Simultaneous measurement of soil organic and inorganic carbon: evaluation of a thermal gradient analysis

Purpose

The best method for determining soil organic carbon (SOC) in carbonate-containing samples is still open to debate. The objective of this work was to evaluate a thermal gradient method (ThG), which can determine simultaneously inorganic carbon (SIC) and SOC in a wide range of soil samples.

Materials and methods

The determination of SOC by ThG (SOC_ThG) was compared to the following widespread standard methods: (1) acidification (ACI) as pretreatment and subsequent dry combustion (SOC_ACI) and (2) volumetric quantification of SIC by a calcimeter (CALC) and subtraction of the total carbon content as determined by dry combustion (SOC_CALC). Precision (F test) and bias (t test) were tested on a subset of seven samples (n?=?3). Comparison of the ThG and CALC methods was performed by regression analysis (n?=?76) on samples representing a wide range of SOC (5.5 to 212.0 g kg^?1) and SIC (0 to 59.2 g kg^?1) contents.

Results and discussion

Tests on the replicated subset showed that the precision of ThG was not significantly different from ACI or CALC (F values?<?39, n?=?3) for SOC and SIC measurements. However, SOC_ACI and SOC_CALC contents were systematically and significantly lower compared to SOC_ThG contents. The positive bias for SOC_ThG relative to SOC_CALC contents appeared also in the regression analysis (given numbers?±?standard errors) of the whole data set (y?=?(4.67?±?0.70)?+?(0.99?±?0.01)x, R ²?=?0.99, n?=?76). When performing a regression with carbonate-free samples, the bias between the methods was negative (?2.90?±?0.63, n?=?29) but was positive in the set with carbonate-containing samples (3.95?±?1.41, n?=?47). This observation corroborated the suspicion that the use of acid for carbonate decomposition can lead to an underestimation of SOC.

Conclusions

All methods were suitable for differentiation between SIC and SOC, but the use of acid resulted in lower estimates of SOC contents. When comparing soil samples with different carbonate concentrations, the use of the ThG method is more reliable.     

Optimized conditions for determination of total soil organic matter in diverse samples by mass loss on ignition

Reliable measurement of soil organic matter (SOM) contents is crucial to assessment of soil health, productive longevity and the effects of climate change. In this study, the loss‐on‐ignition (LOI) method has been used to determine the SOM of dried soil samples with a wide range of clay, sand and silt contents from the Agricultural Laboratory Proficiency (ALP) program. Regressions of ALP participant data against LOI measurements at 350–650°C indicate that the extent of SOM oxidation depends more on the ignition temperature and time than on the sample compositions. Thus, LOI data from ignition at 350–550°C for 12 h relative to ignition at 650°C for 12 h converge at 650°C and the average coefficient of variance decreases to ≈ 4% at 650°C. Also examined are regressions of soil organic C from direct dry combustion as standards with LOI measured at 360°C for 2 h, LOI measured at 650°C for 12 h and with the Walkley‐Black procedure used in the ALP program.     

Density fractionation of organic matter in dolomite‐derived soils

Dolomite (CaMg(CO₃)₂) constitutes half of the global carbonates. Thus, many calcareous soils have been developing rather from dolomitic rocks than from calcite (CaCO₃)‐dominated limestone. We developed a physical fractionation procedure based on three fractionation steps, using sonication with subsequent density fractionation to separate soil organic matter (SOM) from dolomite‐derived soil constituents. The method avoids acidic pretreatment for destruction of carbonates but aims at separating out carbonate minerals according to density. The fractionation was tested on three soils developed on dolostone parent material (alluvial gravel and solid rock), differing in organic‐C (OC) and inorganic‐C (IC) concentrations and degree of carbonate weathering. Soil samples were suspended and centrifuged in Na‐polytungstate (SPT) solutions of increasing density, resulting in five different fractions: two light fractions < 1.8 g cm^–3 (> 20 μm and < 20 μm), rich in OC and free of carbonate, and two organomineral fractions (1.8–2.4 g cm^–3 and 2.4–2.6 g cm^–3), containing 66–145 mg g^–1 and 16–29 mg g^–1 OC. The organomineral fractions consist of residual clay from carbonate weathering such as clay minerals and iron oxides associated with SOM. The fifth fraction (> 2.6 g cm^–3) was dominated by dolomite (85%–95%). The density separation yielded fractions differing in mineral compositions, as well as in SOM, indicated by soil‐type‐specific OC distributions and decreasing OC : N ratios with increasing density of fractions. The presented method is applicable to a wide range of dolomitic and most likely to all other calcareous soils.     

利用烧失量方法精确测定土壤有机质

Wet oxidation procedure,i.e.,Walkley-Black (WB) method,is a routine,relatively accurate,and popular method for the determination of soil organic matter (SOM) but it is time-consuming,costly and also has a high potential to cause environmental pollution because of disposal of chromium and strong acids used in this analysis.Therefore,loss-on-ignition (LOI) procedure,a simple and cheap method for SOM estimation,which also avoids chromic acid wastes,deserves more attention.The aims of this research were to study the statistical relationships between SOM determined with the LOI (SOMLOI) and WB (SOMWB) methods to compare the spatial variability of SOM in two major plains,Shahrekord and Koohrang plains,of Chaharmahal-va-Bakhtiari Province,Iran.Fifty surface soil samples (0-25 cm) were randomly collected in each plain to determine SOM using the WB method and the LOI procedure at 300,360,400,500 and 550 ℃ for 2 h.The samples covered wide ranges of soil texture and calcium carbonate equivalent (CCE).The general linear form of the regression equation was calculated to estimate SOM LOI from SOM obtained by the WB method for both overall samples and individual plains.Forty soil samples were also randomly selected to compare the SOM and CCE before and after ignition at each temperature.Overall accuracy of the continuous maps generated for the LOI and WB methods was considered to determine the accordance of two procedures.Results showed a significant positive linear relationship between SOM LOI and SOM WB.Coefficients of determination (R2) of the equations for individual plains were higher than that of the overall equation.Coefficients of determination and line slopes decreased and root mean square error (RMSE) increased with increasing ignition temperature,which may be due to the mineral structural water loss and destruction of carbonates at higher temperatures.A temperature around 360 ℃ was identified as optimum as it burnt most organic carbon,destroyed less inorganic carbon,caused less clay structural water loss,and used less electrical energy.Although the trends of SOM in the kriged maps by the two procedures accorded well,low overall accuracy was observed for the maps obtained by the two methods.While not suitable for determination where high accuracy is required,determination of organic carbon through LOI is likely suitable for exploratory soil surveys where rough estimation of organic matter is required.     

Estimating soil organic carbon through loss on ignition: effects of ignition conditions and structural water loss

Loss on ignition (LOI) is one of the most widely used methods for measuring organic matter content in soils but does not have a universal standard protocol. A large number of factors may influence its accuracy, such as furnace type, sample mass, duration and temperature of ignition and clay content of samples. We conducted a series of experiments to quantify these effects, which enabled us to derive (i) guidelines for ignition conditions (sample mass, duration and temperature), (ii) temperature‐specific soil organic matter (SOM) to soil organic carbon (SOC) conversion factors and (iii) clay content‐dependent correction factors for structural water loss (SWL). Bulk samples of a sandy soil (4% clay) and a silt loam soil (25% clay) were used to evaluate the effects of ignition conditions. Samples with a range of clay contents (0–50%) were used to quantify conversion and correction factors. Two furnaces, one without and one with pre‐heated air, did not show significant differences in terms of within‐batch LOI variability. In both furnaces less combustion occurred close to the door, which necessitated tray turning at half‐time as this reduced the standard deviation per batch significantly. Variation in mass loss declined exponentially with sample mass (range, 0.15–20 g). The LOI increased with duration at lower temperatures (≤ 550°C) for the sandy soil. At greater temperatures (600 and 650°C), no effect of duration was found. For the silt loam soil, LOI values increased with duration for each temperature, which was attributed to SWL. The SOM to SOC conversion factor decreased strongly with temperature at an ignition duration of 3 hours from 0.70 (350°C) to 0.57 (500°C) and stabilized around 0.55 between 550 and 650°C, indicating that at temperatures ≥ 550°C all SOM had been removed. The clay correction factor for SWL increased from 0.01 to 0.09 as the temperature of ignition increased from 350 to 650°C. To minimize within‐batch LOI variation we recommend a standard ignition duration of 3 hours, tray turning at half‐time, a sample mass ≥ 20 g and temperatures equal to or greater than 550 °C. To avoid over‐estimates of SOM through structural water loss, the presented SWL correction procedure should always be applied.     

Analysis and simulation of soil organic‐carbon stocks in grassland ecosystems in SW Germany

Grassland extensification is followed by a change of soil organic‐matter (SOM) contents. In order to give a better assessment of these developments on grassland sites in SW Germany, the CENTURY Soil Organic Matter Model was used on five long‐term experimental sites under three different management practices (“Mowing”, “Mulching” (mowing without removal of the phytomass), and “Natural succession”). On these sites, soil‐organic‐carbon (SOC) monitoring was continuously done for soil depths of 0–4 and 4–8 cm from 1975 to 2002. The contents of organic carbon (OC) were at steady state or showed a slight decrease for the mulched and succession plots. Carbon contents of the mowed plots were decreasing. Measured C contents were transferred into stocks and compared with the simulated OC stocks. Linear regressions between observed and simulated C stocks were calculated separately for mulched and succession plots. The regressions for OC yielded significant relationships (R² = 0.8) for both kinds of plots. However, the model did not reproduce the short‐term dynamics of C stocks. Whereas SOC stocks on mulched and succession plots are expected to stay stable for the next decades according to the simulation, they are expected to decrease for a couple of years before stabilization on mowed plots.     

Quantitative Measurement of Organic Carbon in Mine Wastes: Methods Comparison for Inorganic Carbon Removal and Organic Carbon Recovery

The present study aims to evaluate carbon recovery and analytical precision of two methods based on dry combustion for organic carbon (OC) quantification in base metal mine tailings: (1) IC subtraction method (inorganic C(IC) measured and subtracted from total C) and (2) direct OC quantification after acid pretreatment. Results showed IC subtraction method effectively hydrolyzed a range of IC minerals [calcium carbonate (CaCO₃), magnesium carbonate (MgCO₃), dolomite, magnesite, calcite] with satisfactory IC (as CO₂ released) recovery (87–103 percent). In the direct OC quantification method, 5 M hydrochloric acid (HCl) pretreatment resulted in a satisfactory recovery (76–92 percent) of most organic compounds [ethylenediaminetetraacetic acid (EDTA), cellulose, plant litter, and charcoal], except for water-soluble OC (sucrose, 40 percent recovery). The precision of both methods declined when C levels were <5 g kg^?1 with RSD (Relative Standard Deviation) > 10 percent. The OC values in test samples of base metal mine tailings were comparable between the two methods. However, IC subtraction method is not applicable for tailings with low OC levels (<5 g kg^?1) until the precision is substantially improved. Moreover, compared to the IC subtraction method, OC values are significantly lower in direct OC quantification method for tailings with high OC levels.     

How are soil use and management reflected by soil organic matter characteristics: a spectroscopic approach

We studied the quantitative and qualitative changes of soil organic matter (SOM) due to different land uses (arable versus grassland) and treatments (organic manure and mineral fertilizer) within an agricultural crop rotation in a long‐term field experiment, conducted since 1956 at Ultuna, Sweden, on a Eutric Cambisol. The organic carbon (OC) content of the grassland plot was 1.8 times greater than that of the similarly fertilized Ca(NO₃)₂ treated cropped plots. The comparison of two dispersion techniques (a low‐energy sonication and a chemical dispersion which yield inherent soil aggregates) showed that increasing OC contents of the silt‐sized fractions were not matched by a linear increase of silt‐sized aggregates. This indicated saturation of the aggregates with OC and a limited capacity of particles to protect OC physically. Thermogravimetric analyses suggested an increase of free organic matter with increasing OC contents. Transmission FT‐IR spectroscopy showed relative enrichment of carboxylic, aromatic, CH and NH groups in plots with increasing OC contents. The silt‐sized fractions contained the largest SOM pool and, as revealed by ¹³C NMR spectroscopy, were qualitatively more influenced by the plant residue versus manure input than the clay fractions. Alkyl and O‐alkyl C in the silt‐sized fractions amounted to 57.4% of organic carbon in the animal manure treated plots and 50–53% in the other treatments.     

Variation of intra‐aggregate organic carbon affects aggregate formation and stability during organic manure fertilization in a fluvo‐aquic soil

The aggregate formation and stability are controlled by the dynamics of soil organic matters (SOM), but how it is related to SOM chemical composition within different‐sized aggregates is largely unknown during manure fertilization. In this study, the variations of intra‐aggregate organic carbon (OC), including intra‐particulate organic matter (iPOM) and mineral‐associated organic matter, were quantitatively and qualitatively analysed, and then, their effects on aggregate formation and stability were assessed under four treatments: control (CK), mineral fertilizer (NPK), reduced manure (30%M) and manure fertilizers (M). Manure application (M) significantly increased macroaggregate proportion, mean weight diameter (MWD), and OC contents within different‐sized aggregates compared to CK, NPK, and 30%M. The OC accumulation of macroaggregate in M was attributed to OC content increase in silt plus clay subfraction rather than iPOM with more labile organic groups; oppositely, in microaggregate it was located in the relatively stable fine iPOM. The macroaggregate formation and stability were controlled by the fine iPOM within macroaggregates, whose abundant polysaccharide‐C and aliphatic‐C after manure fertilization advanced the microbial growth except for Gram‐positive bacteria, which further promoted macroaggregate formation and stability. The free silt plus clay fraction also affected macroaggregate formation and stability, and its polysaccharide‐C derived from microorganisms or decomposing SOM was positively associated with MWD and macroaggregate proportion. Because polysaccharide‐C can be easily associated with mineral particles, further improving micro‐ or macroaggregation. We conclude that continuous manure fertilization could increase labile SOM accumulation within aggregates and then facilitate microbial growth, which collectively are responsible for aggregate formation and stabilization.     

The importance of inorganic carbon in soil carbon databases and stock estimates: a case study from England

Many national and regional databases of soil properties and associated estimates of soil carbon stock consider organic, but not inorganic carbon (IC). Any future change in soil carbon stock resulting from the formation of pedogenic carbonates will be difficult to set in context because historical measurements or estimates of IC concentration and stock may not be available. In their article describing a database of soil carbon for the United Kingdom published in this journal, Bradley et al. [Soil Use and Management (2005) vol. 21, 363–369] only consider data for organic carbon (OC), despite the occurrence of IC‐bearing calcareous soils across a substantial part of southern England. Robust techniques are required for establishing IC concentrations and stocks based on available data. We present linear regression models (R² between 0.8 and 0.88) to estimate IC in topsoil based on total Ca and Al concentrations for soils over two groups of primary, carbonate‐bearing parent materials across parts of southern and eastern England. By applying the regression models to geochemical survey data across the entire area (18 165 km²), we estimate IC concentrations on a regular 500‐m grid by ordinary kriging. Using bulk density data from across the region, we estimate the total IC stock of soil (0–30 cm depth) in this area to be 186 MtC. This represents 15.5 and 5.5% of the estimated total soil carbon stock (OC plus IC) across England and the UK, respectively, based on the data presented by Bradley et al. [Soil Use and Management (2005) vol. 21, 363–369]. Soil geochemical data could be useful for estimating primary IC stocks in other parts of the world.     

Re‐analysis of the Relationship between Organic Carbon and Loss‐on‐Ignition in Soil

The suitability of loss‐on‐ignition (LOI) as an alternative to direct measurement of organic carbon (OC) has been debated for decades without resolution. The literature contains an abundance of different linear regression models to describe the LOI–OC relationship, most based on untransformed values of LOI and OC. Such regression is suspect because the variables are unable to occupy Euclidean space. Logratio transformation—based on relative rather than absolute differences—eliminates this constraint. Re‐analysis of the relationship on new and 10 previously published datasets using logratio techniques reveals that the relationship is nonlinear and that the profusion of regression models is in part a function of the range of LOI. Although LOI may offer a crude estimate of OC at high LOI levels, OC/LOI ratios when LOI is less than about 25% are too variable for reliable OC estimation, and interstudy comparisons remain dubious. Direct measurement of OC is recommended.     

Relationships between four methods of organic carbon determination in leaves of nitrogen‐fixing trees and lignite‐based organic fertilizers

Abstract

Organic carbon (OC) in leaves of seven nitrogen (N₂)‐fixing trees and fifteen lignite‐based fertilizers was measured by loss‐on‐ignition (LOI at 500°C), wet oxidation by the Walkley‐Black method (CWB), Tinsley Dichromate Method (CTS), and dry combustion method using a LECO SC444 Carbon/ Sulphur Resistance Furnace Analyzer (CTO). There were significant differences in the capabilities of the methods in measuring OC from the organic materials with the quantity measured in the following order: LOI > CTO > CTS > CWB. A highly significant difference between LOI and CTO values suggested that components other than organic carbon (C) were removed by LOI since CTO gives total C value. The result also showed that N content in the organic materials was highly correlated with OC measured by individual methods. The LOI, CWB, and CTS were significantly correlated with CTO. The regression equations which were specific for either plant leaves or lignite‐based fertilizers indicated that any of the methods could be used to predict total C in the organic materials with a high degree of precision. In addition to the regression approach, an estimated correction factor of 1.4550 would be more appropriate to predict CTO from CWB for plant leaves than the 1.30 factor usually used for estimating oxidizable C in soils when CWB method is used. Also, a factor of 0.36180 could be used to estimate total C from LOI method for lignite fertilizers instead of merely regarding the difference in weight loss as the total organic matter.     

Quantification of Organic Carbon in Soils: A Comparison of Methodologies and Assessment of the Carbon Content of Organic Matter

Abstract

Renewed interest in temporal soil organic carbon (SOC) stock changes has stressed the importance of reliable methods for quantitative assessment of organic compound (OC) content. Particularly with the establishment of modern dry‐combustion analyzers, which are replacing the traditional wet‐oxidation methods, the need for correct relationships between both is of crucial importance for comparison of past and current SOC data in long‐term SOC stock change studies. Dry combustion with a Variomax CNS‐analyzer was the standard to evaluate three other methods for Belgian agricultural soils. Excellent linear relationships were found with the Walkey and Black method and the Springer and Klee method, whereas a Shimadzu TOC‐analyzer slightly underestimated the OC content. Precision of the investigated methods was comparable and tended to be dependent on the sample size used for measurement. The OC oxidation efficiency of the most widely applied method of Walkey and Black for the soils in this study was very close to the generally accepted 75%. Mass loss on ignition at 800°C could be very well related to the soil OC content and the clay content. The traditional factor of 1.724 used to convert OC measurements to organic matter percentages is not valid for the investigated soils, which demonstrates that rather regional‐specific factors (in this study 1.911) should be determined and adopted.     

Methods for estimating types of soil organic carbon and their application to surveys of UK urban areas

The occurrence of substantial quantities of black carbon (BC) in urban soil due to local dispersal following incomplete combustion of fossil fuel complicates the determination of labile soil organic carbon (SOC). Estimates of SOC content were made from loss on ignition (LOI) analyses undertaken on samples (0–15 cm depth) from comprehensive soil geochemical surveys of three UK urban areas. We randomly selected 10 samples from each decile of the LOI distribution for each of the surveys of Coventry (n = 808), Stoke‐on‐Trent (n = 737) and Glasgow (n = 1382) to investigate the proportions of labile SOC and BC. We determined their total organic carbon (TOC) and BC contents, and by difference the labile SOC content, and investigated the linear relationship of the latter with SOC estimates based on LOI analyses. There was no evidence for a difference in the slope of the regression for the three urban areas. We then used a linear regression of labile SOC based on LOI analyses (r² = 0.81) to predict labile SOC for all survey samples from the three urban areas. We attribute the significantly higher median BC concentrations in Glasgow (1.77%, compared with 0.46 and 0.59% in Coventry and Stoke‐on‐Trent) to greater dispersal of coal ash across the former. An analysis of the 30 samples showed that LOI at 450 °C accounts for a consistent proportion of BC in each sample (r² = 0.97). Differences between TOC (combustion at 1050 °C after removal of inorganic carbon) and an LOI estimate of SOC may be a cost‐effective method for estimation of BC. Previous approaches to estimation of urban SOC contents based on half the mean SOC content of the equivalent associations under pasture, underestimate the empirical mean value.     

Loss‐on‐Ignition in the Determination of Pools of Organic Carbon in Soils of Forests and Afforested Arable Fields

Abstract

Loss‐on‐ignition (LOI) and concentration of organic carbon (Cc) were determined on pristine forest soils and soils from afforested arable fields. The objectives were to investigate the relation between the Cc of soil estimated indirectly from LOI and true Cc from dry combustion (C_LECO) and further to evaluate how the applied analytical method affects the carbon pool estimates. According to results, LOI was a good indicator of Cc in the organic layer. As regards mineral soil, however, C_LECO/LOI ratio significantly decreased with increasing depth, and the ratio changed differently in soils underlying forest sites as opposed to the soils from former fields. The results indicate that estimation of carbon pools from conversion factors would lead to considerable bias and that direct measurement of Cc is preferable to the use of any Cc/LOI ratio. The results also emphasize the need for elimination of carbonate carbon when measuring Cc from the soil of arable fields.     

A Comparative Study of the Use of Organic Carbon and Loss on Ignition in Defining Tropical Organic Soil Materials

Organic soils or Histosols or peats as they are commonly referred to, are characterized by the presence of large amounts of organic soil materials (OSM), which is commonly quantified by the Walkley and Black (1934) (WB) method to determine the soil organic matter (SOM) using a correction factor of 1.724. SOM of Histosols is also identified through a combustion (loss on ignition, LOI) or elemental C-analysis (with a carbon-nitrogen-sulfur (CNS) analyzer with combustion and gas density detector). These methods were established using temperate and boreal peat deposits and here we demonstrate that tropical peat deposits require a modified approach. Typical SE-Asian tropical lowland peat pedons from rain forest and oil palm settings were sampled and the material analysed using a CNS analyzer, WB-C and LOI. The ratios for LOI:CNS-C for the 20 samples yielded values between 2.00–3.09 with a mean of 2.50 while the LOI:WB-C ratio yielded values from 1.75 to 2.58 with a mean of 1.94. A comparison of these values for topsoils and subsoils showed mean ratios (LOI:WB-C) of 1.94 and 1.89 for topsoils and subsoils, respectively. The forest samples had higher LOI:WB-C ratios than the subsoils from oil palm settings (1.94 vs 1.84). These values suggest that the standard factor of 1.724 to correct OSM to SOM for tropical soils is untenable. The values to convert CNS and WB-C values of tropical topsoils/subsoils to SOM or LOI should be 2.5 or 1.9, respectively. Our results indicate a significant difference in the soil organic carbon (SOC) of tropical lowland peats depending on the method used.     

Modified Soil‐Test Methods for Extractable Phosphorus in Acidic,Neutral, and Alkaline Soils

Abstract

Although numerous soil‐test methods for estimating extractable phosphorus (P) have been developed around the world, their results are difficult to compare because of the very different scale levels used. In the present study, the Bray–Kurtz method (Bray‐P) is used as a reference value. Two other methods [lactate‐P and sodium bicarbonate (NaHCO₃)‐P] were modified to facilitate the comparison of extractable‐P determinations, mainly by adjusting the shaking time. These three methods were applied to 101 soil samples from an extensive region of Argentina with soil pH values ranging from 5.5 to 8.5. The results confirm that the Bray‐P and the two modified methods (lactate‐P and NaHCO₃‐P) determine similar contents of extractable P but are not applicable to all types of soils and conditions. Equations that minimize the statistical error were selected for soil properties such as organic carbon (OC) content, pH, soluble salts, and calcium carbonate content. Correlation coefficients between Bray‐P and NaHCO₃‐P increased to 0.91 and 0.95 in soils with high and low OC levels, respectively. It was also demonstrated that the lactate‐P test is not suitable for soils rich in calcium carbonate or soluble salts. These two modified methods are expected to be useful for testing P values that impact agricultural production.     

Paddy management on different soil types does not promote lignin accumulation

Paddy soil management is generally thought to promote the accumulation of soil organic matter (SOM) and specifically lignin. Lignin is considered particularly susceptible to accumulation under these circumstances because of the recalcitrance of its aromatic structure to biodegradation under anaerobic conditions (i.e ., during inundation of paddy fields). The present study investigates the effect of paddy soil management on SOM composition in comparison to nearby agricultural soils that are not used for rice production (non‐paddy soils). Soil types typically used for rice cultivation were selected, including Alisol, Andosol and Vertisol sites in Indonesia (humid tropical climate of Java) and an Alisol site in China (humid subtropical climate, Jiangxi province). These soil types represent a range of soil properties to be expected in Asian paddy fields. All upper‐most A horizons were analysed for their SOM composition by solid‐state ¹³C nuclear magnetic resonance (NMR) spectroscopy and for lignin‐derived phenols by the CuO oxidation method. The SOM composition was similar for all of the above named parent soil types (non‐paddy soils) and was also not affected by paddy soil management. A substantial proportion (up to 23%) of the total aryl‐carbon in some paddy and non‐paddy soils was found to originate from condensed aromatic‐carbon (e.g ., charcoal). This may be attributed to the burning of crop residues. On average, the proportion of lignin was low and made up 20% of the total SOM, and showed no differences between straw, particulate organic matter (POM), and the bulk soil material. The results from CuO oxidation are consistent with the data obtained from solid‐state ¹³C NMR spectroscopy. The extraction of lignin‐derived phenols revealed low VSC (vanillyl, syringyl, cinnamyl) values for all investigated soils in a range (4 to 12 g kg⁻¹ OC) that was typical for agricultural soils. In comparison to adjacent non‐paddy soils, the data do not provide evidence for a substantial accumulation of phenolic lignin‐derived structures in the paddy soils, even for those characterized by higher organic carbon (OC) contents (e.g ., Andosol‐ and Alisol (China)‐derived paddy soils). We conclude that the properties of the parent soil types are more important for the lignin content of the soils than the effect of paddy management itself.     

Loss‐on‐Ignition Method to Assess Soil Organic Carbon in Calcareous Everglades Wetlands

Measurement of soil carbon (C) is important for determining the effects of Everglades restoration projects on C cycling and transformations. Accurate measurement of soil organic C by automated carbon–nitrogen–sulfur (CNS) analysis may be confounded by the presence of calcium carbonate (CaCO₃) in Everglades wetlands. The objectives of this study were to compare a loss‐on‐ignition (LOI) method with CNS analysis for assessment of soil C across a diverse group of calcareous Everglades wetlands. More than 3168 samples were taken from three soil depths (floc, 0–10, 10–30 cm) in 14 wetlands and analyzed for LOI, total C, and total calcium (Ca). The LOI method compared favorably to CNS analysis for LOI contents ranging from 0 to 1000 g kg^?1 and for soil total Ca levels from 0 to 500 g Ca kg^?1. For all wetlands and soil depths, LOI was significantly related to total C (r² = 0.957). However, LOI was a better predictor of total C when LOI exceeded 400 g kg^?1 because of less interference by CaCO₃. Total C measurement by CNS analysis was problematic in soils with high total Ca and low LOI, as the presence of CaCO₃ confounded C analysis for LOI less than 400 g kg^?1. Inclusion of total Ca in regression models with LOI significantly improved the prediction of total C. Estimates of total organic C by CNS analysis were obtained by accounting for C associated with CaCO₃ by calculation, with results being similar to total organic C values obtained from LOI analysis. The proportion of C in organic matter measured by the LOI method (51%) was accurate and applicable across wetlands, soil depths, and total Ca levels; thus LOI was a suitable indicator of total organic C in Everglades wetlands.     

Organic‐carbon fractions in an agricultural topsoil assessed by the determination of the soil mineral surface area

According to recent conceptual models, the organic carbon (OC) of soils can be divided into OC fractions of increasing stability from labile free OC to resistant OC associated with the soil mineral phase. In this study, we present a method for quantifying two OC fractions based on soil aggregate–size fractionation and the N₂ gas–adsorption method. For this purpose, we analyzed soil material of the plow layer of a Haplic Chernozem subjected to different fertilizer treatments (no fertilizer, mineral fertilizer, mineral and organic fertilizer). The total organic‐C concentration (TOC) and the clay content of the different size fractions were determined as well as the specific surface area (SSA_mineral) and the sample pore volume after thermal oxidation (OC‐free). The TOC of the different soil‐aggregate fractions was linearly related to SSA_mineral. Clay‐associated OC and nonassociated OC fractions of the different soil samples were quantified using two methods based on the OC surface loading at the clay fraction. The application of organic fertilizer increased the amount of nonassociated OC but hardly affected the concentration of clay‐associated OC. This finding agrees with previous studies on C dynamics in soils and indicates a finite capacity of soil materials to sequester OC. Even without any addition of organic fertilizer, the mineral phase of the analyzed soil material appears to be C‐saturated.