scholarly journals Isotopic fractionation of N<sub>2</sub>O to quantify N<sub>2</sub>O reduction to N<sub>2</sub> – validation with Helium incubation and <sup>15</sup>N gas flux methods

2016 ◽  
Author(s):  
Dominika Lewicka-Szczebak ◽  
Jürgen Augustin ◽  
Anette Giesemann ◽  
Reinhard Well
Keyword(s):  
Isotopic Fractionation ◽  
Isotopic Signature ◽  
Residual Fraction ◽  
Simultaneous Estimation ◽  
Site Preference ◽  
Isotopic Enrichment ◽  
Gas Flux ◽  
Isotopic Signatures ◽  
Isotopic Analyses

Abstract. Stable isotopic analyses of soil-emitted N2O (δ15Nbulk, δ18O and δ15Nsp = 15N site preference within the linear N2O molecule) may help to quantify N2O reduction to N2, a main unknown magnitude in the soil nitrogen cycling. The N2O residual fraction (rN2O) can be theoretically calculated from the measured isotopic enrichment of the residual N2O. However, various N2O producing pathways may also influence the N2O isotopic signatures, and hence complicate the application of this isotopic fractionation approach. Here this approach was tested based on laboratory soil incubations with two different soil types applying two reference methods for quantification of rN2O: Helium incubation with direct measurement of N2 flux and the 15N gas flux method. This allowed a comparison of the measured rN2O values with the ones calculated based on isotopic enrichment of residual N2O. The results indicate that the performance of the N2O isotopic fractionation approach is related with the accompanying N2O and N2 source processes and the most critical is the determination of the initial isotopic signature of N2O before reduction (δ0). We show that δ0 can be well experimentally determined if stable in time and successfully applied for determination of rN2O based on δ15Nsp values. Much more problematic is to deal with temporal changes of δ0 values leading to failure of the approach based on δ15Nsp values only. For this case we propose here a dual N2O isotopocule mapping approach, where calculations are based on the relation between δ18O and δ15Nsp values. This allows for the simultaneous estimation of the N2O producing pathways contribution and the rN2O value.

scholarly journals Quantifying N<sub>2</sub>O reduction to N<sub>2</sub> based on N<sub>2</sub>O isotopocules – validation with independent methods (helium incubation and <sup>15</sup>N gas flux method)

2017 ◽  
Vol 14 (3) ◽  
pp. 711-732 ◽  
Author(s):  
Dominika Lewicka-Szczebak ◽  
Jürgen Augustin ◽  
Anette Giesemann ◽  
Reinhard Well
Keyword(s):  
Isotopic Fractionation ◽  
Isotopic Signature ◽  
Residual Fraction ◽  
Simultaneous Estimation ◽  
Site Preference ◽  
Isotopic Enrichment ◽  
Flux Method ◽  
Gas Flux ◽  
Isotopic Analyses

Abstract. Stable isotopic analyses of soil-emitted N2O (δ15Nbulk, δ18O and δ15Nsp = 15N site preference within the linear N2O molecule) may help to quantify N2O reduction to N2, an important but rarely quantified process in the soil nitrogen cycle. The N2O residual fraction (remaining unreduced N2O, rN2O) can be theoretically calculated from the measured isotopic enrichment of the residual N2O. However, various N2O-producing pathways may also influence the N2O isotopic signatures, and hence complicate the application of this isotopic fractionation approach. Here this approach was tested based on laboratory soil incubations with two different soil types, applying two reference methods for quantification of rN2O: helium incubation with direct measurement of N2 flux and the 15N gas flux method. This allowed a comparison of the measured rN2O values with the ones calculated based on isotopic enrichment of residual N2O. The results indicate that the performance of the N2O isotopic fractionation approach is related to the accompanying N2O and N2 source processes and the most critical is the determination of the initial isotopic signature of N2O before reduction (δ0). We show that δ0 can be well determined experimentally if stable in time and then successfully applied for determination of rN2O based on δ15Nsp values. Much more problematic to deal with are temporal changes of δ0 values leading to failure of the approach based on δ15Nsp values only. For this case, we propose here a dual N2O isotopocule mapping approach, where calculations are based on the relation between δ18O and δ15Nsp values. This allows for the simultaneous estimation of the N2O-producing pathways' contribution and the rN2O value.

scholarly journals N<sub>2</sub>O isotope approaches for source partitioning of N<sub>2</sub>O production and estimation of N<sub>2</sub>O reduction – validation with <sup>15</sup>N gas-flux method in laboratory and field studies

2020 ◽  
Author(s):  
Dominika Lewicka-Szczebak ◽  
Maciej Piotr Lewicki ◽  
Reinhard Well
Keyword(s):  
Three Dimensional ◽  
Field Studies ◽  
Residual Fraction ◽  
N2o Reduction ◽  
Flux Method ◽  
Gas Flux ◽  
Dual Isotope ◽  
Isotopic Signatures ◽  
First Time

Abstract. The approaches based on natural abundance N2O stable isotopes are often applied for the estimation of mixing proportions between various N2O producing pathways as well as for estimation of the extent of N2O reduction to N2. But such applications are associated with numerous uncertainties and hence their limited accuracy needs to be considered. Here we present the first systematic validation of these methods for laboratory and field studies applying the 15N gas-flux method as the reference approach. Besides applying dual isotope plots for interpretation of N2O isotopic data, for the first time we propose a three dimensional N2O isotopocule model based on Bayesian statistics to estimate the N2O mixing proportions and reduction extent based simultaneously on three N2O isotopic signatures (δ15N, δ15NSP and δ18O). Determination of mixing proportions of individual pathways with N2O isotopic approaches appears often imprecise, mainly due to imperfect isotopic separation of the particular pathways. Nevertheless, the estimation of N2O reduction is much more robust, when applying optimal calculation strategy, reaching typically accuracy of N2O residual fraction determination of about 0.1.

scholarly journals N<sub>2</sub>O isotope approaches for source partitioning of N<sub>2</sub>O production and estimation of N<sub>2</sub>O reduction – validation with the <sup>15</sup>N gas-flux method in laboratory and field studies

2020 ◽  
Vol 17 (22) ◽  
pp. 5513-5537
Author(s):  
Dominika Lewicka-Szczebak ◽  
Maciej Piotr Lewicki ◽  
Reinhard Well
Keyword(s):  
Three Dimensional ◽  
Field Studies ◽  
Residual Fraction ◽  
N2o Reduction ◽  
Flux Method ◽  
Gas Flux ◽  
Dual Isotope ◽  
Isotopic Signatures ◽  
First Time

Abstract. The approaches based on natural abundance N2O stable isotopes are often applied for the estimation of mixing proportions between various N2O-producing pathways as well as for estimation of the extent of N2O reduction to N2. But such applications are associated with numerous uncertainties; hence, their limited accuracy needs to be considered. Here we present the first systematic validation of these methods for laboratory and field studies by applying the 15N gas-flux method as the reference approach. Besides applying dual-isotope plots for interpretation of N2O isotopic data, for the first time we propose a three dimensional N2O isotopocule model based on Bayesian statistics to estimate the N2O mixing proportions and reduction extent based simultaneously on three N2O isotopic signatures (δ15N, δ15NSP, and δ18O). Determination of the mixing proportions of individual pathways with N2O isotopic approaches often appears imprecise, mainly due to imperfect isotopic separation of the particular pathways. Nevertheless, the estimation of N2O reduction is much more robust, when applying an optimal calculation strategy, typically reaching an accuracy of N2O residual fraction determination of about 0.15.

Use of stable isotopes to determine diets of living and extinct bears

1996 ◽  
Vol 74 (11) ◽  
pp. 2080-2088 ◽  
Author(s):  
G. V. Hilderbrand ◽  
S. D. Farley ◽  
C. T. Robbins ◽  
T. A. Hanley ◽  
K. Titus ◽  
...  
Keyword(s):  
Ursus Arctos ◽  
Isotopic Fractionation ◽  
Columbia River ◽  
Late Summer ◽  
Isotopic Signature ◽  
Grizzly Bears ◽  
Brown Bears ◽  
River Drainage ◽  
Carbon And Nitrogen ◽  
Isotopic Analyses

The potential use of stable-isotope analyses (δ13C and δ15N) to estimate bear diets was assessed in 40-day feeding trials using American black bears (Ursus americanus). Bear plasma and red blood cells have half-lives of ~4 days and ~28 days, respectively. The isotopic signature of bear plasma is linearly related to that of the diet, and with the exception of adipose tissue, there is no isotopic fractionation across bear tissues. Isotopic analyses were used to estimate the diets of three bear populations: Pleistocene cave bears (U. speleaus) in Europe, grizzly bears (Ursus arctos horribilis) inhabiting the Columbia River drainage prior to 1931, and brown bears (U. arctos) of Chichagof and Admiralty islands, Alaska. Cave bears were omnivores with terrestrially produced meat contributing from 41 to 78% (58 ± 14%) of their metabolized carbon and nitrogen. Salmon contributed from 33 to 90% (58 ± 23%) of the metabolized carbon and nitrogen in grizzly bears from the Columbia River drainage. Finally, most brown bears on Chichagof and Admiralty islands feed upon salmon during the late summer and fall; however, a subpopulation of bears exists that does not utilize salmon.

Carbon, nitrogen, and sulfur diet–tissue discrimination in mouse tissues

2005 ◽  
Vol 83 (7) ◽  
pp. 989-995 ◽  
Author(s):  
Lynne S Arneson ◽  
Stephen E MacAvoy
Keyword(s):  
Food Web ◽  
Isotopic Signature ◽  
Physiological Status ◽  
Isotopic Signatures ◽  
Adult Mice ◽  
Dietary Choices ◽  
Tissue Discrimination ◽  
Mouse Tissues ◽  
Changes Over Time

Stable-isotope ratios are increasingly being used to examine ecological questions pertaining to dietary choices, physiological status, and animal migration. It has been shown that animal tissues reflect the isotopic signature present in food, altered by a small reproducible fractionation value. The average diet–tissue discrimination for δ13C and δ15N is approximately 1‰ and 3‰, respectively, although the degree of diet–tissue discrimination may be affected by a range of factors and vary between organisms and tissue types. Although the average δ34S is approximately zero, the sulfur diet–tissue discrimination values have only been determined for a few organisms. It is necessary to determine accurate diet–tissue discrimination values between tissue and dietary components to have confidence in any food-web study or determination of diet quality. In this paper, we determine carbon, nitrogen, and sulfur diet–tissue discrimination values for whole blood, liver, skeletal muscle, heart, brain, and fat (carbon only) from adult mice (Mus musculus L., 1758) equilibrated on three diets with unique isotopic signatures for carbohydrate carbon and for protein carbon, nitrogen, and sulfur. These data will aid researchers in choosing tissues to be used to examine food-web changes over time.

scholarly journals Isotopic signatures of production and uptake of H<sub>2</sub> by soil

2015 ◽  
Vol 15 (22) ◽  
pp. 13003-13021 ◽  
Author(s):  
Q. Chen ◽  
M. E. Popa ◽  
A. M. Batenburg ◽  
T. Röckmann
Keyword(s):  
Isotope Effects ◽  
Deposition Velocity ◽  
Isotopic Fractionation ◽  
Isotopic Signature ◽  
Deuterium Content ◽  
Forest Site ◽  
Fractionation Factor ◽  
Isotopic Signatures ◽  
The Difference ◽  
Isotope Equilibrium

Abstract. Molecular hydrogen (H2) is the second most abundant reduced trace gas (after methane) in the atmosphere, but its biogeochemical cycle is not well understood. Our study focuses on the soil production and uptake of H2 and the associated isotope effects. Air samples from a grass field and a forest site in the Netherlands were collected using soil chambers. The results show that uptake and emission of H2 occurred simultaneously at all sampling sites, with strongest emission at the grassland sites where clover (N2 fixing legume) was present. The H2 mole fraction and deuterium content were measured in the laboratory to determine the isotopic fractionation factor during H2 soil uptake (αsoil) and the isotopic signature of H2 that is simultaneously emitted from the soil (δDsoil). By considering all net-uptake experiments, an overall fractionation factor for deposition of αsoil = kHD / kHH = 0.945 ± 0.004 (95 % CI) was obtained. The difference in mean αsoil between the forest soil 0.937 ± 0.008 and the grassland 0.951 ± 0.026 is not statistically significant. For two experiments, the removal of soil cover increased the deposition velocity (vd) and αsoil simultaneously, but a general positive correlation between vd and αsoil was not found in this study. When the data are evaluated with a model of simultaneous production and uptake, the isotopic composition of H2 that is emitted at the grassland site is calculated as δDsoil = (−530 ± 40) ‰. This is less deuterium depleted than what is expected from isotope equilibrium between H2O and H2.

scholarly journals Isotopic signatures of production and uptake of H<sub>2</sub> by soil

2015 ◽  
Vol 15 (17) ◽  
pp. 23457-23506 ◽  
Author(s):  
Q. Chen ◽  
M. E. Popa ◽  
A. M. Batenburg ◽  
T. Röckmann
Keyword(s):  
Isotope Effects ◽  
Deposition Velocity ◽  
Isotopic Fractionation ◽  
Isotopic Signature ◽  
Deuterium Content ◽  
Forest Site ◽  
Fractionation Factor ◽  
Isotopic Signatures ◽  
The Difference ◽  
Isotope Equilibrium

Abstract. Molecular hydrogen (H2) is the second most abundant reduced trace gas (after methane) in the atmosphere, but its biogeochemical cycle is not well understood. Our study focuses on the soil production and uptake of H2 and the associated isotope effects. Air samples from a grass field and a forest site in the Netherlands were collected using soil chambers. The results show that uptake and emission of H2 occurred simultaneously at all sampling sites, with strongest emission at the grassland sites where clover (N2 fixing legume) was present. The H2 mole fraction and deuterium content were measured in the laboratory to determine the isotopic fractionation factor during H2 soil uptake (αsoil) and the isotopic signature of H2 that is simultaneously emitted from the soil (δDsoil). By considering all net-uptake experiments, an overall fractionation factor for deposition of αsoil = kHD/kHH = 0.945 ± 0.004 (95 % CI) was obtained. The difference in mean αsoil between the forest soil 0.937 ± 0.008 and the grassland 0.951 ± 0.025 is not statistically significant. For two experiments, the removal of soil cover increased the deposition velocity (vd) and αsoil simultaneously, but a general positive correlation between vd and αsoil was not found in this study. When the data are evaluated with a model of simultaneous production and uptake, the isotopic composition of H2 that is emitted at the grassland site is calculated as δDsoil = (−530 ± 40) ‰. This is less deuterium-depleted than what is expected from isotope equilibrium between H2O and H2.

Experimental determination of the sources of otolith carbon and associated isotopic fractionation

2006 ◽  
Vol 63 (1) ◽  
pp. 79-89 ◽  
Author(s):  
Christopher T Solomon ◽  
Peter K Weber ◽  
Joseph J Cech, Jr. ◽  
B Lynn Ingram ◽  
Mark E Conrad ◽  
...  
Keyword(s):  
Inorganic Carbon ◽  
Dissolved Inorganic Carbon ◽  
Stable Carbon Isotope ◽  
Isotopic Fractionation ◽  
Enrichment Factors ◽  
Activity Levels ◽  
Isotopic Enrichment ◽  
Rainbow Trout Oncorhynchus Mykiss ◽  
Blood Relative

Otolith stable carbon isotope ratios provide a unique and widely applicable environmental record. Unfortunately, uncertainty regarding the proportion of otolith carbon that derives from metabolized food versus dissolved inorganic carbon (DIC) in the water currently limits utilization of this marker. We manipulated the δ13C of food and ambient DIC in a factorial design with juvenile rainbow trout (Oncorhynchus mykiss). At the activity levels and total metabolic rates characteristic of fish in this study, 17% (±3% standard error, SE) of otolith C was metabolically derived, while >80% was derived from DIC in ambient water. We also estimated isotopic enrichment factors associated with physiological carbon transformations by measuring δ13C of blood and endolymph (which closely tracked otolith δ13C). There was substantial depletion in 13C of blood relative to C sources (εblood–sources = –16.9‰ ± 1.1‰ SE), but substantial enrichment in 13C in otolith relative to blood (εoto–blood = 13.3‰ ± 1.3‰ SE). Net isotopic enrichment between sources and the otolith was therefore slightly negative. Most of the isotopic enrichment between the blood and the otolith was associated with the movement of C from blood to endolymph, while enrichment associated with the precipitation of otolith aragonite from the endolymph was small.

Development and Validation of Derivative Spectroscopic Method for Simultaneous Estimation of Cefadroxil and Probenecid

2014 ◽  
Vol 7 (1) ◽  
pp. 2350-2355
Author(s):  
Pratik S Mehta ◽  
Pratik R. Patel ◽  
Rajesh R Parmar ◽  
M M K Modasiya ◽  
Dushyant A Shah
Keyword(s):  
Spectroscopic Method ◽  
Spectral Interference ◽  
Synthetic Mixture ◽  
Simultaneous Estimation ◽  
Zero Crossing ◽  
First Order ◽  
Derivative Spectroscopy ◽  
Development And Validation ◽  
Crossing Point

A novel, simple, accurate, sensitive, precise and economical derivative spectroscopic method was developed and validated for the determination of cefadroxil and probenecid in synthetic mixture. First order derivative spectroscopy method was adopted to eliminate spectral interference. The method obeys Beer’s Law in concentration ranges of 4-36 μg/ml for cefadroxil and of 5-25 μg/ml of probenecid. The zero crossing point for cefadroxil and probenecid was 260 nm and 237.8 nm respectively in 0.1N HCl. The method was validated in terms of accuracy, precision, linearity, limits of detection, limits of quantitation. This method has been successively applied to synthetic mixture and no interference from the synthetic mixture’s excipients was found.   

scholarly journals Investigations on historical monuments’ deterioration through chemical and isotopic analyses: an Italian case study

2021 ◽  
Author(s):  
Maria Ricciardi ◽  
Concetta Pironti ◽  
Oriana Motta ◽  
Rosa Fiorillo ◽  
Federica Camin ◽  
...  
Keyword(s):  
Potassium Nitrate ◽  
Sewage Water ◽  
X Ray Diffraction ◽  
Italian Case ◽  
Historical Monuments ◽  
Isotopic Analyses ◽  
Historic Centre ◽  
The Church

AbstractIn this paper, we analysed the efflorescences present in the frescos of a monumental complex named S. Pietro a Corte situated in the historic centre of Salerno (Campania, Italy). The groundwater of the historic centre is fed by two important streams (the Rafastia and the Fusandola) that can be the sources of water penetration. The aims of this work are to (i) identify the stream that reaches the ancient frigidarium of S. Pietro a Corte and (ii) characterize the efflorescences on damaged frescos in terms of chemical nature and sources. In order to accomplish the first aim, the water of the Rafastia river (7 samples) and the water of the Fusandola river (7 samples) were analysed and compared with the water of a well of the Church (7 samples). The ionic chromatography measurements on the water samples allowed us to identify the Rafastia as the river that feeds the ancient frigidarium of S. Pietro a Corte. To investigate the nature and the origin of the efflorescences (our second aim), anionic chromatography analyses, X-ray diffraction measurements, and the isotopic determination of nitrogen were performed on the efflorescences (9 samples) and the salts recovered from the well (6 samples). Results of these analyses show that efflorescences are mainly made of potassium nitrate with a δ15N value of + 9.3 ± 0.2‰. Consequently, a plausible explanation for their formation could be the permeation of sewage water on the walls of the monumental complex.

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