Loss-on-ignition for scalable soil carbon monitoring: separating useful method transfer equations from misleading conversion factors
Abstract. A central challenge for monitoring soil organic carbon (SOC) to support soil health assessment, national inventories, and carbon markets is the cost of sampling required to detect significant change over time. Direct measurement by dry combustion (DC) is relatively expensive and can limit sampling intensity. Loss-on-ignition (LOI) offers a low-cost alternative, but confusion persists regarding the sources of measurement error in LOI-derived SOC estimates across diverse soils. This study evaluated three LOI protocols that are in regular use today for measuring SOM and predicting SOC as measured by dry combustion (DC): ignition at 360 °C for 2 h (LOI360), 400 °C for 16 h (LOI400), and 550 °C for 3 h (LOI550), across 423 soil samples from contrasting landform regions, horizons, textures, and inorganic carbon contents. Method transfer equations were developed to relate soil organic matter (SOM) measured by LOI to SOC measured by DC. Those models were evaluated across multiple aspects of performance using measures of precision (R²), accuracy (RMSE, MAE, and MedAE), and overall agreement (concordance correlation coefficient). The use of regression to relate method results, rather than estimating the SOC:SOM conversion ratio, is emphasized. The repeatability of the methods was also assessed by performing multiple measurements and calculating the coefficient of variation. LOI360 and LOI400 produced comparable and relatively strong relationships with DC-SOC, whereas LOI550 exhibited substantially lower precision and accuracy because of additional mineral mass losses during ignition. Only minor improvements over generalized models were achieved by localizing equations based on landform region or soil horizon, which suggests that broadly applicable transfer functions are sufficient for most applications. While DC provided the highest repeatability (CV = 2.60 %), LOI400 demonstrated acceptable repeatability (CV = 5.3 %) and accuracy (RMSE = 0.63 SOC%). LOI400 was also favourable because its method transfer equation had an intercept that was close to zero. These results demonstrate that LOI, when using an optimized and standardized protocol, is a practical and scientifically defensible approach for large-scale SOC monitoring. Although LOI measurements have more measurement error than DC analyses, their substantially lower cost enables much higher sampling densities, improving the characterization of spatial variability and increasing statistical power to detect SOC change. Additionally, LOI400 can serve as a preliminary screening tool to identify zones of contrasting SOC and guide targeted DC analyses, while also supporting the development of large ground-based SOC datasets for remote sensing and machine learning approaches to digital SOC mapping and monitoring.
General comments
The manuscript is well presented with clear objectives and structure. It addresses a fundamental challenge in analytical soil science of accurately monitoring organic carbon content in soils, an area which has seen renewed interest due to climate change mitigation research and carbon markets and will be of broad international interest. The research quantified the relationship between dry combustion and three commonly used loss-on-ignition (LOI) protocols and rigorously evaluated the precision and accuracy of the method transfer equations associated with each LOI protocol and the variability due to measurement error using a suite of statistics. In doing so, the authors attempt to tackle the confusion around the diversity of method parameters used in LOI measurements (primarily temperature and duration) and clarify under what conditions LOI can be used as a scalable and defensible alternative to dry combustion.
Overall, I think this will be suitable for publication after a fundamental analytical query is clarified and some minor comments are addressed.
Main comment
I agree with the authors on their main issues surrounding LOI which has led to LOI being perceived as a low precision method for estimating SOC. They rightly point out lack of consensus on the optimal temperature and ignition duration for measuring SOM, how to account for any mass loss from clay minerals and the cost and time involved to measure both LOI-SOM and DC-SOC to create customized equations as confounding factors. This is explained and structured well within the manuscript. However, further clarification on the analytical procedures used to generate the TC, IC and SOC data in this study would be of benefit to the readers to convince us that comparison of the three LOI methods selected by the authors, which have different heating durations and temperatures, would enable the aim of the research to be met.
The conclusion that an optimized LOI protocol (LOI at 400 °C for 16 h) offered the best compromise among accuracy, repeatability, and scalability when compared with dry combustion analyses and can provide scientifically defensible soil organic carbon estimates at lower cost is a welcome contribution to the vast literature in this area but only if the analytical measurements that underpin this statistical analysis and hence conclusion are robust.
Specific comments:
2.4. Experimental design, Lines 344 – 347. Comparing the intrinsic measurement errors of the different methods.
Operator-related variability and many sample characteristics were considered by the authors that would affect analytical variability but how do the authors account for the variability caused by heterogeneity of the samples when comparing samples using widely different sample preparation techniques? Is it appropriate to expect agreement or compare accuracy, precision and variability of results obtained by a dry combustion method which uses a finely processed (<0.25mm), 30 mg sample size to a coarser (<2mm), 8 g sample size used in the LOI method? The difference in sample heterogeneity between fine and coarse particles and mg to g sample weights would be large (depending on soil type).
Would the accuracy, precision or variability of the LOI protocols improve and agree better with the DC results if you used finely processed (<0.25mm) soil for the LOI measurement i.e. standardised one of these parameters?
What would happen if you heated soil samples at 360°C for 16h, 400°C for 16h and 550 °C for 16 h standardising the heating duration? What about standardising the temperature at 400 °C then comparing results obtained from samples heated for 2 h, 3 h and 16 h duration?
Would your recommendation for the LOI400 protocol still stand if the analytical variability on the LOI measurements had been thoroughly investigated? Any comment?
Introduction, Paragraph 3, Lines 53 – 54 Despite its enduring widespread use as a low-cost assessment of soil fertility and health, LOI is perceived in the scientific community as insufficient for change detection.
References required here to support this statement. Perceived as insufficient for change detection by whom? I suggest this all-encompassing statement should be qualified or removed. LOI as a measure of soil organic matter content or indeed SOC can be sufficient for many researchers’ needs in the scientific community, it depends on the research context and soil type in question.
Introduction, Paragraph 4, Lines 67 – 69 This paper proposes using method transfer equations derived from linear regression, offering a more flexible alternative to fixed conversion factors, which are limited in their ability to account for non-SOM mass losses during LOI.and
Introduction, Paragraph 6, Lines 84 – 86
This approach offers a simple and inexpensive alternative because it estimates SOM from the mass lost after heating soil in a muffle furnace, and it has been widely used to estimate SOC using a standard conversion such as the van Bemmelen factor (Schulte and Hopkins, 1996)
I question whether many people who use LOI as a measure of SOM actually still use the van Bemmelen conversion factor to calculate SOC directly? I believe most current researchers use their own ground truthing with some form of dry combustion analysis combined with stable isotope analysis (δ13C) or Thermogravimetric analysis (TGA) to understand the mineral/inorganic component of their samples then use their own empirical equations, site-specific conversion factor and/or linear regression-based models. The references included to support this statement in this section of the manuscript are very few and quite old. Any further comment on how widespread the use of a LOI measurement with a standard conversion to estimate SOC is? Are there any more recent examples?
Materials and Methods
Some further detail on the laboratory analyses is required to allow the reader to determine whether the analysis has been carried out robustly.
2.2. Lab analysis , 2.2.1. Dry combustion Lines 210 – 215 and 221 – 222. More details of the sample preparation steps prior to DC would be helpful to give an understanding of sample homogenisation and additional details on the DC instrument and methods of analysis for TC and IC such as:
Were any official methods used i.e. ISO or UNE methods as referencing a method would save adding a lot of additional detail to this text?
2.2.2. Loss on ignition Line 233. Sixty-two Fisher brand FB-965-E crucibles were filled with 8 g of < 2-mm oven-dry soil per run.
Line 239. Was there a specific reason why LOI was presented in g kg-1 rather than the usual % value?
Minor Comments:
Results and Discussion 3.3. Repeatability and evaluation of measurement error, Line 609 multi-sensor SOC models that use different indices (e.g., NDVI, SAVI, EVI)
It would be helpful to readers unfamiliar with these metrics to include abbreviations in full i.e. normalised difference vegetation index and so on.
Technical Correction:
References, Line 790 Stanley, P., et al
Check – publication title split unnecessarily over two lines