should also be treated in the same way as the samples. For accurate determination, it is essential to know the exact amount of water in the vial and the density of the sample. This requires weighing of each vial before and after injection of the water sample. For stable isotope analysis, the required signal height can be adjusted by the sample amount. Therefore this method is suitable for analysing samples with highly differing DIC concentrations. Reproducibility and accuracy of the quantitative analysis of the dissolved inorganic carbon need to be verified by independent control standards, treated as samples. This study was conducted as a part of the R&D programme CLEAN, which is funded by the German Federal Ministry of Education in the framework of the programme GEOTECHNOLOGIEN. We would like to thank GDF SUEZ for permitting us to conduct sampling campaigns at their site.

Sintering time optimization on red photoluminescence properties of manganese-doped boron carbon oxynitride (BCNO:Mn) phosphor

NASA Astrophysics Data System (ADS)

Wahid Nuryadin, Bebeh; Suryani, Yayu; Yuliani, Yuli; Setiadji, Soni; Yeti Nuryantini, Ade; Iskandar, Ferry

2018-04-01

The effect of sintering time to the transient nature and optimization of red photoluminescence manganese-doped boron carbon oxynitride (BCNO:Mn) phosphor was investigated. The BCNO:Mn samples were synthesized using a facile urea-assisted combustion route involving boric acid, citric acid, manganese salt and urea. The optimized intensity of the dual peak emission at 420 nm (blue emission) and 630 nm (red emission) in the photoluminescence (PL) spectrum could be achieved by controlling the sintering time of the BCNO:Mn. The BCNO:Mn samples in high-crystalline form was found to be in a cubic and hexagonal structure. Based on the PL analysis, it is suggested that the BCNO:Mn symmetric band at 630 nm can be attributed to the 4T1(4G)—6A1(6S) transition absorption of Mn2+ ions into the hexagonal structure. Microstructure analysis showed an irregular and agglomerated shape of the BCNO:Mn sample.

Balloon-Borne Full-Column Greenhouse Gas Profiling Field Campaign Report

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

Fischer, Marc L

The vertical distributions of CO2, CH4, and other gases provide important constraints for the determination of terrestrial and ocean sources and sinks of carbon and other biogeochemical processes in the Earth system. The DOE Biological and Environmental Research Program (DOE-BER) and the NOAA Earth System Research Laboratory (NOAA-ESRL) collaborate to quantify the vertically resolved distribution of atmospheric carbon-cycle gases (CO2, and CH4) within approximately 99% of the atmospheric column at the DOE ARM Southern Great Plains Facility in Oklahoma. In 2015, flights were delayed while research at NOAA focused on evaluating sources of systematic errors in the gas collection andmore » analysis system and modifying the sampling system to provide duplicate air samples in a single flight package. In 2017, we look forward to proposing additional sampling and analysis at ARM-SGP (and other sites) that characterize the vertical distribution of CO2 and CH4 over time and space.« less

Effect of nitrogen plasma afterglow on the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films

NASA Astrophysics Data System (ADS)

Kayed, Kamal

2018-06-01

The aim of this paper is to investigate the relationship between the micro structure and the surface charge effect resulted during XPS surface analysis of amorphous carbon nitride thin films prepared by laser ablation method. The study results show that the charge effect coefficient (E) is not just a correction factor. We found that the changes in this coefficient value due to incorporation of nitrogen atoms into the carbon network are related to the spatial configurations of the sp2 bonded carbon atoms, order degree and sp2 clusters size. In addition, results show that the curve E vs. C(sp3)-N is a characteristic curve of the micro structure. This means that using this curve makes it easy to sorting the samples according to the micro structure (hexagonal rings or chains).

Coaxial carbon plasma gun deposition of amorphous carbon films

NASA Technical Reports Server (NTRS)

Sater, D. M.; Gulino, D. A.; Rutledge, S. K.

1984-01-01

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Dietary practices in ancient populations from northern Chile during the transition to agriculture (Tarapacá region, 1000 BC-AD 900).

PubMed

Santana-Sagredo, Francisca; Uribe, Mauricio; Herrera, María José; Retamal, Rodrigo; Flores, Sergio

2015-12-01

The goal of this research is to understand the relevance of diet diversity during the transition to agriculture, in ancient populations from northern Chile, especially considering the significance of marine resources and crops in a lesser degree. A total of 14 human individuals were sampled from the Tarapacá 40 cemetery. Both bone and tooth samples were collected. Samples were studied from bone/dentine collagen for carbon and nitrogen isotopic analysis; and bone/enamel apatite for carbon isotope analysis. Inferential statistical analyses were performed in order to compare Tarapacá 40 stable carbon and nitrogen isotope values with other Formative and Late Intermediate Period groups. A nonparametrical hypothesis Kruskal-Wallis test was used. The results show that the individuals from Tarapacá 40 are intermediate to the values observed for terrestrial and marine fauna as well as C3 and C4 plants. A gradual transition to crop consumption, especially maize, is suggested. This complemented the earlier hunter-gatherer tradition of marine resources and wild fruit consumption. Contrarily to the predictions made by some archaeologists, the results obtained for northern Chile contrast with the classical perspective of a "Neolithic Revolution" in which transition to agriculture occurred more abruptly and linearly. © 2015 Wiley Periodicals, Inc.

Inaccurate reporting of mineral composition by commercial stone analysis laboratories: implications for infection and metabolic stones.

PubMed

Krambeck, Amy E; Khan, Naseem F; Jackson, Molly E; Lingeman, James E; McAteer, James A; Williams, James C

2010-10-01

We determined the accuracy of stone composition analysis at commercial laboratories. A total of 25 human renal stones with infrared spectroscopy determined composition were fragmented into aliquots and studied with micro computerized tomography to ensure fragment similarity. Representative fragments of each stone were submitted to 5 commercial stone laboratories for blinded analysis. All laboratories agreed on the composition of 6 pure stones. Only 2 of 4 stones (50%) known to contain struvite were identified as struvite at all laboratories. Struvite was reported as a component by some laboratories for 4 stones previously determined not to contain struvite. Overall there was disagreement regarding struvite in 6 stones (24%). For 9 calcium oxalate stones all laboratories reported some mixture of calcium oxalate but the quantity of subtypes differed significantly among laboratories. In 6 apatite containing stones apatite was missed by the laboratories in 20% of samples. None of the laboratories identified atazanavir in a stone containing that antiviral drug. One laboratory reported protein in every sample while all others reported it in only 1. Nomenclature for apatite differed among laboratories with 1 reporting apatite as carbonate apatite and never hydroxyapatite, another never reporting carbonate apatite and always reporting hydroxyapatite, and a third reporting carbonate apatite as apatite with calcium carbonate. Commercial laboratories reliably recognize pure calculi. However, variability in the reporting of mixed calculi suggests a problem with the accuracy of stone analysis results. There is also a lack of standard nomenclature used by laboratories. Copyright © 2010 American Urological Association Education and Research, Inc. Published by Elsevier Inc. All rights reserved.

Thermal/Optical Methods for Elemental Carbon Quantification in Soils and Urban Dusts: Equivalence of Different Analysis Protocols

PubMed Central

Han, Yongming; Chen, Antony; Cao, Junji; Fung, Kochy; Ho, Fai; Yan, Beizhan; Zhan, Changlin; Liu, Suixin; Wei, Chong; An, Zhisheng

2013-01-01

Quantifying elemental carbon (EC) content in geological samples is challenging due to interferences of crustal, salt, and organic material. Thermal/optical analysis, combined with acid pretreatment, represents a feasible approach. However, the consistency of various thermal/optical analysis protocols for this type of samples has never been examined. In this study, urban street dust and soil samples from Baoji, China were pretreated with acids and analyzed with four thermal/optical protocols to investigate how analytical conditions and optical correction affect EC measurement. The EC values measured with reflectance correction (ECR) were found always higher and less sensitive to temperature program than the EC values measured with transmittance correction (ECT). A high-temperature method with extended heating times (STN120) showed the highest ECT/ECR ratio (0.86) while a low-temperature protocol (IMPROVE-550), with heating time adjusted for sample loading, showed the lowest (0.53). STN ECT was higher than IMPROVE ECT, in contrast to results from aerosol samples. A higher peak inert-mode temperature and extended heating times can elevate ECT/ECR ratios for pretreated geological samples by promoting pyrolyzed organic carbon (PyOC) removal over EC under trace levels of oxygen. Considering that PyOC within filter increases ECR while decreases ECT from the actual EC levels, simultaneous ECR and ECT measurements would constrain the range of EC loading and provide information on method performance. Further testing with standard reference materials of common environmental matrices supports the findings. Char and soot fractions of EC can be further separated using the IMPROVE protocol. The char/soot ratio was lower in street dusts (2.2 on average) than in soils (5.2 on average), most likely reflecting motor vehicle emissions. The soot concentrations agreed with EC from CTO-375, a pure thermal method. PMID:24358286

Diet of spotted bats (Euderma maculatum) in Arizona as indicated by fecal analysis and stable isotopes

EPA Science Inventory

We assessed diet of spotted bats (Euderma maculatum (J.A. Allen, 1891)) by visual analysis of bat feces and stable carbon (δ13C) and nitrogen (δ15N) isotope analysis of bat feces, wing, hair, and insect prey. We collected 33 fecal samples from spotted bats and trapped 3755 insect...

Materials and Methods for Streamlined Laboratory Analysis of Environmental Samples, FY 2016 Report

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

Addleman, Raymond S.; Naes, Benjamin E.; McNamara, Bruce K.

The International Atomic Energy Agency (IAEA) relies upon laboratory analysis of environmental samples (typically referred to as “swipes”) collected during on-site inspections of safeguarded facilities to support the detection and deterrence of undeclared activities. Unfortunately, chemical processing and assay of the samples is slow and expensive. A rapid, effective, and simple extraction process and analysis method is needed to provide certified results with improved timeliness at reduced costs (principally in the form of reduced labor), while maintaining or improving sensitivity and efficacy. To address these safeguard needs the Pacific Northwest National Laboratory (PNNL) explored and demonstrated improved methods for environmentalmore » sample (ES) analysis. Improvements for both bulk and particle analysis were explored. To facilitate continuity and adoption, the new sampling materials and processing methods will be compatible with existing IAEA protocols for ES analysis. PNNL collaborated with Oak Ridge National Laboratory (ORNL), which performed independent validation of the new bulk analysis methods and compared performance to traditional IAEA’s Network of Analytical Laboratories (NWAL) protocol. ORNL efforts are reported separately. This report describes PNNL’s FY 2016 progress, which was focused on analytical application supporting environmental monitoring of uranium enrichment plants and nuclear fuel processing. In the future the technology could be applied to other safeguard applications and analytes related to fuel manufacturing, reprocessing, etc. PNNL’s FY 2016 efforts were broken into two tasks and a summary of progress, accomplishments and highlights are provided below. Principal progress and accomplishments on Task 1, Optimize Materials and Methods for ICP-MS Environmental Sample Analysis, are listed below. • Completed initial procedure for rapid uranium extraction from ES swipes based upon carbonate-peroxide chemistry (delivered to ORNL for evaluation). • Explored improvements to carbonate-peroxide rapid uranium extraction chemistry. • Evaluated new sampling materials and methods (in collaboration with ORNL). • Demonstrated successful ES extractions from standard and novel swipes for a wide range uranium compounds of interest including UO 2F 2 and UO 2(NO 3) 2, U 3O 8 and uranium ore concentrate. • Completed initial discussions with commercial suppliers of PTFE swipe materials. • Submitted one manuscript for publication. Two additional drafts are being prepared. Principal progress and accomplishments on Task 2, Optimize Materials and Methods for Direct SIMS Environmental Sample Analysis, are listed below. • Designed a SIMS swipe sample holder that retrofits into existing equipment and provides simple, effective, and rapid mounting of ES samples for direct assay while enabling automation and laboratory integration. • Identified preferred conductive sampling materials with better performance characteristics. • Ran samples on the new PNNL NWAL equivalent Cameca 1280 SIMS system. • Obtained excellent agreement between isotopic ratios for certified materials and direct SIMS assay of very low levels of LEU and HEU UO 2F 2 particles on carbon fiber sampling material. Sample activities range from 1 to 500 CPM (uranium mass on sample is dependent upon specific isotope ratio but is frequently in the subnanogram range). • Found that the presence of the UF molecular ions, as measured by SIMS, provides chemical information about the particle that is separate from the uranium isotopics and strongly suggests that those particles originated from an UF6 enrichment activity. • Submitted one manuscript for publication. Another manuscript is in preparation.« less

Environmental Remediation and Conversion of Carbon Dioxide (CO2) into Useful Green Products by Accelerated Carbonation Technology

PubMed Central

Lim, Mihee; Han, Gi-Chun; Ahn, Ji-Whan; You, Kwang-Suk

2010-01-01

This paper reviews the application of carbonation technology to the environmental industry as a way of reducing carbon dioxide (CO2), a green house gas, including the presentation of related projects of our research group. An alternative technology to very slow natural carbonation is the co-called ‘accelerated carbonation’, which completes its fast reaction within few hours by using pure CO2. Carbonation technology is widely applied to solidify or stabilize solid combustion residues from municipal solid wastes, paper mill wastes, etc. and contaminated soils, and to manufacture precipitated calcium carbonate (PCC). Carbonated products can be utilized as aggregates in the concrete industry and as alkaline fillers in the paper (or recycled paper) making industry. The quantity of captured CO2 in carbonated products can be evaluated by measuring mass loss of heated samples by thermo-gravimetric (TG) analysis. The industrial carbonation technology could contribute to both reduction of CO2 emissions and environmental remediation. PMID:20195442

Preparation and surface characterization of activated carbons from Euphorbia rigida by chemical activation with ZnCl2, K2CO3, NaOH and H3PO4

NASA Astrophysics Data System (ADS)

Kılıç, Murat; Apaydın-Varol, Esin; Pütün, Ayşe Eren

2012-11-01

Preparation of activated carbons from Euphorbia rigida by chemical activation with different impregnation agents and ratios was studied. ZnCl2, K2CO3, NaOH and H3PO4 were used as chemical activation agents and four impregnation ratios (25-50-75-100%) by mass were applied on biomass. Activation is applied to impregnated biomass samples at 700 °C under sweeping gas in a fixed bed reactor. For determination of chemical and physical properties of the obtained activated carbons; elemental analysis was applied to determine the elemental composition (C, H, N, O) and FT-IR spectra was used to analyze the functional groups. BET equation was used to calculate the surface areas of activated carbons. For understanding the changes in the surface structure, activated carbons were conducted to Scanning Electron Microscopy (SEM). Maximum BET surface area (2613 m2/g) was reached with 75% K2CO3 impregnated biomass sample. Experimental results showed that impregnation types and ratios have a significant effect on the pore structure of activated carbon and E. rigida seems to be an alternative precursor for commercial activated carbon production.

Yucca Mountain Area Saturated Zone Dissolved Organic Carbon Isotopic Data

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

Thomas, James; Decker, David; Patterson, Gary

2007-06-25

Groundwater samples in the Yucca Mountain area were collected for chemical and isotopic analyses and measurements of water temperature, pH, specific conductivity, and alkalinity were obtained at the well or spring at the time of sampling. For this project, groundwater samples were analyzed for major-ion chemistry, deuterium, oxygen-18, and carbon isotopes of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC). The U.S. Geological Survey (USGS) performed all the fieldwork on this project including measurement of water chemistry field parameters and sample collection. The major ions dissolved in the groundwater, deuterium, oxygen-18, and carbon isotopes of dissolved inorganic carbon (DIC)more » were analyzed by the USGS. All preparation and processing of samples for DOC carbon isotopic analyses and geochemical modeling were performed by the Desert Research Institute (DRI). Analysis of the DOC carbon dioxide gas produced at DRI to obtain carbon-13 and carbon-14 values was conducted at the University of Arizona Accelerator Facility (a NSHE Yucca Mountain project QA qualified contract facility). The major-ion chemistry, deuterium, oxygen-18, and carbon isotopes of DIC were used in geochemical modeling (NETPATH) to determine groundwater sources, flow paths, mixing, and ages. The carbon isotopes of DOC were used to calculate groundwater ages that are independent of DIC model corrected carbon-14 ages. The DIC model corrected carbon-14 calculated ages were used to evaluate groundwater travel times for mixtures of water including water beneath Yucca Mountain. When possible, groundwater travel times were calculated for groundwater flow from beneath Yucca Mountain to down gradient sample sites. DOC carbon-14 groundwater ages were also calculated for groundwaters in the Yucca Mountain area. When possible, groundwater travel times were estimated for groundwater flow from beneath Yucca Mountain to down gradient groundwater sample sites using the DOC calculated groundwater ages. The DIC calculated groundwater ages were compared with DOC calculated groundwater ages and both of these ages were compared to travel times developed in ground-water flow and transport models. If nuclear waste is stored in Yucca Mountain, the saturated zone is the final barrier against the release of radionuclides to the environment. The most recent rendition of the TSPA takes little credit for the presence of the saturated zone and is a testament to the inadequate understanding of this important barrier. If radionuclides reach the saturated zone beneath Yucca Mountain, then there is a travel time before they would leave the Yucca Mountain area and flow down gradient to the Amargosa Valley area. Knowing how long it takes groundwater in the saturated zone to flow from beneath Yucca Mountain to down gradient areas is critical information for potential radionuclide transport. Radionuclide transport in groundwater may be the quickest pathway for radionuclides in the proposed Yucca Mountain repository to reach land surface by way of groundwater pumped in Amargosa Valley. An alternative approach to ground-water flow and transport models to determine the travel time of radionuclides from beneath Yucca Mountain to down gradient areas in the saturated zone is by carbon-14 dating of both inorganic and organic carbon dissolved in the groundwater. A standard method of determining ground-water ages is to measure the carbon-13 and carbon-14 of DIC in the groundwater and then correct the measured carbon-14 along a flow path for geochemical reactions that involve carbon containing phases. These geochemical reactions are constrained by carbon-13 and isotopic fractionations. Without correcting for geochemical reactions, the ground-water ages calculated from only the differences in carbon-14 measured along a flow path (assuming the decrease in carbon-14 is due strictly to radioactive decay) could be tens of thousands of years too old. The computer program NETPATH, developed by the USGS, is the best geochemical program for correcting carbon-14 activities for geochemical reactions. The DIC carbon-14 corrected ages can be further constrained by measuring the carbon isotopes of DOC. Because the only source of organic carbon in aquifers is almost always greater than 40,000 years old, any organic carbon that may be added to the groundwater would contain no carbon-14. Thus, ground-water ages determined by carbon isotopes of DOC should be maximum ages that can be used to constrain DIC corrected ages.« less

Biocompatible nanocrystalline natural bonelike carbonated hydroxyapatite synthesized by mechanical alloying in a record minimum time.

PubMed

Lala, S; Brahmachari, S; Das, P K; Das, D; Kar, T; Pradhan, S K

2014-09-01

Single phase nanocrystalline biocompatible A-type carbonated hydroxyapatite (A-cHAp) powder has been synthesized by mechanical alloying the stoichiometric mixture of CaCO3 and CaHPO4.2H2O powders in open air at room temperature within 2h of milling. The A-type carbonation in HAp is confirmed by FTIR analysis. Structural and microstructure parameters of as-milled powders are obtained from both Rietveld's powder structure refinement analysis and transmission electron microscopy. Size and lattice strain of nanocrystalline HAp particles are found to be anisotropic in nature. Mechanical alloying causes amorphization of a part of crystalline A-cHAp which is analogous to native bone mineral. Some primary bond lengths of as-milled samples are critically measured. MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assay test reveals high percentage of cell viability and hence confirms the biocompatibility of the sample. The overall results indicate that the processed A-cHAp has a chemical composition very close to that of biological apatite. Copyright © 2014 Elsevier B.V. All rights reserved.

Fatty Acid Detection in Mars-Analogous Rock Samples with the TMAH Wet Chemistry Experiment on the Sample Analysis at Mars (SAM) Instrument

NASA Astrophysics Data System (ADS)

Williams, A. J.; Eigenbrode, J. L.; Wilhelm, M. B.; Johnson, S. S.; Craft, K.; O'Reilly, S.; Lewis, J. M. T.; Williams, R.; Summons, R. E.; Benison, K. C.; Mahaffy, P. R.

2017-12-01

The Curiosity rover is exploring sedimentary rock sequences in Gale Crater for evidence of habitability and searching for organic compounds using the Sample Analysis at Mars (SAM) instrument suite. SAM includes a gas chromatograph mass spectrometer (GC-MS) and pyrolysis ovens. SAM has the ability to perform wet chemistry experiments, one of which uses tetramethylammonium hydroxide (TMAH) thermochemolysis to liberate bound lipids, making them sufficiently volatile for detection by GC-MS. To determine the effectiveness of the SAM-like TMAH experiment on fatty acid methyl ester (FAME) biomarker identification, rock and sediment samples were collected from a variety of Mars analog environments including iron oxides from a modern mineral precipitate and older surface gossan at Iron Mountain, CA, as well as modern acid salt and neutral lake sediments with mixed iron oxides and clays from Western Australia; siliceous sinter from recently inactive and modern near-vent Icelandic hot springs deposits; modern carbonate ooids from The Bahamas, and organic-rich shale from Germany. Samples underwent pyrolysis with TMAH. Fatty acids were analyzed by pyro-GC-MS using a SAM-like heating ramp (35°C/min) as well as a 500°C flash on a Frontier pyrolyzer and Agilent GC-MS instrument. Results reveal that FAMEs were detectable with the TMAH experiment in nearly all samples. Low molecular weight (MW) C6:0-C10:0 FAMEs were present in all samples, medium MW C11:0-C18:2 FAMEs were present in select samples, and high MW (HMW) C20:0-C30:0 FAMEs were present in the shale sample. Many of these samples exhibited an even-over-odd carbon number preference, indicating biological production. These experiments demonstrate that TMAH thermochemolysis with SAM-like pyro-GC-MS is effective in fatty acid analysis from natural Mars-analog samples that vary in mineralogy, age, and microbial community input. HMW FAMEs are not detected in iron-dominated samples, and may not be detectable at low concentrations. Although mineralogies such as sinter, carbonates, and shales are not likely in Gale Crater, iron oxides mixed with clays are known to be present in the path of the Curiosity rover. Environments with these mineralogies may provide the optimal opportunity to detect fatty acids, if present in Gale Crater.

Characterization of mechanical properties of hydroxyapatite-silicon-multi walled carbon nano tubes composite coatings synthesized by EPD on NiTi alloys for biomedical application.

PubMed

Khalili, Vida; Khalil-Allafi, Jafar; Sengstock, Christina; Motemani, Yahya; Paulsen, Alexander; Frenzel, Jan; Eggeler, Gunther; Köller, Manfred

2016-06-01

Release of Ni(1+) ions from NiTi alloy into tissue environment, biological response on the surface of NiTi and the allergic reaction of atopic people towards Ni are challengeable issues for biomedical application. In this study, composite coatings of hydroxyapatite-silicon multi walled carbon nano-tubes with 20wt% Silicon and 1wt% multi walled carbon nano-tubes of HA were deposited on a NiTi substrate using electrophoretic methods. The SEM images of coated samples exhibit a continuous and compact morphology for hydroxyapatite-silicon and hydroxyapatite-silicon-multi walled carbon nano-tubes coatings. Nano-indentation analysis on different locations of coatings represents the highest elastic modulus (45.8GPa) for HA-Si-MWCNTs which is between the elastic modulus of NiTi substrate (66.5GPa) and bone tissue (≈30GPa). This results in decrease of stress gradient on coating-substrate-bone interfaces during performance. The results of nano-scratch analysis show the highest critical distance of delamination (2.5mm) and normal load before failure (837mN) as well as highest critical contact pressure for hydroxyapatite-silicon-multi walled carbon nano-tubes coating. The cell culture results show that human mesenchymal stem cells are able to adhere and proliferate on the pure hydroxyapatite and composite coatings. The presence of both silicon and multi walled carbon nano-tubes (CS3) in the hydroxyapatite coating induce more adherence of viable human mesenchymal stem cells in contrast to the HA coated samples with only silicon (CS2). These results make hydroxyapatite-silicon-multi walled carbon nano-tubes a promising composite coating for future bone implant application. Copyright © 2016 Elsevier Ltd. All rights reserved.

Methods and equations for estimating aboveground volume, biomass, and carbon for trees in the U.S. forest inventory, 2010

Treesearch

Christopher W. Woodall; Linda S. Heath; Grant M. Domke; Michael C. Nichols

2011-01-01

The U.S. Forest Service, Forest Inventory and Analysis (FIA) program uses numerous models and associated coefficients to estimate aboveground volume, biomass, and carbon for live and standing dead trees for most tree species in forests of the United States. The tree attribute models are coupled with FIA's national inventory of sampled trees to produce estimates of...

Changes in Dissolved Organic Matter Composition and Disinfection Byproduct Precursors in Advanced Drinking Water Treatment Processes.

PubMed

Phungsai, Phanwatt; Kurisu, Futoshi; Kasuga, Ikuro; Furumai, Hiroaki

2018-03-20

Molecular changes in dissolved organic matter (DOM) from treatment processes at two drinking water treatment plants in Japan were investigated using unknown screening analysis by Orbitrap mass spectrometry. DOM formulas with carbon, hydrogen and oxygen (CHO-DOM) were the most abundant class in water samples, and over half of them were commonly found at both plants. Among the treatment processes, ozonation induced the most drastic changes to DOM. Mass peak intensities of less saturated CHO-DOM (positive (oxygen subtracted double bond equivalent per carbon (DBE-O)/C)) decreased by ozonation, while more saturated oxidation byproducts (negative (DBE-O)/C) increased and new oxidation byproducts (OBPs) were detected. By Kendrick mass analysis, ozone reactions preferred less saturated CHO-DOM in the same alkylation families and produced more saturated alkylation families of OBPs. Following ozonation, biological activated carbon filtration effectively removed <300 Da CHO-DOM, including OBPs. Following chlorination, over 50 chlorinated formulas of disinfection byproducts (DBPs) were found in chlorinated water samples where at least half were unknown. Putative precursors of these DBPs were determined based on electrophilic substitutions and addition reactions. Ozonation demonstrated better decomposition of addition reaction-type precursors than electrophilic substitution-type precursors; over half of both precursor types decreased during biological activated carbon filtration.

Methods of analysis for complex organic aerosol mixtures from urban emission sources of particulate carbon

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

Mazurek, M.A.; Hildemann, L.M.; Cass, G.R.

1990-04-01

Extractable organic compounds having between 6 to 40 carbon atoms comprise an important mass fraction of the fine particulate matter samples from major urban emission sources. Depending on the emission source type, this solvent-soluble fraction accounts for <20% to 100% of the total organic aerosol mass, as measured by quantitative high-resolution has chromatography (HRGC) with flame ionization detection. In addition to total extract quantitation, HRGC can be applied to further analyses of the mass distributions of elutable organics present in the complex aerosol extract mixtures, thus generating profiles that serve as fingerprints'' for the sources of interest. This HRGC analyticalmore » method is applied to emission source samples that contain between 7 to 12,000 {mu}g/filter organic carbon. It is shown to be a sensitive technique for analysis of carbonaceous aerosol extract mixtures having diverse mass loadings and species distributions. This study describes the analytical chemical methods that have been applied to: the construction of chemical mass balances based on the mass of fine organic aerosol emitted for major urban sources of particulate carbon; and the generation of discrete emission source chemical profiles derived from chromatographic characteristics of the organic aerosol components. 21 refs., 1 fig., 2 tabs.« less

Stable carbon isotope ratio in atmospheric CO2 collected by new diffusive devices.

PubMed

Proto, Antonio; Cucciniello, Raffaele; Rossi, Federico; Motta, Oriana

2014-02-01

In this paper, stable carbon isotope ratios (δ (13)C) were determined in the atmosphere by using a Ca-based sorbent, CaO/Ca12Al14O33 75:25 w/w, for passively collecting atmospheric CO2, in both field and laboratory experiments. Field measurements were conducted in three environments characterized by different carbon dioxide sources. In particular, the environments under consideration were a rather heavily trafficked road, where the source of CO2 is mostly vehicle exhaust, a rural unpolluted area, and a private kitchen where the major source of CO2 was gas combustion. Samplers were exposed to the free atmosphere for 3 days in order to allow collection of sufficient CO2 for δ(13)C analysis, then the collected CO2 was desorbed from the adsorbent with acid treatment, and directly analyzed by nondispersive infrared (NDIR) instrument. δ (13)C results confirmed that the samplers collected representative CO2 samples and no fractionation occurred during passive trapping, as also confirmed by an appositely designed experiment conducted in the laboratory. Passive sampling using CaO/Ca12Al14O33 75:25 w/w proved to be an easy and reliable method to collect atmospheric carbon dioxide for δ (13)C analysis in both indoor and outdoor places.

Thermal degradation of hexachlorobenzene in the presence of calcium oxide at 340-400 °C.

PubMed

Yin, Keqing; Gao, Xingbao; Sun, Yifei; Zheng, Lei; Wang, Wei

2013-11-01

Hexachlorobenzene (HCB) in the milligram range was co-heated with calcium oxide (CaO) powder in sealed glass ampoules at 340-400 °C. The heated samples were characterized and analyzed by Raman spectroscopy, elemental analysis, gas chromatography/mass spectrometry, ion chromatography, and thermal/optical carbon analysis. The degradation products of HCB were studied at different temperatures and heated times. The amorphous carbon was firstly quantitatively evaluated and was thought to be important fate of the C element of HCB. The yield of amorphous carbon in products increased with heating time, for samples treated for 8h at 340, 380 °C and 400 °C, the value were 17.5%, 34.8% and 50.2%, respectively. After identification of the dechlorination products, the HCB degradation on CaO at 340-400 °C was supposed to through dechlorination/polymerization pathway, which is induced by electron transfer, generate chloride ions and form high-molecular weight intermediates with significant levels of both hydrogen and chlorine, and finally form amorphous carbon. Higher temperature was beneficial for the dechlorination/polymerization efficiency. The results are helpful for clarifying the reaction mechanism for thermal degradation of chlorinated aromatics in alkaline matrices. Copyright © 2013 Elsevier Ltd. All rights reserved.

Characteristics of dissolved organic matter in the Upper Klamath River, Lost River, and Klamath Straits Drain, Oregon and California

USGS Publications Warehouse

Goldman, Jami H.; Sullivan, Annett B.

2017-12-11

Concentrations of particulate organic carbon (POC) and dissolved organic carbon (DOC), which together comprise total organic carbon, were measured in this reconnaissance study at sampling sites in the Upper Klamath River, Lost River, and Klamath Straits Drain in 2013–16. Optical absorbance and fluorescence properties of dissolved organic matter (DOM), which contains DOC, also were analyzed. Parallel factor analysis was used to decompose the optical fluorescence data into five key components for all samples. Principal component analysis (PCA) was used to investigate differences in DOM source and processing among sites.At all sites in this study, average DOC concentrations were higher than average POC concentrations. The highest DOC concentrations were at sites in the Klamath Straits Drain and at Pump Plant D. Evaluation of optical properties indicated that Klamath Straits Drain DOM had a refractory, terrestrial source, likely extracted from the interaction of this water with wetland peats and irrigated soils. Pump Plant D DOM exhibited more labile characteristics, which could, for instance, indicate contributions from algal or microbial exudates. The samples from Klamath River also had more microbial or algal derived material, as indicated by PCA analysis of the optical properties. Most sites, except Pump Plant D, showed a linear relation between fluorescent dissolved organic matter (fDOM) and DOC concentration, indicating these measurements are highly correlated (R2=0.84), and thus a continuous fDOM probe could be used to estimate DOC loads from these sites.

Dissolved Organic Carbon Degradation in Response to Nutrient Amendments in Southwest Greenland Lakes

NASA Astrophysics Data System (ADS)

Burpee, B. T.; Northington, R.; Simon, K. S.; Saros, J. E.

2014-12-01

Aquatic ecosystems across the Arctic are currently experiencing rapid shifts in biotic, chemical, and physical factors in response to climate change. Preliminary data from multiple lakes in southwestern Greenland indicate decreasing dissolved organic carbon (DOC) concentrations over the past decade. Though several factors may be contributing to this phenomenon, this study attempts to elucidate the potential of heterotrophic bacteria to degrade DOC in the presence of increasing nutrient concentrations. In certain Arctic regions, nutrient subsidies have been released into lakes due to permafrost thaw. If this is occurring in southwestern Greenland, we hypothesized that increased nutrient concentrations will relieve nutrient limitation, thereby allowing heterotrophic bacteria to utilize DOC as an energy source. This prediction was tested using experimental DOC degradation assays from four sample lakes. Four nutrient amendment treatments (control, N, P, and N + P) were used to simulate in situ subsidies. Five time points were sampled during the incubation: days 0, 3, 6, 14, and 60. Total organic carbon (TOC) and parallel factor (PARAFAC) analysis were used to monitor the relative concentrations of different DOC fractions over time. In addition, samples for extracellular enzyme activity (EEA) analysis were collected at every time point. Early analysis of fulvic and humic pools of DOC do not indicate any significant change from days 0 to 14. This could be due to the fact that these DOC fractions are relatively recalcitrant. This study will be important in determining whether bacterial degradation could be a contributing factor to DOC decline in arctic lakes.

Energy expenditure in space flight (doubly labelled water method) (8-IML-1)

NASA Technical Reports Server (NTRS)

Parsons, Howard G.

1992-01-01

The objective of the Energy Expenditure in Space Flight (ESS) experiment is to demonstrate and evaluate the doubly labeled water method of measuring the energy expended by crew members during approximately 7 days in microgravity. The doubly labeled water technique determines carbon dioxide production which is then used to calculate energy expenditure. The method relies on the equilibrium between oxygen in respiratory carbon dioxide and oxygen in body water. Because of this equilibrium, the kinetic of water turnover and respiration are interdependent. Under normal conditions, man contains small but significant amounts of deuterium and oxygen 18. Deuterium is eliminated from the body as water while oxygen 18 is eliminated as water and carbon dioxide. The difference in the turnover rates in the two isotopes is proportional to the carbon dioxide production. Deliberately enriching the total body water with both of these isotopes allows the isotope turnovers to be accurately measured in urine, plasma, or saliva samples. The samples are taken to the laboratory for analysis using an ion-ratio spectrometer.

Decarboxylation of Carbon Compounds as a Potential Source for CO2 and CO Observed by SAM at Yellowknife Bay, Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Eigenbrode, J. L.; Bower, H.; Archer, P. Jr.

2014-01-01

Martian carbon was detected in the Sheepbed mudtsone at Yellowknife Bay, Gale Crater, Mars by the Sample Analysis at Mars (SAM) instrument onboard Curiosity, the rover of the Mars Science Laboratory missio]. The carbon was detected as CO2 thermally evolved from drilled and sieved rock powder that was delivered to SAM as a <150-micron-particle- size fraction. Most of the CO2 observed in the Cumberland (CB) drill hole evolved between 150deg and 350deg C. In the John Klein (JK) drill hole, the CO2 evolved up to 500deg C. Hypotheses for the source of the the CO2 include the breakdown of carbonate minerals reacting with HCl released from oxychlorine compounds, combustion of organic matter by O2 thermally evolved from the same oxychlorine minerals, and the decarboxylation of organic molecules indigenous to the martian rock sample. Here we explore the potential for the decarboxylation hypothesis.

Silver(I) Ions Ultrasensitive Detection at Carbon Electrodes—Analysis of Waters, Tobacco Cells and Fish Tissues

PubMed Central

Krizkova, Sona; Krystofova, Olga; Trnkova, Libuse; Hubalek, Jaromir; Adam, Vojtech; Beklova, Miroslava; Horna, Ales; Havel, Ladislav; Kizek, Rene

2009-01-01

We used carbon paste electrodes and a standard potentiostat to detect silver ions. The detection limit (3 Signal/Noise ratio) was estimated as 0.5 μM. A standard electrochemical instrument microanalysis of silver(I) ions was suggested. As a working electrode a carbon tip (1 mL) or carbon pencil was used. Limits of detection estimated by dilution of a standard were 1 (carbon tip) or 10 nM (carbon pencil). Further we employed flow injection analysis coupled with carbon tip to detect silver(I) ions released in various beverages and mineral waters. During first, second and third week the amount of silver(I) ions releasing into water samples was under the detection limit of the technique used for their quantification. At the end of a thirteen weeks long experiment the content of silver(I) ions was several times higher compared to the beginning of release detected in the third week and was on the order of tens of nanomoles. In subsequent experiments the influence of silver(I) ions (0, 5 and 10 μM) on a plant model system (tobacco BY-2 cells) during a four-day exposition was investigated. Silver(I) ions were highly toxic to the cells, which was revealed by a double staining viability assay. Moreover we investigated the effect of silver(I) ions (0, 0.3, 0.6, 1.2 and 2.5 μM) on guppies (Poecilia reticulata). Content of Ag(I) increased with increasing time of the treatment and applied concentrations in fish tissues. It can be concluded that a carbon tip or carbon pencil coupled with a miniaturized potentiostat can be used for detection of silver(I) ions in environmental samples and thus represents a small, portable, low cost and easy-to-use instrument for such purposes. PMID:22399980

Simulated In Situ Determination of Soil Profile Organic and Inorganic Carbon With LIBS and VisNIR

NASA Astrophysics Data System (ADS)

Bricklemyer, R. S.; Brown, D. J.; Clegg, S. M.; Barefield, J. E.

2008-12-01

There is growing need for rapid, accurate, and inexpensive methods to measure, and verify soil organic carbon (SOC) change for national greenhouse gas accounting and the development of a soil carbon trading market. Laser Induced Breakdown Spectroscopy (LIBS) and Visible and Near Infrared Spectroscopy (VisNIR) are complementary analytical techniques that have the potential to fill that need. The LIBS method provides precise elemental analysis of soils, but generally cannot distinguish between organic C and inorganic C. VisNIR has been established as a viable technique for measuring soil properties including SOC and inorganic carbon (IC). As part of the Big Sky Carbon Sequestration Regional Partnership, 240 intact core samples (3.8 x 50 cm) have been collected from six agricultural fields in north central Montana, USA. Each of these core samples were probed concurrently with LIBS and VisNIR at 2.5, 7.5, 12.5, 17.5, 22.5, 27.5, 35 and 45 cm (+/- 1.5 cm) depths. VisNIR measurements were taken using an Analytical Spectral Devices (ASD, Boulder, CO, USA) Agrispec spectrometer to determine the partition of SOC vs. IC in the samples. The LIBS scans were collected with the LANL LIBS Core Scanner Instrument which collected the entire 200 - 900 nm plasma emission including the 247.8 nm carbon emission line. This instrument also collected the emission from the elements typically found in inorganic carbon (Ca and Mg) and organic carbon (H, O, and N). Subsamples of soil (~ 4 g) were taken from interrogation points for laboratory determination of SOC and IC. Using this analytical data, we constructed several full spectrum multivariate VisNIR/LIBS calibration models for SOC and IC. These models were then applied to independent validation cores for model evaluation.

Limitations of using Raman microscopy for the analysis of high-content-carbon-filled ethylene propylene diene monomer rubber.

PubMed

Ghanbari-Siahkali, Afshin; Almdal, Kristoffer; Kingshott, Peter

2003-12-01

The effects of laser irradiation on changes to the surface chemistry and structure of a commercially available ethylene propylene diene monomer (EPDM) rubber sample after Raman microscopy analysis was investigated. The Raman measurements were carried out with different levels of laser power on the sample, ranging from 4.55 mW to 0.09 mW. The surface of the EPDM was analyzed before and after laser exposure using X-ray photoelectron spectroscopy (XPS) and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy. The techniques have surface probe depths of approximately < or = 10 nm and 1 microm, respectively. Both sets of analysis show that ingredients of the blended EPDM rubber "bloom" to the surface as a result of local heating that takes place due to the absorption of laser by carbon black during the Raman analysis. Scanning electron microscopy (SEM) analysis was also performed on the Raman analyzed areas to visually illustrate the effects created due to laser light exposure (i.e., burning marks). The change in surface chemistry also occurs in regions a few millimeters from the exposed sites, indicating that the effect is quite long range. However, this phenomenon has no major influence, as far as XPS or ATR-FTIR results disclose, on the backbone structure of the rubber sample. The results indicate that precautions should be taken when analyzing complex blended polymer samples using Raman spectroscopy.

Characterization of diesel fuel by chemical separation combined with capillary gas chromatography (GC) isotope ratio mass spectrometry (IRMS).

PubMed

Harvey, Scott D; Jarman, Kristin H; Moran, James J; Sorensen, Christina M; Wright, Bob W

2012-09-15

The purpose of this study was to perform a preliminary investigation of compound-specific isotope analysis (CSIA) of diesel fuels to evaluate whether the technique could distinguish diesel samples from different sources/locations. The ability to differentiate or correlate diesel samples could be valuable for discovering fuel tax evasion schemes or for environmental forensic studies. Two urea adduction-based techniques were used to isolate the n-alkanes from the fuel. Both carbon isotope ratio (δ(13)C) and hydrogen isotope ratio (δD) values for the n-alkanes were then determined by CSIA in each sample. The samples investigated had δ(13)C values that ranged from -30.1‰ to -26.8‰, whereas δD values ranged from -83‰ to -156‰. Plots of δD versus δ(13)C with sample n-alkane points connected in order of increasing carbon number gave well-separated clusters with characteristic shapes for each sample. Principal components analysis (PCA) with δ(13)C, δD, or combined δ(13)C and δD data was applied to extract the maximum information content. PCA scores plots could clearly differentiate the samples, thereby demonstrating the potential of this approach for distinguishing (e.g., fingerprinting) fuel samples using δ(13)C and δD values. Copyright © 2012 Elsevier B.V. All rights reserved.

Surface and catalytic properties of acid metal carbons prepared by the sol gel method

NASA Astrophysics Data System (ADS)

Aguado-Serrano, J.; Rojas-Cervantes, M. L.; Martín-Aranda, R. M.; López-Peinado, A. J.; Gómez-Serrano, V.

2006-06-01

The sol-gel method has been applied for the synthesis of a series of acid metal-carbon xerogels (with M = V, Cr, Mo and Ni) by polymerisation of resorcinol with formaldehyde in the presence of metallic precursors. A blank sample was also prepared without any metal addition. The xerogels were heated in nitrogen at 1000 °C to obtain the pyrolysed products. The samples were characterised by different techniques such as thermal-mass spectrometry analysis, gas physisorption, and mercury porosimetry. In addition, the acid character of the pyrolysed products was tested by the Claisen-Schmidt condensation between benzaldehyde and acetophenone for the formation of chalcones.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

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

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Analysis of PM2.5 in Córdoba, Argentina under the effects of the El Niño Southern Oscillation

NASA Astrophysics Data System (ADS)

Lanzaco, Bethania L.; Olcese, Luis E.; Querol, Xavier; Toselli, Beatriz M.

2017-12-01

In this work, PM2.5 samples were collected in the winter-spring months of 2014-2016 at an urban site in Córdoba. Córdoba is the second largest city in Argentina and is an important industrial and touristic center. The collected samples were individually analyzed for chemical composition using different techniques. The soluble inorganic ions and carbonaceous particles were determined from bulk aerosol samples for the first time in the city. The mass concentrations of PM2.5, organic carbon, elemental carbon, inorganic ions and metals were determined according to the mass balance. The dominant mass components were organic matter and elemental carbon (54.8%), mineral dust (6.1%), secondary inorganic aerosols (3.0%), and salt (1.2%). A principal component analysis was applied to the samples and resulted in five major factors that explained 79% of the variance in PM2.5. These factors represented combustion, industrial sources, soil dust, secondary inorganic aerosol, and salt, and each explained between 11% and 20% of the variance. A comparison with the results from a previous campaign (2010-2011) revealed appreciable changes in the PM2.5 chemical composition. These changes were attributed to the two extreme meteorological conditions that prevailed in the region. The years 2014-2016 were largely dominated by the warm phase of the El Niño-Southern Oscillation, which leads to humid and cold weather in the Córdoba region, while the samples from 2010 to 2011 were collected during the dry and hot years resulting from the La Niña regime.

Biogenic carbon in combustible waste: waste composition, variability and measurement uncertainty.

PubMed

Larsen, Anna W; Fuglsang, Karsten; Pedersen, Niels H; Fellner, Johann; Rechberger, Helmut; Astrup, Thomas

2013-10-01

Obtaining accurate data for the contents of biogenic and fossil carbon in thermally-treated waste is essential for determination of the environmental profile of waste technologies. Relations between the variability of waste chemistry and the biogenic and fossil carbon emissions are not well described in the literature. This study addressed the variability of biogenic and fossil carbon in combustible waste received at a municipal solid waste incinerator. Two approaches were compared: (1) radiocarbon dating ((14)C analysis) of carbon dioxide sampled from the flue gas, and (2) mass and energy balance calculations using the balance method. The ability of the two approaches to accurately describe short-term day-to-day variations in carbon emissions, and to which extent these short-term variations could be explained by controlled changes in waste input composition, was evaluated. Finally, the measurement uncertainties related to the two approaches were determined. Two flue gas sampling campaigns at a full-scale waste incinerator were included: one during normal operation and one with controlled waste input. Estimation of carbon contents in the main waste types received was included. Both the (14)C method and the balance method represented promising methods able to provide good quality data for the ratio between biogenic and fossil carbon in waste. The relative uncertainty in the individual experiments was 7-10% (95% confidence interval) for the (14)C method and slightly lower for the balance method.

Molecular selectivity of brown carbon chromophores.

PubMed

Laskin, Julia; Laskin, Alexander; Nizkorodov, Sergey A; Roach, Patrick; Eckert, Peter; Gilles, Mary K; Wang, Bingbing; Lee, Hyun Ji Julie; Hu, Qichi

2014-10-21

Complementary methods of high-resolution mass spectrometry and microspectroscopy were utilized for molecular analysis of secondary organic aerosol (SOA) generated from ozonolysis of two structural monoterpene isomers: D-limonene SOA (LSOA) and α-pinene SOA (PSOA). The LSOA compounds readily formed adducts with Na(+) under electrospray ionization conditions, with only a small fraction of compounds detected in the protonated form. In contrast, a significant fraction of PSOA compounds appeared in the protonated form because of their increased molecular rigidity. Laboratory simulated aging of LSOA and PSOA, through conversion of carbonyls into imines mediated by NH3 vapors in humid air, resulted in selective browning of the LSOA sample, while the PSOA sample remained white. Comparative analysis of the reaction products in the aged LSOA and PSOA samples provided insights into chemistry relevant to formation of brown carbon chromophores. A significant fraction of carbonyl-imine conversion products with identical molecular formulas was detected in both samples. This reflects the high level of similarity in the molecular composition of these two closely related SOA materials. Several highly conjugated products were detected exclusively in the brown LSOA sample and were identified as potential chromophores responsible for the observed color change. The majority of the unique products in the aged LSOA sample with the highest number of double bonds contain two nitrogen atoms. We conclude that chromophores characteristic of the carbonyl-imine chemistry in LSOA are highly conjugated oligomers of secondary imines (Schiff bases) present at relatively low concentrations. Formation of this type of conjugated compounds in PSOA is hindered by the structural rigidity of the α-pinene oxidation products. Our results suggest that the overall light-absorbing properties of SOA may be determined by trace amounts of strong brown carbon chromophores.

Soil Organic Carbon and Nutrient Dynamics in Reclaimed Appalachian Mine Soil

NASA Astrophysics Data System (ADS)

Acton, P.; Fox, J.; Campbell, J. E.; Rowe, H. D.; Jones, A.

2011-12-01

Past research has shown that drastically disturbed and degraded soils can offer a high potential for soil organic carbon and aboveground carbon sequestration. Little work has been done on both the functioning of soil carbon accumulation and turnover in reclaimed surface mining soils. Reclamation practices of surface coal mine soils in the Southern Appalachian forest region of the United States emphasizes heavy compaction of surface material to provide slope stability and reduce surface erosion, and topsoil is not typically added. An analysis of the previously collected data has provided a 14 year chronosequence of SOC uptake and development in the soil column and revealed that these soils are sequestering carbon at a rate of 1.3 MgC ha-1 yr-1, which is 1.6 to 3 times less than mining soils reported for other regions. Results of bulk density analysis indicate a contrast between 0 - 10 cm (1.51 g cm-3) and 10 - 50 cm (2.04 g cm-3) depth intervals. Aggregate stability was also quantified as well as dynamic soil texture measurements. With this analysis, it has been established that these soils are well below their potential in terms of the ability to store and cycle carbon and other nutrients as well their ability to sustain a fully-functioning forested ecosystem typical for the region. We are taking an integrated approach that relies on ecological observations for present conditions combined with computational modeling to understand long-term soil organic carbon (SOC) accumulation and turnover in regards to SOC sequestration potential and quantification of specific processes by which these soils develop. A dual-isotope end-member model, utilizing the carbon 13 and nitrogen 15 stable isotopes, is being developed to provide greater input into the mathematical separation of organic carbon derived from new soil inputs and existing coal carbon. Soils from the study sites have been isolated into three distinct size pools, and elemental and isotopic analysis of these samples was performed. These results are being used to calibrate an isotope fractionation model to quantify decomposition rates of various conceptual organic matter pools. The hydrology of the mine soils is being modeled using the SCS curve number method to quantify infiltration rates. An assessment of above and belowground biomass was performed to provide estimates for annual plant production. Soil samples will be analyzed for micronutrient content. The CENTURY soil organic matter model will be utilized to provide a biogeochemical analysis of the plant and soil ecosystem. Simulations will be made under varying climatic and land-use changes. Surface coal mine extraction can act as a disturbance and greatly impacts the terrestrial carbon reservoir through initial removal of aboveground biomass and soil carbon and thereafter mineland reclamation. This research will provide a better understanding of the net impact of surface coal mining on terrestrial carbon, thus accounting for long term C sequestration in the soils and aboveground biomass that might offset drastic carbon disturbance in the initial stage of surface mining.

Characterization of Spitsbergen Disks by Transmission Electron Microscopy and Raman Spectroscopy

NASA Technical Reports Server (NTRS)

Thomas-Keprta, K. L.; Clemett, S. J.; Le, L.; Ross, K.; McKay, David S.; Gibson, E. K., Jr.

2010-01-01

'Carbonate disks' found in the fractures and pores spaces of peridotite xenoliths and basalts from the island of Spitsbergen in the Norwegian Svalbard archipelago have been suggested to be "The best (and best documented) terrestrial analogs for the [Martian meteorite] ALH84001 carbonate globules ..." Previous studies have indicated that Spitsbergen carbonates show broadly comparable internal layering and mineral compositions to ALH84001 carbonate-magnetite disks. We report here for the first time, the detailed mineral characterization of Spitsbergen carbonates and their spatial relationship to the host mineral assemblages in the xenolith, using high resolution TEM (as used previously for ALH84001 carbonate disks). These studies were conducted in concert with complementary Raman and SEM analysis of the same samples. Our results indicate that there are significant chemical and physical differences between the disks in Spitsbergen and the carbonates present in ALH84001.

Hydrothermal Alteration of the Mt Unzen Conduit (Shimabara/Japan)

NASA Astrophysics Data System (ADS)

Yilmaz, T. I.; Mayer, K.; Hess, K. U.; Janots, E.; Gilg, H. A.; Dingwell, D. B.

2016-12-01

Investigations were carried out on hydrothermally altered coherent dacitic dykes samples from (USDP-4) drill core at Mt Unzen stratovolcano (Shimabara/Japan). XRF, XRD, EMPA, and C-O-isotope analysis led to insights concerning chemistry, mineralogy, and intensity of alteration as well as the origin of carbonate-precipitating fluids. Additionally a textural characterization of the occurring replacement features in the magma conduit zone was performed. The occurrence of the main secondary phases such as chlorite, pyrite, carbonates, and R1 (Reichweite parameter) illite-smectite indicate a weak to moderate propylitic to phyllic hydrothermal alteration. The dacitic samples of the dykes show different hydrothermal alteration features: (i) carbonate pseudomorphs after hornblende as well as core and zonal textures due to replacement of plagioclase by R1 illite-smectite, (ii) colloform banded fracture fillings and fillings in dissolution vugs, and (iii) chlorite and R1 illite-smectite in the groundmass. Carbonates in fractures comprise iron-rich dolomite solid solutions ("ankerite") and calcite. Isotopic values of d13Cvpdb = -4.59 ± 0.6‰ and d18Ovpdb = -21.73 ± 0.5‰ indicate a hydrothermal-magmatic origin for the carbonate formation. The chlorite-carbonate-pyrite index (CCPI) and the Ishikawa alteration index (AI), applied to the investigated samples show significant differences (CCPI=52.7-57.8; AI=36.1-40.6) indicating their different degree of alteration. According to Nakada et al., 2005, the C13 to C16 dykes represent the feeder dyke from the latest eruption (1991-1995) whereas C8 represents an earlier dyke feeder dyke from an older eruption. Weakest conduit alteration, which was obtained in samples C16-1-5 and C13-2-5, correlates with the alteration degree of the pristine dome rocks. Highest CCPI value was determined for sample C14-1-5 and the highest AI value was determined for sample C15-2-6. The degrees of alteration do not indicate highest alteration of the samples C8-1-2 and C8-2-1 from the older dykes.

Rapid preconcentration method for the determination of azadirachtin-A and -B, nimbin and salannin in neem oil samples by using graphitised carbon solid phase extraction.

PubMed

Ramesh, A; Balasubramanian, M

1999-01-01

A simple and rapid method involving solid phase extraction and liquid chromatography for the determination of azadirachtin-A and -B, nimbin and salannin at nanogram levels in neem oil samples is presented. The neem oil samples are defatted and the compounds of interest extracted by mixing the sample with hexane and passing the hexane solution through a graphitised carbon black column. After washing the column with 2 ml of hexane, azadirachtin-A and -B, nimbin and salannin are eluted with 5 ml of acetonitrile and quantified using HPLC with UV detection. The recoveries of azadirachtin-A and -B, nimbin and salannin in fortified oil samples were 97.4-104.7%. The upper limit of quantification is up to 100 micrograms ml-1 without any additional clean-up and with little interference from lipids during the analysis by HPLC. The method was successfully applied to various neem oil samples collected from different locations in India.

Stable carbon and nitrogen isotope ratios of sodium and potassium cyanide as a forensic signature.

PubMed

Kreuzer, Helen W; Horita, Juske; Moran, James J; Tomkins, Bruce A; Janszen, Derek B; Carman, April

2012-01-01

Sodium and potassium cyanide are highly toxic, produced in large amounts by the chemical industry, and linked to numerous high-profile crimes. The U.S. Centers for Disease Control and Prevention has identified cyanide as one of the most probable agents to be used in a chemical terrorism event. We investigated whether stable C and N isotopic content of sodium and potassium cyanide could serve as a forensic signature for sample matching, using a collection of 65 cyanide samples. Upon analysis, a few of the cyanide samples displayed nonhomogeneous isotopic content associated with degradation to a carbonate salt and loss of hydrogen cyanide. Most samples had highly reproducible isotope content. Of the 65 cyanide samples, >95% could be properly matched based on C and N isotope ratios, with a false match rate <3%. These results suggest that stable C and N isotope ratios are a useful forensic signature for matching cyanide samples. © 2011 American Academy of Forensic Sciences.

Environmental Survey Plans, Fort Sheridan, Sampling and Analysis Plan, Fort Sheridan, Illinois

DTIC Science & Technology

1990-07-01

technique. The flameless AA procedure is based on the absorption of radiation at 253.7 nm by Hg vapor. The Hg is reduced to the elemental state and aerated...desiccator, cupric oxide is added, and the sample is combusted in an induction furnace. The organic carbon content is determined through a calculation in

Sediment Grain Size Measurements: Is There a Differenc Between Digested and Un-digested Samples? And Does the Organic Carbon of the Sample Play a Role

EPA Science Inventory

Grain size is a physical measurement commonly made in the analysis of many benthic systems. Grain size influences benthic community composition, can influence contaminant loading and can indicate the energy regime of a system. We have recently investigated the relationship betw...

Heavy metals content in degraded agricultural soils of a mountain region related to soil properties

NASA Astrophysics Data System (ADS)

Navarro-Pedreño, José; Belén Almendro-Candel, María; Gómez, Ignacio; Jordán, Manuel M.; Bech, Jaume; Zorpas, Antonis

2017-04-01

Agriculture has been practiced for long time in Mediterranean regions. Intensive agriculture and irrigation have developed mainly in the valleys and coastal areas. In the mountainous areas, dry farming has been practiced for centuries. Soils have been fertilized using mainly organic amendments. Plants extracted nutrients and other elements like heavy metals presented in soils and agricultural practices modified soil properties that could favor the presence of heavy metals. In this work, it has been checked the content of heavy metals in 100 agricultural soils samples of the NorthWest area of the province of Alicante (Spain) which has been long cultivated with cereals and olive trees, and now soils are abandoned and degraded because of the low agricultural yields. European policy has the aim to improve the sustainable agriculture and recover landscapes of mountain regions. So that, it is important to check the state of the soils (Marques et al. 2007). Soils samples (arable layer) were analyzed determining: pH (1:5, w/v, water extract), equivalent calcium carbonate content, organic matter by Walkley-Black method (Nelson and Sommers 1996), micronutrients (Cu, Fe, Mn, Zn) extracted with DTPA (Lindsay and Norvell, 1978) and measured by atomic absorption spectrometry, and total content of metals (Cd, Cr, Ni, Pb) measured in soil samples after microwave acid digestion (Moral et al. 1996), quantifying the content of metals by ICP analysis. The correlation between soil properties and metals. The results indicated that pH and carbonates are the most important properties of these soils correlated with the metals (both micronutrients and heavy metals). The available micronutrients (all of them) are close correlated with the pH and carbonates in soils. Moreover, heavy metals like Pb and Ni are related to available Mn and Zn. Keywords: pH, carbonates, heavy metals, abandoned soils. References: Lindsay,W.L., andW.A. Norvell. 1978. "Development of a DTPA Soil Test for Zinc, Iron, Manganese and Copper." Soil Science Society of America Journal 42: 421-428. Marques,M.J., R. Jimenez-Ballesta, A. Á lvarez, and R. Bienes. 2007. "Spanish Research on Soil Damage." Science of the Total Environment 378: 1-4. Moral, R., J. Navarro-Pedreño, I. Gómez, and J. Mataix. 1996. "Quantitative Analysis of Organic Residues: Effects of Samples Preparation in the Determination of Metal." Communications in Soil Science and Plant Analysis 27: 753-761. Nelson, D.W., and L.E. Sommers. 1996. "Total Carbon, Organic Carbon, and Organic Matter." In Methods of Soil Analysis. Part 3. Chemical Methods, edited by D.L. Sparks, A.L. Page, P.A. Helmke, R.H. Loeppert, P.N. Soltanpour, M.A. Tabatabai, C.T. Johnston, M.E. Sumner. Madison, WI: American Society of Agronomy.

The Time-Dependency of Deformation in Porous Carbonate Rocks

NASA Astrophysics Data System (ADS)

Kibikas, W. M.; Lisabeth, H. P.; Zhu, W.

2016-12-01

Porous carbonate rocks are natural reservoirs for freshwater and hydrocarbons. More recently, due to their potential for geothermal energy generation as well as carbon sequestration, there are renewed interests in better understanding of the deformation behavior of carbonate rocks. We conducted a series of deformation experiments to investigate the effects of strain rate and pore fluid chemistry on rock strength and transport properties of porous limestones. Indiana limestone samples with initial porosity of 16% are deformed at 25 °C under effective pressures of 10, 30, and 50 MPa. Under nominally dry conditions, the limestone samples are deformed under 3 different strain rates, 1.5 x 10-4 s-1, 1.5 x 10-5 s-1 and 1.5 x 10-6 s-1 respectively. The experimental results indicate that the mechanical behavior is both rate- and pressure-dependent. At low confining pressures, post-yielding deformation changes from predominantly strain softening to strain hardening as strain rate decreases. At high confining pressures, while all samples exhibit shear-enhanced compaction, decreasing strain rate leads to an increase in compaction. Slower strain rates enhance compaction at all confining pressure conditions. The rate-dependence of deformation behaviors of porous carbonate rocks at dry conditions indicates there is a strong visco-elastic coupling for the degradation of elastic modulus with increasing plastic deformation. In fluid saturated samples, inelastic strain of limestone is partitioned among low temperature plasticity, cataclasis and solution transport. Comparison of inelastic behaviors of samples deformed with distilled water and CO2-saturated aqueous solution as pore fluids provide experimental constraints on the relative activities of the various mechanisms. Detailed microstructural analysis is conducted to take into account the links between stress, microstructure and the inelastic behavior and failure mechanisms.

Carbon isotope analyses of n-alkanes released from rapid pyrolysis of oil asphaltenes in a closed system.

PubMed

Chen, Shasha; Jia, Wanglu; Peng, Ping'an

2016-08-15

Carbon isotope analysis of n-alkanes produced by the pyrolysis of oil asphaltenes is a useful tool for characterizing and correlating oil sources. Low-temperature (320-350°C) pyrolysis lasting 2-3 days is usually employed in such studies. Establishing a rapid pyrolysis method is necessary to reduce the time taken for the pretreatment process in isotope analyses. One asphaltene sample was pyrolyzed in sealed ampoules for different durations (60-120 s) at 610°C. The δ(13) C values of the pyrolysates were determined by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS). The molecular characteristics and isotopic signatures of the pyrolysates were investigated for the different pyrolysis durations and compared with results obtained using the normal pyrolysis method, to determine the optimum time interval. Several asphaltene samples derived from various sources were analyzed using this method. The asphaltene pyrolysates of each sample were similar to those obtained by the flash pyrolysis method on similar samples. However, the molecular characteristics of the pyrolysates obtained over durations longer than 90 s showed intensified secondary reactions. The carbon isotopic signatures of individual compounds obtained at pyrolysis durations less than 90 s were consistent with those obtained from typical low-temperature pyrolysis. Several asphaltene samples from various sources released n-alkanes with distinct carbon isotopic signatures. This easy-to-use pyrolysis method, combined with a subsequent purification procedure, can be used to rapidly obtain clean n-alkanes from oil asphaltenes. Carbon isotopic signatures of n-alkanes released from oil asphaltenes from different sources demonstrate the potential application of this method in 'oil-oil' and 'oil-source' correlations. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

δ13C and δ18O isotopic composition of CaCO3 measured by continuous flow isotope ratio mass spectrometry: statistical evaluation and verification by application to Devils Hole core DH-11 calcite

USGS Publications Warehouse

Revesz, Kinga M.; Landwehr, Jurate M.

2002-01-01

A new method was developed to analyze the stable carbon and oxygen isotope ratios of small samples (400 ± 20 µg) of calcium carbonate. This new method streamlines the classical phosphoric acid/calcium carbonate (H3PO4/CaCO3) reaction method by making use of a recently available Thermoquest-Finnigan GasBench II preparation device and a Delta Plus XL continuous flow isotope ratio mass spectrometer. Conditions for which the H3PO4/CaCO3 reaction produced reproducible and accurate results with minimal error had to be determined. When the acid/carbonate reaction temperature was kept at 26 °C and the reaction time was between 24 and 54 h, the precision of the carbon and oxygen isotope ratios for pooled samples from three reference standard materials was ≤0.1 and ≤0.2 per mill or ‰, respectively, although later analysis showed that materials from one specific standard required reaction time between 34 and 54 h for δ18O to achieve this level of precision. Aliquot screening methods were shown to further minimize the total error. The accuracy and precision of the new method were analyzed and confirmed by statistical analysis. The utility of the method was verified by analyzing calcite from Devils Hole, Nevada, for which isotope-ratio values had previously been obtained by the classical method. Devils Hole core DH-11 recently had been re-cut and re-sampled, and isotope-ratio values were obtained using the new method. The results were comparable with those obtained by the classical method with correlation = +0.96 for both isotope ratios. The consistency of the isotopic results is such that an alignment offset could be identified in the re-sampled core material, and two cutting errors that occurred during re-sampling then were confirmed independently. This result indicates that the new method is a viable alternative to the classical reaction method. In particular, the new method requires less sample material permitting finer resolution and allows automation of some processes resulting in considerable time savings. 

Multi-element compound specific stable isotope analysis of volatile organic compounds at trace levels in groundwater samples

NASA Astrophysics Data System (ADS)

Herrero-Martín, Sara; Nijenhuis, Ivonne; Schmidt, Marie; Wolfram, Diana; Richnow, Hans. H.; Gehre, Matthias

2013-04-01

Groundwater pollution remains one of the major environmental and health concerns. A thorough understanding of sources, sinks and transformation processes of groundwater contaminants is needed to improve risk management evaluation, and to design efficient remediation and water treatment strategies. Isotopic tools provide unique information for an in-depth understanding of the fate of organic chemicals in the environment. During the last decades compound specific isotope analysis (CSIA) of complex mixtures, using gas chromatography-isotope ratio mass spectrometry (GC-IRMS), has gained popularity for the characterization and risk assessment of hazardous waste sites and for isotope forensics of organic contaminants. Multi-element isotope fingerprinting of organic substances provides a more robust framework for interpretation than the isotope analysis of only one element. One major challenge for application of CSIA is the analysis of trace levels of organic compounds in environmental matrices. It is necessary to inject 1 nmol carbon or 8 nmol hydrogen on column, to obtain an accurate and precise measurement of the isotope ratios, which is between two and three orders of magnitude larger than the amount of compound needed for conventional analysis of compound concentrations. Therefore, efficient extraction and pre-concentration techniques have to be integrated with GC-IRMS. Further research is urgently needed in this field, to evaluate the potential of novel and environmental-friendly sample pre-treatment techniques for CSIA to lower the detection limits and extending environmental applications. In this study, the novel coupling of a headspace autosampler (HS) with a programmed temperature vaporizer (PTV), allowing large volume injection of headspace samples, is proposed to improve the sensitivity of CSIA. This automatic, fast and solvent free strategy provides a significant increase on the sensitivity of GC-based methods maintaining the simple headspace instrumentation. The method was developed for the multi-element isotope analysis (carbon and hydrogen) of priority volatile organic groundwater pollutants (methyl tert-butyl ether (MTBE), benzene, toluene, ethylbenzene and o-xylene (BTEX)), and for carbon isotope analysis of chlorinated benzenes and ethenes. The extraction and injection conditions were optimized in terms of maximum sensitivity and minimum isotope effects. During the injection of the headspace sample, the liner is maintained at a low temperature, such that the compounds are retained in a hydrophobic insert packing while the water vapor is eliminated through the split line. With the optimized conditions, it was possible to inject up to 5mL headspace sample with no significant carbon or hydrogen isotopic effects except for the most hydrophobic substance (MTBE), which was subject to a small and reproducible isotope fractionation for hydrogen. The increment on method sensitivity was at least 20 fold in comparison with conventional static headspace analysis. The environmental applicability of the HS-PTV-GC-IRMS method was evaluated by the analysis of groundwater samples from different contaminated field sites, containing BTEX and chlorinated volatile organic contaminants in the low µg/L range. The results obtained demonstrate that this pre-concentration technique is highly promising to enhance the limits of detection of current CSIA methods and broaden its possibilities.

Determining the Local Abundance of Martian Methane and its 13-C/l2-C and D/H Isotopic Ratios for Comparison with Related Gas and Soil Analysis on the 2011 Mars Science Laboratory (MSL) Mission

NASA Technical Reports Server (NTRS)

Webster, Christopher R.; Mahaffy, Paul R.

2011-01-01

Understanding the origin of Martian methane will require numerous complementary measurements from both in situ and remote sensing investigations and laboratory work to correlate planetary surface geophysics with atmospheric dynamics and chemistry. Three instruments (Quadrupole Mass Spectrometer (QMS), Gas Chromatograph (GC) and Tunable Laser Spectrometer (TLS)) with sophisticated sample handling and processing capability make up the Sample Analysis at Mars (SAM) analytical chemistry suite on NASA s 2011 Mars Science Laboratory (MSL) Mission. Leveraging off the SAM sample and gas processing capability that includes methane enrichment, TLS has unprecedented sensitivity for measuring absolute methane (parts-per-trillion), water, and carbon dioxide abundances in both the Martian atmosphere and evolved from heated soil samples. In concert with a wide variety of associated trace gases (e.g. SO2, H2S, NH3, higher hydrocarbons, organics, etc.) and other isotope ratios measured by SAM, TLS will focus on determining the absolute abundances of methane, water and carbon dioxide, and their isotope ratios: 13C/12C and D/H in methane; 13C/12C and 18O/17O/16O in carbon dioxide; and 18O/17O/16O and D/H in water. Measurements near the MSL landing site will be correlated with satellite (Mars Express, Mars 2016) and ground-based observations.

Direct analysis of δ13C and concentration of dissolved organic carbon (DOC) in environmental samples by TOC-IRMS

NASA Astrophysics Data System (ADS)

Kirkels, Frédérique; Cerli, Chiara; Federherr, Eugen; Kalbitz, Karsten

2014-05-01

Dissolved organic carbon (DOC) plays an important role in carbon cycling in terrestrial and aquatic systems. Stable isotope analysis (delta 13C) of DOC could provide valuable insights in its origin, fluxes and environmental fate. Precise and routine analysis of delta 13C and DOC concentration are therefore highly desirable. A promising, new system has been developed for this purpose, linking a high-temperature combustion TOC analyzer trough an interface with a continuous flow isotope ratio mass spectrometer (Elementar group, Hanau, Germany). This TOC-IRMS system enables simultaneous stable isotope (bulk delta 13C) and concentration analysis of DOC, with high oxidation efficiency by high-temperature combustion for complex mixtures as natural DOC. To give delta 13C analysis by TOC-IRMS the necessary impulse for broad-scale application, we present a detailed evaluation of its analytical performance for realistic and challenging conditions inclusive low DOC concentrations and environmental samples. High precision (standard deviation, SD predominantly < 0.15 permil) and accuracy (R2 = 0.9997, i.e. comparison TOC-IRMS and conventional EA-IRMS) were achieved by TOC-IRMS for a broad diversity of DOC solutions. This precision is comparable or even slightly better than that typically reported for EA-IRMS systems, and improves previous techniques for δ13C analysis of DOC. Simultaneously, very good precision was obtained for DOC concentration measurements. Assessment of natural abundance and slightly 13C enriched DOC, a wide range of concentrations (0.2-150 mgC/L) and injection volumes (0.05-3 ml), demonstrated good analytical performance with negligible memory effects, no concentration/volume effects and a wide linearity. Low DOC concentrations (< 2 mgC/L), were correctly analyzed without any pre-concentration. Moreover, TOC-IRMS was successfully applied to analyze DOC from diverse terrestrial, freshwater and marine environments (SD < 0.23 permil). In summary, the TOC-IRMS performs fast and reliable analysis of DOC concentration and δ13C in aqueous samples, without any pre-concentration/freeze-drying. Flexible usage is highlighted by automated, online analysis, a variable injection volume, high throughput and no extensive maintenance. Sample analysis is simple, using small aliquots and with minimal sample preparation. Further investigations should focus on complex, saline matrices and very low DOC concentrations, to achieve a potential lower limit of 0.2 mgC/L. High-resolution, routine delta 13C analysis of DOC by TOC-IRMS offers opportunities for wide-scale application in terrestrial, freshwater and marine research to elucidate the role of DOC in biogeochemical processes and ecosystem functioning.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York-July 1997 through June 1999

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance/quality-control data for the time period addressed in this report were stored in the laboratory's SAS data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality- control samples analyzed from July 1997 through June 1999. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration and (or) low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, ammonium, calcium, chloride, specific conductance, and sulfate. The data from the potassium and sodium analytical procedures are insufficient for evaluation. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 11 of 13 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. Blank analysis results for chloride showed that 22 percent of blanks did not meet data-quality objectives and results for dissolved organic carbon showed that 31 percent of the blanks did not meet data-quality objectives. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 14 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except total aluminum (70 percent of samples met objectives) and potassium (83 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality for most constituents over the time period. The P-sample (low-ionic-strength constituents) analysis had good ratings in two of these studies and a satisfactory rating in the third. The results of the T-sample (trace constituents) analysis indicated high data quality with good ratings in all three studies. The N-sample (nutrient constituents) studies had one each of excellent, good, and satisfactory ratings. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 80 percent of the samples met data-quality objectives for 9 of the 13 analytes; the exceptions were dissolved organic carbon, ammonium, chloride, and specific conductance. Data-quality objectives were not met for dissolved organic carbon in two NWRI studies, but all of the samples were within control limits for the last study. Data-quality objectives were not met in 41 percent of samples analyzed for ammonium, 25 percent of samples analyzed for chloride, and 30 percent of samples analyzed for specific conductance. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 84 percent of the samples analyzed for calcium, chloride, magnesium, pH, and potassium. Data-quality objectives were met by 73 percent of those analyzed for sulfate. The data-quality objective was not met for sodium. The data are insufficient for evaluation of the specific conductance results.

Effect of polyaniline on MWCNTs supercapacitor properties prepared by electrophoretic deposition

NASA Astrophysics Data System (ADS)

Razak, Rozelia Azila Abd; Eleas, Nor Hamizah; Mohammad, Nurul Nazwa; Yusof, Azmi Mohamed; Zaine, Intan Syaffinazzilla

2017-08-01

Multi-walled carbon nanotubes (MWCNTs) is widely used as supercapacitor electrode material. However, the specific capacitance of MWCNTs cannot achieve optimum value to facilitate required demand. Conducting polymers have been introduced to achieve optimum energy density and power density of supercapacitor electrode material. Previous work had demonstrated the effects of adding conducting polymer into carbon base material to get pseudocapacitance effect. Nevertheless the effects specifically of polyaniline (PANi) to MWCNTs were significantly low. This work describes the effect of PANi adding on MWCNTs film prepared by electrophoretic deposition (EPD) technique in order to increase the specific capacitance of MWCNTs. The commercial MWCNTs is dispersed in deionized water by using crystal violet. The admixtures without PANi (sample A), 5wt.% of PANi (sample B) and 10wt.% of PANi (sample C) have been prepared by ex-situ polymerization. The voltage supplied for film deposition is 8 V for 5 minutes. The morphology, functional group and electrochemical properties of MWCNTs due to the presence of PANi had been studied. From FESEM analysis, the presence of PANi can be clearly observed for sample B and sample C while FTIR analysis, proves PANi structure on MWCNTs with its functional group presence in sample B and sample C through the absorbtion band which obviously shifted to higher value compare to sample A. Cyclic voltammogram (CV) analysis shown redox activity occurred in sample B and sample C with identical anodic and cathodic peaks. Sample B hold the higher specific capacitance and higher energy density compared than sample A and sample B. From galvanostatic charge-discharge (CD) measurement, the charge and discharge process for sample B is longer than sample A and sample C which consequently lower its power density. The presence of PANi at 5wt.% is able to increase specific capacitance as well as energy density to optimum value.

Carbon and Oxygen Isotope Measurements of Ordinary Chondrite (OC) Meteorites from Antarctica Indicate Distinct Terrestrial Carbonate Species using a Stepped Acid Extraction Procedure Impacting Mars Carbonate Research

NASA Astrophysics Data System (ADS)

Evans, M. E.; Niles, P. B.; Locke, D.

2015-12-01

The purpose of this study is to characterize the stable isotope values of terrestrial, secondary carbonate minerals from five OC meteorites collected in Antarctica. These samples were selected for analysis based upon their size and collection proximity to known Martian meteorites. They were also selected based on petrologic type (3+) such that they were likely to be carbonate-free before falling to Earth. This study has two main tasks: 1) characterize the isotopic composition of terrestrial, secondary carbonate minerals formed on meteorites in Antarctica, and 2) study the mechanisms of carbonate formation in cold and arid environments with Antarctica as an analog for Mars. Two samples from each meteorite, each ~0.5g, was crushed and dissolved in pure phosphoric acid for 3 sequential reactions: a) Rx0 for 1 hour at 30°C, b) Rx1 for 18 hours at 30°C, and c) Rx2 for 3 hours at 150°C. CO2 was distilled by freezing with liquid nitrogen from each sample tube, then separated from organics and sulfides with a TRACE GC using a Restek HayeSep Q 80/100 6' 2mm stainless column, and then analyzed on a Thermo MAT 253 IRMS in Dual Inlet mode. This system was built at NASA/JSC over the past 3 years and proof tested with known carbonate standards to develop procedures, assess yield, and quantify expected uncertainties. Two distinct species of carbonates are found based on the stepped extraction technique: 1) Ca-rich carbonate released at low temperatures, and 2) Mg, or Fe-rich carbonate released at high temperatures. Preliminary results indicate that most of the carbonates present in the ordinary chondrites analyzed have δ13C=+5‰, which is consistent with formation from atmospheric CO2 δ13C=-7‰ at -20°C. The oxygen isotopic compositions of the carbonates vary between +4‰ and +34‰ with the Mg-rich and/or Fe-rich carbonates possessing the lowest δ18O values. This suggests that the carbonates formed under a wide range of temperatures. However, the carbonate oxygen isotope compositions are consistently heavier than what would be expected if the carbonates formed in equilibrium with melted ice in Antarctica.

Identification of sources of tar balls deposited along the Goa coast, India, using fingerprinting techniques.

PubMed

Suneel, V; Vethamony, P; Zakaria, M P; Naik, B G; Prasad, K V S R

2013-05-15

Deposition of tar balls along the coast of Goa, India is a common phenomenon during the southwest monsoon. Representative tar ball samples collected from various beaches of Goa and one Bombay High (BH) crude oil sample were subjected to fingerprint analysis based on diagnostic ratios of n-alkane, biomarkers of pentacyclic tri-terpanes and compound specific stable carbon isotope (δ¹³C) analysis to confirm the source. The results were compared with the published data of Middle East Crude Oil (MECO) and South East Asian Crude Oil (SEACO). The results revealed that the tar balls were from tanker-wash derived spills. The study also confirmed that the source is not the BH, but SEACO. The present study suggests that the biomarkers of alkanes and hopanes coupled with stable carbon isotope analysis act as a powerful tool for tracing the source of tar balls, particularly when the source specific biomarkers fail to distinguish the source. Copyright © 2013 Elsevier Ltd. All rights reserved.

An electrochemical impedance spectroscopy study of polymer electrolyte membrane fuel cells electrocatalyst single wall carbon nanohorns-supported.

PubMed

Brandão, Lúcia; Boaventura, Marta; Passeira, Carolina; Gattia, Daniele Mirabile; Marazzi, Renzo; Antisari, Marco Vittori; Mendes, Adélio

2011-10-01

Electrochemical impedance spectroscopy (EIS) was used to study the polymer electrolyte membrane fuel cells (PEMFC) performance when using single wall carbon nanohorns (SWNH) to support Pt nanoparticles. Additionally, as-prepared and oxidized SWNH Pt-supports were compared with conventional carbon black. Two different oxidizing treatments were considered: oxygen flow at 500 degrees C and reflux in an acid solution at 85 degrees C. Both oxidizing treatments increased SWNH surface area; oxygen treatment increased surface area 4 times while acid treatment increased 2.6 times. The increase in surface area should be related to the opening access to the inner tube of SWNH. Acid treatment of SWNH increased chemical fragility and decreased electrocatalyst load in comparison with as-prepared SWNH. On the other hand, the oxygen treated SWNH sample allowed to obtain the highest electrocatalyst load. The use of as-prepared and oxygen treated SWNH showed in both cases catalytic activities 60% higher than using conventional carbon black as electrocatalyst support in PEMFC. Moreover, EIS analysis indicated that the major improvement in performance is related to the cathode kinetics in the as-prepared SWNH sample, while concerning the oxidized SWNH sample, the improvements are related to the electrokinetics in both anode and cathode electrodes. These improvements should be related with differences in the hydrophobic character between SWNH and carbon black.

Woodstove smoke and CO emissions: comparison of reference methods with the VIP sampler.

PubMed

Jaasma, D R; Champion, M C; Shelton, J W

1990-06-01

A new field sampler has been developed for measuring the particulate matter (PM) and carbon monoxide emissions of woodburning stoves. Particulate matter is determined by carbon balance and the workup of a sample train which is similar to a room-temperature EPA Method 5G train. A steel tank, initially evacuated, serves as the motive force for sampling and also accumulates a gas sample for post-test analysis of time-averaged stack CO and CO2 concentrations. Workup procedures can be completed within 72 hours of sampler retrieval. The system has been compared to reference methods in two laboratory test series involving six different woodburning appliances and two independent laboratories. The correlation of field sampler emission rates and reference method rates is strong.

Woodstove smoke and CO emissions: Comparison of reference methods with the VIP sampler

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

Jaasma, D.R.; Champion, M.C.; Shelton, J.W.

1990-06-01

A new field sampler has been developed for measuring the particulate matter (PM) and carbon monoxide emissions of woodburning stoves. Particulate matter is determined by carbon balance and the workup of a sample train which is similar to a room-temperature EPA Method 5G train. A steel tank, initially evacuated, serves as the motive force for sampling and also accumulates a gas sample for post-test analysis of time-averaged stack CO and CO{sub 2} concentrations. Workup procedures can be completed within 72 hours of sampler retrieval. The system has been compared to reference methods in two laboratory test series involving six differentmore » woodburning appliances and two independent laboratories. The correlation of field sampler emission rates and reference method rates is strong.« less

Photodetector based on carbon nanotubes

NASA Astrophysics Data System (ADS)

Pavlov, A.; Kitsyuk, E.; Ryazanov, R.; Timoshenkov, V.; Adamov, Y.

2015-09-01

Photodetector based on carbon nanotubes (CNT) was investigated. Sensors were done on quartz and silicon susbtrate. Samples of photodetectors sensors were produced by planar technology. This technology included deposition of first metal layer (Al), lithography for pads formation, etching, and formation of local catalyst area by inverse lithography. Vertically-aligned multi-wall carbon nanotubes were directly synthesized on substrate by PECVD method. I-V analysis and spectrum sensitivity of photodetector were investigated for 0.4 μm - 1.2 μm wavelength. Resistivity of CNT layers over temperature was detected in the range of -20°C to 100°C.

[Improvement of the determination method of benzene, toluene, ethylbenzene and xylene(BTEX) in water using activated carbon fiber solid-phase microextraction/gas chromatography-mass spectrometry(GC-MS)].

PubMed

Jia, Jin-ping; Feng, Xue; Fang, Neng-hu; Huang, Jia-liang

2002-01-01

The methods of direct injection, carbon disulfide extraction and activated carbon fiber solid-phase microextraction/GC-MS, usually used in the determination of BTEX in water matrix, are compared and discussed. Experimental data of linearity, precision and limit of detection illustrate that the last one is better than the two other methods. This method was tested by the practical sample experiments and expected to be a simple and sensitive new method for the analysis of BTEX in water.

Forensic utility of the carbon isotope ratio of PVC tape backings

NASA Astrophysics Data System (ADS)

Stern, L. A.; Thompson, A. H.; Mehltretter, A. H.; McLaskey, V.; Parish, A.; Aranda, R.

2008-12-01

Forensic interest in adhesive tapes with PVC-backings (polyvinyl chloride, electrical tapes) derives from their use in construction of improvised explosive devices, drug packaging and in a variety of other illicit activities. Due to the range of physical characteristics and chemical compositions of such tapes, traditional microscopic and chemical analysis of the tape backings and adhesives offer a high degree of discrimination between tapes from different manufacturers and products. To evaluate whether carbon isotope ratios may be able to increase discrimination of electrical tapes, particularly with regards to different tapes of the same product, we assessed the PVC-backings of 87 rolls of black electrical tape for their δ13C values. The adhesive on these tapes was physically removed with hexane, and plasticizers within the PVC tape backings were removed by three-20 minute extractions with chloroform. The δ13C values of the PVC tape backings ranged between -23.8 and -41.5 (‰ V-PDB). The carbon isotopic variation within a product (identical brand and product identification) is significant, based on five products with at least 3 rolls (ranges of 7.4‰ (n=3), 10.0‰ (n=6), 4.2‰ (n=16), 3.8‰ (n=6), and 11.5‰ (n=8), respectively). There was no measurable carbon isotope variation in regards to the following: a) along the length of a roll (4 samples from 1 roll); b) between the center and edge of a strip of tape (1 pair); c) between rolls assumed to be from the same lot of tape (2 pairs); d) between different rolls from the same batch of tape (same product purchased at the same time and place; 5 pairs); and e) between samples of a tape at room temperature, heated to 50° C and 80° C for 1 week. For each sample within the population of 87 tapes, carbon isotopes alone exclude 80 to 100% of the tapes as a potential match, with an average exclusion power of 92.5%, using a window of ± 0.4‰. Carbon isotope variations originate from variations in starting materials and recycling reactants during manufacture; as a result, tapes may be otherwise physically and chemical indistinguishable, but may have distinct carbon isotope ratios. We compared the carbon isotope ratios of 6 pairs of pre- and post-blast samples of PVC tapes adhered to explosive charges. The carbon isotope ratios of the post-blast samples were 0 to 0.5 ‰ higher than the corresponding pre-blast samples. Possible causes of this carbon isotope increase may be the reaction of the plasticizer and/or adhesive with the PVC backing during the explosion or the addition of debris to the tape backing during the explosion. Even with these minor explosive-induced carbon isotope alterations, the δ13C values of post-blast PVC tape backings were similar enough to the starting material to make carbon isotope ratios of post-blast tape a useful forensic tool. The range of carbon isotope ratios that would be used to exclude potential matches would have to be larger for post-blast samples, but with a 17 ‰ range in the population, this approach may still be useful for post-blast tape samples.

Coal liquefaction process streams characterization and evaluation. Gold tube carbonization and reflectance microscopy

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

Mitchell, G.; Davis, A.; Burke, F.P.

1991-12-01

This study demonstrated the use of the gold tube carbonization technique and reflectance microscopy analysis for the examination of process-derived materials from direct coal liquefaction. The carbonization technique, which was applied to coal liquefaction distillation resids, yields information on the amounts of gas plus distillate, pyridine-soluble resid, and pyridine-insoluble material formed when a coal liquid sample is heated to 450{degree}C for one hour at 5000 psi in an inert atmosphere. The pyridine-insolubles then are examined by reflectance microscopy to determine the type, amount, and optical texture of isotropic and anisotropic carbon formed upon carbonization. Further development of these analytical methodsmore » as process development tools may be justified on the basis of these results.« less

Effects of Water Vapor on the Data Quality of the Stable Oxygen Isotopic Ratio of Atmospheric Carbon Dioxide

NASA Astrophysics Data System (ADS)

Evans, C. U.; White, J. W.; Vaughn, B.; Tans, P. P.; Pardo, L.

2007-12-01

The stable oxygen isotopic ratio of carbon dioxide can potentially track fundamental indicators of environmental change such as the balance between photosynthesis and respiration on regional to global scales. The Stable Isotope Laboratory (SIL) at the Institute of Arctic and Alpine Research (INSTAAR), University of Colorado at Boulder, has measured the stable isotopes of atmospheric carbon dioxide from more than 60 NOAA/Earth System Research Laboratory (ESRL) air flask-sampling sites since the early 1990s. If air is sampled without drying, oxygen can exchange between carbon dioxide and water in the flasks, entirely masking the desired signal. An attempt to investigate how water vapor is affecting the δ18O signal is accomplished by comparing the SIL measurements with specific humidity, calculated from the National Climatic Data Center (NCDC) global integrated surface hourly temperature and dew point database, at the time of sampling. Analysis of sites where samples have been collected initially without drying, and subsequently with a drying kit, in conjunction with the humidity data, has led to several conclusions. Samples that initially appear isotopically unaltered, in that their δ18O values are within the expected range, are being subtly influenced by the water vapor in the air. At Bermuda and other tropical to semi-tropical sites, the 'wet' sampling values have a seasonal cycle that is strongly anti-correlated to the specific humidity, while the 'dry' values have a seasonal cycle that is shifted earlier than the specific humidity cycle by 1-2 months. The latter phasing is expected given the seasonal phasing between climate over the ocean and land, while the former is consistent with a small, but measurable isotope exchange in the flasks. In addition, we note that there is a strong (r > 0.96) correlation between the average specific humidity and the percent of rejected samples for 'wet' sampling. This presents an opportunity for determining a threshold of specific humidity, below which air flask samples can be trusted. This approach may allow segregation of suspect and trusted data, and thus provide an improved record of oxygen isotopic ratios of carbon dioxide over the past two decades.

Air pollution from aircraft. [jet exhaust - aircraft fuels/combustion efficiency

NASA Technical Reports Server (NTRS)

Heywood, J. B.; Chigier, N. A.

1975-01-01

A model which predicts nitric oxide and carbon monoxide emissions from a swirl can modular combustor is discussed. A detailed analysis of the turbulent fuel-air mixing process in the swirl can module wake region is reviewed. Hot wire anemometry was employed, and gas sampling analysis of fuel combustion emissions were performed.

Automated simultaneous measurement of the δ(13) C and δ(2) H values of methane and the δ(13) C and δ(18) O values of carbon dioxide in flask air samples using a new multi cryo-trap/gas chromatography/isotope ratio mass spectrometry system.

PubMed

Brand, Willi A; Rothe, Michael; Sperlich, Peter; Strube, Martin; Wendeberg, Magnus

2016-07-15

The isotopic composition of greenhouse gases helps to constrain global budgets and to study sink and source processes. We present a new system for high-precision stable isotope measurements of carbon, hydrogen and oxygen in atmospheric methane and carbon dioxide. The design is intended for analyzing flask air samples from existing sampling programs without the need for extra sample air for methane analysis. CO2 and CH4 isotopes are measured simultaneously using two isotope ratio mass spectrometers, one for the analysis of δ(13) C and δ(18) O values and the second one for δ(2) H values. The inlet carousel delivers air from 16 sample positions (glass flasks 1-5 L and high-pressure cylinders). Three 10-port valves take aliquots from the sample stream. CH4 from 100-mL air aliquots is preconcentrated in 0.8-mL sample loops using a new cryo-trap system. A precisely calibrated working reference air is used in parallel with the sample according to the Principle of Identical Treatment. It takes about 36 hours for a fully calibrated analysis of a complete carousel including extractions of four working reference and one quality control reference air. Long-term precision values, as obtained from the quality control reference gas since 2012, account for 0.04 ‰ (δ(13) C values of CO2 ), 0.07 ‰ (δ(18) O values of CO2 ), 0.11 ‰ (δ(13) C values of CH4 ) and 1.0 ‰ (δ(2) H values of CH4 ). Within a single day, the system exhibits a typical methane δ(13) C standard deviation (1σ) of 0.06 ‰ for 10 repeated measurements. The system has been in routine operation at the MPI-BGC since 2012. Consistency of the data and compatibility with results from other laboratories at a high precision level are of utmost importance. A high sample throughput and reliability of operation are important achievements of the presented system to cope with the large number of air samples to be analyzed. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Long-term measurements (2010-2014) of carbonaceous aerosol and carbon monoxide at the Zotino Tall Tower Observatory (ZOTTO) in central Siberia

NASA Astrophysics Data System (ADS)

Mikhailov, Eugene F.; Mironova, Svetlana; Mironov, Gregory; Vlasenko, Sergey; Panov, Alexey; Chi, Xuguang; Walter, David; Carbone, Samara; Artaxo, Paulo; Heimann, Martin; Lavric, Jost; Pöschl, Ulrich; Andreae, Meinrat O.

2017-12-01

We present long-term (5-year) measurements of particulate matter with an upper diameter limit of ˜ 10 µm (PM10), elemental carbon (EC), organic carbon (OC), and water-soluble organic carbon (WSOC) in aerosol filter samples collected at the Zotino Tall Tower Observatory in the middle-taiga subzone (Siberia). The data are complemented with carbon monoxide (CO) measurements. Air mass back trajectory analysis and satellite image analysis were used to characterise potential source regions and the transport pathway of haze plumes. Polluted and background periods were selected using a non-parametric statistical approach and analysed separately. In addition, near-pristine air masses were selected based on their EC concentrations being below the detection limit of our thermal-optical instrument. Over the entire sampling campaign, 75 and 48 % of air masses in winter and in summer, respectively, and 42 % in spring and fall are classified as polluted. The observed background concentrations of CO and EC showed a sine-like behaviour with a period of 365 ± 4 days, mostly due to different degrees of dilution and the removal of polluted air masses arriving at the Zotino Tall Tower Observatory (ZOTTO) from remote sources. Our analysis of the near-pristine conditions shows that the longest periods with clean air masses were observed in summer, with a frequency of 17 %, while in wintertime only 1 % can be classified as a clean. Against a background of low concentrations of CO, EC, and OC in the near-pristine summertime, it was possible to identify pollution plumes that most likely came from crude-oil production sites located in the oil-rich regions of Western Siberia. Overall, our analysis indicates that most of the time the Siberian region is impacted by atmospheric pollution arising from biomass burning and anthropogenic emissions. A relatively clean atmosphere can be observed mainly in summer, when polluted species are removed by precipitation and the aerosol burden returns to near-pristine conditions.

Carbon budget for a British upland peat catchment.

PubMed

Worrall, Fred; Reed, Mark; Warburton, Jeff; Burt, Tim

2003-08-01

This study describes the analysis of fluvial carbon flux from an upland peat catchment in the North Pennines. Dissolved organic carbon (DOC), pH, alkalinity and calcium were measured in weekly samples, with particulate organic carbon (POC) measured from the suspended sediment load from the stream outlet of an 11.4-km(2) catchment. For calendar year 1999, regular monitoring of the catchment was supplemented with detailed quasi-continuous measurements of flow and stream temperature, and DOC for the months September through November. The measurements were used to calculate the annual flux of dissolved CO(2), dissolved inorganic carbon, DOC and POC from the catchment and were combined with CO(2) and CH(4) gaseous exchanges calculated from previously published values and the observations of water table height within the peat. The study catchment represents a net sink of 15.4+/-11.9 gC/m(2)/yr. Carbon flows calculated for the study catchment are combined with values in the literature, using a Monte Carlo method, to estimate the carbon budget for British upland peat. For all British upland peat the calculation suggests a net carbon sink of between 0.15 and 0.29 MtC/yr. This is the first study to include a comprehensive study of the fluvial export of carbon within carbon budgets and shows the size of the peat carbon sink to be smaller than previous estimates, although sensitivity analysis shows that the primary productivity rather than fluvial carbon flux is a more important element in estimating the carbon budget in this regard.

Re-evaluation of forest biomass carbon stocks and lessons from the world's most carbon-dense forests.

PubMed

Keith, Heather; Mackey, Brendan G; Lindenmayer, David B

2009-07-14

From analysis of published global site biomass data (n = 136) from primary forests, we discovered (i) the world's highest known total biomass carbon density (living plus dead) of 1,867 tonnes carbon per ha (average value from 13 sites) occurs in Australian temperate moist Eucalyptus regnans forests, and (ii) average values of the global site biomass data were higher for sampled temperate moist forests (n = 44) than for sampled tropical (n = 36) and boreal (n = 52) forests (n is number of sites per forest biome). Spatially averaged Intergovernmental Panel on Climate Change biome default values are lower than our average site values for temperate moist forests, because the temperate biome contains a diversity of forest ecosystem types that support a range of mature carbon stocks or have a long land-use history with reduced carbon stocks. We describe a framework for identifying forests important for carbon storage based on the factors that account for high biomass carbon densities, including (i) relatively cool temperatures and moderately high precipitation producing rates of fast growth but slow decomposition, and (ii) older forests that are often multiaged and multilayered and have experienced minimal human disturbance. Our results are relevant to negotiations under the United Nations Framework Convention on Climate Change regarding forest conservation, management, and restoration. Conserving forests with large stocks of biomass from deforestation and degradation avoids significant carbon emissions to the atmosphere, irrespective of the source country, and should be among allowable mitigation activities. Similarly, management that allows restoration of a forest's carbon sequestration potential also should be recognized.

Carbon Isotope Composition of Mysids at a Terrestrial-Marine Ecotone, Clayoquot Sound, British Columbia, Canada

NASA Astrophysics Data System (ADS)

Mulkins, L. M.; Jelinski, D. E.; Karagatzides, J. D.; Carr, A.

2002-04-01

The relative contribution of summertime terrestrial versus marine carbon to an estuary on coastal British Columbia, Canada was explored using stable carbon isotopic (δ 13C values) analysis of mysid crustaceans (Malacostraca: Peracarida: Mysidacea). We hypothesized that landscape linkages between the forested upland and adjacent inshore marine waters, via river, groundwater and overland flows, may influence carbon content and metabolism in the coastal zone. We sampled 14 stations spatially distributed in a grid and found δ 13C compositions of mysids ranged from -15·2 to -18·4‰. There was, however, no obvious spatial distribution of δ 13C values relative to the estuarine gradient in Cow Bay. Heavy tidal mixing is suggested to disperse marine and terrestrial carbon throughout the entire bay. From a temporal perspective however, mysid δ 13C signatures became enriched over the sampling period (mid-July to mid-August), which is representative of a stronger marine influence. This may arise because mysids are exposed to greater marine-derived carbon sources later in the summer, a decrease in freshwater input (and hence terrestrial carbon), changes in phytoplankton or macrophyte community structure, or that mysids preferentially feed on marine food sources. Overall, the recorded isotopic values are characteristic of marine organic carbon signatures suggesting that in summer, despite the proximity to shore, little or no terrestrial carbon penetrates the food web at the trophic level of mysids. This notwithstanding we believe there is a strong need for additional study of carbon flows at the marine-terrestrial interface, especially for disturbed watersheds.

Re-evaluation of forest biomass carbon stocks and lessons from the world's most carbon-dense forests

PubMed Central

Keith, Heather; Mackey, Brendan G.; Lindenmayer, David B.

2009-01-01

From analysis of published global site biomass data (n = 136) from primary forests, we discovered (i) the world's highest known total biomass carbon density (living plus dead) of 1,867 tonnes carbon per ha (average value from 13 sites) occurs in Australian temperate moist Eucalyptus regnans forests, and (ii) average values of the global site biomass data were higher for sampled temperate moist forests (n = 44) than for sampled tropical (n = 36) and boreal (n = 52) forests (n is number of sites per forest biome). Spatially averaged Intergovernmental Panel on Climate Change biome default values are lower than our average site values for temperate moist forests, because the temperate biome contains a diversity of forest ecosystem types that support a range of mature carbon stocks or have a long land-use history with reduced carbon stocks. We describe a framework for identifying forests important for carbon storage based on the factors that account for high biomass carbon densities, including (i) relatively cool temperatures and moderately high precipitation producing rates of fast growth but slow decomposition, and (ii) older forests that are often multiaged and multilayered and have experienced minimal human disturbance. Our results are relevant to negotiations under the United Nations Framework Convention on Climate Change regarding forest conservation, management, and restoration. Conserving forests with large stocks of biomass from deforestation and degradation avoids significant carbon emissions to the atmosphere, irrespective of the source country, and should be among allowable mitigation activities. Similarly, management that allows restoration of a forest's carbon sequestration potential also should be recognized. PMID:19553199

Methane and Carbon Dioxide Production Rates in Lake Sediments from Sub-Arctic Sweden

NASA Astrophysics Data System (ADS)

DeStasio, J.; Halloran, M.; Erickson, L. M.; Varner, R. K.; Johnson, J. E.; Setera, J.; Prado, M. F.; Wik, M.; Crill, P. M.

2013-12-01

Ecosystems at high latitudes are undergoing rapid change due to amplified arctic warming. Lakes in these regions are sources of both methane (CH4) and carbon dioxide (CO2) to the atmosphere and will likely be impacted by elevated temperatures. Because of the potential increase in the release of organic carbon due to thawing permafrost, it is believed that methanogenesis rates within neighboring fresh water sediments will display a positive feedback response, by increasing CH4 emission to the atmosphere. We studied CH4 production potential of sediments using cores from three lakes in the Stordalen Mire complex in sub-Arctic, Sweden: Inre Harrsjön, Mellan Harrsjön, and Villasjön. Sediment cores were incubated to determine CO2 and CH4 production rates and were analyzed for CH4 concentrations, dissolved inorganic carbon (DIC) concentrations, total organic carbon (TOC) concentrations, as well as carbon, nitrogen and sulfur content. Our results from the Villasjön cores indicate that CH4 production rates were highest at the same sediment depths as peak dissolved CH4 concentrations, with maximum values between depths of approximately 10cm and 30cm. Additionally, the highest observed CH4 production rates were in sediments from areas within Villasjön known to have the highest rates of CH4 ebullition. CO2 production rates were generally highest within surface sediments ranging from about 4cm to 11cm in depth, with production rates displaying a steady decrease below 11cm. Additionally, observed CO2 production rates correlated with total organic carbon (TOC) concentrations with respect to sediment depth, but displayed no relationship with dissolved inorganic carbon (DIC). Further analysis will be conducted to determine how CH4 and CO2 production characteristics vary between sediment core samples, as well as isotopic analysis of select samples taken from each lake.

Dissolution-Assisted Pattern Formation During Olivine Carbonation

NASA Astrophysics Data System (ADS)

Lisabeth, Harrison; Zhu, Wenlu; Xing, Tiange; De Andrade, Vincent

2017-10-01

Olivine and pyroxene-bearing rocks in the oceanic crust react with hydrothermal fluids producing changes in the physical characteristics and behaviors of the altered rocks. Notably, these reactions tend to increase solid volume, reducing pore volume, permeability, and available reactive surface area, yet entirely hydrated and/or carbonated rocks are commonly observed in the field. We investigate the evolution of porosity and permeability of fractured dunites reacted with CO2-rich solutions in laboratory experiments. The alteration of crack surfaces changes the mechanical and transport properties of the bulk samples. Analysis of three-dimensional microstructural data shows that although precipitation of secondary minerals causes the total porosity of the sample to decrease, an interconnected network of porosity is maintained through channelized dissolution and coupled carbonate precipitation. The observed microstructure appears to be the result of chemo-mechanical coupling, which may provide a mechanism of porosity maintenance without the need to invoke reaction-driven cracking.

Sensitive and selective cocaine electrochemical detection using disposable sensors.

PubMed

Asturias-Arribas, Laura; Alonso-Lomillo, M Asunción; Domínguez-Renedo, Olga; Arcos-Martínez, M Julia

2014-06-27

This paper describes the voltammetric determination of cocaine in presence of three different interferences that could be found in street samples using disposable sensors. The electrochemical analysis of this alkaloid can be affected by the presence of codeine, paracetamol or caffeine, whose oxidation peaks may overlap and lead to false positives. This work describes two different solutions to this problem. On one hand, the modification of disposable carbon sensors with carbon nanotubes allows the voltammetric quantification of cocaine by using ordinary least squares regressions in the concentration range from 10 to 155 μmol L(-1), with a reproducibility of 5.6% (RSD, n = 7. On the other hand, partial least squares regressions are used for the resolution of the overlapped voltammetric signals when using screen-printed carbon electrodes without any modification. Both procedures have been successfully applied to the evaluation of the purity of cocaine street samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Dissolution-Assisted Pattern Formation During Olivine Carbonation

DOE PAGES

Lisabeth, Harrison; Zhu, Wenlu; Xing, Tiange; ...

2017-08-31

Olivine and pyroxene bearing rocks in the oceanic crust react with hydrothermal fluids producing changes in the physical characteristics and behaviors of the altered rocks. Notably, these reactions tend to increase solid volume, reducing pore volume, permeability and available reactive surface area; yet, entirely hydrated and/or carbonated rocks are commonly observed in the field. We investigate the evolution of porosity and permeability of fractured dunites reacted with CO 2-rich solutions in laboratory experiments. The alteration of crack surfaces changes the mechanical and transport properties of the bulk samples. Analysis of three-dimensional microstructural data shows that although precipitation of secondary mineralsmore » causes the total porosity of the sample to decrease, an interconnected network of porosity is maintained through channelized dissolution and coupled carbonate precipitation. Lastly, the observed microstructure appears to be the result of chemo-mechanical coupling, which may provide a mechanism of porosity maintenance without the need to invoke reaction-driven cracking.« less

Matrix coatings based on anodic alumina with carbon nanostructures in the pores

NASA Astrophysics Data System (ADS)

Gorokh, G. G.; Pashechko, M. I.; Borc, J. T.; Lozovenko, A. A.; Kashko, I. A.; Latos, A. I.

2018-03-01

The nanoporous anodic alumina matrixes thickness of 1.5 mm and pore sizes of 45, 90 and 145 nm were formed on Si substrates. The tubular carbon nanostructures were synthesized into the matrixes pores by pyrolysis of fluid hydrocarbon xylene with 1% ferrocene. The structure and composition of the matrix coatings were examined by scanning electron microscopy, Auger analysis and Raman spectroscopy. The carbon nanostructures completely filled the pores of templates and uniformly covered the tops. The structure of carbon nanostructures corresponded to the structure of multiwall carbon nanotubes. Investigations of mechanical and tribological properties of nanostructured oxide-carbon composite performed by scratching and nanoindentation showed nonlinear dependencies of the frictional force, penetration depth of the cantilever, hardness and plane strain modulus on the load. It was found that the microhardness of the samples increases with reduced of alumina pore diameter, and the penetration depth of the cantilever into the film grows with carbon nanostructures size. The results showed the high mechanical strength of nanostructured oxide-carbon composite.

Chemical vapor deposition: Stable carbons from low-rank coals

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

Sharma, R.K.; Kulas, R.W.; Olson, E.S.

1996-12-31

A chemical vapor deposition (CVD) technique has been used to increase the oxidative stability of activated carbons. Activated carbons prepared from Gascoyne lignite (North Dakota) by thermal or potassium hydroxide activations were subjected to BCI, in helium at 727{degrees}C with or without benzene for a limited period of time, followed by annealing in helium at 900{degrees}C for three days. Untreated and acid-washed coal samples were used to assess the magnitude of the effect of mineral matter in the coal on the boron coating. The oxidative stability of the boron-modified carbons was determined from the decomposition curves obtained from the thermogravimetricmore » analysis. Modification of the as-received, KOH-treated carbon yielded oxidatively stable carbons up to an initial temperature of 520{degrees}C, compared to about 350{degrees}C for the starting material. Similar results were obtained for the carbonized Gascoyne lignite. Sulfurous acid washing of the Gascoyne significantly enhanced the thermal stability (600{degrees}C) of the boron-modified carbon.« less

Preparation of surface-functionalized porous clay heterostructures via carbonization of soft-template and their adsorption performance for toluene

NASA Astrophysics Data System (ADS)

Wang, Yuebo; Su, Xiaoli; Xu, Zhen; Wen, Ke; Zhang, Ping; Zhu, Jianxi; He, Hongping

2016-02-01

A new type of surface-functionalized porous clay heterostructures (SF-PCH) was synthesized via carbonization of the template agents with sulfuric acid. The converted carbons deposited on the porous surface of the SF-PCH samples and changed their surface chemical properties. The composites possessed a maximum carbon content of 5.35%, a large specific surface area of 428 m2/g and micropore volume of approximately 0.2 cm3/g. The layered and porous structure of SF-PCH was retained after carbonization and calcination when sulfuric acid solution with a mild concentration was used. Analysis by XPS confirmed that the carbonaceous matter in the pore channels was functionalized with various organic groups, including carbonaceous, nitrogenous, and sulfated groups. Both the surface chemical property and structural characteristic of adsorbents have effects on the adsorption properties of SF-PCH for toluene. The SF-PCH samples exhibited a stronger adsorption affinity to toluene compared with untreated PCH in the low pressure region, which is more valuable in the practical applications. These results demonstrate that carbonization of soft-template is a feasible process for the surface modification of PCH, enabling the resulting composites to become promising candidates for application in toluene emission control.

Electrical and galvanomagnetic properties of nanoporous carbon samples impregnated with bromine

NASA Astrophysics Data System (ADS)

Danishevskii, A. M.; Popov, V. V.; Kyutt, R. N.; Gordeev, S. K.

2013-07-01

Nanoporous carbon samples with a large specific surface area can be filled with heavier elements or their compounds, which makes it possible to investigate the interaction of their electronic subsystems with carbon. One of the elements convenient for filling pores of carbon materials is bromine. Impregnation of nanoporous carbon samples with bromine causes the occurrence of the processes of micropore filling, monolayer adsorption, and intercalation. It has been found that samples impregnated with bromine substantially change their electrical and galvanomagnetic properties, and these changes depend on the structure of the samples. It has been shown that, if in the skeleton of a porous carbon sample there is a fraction of graphite clusters, the impregnation of the sample with bromine increases the concentration of charged carriers (holes). But when the sample has a quasi-amorphous structure, the injection of bromine into the sample leads to the appearance of a certain concentration of electrons in addition to charged mobile holes of the initial sample; i.e., the electrical conductivity becomes bipolar. In the former case, bromine molecules intercalate graphite clusters and, since bromine is an acceptor during intercalation of graphite, the hole concentration in the carbon skeleton network increases. In the latter case, bromine molecules can only be adsorbed on pore walls. As a result, the adsorption interaction between the electron shells of bromine molecules and the carbon surface leads to the formation of a donor layer near the surface and to the generation of electrons in the carbon skeleton network.

SAMPLING ARTIFACTS IN MEASUREMENT OF ELEMENTAL AND ORGANIC CARBON: LOW VOLUME SAMPLING IN INDOOR AND OUTDOOR ENVIRONMENTS

EPA Science Inventory

Experiments were completed to determine the extent of artifacts from sampling elemental carbon (EC) and organic carbon (OC) under sample conditions consistent with personal sampling. Two different types of experiments were completed; the first examined possible artifacts from oil...

Online combination of reversed-phase/reversed-phase and porous graphitic carbon liquid chromatography for multicomponent separation of proteomics and glycoproteomics samples.

PubMed

Lam, Maggie P Y; Lau, Edward; Siu, S O; Ng, Dominic C M; Kong, Ricky P W; Chiu, Philip C N; Yeung, William S B; Lo, Clive; Chu, Ivan K

2011-11-01

In this paper, we describe an online combination of reversed-phase/reversed-phase (RP-RP) and porous graphitic carbon (PGC) liquid chromatography (LC) for multicomponent analysis of proteomics and glycoproteomics samples. The online RP-RP portion of this system provides comprehensive 2-D peptide separation based on sequence hydrophobicity at pH 2 and 10. Hydrophilic components (e.g. glycans, glycopeptides) that are not retained by RP are automatically diverted downstream to a PGC column for further trapping and separation. Furthermore, the RP-RP/PGC system can provide simultaneous extension of the hydropathy range and peak capacity for analysis. Using an 11-protein mixture, we found that the system could efficiently separate native peptides and released N-glycans from a single sample. We evaluated the applicability of the system to the analysis of complex biological samples using 25 μg of the lysate of a human choriocarcinoma cell line (BeWo), confidently identifying a total of 1449 proteins from a single experiment and up to 1909 distinct proteins from technical triplicates. The PGC fraction increased the sequence coverage through the inclusion of additional hydrophilic sequences that accounted for up to 6.9% of the total identified peptides from the BeWo lysate, with apparent preference for the detection of hydrophilic motifs and proteins. In addition, RP-RP/PGC is applicable to the analysis of complex glycomics samples, as demonstrated by our analysis of a concanavalin A-extracted glycoproteome from human serum; in total, 134 potentially N-glycosylated serum proteins, 151 possible N-glycosylation sites, and more than 40 possible N-glycan structures recognized by concanavalin A were simultaneously detected. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evolution of strength and physical properties of carbonate and ultramafic rocks under hydrothermal conditions

NASA Astrophysics Data System (ADS)

Lisabeth, Harrison Paul

Interaction of rocks with fluids can significantly change mineral assemblage and structure. This so-called hydrothermal alteration is ubiquitous in the Earth's crust. Though the behavior of hydrothermally altered rocks can have planet-scale consequences, such as facilitating oceanic spreading along slow ridge segments and recycling volatiles into the mantle at subduction zones, the mechanisms involved in the hydrothermal alteration are often microscopic. Fluid-rock interactions take place where the fluid and rock meet. Fluid distribution, flux rate and reactive surface area control the efficiency and extent of hydrothermal alteration. Fluid-rock interactions, such as dissolution, precipitation and fluid mediated fracture and frictional sliding lead to changes in porosity and pore structure that feed back into the hydraulic and mechanical behavior of the bulk rock. Examining the nature of this highly coupled system involves coordinating observations of the mineralogy and structure of naturally altered rocks and laboratory investigation of the fine scale mechanisms of transformation under controlled conditions. In this study, I focus on fluid-rock interactions involving two common lithologies, carbonates and ultramafics, in order to elucidate the coupling between mechanical, hydraulic and chemical processes in these rocks. I perform constant strain-rate triaxial deformation and constant-stress creep tests on several suites of samples while monitoring the evolution of sample strain, permeability and physical properties. Subsequent microstructures are analyzed using optical and scanning electron microscopy. This work yields laboratory-based constraints on the extent and mechanisms of water weakening in carbonates and carbonation reactions in ultramafic rocks. I find that inundation with pore fluid thereby reducing permeability. This effect is sensitive to pore fluid saturation with respect to calcium carbonate. Fluid inundation weakens dunites as well. The addition of carbon dioxide to pore fluid enhances compaction and partial recovery of strength compared to pure water samples. Enhanced compaction in CO2-rich fluid samples is not accompanied by enhanced permeability reduction. Analysis of sample microstructures indicates that precipitation of carbonates along fracture surfaces is responsible for the partial restrengthening and channelized dissolution of olivine is responsible for permeability maintenance.

The impact of local government investment on the carbon emissions reduction effect: An empirical analysis of panel data from 30 provinces and municipalities in China.

PubMed

He, Lingyun; Yin, Fang; Zhong, Zhangqi; Ding, Zhihua

2017-01-01

Among studies of the factors that influence carbon emissions and related regulations, economic aggregates, industrial structures, energy structures, population levels, and energy prices have been extensively explored, whereas studies from the perspective of fiscal leverage, particularly of local government investment (LGI), are rare. Of the limited number of studies on the effect of LGI on carbon emissions, most focus on its direct effect. Few studies consider regulatory effects, and there is a lack of emphasis on local areas. Using a cointegration test, a panel data model and clustering analysis based on Chinese data between 2000 and 2013, this study measures the direct role of LGI in carbon dioxide (CO2) emissions reduction. First, overall, within the sample time period, a 1% increase in LGI inhibits carbon emissions by 0.8906% and 0.5851% through its influence on the industrial structure and energy efficiency, respectively, with the industrial structure path playing a greater role than the efficiency path. Second, carbon emissions to some extent exhibit inertia. The previous year's carbon emissions impact the following year's carbon emissions by 0.5375%. Thus, if a reduction in carbon emissions in the previous year has a positive effect, then the carbon emissions reduction effect generated by LGI in the following year will be magnified. Third, LGI can effectively reduce carbon emissions, but there are significant regional differences in its impact. For example, in some provinces, such as Sichuan and Anhui, economic growth has not been decoupled from carbon emissions. Fourth, the carbon emissions reduction effect in the 30 provinces and municipalities sampled in this study can be classified into five categories-strong, relatively strong, medium, relatively weak and weak-based on the degree of local governments' regulation of carbon emissions. The carbon emissions reduction effect of LGI is significant in the western and central regions of China but not in the eastern and northeast regions. This study helps overcome the limitations of previous studies on the regulatory effects of LGI on carbon emissions, and the constructed model may more closely reflect actual economic conditions. Moreover, the current study can benefit countries similar to China that aim to objectively identify the impacts of their LGI on carbon emissions, and such countries can use it as a reference in the formulation of investment policies based on their economic and industrial characteristics.

The impact of local government investment on the carbon emissions reduction effect: An empirical analysis of panel data from 30 provinces and municipalities in China

PubMed Central

He, Lingyun; Yin, Fang; Zhong, Zhangqi; Ding, Zhihua

2017-01-01

Among studies of the factors that influence carbon emissions and related regulations, economic aggregates, industrial structures, energy structures, population levels, and energy prices have been extensively explored, whereas studies from the perspective of fiscal leverage, particularly of local government investment (LGI), are rare. Of the limited number of studies on the effect of LGI on carbon emissions, most focus on its direct effect. Few studies consider regulatory effects, and there is a lack of emphasis on local areas. Using a cointegration test, a panel data model and clustering analysis based on Chinese data between 2000 and 2013, this study measures the direct role of LGI in carbon dioxide (CO2) emissions reduction. First, overall, within the sample time period, a 1% increase in LGI inhibits carbon emissions by 0.8906% and 0.5851% through its influence on the industrial structure and energy efficiency, respectively, with the industrial structure path playing a greater role than the efficiency path. Second, carbon emissions to some extent exhibit inertia. The previous year’s carbon emissions impact the following year’s carbon emissions by 0.5375%. Thus, if a reduction in carbon emissions in the previous year has a positive effect, then the carbon emissions reduction effect generated by LGI in the following year will be magnified. Third, LGI can effectively reduce carbon emissions, but there are significant regional differences in its impact. For example, in some provinces, such as Sichuan and Anhui, economic growth has not been decoupled from carbon emissions. Fourth, the carbon emissions reduction effect in the 30 provinces and municipalities sampled in this study can be classified into five categories—strong, relatively strong, medium, relatively weak and weak—based on the degree of local governments’ regulation of carbon emissions. The carbon emissions reduction effect of LGI is significant in the western and central regions of China but not in the eastern and northeast regions. This study helps overcome the limitations of previous studies on the regulatory effects of LGI on carbon emissions, and the constructed model may more closely reflect actual economic conditions. Moreover, the current study can benefit countries similar to China that aim to objectively identify the impacts of their LGI on carbon emissions, and such countries can use it as a reference in the formulation of investment policies based on their economic and industrial characteristics. PMID:28727783

Scaling craters in carbonates: Electron paramagnetic resonance analysis of shock damage

NASA Technical Reports Server (NTRS)

Polanskey, Carol A.; Ahrens, Thomas J.

1994-01-01

Carbonate samples from the 8.9-Mt nuclear (near-surface explosion) crater, OAK, and a terrestrial impact crater, Meteor Crater, were analyzed for shock damage using electron paramagnetic resonance (EPR). Samples from below the OAK apparent crater floor were obtained from six boreholes, as well as ejecta recovered from the crater floor. The degree of shock damage in the carbonate material was assessed by comparing the sample spectra to the spectra of Solenhofen and Kaibab limestone, which had been skocked to known pressures. Analysis of the OAK Crater borehole samples has identified a thin zone of allocthonous highly shocked (10-13 GPa) carbonate material underneath the apparent crater floor. This approx. 5- to 15-m-thick zone occurs at a maximum depth of approx. 125 m below current seafloor at the borehole, sited at the initial position of the OAK explosive, and decreases in depth towards the apparent crater edge. Because this zone of allocthonous shocked rock delineates deformed rock below, and a breccia of mobilized sand and collapse debris above, it appears to outline the transient crater. The transient crater volume inferred in this way is found to by 3.2 +/- 0.2 times 10(exp 6)cu m, which is in good agreement with a volume of 5.3 times 10(exp 6)cu m inferred from gravity scaling of laboratory experiments. A layer of highly shocked material is also found near the surface outside the crater. The latter material could represent a fallout ejecta layer. The ejecta boulders recovered from the present crater floor experienced a range of shock pressures from approx. 0 to 15 GPa with the more heavily shocked samples all occurring between radii of 360 and approx. 600 m. Moreover, the fossil content, lithology and Sr isotopic composition all demonstrate that the initial position of the bulk of the heavily shocked rock ejecta sampled was originally near surface rock at initial depths in the 32 to 45-m depth (below sea level) range. The EPR technique is also sensitive to prehistoric shock damage. This is demonstrated by our study of shocked Kaibab limestone from the 49,000-year-old Meteor (Barringer) Crater Arizona.

Return to the Strangelove Ocean?: Preliminary results of carbon and oxygenisotope compositions of post-impact sediments, IODP Expedition 364 "Chicxulub Impact Crater"

NASA Astrophysics Data System (ADS)

Yamaguchi, K. E.; Ikehara, M.; Hayama, H.; Takiguchi, S.; Masuda, S.; Ogura, C.; Fujita, S.; Kurihara, E.; Matsumoto, T.; Oshio, S.; Ishihata, K.; Fuchizawa, Y.; Noda, H.; Sakurai, U.; Yamane, T.; Morgan, J. V.; Gulick, S. P. S.

2017-12-01

The Chicxulub crater in the northern Yucatan Peninsula, Mexico was formed by the asteroid impact at the Cretaceous-Paleogene boundary (66.0 Ma). In early 2016 the IODP Exp. 364 successfully drilled the materials from the topographic peak ring within the crater that was previously identified by seismological observations. A continuous core was recovered. The 112m-thick uppermost part of the continuous core (505.7-1334.7 mbsf) is post-impact sediments, including the PETM, that are mainly composed of carbonate with intercalation of siliciclastics and variable contents of organic carbon. More than 300 samples from the post-impact section were finely powdered for a variety of geochemical analysis. Here we report their carbon and oxygen isotope compositions of the carbonate fraction (mostly in the lower part of the analyzed section) and carbon and nitrogen isotope compositions of organic matter (mostly in the middle-upper part of the analyzed section). Isotope mass spectrometer Isoprime was used for the former analysis, and EA-irMS (elemental analyzer - isotope ratio mass spectrometer) was used for the latter analysis, both at CMCR, Kochi Univ. Depth profile of oxygen isotope compositions of carbonate fraction is variable and somewhat similar to those of Zachos et al. (2001; Science). Carbon isotope compositions of carbonate and organic carbon in the lower part of the analyzed section exhibit some excursions that could correspond to the hyperthemals in the early Paleogene. Their variable nitrogen isotope compositions reflect temporal changes in the style of biogeochemical cycles involving denitrification and nitrogen fixation. Coupled temporal changes in the carbon isotope compositions of organic and carbonate carbon immediately after the K-Pg boundary might support a Strangelove ocean (Kump, 1991; Geology), however high export production (Ba/Ti, nannoplankton and calcisphere blooms, high planktic foram richness, and diverse and abundant micro- and macrobenthic organisms) at the base of the Danian limestone cored during Exp. 364 contradict a Strangelove Ocean.

Evidence of organic matter in the Ocean-Continent Transition of Alpine Tethys from Totalp, Eastern Swiss Alps

NASA Astrophysics Data System (ADS)

Mateeva, Tsvetomila; Kusznir, Nick; Wolff, George; Wheeler, John; Manatschal, Gianreto

2015-04-01

Evidence from ocean ridge drilling and dredging and from the exhumed Tethyan continental margin in the Alps demonstrates that mantle serpentinization occurs at slow-spreading ocean ridges and magma-poor rifted continental margins. Observations at white smokers suggest that methane produced by serpentinization can support methanotrophic bio-systems which use methane as their only source of carbon. An important question is whether such biosystems are more generally pervasive in their association with serpentinized mantle in the subsurface. The answer to this question has important global implications for the importance of the hidden sub-surface bio-systems, the fate of methane and the carbon cycle. We examine whether serpentinized exhumed mantle at magma-poor rifted continental margins shows evidence for methanotrophy. Fieldwork sampling of km scale exposure of orogenically exhumed serpentinized mantle in the eastern Swiss Alps allows 3D mantle sampling not possible at ocean ridges and has the potential to answer the question regarding localized versus pervasive sub-surface methanotrophic biosystems. The Totalp massif in the eastern Swiss Alps has been chosen for an initial study to investigate the presence or absence of methanotrophic biosystem within serpentinized exhumed mantle in the Tethyan OCT. Totalp has little Alpine deformation and its metamorphism is no more than prehnite-pumpellyite grade. Hands specimens and cores have been taken from the Totalp area in order to sample serpentinization and its lithological diversity in the search for presence or absence of biomarkers. Thin sections analysis reveals multiple serpentinization events. XRD analysis shows complete serpentinization of the olivines and orthopyroxenes. The samples for bio-geochemical analysis were cut and ground to powder, processed by soxhlet extraction and then analysed by GC and GCMS in order to determine the full range of biomarkers. Total carbon and total organic carbon was also determined for the samples. Samples collected from the Totalp area show evidence of organic hydrocarbon in the form of alkanes. The majority of the samples contain n-alkanes in the range C20 - C32. Some samples contain isoprenoids in different concentrations dependent on their lithology, for example pristane and phytane are found in Totalp's sediments. The organic molecular distribution is consistent with the temperature history of the basin. Totalp samples are characterized by TC contents of 0.03% to 12.90% and TOC contents of 0.10% to 1.90%. This large range of values correlates with the large lithological diversity of this area. These first results from Totalp showing evidence for preserved organic matter and biosystems in the serpentinized mantle of the ancient Tethyan OCT are encouraging. Much more work is required to understand whether the organic matter is generated from methane-driven biosystems, and if so whether the methane originated from an organic or inorganic source?

Composition and properties of the so-called 'diamond-like' amorphous carbon films

NASA Technical Reports Server (NTRS)

Angus, J. C.; Stultz, J. E.; Shiller, P. J.; Macdonald, J. R.; Mirtich, M. J.

1984-01-01

The composition of amorphous 'diamond-like' films made by direct low energy ion beam deposition, R.F. discharge and sputtering was determined by nuclear reaction analysis, IR spectroscopy and microcombustion chemical analysis. The nuclear reaction analysis showed very similar hydrogen depth profiles for all three types of samples. The atomic ratio of hydrogen to carbon was approximately 0.2 at the film surface and rose to approximately 1.0 at a depth of 500 A. The integrated intensity of the C-H stretching band at about 2900 per cm indicates that the amount of chemically bonded hydrogen is less than the total hydrogen content. Combustion analysis confirmed the overall atomic ratio of hydrogen to carbon determined by nuclear reaction analysis. The chemical state of the non-bonded hydrogen was not determined; however, the effective diffusion coefficient computed from the hydrogen depth profile was extremely low. This indicates either that the films are exceedingly impermeable or that the non-bonded hydrogen requires an additional activated step to leave the films, e.g., desorption or chemical reaction.

Improving Processing and Performance of Pure Lignin Carbon Fibers through Hardwood and Herbaceous Lignin Blends.

PubMed

Hosseinaei, Omid; Harper, David P; Bozell, Joseph J; Rials, Timothy G

2017-07-01

Lignin/lignin blends were used to improve fiber spinning, stabilization rates, and properties of lignin-based carbon fibers. Organosolv lignin from Alamo switchgrass ( Panicum virgatum ) and yellow poplar ( Liriodendron tulipifera ) were used as blends for making lignin-based carbon fibers. Different ratios of yellow poplar:switchgrass lignin blends were prepared (50:50, 75:25, and 85:15 w/w ). Chemical composition and thermal properties of lignin samples were determined. Thermal properties of lignins were analyzed using thermogravimetric analysis and differential scanning calorimetry. Thermal analysis confirmed switchgrass and yellow poplar lignin form miscible blends, as a single glass transition was observed. Lignin fibers were produced via melt-spinning by twin-screw extrusion. Lignin fibers were thermostabilized at different rates and subsequently carbonized. Spinnability of switchgrass lignin markedly improved by blending with yellow poplar lignin. On the other hand, switchgrass lignin significantly improved thermostabilization performance of yellow poplar fibers, preventing fusion of fibers during fast stabilization and improving mechanical properties of fibers. These results suggest a route towards a 100% renewable carbon fiber with significant decrease in production time and improved mechanical performance.

Improving Processing and Performance of Pure Lignin Carbon Fibers through Hardwood and Herbaceous Lignin Blends

PubMed Central

Hosseinaei, Omid; Bozell, Joseph J.; Rials, Timothy G.

2017-01-01

Lignin/lignin blends were used to improve fiber spinning, stabilization rates, and properties of lignin-based carbon fibers. Organosolv lignin from Alamo switchgrass (Panicum virgatum) and yellow poplar (Liriodendron tulipifera) were used as blends for making lignin-based carbon fibers. Different ratios of yellow poplar:switchgrass lignin blends were prepared (50:50, 75:25, and 85:15 w/w). Chemical composition and thermal properties of lignin samples were determined. Thermal properties of lignins were analyzed using thermogravimetric analysis and differential scanning calorimetry. Thermal analysis confirmed switchgrass and yellow poplar lignin form miscible blends, as a single glass transition was observed. Lignin fibers were produced via melt-spinning by twin-screw extrusion. Lignin fibers were thermostabilized at different rates and subsequently carbonized. Spinnability of switchgrass lignin markedly improved by blending with yellow poplar lignin. On the other hand, switchgrass lignin significantly improved thermostabilization performance of yellow poplar fibers, preventing fusion of fibers during fast stabilization and improving mechanical properties of fibers. These results suggest a route towards a 100% renewable carbon fiber with significant decrease in production time and improved mechanical performance. PMID:28671571

Dissolved organic carbon in the precipitation of Seoul, Korea: Implications for global wet depositional flux of fossil-fuel derived organic carbon

NASA Astrophysics Data System (ADS)

Yan, Ge; Kim, Guebuem

2012-11-01

Precipitation was sampled in Seoul over a one-year period from 2009 to 2010 to investigate the sources and fluxes of atmospheric dissolved organic carbon (DOC). The concentrations of DOC varied from 15 μM to 780 μM, with a volume-weighted average of 94 μM. On the basis of correlation analysis using the commonly acknowledged tracers, such as vanadium, the combustion of fossil-fuels was recognized to be the dominant source. With the aid of air mass backward trajectory analyses, we concluded that the primary fraction of DOC in our precipitation samples originated locally in Korea, albeit the frequent long-range transport from eastern and northeastern China might contribute substantially. In light of the relatively invariant organic carbon to sulfur mass ratios in precipitation over Seoul and other urban regions around the world, the global magnitude of wet depositional DOC originating from fossil-fuels was calculated to be 36 ± 10 Tg C yr-1. Our study further underscores the potentially significant environmental impacts that might be brought about by this anthropogenically derived component of organic carbon in the atmosphere.

Analysis of the production and transaction costs of forest carbon offset projects in the USA.

PubMed

Galik, Christopher S; Cooley, David M; Baker, Justin S

2012-12-15

Forest carbon offset project implementation costs, comprised of both production and transaction costs, could present an important barrier to private landowner participation in carbon offset markets. These costs likewise represent a largely undocumented component of forest carbon offset potential. Using a custom spreadsheet model and accounting tool, this study examines the implementation costs of different forest offset project types operating in different forest types under different accounting and sampling methodologies. Sensitivity results are summarized concisely through response surface regression analysis to illustrate the relative effect of project-specific variables on total implementation costs. Results suggest that transaction costs may represent a relatively small percentage of total project implementation costs - generally less than 25% of the total. Results also show that carbon accounting methods, specifically the method used to establish project baseline, may be among the most important factors in driving implementation costs on a per-ton-of-carbon-sequestered basis, dramatically increasing variability in both transaction and production costs. This suggests that accounting could be a large driver in the financial viability of forest offset projects, with transaction costs likely being of largest concern to those projects at the margin. Copyright © 2012 Elsevier Ltd. All rights reserved.

Dynamic behaviour of river colloidal and dissolved organic matter through cross-flow ultrafiltration system.

PubMed

Wilding, Andrew; Liu, Ruixia; Zhou, John L

2005-07-01

Through cross-flow filtration (CFF) with a 1-kDa regenerated cellulose Pellicon 2 module, the ultrafiltration characteristics of river organic matter from Longford Stream, UK, were investigated. The concentration of organic carbon (OC) in the retentate in the Longford Stream samples increased substantially with the concentration factor (cf), reaching approximately 40 mg/L at cf 15. The results of dissolved organic carbon (DOC) and colloidal organic carbon (COC) analysis, tracking the isolation of colloids from river waters, show that 2 mg/L of COC was present in those samples and good OC mass balance (77-101%) was achieved. Fluorescence measurements were carried out for the investigation of retentate and permeate behaviour of coloured dissolved organic materials (CDOM). The concentrations of CDOM in both the retentate and permeate increased with increasing cf, although CDOM were significantly more concentrated in the retentate. The permeation model expressing the correlation between log[CDOM] in the permeate and logcf was able to describe the permeation behaviour of CDOM in the river water with regression coefficients (r(2)) of 0.94 and 0.98. Dry weight analysis indicated that the levels of organic colloidal particles were from 49 to 71%, and between 29 and 51% of colloidal particles present were inorganic. COC as a percentage of DOC was found to be 10-16% for Longford Stream samples.

Water-quality data for water- and wastewater-treatment plants along the Red River of the North, North Dakota and Minnesota, January through October 2006

USGS Publications Warehouse

Damschen, William C.; Hansel, John A.; Nustad, Rochelle A.

2008-01-01

From January through October 2006, six sets of water-quality samples were collected at 28 sites, which included inflow and outflow from seven major municipal water-treatment plants (14 sites) and influent and effluent samples from seven major municipal wastewater treatment plants (14 sites) along the Red River of the North in North Dakota and Minnesota. Samples were collected in cooperation with the Bureau of Reclamation for use in the development of return-flow boundary conditions in a 2006 water-quality model for the Red River of the North. All samples were analyzed for nutrients and major ions. For one set of effluent samples from each of the wastewater-treatment plants, water was analyzed for Eschirichia coli, fecal coliform, 20-day biochemical oxygen demand, 20-day nitrogenous biochemical oxygen demand, total organic carbon, and dissolved organic carbon. In general, results from the field equipment blank and replicate samples indicate that the overall process of sample collection, processing, and analysis did not introduce substantial contamination and that consistent results were obtained.

The variation in surface morphology and hardness of human deciduous teeth samples after laser irradiation

NASA Astrophysics Data System (ADS)

Khalid, Arooj; Bashir, Shazia; Akram, Mahreen; Salman Ahmed, Qazi

2017-11-01

The variation in surface morphology and hardness of human deciduous teeth samples has been investigated after laser irradiation at different wavelengths and energies. Nd:YAG was employed as a source of irradiation for IR (1064 nm) and visible (532 nm) radiation, whereas an excimer laser was used as the source of UV (248 nm) radiation. Scanning electron microscope (SEM) analysis was carried out to reveal the surface morphological evolution of teeth samples. Vickers microhardness tester was employed to investigate the modifications in the hardness of the laser-treated samples. It is observed from SEM analysis that IR wavelength is responsible for ablation of collagen matrix and intertubular dentine. For visible radiation, the ablation of collagen along with hydroxypatite is observed. With UV radiation, the ablation of peritubular dentine is dominant and is responsible for the sealing of tubules. The decrease in hardness at lower energy for both wavelengths is due to the evaporation of carbon content. With increasing energy, evaporation of water along with carbon content, and resolidification and re-organization of inorganic content causes the increase in hardness of the treated dentine. SEM as well as microhardness analyses reveal that laser wavelengths and energy of laser radiation significantly influence the surface morphology and hardness of samples.

New tool for getting data on the field for paleoclimate and paleoceanography data based on isotope 13C and 18O measurements

NASA Astrophysics Data System (ADS)

Mandic, M.; Stöbener, N.; Smajgl, D.

2017-12-01

For many decades different instrumental methods involving generations of the isotope ratio mass spectrometers with different periphery units for sample preparation, have provided scientifically required high precision, and high throughput of samples for varies application - from geological and hydrological to food and forensic. With this work we introduce automated measurement of δ13C and δ18O from solid carbonate samples, DIC and δ18O of water. We have demonstrated usage of a Thermo Scientific™ Delta Ray™ IRIS with URI Connect on certified reference materials and confirmed the high achievable accuracy and a precision better then <0.1‰ for both δ13C and δ18O, in the laboratory or the field with same precision and throughput of samples. With equilibration method for determination of δ18O in water samples, which we present in this work, achieved repeatability and accuracy are 0.12‰ and 0.68‰ respectively, which fulfill requirements of regulatory methods. The preparation of the samples for carbonate and DIC analysis on the Delta Ray IRIS with URI Connect is similar to the previously mentioned Gas Bench II methods. Samples are put into vials and phosphoric acid is added. The resulting sample-acid chemical reaction releases CO2 gas, which is then introduced into the Delta Ray IRIS via the Variable Volume. Three international standards of carbonate materials (NBS-18, NBS-19 and IAEA-CO-1) were analyzed. NBS-18 and NBS-19 were used as standards for calibration, and IAEA-CO-1 was treated as unknown. For water sample analysis equilibration method with 1% of CO2 in dry air was used. Test measurements and conformation of precision and accuracy of method determination δ18O in water samples were done with three lab standards, namely ANST, OCEAN 2 and HBW. All laboratory standards were previously calibrated with international reference material VSMOW2 and SLAP2 to assure accuracy of the isotopic values. The Principle of Identical Treatment was applied in sample and standard preparation, in measurement procedure, as well as in the evaluation of the results.

Preparation of water samples for carbon-14 dating

USGS Publications Warehouse

Feltz, H.R.; Hanshaw, Bruce B.

1963-01-01

For most natural water, a large sample is required to provide the 3 grams of carbon needed for a carbon-14 determination. A field procedure for isolating total dissolved-carbonate species is described. Carbon dioxide gas is evolved by adding sulfuric acid to the water sample; the gas is then collected in a sodium hydroxide trap by recycling in a closed system. The trap is then transported to the dating laboratory where the carbon-14 is counted.

Effects of mining activities on evolution of water chemistry in coal-bearing aquifers in karst region of Midwestern Guizhou, China: evidences from δ13C of dissolved inorganic carbon and δ34S of sulfate.

PubMed

Li, Qingguang; Wu, Pan; Zha, Xuefang; Li, Xuexian; Wu, Linna; Gu, Shangyi

2018-04-24

The generation of acid mine drainage (AMD) may accelerate watershed erosion and promote the migration of heavy metals, then threaten local ecosystems such as aquatic life and even human health. Previous studies have focused primarily on influence of AMD in surface environment. In order to reveal the acidizing processes in karst high-sulfur coalfield in Southwest China, this study, by contrast, focused on the hydrogeochemical evolution process and acidification mechanism of mine water in Zhijin coalfield, western Guizhou Province. The oxidation of pyrite and other sulfides induced strong acidification of mine water according to the water chemical analysis. As a result, a series of geochemical processes such as dissolution of carbonates and silicates, hydrolysis of metal ions, and degassing of CO 2 complicated water chemical evolution. The dissolution of silicates controlled the chemical composition of mine water, but more carbonates might be dissolved during the acidification of mine water. The sources of sulfate are quite different in water samples collected from the two selected mine. According to sulfur isotope analysis, the dissolution of gypsum is the primary source of sulfate in samples from Hongfa mine, whereas sulfide oxidation contributed a large amount of sulfate to the mine water in Fenghuangshan mine. The dissolution of carbonates should be an important source of DIC in mine water and CO 2 originating from organic mineralization might also have a certain contribution. This study elucidated the groundwater chemical evolution processes in high-sulfur coal-bearing strata and provided a foundation for further study of carbonates erosion and carbon emission during acidification of mine water.

Synthesis of carbon nanostructures from high density polyethylene (HDPE) and polyethylene terephthalate (PET) waste by chemical vapour deposition

NASA Astrophysics Data System (ADS)

Hatta, M. N. M.; Hashim, M. S.; Hussin, R.; Aida, S.; Kamdi, Z.; Ainuddin, AR; Yunos, MZ

2017-10-01

In this study, carbon nanostructures were synthesized from High Density Polyethylene (HDPE) and Polyethylene terephthalate (PET) waste by single-stage chemical vapour deposition (CVD) method. In CVD, iron was used as catalyst and pyrolitic of carbon source was conducted at temperature 700, 800 and 900°C for 30 minutes. Argon gas was used as carrier gas with flow at 90 sccm. The synthesized carbon nanostructures were characterized by FESEM, EDS and calculation of carbon yield (%). FESEM micrograph shows that the carbon nanostructures were only grown as nanofilament when synthesized from PET waste. The synthesization of carbon nanostructure at 700°C was produced smooth and the smallest diameter nanofilament compared to others. The carbon yield of synthesized carbon nanostructures from PET was lower from HDPE. Furthermore, the carbon yield is recorded to increase with increasing of reaction temperature for all samples. Elemental study by EDS analysis were carried out and the formation of carbon nanostructures was confirmed after CVD process. Utilization of polymer waste to produce carbon nanostructures is beneficial to ensure that the carbon nanotechnology will be sustained in future.

Fluorination of vertically aligned carbon nanotubes: from CF4 plasma chemistry to surface functionalization.

PubMed

Struzzi, Claudia; Scardamaglia, Mattia; Colomer, Jean-François; Verdini, Alberto; Floreano, Luca; Snyders, Rony; Bittencourt, Carla

2017-01-01

The surface chemistry of plasma fluorinated vertically aligned carbon nanotubes (vCNT) is correlated to the CF 4 plasma chemical composition. The results obtained via FTIR and mass spectrometry are combined with the XPS and Raman analysis of the sample surface showing the dependence on different plasma parameters (power, time and distance from the plasma region) on the resulting fluorination. Photoemission and absorption spectroscopies are used to investigate the evolution of the electronic properties as a function of the fluorine content at the vCNT surface. The samples suffer a limited ageing effect, with a small loss of fluorine functionalities after two weeks in ambient conditions.

Synthesis of copper coated carbon nanotubes for aluminium matrix composites

NASA Astrophysics Data System (ADS)

Maqbool, Adnan; Khalid, F. Ahmad; Hussain, M. Asif; Bakhsh, Nabi

2014-06-01

In this investigation copper coated carbon nanotubes (CNTs) were prepared to enhance the interfacial bonding between CNTs and aluminum matrix by the molecular-level mixing process. In optimized plating bath of (1:1) by wt. CNT with Cu, thickness of coated CNTs is reduced to 100 nm to promote uniform distribution of Cu nanoparticle on the surface of pretreated CNTs. The mixing of CNTs was accomplished by ultrasonication and ball milling. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in nanocomposites samples compared to the uncoated CNTs. The samples were pressureless sintered under vacuum. The densification increased with the increase in the CNTs content and is more pronounced in Cu-coated CNT nanocomposites.

Fluorination of vertically aligned carbon nanotubes: from CF4 plasma chemistry to surface functionalization

PubMed Central

Scardamaglia, Mattia; Colomer, Jean-François; Verdini, Alberto; Floreano, Luca; Snyders, Rony; Bittencourt, Carla

2017-01-01

The surface chemistry of plasma fluorinated vertically aligned carbon nanotubes (vCNT) is correlated to the CF4 plasma chemical composition. The results obtained via FTIR and mass spectrometry are combined with the XPS and Raman analysis of the sample surface showing the dependence on different plasma parameters (power, time and distance from the plasma region) on the resulting fluorination. Photoemission and absorption spectroscopies are used to investigate the evolution of the electronic properties as a function of the fluorine content at the vCNT surface. The samples suffer a limited ageing effect, with a small loss of fluorine functionalities after two weeks in ambient conditions. PMID:28904833

Detection of Multi-walled Carbon Nanotubes and Carbon Nanodiscs on Workplace Surfaces at a Small-Scale Producer.

PubMed

Hedmer, Maria; Ludvigsson, Linus; Isaxon, Christina; Nilsson, Patrik T; Skaug, Vidar; Bohgard, Mats; Pagels, Joakim H; Messing, Maria E; Tinnerberg, Håkan

2015-08-01

The industrial use of novel-manufactured nanomaterials such as carbon nanotubes and carbon nanodiscs is increasing globally. Occupational exposure can occur during production, downstream use, and disposal. The health effects of many nanomaterials are not yet fully characterized and to handle nano-objects, their aggregates and agglomerates >100nm (NOAA), a high degree of control measures and personal protective equipment are required. The emission of airborne NOAA during production and handling can contaminate workplace surfaces with dust, which can be resuspended resulting in secondary inhalation exposures and dermal exposures. This study surveys the presence of carbon-based nanomaterials, such as multi-walled carbon nanotubes (MWCNTs) and carbon nanodiscs, as surface contamination at a small-scale producer using a novel tape sampling method. Eighteen different surfaces at a small-scale producer were sampled with an adhesive tape sampling method. The surfaces selected were associated with the production and handling of MWCNT powder in the near-field zone. Surfaces in the far-field zone were also sampled. In addition, tape stripping of the skin was performed on one worker. The tape samples were analysed with scanning electron microscopy to detect the carbon-based NOAA. Air sampling with a personal impactor was also performed on a worker who was producing MWCNTs the same day as the tape samples were collected. MWCNTs were detected in 50% of the collected tape samples and carbon nanodiscs in 17%. MWCNTs and carbon nanodiscs were identified in all parts of the workplace, thus, increasing the risk for secondary inhalation and dermal exposure of the workers. Both airborne MWCNTs and carbon nanodiscs were detected in the personal impactor samples. The tape-strip samples from the worker showed no presence of carbon-containing nanoparticles. Tape sampling is a functional method for detecting surface contamination of carbon-based NOAA and for exposure control during production at potentially any workplace that produces or handles such manufactured nanomaterials. With the tape method, it is possible to monitor if a potential for secondary inhalation exposure or dermal exposure exists through resuspension of dust deposited on workplace surfaces. By means of air sampling, we could confirm that carbon nanodiscs were resuspended into the air at the workplace even though they were not handled during that particular work shift. MWCNTs were detected in the air samples, but can have been derived from either resuspension or from the work tasks with MWCNTs that were performed during the air sampling. Tape sampling is a complementary method to air sampling and together these two methods provide a better view of the hygienic situation in workplaces where NOAA can be emitted into work environments. © The Author 2015. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

Direct synthesis of nitrogen-containing carbon nanotubes on carbon paper for fuel cell electrode

NASA Astrophysics Data System (ADS)

Yin, Wong Wai; Daud, Wan Ramli Wan; Mohamad, Abu Bakar; Kadhum, Abdul Amir Hassan; Majlan, Edy Herianto; Shyuan, Loh Kee

2012-06-01

Organic catalyst has recently been identified as the potential substitution for expensive platinum electrocatalyst for fuel cell application. Numerous studies have shown that the nitrogen-containing carbon nanotubes (N-CNT) can be synthesized through spray pyrolysis or floating chemical vapor deposition (CVD) technique using various type of organometallic as precursors. This paper presents the method of synthesis and the initial findings of the growth of N-CNT directly on carbon paper using a modified CVD technique. In this research, nickel (II) phthalocyanines (Ni-Pc) as precursor was dissolved in ethanol solvent, stirred and sonicated to become homogenized. The solution was poured into a bubbler and heated up to allow the mixture to vaporize. Subsequently, the solution vapor was flowed into the tubical reactor maintained at 900°C. Carbon paper sputtered with nickel nanoparticles was used as the substrate. The synthesized sample was examined through Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM) and Fourier Transform Infra-Red (FTIR). Long, entangled and compartmentalized nanotubes with tube diameter ranging 23-27 nm were found covered the carbon paper surface with approximate of 5.5-6.0 μm in thickness. EDX analysis has successfully showed the presence of nitrogen in the carbon nanotube. FTIR analysis showed the presence of the C-N bond on CNT.

Carbon Abundances in Starburst Galaxies of the Local Universe

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

Peña-Guerrero, María A.; Leitherer, Claus; Mink, Selma de

The cosmological origin of carbon, the fourth most abundant element in the universe, is not well known and a matter of heavy debate. We investigate the behavior of C/O to O/H in order to constrain the production mechanism of carbon. We measured emission-line intensities in the spectral range from 1600 to 10000 Å on Space Telescope Imaging Spectrograph (STIS) long-slit spectra of 18 starburst galaxies in the local universe. We determined chemical abundances through traditional nebular analysis, and we used a Markov Chain Monte Carlo method to determine where our carbon and oxygen abundances lie in the parameter space. Wemore » conclude that our C and O abundance measurements are sensible. We analyzed the behavior of our sample in the [C/O] versus [O/H] diagram with respect to other objects such as DLAs, neutral ISM measurements, and disk and halo stars, finding that each type of object seems to be located in a specific region of the diagram. Our sample shows a steeper C/O versus O/H slope with respect to other samples, suggesting that massive stars contribute more to the production of C than N at higher metallicities, only for objects where massive stars are numerous; otherwise, intermediate-mass stars dominate the C and N production.« less

Carbonate Chemistry and Isotope Characteristics of Groundwater of Ljubljansko Polje and Ljubljansko Barje Aquifers in Slovenia

PubMed Central

2013-01-01

Ljubljansko polje and Ljubljansko Barje aquifers are the main groundwater resources for the needs of Ljubljana, the capital of Slovenia. Carbonate chemistry and isotope analysis of the groundwater were performed to acquire new hydrogeological data, which should serve as a base for improvement of hydrogeological conceptual models of both aquifers. A total of 138 groundwater samples were collected at 69 sampling locations from both aquifers. Major carbonate ions and the stable isotope of oxygen were used to identify differences in the recharging areas of aquifers. Four groups of groundwater were identified: (1) Ljubljansko polje aquifer, with higher Ca2+values, as limestone predominates in its recharge area, (2) northern part of Ljubljansko Barje aquifer, with prevailing dolomite in its recharge area, (3) central part of Ljubljansko Barje aquifer, which lies below surface cover of impermeable clay and is poor in carbonate, and (4) Brest and Iški vršaj aquifer in the southern part of Ljubljansko Barje with higher Mg2+ in groundwater and dolomite prevailing in its recharge area. The radioactive isotope tritium was also used to estimate the age of groundwater. Sampled groundwater is recent with tritium activity between 4 and 8 TU and residence time of up to 10 years. PMID:24453928

Carbon Abundances in Starburst Galaxies of the Local Universe

NASA Astrophysics Data System (ADS)

Peña-Guerrero, María A.; Leitherer, Claus; de Mink, Selma; Wofford, Aida; Kewley, Lisa

2017-10-01

The cosmological origin of carbon, the fourth most abundant element in the universe, is not well known and a matter of heavy debate. We investigate the behavior of C/O to O/H in order to constrain the production mechanism of carbon. We measured emission-line intensities in the spectral range from 1600 to 10000 Å on Space Telescope Imaging Spectrograph (STIS) long-slit spectra of 18 starburst galaxies in the local universe. We determined chemical abundances through traditional nebular analysis, and we used a Markov Chain Monte Carlo method to determine where our carbon and oxygen abundances lie in the parameter space. We conclude that our C and O abundance measurements are sensible. We analyzed the behavior of our sample in the [C/O] versus [O/H] diagram with respect to other objects such as DLAs, neutral ISM measurements, and disk and halo stars, finding that each type of object seems to be located in a specific region of the diagram. Our sample shows a steeper C/O versus O/H slope with respect to other samples, suggesting that massive stars contribute more to the production of C than N at higher metallicities, only for objects where massive stars are numerous; otherwise, intermediate-mass stars dominate the C and N production.

Post-Mortem Identification of a Fire Carbonized Body by STR Genotyping.

PubMed

Dumache, Raluca; Muresan, Camelia; Ciocan, Veronica; Rogobete, Alexandru F; Enache, Alexandra

2016-10-01

Identification of bodies of unknown identity that are victims of exposure to very high temperatures, resulting from fires, plane crashes, and terrorist attacks, represents one of the most difficult sides of forensic genetics, because of the advanced state of decomposition. The aim of this study was the identification of the carbonized cadaver of a fire victim through STR genotyping. We used blood samples obtained from the iliac artery during the autopsy examination as biological samples from the unidentified victim. After DNA isolation and quantification, we proceeded to its amplification using the multiplex PCR kit AmpFlSTR Identifiler. The DNA products were separated using an ABI 3500 genetic analyzer. Further analysis of the data was done using Gene Mapper ID-X version 1.4 software. In this case, it was possible to obtain a complete DNA profile from the biological samples. Due to the fact that the amelogenin gene presented two alleles, X and Y, we concluded that the victim was a man. We conclude that STR profiling of unidentified bodies (carbonized, decomposed) represents a powerful method of human identification in forensic medicine.

Magnetic porous carbon derived from a bimetallic metal-organic framework for magnetic solid-phase extraction of organochlorine pesticides from drinking and environmental water samples.

PubMed

Liu, Yaxi; Gao, Zongjun; Wu, Ri; Wang, Zhenhua; Chen, Xiangfeng; Chan, T-W Dominic

2017-01-06

In this work, magnetic porous carbon material derived from a bimetallic metal-organic framework was explored as an adsorbent for magnetic solid-phase extraction of organochlorine pesticides (OCPs). The synthesized porous carbon possessed a high specific surface area and magnetization saturation. The OCPs in the samples were quantified using gas chromatography coupled with a triple quadrupole mass spectrometer. The experimental parameters, including the desorption solvent and conditions, amount of adsorbent, extraction time, extraction temperature, and ionic strength of the solution, were optimized. Under optimal conditions, the developed method displayed good linearity (r>0.99) within the concentration range of 2-500ngL -1 . Low limits of detection (0.39-0.70ngL -1 , signal-to-noise ratio=3:1) and limits of quantification (1.45-2.0ngL -1 , signal-to-noise ratio=10:1) as well as good precision (relative standard deviation<10%) were also obtained. The developed method was applied in the analysis of OCPs in drinking and environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Deep soil carbon dynamics are driven more by soil type than by climate: a worldwide meta-analysis of radiocarbon profiles.

PubMed

Mathieu, Jordane A; Hatté, Christine; Balesdent, Jérôme; Parent, Éric

2015-11-01

The response of soil carbon dynamics to climate and land-use change will affect both the future climate and the quality of ecosystems. Deep soil carbon (>20 cm) is the primary component of the soil carbon pool, but the dynamics of deep soil carbon remain poorly understood. Therefore, radiocarbon activity (Δ14C), which is a function of the age of carbon, may help to understand the rates of soil carbon biodegradation and stabilization. We analyzed the published 14C contents in 122 profiles of mineral soil that were well distributed in most of the large world biomes, except for the boreal zone. With a multivariate extension of a linear mixed-effects model whose inference was based on the parallel combination of two algorithms, the expectation-maximization (EM) and the Metropolis-Hasting algorithms, we expressed soil Δ14C profiles as a four-parameter function of depth. The four-parameter model produced insightful predictions of soil Δ14C as dependent on depth, soil type, climate, vegetation, land-use and date of sampling (R2=0.68). Further analysis with the model showed that the age of topsoil carbon was primarily affected by climate and cultivation. By contrast, the age of deep soil carbon was affected more by soil taxa than by climate and thus illustrated the strong dependence of soil carbon dynamics on other pedologic traits such as clay content and mineralogy. © 2015 John Wiley & Sons Ltd.

Chemical analysis of water samples and geophysical logs from cored test holes drilled in the central Oklahoma Aquifer, Oklahoma

USGS Publications Warehouse

Schlottmann, Jamie L.; Funkhouser, Ron A.

1991-01-01

Chemical analyses of water from eight test holes and geophysical logs for nine test holes drilled in the Central Oklahoma aquifer are presented. The test holes were drilled to investigate local occurrences of potentially toxic, naturally occurring trace substances in ground water. These trace substances include arsenic, chromium, selenium, residual alpha-particle activities, and uranium. Eight of the nine test holes were drilled near wells known to contain large concentrations of one or more of the naturally occurring trace substances. One test hole was drilled in an area known to have only small concentrations of any of the naturally occurring trace substances.Water samples were collected from one to eight individual sandstone layers within each test hole. A total of 28 water samples, including four duplicate samples, were collected. The temperature, pH, specific conductance, alkalinity, and dissolved-oxygen concentrations were measured at the sample site. Laboratory determinations included major ions, nutrients, dissolved organic carbon, and trace elements (aluminum, arsenic, barium, beryllium, boron, cadmium, chromium, hexavalent chromium, cobalt, copper, iron, lead, lithium, manganese, mercury, molybdenum, nickel, selenium, silver, strontium, vanadium and zinc). Radionuclide activities and stable isotope (5 values also were determined, including: gross-alpha-particle activity, gross-beta-particle activity, radium-226, radium-228, radon-222, uranium-234, uranium-235, uranium-238, total uranium, carbon-13/carbon-12, deuterium/hydrogen-1, oxygen-18/oxygen-16, and sulfur-34/sulfur-32. Additional analyses of arsenic and selenium species are presented for selected samples as well as analyses of density and iodine for two samples, tritium for three samples, and carbon-14 for one sample.Geophysical logs for most test holes include caliper, neutron, gamma-gamma, natural-gamma logs, spontaneous potential, long- and short-normal resistivity, and single-point resistance. Logs for test-hole NOTS 7 do not include long- and short-normal resistivity, spontaneous-potential, or single-point resistivity. Logs for test-hole NOTS 7A include only caliper and natural-gamma logs.

Comparison and evaluation of in situ and filter carbon measurements at the Fresno Supersite

NASA Astrophysics Data System (ADS)

Watson, John G.; Chow, Judith C.

2002-11-01

The Fresno Supersite in Fresno, California, USA, acquires in situ 5- to 60-min average PM2.5 organic carbon (OC), elemental carbon (EC), and total carbon (TC) measurements by the following methods: (1) thermal evolution carbon analyzer for organic, elemental, and total carbon; (2) single-wavelength and seven-color aethalometer for black carbon (BC); and (3) photoionization for particle-bound polycyclic aromatic hydrocarbons. Twenty-four-hour average PM2.5 filter-based measurements include (1) nondenuded quartz filters with no backup filter in a PM2.5 Federal Reference Method (FRM) sampler; (2) quartz filters behind an organic carbon denuder with a quartz backup filter in a Reference Ambient Aerosol Sampler (RAAS); (3) nondenuded quartz filters with backup filter in a RAAS; and (4) nondenuded quartz filters with no backup filter in a sequential filter sampler. Filter samples are analyzed after sampling by the Interagency Monitoring of Protected Visual Environments (IMPROVE) thermal/optical reflectance carbon analysis protocol. Collocated measurements are examined for year 2000. Measurement equivalence is found for PM2.5 mass, light transmission, and TC between the FRM and RAAS speciation samplers. The average ratios of front filter carbon between the denuded and nondenuded channels in the RAAS sampler are 0.83 ± 0.19 for TC, 0.81 ± 0.20 for OC, and 1.01 ± 0.33 for EC. The average differences for TC and OC are low (1.2 to 1.4 μg m-3) and are comparable to the measurement uncertainties. Continuous thermal evolution carbon measurements are not comparable to filter measurements. Aethalometer BC and filter EC are highly correlated, but filter EC is consistently 20-25% higher than continuous aethalometer BC. Pairwise comparisons show filter EC measurements acquired in this study are predictable from aethalometer BC measurements.

[Ultra-Fine Pressed Powder Pellet Sample Preparation XRF Determination of Multi-Elements and Carbon Dioxide in Carbonate].

PubMed

Li, Xiao-li; An, Shu-qing; Xu, Tie-min; Liu, Yi-bo; Zhang, Li-juan; Zeng, Jiang-ping; Wang, Na

2015-06-01

The main analysis error of pressed powder pellet of carbonate comes from particle-size effect and mineral effect. So in the article in order to eliminate the particle-size effect, the ultrafine pressed powder pellet sample preparation is used to the determination of multi-elements and carbon-dioxide in carbonate. To prepare the ultrafine powder the FRITSCH planetary Micro Mill machine and tungsten carbide media is utilized. To conquer the conglomeration during the process of grinding, the wet grinding is preferred. The surface morphology of the pellet is more smooth and neat, the Compton scatter effect is reduced with the decrease in particle size. The intensity of the spectral line is varied with the change of the particle size, generally the intensity of the spectral line is increased with the decrease in the particle size. But when the particle size of more than one component of the material is decreased, the intensity of the spectral line may increase for S, Si, Mg, or decrease for Ca, Al, Ti, K, which depend on the respective mass absorption coefficient . The change of the composition of the phase with milling is also researched. The incident depth of respective element is given from theoretical calculation. When the sample is grounded to the particle size of less than the penetration depth of all the analyte, the effect of the particle size on the intensity of the spectral line is much reduced. In the experiment, when grounded the sample to less than 8 μm(d95), the particle-size effect is much eliminated, with the correction method of theoretical α coefficient and the empirical coefficient, 14 major, minor and trace element in the carbonate can be determined accurately. And the precision of the method is much improved with RSD < 2%, except Na2O. Carbon is ultra-light element, the fluorescence yield is low and the interference is serious. With the manual multi-layer crystal PX4, coarse collimator, empirical correction, X-ray spectrometer can be used to determine the carbon dioxide in the carbonate quantitatively. The intensity of the carbon is increase with the times of the measurement and the time delay even the pellet is stored in the dessicator. So employing the latest pressed powder pellet is suggested.

Measurement of carbon storage in landfills from the biogenic carbon content of excavated waste samples.

PubMed

De la Cruz, Florentino B; Chanton, Jeffrey P; Barlaz, Morton A

2013-10-01

Landfills are an anaerobic ecosystem and represent the major disposal alternative for municipal solid waste (MSW) in the U.S. While some fraction of the biogenic carbon, primarily cellulose (Cel) and hemicellulose (H), is converted to carbon dioxide and methane, lignin (L) is essentially recalcitrant. The biogenic carbon that is not mineralized is stored within the landfill. This carbon storage represents a significant component of a landfill carbon balance. The fraction of biogenic carbon that is not reactive in the landfill environment and therefore stored was derived for samples of excavated waste by measurement of the total organic carbon, its biogenic fraction, and the remaining methane potential. The average biogenic carbon content of the excavated samples was 64.6±18.0% (average±standard deviation), while the average carbon storage factor was 0.09±0.06g biogenic-C stored per g dry sample or 0.66±0.16g biogenic-C stored per g biogenic C. Published by Elsevier Ltd.