Determination Of Carbon In Soils Research Articles

Sustainable Wet Method for Determination of Total Organic Carbon in Soils Using Potassium Permanganate as a Substitute for Potassium Dichromate

Sustainable Wet Method for Determination of Total Organic Carbon in Soils Using Potassium Permanganate as a Substitute for Potassium Dichromate

Evaluation of univariate and multivariate calibration strategies for the direct determination of total carbon in soils by laser-induced breakdown spectroscopy: tutorial

The correct choice of the calibration strategy method is a step that can ensure the accuracy of carbon determination in soils by laser-induced breakdown spectroscopy. In this paper, we evaluate and discuss the intrinsic characteristics of univariate and multivariate calibration strategies in overcoming soil matrix effects and their influence on the magnitude of calibration and prediction error values. The matrix-matching calibration with previous correction of Al spectral interference in the C I line at 193.03 nm was the best strategy of the 13 univariate models evaluated [root-mean-square error of calibration—(RMSEP)=0.2wt.%C]. In the multivariate evaluation of the 22 models obtained, the artificial neural network allowed obtaining a lower value of prediction error for C (RMSEP=0.1wt.%C) with very good accuracy (98%) for the set samples of validation. The observation of these results was justified considering the advantages and limitations of each calibration strategy explored.

A GREEN AND RELIABLE TITRIMETRIC METHOD FOR TOTAL ORGANIC CARBON DETERMINATION WITH POTASSIUM PERMANGANATE

The determination of total organic carbon in soils, fertilizers, sewage sludge, sediments, and humic extracts is widely performed by chemical oxidation methods with K2Cr2O7. The Yeomans-Bremner (YB) method is currently the one that stands out the most. The drawback of these methods is the large amount of concentrated H2SO4 used, which generates a large amount of hazardous waste. This work proposes using KMnO4 as an alternative to K2Cr2O7 for a lower consumption of H2SO4. The method uses the back titration of Fe2+ added to consume both the MnO2 produced and the excess KMnO4 that was not consumed in the OM oxidation. A non-trivial and yet not explored stoichiometry was applied for this purpose, providing a success not yet achieved in using permanganate to determine TOC by titration. The ideal condition for the oxidation of OC was determined by the analysis of a potassium hydrogen phthalate standard and involved the use of 0.125 mol L-1 H2SO4 and temperature of 70 °C, obtaining a significant advantage over the YB method (concentrated H2SO4 and 170 °C). The proposed method was applied to the analysis of soil samples, producing conversion factors for soil organic carbon that varied between 0.652 and 1.12.

Effect of the sample measurement representativeness on soil carbon determination using near-infrared compact spectrophotometers

Compact or miniaturized near-infrared (NIR) spectrophotometers are inexpensive instruments that can boost the use of NIR spectroscopy (NIRS) for determining soil organic carbon (SOC). Nevertheless, these instruments are deficient concerning the probing capability due the small area of the sample assessed in spectra measurement. Protocols normally used during spectral data acquisition can be insufficient to obtain representative spectra, which can affect the performance of the models to estimate SOC. This paper aimed to understand how the representativeness of soil spectra is affected by increasing the area probed during spectra acquisition and determine its effect on the performance of multivariate regression models constructed using compact NIR spectrophotometers for SOC determination. Four measurement modes of the flask containing the soil sample were evaluated using a compact FT-NIR. Measurement modes I (full radial and axial scanning of sample flask) and II (full radial scanning in a fixed axial line of sample flask) were performed using a rotational-linear sample probing device to move the sample flask over the optical probing beam during spectral data acquisition. Measurement modes III and IV, in turn, were performed in static mode. Using the measurement mode III, the spectral data were acquired at variable points of the sample flask, and using the measurement mode IV, the spectral data were acquired at a single fixed point in the sample flask. The study was developed in two stages. Firstly, five spectra of three soil samples (selected according to their carbon content) were acquired using the measurement modes. The repeatability and representativeness of the spectral data were then evaluated using principal component analysis (PCA). Partial least square regression (PLSR) models were constructed to determine the quantitative effects of the representativeness of the four measurement modes used to acquire the spectral data set. The calibration and independent validation sets were composed of 49 and 20 soil samples, respectively. The increase in the sample area probed using the a rotational-linear sample probing device resulted in more representative and reproducible spectral data, which improves the performance of compact spectrophotometer in SOC determination. Significant enhancements in SOC determination ranged from 146 to 400 % were found, considering the most (mode I) over less representative measurement modes. These results were verified by a comparative randomization test between models’ prediction performances. In this context, using a rotational-linear sample probing device is recommended for SOC determinations using compact NIR spectrophotometers.

Evaluation of a rapid microwave digestion method for determination of total organic carbon in soil

ABSTRACTPrecise measurement of soil organic carbon (SOC) is essential for constructing regional inventories, developing best agricultural management practices, and modeling purposes. Currently, the automated dry combustion method is considered standard, but the method is both costly and time-consuming. There is a need for a simple, easy to use and cost-effective method of organic C determination in soil. A simple method of total organic carbon (TOC) determination in soil that involved wet digestion of K2Cr2O7-H2SO4-soil mixture in a commercial microwave oven followed by spectrophotomteric measurement of Cr (III) was evaluated. The method was compared with automated dry combustion and two other wet digestion methods. The method showed close agreement with dry combustion method (R2 = 0.90; root mean square error = 0.70) and the TOC measured with the two methods did not differ for a range of soils drawn from lowland and upland land-uses and varying in pH (6.2–9.3), TOC (2.8–14 g kg−1), and calcium carbonate content (0–6.7%). The recovery of the added organic C by the microwave method was 98.6 ± 4.2%. The results suggested that microwave-spectrophotometric method could be easily adopted in routine soil analysis as it is not only precise, rapid, and cost-effective but also produced small volume of reagent waste.

Determination of organic carbon in soils and sediments in an automatic method

Determination of organic carbon in soils and sediments in an automatic method

Quantifying organic carbon storage and sources in sediments of Dong Rui mangrove forests, Tien Yen district, Quang Ninh province using carbon stable isotope

Quantifying organic carbon storage and sources in sediments of Dong Rui mangrove forests, Tien Yen district, Quang Ninh province using carbon stable isotope

Espectroscopia no Infravermelho Próximo para a Quantificação de Carbono em Solos da Bacia do Acre

In soil carbon determination various techniques are used, predominating in Brazil methods based on oxidation of organic matter in the presence of potassium dichromate in an acidic medium and the elemental analysis. The objective of this study was to evaluate the technical viability of NIR spectroscopy combined with multivariate calibration analysis to quantify the carbon content of the soil Acre basin. We use 190 soil samples, collected in various locations of Acre basin, in order to test the NIR technique for determining the soil carbon content. We compared the NIR technique, dichromate oxidation in acidic media and elemental analysis methods. The amounts of carbon was obtained by oxidation and elemental analysis methods using the method of elemental analysis as a reference, it is found that the oxidation method recovered an average of 63.8% of carbon determined by the reference method. We suggest to adjust the amount of carbon obtained by the oxidation method should be adopted the coefficient 1.55. Regarding the use of NIR spectroscopy, the model developed for soil carbon analysis Acre basin by NIR spectroscopy showed good classification according to R 2 values and excellent rating under the RMSEC < RMSEP and RPD values, with reference to carbon determined by the elemental analysis method. Keywords : organic matter; Amazon; tropical soils; analytical methods.

Benchmarking the Inelastic Neutron Scattering Soil Carbon Method

The herein described inelastic neutron scattering (INS) method of measuring soil carbon was based on a new procedure for extracting the net carbon signal (NCS) from the measured γ spectra and determination of the average carbon weight percent in the upper ∼8‐cm soil layer (AvgCw%8). The NCS extraction utilized the net‐INS spectrum, which was the difference between the INS and thermal neutron capture (TNC) spectra and the net‐INS system background spectrum. The proportionality between NCS and AvgCw%8 for any shape of soil carbon depth distribution was demonstrated theoretically. The theoretical model for NCS calculations accounted for carbon depth distribution and neutron and γ ray propagation laws in our analysis; previous model results were verified by comparison with a Monte Carlo simulation using Geant4. The experimental results confirmed the identified proportionality. The mobile INS system was calibrated using pits filled with synthetic soil; this calibration was used for AvgCw%8 determinations in INS field measurements. The AvgCw%8 was also determined by the dry combustion method. Benchmarking the soil carbon determination by INS demonstrated results that coincided with dry combustion technique (DCT) results (within experimental error limits). Given the agreement between these methods, the described INS measurement system can be recommended as a reliable alternative means for measuring soil carbon.

Improving the application of laser-induced breakdown spectroscopy for the determination of total carbon in soils.

The increase of atmospheric greenhouse gases such as CO2 has caused noticeable climate change. Since increased CO2 may contribute to carbon storage in terrestrial ecosystems through the CO2 cycle between the atmosphere and vegetation, it is necessary to improve methods for measuring C in soil. In this study, we determined the total carbon concentrations of soils using a highly sensitive and rapid method, laser-induced breakdown spectroscopy. The presence of C has been measured by detecting signal at the wavelength of 247.86 nm. The obstacle of Fe interference at the C measurement wavelength of 247.86 nm was reduced by selecting the optimal delay time of 1.4 μs. The ratio of peak intensities (areas) at 247.86 nm for C and 248.20 nm for Fe was then successfully applied to the calibration curve. In addition, to dismiss the problem of measuring the C lines at 247.86 nm, 193.03 nm has been used to observe C emission. Both the 193.03- and 247.86-nm lines provided significant linear calibrations. The 193.03-nm lines presented stronger relative accuracies in predicting the lower C concentrations of the unknown samples than that one at 247.86 nm.

Soil carbon determination by thermogravimetrics

Determination of soil constituents and structure has a vital role in agriculture generally. Methods for the determination of soil carbon have in particular gained greater currency in recent times because of the potential that soils offer in providing offsets for greenhouse gas (CO2-equivalent) emissions. Ideally, soil carbon which can also be quite diverse in its makeup and origin, should be measureable by readily accessible, affordable and reliable means. Loss-on-ignition is still a widely used method being suitably simple and available but may have limitations for soil C monitoring. How can these limitations be better defined and understood where such a method is required to detect relatively small changes during soil-C building? Thermogravimetric (TGA) instrumentation to measure carbonaceous components has become more interesting because of its potential to separate carbon and other components using very precise and variable heating programs. TGA related studies were undertaken to assist our understanding in the quantification of soil carbon when using methods such as loss-on-ignition. Combining instrumentation so that mass changes can be monitored by mass spectrometer ion currents has elucidated otherwise hidden features of thermal methods enabling the interpretation and evaluation of mass-loss patterns. Soil thermogravimetric work has indicated that loss-on-ignition methods are best constrained to temperatures from 200 to 430 °C for reliable determination for soil organic carbon especially where clay content is higher. In the absence of C-specific detection where mass only changes are relied upon, exceeding this temperature incurs increasing contributions from inorganic sources adding to mass losses with diminishing contributions related to organic matter. The smaller amounts of probably more recalcitrant organic matter released at the higher temperatures may represent mineral associated material and/or simply more refractory forms.

Soil Carbon Determination in a Mediterranean Vertisol by Visible and near Infrared Reflectance Spectroscopy

The monitoring of the C content of agricultural lands requires long-term experiments, the analysis of a large number of samples, various sampling depths and adequate analytical tools to perform the experiments. Near infrared (NIR) reflectance spectroscopy is a fast, reliable and low-cost analytical tool for the determination of soil C content. The objective of this study was to present NIR spectroscopy technology as a reliable method to monitor C concentration (total C, inorganic C and organic C) of soil samples from a long-term experiment established in 1986 in Cordoba (Spain). The soil is a rain-fed vertisol, characteristic of Mediterranean agricultural systems. The soil samples studied from four different years (1997, 2000, 2003 and 2006) included all of the variabilities existing in the long-term experiment: tillage system (conventional tillage vs no tillage), crop rotations [wheat ( Triticum aestivum L)-chickpea ( Cicer arietinum L), wheat-faba bean ( Vicia faba L), wheat-sunflower ( Helianthus annus L), wheat-fallow and wheat-wheat], N fertiliser rate (0 kg N ha−1, 50 kg N ha−1, 100 kg N ha−1 and 150 kg N ha−1), as well as different soil depths (0–15 cm, 15–30 cm, 30–60 cm and 60–90 cm). Calibration models were obtained with 492 samples from the aforementioned vertisol using visible and NIR spectroscopy (vis-NIR) and, when tested using a validation sample set, returned the values: total C ( r2 = 0.92, SEP = 1 g kg−1, RER = 26, RPD = 4.8); inorganic C ( r2 = 0.95, SEP = 1.5 g kg−1, RER = 26.6, RPD = 4.6) and organic C ( r2 = 0.76, SEP = 0.8 g kg−1 RER = 12.3, RPD = 2). The vis-NIR models developed reliably predicted the total, inorganic and organic C content at plot scale (homogeneous sample set). The advantage deriving from very specific vis-NIR calibrations for prediction of soil C is that one can rapidly and economically predict C in the study area, enabling monitoring to compare soil C evolution depending on time and variables such as tillage, crop rotation and fertilisation. To develop vis-NIR models at local and regional scales would require a more heterogeneous sample set and adequate calibration/validation strategies.

Determination of carbon in soil by laser spectral analysis

We have used a combination laser/electrospark method for fast determination of carbon content in soil. Excitation of the spectra is carried out both directly in a laser ablation plume and when a pulsed electric discharge is applied to it. We have plotted a calibration curve that is linear for the major concentration range of practical importance for the analyte element, all the way up to 8.6%. The carbon detection limit for the combination discharge approach is 0.07%. We have analyzed the ratio of the nitrogen and carbon contents, and also the hydrogen and carbon contents as a function of the carbon concentration in the studied soils samples.

Colorimetric Determination of Organic Carbon in Soils by Dichromate Digestion in a Microwave Oven

Colorimetric Determination of Organic Carbon in Soils by Dichromate Digestion in a Microwave Oven

Carbono do solo e a mitigação da mudança climática global

The soils of the world contain more carbon than the combined total amounts occurring in vegetation and the atmosphere. Hence soils are a major reservoir of carbon in terrestrial ecosystems and an important sink. Recently, emphasis has been placed on the need to sequester carbon from atmospheric carbon dioxide into soil organic matter because of international concerns about greenhouse gas emissions and global climate change. The best strategies to built-up carbon stocks in the soil are basically those that increase the input of organic matter to the soil, and/or decrease the rate of soil organic matter decomposition. Grain crop systems based on soil ploughing and harrowing lead to CO2 emissions combined with tremendous soil losses. In Brazil, no-tillage system was introduced to combat soil erosion by water and this soil management led to the build-up of soil carbon stocks with simultaneous high crop yields. However, the present procedure used to quantify carbon stocks in soils is laborious and of high cost. The use of infrared spectroscopy is very promising as an alternative low-cost method of soil carbon determination.

A simple procedure for colorimetric determination of organic carbon in soil

Abstract A simple procedure is described for the rapid determination of organic carbon content in a large number of soil samples using an automated segmented flow analyser. The method is a modification of the wet oxidation/ digestion methods based on potassium dichromate combined with a colorimetric method for determination of chromic oxide (Stevenson and Clare, 1962). Using a segmented flow analyser for the colorimetry, the procedure is capable of automated routine analyses of large numbers of samples and was shown to give high and repeatable recoveries of organic carbon from a range of compounds. Organic carbon values for a range of soils analysed by the reported method and by the dry combustion technique showed a high correlation.

Spectrophotometric determination of organic carbon in soil

Abstract A detailed study was made of the well‐known organic carbon determination that is based on measuring the absorbance of the green chromium(III) complex generated when organic matter is oxidized by potassium dichromate in acidic medium. The green chromic colour proved to be unstable, turning slowly to a violet colour. It was also found that chromic sulphate exerts a catalytic influence on the decomposition of excess dichromate. Based on this work, a modified method was developed which is simple, rapid, and very accurate when working under carefully controlled conditions.

A comparison of some methods for soil organic carbon determination

Abstract This study compared three dichromate‐oxidation methods adapted for use with 100‐mL digestion tubes and 40‐tube block digester (for controlled heating), the Walkley‐Black method, a loss‐on‐ignition procedure and an automated dry combustion method for the determination of organic carbon in soils of the northwestern Canadian prairie. The Walkley‐Black method required a correction factor of 1.40. The modified Tinsley method and the Mebius procedure, adapted for use with 100‐mL digestion tubes, recovered 95% and 98%, respectively, of soil carbon against the dry combustion procedure. The presence of elemental carbon in some soils probably caused, at least partially, the slightly incomplete recovery; thermal decomposition of dichromate may not have been accurately corrected for. A dichromate‐oxidation procedure with controlled digestion at 135°C gave 100% recovery, but somewhat more variable results. The loss‐on‐ignition procedure, even when allowance was made for clay content of the soils, was the leas...

Determination of organic carbon in soils and fertilizers

Abstract Many methods have been proposed to determine the total amount of organic carbon in soil; some of them determine only a percentage of the actual carbon content and therefore the results need the application of a correction factor. Methods for the determination of organic carbon in soil have been rarely extended to organic fertilizers and amendments. We propose a rapid method based on a modification of the original Springer and Klee10procedure. Samples are oxidized for exactly 10 minutes with a mixture of 20 ml 2N K2Cr2O7and 26 ml conc. H2SO4at 160±2°C; the excess dichromate is titrated either potentiometrically or manually with FeSO4. The method is fast, accurate, and more reliable than other commonly used procedures. The procedure can be easily adopted for serial determination of carbon in both soils and organic fertilizers or amendments

A rapid and precise method for routine determination of organic carbon in soil

Abstract A simple method for routine determination of organic carbon in soil by a modified Mebius procedure is described. It involves (a) digestion of the soil sample with an acidified dichromate (K2Cr2O7‐H2SO4) solution for 30 minutes in a Pyrex digestion tube in a 40‐tube block digester preheated to 170°C and (b) estimation of the unreacted dichromate by titration of the cooled digest with an acidified solution of ferrous ammonium sulfate with use ofN‐phenylanthranilic acid as an indicator. The method is more rapid and precise than the Mebius procedure commonly used for routine analysis of soils for organic carbon, and the only equipment required for its use is equipment now commonly used for routine Kjeldahl analysis of soils for total nitrogen.